40 CFR 60.748 Pt. 60, App. A, Meth. 1A
1.1 The applicability and principle of this method are identical to
Method 1, except this method's applicability is limited to stacks or
ducts less than about 0.30 meter (12 in.) in diameter or 0.071 m /2/
(113 in. /2/ ) in cross-sectional area, but equal to or greater than
about 0.10 meter (4 in.) in diameter or 0.0081 m /2/ (12.57 in. /2/ )
in cross-sectional area.
1.2 In these small diameter stacks or ducts, the conventional Method
5 stack assembly (consisting of a Type S pitot tube attached to a
sampling probe, equipped with a nozzle and thermocouple) blocks a
significant portion of the cross section of the duct and causes
inaccurate measurements. Therefore, for particulate matter (PM)
sampling in small stacks or ducts, the gas velocity is measured using a
standard pitot tube downstream of the actual emission sampling site.
The straight run of duct between the PM sampling and velocity
measurement sites allows the flow profile, temporarily disturbed by the
presence of the sampling probe, to redevelop and stabilize.
1.3 The cross-sectional layout and location of traverse points and
the verification of the absence of cyclonic flow are the same as in
Method 1, Sections 2.3 and 2.4, respectively. Differences from Method 1,
except as noted, are given below.
2.1 Selection of Sampling and Measurement Sites.
2.1.1 PM Measurements. Select a PM sampling site located preferably
at least 8 equivalent stack or duct diameters downstream and 10
equivalent diameters upstream from any flow disturbances such as bends,
expansions, or contractions in the stack, or from a visible flame.
Next, locate the velocity measurement site 8 equivalent diameters
downstream of the PM sampling site. See Figure 1A-1. If such locations
are not available, select an alternative PM sampling site that is at
least 2 equivalent stack or duct diameters downstream and 2 1/2
diameters upstream from any flow disturbance. Then, locate the velocity
measurement site 2 equivalent diameters downstream from the PM sampling
site. Follow Section 2.1 of Method 1 for calculating equivalent
diameters for a rectangular cross section.
Insert Illustration 0 807
2.1.2 PM Sampling (Steady Flow) or only Velocity Measurements. For
PM sampling when the volumetric flow rate in a duct is constant with
respect to time, Section 2.1 of Method 1 may be followed, with the PM
sampling and velocity measurement performed at one location. To
demonstrate that the flow rate is constant (within 10 percent) when PM
measurements are made, perform complete velocity traverses before and
after the PM sampling run, and calculate the deviation of the flow rate
derived after the PM sampling run from the one derived before the PM
sampling run. The PM sampling run is acceptable if the deviation does
not exceed 10 percent.
2.2 Determining the Number of Traverse Points.
2.2.1 PM Sampling. Use Figure 1-1 of Method 1 to determine the
number of traverse points to use at both the velocity measurement and PM
sampling locations. Before referring to the figure, however, determine
the distances between both the velocity measurement and PM sampling
sites to the nearest upstream and downstream disturbances. Then divide
each distance by the stack diameter or equivalent diameter to express
the distances in terms of the number of duct diameters. Next, determine
the number of traverse points from Figure 1-1 of Method 1 corresponding
to each of these four distances. Choose the highest of the four numbers
of traverse points (or a greater number) so that, for circular ducts,
the number is a multiple of four, and for rectangular ducts, the number
is one of those shown in Table 1-1 of Method 1. When the optimum duct
diameter location criteria can be satisfied, the minimum number of
traverse points required is eight for circular ducts and nine for
rectangular ducts.
2.2.2 PM Sampling (Steady Flow) or Velocity Measurements. Use Figure
1-2 of Method 1 to determine the number of traverse points, following
the same procedure used for PM sampling traverses as described in
Section 2.2.1 of Method 1. When the optimum duct diameter location
criteria can be satisfied, the minimum number of traverse points
required is eight for circular ducts and nine for rectangular ducts.
1. Same as in Method 1, Section 3, Citations 1 through 6.
2. Vollaro, Robert F. Recommended Procedure for Sample Traverses in
Ducts Smaller Than 12 Inches in Diameter. U.S. Environmental Protection
Agency, Emission Measurement Branch, Research Triangle Park, NC.
January 1977.
40 CFR 60.748 Pt. 60, App. A, Meth. 2
1. Principle and Applicability
1.1 Principle. The average gas velocity in a stack is determined from
the gas density and from measurement of the average velocity head with a
Type S (Stausscheibe or reverse type) pitot tube.
1.2 Applicability. This method is applicable for measurement of the
average velocity of a gas stream and for quantifying gas flow.
This procedure is not applicable at measurement sites which fail to
meet the criteria of Method 1, Section 2.1. Also, the method cannot be
used for direct measurement in cyclonic or swirling gas streams;
Section 2.4 of Method 1 shows how to determine cyclonic or swirling flow
conditions. When unacceptable conditions exist, alternative procedures,
subject to the approval of the Administrator, U.S. Environmental
Protection Agency, must be employed to make accurate flow rate
determinations; examples of such alternative procedures are: (1) to
install straightening vanes; (2) to calculate the total volumetric flow
rate stoichiometrically, or (3) to move to another measurement site at
which the flow is acceptable.
2. Apparatus
Specifications for the apparatus are given below. Any other
apparatus that has been demonstrated (subject to approval of the
Administrator) to be capable of meeting the specifications will be
considered acceptable.
Insert illus. 204B
2.1 Type S Pitot Tube. The Type S pitot tube (Figure 2-1) shall be
made of metal tubing (e.g., stainless steel). It is recommended that
the external tubing diameter (dimension Dt Figure 2-2b) be between 0.48
and 0.95 centimeter ( 3/16 and 3/8 inch). There shall be an equal
distance from the base of each leg of the pitot tube to its face-opening
plane (dimensions PA and PB Figure 2-2b); it is recommended that this
distance be between 1.05 and 1.50 times the external tubing diameter.
The face openings of the pitot tube shall, preferably, be aligned as
shown in Figure 2-2; however, slight misalignments of the openings are
permissible (see Figure 2-3).
The Type S pitot tube shall have a known coefficient, determined as
outlined in Section 4. An identification number shall be assigned to
the pitot tube; this number shall be permanently marked or engraved on
the body of the tube.
Insert illus.
OMITT500000000 ED
Insert illus.
OMITT500000000 ED
shown in: (a) end view; face opening planes
perpendicular to transverse axis; (b) top view; face
opening planes parallel to longitudinal axis; (c)
side view; both legs of equal length and centerlines
coincident, when viewed from both sides. Baseline
coefficient values of 0.84 may be assigned to pitot
tubes constructed this way.
Insert illus.
OMITT500000000 ED
result from field use or improper construction of Type
S pitot tubes. These will not affect the baseline
value of Cp(s) so long as 1 and 2 10 , 1 and 2
5 , z 0.32 cm (1/8 in.) and w 0.08 cm (1/32 in.)
(citation 11 in Bibliography).
A standard pitot tube may be used instead of a Type S, provided that
it meets the specifications of Sections 2.7 and 4.2; note, however,
that the static and impact pressure holes of standard pitot tubes are
susceptible to plugging in particulate-laden gas streams. Therefore,
whenever a standard pitot tube is used to perform a traverse, adequate
proof must be furnished that the openings of the pitot tube have not
plugged up during the traverse period; this can be done by taking a
velocity head ( p) reading at the final traverse point, cleaning out the
impact and static holes of the standard pitot tube by ''back-purging''
with pressurized air, and then taking another p reading. If the p
readings made before and after the air purge are the same ( 5 percent),
the traverse is acceptable. Otherwise, reject the run. Note that if p
at the final traverse point is unsuitably low, another point may be
selected. If ''back-purging'' at regular intervals is part of the
procedure, then comparative p readings shall be taken, as above, for
the last two back purges at which suitably high p readings are
observed.
2.2 Differential Pressure Gauge. An inclined manometer or equivalent
device is used. Most sampling trains are equipped with a 10-in. (water
column) inclined-vertical manometer, having 0.01-in. H2O divisions on
the 0-to 1-in. inclined scale, and 0.1-in. H2O divisions on the 1- to
10-in. vertical scale. This type of manometer (or other gauge of
equivalent sensitivity) is satisfactory for the measurement of p values
as low as 1.3 mm (0.05 in.) H2O. However, a differential pressure gauge
of greater sensitivity shall be used (subject to the approval of the
Administrator), if any of the following is found to be true: (1) the
arithmetic average of all p readings at the traverse points in the
stack is less than 1.3 mm (0.05 in.) H2O; (2) for traverses of 12 or
more points, more than 10 percent of the individual p readings are
below 1.3 mm (0.05 in.) H2O; (3) for traverses of fewer than 12 points,
more than one p reading is below 1.3 mm (0.05 in.) H2O. Citation 18 in
Bibliography describes commercially available instrumentation for the
measurement of low-range gas velocities.
As an alternative to criteria (1) through (3) above, the following
calculation may be performed to determine the necessity of using a more
sensitive differential pressure gauge:
Insert illus. 207
Where:
pi=Individual velocity head reading at a traverse point, mm H2O (in.
H2O).
n=Total number of traverse points.
K=0.13 mm H2O when metric units are used and 0.005 in. H2O when
English units are used.
If T is greater than 1.05, the velocity head data are unacceptable
and a more sensitive differential pressure gauge must be used.
Note: If differential pressure gauges other than inclined manometers
are used (e.g., magnehelic gauges), their calibration must be checked
after each test series. To check the calibration of a differential
pressure gauge, compare p readings of the gauge with those of a
gauge-oil manometer at a minimum of three points, approximately
representing the range of p values in the stack. If, at each point,
the values of p as read by the differential pressure gauge and
gauge-oil manometer agree to within 5 percent, the differential pressure
gauge shall be considered to be in proper calibration. Otherwise, the
test series shall either be voided, or procedures to adjust the measured
p values and final results shall be used subject to the approval of the
Administrator.
2.3 Temperature Gauge. A thermocouple, liquid-filled bulb
thermometer, bimetallic thermometer, mercury-in-glass thermometer, or
other gauge, capable of measuring temperature to within 1.5 percent of
the minimum absolute stack temperature shall be used. The temperature
gauge shall be attached to the pitot tube such that the sensor tip does
not touch any metal; the gauge shall be in an interference-free
arrangement with respect to the pitot tube face openings (see Figure 2-1
and also Figure 2-7 in Section 4). Alternative positions may be used if
the pitot tube-temperature gauge system is calibrated according to the
procedure of Section 4. Provided that a difference of not more than 1
percent in the average velocity measurement is introduced, the
temperature gauge need not be attached to the pitot tube; this
alternative is subject to the approval of the Administrator.
2.4 Pressure Probe and Gauge. A piezometer tube and mercury- or
water-filled U-tube manometer capable of measuring stack pressure to
within 2.5 mm (0.1 in.) Hg is used. The static tap of a standard type
pitot tube or one leg of a Type S pitot tube with the face opening
planes positioned parallel to the gas flow may also be used as the
pressure probe.
2.5 Barometer. A mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg) may be
used. In many cases, the barometric reading may be obtained from a
nearby National Weather Service station, in which case the station value
(which is the absolute barometric pressure) shall be requested and an
adjustment for elevation differences between the weather station and the
sampling point shall be applied at a rate of minus 2.5 mm (0.1 in.) Hg
per 30-meter (100 foot) elevation increase or vice-versa for elevation
decrease.
2.6 Gas Density Determination Equipment. Method 3 equipment, if
needed (see Section 3.6), to determine the stack gas dry molecular
weight, and Reference Method 4 or Method 5 equipment for moisture
content determination; other methods may be used subject to approval of
the Administrator.
2.7 Calibration Pitot Tube. When calibration of the Type S pitot
tube is necessary (see Section 4), a standard pitot tube is used as a
reference. The standard pitot tube shall, preferably, have a known
coefficient, obtained either (1) directly from the National Bureau of
Standards, Route 270, Quince Orchard Road, Gaithersburg, Maryland, or
(2) by calibration against another standard pitot tube with an
NBS-traceable coefficient. Alternatively, a standard pitot tube
designed according to the criteria given in 2.7.1 through 2.7.5 below
and illustrated in Figure 2-4 (see also Citations 7, 8, and 17 in
Bibliography) may be used. Pitot tubes designed according to these
specifications will have baseline coefficients of about 0.99 0.01.
2.7.1 Hemispherical (shown in Figure 2-4), ellipsoidal, or conical
tip.
2.7.2 A minimum of six diameters straight run (based upon D, the
external diameter of the tube) between the tip and the static pressure
holes.
2.7.3 A minimum of eight diameters straight run between the static
pressure holes and the centerline of the external tube, following the 90
degree bend.
2.7.4 Static pressure holes of equal size (approximately 0.1 D),
equally spaced in a piezometer ring configuration.
2.7.5 Ninety degree bend, with curved or mitered junction.
2.8 Differential Pressure Gauge for Type S Pitot Tube Calibration.
An inclined manometer or equivalent is used. If the single-velocity
calibration technique is employed (see Section 4.1.2.3), the calibration
differential pressure gauge shall be readable to the nearest 0.13 mm H2O
(0.005 in. H2O). For multivelocity calibrations, the gauge shall be
readable to the nearest 0.13 mm H2O (0.005 in. H2O) for p values
between 1.3 and 25 mm H2O (0.05 and 1.0 in. H2O), and to the nearest 1.3
mm H2O (0.05 in. H2O) for p values above 25 mm H2O (1.0 in. H2O). A
special, more sensitive gauge will be required to read p values below
1.3 mm H2O (0.05 in. H2O) (see Citation 18 in Bibliography).
Insert illus. 208
3. Procedure
3.1 Set up the apparatus as shown in Figure 2-1. Capillary tubing or
surge tanks installed between the manometer and pitot tube may be used
to dampen p fluctuations. It is recommended, but not required, that a
pretest leak-check be conducted, as follows: (1) blow through the pitot
impact opening until at least 7.6 cm (3 in.) H2O velocity pressure
registers on the manometer; then, close off the impact opening. The
pressure shall remain stable for at least 15 seconds; (2) do the same
for the static pressure side, except using suction to obtain the minimum
of 7.6 cm (3 in.) H2O. Other leak-check procedures, subject to the
approval of the Administrator, may be used.
3.2 Level and zero the manometer. Because the manometer level and
zero may drift due to vibrations and temperature changes, make periodic
checks during the traverse. Record all necessary data as shown in the
example data sheet (Figure 2-5).
3.3 Measure the velocity head and temperature at the traverse points
specified by Method 1. Ensure that the proper differential pressure
gauge is being used for the range of p values encountered (see Section
2.2). If it is necessary to change to a more sensitive gauge, do so, and
remeasure the p and temperature readings at each traverse point.
Conduct a post-test leak-check (mandatory), as described in Section 3.1
above, to validate the traverse run.
3.4 Measure the static pressure in the stack. One reading is usually
adequate.
3.5 Determine the atmospheric pressure.
Insert illus. 209
3.6 Determine the stack gas dry molecular weight. For combustion
processes or processes that emit essentially CO2, O2, CO, and N2, use
Method 3. For processes emitting essentially air, an analysis need not
be conducted; use a dry molecular weight of 29.0. For other processes,
other methods, subject to the approval of the Administrator, must be
used.
3.7 Obtain the moisture content from Reference Method 4 (or
equivalent) or from Method 5.
3.8 Determine the cross-sectional area of the stack or duct at the
sampling location. Whenever possible, physically measure the stack
dimensions rather than using blueprints.
4. Calibration
4.1 Type S Pitot Tube. Before its initial use, carefully examine the
Type S pitot tube in top, side, and end views to verify that the face
openings of the tube are aligned within the specifications illustrated
in Figure 2-2 or 2-3. The pitot tube shall not be used if it fails to
meet these alignment specifications.
After verifying the face opening alignment, measure and record the
following dimensions of the pitot tube: (a) the external tubing
diameter (dimension Dt, Figure 2-2b); and (b) the base-to-opening plane
distances (dimensions PA and PB, Figure 2-2b). If Dt is between 0.48
and 0.95 cm ( 3/16 and 3/8 in.) and if PA and PB are equal and between
1.05 and 1.50 Dt, there are two possible options: (1) the pitot tube
may be calibrated according to the procedure outlined in Sections 4.1.2
through 4.1.5 below, or (2) a baseline (isolated tube) coefficient value
of 0.84 may be assigned to the pitot tube. Note, however, that if the
pitot tube is part of an assembly, calibration may still be required,
despite knowledge of the baseline coefficient value (see Section 4.1.1).
If Dt, PA, and PB are outside the specified limits, the pitot tube
must be calibrated as outlined in 4.1.2 through 4.1.5 below.
4.1.1 Type S Pitot Tube Assemblies. During sample and velocity
traverses, the isolated Type S pitot tube is not always used; in many
instances, the pitot tube is used in combination with other
source-sampling components (thermocouple, sampling probe, nozzle) as
part of an ''assembly.'' The presence of other sampling components can
sometimes affect the baseline value of the Type S pitot tube coefficient
(Citation 9 in Bibliography); therefore an assigned (or otherwise
known) baseline coefficient value may or may not be valid for a given
assembly. The baseline and assembly coefficient values will be
identical only when the relative placement of the components in the
assembly is such that aerodynamic interference effects are eliminated.
Figures 2-6 through 2-8 illustrate interference-free component
arrangements for Type S pitot tubes having external tubing diameters
between 0.48 and 0.95 cm ( 3/16 and 3/8 in.). Type S pitot tube
assemblies that fail to meet any or all of the specifications of Figures
2-6 through 2-8 shall be calibrated according to the procedure outlined
in Sections 4.1.2 through 4.1.5 below, and prior to calibration, the
values of the intercomponent spacings (pitot-nozzle, pitot-thermocouple,
pitot-probe sheath) shall be measured and recorded.
Note: Do not use any Type S pitot tube assembly which is constructed
such that the impact pressure opening plane of the pitot tube is below
the entry plane of the nozzle (see Figure 2-6b).
4.1.2 Calibration Setup. If the Type S pitot tube is to be
calibrated, one leg of the tube shall be permanently marked A, and the
other, B. Calibration shall be done in a flow system having the
following essential design features:
Insert illus. 210
Figure 2-6. Proper pitot tube-sampling nozzle configuration to
prevent aerodynamic interference; buttonhook-type nozzle; centers of
nozzle and pitot opening aligned; Dt between 0.48 and 0.95 cm ( 3/16
and 3/8 in.).
Insert illus. 211, and 212
4.1.2.1 The flowing gas stream must be confined to a duct of definite
cross-sectional area, either circular or rectangular. For circular
cross-sections, the minimum duct diameter shall be 30.5 cm (12 in.);
for rectangular cross-sections, the width (shorter side) shall be at
least 25.4 cm (10 in.).
4.1.2.2 The cross-sectional area of the calibration duct must be
constant over a distance of 10 or more duct diameters. For a
rectangular cross-section, use an equivalent diameter, calculated from
the following equation, to determine the number of duct diameters:
Where:
De=Equivalent diameter
L=Length
W=Width
To ensure the presence of stable, fully developed flow patterns at
the calibration site, or ''test section,'' the site must be located at
least eight diameters downstream and two diameters upstream from the
nearest disturbances.
Note: The eight- and two-diameter criteria are not absolute; other
test section locations may be used (subject to approval of the
Administrator), provided that the flow at the test site is stable and
demonstrably parallel to the duct axis.
4.1.2.3 The flow system shall have the capacity to generate a
test-section velocity around 915 m/min (3,000 ft/min). This velocity
must be constant with time to guarantee steady flow during calibration.
Note that Type S pitot tube coefficients obtained by single-velocity
calibration at 915 m/min (3,000 ft/min) will generally be valid to
within 3 percent for the measurement of velocities above 305 m/min
(1,000 ft/min) and to within 5 to 6 percent for the measurement of
velocities between 180 and 305 m/min (600 and 1,000 ft/min). If a more
precise correlation between Cp and velocity is desired, the flow system
shall have the capacity to generate at least four distinct,
time-invariant test-section velocities covering the velocity range from
180 to 1,525 m/min (600 to 5,000 ft/min), and calibration data shall be
taken at regular velocity intervals over this range (see Citations 9 and
14 in Bibliography for details).
4.1.2.4 Two entry ports, one each for the standard and Type S pitot
tubes, shall be cut in the test section; the standard pitot entry port
shall be located slightly downstream of the Type S port, so that the
standard and Type S impact openings will lie in the same cross-sectional
plane during calibration. To facilitate alignment of the pitot tubes
during calibration, it is advisable that the test section be constructed
of plexiglas or some other transparent material.
4.1.3 Calibration Procedure. Note that this procedure is a general
one and must not be used without first referring to the special
considerations presented in Section 4.1.5. Note also that this procedure
applies only to single-velocity calibration. To obtain calibration data
for the A and B sides of the Type S pitot tube, proceed as follows:
4.1.3.1 Make sure that the manometer is properly filled and that the
oil is free from contamination and is of the proper density. Inspect
and leak-check all pitot lines; repair or replace if necessary.
4.1.3.2 Level and zero the manometer. Turn on the fan and allow the
flow to stabilize. Seal the Type S entry port.
4.1.3.3 Ensure that the manometer is level and zeroed. Position the
standard pitot tube at the calibration point (determined as outlined in
Section 4.1.5.1), and align the tube so that its tip is pointed directly
into the flow. Particular care should be taken in aligning the tube to
avoid yaw and pitch angles. Make sure that the entry port surrounding
the tube is properly sealed.
4.1.3.4 Read pstd and record its value in a data table similar to
the one shown in Figure 2-9. Remove the standard pitot tube from the
duct and disconnect it from the manometer. Seal the standard entry
port.
4.1.3.5 Connect the Type S pitot tube to the manometer. Open the
Type S entry port. Check the manometer level and zero. Insert and
align the Type S pitot tube so that its A side impact opening is at the
same point as was the standard pitot tube and is pointed directly into
the flow. Make sure that the entry port surrounding the tube is
properly sealed.
4.1.3.6 Read p8 and enter its value in the data table. Remove the
Type S pitot tube from the duct and disconnect it from the manometer.
4.1.3.7 Repeat steps 4.1.3.3 through 4.1.3.6 above until three pairs
of p readings have been obtained.
4.1.3.8 Repeat steps 4.1.3.3 through 4.1.3.7 above for the B side of
the Type S pitot tube.
4.1.3.9 Perform calculations, as described in Section 4.1.4 below.
4.1.4 Calculations.
4.1.4.1 For each of the six pairs of p readings (i.e., three from
side A and three from side B) obtained in Section 4.1.3 above, calculate
the value of the Type S pitot tube coefficient as follows:
Insert illus. 213
Insert illus. 214
Where:
Cp(s)=Type S pitot tube coefficient
Cp(std)=Standard pitot tube coefficient; use 0.99 if the coefficient
is unknown and the tube is designed according to the criteria of
Sections 2.7.1 to 2.7.5 of this method.
pstd=Velocity head measured by the standard pitot tube, cm H2O (in.
H2O)
ps=Velocity head measured by the Type S pitot tube, cm H2O (in.
H2O)
4.1.4.2 Calculate C8p (side A), the mean A-side coefficient, and C8p
(side B), the mean B-side coefficient: calculate the difference between
these two average values.
4.1.4.3 Calculate the deviation of each of the three A-side values of
Cp(s) from C8p (side A), and the deviation of each B-side value of Cp(s)
from C8p (side B). Use the following equation:
Insert illus. 215
4.1.4.4 Calculate s, the average deviation from the mean, for both
the A and B sides of the pitot tube. Use the following equation:
Insert illus. 216
4.1.4.5 Use the Type S pitot tube only if the values of s (side A)
and s (side B) are less than or equal to 0.01 and if the absolute value
of the difference between C8p (A) and C8p (B) is 0.01 or less.
4.1.5 Special considerations.
4.1.5.1 Selection of calibration point.
4.1.5.1.1 When an isolated Type S pitot tube is calibrated, select a
calibration point at or near the center of the duct, and follow the
procedures outlined in Sections 4.1.3 and 4.1.4 above. The Type S pitot
coefficients so obtained, i.e., C8p (side A) and C8p (side B), will be
valid, so long as either: (1) the isolated pitot tube is used; or (2)
the pitot tube is used with other components (nozzle, thermocouple,
sample probe) in an arrangement that is free from aerodynamic
interference effects (see Figures 2-6 through 2-8).
4.1.5.1.2 For Type S pitot tube-thermocouple combinations (without
sample probe), select a calibration point at or near the center of the
duct, and follow the procedures outlined in Sections 4.1.3 and 4.1.4
above. The coefficients so obtained will be valid so long as the pitot
tube-thermocouple combination is used by itself or with other components
in an interference-free arrangement (Figures 2-6 and 2-8).
4.1.5.1.3 For assemblies with sample probes, the calibration point
should be located at or near the center of the duct; however, insertion
of a probe sheath into a small duct may cause significant
cross-sectional area blockage and yield incorrect coefficient values
(Citation 9 in Bibliography). Therefore, to minimize the blockage
effect, the calibration point may be a few inches off-center if
necessary. The actual blockage effect will be negligible when the
theoretical blockage, as determined by a projected-area model of the
probe sheath, is 2 percent or less of the duct cross-sectional area for
assemblies without external sheaths (Figure 2-10a), and 3 percent or
less for assemblies with external sheaths (Figure 2-10b).
4.1.5.2 For those probe assemblies in which pitot tube-nozzle
interference is a factor (i.e., those in which the pitot-nozzle
separation distance fails to meet the specification illustrated in
Figure 2-6a), the value of Cp(s) depends upon the amount of free-space
between the tube and nozzle, and therefore is a function of nozzle size.
In these instances, separate calibrations shall be performed with each
of the commonly used nozzle sizes in place. Note that the
single-velocity calibration technique is acceptable for this purpose,
even though the larger nozzle sizes ( 0.635 cm or 1/4 in.) are not
ordinarily used for isokinetic sampling at velocities around 915 m/min
(3,000 ft/min), which is the calibration velocity; note also that it is
not necessary to draw an isokinetic sample during calibration (see
Citation 19 in Section 6).
4.1.5.3 For a probe assembly constructed such that its pitot tube is
always used in the same orientation, only one side of the pitot tube
need be calibrated (the side which will face the flow). The pitot tube
must still meet the alignment specifications of Figure 2-2 or 2-3,
however, and must have an average deviation (s) value of 0.01 or less
(see Section 4.1.4.4).
Insert illus. 217
4.1.6 Field Use and Recalibration.
4.1.6.1 Field Use.
4.1.6.1.1 When a Type S pitot tube (isolated tube or assembly) is
used in the field, the appropriate coefficient value (whether assigned
or obtained by calibration) shall be used to perform velocity
calculations. For calibrated Type S pitot tubes, the A side coefficient
shall be used when the A side of the tube faces the flow, and the B side
coefficient shall be used when the B side faces the flow;
alternatively, the arithmetic average of the A and B side coefficient
values may be used, irrespective of which side faces the flow.
4.1.6.1.2 When a probe assembly is used to sample a small duct (12 to
36 in. in diameter), the probe sheath sometimes blocks a significant
part of the duct cross-section, causing a reduction in the effective
value of Cp(s). Consult Citation 9 in Bibliography for details.
Conventional pitot-sampling probe assemblies are not recommended for use
in ducts having inside diameters smaller than 12 inches (Citation 16 in
Bibliography).
4.1.6.2 Recalibration.
4.1.6.2.1 Isolated Pitot Tubes. After each field use, the pitot tube
shall be carefully reexamined in top, side, and end views. If the pitot
face openings are still aligned within the specifications illustrated in
Figure 2-2 or 2-3, it can be assumed that the baseline coefficient of
the pitot tube has not changed. If, however, the tube has been damaged
to the extent that it no longer meets the specifications of Figure 2-2
or 2-3, the damage shall either be repaired to restore proper alignment
of the face openings or the tube shall be discarded.
4.1.6.2.2 Pitot Tube Assemblies. After each field use, check the
face opening alignment of the pitot tube, as in Section 4.1.6.2.1;
also, remeasure the intercomponent spacings of the assembly. If the
intercomponent spacings have not changed and the face opening alignment
is acceptable, it can be assumed that the coefficient of the assembly
has not changed. If the face opening alignment is no longer within the
specifications of Figures 2-2 or 2-3, either repair the damage or
replace the pitot tube (calibrating the new assembly, if necessary). If
the intercomponent spacings have changed, restore the original spacings
or recalibrate the assembly.
4.2 Standard pitot tube (if applicable). If a standard pitot tube is
used for the velocity traverse, the tube shall be constructed according
to the criteria of Section 2.7 and shall be assigned a baseline
coefficient value of 0.99. If the standard pitot tube is used as part of
an assembly, the tube shall be in an interference-free arrangement
(subject to the approval of the Administrator).
4.3 Temperature Gauges. After each field use, calibrate dial
thermometers, liquid-filled bulb thermometers,
thermocouple-potentiometer systems, and other gauges at a temperature
within 10 percent of the average absolute stack temperature. For
temperatures up to 405 C (761 F), use an ASTM mercury-in-glass
reference thermometer, or equivalent, as a reference; alternatively,
either a reference thermocouple and potentiometer (calibrated by NBS) or
thermometric fixed points, e.g., ice bath and boiling water (corrected
for barometric pressure) may be used. For temperatures above 405 C
(761 F), use an NBS-calibrated reference thermocouple-potentiometer
system or an alternate reference, subject to the approval of the
Administrator.
If, during calibration, the absolute temperatures measured with the
gauge being calibrated and the reference gauge agree within 1.5 percent,
the temperature data taken in the field shall be considered valid.
Otherwise, the pollutant emission test shall either be considered
invalid or adjustments (if appropriate) of the test results shall be
made, subject to the approval of the Administrator.
4.4 Barometer. Calibrate the barometer used against a mercury
barometer.
5. Calculations
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after final
calculation.
5.1 Nomenclature.
A=Cross-sectional area of stack, m2 (ft2).
Bws=Water vapor in the gas stream (from Method 5 or Reference Method
4), proportion by volume.
Cp=Pitot tube coefficient, dimensionless.
Kp=Pitot tube constant,
Insert illus. 218
for the metric system and
Insert illus. 219
for the English system.
Md=Molecular weight of stack gas, dry basis (see Section 3.6)
g/g-mole (lb/lb-mole).
Ms=Molecular weight of stack gas, wet basis, g/g-mole (lb/lb-mole).
=Md (1^Bws) +18.0 Bws
Eq. 2-5
Pbar=Barometric pressure at measurement site, mm Hg (in. Hg).
Pg=Stack static pressure, mm Hg (in. Hg).
Ps=Absolute stack gas pressure, mm Hg (in. Hg).
=Pbar+Pg
Eq. 2-6
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
Qsd=Dry volumetric stack gas flow rate corrected to standard
conditions, dscm/hr (dscf/hr).
ts=Stack temperature, C ( F).
Ts=Absolute stack temperature, K, ( R).
=273+ts for metric.
Eq. 2-7
=460+ts for English.
Eq. 2-8
Tstd=Standard absolute temperature, 293 K (528 R).
vs=Average stack gas velocity, m/sec (ft/sec).
p=Velocity head of stack gas, mm H2O (in. H2O).
3,600=Conversion factor, sec/hr.
18.0=Molecular weight of water, g/g-mole (lb/lb-mole).
5.2 Average Stack Gas Velocity.
Insert illus. 220
5.3 Average Stack Gas Dry Volumetric Flow Rate.
Eq. 2-10
To convert Qsd from dscm/hr (dscf/hr) to dscm/min (dscf/min), divide
Qsd by 60.
6. Bibliography
1. Mark, L. S. Mechanical Engineers' Handbook. New York,
McGraw-Hill Book Co., Inc. 1951.
2. Perry, J. H. Chemical Engineers' Handbook. New York.
McGraw-Hill Book Co., Inc. 1960.
3. Shigehara, R. T., W. F. Todd, and W. S. Smith. Significance of
Errors in Stack Sampling Measurements. U.S. Environmental Protection
Agency, Research Triangle Park, NC (Presented at the Annual Meeting of
the Air Pollution Control Association, St. Louis, MO, June 14-19, 1970.)
4. Standard Method for Sampling Stacks for Particulate Matter. In:
1971 Book of ASTM Standards, Part 23. Philadelphia, PA 1971. ASTM
Designation D-2928-71.
5. Vennard, J. K. Elementary Fluid Mechanics. New York. John Wiley
and Sons, Inc. 1947.
6. Fluid Meters -- Their Theory and Application. American Society of
Mechanical Engineers, New York, NY 1959.
7. ASHRAE Handbook of Fundamentals. 1972. p. 208.
8. Annual Book of ASTM Standards, Part 26. 1974. p. 648.
9. Vollaro, R. F. Guidelines for Type S Pitot Tube Calibration.
U.S. Environmental Protection Agency. Research Triangle Park, NC
(Presented at 1st Annual Meeting, Source Evaluation Society, Dayton, OH,
September 18, 1975.)
10. Vollaro, R. F. A Type S Pitot Tube Calibration Study. U.S.
Environmental Protection Agency, Emission Measurement Branch, Research
Triangle Park, NC July 1974.
11. Vollaro, R. F. The Effects of Impact Opening Misalignment on the
Value of the Type S Pitot Tube Coefficient. U.S. Environmental
Protection Agency, Emission Measurement Branch, Research Triangle Park,
NC. October 1976.
12. Vollaro, R. F. Establishment of a Basline Coefficient Value for
Properly Constructed Type S Pitot Tubes. U.S. Environmental Protection
Agency, Emission Measurement Branch, Research Triangle Park, NC.
November 1976.
13. Vollaro, R. F. An Evaluation of Single-Velocity Calibration
Technique as a Means of Determining Type S Pitot Tubes Coefficient.
U.S. Environmental Protection Agency, Emission Measurement Branch,
Research Triangle Park, NC. August 1975.
14. Vollaro, R. F. The Use of Type S Pitot Tubes for the Measurement
of Low Velocities. U.S. Environmental Protection Agency, Emission
Measurement Branch, Research Triangle Park, NC. November 1976.
15. Smith, Marvin L. Velocity Calibration of EPA Type Source
Sampling Probe. United Technologies Corporation, Pratt and Whitney
Aircraft Division, East Hartford, CN. 1975.
16. Vollaro, R. F. Recommended Procedure for Sample Traverses in
Ducts Smaller than 12 Inches in Diameter. U.S. Environmental Protection
Agency, Emission Measurement Branch, Research Triangle Park, NC.
November 1976.
17. Ower, E. and R. C. Pankhurst. The Measurement of Air Flow, 4th
Ed., London, Pergamon Press. 1966.
18. Vollaro, R. F. A Survey of Commercially Available
Instrumentation for the Measurement of Low-Range Gas Velocities. U.S.
Environmental Protection Agency, Emission Measurement Branch, Research
Triangle Park, NC. November 1976. (Unpublished Paper)
19. Gnyp, A. W., C. C. St. Pierre, D. S. Smith, D. Mozzon, and J.
Steiner. An Experimental Investigation of the Effect of Pitot
Tube-Sampling Probe Configurations on the Magnitude of the S Type Pitot
Tube Coefficient for Commercially Available Source Sampling Probes.
Prepared by the University of Windsor for the Ministry of the
Environment, Toronto, Canada. February 1975.
40 CFR 60.748 Pt. 60, App. A, Meth. 2A
1. Applicability and Principle
1.1 Applicability. This method applies to the measurement of gas flow
rates in pipes and small ducts, either in-line or at exhaust positions,
within the temperature range of 0 to 50 C.
1.2 Principle. A gas volume meter is used to measure gas volume
directly. Temperature and pressure measurements are made to correct the
volume to standard conditions.
2. Apparatus
Specifications for the apparatus are given below. Any other
apparatus that has been demonstrated (subject to approval of the
Administrator) to be capable of meeting the specifications will be
considered acceptable.
2.1 Gas Volume Meter. A positive displacement meter, turbine meter,
or other direct volume measuring device capable of measuring volume to
within 2 percent. The meter shall be equipped with a temperature gauge
( 2 percent of the minimum absolute temperature) and a pressure gauge (
2.5 mm Hg). The manufacturer's recommended capacity of the meter shall
be sufficient for the expected maximum and minimum flow rates at the
sampling conditions. Temperature, pressure, corrosive characteristics,
and pipe size are factors necessary to consider in choosing a suitable
gas meter.
2.2 Barometer. A mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg. In many cases, the
barometric reading may be obtained from a nearby National Weather
Service station, in which case the station value (which is the absolute
barometric pressure) shall be requested, and an adjustment for elevation
differences between the weather station and the sampling point shall be
applied at a rate of minus 2.5 mm Hg per 30-meter elevation increase, or
vice-versa for elevation decrease.
2.3 Stopwatch. Capable of measurement to within 1 second.
3. Procedure
3.1 Installation. As there are numerous types of pipes and small
ducts that may be subject to volume measurement, it would be difficult
to describe all possible installation schemes. In general, flange
fittings should be used for all connections wherever possible. Gaskets
or other seal materials should be used to assure leak-tight connections.
The volume meter should be located so as to avoid severe vibrations and
other factors that may affect the meter calibration.
3.2 Leak Test. A volume meter installed at a location under positive
pressure may be leak-checked at the meter connections by using a liquid
leak detector solution containing a surfactant. Apply a small amount of
the solution to the connections. If a leak exists, bubbles will form,
and the leak must be corrected.
A volume meter installed at a location under negative pressure is
very difficult to test for leaks without blocking flow at the inlet of
the line and watching for meter movement. If this procedure is not
possible, visually check all connections and assure tight seals.
3.3 Volume Measurement.
3.3.1 For sources with continuous, steady emission flow rates, record
the initial meter volume reading, meter temperature(s), meter pressure,
and start the stopwatch. Throughout the test period, record the meter
temperature(s) and pressure so that average values can be determined.
At the end of the test, stop the timer and record the elapsed time, the
final volume reading, meter temperature(s), and pressure. Record the
barometric pressure at the beginning and end of the test run. Record
the data on a table similar to Figure 2A-1.
Insert illus. 002A
3.3.2 For sources with noncontinuous, non-steady emission flow rates,
use the procedure in 3.3.1 with the addition of the following: Record
all the meter parameters and the start and stop times corresponding to
each process cyclical or noncontinuous event.
4. Calibration
4.1 Volume Meter. The volume meter is calibrated against a standard
reference meter prior to its initial use in the field. The reference
meter is a spirometer or liquid displacement meter with a capacity
consistent with that of the test meter.
Alternatively, a calibrated, standard pitot may be used as the
reference meter in conjunction with a wind tunnel assembly. Attach the
test meter to the wind tunnel so that the total flow passes through the
test meter. For each calibration run, conduct a 4-point traverse along
one stack diameter at a position at least eight diameters of straight
tunnel downstream and two diameters upstream of any bend, inlet, or air
mover. Determine the traverse point locations as specified in Method 1.
Calculate the reference volume using the velocity values following the
procedure in Method 2, the wind tunnel cross-sectional area, and the run
time.
Set up the test meter in a configuration similar to that used in the
field installation (i.e., in relation to the flow moving device).
Connect the temperature and pressure gauges as they are to be used in
the field. Connect the reference meter at the inlet of the flow line,
if appropriate for the meter, and begin gas flow through the system to
condition the meters. During this conditioning operation, check the
system for leaks.
The calibration shall be run over at least three different flow
rates. The calibration flow rates shall be about 0.3, 0.6, and 0.9
times the test meter's rated maximum flow rate.
For each calibration run, the data to be collected include:
reference meter initial and final volume readings, the test meter
initial and final volume reading, meter average temperature and
pressure, barometric pressure, and run time. Repeat the runs at each
flow rate at least three times.
Calculate the test meter calibration coefficient, Ym, for each run as
follows:
Eq. 2A-1
Where:
Ym=Test volume meter calibration coefficient, dimensionless.
Vr=Reference meter volume reading, m3.
Vm=Test meter volume reading, m3.
tr=Reference meter average temperature, C.
tm=Test meter average temperature, C.
Pb=Barometric pressure, mm Hg.
Pg=Test meter average static pressure, mm Hg.
f=Final reading for run.
i=Initial reading for run.
Compare the three Ym values at each of the flow rates tested and
determine the maximum and minimum values. The difference between the
maximum and minimum values at each flow rate should be no greater than
0.030. Extra runs may be required to complete this requirement. If this
specification cannot be met in six successive runs, the test meter is
not suitable for use. In addition, the meter coefficients should be
between 0.95 and 1.05. If these specifications are met at all the flow
rates, average all the Ym values from runs meeting the specifications to
obtain an average meter calibration coefficient, Ym.
The procedure above shall be performed at least once for each volume
meter. Thereafter, an abbreviated calibration check shall be completed
following each field test. The calibration of the volume meter shall be
checked by performing three calibration runs at a single, intermediate
flow rate (based on the previous field test) with the meter pressure set
at the average value encountered in the field test. Calculate the
average value of the calibration factor. If the calibration has changed
by more than 5 percent, recalibrate the meter over the full range of
flow as described above.
Note. -- If the volume meter calibration coefficient values obtained
before and after a test series differ by more than 5 percent, the test
series shall either be voided, or calculations for the test series shall
be performed using whichever meter coefficient value (i.e., before or
after) gives the greater value of pollutant emission rate.
4.2 Temperature Gauge. After each test series, check the temperature
gauge at ambient temperature. Use an American Society for Testing and
Materials (ASTM) mercury-in-glass reference thermometer, or equivalent,
as a reference. If the gauge being checked agrees within 2 percent
(absolute temperature) of the reference, the temperature data collected
in the field shall be considered valid. Otherwise, the test data shall
be considered invalid or adjustments of the test results shall be made,
subject to the approval of the Administrator.
4.3 Barometer. Calibrate the barometer used against a mercury
barometer prior to the field test.
5. Calculations
Carry out the calculations, retaining at least one extra decimal
figure beyond that of the acquired data. Round off figures after the
final calculation.
5.1 Nomenclature.
Pb=Barometric pressure, mm Hg.
Pg=Average static pressure in volume meter, mm Hg.
Qs=Gas flow rate, m3/min, standard conditions.
Tm=Average absolute meter temperature, K.
Vm=Meter volume reading, m3.
Ym=Average meter calibration coefficient, dimensionless.
f=Final reading for test period.
i=Initial reading for test period.
s=Standard conditions, 20 C and 760 mm Hg.
U=Elapsed test period time, min.
5.2 Volume.
Eq. 2A-2
5.3 Gas Flow Rate.
6. Bibliography
1. Rom, Jerome J. Maintenance, Calibration, and Operation of
Isokinetic Source Sampling Equipment. U.S. Environmental Protection
Agency. Research Triangle Park, NC, Publication No. APTD-0576. March
1972.
2. Wortman, Martin, R. Vollaro, and P.R. Westlin. Dry Gas Volume
Meter Calibrations. Source Evaluation Society Newsletter. Vol. 2, No.
2. May 1977.
3. Westlin, P.R. and R.T. Shigehara. Procedure for Calibrating and
Using Dry Gas Volume Meters as Calibration Standards. Source Evaluation
Society Newsletter. Vol. 3, No. 1. February 1978.
40 CFR 60.748 Pt. 60, App. A, Meth. 2B
1. Applicability and Principle
1.1 Applicability. This method applies to the measurement of exhaust
volume flow rate from incinerators that process gasoline vapors
consisting primarily of alkanes, alkenes, and/or arenes (aromatic
hydrocarbons). It is assumed that the amount of auxiliary fuel is
negligible.
1.2 Principle. The incinerator exhaust flow rate is determined by
carbon balance. Organic carbon concentration and volume flow rate are
measured at the incinerator inlet. Organic carbon, carbon dioxide
(CO2), and carbon monoxide (CO) concentrations are measured at the
outlet. Then the ratio of total carbon at the incinerator inlet and
outlet is multiplied by the inlet volume to determine the exhaust volume
and volume flow rate.
2. Apparatus
2.1 Volume Meter. Equipment described in Method 2A.
2.2 Organic Analyzers (2). Equipment described in Method 25A or 25B.
2.3 CO Analyzer. Equipment described in Method 10.
2.4 CO2 Analyzer. A nondispersive infrared (NDIR) CO2 analyzer and
supporting equipment with comparable specifications as CO analyzer
described in Method 10.
3. Procedure
3.1 Inlet Installation. Install a volume meter in the vapor line to
incinerator inlet according to the procedure in Method 2A. At the
volume meter inlet, install a sample probe as described in Method 25A.
Connect to the probe a leak-tight, heated (if necessary to prevent
condensation) sample line (stainless steel or equivalent) and an organic
analyzer system as described in Method 25A or 25B.
3.2 Exhaust Installation. Three sample analyzers are required for
the incinerator exhaust: CO2, CO, and organic analyzers. A sample
manifold with a single sample probe may be used. Install a sample probe
as described in Method 25A. Connect a leak-tight heated sample line to
the sample probe. Heat the sample line sufficiently to prevent any
condensation.
3.3 Recording Requirements. The output of each analyzer must be
permanently recorded on an analog strip chart, digital recorder, or
other recording device. The chart speed or number of readings per time
unit must be similar for all analyzers so that data can be correlated.
The minimum data recording requirement for each analyzer is one
measurement value per minute.
3.4 Preparation. Prepare and calibrate all equipment and analyzers
according to the procedures in the respective methods. For the CO2
analyzer, follow the procedures described in Method 10 for CO analysis
substituting CO2 calibration gas where the method calls for CO
calibration gas. The span value for the CO2 analyzer shall be 15
percent by volume. All calibration gases must be introduced at the
connection between the probe and the sample line. If a manifold system
is used for the exhaust analyzers, all the analyzers and sample pumps
must be operating when the calibrations are done. Note: For the
purposes of this test, methane should not be used as an organic
calibration gas.
3.5 Sampling. At the beginning of the test period, record the initial
parameters for the inlet volume meter according to the procedures in
Method 2A and mark all of the recorder strip charts to indicate the
start of the test. Continue recording inlet organic and exhaust CO2,
CO, and organic concentrations throughout the test. During periods of
process interruption and halting of gas flow, stop the timer and mark
the recorder strip charts so that data from this interruption are not
included in the calculations. At the end of the test period, record the
final parameters for the inlet volume meter and mark the end on all of
the recorder strip charts.
3.6 Post Test Calibrations. At the conclusion of the sampling
period, introduce the calibration gases as specified in the respective
reference methods. If an analyzer output does not meet the
specifications of the method, invalidate the test data for the period.
Alternatively, calculate the volume results using initial calibration
data and using final calibration data and report both resulting volumes.
Then, for emissions calculations, use the volume measurement resulting
in the greatest emission rate or concentration.
4. Calculations
Carry out the calculations, retaining at least one extra decimal
figure beyond that of the acquired data. Round off figures after the
final calculation.
4.1 Nomenclature.
COe=Mean carbon monoxide concentration in system exhaust, ppm.
CO2e=Mean carbon dioxide concentration in system exhaust, ppm.
HCe=Mean organic concentration in system exhaust as defined by the
calibration gas, ppm.
HCi=Mean organic concentration in system inlet as defined by the
calibration gas, ppm.
K=Calibration gas factor
=2 for ethane calibration gas.
=3 for propane calibration gas.
=4 for butane calibration gas.
=Appropriate response factor for other calibration gas.
Ves=Exhaust gas volume, m3.
Vis=Inlet gas volume, m3.
Qes=Exhaust gas volume flow rate, m3/min.
Qis=Inlet gas volume flow rate, m3/min.
Q=Sample run time, min.
s=Standard conditions: 20 C, 760 mm Hg.
300=Estimated concentration of ambient CO2, ppm. (CO2 concentration
in the ambient air may be measured during the test period using an
NDIR).
4.2 Concentrations. Determine mean concentrations of inlet organics,
outlet CO2, outlet CO, and outlet organics according to the procedures
in the respective methods and the analyzers' calibration curves, and for
the time intervals specified in the applicable regulations.
Concentrations should be determined on a parts per million by volume
(ppm) basis.
4.3 Exhaust Gas Volume. Calculate the exhaust gas volume as follows:
Eq. 2B-1
4.4 Exhaust Gas Volume Flow Rate. Calculate the exhaust gas volume
flow rate as follows:
Eq. 2B-2
5. Bibliography
1. Measurement of Volatile Organic Compounds. U.S. Environmental
Protection Agency. Office of Air Quality Planning and Standards,
Research Triangle Park, NC 27711. Publication No. EPA-450/2-78-041.
October 1978. 55 p.
40 CFR 60.748 Pt. 60, App. A, Meth. 2C
1.1 Applicability.
1.1.1 The applicability of this method is identical to Method 2,
except this method is limited to stationery source stacks or ducts less
than about 0.30 meter (12 in.) in diameter or 0.071 m2 (113 in.2) in
cross-sectional area, but equal to or greater than about 0.10 meter (4
in.) in diameter or 0.0081 m2 (12.57 in.2) in cross-sectional area.
1.1.2 The apparatus, procedure, calibration, calculations, and
biliography are the same as in Method 2, Sections 2, 3, 4, 5, and 6,
except as noted in the following sections.
1.2 Principle. The average gas velocity in a stack or duct is
determined from the gas density and from measurement of velocity heads
with a standard pitot tube.
2.1 Standard Pitot Tube (instead of Type S). Use a standard pitot
tube that meets the specifications of Section 2.7 of Method 2. Use a
coefficient value of 0.99 unless it is calibrated against another
standard pitot tube with an NBS-traceable coefficient.
2.2 Alternative Pitot Tube. A modified hemispherical-nosed pitot
tube (see Figure 2C-1), which features a shortened stem and enlarged
impact and static pressure holes, may be used. This pitot tube is
useful in liquid drop-laden gas streams when a pitot ''back purge'' is
ineffective. Use a coefficient value of 0.99 unless the pitot is
calibrated as mentioned in Section 2.1 above.
Insert illustration 0 811
Follow the general procedures in Section 3 of Method 2, except
conduct the measurements at the traverse points specified in Method 1A.
The static and impact pressure holes of standard pitot tubes are
susceptible to plugging in PM-laden gas streams. Therefore, the tester
must furnish adequate proof that the openings of the pitot tube have not
plugged during the traverse period; this proof can be obained by first
recording the velocity head (Dp) reading at the final traverse point,
then cleaning out the impact and static holes of the standard pitot tube
by ''back-purging'' with pressurized air, and finally by recording
another Dp reading at the final traverse point. If the Dp reading made
after the air purge is within 5 percent of the reading during the
traverse, then the traverse is acceptable. Otherwise, reject the run.
Note that if the Dp at the final traverse point is so low as to make
this determination too difficult, then another traverse point may be
selected. If ''back purging'' at regular intervals is part of the
procedure, then take comparative Dp readings, as above, for the last two
back purges at which suitable high Dp readings are observed.
40 CFR 60.748 Pt. 60, App. A, Meth. 2D
1.1 Applicability. This method applies to the measurement of gas flow
rates in small pipes and ducts, either before or after emission control
devices.
1.2 Principle. To measure flow rate or pressure drop, all the stack
gas is directed through a rotameter, orifice plate or similar flow rate
measuring device. The measuring device has been previously calibrated
in a manner that insures its proper calibration for the gas or gas
mixture being measured. Absolute temperature and pressure measurements
are also made to calculate volumetric flow rates at standard conditions.
Specifications for the apparatus are given below. Any other
apparatus that has been demonstrated (subject to approval of the
Administrator) to be capable of meeting the specifications will be
considered acceptable.
2.1 Flow Rate Measuring Device. A rotameter, orifice plate, or other
flow rate measuring device capable of measuring all the stack flow rate
to within 5 percent of its true value. The measuring device shall be
equipped with a temperature gauge accurate to within 2 percent of the
minimum absolute stack temperature and a pressure gauge accurate to
within 5 mm Hg. The capacity of the measuring device shall be
sufficient for the expected maximum and minimum flow rates at the stack
gas conditions. The magnitude and variability of stack gas flow rate,
molecular weight, temperature, pressure, compressibility, dew point,
corrosiveness, and pipe or duct size are all factors to consider in
choosing a suitable measuring device.
2.2 Barometer. Same as in Method 2, Section 2.5.
2.3 Stopwatch. Capable of incremental time measurement to within 1
second.
3.1 Installation. Use the procedure in Method 2A, Section 3.1.
3.2 Leak Check. Use the procedure in Method 2A, Section 3.2.
3.3 Flow Rate Measurement.
3.3.1 Continuous, Steady Flow. At least once an hour, record the
measuring device flow rate reading, and the measuring device temperature
and pressure. Make a minimum of twelve equally spaced readings of each
parameter during the test period. Record the barometric pressure at the
beginning and end of the test period. Record the data on a table
similar to Figure 2D-1.
-- --
PlantXXXXXXXXXXXXXXX
DateXXXXXXX Run numberXXXX
Sample locationXXXXXXXXXXX
Barometric pressure, mm (in.) Hg StartXXX FinishXXX
Operators XXXXXXXXXX
Measuring device numberXXX Calibration coefficientXXX
Calibration gasXXXXX
Last date calibratedXXXX
Figure 2D-1. Flow rate measurement data.
3.3.2 Noncontinuous and Nonsteady Flows. Use flow rate measuring
devices with particular caution. Calibration will be affected by
variation in stack gas temperature, pressure, compressibility, and
molecular weight. Use the procedure in Section 3.3.1. Record all the
measuring device parameters on a time interval frequency sufficient to
adequately profile each process cyclical or noncontinuous event. A
multichannel continuous recorder may be used.
4.1 Flow Rate Measuring Device. Use the procedure in Method 2A,
Section 4, and apply the same performance standards. Calibrate the
measuring device with the principal stack gas to be measured (e.g., air,
nitrogen) against a standard reference meter. A calibrated dry gas
meter is an acceptable reference meter. Ideally, calibrate the
measuring device in the field with the actual gas to be measured. For
measuring devices that have a volume rate readout, calculate the
measuring device calibration coefficient, Ym, for each run as follows:
where:
Qr=reference meter flow rate reading, m3/min (ft3/min).
Qm=measuring device flow rate reading, m3/min (ft3/min).
Tr=reference meter average absolute temperature, K ( R).
Tm=measuring device average absolute temperature, K ( R).
Pbar=barometric pressure, mm Hg (in. Hg).
Pg=measuring device average static pressure, mm Hg (in. Hg).
For measuring devices that do not have a readout as flow rate, refer
to the manufacturer's instructions to calculate the Qm corresponding to
each Qr.
4.2 Temperature Gauge. Use the procedure and specifications in
Method 2A, Section 4.2. Perform the calibration at a temperature that
approximates field test conditions.
4.3 Barometer. Calibrate the barometer to be used in the field test
with a mercury barometer prior to the field test.
Calculate the stack gas flow rate, Qs, as follows:
where:
Kl = 0.3858 for international system of units (SI); 17.64 for
English units.
1. Spink, L.K. Principles and Practice of Flowmeter Engineering. The
Foxboro Company. Foxboro, MA. 1967.
2. Benedict, Robert P. Fundamentals of Temperature, Pressure, and
Flow Measurements. John Wiley and Sons, Inc. New York, NY. 1969.
3. Orifice Metering of Natural Gas. American Gas Association.
Arlington, VA. Report No. 3. March 1978. 88 p.
40 CFR 60.748 Pt. 60, App. A, Meth. 3
1.1.1 This method is applicable for determining carbon dioxide (CO2)
and oxygen (O2) concentrations and dry molecular weight of a sample from
a gas stream of a fossil-fuel combustion process. The method may also
be applicable to other processes where it has been determined that
compounds other than CO2, O2, carbon monoxide (CO), and nitrogen (N2)
are not present in concentrations sufficient to affect the results.
1.1.2 Other methods, as well as modifications to the procedure
described herein, are also applicable for some or all of the above
determinations. Examples of specific methods and modifications include:
(1) A multi-point sampling method using an Orsat analyzer to analyze
individual grab samples obtained at each point; (2) a method using CO2
or O2 and stoichiometric calculations to determine dry molecular weight;
and (3) assigning a value of 30.0 for dry molecular weight, in lieu of
actual measurements, for processes burning natural gas, coal, or oil.
These methods and modifications may be used, but are subject to the
approval of the Administrator, U.S. Environmental Protection Agency
(EPA).
1.1.3 Note. Mention of trade names or specific products does not
constitute endorsements by EPA.
1.2 Principle. A gas sample is extracted from a stack by one of the
following methods: (1) Single-point, grab sampling; (2) single-point,
integrated sampling; or (3) multi-point, integrated sampling. The gas
sample is analyzed for pecent CO2, percent O2, and if necessary, for
percent CO. For dry molecular weight determination, either an Orsat or
a Fyrite analyzer may be used for the analysis.
As an alternative to the sampling apparatus and systems described
herein, other sampling systems (e.g., liquid displacement) may be used,
provided such systems are capable of obtaining a representative sample
and maintaining a constant sampling rate, and are, otherwise, capable of
yielding acceptable results. Use of such systems is subject to the
approval of the Administrator.
2.1.1 Probe. Stainless steel or borosilicate glass tubing equipped
with an in-stack or out-stack filter to remove particulate matter (a
plug of glass wool is satisfactory for this purpose). Any other
materials, inert to O2, CO2, CO, and N2 and resistant to temperature at
sampling conditions, may be used for the probe. Examples of such
materials are aluminum, copper, quartz glass, and Teflon.
2.1.2 Pump. A one-way squeeze bulb, or equivalent, to transport the
gas sample to the analyzer.
2.2 Integrated Sampling (Figure 3-2).
2.2.1 Probe. Same as in Section 2.1.1.
2.2.2 Condenser. An air-cooled or water-cooled condenser, or other
condenser no greater than 250 ml that will not remove O2, CO2, CO, and
N2, to remove excess moisture which would interfere with the operation
of the pump and flowmeter.
2.2.3 Valve. A needle valve, to adjust sample gas flow rate.
Insert Illustration 0041
2.2.4 Pump. A leaf-free, diaphragm-type pump, or equivalent, to
transport sample gas to the flexible bag. Install a small surge tank
between the pump and rate meter to eliminate the pulsation effect of the
diaphragm pump on the rotameter.
2.2.5 Rate Meter. A rotameter, or equivalent rate meter, capable of
measuring flow rate to within 2 percent of the selected flow rate. A
flow rate range of 500 to 1000 cc/min is suggested.
2.2.6 Flexible Bag. Any leak-free plastic (e.g., Tedlar, Mylar,
Teflon) or plastic-coated aluminum (e.g., aluminized Mylar) bag, or
equivalent, having a capacity consistent with the selected flow rate and
time length of the test run. A capacity in the range of 55 to 90 liters
is suggested. To leak check the bag, connect it to a water manometer,
and pressurize the bag to 5 to 10 cm H2O (2 to 4 in. H2O). Allow to
stand for 10 minutes. Any displacement in the water manometer indicates
a leak. An alternative leak-check method is to pressurize the bag to 5
to 10 cm (2 to 4 in.) H2O and allow to stand overnight. A deflated bag
indicates a leak.
2.2.7 Pressure Gauge. A water-filled U-tube manometer, or
equivalent, of about 30 cm (12 in.), for the flexible bag leak check.
2.2.8 Vacuum Gauge. A mercury manometer, or equivalent, of at least
760 mm (30 in.) Hg, for the sampling train leak check.
2.3 Analysis. An Orsat or Fyrite type combustion gas analyzer. For
Orsat and Fyrite analyzer maintenance and operation procedures, follow
the instructions recommended by the manufacturer, unless otherwise
specified herein.
3.1 The sampling point in the duct shall either be at the centroid of
the cross section or at a point no closer to the walls than 1.00 m (3.3
ft), unless otherwise specified by the Administrator.
3.2 Set up the equipment as shown in Figure 3-1, making sure all
connections ahead of the analyzer are tight. If an Orsat analyzer is
used, it is recommended that the analyzer be leak checked by following
the procedure in Section 6; however, the leak check is optional.
3.3 Place the probe in the stack, with the tip of the probe
positioned at the sampling point; purge the sampling line long enough
to allow at least five exchanges. Draw a sample into the analyzer, and
immediately analyze it for percent CO2 and percent O2. Determine the
percentage of the gas that is N2 and CO by subtracting the sum of the
percent CO2 and percent 02O from 100 percent. Calculate the dry
molecular weight as indicated in Section 7.2.
3.4 Repeat the sampling, analysis, and calculation procedures until
the dry molecular weights of any three grab samples differ from their
mean by no more than 0.3 g/g-mole (0.3 lb/lb-mole). Average these three
molecular weights, and report the results to the nearest 0.1 g/g-mole
(0.1 lb/lb-mole).
4.1 The sampling point in the duct shall be located as specified in
Section 3.1.
4.2 Leak check (optional) the flexible bag as in Section 2.2.6. Set
up the equipment as shown in Figure 3-2. Just before sampling, leak
check (optional) the train by placing a vacuum gauge at the condenser
inlet, pulling a vacuum of at least 250 mm Hg (10 in. Hg), plugging the
outlet at the quick disconnect, and then turning off the pump. The
vacuum should remain stable for at least 0.5 minute. Evacuate the
flexible bag. Connect the probe, and place it in the stack, with the
tip of the probe positioned at the sampling point; purge the sampling
line. Next, connect the bag, and make sure that all connections are
tight.
4.3 Sample at a constant rate. The sampling run should be
simultaneous with, and for the same total length of time as, the
pollutant emission rate determination. Collection of at least 30 liters
(1.00 ft3) of sample gas is recommended; however, smaller volumes may
be collected, if desired.
4.4 Obtain one integrated flue gas sample during each pollutant
emission rate determination. Within 8 hours after the sample is taken,
analyze it for percent CO2 and percent O2 using either an Orsat analyzer
or a Fyrite type combustion gas analyzer. If an Orsat analyzer is used,
it is recommended that Orsat leak check described in Section 6, be
performed before this determination; however, the check is optional.
Determine the percentage of the gas that is N2 and CO by subtracting the
sum of the percent CO2 and percent 0 from 100 percent. Calculate the
dry molecular weight as indicated in Section 7.2.
4.5 Repeat the analysis and calculation procedures until the
individual dry molecular weights for any three analyses differ from
their mean by no more than 0.3 g/g-mole (0.3 lb/lb-mole). Average these
three molecular weights, and report the results to the nearest 0.1
g/g-mole (0.1 lb/lb-mole).
5.1 Unless otherwise specified by the Administrator, a minimum of
eight traverse points shall be used for circular stacks having diameters
less than 0.61 m (24 in.), a minimum of nine shall be used for
rectangular stacks having equivalent diameters less than 0.61 m (24
in.), and a minimum of 12 traverse points shall be used for all other
cases. The traverse points shall be located according to Method 1. The
use of fewer points is subject to approval of the Administrator.
5.2 Follow the procedures outlined in Sections 4.2 through 4.5,
except for the following: Traverse all sampling points, and sample at
each point for an equal length of time. Record sampling data as shown
in Figure 3-3.
Moving an Orsat analyzer frequently causes it to leak. Therefore, an
Orsat analyzer should be thoroughly leak checked on site before the flue
gas sample is introduced into it. The procedure for leak checking an
Orsat analyzer is as follows:
6.1 Bring the liquid level in each pipette up to the reference mark
on the capillary tubing, and then close the pipette stopcock.
6.2 Raise the leveling bulb sufficiently to bring the confining
liquid meniscus onto the graduated portion of the burette, and then
close the manifold stopcock.
6.4 Observe the menisus in the burette and the liquid level in the
pipette for movement over the next 4 minutes.
6.5 For the Orsat analyzer to pass the leak check, two conditions
must be met:
6.5.1 The liquid level in each pipette must not fall below the botton
of the capillary tubing during this 4-minute interval.
6.5.2 The menisus in the burette must not change by more than 0.2 ml
during this 4-minute interval.
6.6 If the anlyzer fails the leak-check procedure, check all rubber
connections and stopcocks to determine whether they might be the cause
of the leak. Disassemble, clean, and regrease leaking stopcocks.
Replace leaking rubber connections. After the analyzer is reassembled,
repeat the lead-check procedure.
Md = Dry molecular weight, g/g-mole (1b/1b-mole).
%CO2 = Percent CO2 by volume, dry basis.
%O2 = Percent O2 by volume, dry basis.
%CO = Percent CO by volume, dry basis.
%N2 = Percent N2 by volume, dry basis.
0.280 = Molecular weight of N2 or CO, divided by 100.
0.320 = Molecular wight of O2 divided by 100.
0.440 = Molecular weight of CO2 divided by 100.
7.2 Dry Molecular Weight. Use Equation 3-1 to calculate the dry
molecular weight of the stack gas.
Md = 0.440(%CO2) + 0.320 (%O2) + 0.280(%N2 + %CO) Eq. 3-1
Note. The above equation does not consider argon in air (about 0.9
percent, molecular weight of 39.9). A negative error of about 0.4
percent is introduced. The tester may choose to include argon in the
analysis using procedures subject to approval of the Administrator.
1. Altshuller, A.P. Storage of Gases and Vapors in Plastic Bags.
International Journal of Air and Water Pollution. 6:75-81. 1963.
2. Conner, William D. and J.S. Nader. Air Sampling with Plastic
Bags. Journal of the American Industrial Hygiene Association.
25:292-297. 1964.
3. Burrell Manual for Gas Analysts, Seventh edition. Burrell
Corporation, 2223 Fifth Avenue, Pittsburgh, PA. 15219. 1951.
4. Mitchell, W.J. and M.R. Midgett, Field Reliability of the Orsat
Analyzer. Journal of Air Pollution Control Association. 26:491-495.
May 1976.
5. Shigehara, R.T., R. M. Neulicht, and W.S. Smith. Validating Orsat
Analysis Data from Fossil Fuel-Fired Units. Stack Sampling News.
4(2):21-26. August 1976.
40 CFR 60.748 Pt. 60, App. A, Meth. 3A
1. Applicability and Principle
1.1 Applicability. This method is applicable to the determination of
oxygen (O2) and carbon dioxide (CO2) concentrations in emissions from
stationary sources only when specified within the regulations.
1.2 Principle. A sample is continuously extracted from the effluent
stream: a portion of the sample stream is conveyed to an instrumental
analyzer(s) for determination of O2 and CO2 concentration(s).
Performance specifications and test procedures are provided to ensure
reliable data.
2. Range and Sensitivity
Same as Method 6C, Sections 2.1 and 2.2, except that the span of the
monitoring system shall be selected such that the average O2 or CO2
concentration is not less than 20 percent of the span.
3. Definitions
3.1 Measurement System. The total equipment required for the
determination of the O2 or CO2 concentration. The measurement system
consists of the same major subsystems as defined in Method 6C, Sections
3.1.1, 3.1.2, and 3.1.3.
3.2 Span, Calibration Gas, Analyzer Calibration Error, Sampling
System Bias, Zero Drift, Calibration Drift, Response Time, and
Calibration Curve. Same as Method 6C, Sections 3.2 through 3.8, and
3.10.
3.3 Interference Response. The output response of the measurement
system to a component in the sample gas, other than the gas component
being measured.
4. Measurement System Performance Specifications
Same as Method 6C, Sections 4.1 through 4.4.
5. Apparatus and Reagents
5.1 Measurement System. Any measurement system for O2 or CO2 that
meets the specifications of this method. A schematic of an acceptable
measurement system is shown in Figure 6C-1 of Method 6C. The essential
components of the measurement system are described below:
5.1.1 Sample Probe. A leak-free probe, of sufficient length to
traverse the sample points.
5.1.2 Sample Line. Tubing, to transport the sample gas from the
probe to the moisture removal system. A heated sample line is not
required for systems that measure the O2 or CO2 concentration on a dry
basis, or transport dry gases.
5.1.3 Sample Transport Line, Calibration Value Assembly, Moisture
Removal System, Particulate Filter, Sample Pump, Sample Flow Rate
Control, Sample Gas Manifold, and Data Recorder. Same as Method 6C,
Sections 5.1.3 through 5.1.9, and 5.1.11, except that the requirements
to use stainless steel, Teflon, and nonreactive glass filters do not
apply.
5.1.4 Gas Analyzer. An analyzer to determine continuously the O2 or
CO2 concentration in the sample gas stream. The analyzer shall meet the
applicable performance specifications of Section 4. A means of
controlling the analyzer flow rate and a device for determining proper
sample flow rate (e.g., precision rotameter, pressure gauge downstream
of all flow controls, etc.) shall be provided at the analyzer. The
requirements for measuring and controlling the analyzer flow rate are
not applicable if data are presented that demonstrate the analyzer is
insensitive to flow variations over the range encountered during the
test.
5.2 Calibration Gases. The calibration gases for CO2 analyzers shall
be CO2 in N2 or CO2 in air. Alternatively, CO2/SO2, O2/SO2 , or
O2/CO2/SO2 gas mixtures in N2 may be used. Three calibration gases, as
specified Section 5.3.1 through 5.3.3 of Method 6C, shall be used. For
O2 monitors that cannot analyze zero gas, a calibration gas
concentration equivalent to less than 10 percent of the span may be used
in place of zero gas.
6. Measurement System Performance Test Procedures
Perform the following procedures before measurement of emissions
(Section 7).
6.1 Calibration Concentration Verification. Follow Section 6.1 of
Method 6C, except if calibration gas analysis is required, use Method 3
and change the acceptance criteria for agreement among Method 3 results
to 5 percent (or 0.2 percent by volume, whichever is greater).
6.2 Interference Response. Conduct an interference response test of
the analyzer prior to its initial use in the field. Thereafter, recheck
the measurement system if changes are made in the instrumentation that
could alter the interference response (e.g., changes in the type of gas
detector). Conduct the interference response in accordance with Section
5.4 of Method 20.
6.3 Measurement System Preparation, Analyzer Calibration Error, and
Sampling System Bias Check. Follow Sections 6.2 through 6.4 of Method
6C.
7. Emission Test Procedure
7.1 Selection of Sampling Site and Sampling Points. Select a
measurement site and sampling points using the same criteria that are
applicable to tests performed using Method 3.
7.2 Sample Collection. Position the sampling probe at the first
measurement point, and begin sampling at the same rate as used during
the sampling system bias check. Maintain constant rate sampling (i.e.,
10 percent) during the entire run. The sampling time per run shall be
the same as for tests conducted using Method 3 plus twice the system
response time. For each run, use only those measurements obtained after
twice the response time of the measurement system has elapsed to
determine the average effluent concentration.
7.3 Zero and Calibration Drift Test. Follow Section 7.4 of Method
6C.
8. Quality Control Procedures
The following quality control procedures are recommended when the
results of this method are used for an emission rate correction factor,
or excess air determination. The tester should select one of the
following options for validating measurement results:
8.1 If both O2 and CO2 are measured using Method 3A, the procedures
described in Section 4.4 of Method 3 should be followed to validate the
O2 and CO2 measurement results.
8.2 If only O2 is measured using Method 3A, measurements of the
sample stream CO2 concentration should be obtained at the sample by-pass
vent discharge using an Orsat or Fyrite analyzer, or equivalent.
Duplicate samples should be obtained concurrent with at least one run.
Average the duplicate Orsat or Fyrite analysis results for each run.
Use the average CO2 values for comparison with the O2 measurements in
accordance with the procedures described in Section 4.4 of Method 3.
8.3 If only CO2 is measured using Method 3A, concurrent measurements
of the sample stream CO2 concentration should be obtained using an Orsat
or Fyrite analyzer as described in Section 8.2. For each run,
differences greater than 0.5 percent between the Method 3A results and
the average of the duplicate Fyrite analysis should be investigated.
9. Emission Calculation
For all CO2 analyzers, and for O2 analyzers that can be calibrated
with zero gas, follow Section 8 of Method 6C, except express all
concentrations as percent, rather than ppm.
For O2 analyzers that use a low-level calibration gas in place of a
zero gas, calculate the effluent gas concentration using Equation 3A-1.
Eq. 3A-1
Where:
Cgas=Effluent gas concentration, dry basis, percent.
Cma=Actual concentration of the upscale calibration gas, percent.
Coa=Actual concentration of the low-level calibration gas, percent.
Cm=Average of initial and final system calibration bias check
responses for the upscale calibration gas, percent.
Co=Average of initial and final system calibration bias check
responses for the low-level gas, percent.
C8=Average gas concentration indicated by the gas analyzer, dry
basis, percent.
10. Bibliography
Same as bibliography of Method 6C.
40 CFR 60.748 Pt. 60, App. A, Meth. 3B
1.1.1 This method is applicable for determining carbon dioxide (CO2),
oxygen (O2), and carbon monoxide (CO) concentrations of a sample from a
gas stream of a fossil-fuel combustion provess for excess air or
emission rate correction factor calculations.
1.1.2 Other methods, as well as modifications to the procedure
described herein, are also applicable for all of the above
determinations. Examples of specific methods and modifications include:
(1) A multi-point sampling method using an Orsat analyzer to analyze
individual grab samples obtained at each point, and (2) a method using
CO2 or O2 and stoichiometric calculations to determine excess air.
These methods and modifications may be used, but are subject to the
approval of the Administrator, U.S. Environmental Protection Agency
(FPA).
1.1.3 Note. Mention of trade names or specific products does not
constitute endorsement by EPA.
1.2 Principle. A gas sample is extracted from a stack by one of the
following methods: (1) Single-point, grab sampling; (2) single-point,
integrated sampling; or (3) multi-point, integrated sampling. The gas
sample is analyzed for percent CO2 percent O2, and, if necessary,
percent CO. An Orsat analyzer must be used for excess air or emission
rate correction factor determinations.
The alternative sampling systems are the same as those mentioned in
Section 2 of Method 3.
2.1 Grab Sampling and Integrated Sampling. Same as in Sections 2.1
and 2.2, respectively, of Method 3.
2.2 Analysis. An Orsat analyzer only. For low CO2 (less than 4.0
percent) or high O2 (greater than 15.0 percent) concentrations, the
measuring burette of the Orsat must have at least 0.1 percent
subdivisions. For Orsat maintenance and operation procedures, follow
the instructions recommended by the manufacturer, unless otherwise
specified herein.
Each of the three procedures below shall be used only when specified
in an applicable subpart of the standards. The use of these procedures
for other purposes must have specific prior approval of the
Adminsitrator.
Note. -- A Fyrite-type combustion gas analyzer is not acceptable for
excess air or emission rate correction factor determinations, unless
approved by the Administrator. If both percent CO2 and percent O2 are
measured, the analytical results of any of the three procedures given
below may be used for calculating the dry molecular weight (see Method
3).
3.1.1 The sampling point in the duct shall be as described in Section
3.1 of Method 3.
3.1.2 Set up the equipment as shown in Figure 3-1 of Method 3, making
sure all connections ahead of the analyzer are tight. Leak check the
Orsat analyzer according to the procedure described in Section 6 of
Method 3. This leak check is mandatory.
3.1.3 Place the probe in the stack, with the tip of the probe
positioned at the sampling point; purge the sampling line long enough
to allow at least five exchanges. Draw a sample into the analyzer. For
emission rate correction factor determinations, immediately analyze the
sample, as outlined in Sections 3.1.4 and 3.1.5, for percent CO2 or
percent O2. If excess air is desired, proceed as follows: (1)
immediately analyze the sample, as in Sections 3.1.4 and 3.1.5, for
percent CO2, O2, and CO; (2) determine the percentage of the gas that
is N2 by subtracting the sum of the percent CO2, percent O2, and percent
CO from 100 percent, and (3) calculate percent excess air as outlined in
Section 4.2.
3.1.4 To ensure complete absorption of the CO2, O2, or if applicable,
CO, make repeated passes through each absorbing solution until two
consecutive readings are the same. Several passes (three or four)
should be made between readings. (If constant readings cannot be
obtained after three consecutive readings, replace the absorbing
solution.)
Note. -- Since this single-point, grab sampling and analytical
procedure is normally conducted in conjunction with a single-point, grab
sampling and analytical procedure for a pollutant, only one analysis is
ordinarily conducted. Therefore, great care must be taken to obtain a
valid sample and analysis. Although in most cases, only CO2 or O2 is
required, it is recommended that both CO2 and O2 be measured, and that
Section 3.4 be used to validate the analytical data.
3.1.5 After the analysis is completed, leak check (mandatory) the
Orsat analyzer once again, as described in Section 6 of Method 3. For
the results of the analysis to be valid, the Orsat analyzer must pass
this leak test before and after the analysis.
3.2.1 The sampling point in the duct shall be located as specified in
Section 3.1.1.
3.2.2 Leak check (mandatory) the flexible bag as in Section 2.2.6 of
Method 3. Set up the equipment as shown in Figure 3-2 of Method 3.
Just before sampling, leak check (mandatory) the train as described in
Section 4.2 of Method 3.
3.2.3 Sample at a constant rate, or as specified by the
Administrator. The sampling run must be simultaneous with, and for the
same total length of time as, the pollutant emission rate determination.
Collect at least 30 liters (1.00 ft /3/ ) of sample gas. Smaller
volumes may be collected, subject to approval of the Administrator.
3.2.4 Obtain one integrated flue gas sample during each pollutant
emission rate determination. For emission rate correction factor
determination, analyze the sample within 4 hours after it is taken for
percent CO2 or percent O2 (as outlined in Sections 3.2.5 through 3.2.7).
The Orsat analyzer must be leak checked (see Section 6 of Method 3)
before the analysis. If excess air is desired, proceded as follows:
(1) within 4 hours after the sample is taken, analyze it (as in Sections
3.2.5 through 3.2.7) for percent CO2, O2, and CO; (2) determine the
percentage of the gas that is N2 by substracting the sum of the percent
CO2, percent O2, and percent CO from 100 percent; and (3) calculate
percent excess air, as outlined in Section 4.2.
3.2.5 To ensure complete absorption of the CO2, O2, or if applicable,
CO, follow the procedure described in Section 3.1.4.
Note. -- Although in most instances only CO2 or O2 is required, it is
recommended that both CO2 and O2 be measured, and that Section 3.4.1 be
used to validate the analytical data.
3.2.6 Repeat the analysis until the following criteria are met:
3.2.6.1 For percent CO2, repeat the analytical procedure until the
results of any three analyses differ by no more than (a) 0.3 percent by
volume when CO2 is greater than 4.0 percent or (b) 0.2 percent by volume
when CO2 is less than or equal to 4.0 percent. Average three acceptable
values of percent CO2, and report the results to the nearest 0.2
percent.
3.2.6.2 For percent O2, repeat the analytical procedure until the
results of any three analyses differ by no more than (a) 0.3 percent by
volume when O2 is less than 15.0 percent or (b) 0.2 percent by volume
when O2 is greater than or equal to 15.0 percent. Average the three
acceptable values of percent O2, and report the results to the nearest
0.1 percent.
3.2.6.3 For percent CO, repeat the analytical procedure until the
results of any three analyses differ by no more than 0.3 percent.
Average the three acceptable values of percent CO, and report the
results to the nearest 0.1 percent.
3.2.7 After the analysis is completed, leak check (mandatory) the
Orsat analyzer once again, as described in Section 6 of Method 3. For
the results of the analysis to be valid, the Orsat analyzer must pass
this leak test before and after the analysis.
3.3.1 The sampling points shall be determined as specified in Section
5.3 of Method 3.
3.3.2 Follow the procedures outlined in Sections 3.2.2 through 3.2.7,
except for the following: Traverse all sampling points, and sample at
each point for an equal length of time. Record sampling data as shown
in Figure 3-3 of Method 3.
3.4.1 Data Validation When Both CO2 and O2 Are Measured. Although in
most instances, only CO2 or O2 measurement is required, it is
recommended that both CO2 and O2 be measured to provide a check on the
quality of the data. The following quality control procedure is
suggested.
Note. -- Since the method for validating he CO2 and O2 analyses is
based on combustion of organic and fossil fuels and dilution of the gas
stream with air, this method does not apply to sources that (1) remove
CO2 or O2 through processes other than combustion, (2) add O2 (e.g.,
oxygen enrichment) and N2 in proportions different from that of air, (3)
add CO2 (e.g., cement or lime kilns), or (4) have no fuel factor, Fo,
values obtainable (e.g., extremely variable waste mixtures). This
method validates the measured proportions of CO2 and O2 for fuel type,
but the method does not detect sample dilution resulting from leaks
during or after sample collection. The method is applicable for samples
collected downstream of most lime or limestone flue-gas desulfurization
units as the CO2 added or removed from the gas stream is not significant
in relation to the total CO2 concentration. The CO2 concentrations from
other types of scrubbers using only water or basic slurry can be
significantly affected and would render the Fo check minimally useful.
3.4..1.1 Calculate a fuel factor, Fo, using the following equation:
where:
%O2=Percent O2 by volume, dry basis.
%CO2=Percent CO2 by volume, dry basis.
20.9=Percent O2 by volume in ambient air.
If CO present in quantities measurable by this method, adjust the O2
and CO2 values before performing the calculation for F0 as follows:
%CO2 (adj) = %CO2 + %CO
%O2 (adj) = %O2 ^ 0.5 %CO
where:
%5CO = Percent CO by volume, dry basis.
3.4.1.2 Compare the calculated F0 factor with the expected F0 values.
The following table may be used in establishing acceptable ranges for
the expected F0 if the fuel being burned is known. When fuels are
burned in combinations, calculate the combined fuel Fd and Fc factors
(as defined in Method 19) according to the procedure in Method 19,
Section 5.2.3. Then calculate the F0 factor as follows:
3.4.1.3 Calculated F0 values, beyond the acceptable ranges shown in
this table, should be investigated before accepting the test results.
For example, the strength of the solutions in the gas analyzer and the
analyzing technique should be checked by sampling and analyzing a known
concentration, such as air; the fuel factor should be reviewed and
verified. An acceptability range of 12 percent is appropriate for the
F0 factor of mixed fuels with variable fuel ratios. The level of the
emission rate relative to the compliance level should be considered in
determining if a retest is appropriate, i.e.; if the measured emissions
are much lower or much greater than the compliance limit, repetition of
the test would not significantly change the compliance status of the
source and would be unnecessarily time consuming and costly.
4.1 Nomenclature. Same as Section 5 of Method 3 with the addition of
the following:
%EA = Percent excess air.
0.264 = Ratio of O2 to N2 in air, v/v.
4.2 Percent Excess Air. Calculate the percent excess air (if
applicable) by substituting the appropriate values of percent O2, CO,
and N2 (obtained from Section 3.1.3 or 3.2.4) into Equation 3B-3.
Note. -- The equation above assumes that ambient air is used as the
source of O2 and that the fuel does not contain appreciable amounts of
N2 (as do coke oven or blast furnace gases). For those cases when
appreciable amounts of N2 are present (coal, oil and natural gas do not
contain appreciable amounts of N2) or when oxygen enrichment is used,
alternative methods, subject to approval of the Administrator, are
required.
Same as Method 3.
40 CFR 60.748 Pt. 60, App. A, Meth. 4
1. Principle and Applicability
1.1 Principle. A gas sample is extracted at a constant rate from the
source; moisture is removed from the sample stream and determined
either volumetrically or gravimetrically.
1.2 Applicability. This method is applicable for determining the
moisture content of stack gas.
Two procedures are given. The first is a reference method, for
accurate determinations of moisture content (such as are needed to
calculate emission data). The second is an approximation method, which
provides estimates of percent moisture to aid in setting isokinetic
sampling rates prior to a pollutant emission measurement run. The
approximation method described herein is only a suggested approach;
alternative means for approximating the moisture content, e.g., drying
tubes, wet bulb-dry bulb techniques, condensation techniques,
stoichiometric calculations, previous experience, etc., are also
acceptable.
The reference method is often conducted simultaneously with a
pollutant emission measurement run; when it is, calculation of percent
isokinetic, pollutant emission rate, etc., for the run shall be based
upon the results of the reference method or its equivalent; these
calculations shall not be based upon the results of the approximation
method, unless the approximation method is shown, to the satisfaction of
the Administrator, U.S. Environmental Protection Agency, to be capable
of yielding results within 1 percent H2O of the reference method.
Note: The reference method may yield questionable results when
applied to saturated gas streams or to streams that contain water
droplets. Therefore, when these conditions exist or are suspected, a
second determination of the moisture content shall be made
simultaneously with the reference method, as follows: Assume that the
gas stream is saturated. Attach a temperature sensor (capable of
measuring to 1 C (2 F)) to the reference method probe. Measure the
stack gas temperature at each traverse point (see Section 2.2.1) during
the reference method traverse; calculate the average stack gas
temperature. Next, determine the moisture percentage, either by: (1)
using a psychrometric chart and making appropriate corrections if stack
pressure is different from that of the chart, or (2) using saturation
vapor pressure tables. In cases where the pyschrometric chart or the
saturation vapor pressure tables are not applicable (based on evaluation
of the process), alternative methods, subject to the approval of the
Administrator, shall be used.
2. Reference Method
The procedure described in Method 5 for determining moisture content
is acceptable as a reference method.
2.1 Apparatus. A schematic of the sampling train used in this
reference method is shown in Figure 4-1. All components shall be
maintained and calibrated according to the procedure outlined in Method
5.
Insert illus. 225
2.1.1 Probe. The probe is constructed of stainless steel or glass
tubing, sufficiently heated to prevent water condensation, and is
equipped with a filter, either in-stack (e.g., a plug of glass wool
inserted into the end of the probe) or heated out-stack (e.g., as
described in Method 5), to remove particular matter.
When stack conditions permit, other metals or plastic tubing may be
used for the probe, subject to the approval of the Administrator.
2.1.2 Condenser. The condenser consists of four impingers connected
in series with ground glass, leak-free fittings or any similarly
leak-free non-contaminating fittings. The first, third, and fourth
impingers shall be of the Greenburg-Smith design, modified by replacing
the tip with a 1.3 centimeter ( 1/2 inch) ID glass tube extending to
about 1.3 cm ( 1/2 in.) from the bottom of the flask. The second
impinger shall be of the Greenburg-Smith design with the standard tip.
Modifications (e.g., using flexible connections between the impingers,
using materials other than glass, or using flexible vacuum lines to
connect the filter holder to the condenser) may be used, subject to the
approval of the Administrator.
The first two impingers shall contain known volumes of water, the
third shall be empty, and the fourth shall contain a known weight of 6-
to 16-mesh indicating type silica gel, or equivalent desiccant. If the
silica gel has been previously used, dry at 175 C (350 F) for 2 hours.
New silica gel may be used as received. A thermometer, capable of
measuring temperature to within 1 C (2 F), shall be placed at the
outlet of the fourth impinger, for monitoring purposes.
Alternatively, any system may be used (subject to the approval of the
Administrator) that cools the sample gas stream and allows measurement
of both the water that has been condensed and the moisture leaving the
condenser, each to within 1 ml or 1 g. Acceptable means are to measure
the condensed water, either gravimetrically or volumetrically, and to
measure the moisture leaving the condenser by: (1) monitoring the
temperature and pressure at the exit of the condenser and using Dalton's
law of partial pressures, or (2) passing the sample gas stream through a
tared silica gel (or equivalent desiccant) trap, with exit gases kept
below 20 C (68 F), and determining the weight gain.
If means other than silica gel are used to determine the amount of
moisture leaving the condenser, it is recommended that silica gel (or
equivalent) still be used between the condenser system and pump, to
prevent moisture condensation in the pump and metering devices and to
avoid the need to make corrections for moisture in the metered volume.
2.1.3 Cooling System. An ice bath container and crushed ice (or
equivalent) are used to aid in condensing moisture.
2.1.4 Metering System. This system includes a vacuum gauge,
leak-free pump, thermometers capable of measuring temperature to within
3 C (5.4 F), dry gas meter capable of measuring volume to within 2
percent, and related equipment as shown in Figure 4-1. Other metering
systems, capable of maintaining a constant sampling rate and determining
sample gas volume, may be used, subject to the approval of the
Administrator.
2.1.5 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg) may be
used. In many cases, the barometric reading may be obtained from a
nearby National Weather Service station, in which case the station value
(which is the absolute barometric pressure) shall be requested and an
adjustment for elevation differences between the weather station and the
sampling point shall be applied at a rate of minus 2.5 mm Hg (0.1 in.
Hg) per 30 m (100 ft) elevation increase or vice versa for elevation
decrease.
2.1.6 Graduated Cylinder and/or Balance. These items are used to
measure condensed water and moisture caught in the silica gel to within
1 ml or 0.5 g. Graduated cylinders shall have subdivisions no greater
than 2 ml. Most laboratory balances are capable of weighing to the
nearest 0.5 g or less. These balances are suitable for use here.
2.2 Procedure. The following procedure is written for a condenser
system (such as the impinger system described in Section 2.1.2)
incorporating volumetric analysis to measure the condensed moisture, and
silica gel and gravimetric analysis to measure the moisture leaving the
condenser.
2.2.1 Unless otherwise specified by the Administrator, a minimum of
eight traverse points shall be used for circular stacks having diameters
less than 0.61 m (24 in.), a minimum of nine points shall be used for
rectangular stacks having equivalent diameters less than 0.61 m (24
in.), and a minimum of twelve traverse points shall be used in all other
cases. The traverse points shall be located according to Method 1. The
use of fewer points is subject to the approval of the Administrator.
Select a suitable probe and probe length such that all traverse points
can be sampled. Consider sampling from opposite sides of the stack
(four total sampling ports) for large stacks, to permit use of shorter
probe lengths. Mark the probe with heat resistant tape or by some other
method to denote the proper distance into the stack or duct for each
sampling point. Place known volumes of water in the first two
impingers. Weigh and record the weight of the silica gel to the nearest
0.5 g, and transfer the silica gel to the fourth impinger;
alternatively, the silica gel may first be transferred to the impinger,
and the weight of the silica gel plus impinger recorded.
2.2.2 Select a total sampling time such that a minimum total gas
volume of 0.60 scm (21 scf) will be collected, at a rate no greater than
0.021 m3/min (0.75 cfm). When both moisture content and pollutant
emission rate are to be determined, the moisture determination shall be
simultaneous with, and for the same total length of time as, the
pollutant emission rate run, unless otherwise specified in an applicable
subpart of the standards.
2.2.3 Set up the sampling train as shown in Figure 4-1. Turn on the
probe heater and (if applicable) the filter heating system to
temperatures of about 120 C (248 F), to prevent water condensation
ahead of the condenser; allow time for the temperatures to stabilize.
Place crushed ice in the ice bath container. It is recommended, but not
required, that a leak check be done, as follows: Disconnect the probe
from the first impinger or (if applicable) from the filter holder. Plug
the inlet to the first impinger (or filter holder) and pull a 380 mm (15
in.) Hg vacuum; a lower vacuum may be used, provided that it is not
exceeded during the test. A leakage rate in excess of 4 percent of the
average sampling rate or 0.00057 m3/min (0.02 cfm), whichever is less,
is unacceptable. Following the leak check, reconnect the probe to the
sampling train.
2.2.4 During the sampling run, maintain a sampling rate within 10
percent of constant rate, or as specified by the Administrator. For
each run, record the data required on the example data sheet shown in
Figure 4-2. Be sure to record the dry gas meter reading at the
beginning and end of each sampling time increment and whenever sampling
is halted. Take other appropriate readings at each sample point, at
least once during each time increment.
2.2.5 To begin sampling, position the probe tip at the first traverse
point. Immediately start the pump and adjust the flow to the desired
rate. Traverse the cross section, sampling at each traverse point for
an equal length of time. Add more ice and, if necessary, salt to
maintain a temperature of less 20 C (68 F) at the silica gel outlet.
2.2.6 After collecting the sample, disconnect the probe from the
filter holder (or from the first impinger) and conduct a leak check
(mandatory) as described in Section 2.2.3. Record the leak rate. If the
leakage rate exceeds the allowable rate, the tester shall either reject
the test results or shall correct the sample volume as in Section 6.3 of
Method 5. Next, measure the volume of the moisture condensed to the
nearest ml. Determine the increase in weight of the silica gel (or
silica gel plus impinger) to the nearest 0.5 g. Record this information
(see example data sheet, Figure 4-3) and calculate the moisture
percentage, as described in 2.3 below.
2.2.7 A quality control check of the volume metering system at the
field site is suggested before collecting the sample following the
procedure in Method 5, Section 4.4
2.3 Calculations. Carry out the following calculations, retaining at
least one extra decimal figure beyond that of the acquired data. Round
off figures after final calculation.
2.3.1 Nomenclature.
Bws=Proportion of water vapor, by volume, in the gas stream.
Mw=Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb-mole).
Pm=Absolute pressure (for this method, same as barometric pressure)
at the dry gas meter, mm Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
R=Ideal gas constant, 0.06236 (mm Hg) (m3)/(g-mole) ( K) for metric
units and 21.85 (in. Hg) (ft3)/(lb-mole) ( R) for English units.
Tm=Absolute temperature at meter, K ( R).
Tstd=Standard absolute temperature, 293 K (528 R).
Vm=Dry gas volume measured by dry gas meter, dcm (dcf).
Vm=Incremental dry gas volume measured by dry gas meter at each
traverse point, dcm (dcf).
Vm(std)=Dry gas volume measured by the dry gas meter, corrected to
standard conditions, dscm (dscf).
Vwc(std)=Volume of water vapor condensed corrected to standard
conditions, scm (scf).
Vwsg(std)=Volume of water vapor collected in silica gel corrected to
standard conditions, scm (scf).
Vf=Final volume of condenser water, ml.
Vi=Initial volume, if any, of condenser water, ml.
Wf=Final weight of silica gel or silica gel plus impinger, g.
Wi=Initial weight of silica gel or silica gel plus impinger, g.
Y=Dry gas meter calibration factor.
w=Density of water, 0.9982 g/ml (0.002201 lb/ml).
2.3.2 Volume of Water Vapor Condensed.
Eq. 4-1
Where:
K1=0.001333 m3/ml for metric units
=0.04707 ft3/ml for English units
2.3.3 Volume of Water Vapor Collected in Silica Gel.
Eq. 4-2
Where:
K2=0.001335 m3/g for metric units
=0.04715 ft3/g for English units
2.3.4 Sample Gas Volume.
Eq. 4-3
Where:
K3=0.3858 K/mm Hg for metric units
=17.64 R/in. Hg for English units
Note: If the post-test leak rate (Section 2.2.6) exceeds the
allowable rate, correct the value of Vm in Equation 4-3, as described in
Section 6.3 of Method 5.
2.3.5 Moisture Content.
Eq. 4-4
Note: In saturated or moisture droplet-laden gas streams, two
calculations of the moisture content of the stack gas shall be made, one
using a value based upon the saturated conditions (see Section 1.2), and
another based upon the results of the impinger analysis. The lower of
these two values of Bws shall be considered correct.
2.3.6 Verification of Constant Sampling Rate. For each time
increment, determine the Vm. Calculate the average. If the value for
any time increment differs from the average by more than 10 percent,
reject the results and repeat the run.
3. Approximation Method
The approximation method described below is presented only as a
suggested method (see Section 1.2).
3.1 Apparatus.
3.1.1 Probe. Stainless steel glass tubing, sufficiently heated to
prevent water condensation and equipped with a filter (either in-stack
or heated out-stack) to remove particulate matter. A plug of glass
wool, inserted into the end of the probe, is a satisfactory filter.
3.1.2 Impingers. Two midget impingers, each with 30 ml capacity, or
equivalent.
3.1.3 Ice Bath. Container and ice, to aid in condensing moisture in
impingers.
3.1.4 Drying Tube. Tube packed with new or regenerated 6- to 16-mesh
indicating-type silica gel (or equivalent desiccant), to dry the sample
gas and to protect the meter and pump.
3.1.5 Valve. Needle valve, to regulate the sample gas flow rate.
3.1.6 Pump. Leak-free, diaphragm type, or equivalent, to pull the gas
sample through the train.
3.1.7 Volume Meter. Dry gas meter, sufficiently accurate to measure
the sample volume within 2%, and calibrated over the range of flow rates
and conditions actually encountered during sampling.
3.1.8 Rate Meter. Rotameter, to measure the flow range from 0 to 3
lpm (0 to 0.11 cfm).
3.1.9 Graduated Cylinder. 25 ml.
3.1.10 Barometer. Mercury, aneroid, or other barometer, as described
in Section 2.1.5 above.
3.1.11 Vacuum Gauge. At least 760 mm Hg (30 in. Hg) gauge, to be
used for the sampling leak check.
3.2 Procedure.
3.2.1 Place exactly 5 ml distilled water in each impinger.
Leak check the sampling train as follows: Temporarily insert a
vacuum gauge at or near the probe inlet; then, plug the probe inlet and
pull a vacuum of at least 250 mm Hg (10 in. Hg). Note the time rate of
change of the dry gas meter dial; alternatively, a rotameter (0-40
cc/min) may be temporarily attached to the dry gas meter outlet to
determine the leakage rate. A leak rate not in excess of 2 percent of
the average sampling rate is acceptable.
Note: Carefully release the probe inlet plug before turning off the
pump.
Insert Fig. 4-4
3.2.2 Connect the probe, insert it into the stack, and sample at a
constant rate of 2 lpm (0.071 cfm). Continue sampling until the dry gas
meter registers about 30 liters (1.1 ft3) or until visible liquid
droplets are carried over from the first impinger to the second. Record
temperature, pressure, and dry gas meter readings as required by Figure
4-5.
3.2.3 After collecting the sample, combine the contents of the two
impingers and measure the volume to the nearest 0.5 ml.
3.3 Calculations. The calculation method presented is designed to
estimate the moisture in the stack gas; therefore, other data, which
are only necessary for accurate moisture determinations, are not
collected. The following equations adequately estimate the moisture
content, for the purpose of determining isokinetic sampling rate
settings.
3.3.1 Nomenclature.
Bwm=Approximate proportion, by volume, of water vapor in the gas
stream leaving the second impinger, 0.025.
Bws=Water vapor in the gas stream, proportion by volume.
Mw=Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb-mole).
Pm=Absolute pressure (for this method, same as barometric pressure)
at the dry gas meter.
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
R=Ideal gas constant, 0.06236 (mm Hg) (m3)/(g-mole) ( K) for metric
units and 21.85 (in. Hg) (ft3)/lb-mole) ( R) for English units.
Tm=Absolute temperature at meter, K ( R).
Tstd=Standard absolute temperature, 293 K (528 R).
Vf=Final volume of impinger contents, ml.
Vi=Initial volume of impinger contents, ml.
Vm=Dry gas volume measured by dry gas meter, dcm (dcf).
Vm(std)=Dry gas volume measured by dry gas meter, corrected to
standard conditions, dscm (dscf).
Vwc(std)=Volume of water vapor condensed, corrected to standard
conditions, scm (scf).
w=Density of water, 0.9982 g/ml (0.002201 lb/ml).
Y=Dry gas meter calibration factor.
3.3.2 Volume of Water Vapor Collected.
Eq. 4-5
Where:
K1=0.001333 m3/ml for metric units
=0.04707 ft3/ml for English units.
3.3.3 Gas Volume.
Insert illus. 233
where:
K2=0.3858 K/mm Hg for metric units
=17.64 R/in. Hg for English units
3.3.4 Approximate Moisture Content.
Insert illus. 234
4. Calibration
4.1 For the reference method, calibrate equipment as specified in the
following sections of Method 5: Section 5.3 (metering system); Section
5.5 (temperature gauges); and Section 5.7 (barometer). The recommended
leak check of the metering system (Section 5.6 of Method 5) also applies
to the reference method. For the approximation method, use the
procedures outlined in Section 5.1.1 of Method 6 to calibrate the
metering system, and the procedure of Method 5, Section 5.7 to calibrate
the barometer.
5. Bibliography
1. Air Pollution Engineering Manual (Second Edition). Danielson, J.
A. (ed.). U.S. Environmental Protection Agency, Office of Air Quality
Planning and Standards. Research Triangle Park, NC. Publication No.
AP-40. 1973.
2. Devorkin, Howard. et al. Air Pollution Source Testing Manual.
Air Pollution Control District, Los Angeles, CA. November, 1963.
3. Methods for Determination of Velocity, Volume, Dust and Mist
Content of Gases. Western Precipitation Division of Joy Manufacturing
Co., Los Angeles, CA. Bulletin WP-50. 1968.
40 CFR 60.748 Pt. 60, App. A, Meth. 5
1. Principle and Applicability
1.1 Principle. Particulate matter is withdrawn isokinetically from
the source and collected on a glass fiber filter maintained at a
temperature in the range of 120 14 C (248 25 F) or such other
temperature as specified by an applicable subpart of the standards or
approved by Administrator, U.S. Environmental Protection Agency, for a
particular application. The particulate mass, which includes any
material that condenses at or above the filtration temperature, is
determined gravimetrically after removal of uncombined water.
1.2 Applicability. This method is applicable for the determination of
particulate emissions from stationary sources.
2. Apparatus
2.1 Sampling Train. A schematic of the sampling train used in this
method is shown in Figure 5-1. Complete construction details are given
in APTD-0581 (Citation 2 in Bibliography); commercial models of this
train are also available. For changes from APTD-0581 and for allowable
modifications of the train shown in Figure 5-1, see the following
subsections.
The operating and maintenance procedures for the sampling train are
described in APTD-0576 (Citation 3 in Bibliography). Since correct
usage is important in obtaining valid results, all users should read
APTD-0576 and adopt the operating and maintenance procedures outlined in
it, unless otherwise specified herein. The sampling train consists of
the following components:
Insert illus. 235
2.1.1 Probe Nozzle. Stainless steel (316) or glass with sharp,
tapered leading edge. The angle of taper shall be 30 and the taper
shall be on the outside to preserve a constant internal diameter. The
probe nozzle shall be of the button-hook or elbow design, unless
otherwise specified by the Administrator. If made of stainless steel,
the nozzle shall be constructed from seamless tubing; other materials
of construction may be used, subject to the approval of the
Administrator.
A range of nozzle sizes suitable for isokinetic sampling should be
available, e.g., 0.32 to 1.27 cm ( 1/8 to 1/2 in.) -- or larger if
higher volume sampling trains are used -- inside diameter (ID) nozzles
in increments of 0.16 cm ( 1/16 in.). Each nozzle shall be calibrated
according to the procedures outlined in Section 5.
2.1.2 Probe Liner. Borosilicate or quartz glass tubing with a
heating system capable of maintaining a gas temperature at the exit end
during sampling of 120 14 C (248 25 F), or such other temperature as
specified by an applicable subpart of the standards or approved by the
Administrator for a particular application. (The tester may opt to
operate the equipment at a temperature lower than that specified.) Since
the actual temperature at the outlet of the probe is not usually
monitored during sampling, probes constructed according to APTD-0581 and
utilizing the calibration curves of APTD-0576 (or calibrated according
to the procedure outlined in APTD-0576) will be considered acceptable.
Either borosilicate or quartz glass probe liners may be used for
stack temperatures up to about 480 C (900 F); quartz liners shall be
used for temperatures between 480 and 900 C (900 and 1,650 F). Both
types of liners may be used at higher temperatures than specified for
short periods of time, subject to the approval of the Administrator.
The softening temperature for borosilicate is 820 C (1,508 F), and for
quartz it is 1,500 C (2,732 F).
Whenever practical, every effort should be made to use borosilicate
or quartz glass probe liners. Alternatively, metal liners (e.g., 316
stainless steel, Incoloy 825,2 or other corrosion resistant metals) made
of seamless tubing may be used, subject to the approval of the
Administrator.
2.1.3 Pitot Tube. Type S, as described in Section 2.1 of Method 2,
or other device approved by the Administrator. The pitot tube shall be
attached to the probe (as shown in Figure 5-1) to allow constant
monitoring of the stack gas velocity. The impact (high pressure)
opening plane of the pitot tube shall be even with or above the nozzle
entry plane (see Method 2, Figure 2-6b) during sampling. The Type S
pitot tube assembly shall have a known coefficient, determined as
outlined in Section 4 of Method 2.
2.1.4 Differential Pressure Gauge. Inclined manometer or equivalent
device (two), as described in Section 2.2 of Method 2. One manometer
shall be used or velocity head ( ) readings, and the other, for orifice
differential pressure readings.
2.1.5 Filter Holder. Borosilicate glass, with a glass frit filter
support and a silicone rubber gasket. Other materials of construction
(e.g., stainless steel, Teflon, Viton) may be used, subject to approval
of the Administrator. The holder design shall provide a positive seal
against leakage from the outside or around the filter. The holder shall
be attached immediately at the outlet of the probe (or cyclone, it
used).
2.1.6 Filter Heating System. Any heating system capable of
maintaining a temperature around the filter holder during sampling of
120 14 C (248 25 F), or such other temperature as specified by an
applicable subpart of the standards or approved by the Administrator for
a particular application. Alternatively, the tester may opt to operate
the equipment at a temperature lower than that specified. A temperature
gauge capable of measuring temperature to within 3 C (5.4 F) shall be
installed so that the temperature around the filter holder can be
regulated and monitored during sampling. Heating systems other than the
one shown in APTD-0581 may be used.
2.1.7 Condenser. The following system shall be used to determine the
stack gas moisture content: Four impingers connected in series with
leak-free ground glass fittings or any similar leak-free
non-contaminating fittings. The first, third, and fourth impingers
shall be of the Greenburg-Smith design, modified by replacing the tip
with 1.3 cm ( 1/2 in.) ID glass tube extending to about 1.3 cm ( 1/2
in.) from the bottom of the flask. The second impinger shall be of the
Greenburg-Smith design with the standard tip. Modifications (e.g.,
using flexible connections between the impingers, using materials other
than glass, or using flexible vacuum lines to connect the filter holder
to the condenser) may be used, subject to the approval of the
Administrator. The first and second impingers shall contain known
quantities of water (Section 4.1.3), the third shall be empty, and the
fourth shall contain a known weight of silica gel, or equivalent
desiccant. A thermometer, capable of measuring temperature to within 1
C (2 F) shall be placed at the outlet of the fourth impinger for
monitoring purposes.
Alternatively, any system that cools the sample gas stream and allows
measurement of the water condensed and moisture leaving the condenser,
each to within 1 ml or 1 g may be used, subject to the approval of the
Administrator. Acceptable means are to measure the condensed water
either gravimetrically or volumetrically and to measure the moisture
leaving the condenser by: (1) monitoring the temperature and pressure
at the exit of the condenser and using Dalton's law of partial
pressures; or (2) passing the sample has stream through a tared silica
gel (or equivalent desiccant) trap with exit gases kept below 20 C (68
F) and determining the weight gain.
If means other than silica gel are used to determine the amount of
moisture leaving the condenser, it is recommended that silica gel (or
equivalent) still be used between the condenser system and pump to
prevent moisture condensation in the pump and metering devices and to
avoid the need to make corrections for moisture in the metered volume.
Note: If a determination of the particulate matter collected in the
impingers is desired in addition to moisture content, the impinger
system described above shall be used, without modification. Individual
States or control agencies requiring this information shall be contacted
as to the sample recovery and analysis of the impinger contents.
2.1.8 Metering System. Vacuum gauge, leak-free pump, thermometers
capable of measuring temperature to within 3 C (5.4 F), dry gas meter
capable of measuring volume to within 2 percent, and related equipment,
as shown in Figure 5-1. Other metering systems capable of maintaining
sampling rates within 10 percent of isokinetic and of determining sample
volumes to within 2 percent may be used, subject to the approval of the
Administrator. When the metering system is used in conjunction with a
pitot tube, the system shall enable checks of isokinetic rates.
Sampling trains utilizing metering systems designed for higher flow
rates than that decribed in APTD-0581 or APDT-0576 may be used provided
that the specifications of this method are met.
2.1.9 Barometer. Mercury aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg). In many
cases the barometric reading may be obtained from a nearby National
Weather Service station, in which case the station value (which is the
absolute barometric pressure) shall be requested and an adjustment for
elevation differences between the weather station and sampling point
shall be applied at a rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 m
(100 ft) elevation increase or vice versa for elevation decrease.
2.1.10 Gas Density Determination Equipment. Temperature sensor and
pressure gauge, as described in Sections 2.3 and 2.4 of Method 2, and
gas analyzer, if necessary, as described in Method 3. The temperature
sensor shall, preferably, be permanently attached to the pitot tube or
sampling probe in a fixed configuration, such that the tip of the sensor
extends beyond the leading edge of the probe sheath and does not touch
any metal. Alternatively, the sensor may be attached just prior to use
in the field. Note, however, that if the temperature sensor is attached
in the field, the sensor must be placed in an interference-free
arrangement with respect to the Type S pitot tube openings (see Method
2, Figure 2-7). As a second alternative, if a difference of not more
than 1 percent in the average velocity measurement is to be introduced,
the temperature gauge need not be attached to the probe or pitot tube.
(This alternative is subject to the approval of the Administrator.)
2.2 Sample Recovery. The following items are needed.
2.2.1 Probe-Liner and Probe-Nozzle Brushes. Nylon bristle brushes
with stainless steel wire handles. The probe brush shall have
extensions (at least as long as the probe) of stainless steel, Nylon,
Teflon, or similarly inert material. The brushes shall be properly
sized and shaped to brush out the probe liner and nozzle.
2.2.2 Wash Bottles -- Two. Glass wash bottles are recommended;
polyethylene wash bottles may be used at the option of the tester. It
is recommended that acetone not be stored in polyethylene bottles for
longer than a month.
2.2.3 Glass Sample Storage Containers. Chemically resistant,
borosilicate glass bottles, for acetone washes, 500 ml or 1000 ml.
Screw cap liners shall either be rubber-backed Teflon or shall be
constructed so as to be leak-free and resistant to chemical attack by
acetone. (Narrow mouth glass bottles have been found to be less prone
to leakage.) Alternatively, polyethylene bottles may be used.
2.2.4 Petri Dishes. For filter samples, glass or polyethylene,
unless otherwise specified by the Administrator.
2.2.5 Graduated Cylinder and/or Balance. To measure condensed water
to within 1 ml or 1 g. Graduated cylinders shall have subdivisions no
greater than 2 ml. Most laboratory balances are capable of weighing to
the nearest 0.5 g or less. Any of these balances is suitable or use
here and in Section 2.3.4.
2.2.6 Plastic Storage Containers. Air-tight containers to store
silica gel.
2.2.7 Funnel and Rubber Policeman. To aid in transfer of silica gel
to container; not necessary if silica gel is weighed in the field.
2.2.8 Funnel. Glass or polyethylene, to aid in sample recovery.
2.3 Analysis. For analysis, the following equipment is needed.
2.3.1 Glass Weighing Dishes.
2.3.2 Desiccator.
2.3.3 Analytical Balance. To measure to within 0.1 mg.
2.3.4 Balance. To measure to within 0.5 g.
2.3.5 Beakers. 250 ml.
2.3.6 Hygrometer. To measure the relative humidity of the laboratory
environment.
2.3.7 Temperature Gauge. To measure the temperature of the
laboratory environment.
3. Reagents
3.1 Sampling. The reagents used in sampling are as follows:
3.1.1 Filters. Glass fiber filters, without organic binder,
exhibiting at least 99.95 percent efficiency (<0.05 percent penetration)
on 0.3-micron dioctyl phthalate smoke particles. The filter efficiency
test shall be conducted in accordance with ASTM Standard Method D2986-71
(Reapproved 1978) (incorporated by reference -- see 60.17). Test data
from the supplier's quality control program are sufficient for this
purpose. In sources containing SO2 or SO3, the filter material must be
of a type that is unreactive to SO2 or SO3. Citation 10 in
Bibliography, may be used to select the appropriate filter.
3.1.2 Silica Gel. Indicating type, 6 to 16 mesh. If previously
used, dry at 175 C (350 F) for 2 hours. New silica gel may be used as
received. Alternatively, other types of desiccants (equivalent or
better) may be used, subject to the approval of the Administrator.
3.1.3 Water. When analysis of the material caught in the impingers is
required, deionized distilled water shall be used. Run blanks prior to
field use to eliminate a high blank on test samples.
3.1.4 Crushed Ice.
3.1.5 Stopcock Grease. Acetone-insoluble, heat-stable silicone
grease. This is not necessary if screw-on connectors with Teflon
sleeves, or similar, are used. Alternatively, other types of stopcock
grease may be used, subject to the approval of the Administrator.
3.2 Sample Recovery. Acetone-reagent grade, 0.001 percent residue,
in glass bottles -- is required. Acetone from metal containers
generally has a high residue blank and should not be used. Sometimes,
suppliers transfer acetone to glass bottles from metal containers;
thus, acetone blanks shall be run prior to field use and only acetone
with low blank values ( 0.001 percent) shall be used. In no case shall
a blank value of greater than 0.001 percent of the weight of acetone
used be subtracted from the sample weight.
3.3 Analysis. Two reagents are required for the analysis:
3.3.1 Acetone. Same as 3.2.
3.3.2 Desiccant. Anhydrous calcium sulfate, indicating type.
Alternatively, other types of desiccants may be used, subject to the
approval of the Administrator.
4. Procedure
4.1 Sampling. The complexity of this method is such that, in order to
obtain reliable results, testers should be trained and experienced with
the test procedures.
4.1.1 Pretest Preparation. It is suggested that sampling equipment
be maintained according to the procedure described in APTD-0576.
Weigh several 200 to 300 g portions of silica gel in air-tight
containers to the nearest 0.5 g. Record the total weight of the silica
gel plus container, on each container. As an alternative, the silica
gel need not be preweighed, but may be weighed directly in the impinger
or sampling holder just prior to train assembly.
Check filters visually against light for irregularities and flaws or
pinhole leaks. Label filters of the proper diameter on the back side
near the edge using numbering machine ink. As an alternative, label the
shipping containers (glass or plastic petri dishes) and keep the filters
in these containers at all times except during sampling and weighing.
Desiccate the filters at 20 5.6 C (68 10 F) and ambient pressure
for at least 24 hours and weigh at intervals of at least 6 hours to a
constant weight, i.e., 0.5 mg change from previous weighing; record
results to the nearest 0.1 mg. During each weighing the filter must not
be exposed to the laboratory atmosphere for a period greater than 2
minutes and a relative humidity above 50 percent. Alternatively (unless
otherwise specified by the Administrator), the filters may be oven dried
at 105 C (220 F) for 2 to 3 hours, desiccated for 2 hours, and
weighed. Procedures other than those described, which account for
relative humidity effects, may be used, subject to the approval of the
Administrator.
4.1.2 Preliminary Determinations. Select the sampling site and the
minimum number of sampling points according to Method 1 or as specified
by the Administrator. Determine the stack pressure, temperature, and
the range of velocity heads using Method 2; it is recommended that a
leak-check of the pitot lines (see Method 2, Section 3.1) be performed.
Determine the moisture content using Approximation Method 4 or its
alternatives for the purpose of making isokinetic sampling rate
settings. Determine the stack gas dry molecular weight, as described in
Method 2, Section 3.6; if integrated Method 3 sampling is used for
molecular weight determination, the integrated bag sample shall be taken
simultaneously with, and for the same total length of time as, the
particulate sample run.
Select a nozzle size based on the range of velocity heads, such that
it is not necessary to change the nozzle size in order to maintain
isokinetic sampling rates. During the run, do not change the nozzle
size. Ensure that the proper differential pressure gauge is chosen for
the range of velocity heads encountered (see Section 2.2 of Method 2).
Select a suitable probe liner and probe length such that all traverse
points can be sampled. For large stacks, consider sampling from
opposite sides of the stack to reduce the length of probes.
Select a total sampling time greater than or equal to the minimum
total sampling time specified in the test procedures for the specific
industry such that (1) the sampling time per point is not less than 2
min (or some greater time interval as specified by the Administrator),
and (2) the sample volume taken (corrected to standard conditions) will
exceed the required minimum total gas sample volume. The latter is
based on an approximate average sampling rate.
It is recommended that the number of minutes sampled at each point be
an integer or an integer plus one-half minute, in order to avoid
timekeeping errors. The sampling time at each point shall be the same.
In some circumstances, e.g., batch cycles, it may be necessary to
sample for shorter times at the traverse points and to obtain smaller
gas sample volumes. In these cases, the Administrator's approval must
first be obtained.
4.1.3 Preparation of Collection Train. During preparation and
assembly of the sampling train, keep all openings where contamination
can occur covered until just prior to assembly or until sampling is
about to begin.
Place 100 ml of water in each of the first two impingers, leave the
third impinger empty, and transfer approximately 200 to 300 g of
preweighed silica gel from its container to the fourth impinger. More
silica gel may be used, but care should be taken to ensure that it is
not entrained and carried out from the impinger during sampling. Place
the container in a clean place for later use in the sample recovery.
Alternatively, the weight of the silica gel plus impinger may be
determined to the nearest 0.5 g and recorded.
Using a tweezer or clean disposable surgical gloves, place a labeled
(identified) and weighed filter in the filter holder. Be sure that the
filter is properly centered and the gasket properly placed so as to
prevent the sample gas stream from circumventing the filter. Check the
filter for tears after assembly is completed.
When glass liners are used, install the selected nozzle using a Viton
A O-ring when stack temperatures are less than 260 C (500 F) and an
asbestos string gasket when temperatures are higher. See APTD-0576 for
details. Other connecting systems using either 316 stainless steel or
Teflon ferrules may be used. When metal liners are used, install the
nozzle as above or by a leak-free direct mechanical connection. Mark
the probe with heat resistant tape or by some other method to denote the
proper distance into the stack or duct for each sampling point.
Set up the train as in Figure 5-1, using (if necessary) a very light
coat of silicone grease on all ground glass joints, greasing only the
outer portion (see APTD-0576) to avoid possibility of contamination by
the silicone grease. Subject to the approval of the Administrator, a
glass cyclone may be used between the probe and filter holder when the
total particulate catch is expected to exceed 100 mg or when water
droplets are present in the stack gas.
Place crushed ice around the impingers.
4.1.4 Leak-Check Procedures.
4.1.4.1 Pretest Leak-Check. A pretest leak-check is recommended, but
not required. If the tester opts to conduct the pretest leak-check, the
following procedure shall be used.
After the sampling train has been assembled, turn on and set the
filter and probe heating systems at the desired operating temperatures.
Allow time for the temperatures to stabilize. If a Viton A O-ring or
other leak-free connection is used in assembling the probe nozzle to the
probe liner, leak-check the train at the sampling site by plugging the
nozzle and pulling a 380 mm Hg (15 in. Hg) vacuum.
Note: A lower vacuum may be used, provided that it is not exceeded
during the test.
If an asbestos string is used, do not connect the probe to the train
during the leak-check. Instead, leak-check the train by first plugging
the inlet to the filter holder (cyclone, if applicable) and pulling a
380 mm Hg (15 in. Hg) vacuum (see Note immediately above). Then connect
the probe to the train and leak-check at about 25 mm Hg (1 in. Hg)
vacuum; alternatively, the probe may be leak-checked with the rest of
the sampling train, in one step, at 380 mm Hg (15 in. Hg) vacuum.
Leakage rates in excess of 4 percent of the average sampling rate or
0.00057 m3/min (0.02 cfm), whichever is less, are unacceptable.
The following leak-check instructions for the sampling train
described in APTD-0576 and APTD-0581 may be helpful. Start the pump
with bypass valve fully open and coarse adjust valve, completely closed.
Partially open the coarse adjust valve and slowly close the bypass
valve until the desired vacuum is reached. Do not reverse direction of
bypass valve; this will cause water to back up into the filter holder.
If the desired vacuum is exceeded, either leak-check at this higher
vacuum or end the leak-check as shown below and start over.
When the leak-check is completed, first slowly remove the plug from
the inlet to the probe, filter holder, or cyclone (if applicable) and
immediately turn off the vacuum pump. This prevents the water in the
impingers from being forced backward into the filter holder and silica
gel from being entrained backward into the third impinger.
4.1.4.2 Leak-Checks During Sample Run. If, during the sampling run,
a component (e.g., filter assembly or impinger) change becomes
necessary, a leak-check shall be conducted immediately before the change
is made. The leak-check shall be done according to the procedure
outlined in Section 4.1.4.1 above, except that it shall be done at a
vacuum equal to or greater than the maximum value recorded up to that
point in the test. If the leakage rate is found to be no greater than
0.00057 m3/min (0.02 cfm) or 4 percent of the average sampling rate
(whichever is less), the results are acceptable, and no correction will
need to be applied to the total volume of dry gas metered; if, however,
a higher leakage rate is obtained, the tester shall either record the
leakage rate and plan to correct the sample volume as shown in Section
6.3 of this method, or shall void the sampling run.
Immediately after component changes, leak-checks are optional; if
such leak-checks are done, the procedure outlined in Section 4.1.4.1
above shall be used.
4.1.4.3 Post-test Leak-Check. A leak-check is mandatory at the
conclusion of each sampling run. The leak-check shall be done in
accordance with the procedures outlined in Section 4.1.4.1, except that
it shall be conducted at a vacuum equal to or greater than the maximum
value reached during the sampling run. If the leakage rate is found to
be no greater than 0.00057 m3/min (0.02 cfm) or 4 percent of the average
sampling rate (whichever is less), the results are acceptable, and no
correction need be applied to the total volume of dry gas metered. If,
however, a higher leakage rate is obtained, the tester shall either
record the leakage rate and correct the sample volume as shown in
Section 6.3 of this method, or shall void the sampling run.
4.1.5 Particulate Train Operation. During the sampling run, maintain
an isokinetic sampling rate (within 10 percent of true isokinetic unless
otherwise specified by the Administrator) and a temperature around the
filter of 120 14 C (248 25 F), or such other temperature as specified
by an applicable subpart of the standards or approved by the
Administrator.
For each run, record the data required on a data sheet such as the
one shown in Figure 5-2. Be sure to record the initial dry gas meter
reading. Record the dry gas meter readings at the beginning and end of
each sampling time increment, when changes in flow rates are made,
before and after each leak-check, and when sampling is halted. Take
other readings required by Figure 5-2 at least once at each sample point
during each time increment and additional readings when significant
changes (20 percent variation in velocity head readings) necessitate
additional adjustments in flow rate. Level and zero the manometer.
Because the manometer level and zero may drift due to vibrations and
temperature changes, make periodic checks during the traverse.
Clean the portholes prior to the test run to minimize the chance of
sampling deposited material. To begin sampling, remove the nozzle cap,
verify that the filter and probe heating systems are up to temperature,
and that the pitot tube and probe are properly positioned. Position the
nozzle at the first traverse point with the tip pointing directly into
the gas stream. Immediately start the pump and adjust the flow to
isokinetic conditions. Nomographs are available, which aid in the rapid
adjustment of the isokinetic sampling rate without excessive
computations. These nomographs are designed for use when the Type S
pitot tube coefficient is 0.85 0.02, and the stack gas equivalent
density (dry molecular weight) is equal to 29 4. APTD-0576 details the
procedure for using the nomographs. If Cp and Md are outside the above
stated ranges do not use the nomographs unless appropriate steps (see
Citation 7 in Bibliography) are taken to compensate for the deviations.
When the stack is under significant negative pressure (height of
impinger stem), take care to close the coarse adjust valve before
inserting the probe into the stack to prevent water from backing into
the filter holder. If necessary, the pump may be turned on with the
coarse adjust valve closed.
When the probe is in position, block off the openings around the
probe and porthole to prevent unrepresentative dilution of the gas
stream.
Traverse the stack cross-section, as required by Method 1 or as
specified by the Administrator, being careful not to bump the probe
nozzle into the stack walls when sampling near the walls or when
removing or inserting the probe through the portholes; this minimizes
the chance of extracting deposited material.
During the test run, make periodic adjustments to keep the
temperature around the filter holder at the proper level; add more ice
and, if necessary, salt to maintain a temperature of less than 20 C (68
F) at the condenser/silica gel outlet. Also, periodically check the
level and zero of the manometer.
If the pressure drop across the filter becomes too high, making
isokinetic sampling difficult to maintain, the filter may be replaced in
the midst of a sample run. It is recommended that another complete
filter assembly be used rather than attempting to change the filter
itself. Before a new filter assembly is installed, conduct a leak-check
(see Section 4.1.4.2). The total particulate weight shall include the
summation of all filter assembly catches.
A single train shall be used for the entire sample run, except in
cases where simultaneous sampling is required in two or more separate
ducts or at two or more different locations within the same duct, or, in
cases where equipment failure necessitates a change of trains. In all
other situations, the use of two or more trains will be subject to the
approval of the Administrator.
Note that when two or more trains are used, separate analyses of the
front-half and (if applicable) impinger catches from each train shall be
performed, unless identical nozzle sizes were used on all trains, in
which case, the front-half catches from the individual trains may be
combined (as may the impinger catches) and one analysis of front-half
catch and one analysis of impinger catch may be performed. Consult with
the Administrator for details concerning the calculation of results when
two or more trains are used.
At the end of the sample run, turn off the coarse adjust valve,
remove the probe and nozzle from the stack, turn off the pump, record
the final dry gas meter reading, and conduct a post-test leak-check, as
outlined in Section 4.1.4.3. Also, leak-check the pitot lines as
described in Method 2, Section 3.1; the lines must pass this
leak-check, in order to validate the velocity head data.
4.1.6 Calculation of Percent Isokinetic. Calculate percent
isokinetic (see Calculations, Section 6) to determine whether the run
was valid or another test run should be made. If there was difficulty
in maintaining isokinetic rates due to source conditions, consult with
the Administrator for possible variance on the isokinetic rates.
4.2 Sample Recovery. Proper cleanup procedure begins as soon as the
probe is removed from the stack at the end of the sampling period.
Allow the probe to cool.
When the probe can be safely handled, wipe off all external
particulate matter near the tip of the probe nozzle and place a cap over
it to prevent losing or gaining particulate matter. Do not cap off the
probe tip tightly while the sampling train is cooling down as this would
create a vacuum in the filter holder, thus drawing water from the
impingers into the filter holder.
Before moving the sample train to the cleanup site, remove the probe
from the sample train, wipe off the silicone grease, and cap the open
outlet of the probe. Be careful not to lose any condensate that might
be present. Wipe off the silicone grease from the filter inlet where
the probe was fastened and cap it. Remove the umbilical cord from the
last impinger and cap the impinger. If a flexible line is used between
the first impinger or condenser and the filter holder, disconnect the
line at the filter holder and let any condensed water or liquid drain
into the impingers or condenser. After wiping off the silicone grease,
cap off the filter holder outlet and impinger inlet. Either
ground-glass stoppers, plastic caps, or serum caps may be used to close
these openings.
Transfer the probe and filter-impinger assembly to the cleanup area.
This area should be clean and protected from the wind so that the
chances of contaminating or losing the sample will be minimized.
Save a portion of the acetone used for cleanup as a blank. Take 200
ml of this acetone directly from the wash bottle being used and place it
in a glass sample container labeled ''acetone blank.''
Inspect the train prior to and during disassembly and note any
abnormal conditions. Treat the samples as follows:
Container No. 1. Carefully remove the filter from the filter holder
and place it in its identified petri dish container. Use a pair of
tweezers and/or clean disposable surgical gloves to handle the filter.
If it is necessary to fold the filter, do so such that the particulate
cake is inside the fold. Carefully transfer to the petri dish any
particulate matter and/or filter fibers which adhere to the filter
holder gasket, by using a dry Nylon bristle brush and/or a sharp-edged
blade. Seal the container.
Container No. 2. Taking care to see that dust on the outside of the
probe or other exterior surfaces does not get into the sample,
quantitatively recover particulate matter or any condensate from the
probe nozzle, probe fitting, probe liner, and front half of the filter
holder by washing these components with acetone and placing the wash in
a glass container. Distilled water may be used instead of acetone when
approved by the Administrator and shall be used when specified by the
Administrator; in these cases, save a water blank and follow the
Administrator's directions on analysis. Perform the acetone rinses as
follows:
Carefully remove the probe nozzle and clean the inside surface by
rinsing with acetone from a wash bottle and brushing with a Nylon
bristle brush. Brush until the acetone rinse shows no visible
particles, after which make a final rinse of the inside surface with
acetone.
Brush and rinse the inside parts of the Swagelok fitting with acetone
in a similar way until no visible particles remain.
Rinse the probe liner with acetone by tilting and rotating the probe
while squirting acetone into its upper end so that all inside surfaces
will be wetted with acetone. Let the acetone drain from the lower end
into the sample container. A funnel (glass or polyethylene) may be used
to aid on transferring liquid washes to the container. Follow the
acetone rinse with a probe brush. Hold the probe in an inclined
position, squirt acetone into the upper end as the probe brush is being
pushed with a twisting action through the probe; hold a sample
container underneath the lower end of the probe, and catch any acetone
and particulate matter which is brushed from the probe. Run the brush
through the probe three times or more until no visible particulate
matter is carried out with the acetone or until none remains in the
probe liner on visual inspection. With stainless steel or other metal
probes, run the brush through in the above prescribed manner at least
six times since metal probes have small crevices in which particulate
matter can be entrapped. Rinse the brush with acetone, and
quantitatively collect these washings in the sample container. After
the brushing, make a final acetone rinse of the probe as described
above.
It is recommended that two people clean the probe to minimize sample
losses. Between sampling runs, keep brushes clean and protected from
contaminations.
After ensuring that all joints have been wiped clean of silicone
grease, clean the inside of the front half of the filter holder by
rubbing the surfaces with a Nylon bristle brush and rinsing with
acetone. Rinse each surface three times or more if needed to remove
visible particulate. Make a final rinse of the brush and filter holder.
Carefully rinse out the glass cyclone, also (if applicable). After all
acetone washings and particulate matter have been collected in the
sample container, tighten the lid on the sample container so that
acetone will not leak out when it is shipped to the laboratory. Mark
the height of the fluid level to determine whether or not leakage
occured during transport. Label the container to clearly identify its
contents.
Container No. 3. Note the color of the indicating silica gel to
determine if it has been completely spent and make a notation of its
condition. Transfer the silica gel from the fourth impinger to its
original container and seal. A funnel may make it easier to pour the
silica gel without spilling. A rubber policeman may be used as an aid
in removing the silica gel from the impinger. It is not necessary to
remove the small amount of dust particles that may adhere to the
impinger wall and are difficult to remove. Since the gain in weight is
to be used for moisture calculations, do not use any water or other
liquids to transfer the silica gel. If a balance is available in the
field, follow the procedure for container No. 3 in Section 4.3.
Impinger Water. Treat the impingers as follows; Make a notation of
any color or film in the liquid catch. Measure the liquid which is in
the first three impingers to within 1 ml by using a graduated cylinder
or by weighing it to within 0.5 g by using a balance (if one is
available). Record the volume or weight of liquid present. This
information is required to calculate the moisture content of the
effluent gas.
Discard the liquid after measuring and recording the volume or
weight, unless analysis of the impinger catch is required (see Note,
Section 2.1.7).
If a different type of condenser is used, measure the amount of
moisture condensed either volumetrically or gravimetrically.
Whenever possible, containers should be shipped in such a way that
they remain upright at all times.
4.3 Analysis. Record the data required on a sheet such as the one
shown in Figure 5-3. Handle each sample container as follows:
Plant
Date
Run No.
Filter No.
Amount liquid lost during transport
Acetone blank volume, ml
Acetone wash volume, ml
Acetone blank concentration, mg/mg (Equation 5-4)
Acetone wash blank, mg (Equation 5-5)
Container No. 1. Leave the contents in the shipping container or
transfer the filter and any loose particulate from the sample container
to a tared glass weighing dish. Desiccate for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh to a constant weight and
report the results to the nearest 0.1 mg. For purposes of this Section,
4.3, the term ''constant weight'' means a difference of no more than 0.5
mg or 1 percent of total weight less tare weight, whichever is greater,
between two consecutive weighings, with no less than 6 hours of
desiccation time between weighings.
Alternatively, the sample may be oven dried at 105 C (220 F) for 2
to 3 hours, cooled in the desiccator, and weighed to a constant weight,
unless otherwise specified by the Administrator. The tester may also
opt to oven dry the sample at 105 C (220 F) for 2 to 3 hours, weigh
the sample, and use this weight as a final weight.
Container No. 2. Note the level of liquid in the container and
confirm on the analysis sheet whether or not leakage occurred during
transport. If a noticeable amount of leakage has occurred, either void
the sample or use methods, subject to the approval of the Administrator,
to correct the final results. Measure the liquid in this container
either volumetrically to 1 ml or gravimetrically to 0.5 g. Transfer
the contents to a tared 250-ml beaker and evaporate to dryness at
ambient temperature and pressure. Desiccate for 24 hours and weigh to a
constant weight. Report the results to the nearest 0.1 mg.
Container No. 3. Weigh the spent silica gel (or silica gel plus
impinger) to the nearest 0.5 g using a balance. This step may be
conducted in the field.
''Acetone Blank'' Container. Measure acetone in this container
either volumetrically or gravimetrically. Transfer the acetone to a
tared 250-ml beaker and evaporate to dryness at ambient temperature and
pressure. Desiccate for 24 hours and weigh to a constant weight.
Report the results to the nearest 0.1 mg.
Note: At the option of the tester, the contents of Container No. 2
as well as the acetone blank container may be evaporated at temperatures
higher than ambient. If evaporation is done at an elevated temperature,
the temperature must be below the boiling point of the solvent; also,
to prevent ''bumping,'' the evaporation process must be closely
supervised, and the contents of the beaker must be swirled occasionally
to maintain an even temperature. Use extreme care, as acetone is highly
flammable and has a low flash point.
4.4 Quality Control Procedures. The following quality control
procedures are suggested to check the volume metering system calibration
values at the field test site prior to sample collection. These
procedures are optional for the tester.
4.4.1 Meter Orifice Check. Using the calibration data obtained
during the calibration procedure described in Section 5.3, determine the
DH@ for the metering system orifice. The DH@ is the orifice pressure
differential in units of in. H2O that correlates to 0.75 cfm of air at
528 R and 29.92 in. Hg. The DH@ is calculated as follows:
Eq. 5-9
Where:
DH=Average pressure differential across the orifice meter, in. H2O.
Tm=Absolute average dry gas meter temperature, R.
Pbar=Barometric pressure, in. Hg.
U=Total sampling time, min.
Y=Dry gas meter calibration factor, dimensionless.
Vm=Volume of gas sample as measured by dry gas meter, dcf.
0.0319=(0.0567 in. Hg/ R) x (0.75 cfm)2.
Before beginning the field test (a set of three runs usually
constitutes a field test), operate the metering system (i.e., pump,
volume meter, and orifice) at the DH@ pressure differential for 10
minutes. Record the volume collected, the dry gas meter temperature,
and the barometric pressure. Calculate a dry gas meter calibration
check value, Yc, as follows:
Eq. 5-10
Where:
Yc=Dry gas meter calibration check value, dimensionless.
10=10 minutes of run time.
Compare the Yc value with the dry gas meter calibration factor Y to
determine that:
If the Yc value is not within this range, the volume metering system
should be investigated before beginning the test.
4.4.2 Calibrated Critical Orifice. A calibrated critical orifice,
calibrated against a wet test meter or spirometer and designed to be
inserted at the inlet of the sampling meter box may be used as a quality
control check by following the procedure of Section 7.2.
5. Calibration
Maintain a laboratory log of all calibrations.
5.1 Probe Nozzle. Probe nozzles shall be calibrated before their
initial use in the field. Using a micrometer, measure the inside
diameter of the nozzle to the nearest 0.025 mm (0.001 in.). Make three
separate measurements using different diameters each time, and obtain
the average of the measurements. The difference between the high and
low numbers shall not exceed 0.1 mm (0.004 in.). When nozzles become
nicked, dented, or corroded, they shall be reshaped, sharpened, and
recalibrated before use. Each nozzle shall be permanently and uniquely
identified.
5.2 Pitot Tube. The Type S pitot tube assembly shall be calibrated
according to the procedure outlined in Section 4 of Method 2.
5.3 Metering System.
5.3.1 Calibration Prior to Use. Before its initial use in the field,
the metering system shall be calibrated as follows: Connect the
metering system inlet to the outlet of a wet test meter that is accurate
to within 1 percent. Refer to Figure 5.5. The wet test meter should
have a capacity of 30 liters/rev (1 ft /3/ /rev). A spirometer of 400
liters (14 ft /3/ ) or more capacity, or equivalent, may be used for
this calibration, although a wet test meter is usually more practical.
The wet test meter should be periodically calibrated with a spirometer
or a liquid displacement meter to ensure the accuracy of the wet test
meter. Spirometers or wet test meters of other sizes may be used,
provided that the specified accuracies of the procedure are maintained.
Run the metering system pump for about 15 minutes with the orifice
manometer indicating a median reading as expected in field use to allow
the pump to warm up and to permit the interior surface of the wet test
meter to be thoroughly wetted. Then, at each of a minimum of three
orifice manometer settings, pass an exact quantity of gas through the
wet test meter and note the gas volume indicated by the dry gas meter.
Also note the barometric pressure, and the temperatures of the wet test
meter, the inlet of the dry gas meter, and the outlet of the dry gas
meter. Select the highest and lowest orifice settings to bracket the
expected field operating range of the orifice. Use a minimum volume of
0.15 m /3/ (5 cf) at all orifice settings. Record all the data on a
form similar to Figure 5.6, and calculate Y, the dry gas meter
calibration factor, and DH@, the orifice calibration factor, at each
orifice setting as shown on Figure 5.6. Allowable tolerances for
individual Y and DH@, values are given in Figure 5.6. Use the average of
the Y values in the calculations in Section 6.
insert illus 0132A
insert illus 008
Before calibrating the metering system, it is suggested that a
leak-check be conducted. For metering systems having diaphragm pumps,
the normal leak-check procedure will not detect leakages within the
pump. For these cases the following leak-check procedure is suggested:
make a 10-minute calibration run at 0.00057m /3/ /min (0.02 cfm); at
the end of the run, take the difference of the measured wet test meter
and dry gas meter volumes; divide the difference by 10, to get the leak
rate. The leak rate should not exceed 0.00057 m /3/ /min (0.02 cfm).
5.3.2 Calibration After Use. After each field use, the calibration
of the metering system shall be checked by performing three calibration
runs at a single, intermediate orifice setting (based on the previous
field test), with the vacuum set at the maximum value reached during the
test series. To adjust the vacuum, insert a valve between the wet test
meter and the inlet of the metering system. Calculate the average value
of the dry gas meter calibration factor. If the value has changed by
more than 5 percent, recalibrate the meter over the full range of
orifice settings, as previously detailed.
Alternative procedures, e.g., rechecking the orifice meter
coefficient may be used, subject to the approval of the Administrator.
5.3.3 Acceptable Variation in Calibration. If the dry gas meter
coefficient values obtained before and after a test series differ by
more than 5 percent, the test series shall either be voided, or
calculations for the test series shall be performed using whichever
meter coefficient value (i.e., before or after) gives the lower value of
total sample volume.
5.4 Probe Heater Calibration. The probe heating system shall be
calibrated before its initial use in the field.
Use a heat source to generate air heated to selected temperatures
that approximate those expected to occur in the sources to be sampled.
Pass this air through the probe at a typical simple flow rate while
measuring the probe inlet and outlet temperatures at various probe
heater settings. For each air temperature generated, construct a graph
of probe heating system setting versus probe outlet temperature. The
procedure outlined in APTD-0576 can also be used. Probes constructed
according to APTD-0581 need not be calibrated if the calibration curves
in APTD-0576 are used. Also, probes with outlet temperature monitoring
capabilities do not require calibration.
5.5 Temperature Gauges. Use the procedure in Section 4.3 of Method 2
to calibrate in-stack temperature gauges. Dial thermometers, such as
are used for the dry gas meter and condenser outlet, shall be calibrated
against mercury-in-glass thermometers.
5.6 Leak Check of Metering System Shown in Figure 5-1. That portion
of the sampling train from the pump to the orifice meter should be leak
checked prior to initial use and after each shipment. Leakage after the
pump will result in less volume being recorded than is actually sampled.
The following procedure is suggested (see Figure 5-4): Close the main
valve on the meter box. Insert a one-hole rubber stopper with rubber
tubing atached into the orifice exhaust pipe. Disconnect and vent the
low side of the orifice manometer. Close off the low side orifice tap.
Pressurize the system to 13 to 18 cm (5 to 7 in.) water column by
blowing into the rubber tubing. Pinch off the tubing and observe the
manometer for one minute. A loss of pressure on the manometer indicates
a leak in the meter box; leaks, if present, must be corrected.
5.7 Barometer. Calibrate against a mercury barometer.
6. Calculations
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after the final
calculation. Other forms of the equations may be used as long as they
give equivalent results.
Insert illus. 238
6.1 Nomenclature.
An=Cross-sectional area of nozzle, m2 (ft2).
Bws=Water vapor in the gas stream, proportion by volume.
Ca=Acetone blank residue concentration, mg/mg.
cs=Concentration of particulate matter in stack gas, dry basis,
corrected to standard conditions, g/dscm (g/dscf).
I=Percent of isokinetic sampling.
La=Maximum acceptable leakage rate for either a pretest leak check or
for a leak check following a component change; equal to 0.00057 m3/min
(0.02 cfm) or 4 percent of the average sampling rate, whichever is less.
Li=Individual leakage rate observed during the leak check conducted
prior to the ''ith'' component change (i=1, 2, 3....n), m3/min (cfm).
Lp=Leakage rate observed during the post-test leak check, m3/min
(cfm).
ma=Mass of residue of acetone after evaporation, mg.
mn=Total amount of particulate matter collected, mg.
Mw=Molecular weight of water, 18.0 g/g-mole (18.0lb/lb-mole).
Pbar=Barometric pressure at the sampling site, mm Hg (in. Hg).
Ps=Absolute stack gas pressure, mm Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
R=Ideal gas constant, 0.06236 mm Hg-m3/ K-g-mole (21.85 in. Hg-ft3/
R-lb-mole).
Tm=Absolute average dry gas meter temperature (see Figure 5-2), K (
R).
Ts=Absolute average stack gas temperature (see Figure 5-2), K ( R).
Tstd=Standard absolute temperature, 293 K (528 R).
Va=Volume of acetone blank, ml.
Vaw=Volume of acetone used in wash, ml.
Vlc=Total volume of liquid collected in impingers and silica gel (see
Figure 5-3), ml.
Vm=Volume of gas sample as measured by dry gas meter, dcm (dscf).
Vm(std)=Volume of gas sample measured by the dry gas meter, corrected
to standard conditions, dscm (dscf).
Vw(std)=Volume of water vapor in the gas sample, corrected to
standard conditions, scm (scf).
vs=Stack gas velocity, calculated by Method 2, Equation 2-9, using
data obtained from Method 5, m/sec (ft/sec).
Wa=Weight of residue in acetone wash, mg.
Y=Dry gas meter calibration factor.
H=Average pressure differential across the orifice meter (see Figure
5-2), mm H2O (in. H2O).
a=Density of acetone, mg/ml (see label on bottle).
w=Density of water, 0.9982 g/ml (0.002201 lb/ml).
=Total sampling time, min.
1=Sampling time interval, from the beginning of a run until the
first component change, min.
i=Sampling time interval, between two successive component changes,
beginning with the interval between the first and second changes, min.
p=Sampling time interval, from the final (nth) component change
until the end of the sampling run, min.
13.6=Specific gravity of mercury.
60=Sec/min.
100=Conversion to percent.
6.2 Average Dry Gas Meter Temperature and Average Orifice Pressure
Drop. See data sheet (Figure 5-2).
6.3 Dry Gas Volume. Correct the sample volume measured by the dry
gas meter to standard conditions (20 C, 760 mm Hg or 68 F, 29.92 in.
Hg) by using Equation 5-1.
Insert illus. 239
Where;
K1=0.3858 K/mm Hg for metric units
=17.64 R/in. Hg for English units
Note: Equation 5-1 can be used as written unless the leakage rate
observed during any of the mandatory leak checks (i.e., the post-test
leak check or leak checks conducted prior to component changes) exceeds
La. If Lp or i exceeds La, Equation 5-1 must be modified as follows:
(a) Case I. No component changes made during sampling run. In this
case, replace Vm in Equation 5-1 with the expression:
(b) Case II. One or more component changes made during the sampling
run. In this case, replace Vm in Equation 5-1 by the expression:
Insert illus. 241
and substitute only for those leakage rates (Li or Lp) which exceed
La.
6.4 Volume of Water Vapor.
Insert illus. 242
Where:
K2=0.001333 m3/ml for metric units
=0.04707 ft3/ml for English units.
6.5 Moisture Content.
Eq. 5-3
Note: In saturated or water droplet-laden gas streams, two
calculations of the moisture content of the stack gas shall be made, one
from the impinger analysis (Equation 5-3), and a second from the
assumption of saturated conditions. The lower of the two values of Bws
shall be considered correct. The procedure for determining the moisture
content based upon assumption of saturated conditions is given in the
Note of Section 1.2 of Method 4. For the purposes of this method, the
average stack gas temperature from Figure 5-2 may be used to make this
determination, provided that the accuracy of the in-stack temperature
sensor is 1 C (2 F).
6.6 Acetone Blank Concentration.
6.7 Acetone Wash Blank.
6.8 Total Particulate Weight. Determine the total particulate catch
from the sum of the weights obtained from Containers 1 and 2 less the
acetone blank (see Figure 5-3).
Note: Refer to Section 4.1.5 to assist in calculation of results
involving two or more filter assemblies or two or more sampling trains.
6.9 Particulate Concentration.
Eq. 5-6
6.10 Conversion Factors:
6.11 Isokinetic Variation.
6.11.1 Calculation From Raw Data.
Eq. 5-7
Where:
K3=0.003454 mm Hg^m3/ml^ K for metric units.
=0.002669-in. Hg^ft3/ml^ R for English units.
6.11.2 Calculation From Intermediate Values.
Insert illus. 247
Where:
K4=4.320 for metric units
=0.09450 for English units.
6.12 Acceptable Results. If 90 percent I 110 percent, the
results are acceptable. If the particulate results are low in
comparison to the standard, and I is over 110 percent or less than 90
percent, the Administrator may accept the results. Citation 4 in the
bibliography section can be used to make acceptability judgments. If I
is judged to be unacceptable, reject the particulate results and repeat
the test.
6.13 Stack Gas Velocity and Volumetric Flow Rate. Calculate the
average stack gas velocity and volumetric flow rate, if needed, using
data obtained in this method and the equations in Sections 5.2 and 5.3
of Method 2.
7. Alternative Procedures
7.1 Dry Gas Meter as a Calibration Standard. A dry gas meter may be
used as a calibration standard for volume measurements in place of the
wet test meter specified in Section 5.3, provided that it is calibrated
initially and recalibrated periodically as follows:
7.1.1 Standard Dry Gas Meter Calibration.
7.1.1.1 The dry gas meter to be calibrated and used as a secondary
reference meter should be of high quality and have an appropriately
sized capacity, e.g., 3 liters/rev (0.1 ft /3/ /rev). A spirometer (400
liters or more capacity), or equivalent, may be used for this
calibration, although a wet test meter is usually more practical. The
wet test meter should have a capacity of 30 liters/rev (1 ft /3/
/rev) and capable of measuring volume to within 1.0 percent; wet
test meters should be checked against a spirometer or a liquid
displacement meter to ensure the accuracy of the wet test meter.
Spirometers or wet test meters of other sizes may be used, provided that
the specified accuracies of the procedure are maintained.
7.1.1.2 Set up the components as shown in Figure 5.7. A spirometer,
or equivalent, may be used in place of the wet test meter in the system.
Run the pump for at least 5 minutes at a flow rate of about 10
liters/min (0.35 cfm) to condition the interior surface of the wet test
meter. The pressure drop indicated by the manometer at the inlet side
of the dry gas meter should be minimized (no greater than 100 mm H2O (4
in. H2O) at a flow rate of 30 liters/min (1 cfm)). This can be
accomplished by using large diameter tubing connections and straight
pipe fittings.
Insert illus. 0849
7.1.1.3 Collect the data as shown in the example data sheet (see
Figure 5-8). Make triplicate runs at each of the flow rates and at no
less than five different flow rates. The range of flow rates should be
between 10 and 34 liters/min (0.35 and 1.2 cfm) or over the expected
operating range.
Insert illus. 0850
7.1.1.4 Calculate flow rate, Q, for each run using the wet test meter
gas volume, Vw, and the run time, u. Calculate the dry gas meter
coefficient, Yds, for each run. These calculations are as follows:
Where:
Kl=0.3858 for international system of units (SI); 17.64 for English
units.
Vw=Wet test meter volume, liters (ft3).
Vds=Dry gas meter volume, liters (ft3).
tds=Average dry gas meter temperature, C ( F).
tstd=273 C for SI units; 460 F for English units.
tw=Average wet test meter temperature, C ( F).
Pbar=Barometric pressure, mm Hg (in. Hg).
Dp=Dry gas meter inlet differential pressure, mm H2O (in. H2O).
u=Run time, min.
7.1.1.5 Compare the three Yds values at each of the flow rates and
determine the maximum and minimum values. The difference between the
maximum and minimum values at each flow rate should be no greater than
0.030. Extra sets of triplicate runs may be made in order to complete
this requirement. In addition, the meter coefficients should be between
0.95 and 1.05. If these specifications cannot be met in three sets of
successive triplicate runs, the meter is not suitable as a calibration
standard and should not be used as such. If these specifications are
met, average the three Yds values at each flow rate resulting in five
average meter coefficients, Yds.
7.1.1.6 Prepare a curve of meter coefficient, Yds, versus flow rate,
Q, for the dry gas meter. This curve shall be used as a reference when
the meter is used to calibrate other dry gas meters and to determine
whether recalibration is required.
7.1.2 Standard Dry Gas Meter Recalibration.
7.1.2.1 Recalibrate the standard dry gas meter against a wet test
meter or spirometer annually or after every 200 hours of operation,
whichever comes first. This requirement is valid provided the standard
dry gas meter is kept in a laboratory and, if transported, cared for as
any other laboratory instrument. Abuse to the standard meter may cause
a change in the calibration and will require more frequent
recalibrations.
7.1.2.2 As an alternative to full recalibration, a two-point
calibration check may be made. Follow the same procedure and equipment
arrangement as for a full recalibration, but run the meter at only two
flow rates (suggested rates are 14 and 28 liters/min (0.5 and 1.0 cfm)).
Calculate the meter coefficients for these two points, and compare the
values with the meter calibration curve. If the two coefficients are
within 1.5 percent of the calibration curve values at the same flow
rates, the meter need not be recalibrated until the next date for a
recalibration check.
7.2 Critical Orifices As Calibration Standards. Critical orifices
may be used as calibration standards in place of the wet test meter
specified in Section 5.3, provided that they are selected, calibrated,
and used as follows:
7.2.1 Section of Critical Orifices.
7.2.1.1 The procedure that follows describes the use of hypodermic
needles or stainless steel needle tubings which have been found suitable
for use as critical orifices. Other materials and critical orifice
designs may be used provided the orifices act as true critical orifices;
i.e., a critical vacuum can be obtained, as described in Section
7.2.2.2.3. Select five critical orifices that are appropriately sized to
cover the range of flow rates between 10 and 34 liters/min or the
expected operating range. Two of the critical orifices should bracket
the expected operating range.
A minimum of three critical orifices will be needed to calibrate a
Method 5 dry gas meter (DGM); the other two critical orifices can serve
as spares and provide better selection for bracketing the range of
operating flow rates. The needle sizes and tubing lengths shown below
give the following approximate flow rates:
7.2.1.2 These needles can be adapted to a Method 5 type sampling
train as follows: Insert a serum bottle stopper, 13- by 20-mm sleeve
type, into a 1/2-inch Swagelok quick connect. Insert the needle into
the stopper as shown in Figure 5-9.
Insert Illustration 0 620
7.2.2 Critical Orifice Calibration. The procedure described in this
section uses the Method 5 meter box configuration with a DGM as
described in Section 2.1.8 to calibrate the critical orifices. Other
schemes may be used, subject to the approval of the Administrator.
7.2.2.1 Calibration of Meter Box. The critical orifices must be
calibrated in the same configuration as they will be used; i.e., there
should be no connections to the inlet of the orifice.
7.2.2.1.1 Before calibrating the meter box, leak check the system as
follows: Fully open the coarse adjust valve, and completely close the
by-pass valve. Plug the inlet. Then trun on the pump, and determine
whether there is any leakage. The leakage rate shall be zero; i.e., no
detectable movement of the DGM dial shall be seen for 1 minute.
7.2.2.1.2 Check also for leakages in that portion of the sampling
train between the pump and the orifice meter. See Section 5.6 for the
procedure; make any corrections, if necessary. If leakage is detected,
check for cracked gaskets, loose fittings, worn O-rings, etc., and make
the necessary repairs.
7.2.2.1.3 After determining that the meter box is leakless, calibrate
the meter box according to the procedure given in Section 5.3. Make sure
that the wet test meter meets the requirements stated in Section
7.1.1.1. Check the water level in the wet test meter. Record the DGM
calibration factor, Y.
7.2.2.2 Calibration of Critical Orifices. Set up the apparatus as
shown in Figure 5-10.
Insert Illustration 0 622
7.2.2.2.1 Allow a warm-up time of 15 minutes. This step is important
to equilibrate the temperature conditions through the DGM.
7.2.2.2.2 Leak check the system as in Section 7.2.2.1.1. The leakage
rate shall be zero.
7.2.2.2.3 Before calibrating the critical orifice, determine its
suitability and the appropriate operating vacuum as follows: Turn on
the pump, fully open the coarse adjust valve, and adjust the by-pass
valve to give a vacuum reading corresponding to about half of
atmospheric pressure. Observe the meter box orifice manometer reading,
H. Slowly increase the vacuum reading until a stable reading is
obtained on the meter box orifice manometer. Record the critical vacuum
for each orifice.
Orifices that do not reach a critical value shall not be used.
7.2.2.2.4 Obtain the barometric pressure using a barometer as
described in Section 2.1.9. Record the barometric pressure, Pbar, in mm
Hg (in. Hg).
7.2.2.2.5 Conduct duplicate runs at a vacuum of 25 to 50 mm Hg (1 to
2 in. Hg) above the critical vacuum. The runs shall be at least 5
minutes each. The DGM volume readings shall be in increments of 0.00283
m3 (0.1 ft3) or in increments of complete revolutions of the DGM. As a
guideline, the times should not differ by more than 3.0 seconds (this
includes allowance for changes in the DGM temperatures) to achieve 0.5
percent in K . Record the information listed in Figure 5-11.
7.2.2.2.6 Calculate K using Equation 5-9.
Where:
Tamb=Absolute ambient temperature, K ( R).
Average the K values. The individual K values should not differ by
more than 0.5 percent from the average.
7.2.3 Using the Critical Orifices as Calibration Standards.
7.2.3.1 Record the barometric pressure.
Date XXXX Train ID XXXX DGM cal. factor XXXX Critical orifice ID
XXXX
Figure 5-11. Data sheet for determining K' factor.
7.2.3.2 Calibrate the metering system according to the procedure
outlined in Sections 7.2.2.2.1 to 7.2.2.2.5. Record the information
listed in Figure 5.12.
7.2.3.3 Calculate the standard volumes of air passed through the DGM
and the critical orifices, and calculate the DGM calibration factor, Y,
using the equations below:
Eq. 5-10
where:
Vcr(std)=Volume of gas sample passed through the critical orifice,
corrected to standard conditions, dsm3 (dscf).
K1=0.3858 K/mm Hg for metric units
=17.64 R/in. Hg for English units.
7.2.3.4 Average the DGM calibration values for each of the flow
rates. The calibration factor, Y, at each of the flow rates should not
differ by more than 2 percent from the average.
7.2.3.5 To determine the need for recalibrating the critical
orifices, compare the DGM Y factors obtained from two adjacent orifices
each time a DGM is calibrated; for example, when checking 13/2.5, use
orifices 12/10.2 and 13/5.1. If any critical orifice yields a DGM Y
factor differing by more than 2 percent from the others, recalibrate the
critical orifice according to Section 7.2.2.2.
Date XXXX Train ID XXXX Critical orifice ID XXXX Critical orifice K'
factor XXXX
Figure 5-12. Data sheet for determining DGM Y factor.
8. Bibliography
1. Addendum to Specifications for Incinerator Testing at Federal
Facilities. PHS, NCAPC. Dec. 6, 1967.
2. Martin, Robert M. Construction Details of Isokinetic
Source-Sampling Equipment. Environmental Protection Agency. Research
Triangle Park, NC. APTD-0581. April 1971.
3. Rom, Jerome J. Maintenance, Calibration, and Operation of
Isokinetic Source Sampling Equipment. Environmental Protection Agency.
Research Triangle Park, NC. APTD-0576. March, 1972.
4. Smith, W. S., R. T. Shigehara, and W. F. Todd. A Method of
Interpreting Stack Sampling Data. Paper Presented at the 63d Annual
Meeting of the Air Pollution Control Association, St. Louis, MO, June
14-19, 1970.
5. Smith, W. S., et al. Stack Gas Sampling Improved and Simplified
With New Equipment. APCA Paper No. 67-119. 1967.
6. Specifications for Incinerator Testing at Federal Facilities.
PHS, NCAPC. 1967.
7. Shigehara, R. T. Adjustments in the EPA Nomograph for Different
Pitot Tube Coefficients and Dry Molecular Weights. Stack Sampling News
2:4-11, October, 1974.
8. Vollaro, R. F. A Survey of Commercially Available Instrumentation
For the Measurement of Low-Range Gas Velocities. U.S. Environmental
Protection Agency, Emission Measurement Branch. Research Triangle Park,
NC. November, 1976 (unpublished paper).
9. Annual Book of ASTM Standards. Part 26. Gaseous Fuels; Coal and
Coke; Atmospheric Analysis. American Society for Testing and
Materials. Philadelphia, PA. 1974. pp. 617-622.
10. Felix, L. G., G. I. Clinard, G. E. Lacey, and J. D. McCain.
Inertial Cascade Impactor Substrate Media for Flue Gas Sampling. U.S.
Environmental Protection Agency. Research Triangle Park, NC 27711,
Publication No. EPA-600/7-77-060. June 1977. 83 p.
11. Westlin, P. R. and R. T. Shigehara. Procedure for Calibrating
and Using Dry Gas Volume Meters as Calibration Standards. Source
Evaluation Society Newsletter. 3(1):17-30. February 1978.
12. Lodge, J.P., Jr., J.B. Pate, B.E. Ammons, and G.A. Swanson. The
Use of Hypodermic Needles as Critical Orifices in Air Sampling. J. Air
Pollution Control Association. 16:197-200. 1966.
2Mention of trade names or specific product does not constitute
endorsement by the Environmental Protection Agency.
40 CFR 60.748 Pt. 60, App. A, Meth. 5A
1. Applicability and Principle
1.1 Applicability. This method applies to the determination of
particulate emissions from asphalt roofing industry process saturators,
blowing stills, and other sources as specified in the regulations.
1.2 Principle. Particulate matter is withdrawn isokinetically from
the source and collected on a glass filter fiber maintained at a
temperature of 42 10 C (108 18 F). The particulate mass, which
includes any material that condenses at or above the filtration
temperature, is determined gravimetrically after removal of uncombined
water.
2. Apparatus
2.1 Sampling Train. The sampling train configuration is the same as
shown in Figure 5-1 of Method 5. The sampling train consists of the
following components:
2.1.1 Probe Nozzle, Pitot Tube, Differential Pressure Gauge, Filter
Holder, Condenser, Metering System, Barometer, and Gas Density
Determination Equipment. Same as Method 5, Sections 2.1.1, 2.1.3 to
2.1.5, and 2.1.7 to 2.1.10, respectively.
2.1.2 Probe Liner. Same as in Method 5, Section 2.1.2, with the note
that at high stack gas temperatures (greater than 250 C (480 F)),
water-cooled probes may be required to control the probe exit
temperature to 42 10 C (108 18 F).
2.1.3 Precollector Cyclone. Borosilicate glass following the
construction details shown in Air Pollution Technical Document-0581,
''Construction Details of Isokinetic Source-Sampling Equipment''.
Note: The tester shall use the cyclone when the stack gas moisture
is greater than 10 percent. The tester shall not use the precollector
cyclone under other, less severe conditions.
2.1.4 Filter Heating System. Any heating (or cooling) system capable
of maintaining a sample gas temperature at the exit end of the filter
holder during sampling at 42 10 C (108 18 F). Install a temperature
gauge capable of measuring temperature within 3 C (5.4 F) at the exit
side of the filter holder so that the sensing tip of the temperature
gauge is in direct contact with the sample gas, and the sample gas
temperature can be regulated and monitored during sampling. The
temperature gauge shall comply with the calibration specifications
defined in Section 5. The tester may use systems other than the one
shown in APTD-0581.
2.2 Sample Recovery. The equipment required for sample recovery is
as follows:
2.2.1 Probe-Liner and Probe-Nozzle Brushes, Graduated Cylinder and/or
Balance, Plastic Storage Containers, and Funnel and Rubber Policeman.
Same as Method 5, Sections 2.2.1, 2.2.5, 2.2.6, and 2.2.7, respectively.
2.2.2 Wash Bottles. Glass.
2.2.3 Sample Storage Containers. Chemically resistant, borosilicate
glass bottles, with rubber-backed Teflon screw cap liners or caps that
are constructed so as to be leak-free and resistant to chemical attack
by 1,1,1-trichloroethane (TCE), 500-ml or 1000-ml. (Narrow mouth glass
bottles have been found to be less prone to leakage.)
2.2.4 Petri Dishes. Glass, unless otherwise specified by the
Administrator.
2.2.5 Funnel. Glass.
2.3 Analysis. For analysis, the following equipment is needed:
2.3.1 Glass Weighing Dishes, Desiccator, Analytical Balance, Balance,
Hygrometer, and Temperature Gauge. Same as Method 5, Sections 2.3.1 to
2.3.4, 2.3.6, and 2.3.7, respectively.
2.3.2 Beakers. Glass, 250-ml and 500-ml.
2.3.3 Separatory Funnel. 100-ml or greater.
3. Reagents
3.1 Sampling. The reagents used in sampling are as follows:
3.1.1. Filters, Silica Gel, and Crushed Ice. Same as Method 5,
Sections 3.1.1, 3.1.2, and 3.1.4, respectively.
3.1.2 Stopcock Grease. TCE-insoluble, heat-stable grease (if
needed). This is not necessary if screw-on connectors with Teflon
sleeves, or similar, are used.
3.2 Sample Recovery. Reagent grade 1,1,1-trichloroethane (TCE), :
0.001 percent residue and stored in glass bottles, is required. Run TCE
blanks prior to field use and use only TCE with low blank values (:
0.001 percent). The tester shall in no case subtract a blank value of
greater than 0.001 percent of the weight of TCE used from the sample
weight.
3.3 Analysis. Two reagents are required for the analysis:
3.3.1 TCE. Same as 3.2.
3.3.2 Desiccant. Same as Method 5, Section 3.3.2.
4. Procedure
4.1 Sampling Train Operation. The complexity of this method is such
that in order to obtain reliable results, testers should be trained and
experienced with Method 5 test procedures.
4.1.1 Pretest Preparation. Unless otherwise specified, maintain and
calibrate all components according to the procedure described in Air
Pollution Technical Document-0576, ''Maintenance, Calibration, and
Operation of Isokinetic Source-Sampling Equipment''.
Prepare probe liners and sampling nozzles as needed for use.
Thoroughly clean each component with soap and water followed by a
minimum of three TCE rinses. Use the probe and nozzle brushes during at
least one of the TCE rinses (refer to Section 4.2 for rinsing
techniques). Cap or seal the open ends of the probe liners and nozzles
to prevent contamination during shipping.
Prepare silica gel portions and glass filters as specified in Method
5, Section 4.1.1.
4.1.2 Preliminary Determinations. Select the sampling site, probe
nozzle, and probe length as specified in Method 5, Section 4.1.2.
Select a total sampling time greater than or equal to the minimum
total sampling time specified in the test procedures section of the
applicable regulation. Follow the guidelines outlined in Method 5,
Section 4.1.2, for sampling time per point and total sample volume
collected.
4.1.3 Preparation of Collection Train. Prepare the collection train
as specified in Method 5, Section 4.1.3, with the addition of the
following:
Set up the sampling train as shown in Figure 5-1 of Method 5 with the
addition of the precollector cyclone, if used, between the probe and
filter holder. The temperature of the precollector cyclone, if used,
should be about the same as for the filter, i.e., 42 10 C (108 18 F).
Use no stopcock grease on ground glass joints unless the grease is
insoluble in TCE.
4.1.4 Leak Check Procedures. Follow the procedures given in Method
5, Sections 4.1.4.1 (Pretest Leak Check), 4.1.4.2 (Leak Check During
Sample Run), and 4.1.4.3 (Post-Test Leak Check).
4.1.5 Particulate Train Operation. Operate the sampling train as
described in Method 5, Section 4.1.5, except maintain the gas
temperature exiting the filter at 42 10 C (108 18 F).
4.1.6 Calculation of Percent Isokinetic. Same as in Method 5,
Section 4.1.6.
4.2 Sample Recovery. Using the procedures and techniques described
in Method 5, Section 4.2, quantitatively recover any particulate matter
into the following containers (additions and deviations to the stated
procedures are as noted):
4.2.1 Container No. 1 (Filter). Same instructions as Method 5,
Section 4.2, ''Container No. 1.'' If it is necessary to fold the
filter, do so such that the film of oil is inside the fold.
4.2.2 Container No. 2 (Probe to Filter Holder). Taking care to see
that material on the outside of the probe or other exterior surfaces
does not get into the sample, quantitatively recover particulate matter
or any condensate from the probe nozzle, probe fitting, probe liner,
precollector cyclone and collector flask (if used), and front half of
the filter holder by washing these components with TCE and placing the
wash in a glass container. Carefully measure the total amount of TCE
used in the rinses. Perform the TCE rinses as described in Method 5,
Section 4.2, ''Container No. 2,'' using TCE instead of acetone.
Brush and rinse the inside of the cyclone, cyclone collection flask,
and the front half of the filter holder. Brush and rinse each surface
three times or more, if necessary, to remove visible particulate.
4.2.3 Container No. 3 (Silica Gel). Same procedure as in Method 5,
Section 4.2, ''Container No. 3.''
4.2.4 Impinger Water. Treat the impingers as follows: Make a
notation of any color or film in the liquid catch. Follow the same
procedure as in Method 5, Section 4.2, ''Impinger Water.''
4.2.5 Blank. Save a portion of the TCE used for cleanup as a blank.
Take 200 ml of this TCE directly from the wash bottle being used and
place it in a glass sample container labeled ''TCE blank.''
4.3 Analysis. Record the data required on a sheet such as the one
shown in Figure 5A-1. Handle each sample container as follows:
4.3.1 Container No. 1 (Filter). Transfer the filter from the sample
container to a tared glass weighing dish and desiccate for 24 hours in a
desiccator containing anhydrous calcium sulfate. Rinse Container No. 1
with a measured amount of TCE and analyze this rinse with the contents
of Container No. 2. Weigh the filter to a constant weight. For the
purpose of Section 4.3, the term ''constant weight'' means a difference
of no more than 10 percent or 2 mg (whichever is greater) between two
consecutive weighings made 24 hours apart. Report the ''final weight''
to the nearest 0.1 mg as the average of these two values.
4.3.2 Container No. 2 (Probe to Filter Holder). Before adding the
rinse from Container No. 1 to Container No. 2, note the level of
liquid in the container and confirm on the analysis sheet whether or not
leakage occurred during transport. If noticeable leakage occurred,
either void the sample or take steps, subject to the approval of the
Administrator, to correct the final results.
Measure the liquid in this container either volumetrically to 1 ml
or gravimetrically to 0.5 g. Check to see if there is any appreciable
quantity of condensed water present in the TCE rinse (look for a
boundary layer or phase separation). If the volume of condensed water
appears larger than 5 ml, separate the oil-TCE fraction from the water
fraction using a separatory funnel. Measure the volume of the water
phase to the nearest ml; adjust the stack gas moisture content, if
necessary (see Sections 6.4 and 6.5). Next, extract the water phase with
several 25-ml portions of TCE until, by visual observation, the TCE does
not remove any additional organic material. Evaporate the remaining
water fraction to dryness at 93 C (200 F), desiccate for 24 hours, and
weigh to the nearest 0.1 mg.
Treat the total TCE fraction (including TCE from the filter container
rinse and water phase extractions) as follows: Transfer the TCE and oil
to a tared beaker and evaporate at ambient temperature and pressure.
The evaporation of TCE from the solution may take several days. Do not
desiccate the sample until the solution reaches an apparent constant
volume or until the odor of TCE is not detected. When it appears that
the TCE has evaporated, desiccate the sample and weigh it at 24-hour
intervals to obtain a ''constant weight'' (as defined for Container No.
1 above). The ''total weight'' for Container No. 2 is the sum of the
evaporated particulate weight of the TCE-oil and water phase fractions.
Report the results to the nearest 0.1 mg.
4.3.3 Container No. 3 (Silica Gel). This step may be conducted in
the field. Weigh the spent silica gel (or silica gel plus impinger) to
the nearest 0.5 g using a balance.
4.3.4 ''TCE Blank'' Container. Measure TCE in this container either
volumetrically or gravimetrically. Transfer the TCE to a tared 250-ml
beaker and evaporate to dryness at ambient temperature and pressure.
Desiccate for 24 hours and weigh to a constant weight. Report the
results to the nearest 0.1 mg.
Note: In order to facilitate the evaporation of TCE liquid samples,
these samples may be dried in a controlled temperature oven at
temperatures up to 38 C (100 F) until the liquid is evaporated.
4.4 Quality Control Procedures. A quality control (QC) check of the
volume metering system at the field site is suggested before collecting
the sample. Use the procedure defined in Method 5, Section 4.4.
5. Calibration
Calibrate the sampling train components according to the indicated
sections of Method 5: Probe Nozzle (5.1), Pitot Tube Assembly (5.2),
Metering System (5.3), Probe Heater (5.4), Temperature Gauges (5.5),
Leak Check of Metering System (5.6), and Barometer (5.7).
6. Calculations
6.1 Nomenclature. Same as in Method 5, Section 6.1, with the
following additions:
Ct=TCE blank residue concentration, mg/mg.
mt=Mass of residue of TCE after evaporation, mg.
Vpc=Volume of water collected in precollector, ml.
Vt=Volume of TCE blank, ml.
Vtw=Volume of TCE used in wash, ml.
Wt=Weight of residue in TCE wash, mg.
t=Density of TCE, mg/ml (see label on bottle).
6.2 Dry Gas Meter Temperature and Orifice Pressure Drop. Using the
data obtained in this test, calculate the average dry gas meter
temperature and average orifice pressure drop (see Figure 5-2 of Method
5).
6.3 Dry Gas Volume. Using the data from this test, calculate Vm(std)
by using Equation 5-1 of Method 5. If necessary, adjust the volume for
leakages.
6.4 Volume of Water Vapor.
Eq. 5A-1
Where:
Kl=0.00133 m /3/ /ml for metric units.
=0.04707 ft /3/ /ml for English units.
6.5 Moisture Content.
Eq. 5A-2
Note: In saturated or water droplet-laden gas streams, two
calculations of the moisture content of the stack gas shall be made, one
from the impinger and precollector analysis (Equations 5A-1 and 5A-2)
and a second from the assumption of saturated conditions. The lower of
the two values of moisture content shall be considered correct. The
procedure for determining the moisture content based upon assumption of
saturated conditions is given in the note of Section 1.2 of Method 4.
For the purpose of this method, the average stack gas temperature from
Figure 5-2 of Method 5 may be used to make this determination, provided
that the accuracy of the in-stack temperature sensor is within 1 C (2
F).
6.6 TCE Blank Concentration.
Eq. 5A-3
6.7 TCE Wash Blank.
Eq. 5A-4
6.8 Total Particulate Weight. Determine the total particulate catch
from the sum of the weights obtained from Containers 1, 2, and 3, less
the TCE blank.
6.9 Particulate Concentration.
Eq. 5A-5
Where:
K2=0.001 g/mg.
6.10 Isokinetic Variation and Acceptable Results. Same as in Method
5, Sections 6.11 and 6.12, respectively.
7. Bibliography
The bibliography for Method 5A is the same as that for Method 5.
40 CFR 60.748 Pt. 60, App. A, Meth. 5B
1. Applicability and Principle.
1.1 Applicability. This method is to be used for determining
nonsulfuric acid particulate matter from stationary sources. Use of
this method must be specified by an applicable subpart, or approved by
the Administrator, U.S. Environmental Protection Agency, for a
particular application.
1.2 Principle. Particulate matter is withdrawn isokinetically from
the source using the Method 5 train at 160 C (320 F). The collected
sample is then heated in the oven at 160 C (320 F) for 6 hours to
volatilize any condensed sulfuric acid that may have been collected, and
the nonsulfuric acid particulate mass is determined gravimetrically.
2. Procedure.
The procedure is identical to EPA Method 5 except for the following:
2.1 Initial Filter Tare. Oven dry the filter at 160 5 C (320 10 F)
for 2 to 3 hours, cool in a desiccator for 2 hours, and weigh.
Desiccate to constant weight to obtain the initial tare. Use the
applicable specifications and techniques of Section 4.1.1 of Method 5
for this determination.
2.2 Probe and Filter Temperatures. Maintain the probe outlet and
filter temperatures at 160 14 C (320 25 F).
2.3 Analysis. Dry the probe sample at ambient temperature. Then
oven-dry the probe and filter samples at a temperature of 160 5 C (320
10 F) for 6 hours. Cool in a desiccator for 2 hours, and weigh to
constant weight. Use the applicable specifications and techniques of
Section 4.3 of Method 5 for this determination.
40 CFR 60.748 Pt. 60, App. A, Meth. 5D
1. Applicability and Principle
1.1 Applicability. This method applies to the determination of
particulate matter emissions from positive pressure fabric filters.
Emissions are determined in terms of concentration (mg/m /3/ ) and
emission rate (kg/h).
The General Provisions of 40 CFR Part 60, 60.8(e), require that the
owner or operator of an affected facility shall provide performance
testing facilities. Such performance testing facilities include
sampling ports, safe sampling platforms, safe access to sampling sites,
and utilities for testing. It is intended that affected facilities also
provide sampling locations that meet the specification for adequate
stack length and minimal flow disturbances as described in Method 1.
Provisions for testing are often overlooked factors in designing fabric
filters or are extremely costly. The purpose of this procedure is to
identify appropriate alternative locations and procedures for sampling
the emissions from positive pressure fabric filters. The requirements
that the affected facility owner or operator provide adequate access to
performance testing facilities remain in effect.
1.2 Principle. Particulate matter is withdrawn isokinetically from
the source and collected on a glass fiber filter maintained at a
temperature at or above the exhaust gas temperature up to a nominal 120
C (120 14 C or 248 25 F). The particulate mass, which includes any
material that condenses at or above the filtration temperature, is
determined gravimetrically after removal of uncombined water.
2. Apparatus
The equipment requirements for the sampling train, sample recovery,
and analysis are the same as specified in Sections 2.1, 2.2, and 2.3,
respectively, of Method 5 or Method 17.
3. Reagents
The reagents used in sampling, sample recovery, and analysis are the
same as specified in Sections 3.1, 3.2, and 3.3, respectively, of Method
5 or Method 17.
4. Procedure
4.1 Determination of Measurement Site. The configurations of
positive pressure fabric filter structures frequently are not amenable
to emission testing according to the requirements of Method 1.
Following are several alternatives for determining measurement sites for
positive pressure fabric filters.
4.1.1 Stacks Meeting Method 1 Criteria. Use a measurement site as
specified in Method 1, Section 2.1.
4.1.2 Short Stacks Not Meeting Method 1 Criteria. Use stack
extensions and the procedures in Method 1. Alternatively, use flow
straightening vanes of the ''egg-crate'' type (see Figure 5D-1). Locate
the measurement site downstream of the straightening vanes at a distance
equal to or greater than two times the average equivalent diameter of
the vane openings and at least one-half of the overall stack diameter
upstream of the stack outlet.
4.1.3 Roof Monitor or Monovent. (See Figure 5D-2.) For a positive
pressure fabric filter equipped with a peaked roof monitor, ridge vent,
or other type of monovent, use a measurement site at the base of the
monovent. Examples of such locations are shown in Figure 5D-2. The
measurement site must be upstream of any exhaust point (e.g., louvered
vent).
4.1.4 Compartment Housing. Sample immediately downstream of the
filter bags directly above the tops of the bags as shown in the examples
in Figure 5D-2. Depending on the housing design, use sampling ports in
the housing walls or locate the sampling equipment within the
compartment housing.
4.2 Determination of Number and Location of Traverse Points. Locate
the traverse points according to Method 1, Section 2.3. Because a
performance test consists of at least three test runs and because of the
varied configurations of positive pressure fabric filters, there are
several schemes by which the number of traverse points can be determined
and the three test runs can be conducted.
4.2.1 Single Stacks Meeting Method 1 Criteria. Select the number of
traverse points according to Method 1. Sample all traverse points for
each test run.
4.2.2 Other Single Measurement Sites. For a roof monitor or
monovent, single compartment housing, or other stack not meeting Method
1 criteria, use at least 24 traverse points. For example, for a
rectangular measurement site, such as a monovent, use a balanced 5 x 5
traverse point matrix. Sample all traverse points for each test run.
4.2.3 Multiple Measurement Sites. Sampling from two or more stacks
or measurement sites may be combined for a test run, provided the
following guidelines are met:
(a) All measurement sites up to 12 must be sampled. For more than 12
measurement sites, conduct sampling on at least 12 sites or 50 percent
of the sites, whichever is greater. The measurement sites sampled
should be evenly, or nearly evenly, distributed among the available
sites; if not, all sites are to be sampled.
(b) The same number of measurement sites must be sampled for each
test run.
(c) The minimum number of traverse points per test run is 24. An
exception to the 24-point minimum would be a test combining the sampling
from two stacks meeting Method 1 criteria for acceptable stack length,
and Method 1 specifies fewer than 12 points per site.
(d) As long as the 24 traverse points per test run criterion is met,
the number of traverse points per measurement site may be reduced to
eight.
Alternatively, conduct a test run for each measurement site
individually using the criteria in Section 4.2.1 or 4.2.2 for number of
traverse points. Each test run shall count toward the total of three
required for a performance test. If more than three measurement sites
are sampled, the number of traverse points per measurement site may be
reduced to eight as long as at least 72 traverse points are sampled for
all the tests.
The following examples demonstrate the procedures for sampling
multiple measurement sites.
Example 1: A source with nine circular measurement sites of equal
areas may be tested as follows: For each test run, traverse three
measurement sites using four points per diameter (eight points per
measurement site). In this manner, test run number 1 will include
sampling from sites 1, 2, and 3; run 2 will include samples from sites
4, 5, and 6; and run 3 will include sites 7, 8, and 9. Each test area
may consist of a separate test of each measurement site using eight
points. Use the results from all nine tests in determining the emission
average.
Example 2: A source with 30 rectangular measurement sites of equal
areas may be tested as follows: For each of three test runs, traverse
five measurement sites using a 3 x 3 matrix of traverse points for each
site. In order to distribute the sampling evenly over all the available
measurement sites while sampling only 50 percent of the sites, number
the sites consecutively from 1 to 30 and sample all the even numbered
(or odd numbered) sites. Alternatively, conduct a separate test of each
of 15 measurement sites using Section 4.2.1 or 4.2.2 to determine the
number and location of traverse points, as appropriate.
Example 3: A source with two measurement sites of equal areas may be
tested as follows: For each test of three test runs, traverse both
measurement sites using Section 4.2.3 in determining number of traverse
points. Alternatively, conduct two full emission test runs of each
measurement site using the criteria in Section 4.2.1 or 4.2.2 to
determine the number of traverse points.
Other test schemes, such as random determination of traverse points
for a large number of measurement sites, may be used with prior approval
from the Administrator.
4.3 Velocity Determination. The velocities of exhaust gases from
postitive pressure baghouses are often too low to measure accurately
with the type S pitot specified in Method 2 (i.e., velocity head <1.3 mm
H2O (0.05 in. H2O)). For these conditions, measure the gas flow rate at
the fabric filter inlet following the procedures in Method 2. Calculate
the average gas velocity at the measurement site as follows:
Eq. 5D-1
Where:
v8=Average gas velocity at the measurement site(s), m/s (ft/s).
Qi=Inlet gas volume flow rate, m3/s (ft /3/ /s).
Ao=Measurement site(s) total cross-sectional area, m2 (ft2).
To=Temperature of gas at measurement site, K ( R)
Ti=Temperature of gas at inlet, K ( R).
Use the average velocity calculated for the measurement site in
determining and maintaining isokinetic sampling rates. Note: All
sources of gas leakage, into or out of the fabric filter housing between
the inlet measurement site and the outlet measurement site must be
blocked and made leak-tight.
Velocity determinations at measurement sites with gas velocities
within the range measurable with the type S pitot (i.e., velocity head
1.3 mm H2O (0.05 in. H2O)) shall be conducted according to the
procedures in Method 2.
4.4 Sampling. Follow the procedures specified in Section 4.1 of
Method 5 or Method 17 with the exceptions as noted above.
4.5 Sample Recovery. Follow the procedures specified in Section 4.2
of Method 5 or Method 17.
4.6 Sample Analysis. Follow the procedures specified in Section 4.3
of Method 5 or Method 17.
4.7 Quality Control Procedures. A QC check of the volume metering
system at the field site is suggested before collecting the sample. Use
the procedure defined in Section 4.4 of Method 5.
5. Calibration
Follow the procedures as specified in Section 5 of Method 5 or Method
17.
6. Calculations
Follow the procedures as specified in Section 6 of Method 5 or Method
17 with the exceptions as follows:
6.1 Total volume flow rate may be determined using inlet velocity
measurements and stack dimensions.
6.2 Average Particulate Concentration. For multiple measurement
sites, calculate the average particulate concentration as follows:
Eq. 5D-2
Where:
mi=The mass collected for run i of n, mg(gr).
Voli=The sample volume collected for run i of n, sm3 (scf).
C8=Average concentration of particulate for all n runs, mg/sm3
(gr/scf).
7. Bibliography
The bibliography is the same as for Method 5.
Insert illus. 01123
Insert illus. 01124
40 CFR 60.748 Pt. 60, App. A, Meth. 5E
1. Applicability and Principle
1.1 Applicability. This method is applicable for the determination of
particulate emissions from wool fiberglass insulation manufacturing
sources.
1.2 Principle. Particulate matter is withdrawn isokinetically from
the source and collected on a glass fiber filter maintained at a
temperature in the range of 120 14 C (248 25 F) and in solutions
of 0.1 N NaOH. The filtered particulate mass, which includes any
material that condenses at or above the filtration temperature, is
determined gravimetrically after removal of uncombined water. The
condensed particulate material collected in the impinger solutions is
determined as total organic carbon (TOC) using a nondispersive infrared
type of analyzer. The sum of the filtered particulate mass and the
condensed particulate matter is reported as the total particulate mass.
2. Apparatus
2.1 Sampling Train. The equipment list for the sampling train is the
same as described in Section 2.1 of Method 5 except as follows:
2.1.1 Probe Liner. Same as described in Section 2.1.2 of Method 5
except use only borosilicate or quartz glass liners.
2.1.2 Filter Holder. Same as described in Section 2.1.5 of Method 5
with the addition of a leak-tight connection in the rear half of the
filter holder designed for insertion of a thermocouple or other
temperature gauge for measuring the sample gas exist temperature.
2.2 Sample Recovery. The equipment list for sample recovery is the
same as described in Section 2.2 of Method 5 except three wash bottles
are needed instead of two and only glass storage bottles and funnels may
be used.
2.3 Analysis. The equipment list for analysis is the same as Section
2.3 of Method 5 with the additional equipment for TOC analysis as
described below:
2.3.1 Sample Blender or Homogenizer. Waring type of ultrasonic.
2.3.2 Magnetic Stirrer.
2.3.3 Hypodermic Syringe. 0- to 100-ml capacity.
2.3.4 Total Organic Carbon Analyzer. Beckman Model 915 with 215 B
infrared analyzer or equivalent and a recorder.
2.3.5 Beaker. 30 ml.
2.3.6 Water Bath. Temperature-controlled.
2.3.7 Volumetric Flasks. 1,000 ml and 500 ml.
3. Reagents
3.1 Sampling. The reagents used in sampling are the same as used in
Reference Method 5 with the addition of 0.1 N NaOH (dissolve 40 g of ACS
reagent grade NaOH in distilled water and dilute to 1 liter).
3.2 Sample Recovery. The reagents used in sample recovery are the
same as used in Method 5 with the addition of distilled water and 0.1 N
NaOH as described in Section 3.1.
3.3 Analysis. The reagents used in analysis are the same as in Method
5 except as follows:
3.3.1 Carbon Dioxide-Free Water. Distilled or deionized water that
has been freshly boiled for 15 minutes and cooled to room temperature
while preventing exposure to ambient air with a cover vented with an
ascarite tube.
3.3.2 Hydrochloric Acid. HCl, concentrated, with a dropper.
3.3.3 Organic Carbon Stock Solution. Dissolve 2.1254 g of dried
potassium biphthalate in CO2- free water and dilute to 1 liter in a
volumetric flask. This solution contains 1,000 mg/l organic carbon.
3.3.4 Inorganic Carbon Stock Solution. Dissolve 4.404 g anhydrous
sodium carbonate in about 500 ml of CO2-free water in a 1 liter
volumetric flask. Add 3.497 g anhydrous sodium bicarbonate to the flask
and dilute to 1 liter with CO2-free water. This solution contains 1,000
mg/l inorganic carbon.
3.3.5 Oxygen Gas. CO2-free.
4. Procedure
4.1 Sampling. The sampling procedures are the same as in Section 4.1
of Method 5 except as follows:
4.1.1 Filtration Temperature. The temperature of the filtered gas
stream, rather than the filter compartment air temperature, is
maintained at 120 14 C (248 25 F).
4.1.2 Impinger Solutions. 0.1 N NaOH is used in place of water in
the impingers. The volumes of the solutions are the same as in Method
5.
4.2 Sample Recovery. The sample recovery procedure is as follows:
Water is used to rinse and clean the probe parts prior to the acetone
rinse. Save portions of the water, acetone, and 0.1 N NaOH used for
cleanup as blanks following the procedure as in Section 4.2 of Method 5.
Note: All parts of the sample collection portion of the train (e.g.,
probe and nozzle, filter holder, impinger glassware) must be free of
organic solvent residue before sample collection. It is necessary that
all sampling apparatus that have been rinsed with acetone be flushed
twice with water or dilute NaOH before the sample run. The rinse
solutions from this cleaning process should be discarded. If other
solvents that are not readily soluble in water (e.g., TCE) are used,
place the exposed sampling apparatus in a drying oven at 105 C for at
least 30 minutes.
Container No. 1. The filter is removed and stored in the same manner
as in Section 4.2 of Method 5.
Container No. 2. Use water to rinse the sample nozzle, probe, and
front half of the filter holder three times in the manner described in
Section 4.2 of Method 5 except that no brushing is done. Put all the
wash water in one container, seal, and label.
Container No. 3. Rinse and brush the sample nozzle, probe, and front
half of the filter holder with acetone as described for Container No. 2
in Section 4.2 of Method 5.
Container No. 4. Place the contents of the silica gel impinger in
its original container as described for Container No. 3 in Section 4.2
of Method 5.
Container No. 5. Measure the liquid in the first three impingers and
record the volume or weight as described for the Impinger Water in
Section 4.2 of Method 5. Do not discard this liquid, but place it in a
sample container using a glass funnel to aid in the transfer from the
impingers or graduated cylinder (if used) to the sample container.
Rinse each impinger thoroughly with 0.1 N NaOH three times, as well as
the graduated cylinder (if used) and the funnel, and put these rinsings
in the same sample container. Seal the container and label to identify
its contents clearly.
4.3 Analysis. The procedures for analysis are the same as in Section
4.3 of Method 5 with exceptions noted as follows:
Container No. 1. Determination of weight gain on the filter is the
same as described for Container No. 1 in Section 4.3 of Method 5 except
that the filters must be dried at 20 6 C (68 F 10 F) and at ambient
pressure.
Containers Nos. 2 and 3. Analyze the contents of Containers Nos. 2
and 3 as described for Container No. 2 in Section 4.3 of Method 5
except that evaporation of the samples must be at 20 6 C (68 10 F) and
at ambient pressure.
Container No. 4. Weigh the spent silica gel as described for
Container No. 3 in Section 4.3 of Method 5.
''Water and Acetone Blank'' Containers. Determine the water and
acetone blank values following the procedures for Acetone Blank
Container in Section 4.3 of Method 5. Evaporate the samples at ambient
temperature (20 6 C (68 10 F)) and pressure.
Container No. 5. For the determination of total organic carbon,
perform two analyses on successive identical samples, i.e., total carbon
and inorganic carbon. The desired quantity is the difference between
the two values obtained. Both analyses are based on conversion of
sample carbon into carbon dioxide for measurement by a nondispersive
infrared analyzer. Results of analyses register as peaks on a strip
chart recorder.
The principal differences between operating parameters for the two
channels involve the combustion tube packing material and temperature.
In the total carbon channel, a high temperature (950 C (1740 F)) furnace
heats a Hastelloy combustion tube packed with cobalt oxide-impregnated
asbestos fiber. The oxygen in the carrier gas, the elevated
temperature, and catalytic effect of the packing result in oxidation of
both organic and inorganic carbonaceous material to CO2 and steam. In
the inorganic carbon channel, a low temperature (150 C (300 F)) furnace
heats a glass tube containing quartz chips wetted with 85 percent
phosphoric acid. The acid liberates CO2 and steam from inorganic
carbonates. The operating temperature is below that required to oxidize
organic matter. Follow the manufacturer's instructions for assembly,
testing, calibration, and operation of the analyzer.
As samples collected in 0.1 N NaOH often contain a high measure of
inorganic carbon that inhibits repeatable determinations of TOC, sample
pretreatment is necessary. Measure and record the liquid volume of each
sample. If the sample contains solids or an immiscible liquid,
homogenize the sample with a blender or ultrasonics until satisfactory
repeatability is obtained. Transfer a representative portion of 10 to
15 ml to a 30-ml beaker, acidify with about 2 drops of concentrated HCl
to a pH of 2 or less. Warm the acidified sample at 50 C (120 F) in a
water bath for 15 minutes. While stirring the sample with a magnetic
stirrer, withdraw a 20- to 50- l sample from the beaker and inject it
into the total carbon port of the analyzer. Measure the peak height.
Repeat the injections until three consecutive peaks are obtained within
10 percent of the average.
Repeat the analyses for all the samples and the 0.1 N NaOH blank.
Prepare standard curves for total carbon and for inorganic carbon of 10,
20, 30, 40, 50, 60, 80, and 100 mg/l by diluting with CO2-free water 10,
20, 30, 40, and 50 ml of the two stock solutions to 1,000 ml and 30, 40,
and 50 ml of the two stock solutions to 500 ml. Inject samples of these
solutions into the analyzer and record the peak heights as described
above. The acidification and warming steps are not necessary for
preparation of the standard curve.
Ascertain the sample concentrations for the samples from the
corrected peak heights for the samples by reference to the appropriate
standard curve. Calculate the corrected peak height for the standards
and the samples by deducting the blank correction as follows:
Eq. 5E-1
Where:
A=Peak height of standard or sample, mm or other appropriate unit.
B=Peak height of blank, mm or other appropriate unit.
If samples must be diluted for analysis, apply an appropriate
dilution factor.
5. Calibration
Calibration of sampling and analysis equipment is the same as in
Section 5 of Method 5 with the addition of the calibration of the TOC
analyzer described in Section 4.3 of this method.
6. Calculations
The calculations and nomenclature for the calculations are the same
as described in Section 6 of Method 5 with the addition of the
following:
6.1 Mass of Condensed Particulate Material Collected.
Eq. 5E-2
Where:
0.001=Liters per milliliter.
mc=Mass of condensed particulate material collected in the impingers
measured as TOC, mg.
Ctoc=Concentration of TOC in the liquid sample from TOC analysis in
Section 4.3, mg/l.
Vs=Total volume of liquid sample, ml.
6.2 Concentration of Condensed Particulate Material.
Where:
0.001=Grams per milligram.
Cc=Concentration of condensed particulate matter in stack gas, dry
basis, corrected to standard condition, g/dscm.
Vm(std)=Volume of gas sample measured by the dry gas meter, corrected
to standard conditions, dscm, from Section 6.3 of Method 5.
6.3 Total Particulate Concentration.
Where:
Ct=Total particulate concentration, dry basis, corrected to standard
conditions, g/dscm.
Cs=Concentration of filtered particulate matter in stack gas, dry
basis, corrected to standard conditions, g/dscm, from Equation 5-6 of
Method 5.
7. Bibliography
The bibliography is the same as in Method 5 with the addition of the
following:
1. American Public Health Association, American Water Works
Association, Water Pollution Control Federation. Standard Methods for
the Examination of Water and Wastewater. Fifteenth Edition.
Washington, DC 1980.
40 CFR 60.748 Pt. 60, App. A, Meth. 5F
1. Applicability and Principle.
1.1 Applicability. This method is to be used for determining
nonsulfate particulate matter from stationary sources. Use of this
method must be specified by an applicable subpart of the standards, or
approved by the Administrator, U.S. Environmental Protection Agency, for
a particular application.
1.2 Principle. Particulate matter is withdrawn isokinetically from
the source using the Method 5 train at 160 C (320 F). The collected
sample is then extracted with water. A portion of the extract is
analyzed for sulfate content. The remainder is neutralized with
ammonium hydroxide before it is dried and weighed.
2. Apparatus.
The apparatus is the same as Method 5 with the following additions.
2.1 Analysis.
2.1.1 Erlenmeyer Flasks. 125-ml, with ground glass joints.
2.1.2 Air Condenser. With ground glass joint compatible with the
Erlenmeyer flasks.
2.1.3 Beakers. 250-ml.
2.1.4 Volumetric Flasks. 1-liter, 500-ml (one for each sample),
200-ml, and 50-ml (one for each sample and standard).
2.1.5 Pipets. 5-ml (one for each sample and standard).
2.1.6 Ion Chromatograph. The ion chromatograph should have at least
the following components.
2.1.6.1 Columns. An anion separation or other column capable of
resolving the sulfate ion from other species present and a standard
anion suppressor column. Suppressor columns are produced as proprietary
items; however, one can be produced in the laboratory using the resin
available from BioRad Company, 32nd and Griffin Streets, Richmond,
California. Other systems which do not use suppressor columns may also
be used.
2.1.6.2 Pump. Capable of maintaining a steady flow as required by the
system.
2.1.6.3 Flow Gauges. Capable of measuring the specified system flow
rate.
2.1.6.4 Conductivity Detector.
2.1.6.5 Recorder. Compatible with the output voltage range of the
detector.
3. Reagents.
The reagents are the same as for Method 5 with the following
exceptions:
3.1 Sample Recovery. Water, deionized distilled to conform to
American Society for Testing and Materials Specification D1193-74, Type
3, is needed. At the option of the analyst, the KMnO4 test for
oxidizable organic matter may be omitted when high concentrations of
organic matter are not expected to be present.
3.2 Analysis. The following are required:
3.2.1 Water. Same as in Section 3.1.
3.2.2 Stock Standard Solution, 1 mg (NH4)2SO4/ml. Dry an adequate
amount of primary standard grade ammonium sulfate at 105 to 110 C for
a minimum of 2 hours before preparing the standard solution. Then
dissolve exactly 1.000 g of dried (NH4)2SO4 in water in a 1-liter
volumetric flask, and dilute to 1 liter. Mix well.
3.2.3 Working Standard Solution, 25 g (NH4)2SO4/ml. Pipet 5 ml of
the stock standard solution into a 200-ml volumetric flask. Dilute to
200 ml with water.
3.2.4 Eluent Solution. Weigh 1.018 g of sodium carbonate (Na2CO3)
and 1.008 g of sodium bicarbonate (NaHCO3), and dissolve in 4 liters of
water. This solution is 0.0024 M Na2CO3/0.003 M NaHCO3. Other eluents
appropriate to the column type and capable of resolving sulfate ion from
other species present may be used.
3.2.5 Ammonium Hydroxide. Concentrated, 14.8 M.
3.2.6 Phenolphthalein Indicator.
3,3-Bis(4-hydroxyphenyl)-1-(3H)-isobenzofuranone. Dissolve 0.05 g in 50
ml of ethanol and 50 ml of water.
4. Procedure.
4.1 Sampling. The sampling procedure is the same as Method 5, Section
4.1, except that the probe outlet and filter temperatures shall be
maintained at 160 14 C (320 25 F).
4.2 Sample Recovery. The sample recovery procedure is the same as
Method 5, Section 4.2, except that the recovery solvent shall be water
instead of acetone.
4.3 Analysis.
4.3.1 Sample Extraction. Cut the filter into small pieces, and place
it in a 125-ml Erlenmeyer flask with a ground glass joint equipped with
an air condenser. Rinse the shipping container with water, and pour the
rinse into the flask. Add additional water to the flask until it
contains about 75 ml, and place the flask on a hot plate. Gently reflux
the contents for 6 to 8 hours. Cool the solution, and transfer it to a
500-ml volumetric flask. Rinse the Erlenmeyer flask with water, and
transfer the rinsings to the volumetric flask including the pieces of
filter.
Transfer the probe rinse to the same 500-ml volumetric flask with the
filter sample. Rinse the sample bottle with water, and add the rinsings
to the volumetric flask. Dilute the sample to exactly 500 ml with
water.
4.3.2 Sulfate (SO4) Analysis. Allow the sample to settle until all
solid material is at the bottom of the volumetric flask. If necessary,
centrifuge a portion of the sample. Pipet 5 ml of the sample into a
50-ml volumetric flask, and dilute to 50 ml with water. Prepare a
standard calibration curve according to Section 5.1. Analyze the set of
standards followed by the set of samples using the same injection volume
for both standards and samples. Repeat this analysis sequence followed
by a final analysis of the standard set. Average the results. The two
sample values must agree within 5 percent of their mean for the analysis
to be valid. Perform this duplicate analysis sequence on the same day.
Dilute any sample and the blank with equal volumes of water if the
concentration exceeds that of the highest standard.
Document each sample chromatogram by listing the following analytical
parameters: Injection point, injection volume, sulfate retention time,
flow rate, detector sensitivity setting, and recorder chart speed.
4.3.3 Sample Residue. Transfer the remaining contents of the
volumetric flask to a tared 250-ml beaker. Rinse the volumetric flask,
and add the rinsings to the tared beaker. Make certain that all
particulate matter is transferred to the beaker. Evaporate the water in
an oven heated to 105 C until only about 100 ml of water remains.
Remove the beakers from the oven, and allow them to cool.
After the beakers have cooled, add five drops of phenolphthalein
indicator, and then add concentrated ammonium hydroxide until the
solution turns pink. Return the samples to the oven at 105 C, and
evaporate the samples to dryness. Cool the samples in a desiccator, and
weigh the samples to constant weight.
4.4 Blanks.
4.4.1 Filter Blank. Choose a clean filter from the same lot as those
used in the testing. Treat the blank filter as a sample, and analyze
according to Sections 4.3.1 and 4.3.2.
4.4.2 Water. Transfer a measured volume of water between 100 and 200
ml into a tared 250-ml beaker. Treat the blank as a sample, and analyze
according to Section 4.3.3.
5. Calibration.
The calibration procedure is the same as Method 5, Section 5, with
the following additions:
5.1 Standard Calibration Curve. Prepare a series of five standards
by adding 1.0, 2.0, 4.0, 6.0, and 10.0 ml of working standard solution
(25 g/ml) to a series of five 50-ml volumetric flasks. (The standard
masses will equal 25, 50, 100, 150, and 250 g.) Dilute each flask to
volume with water, and mix well. Analyze with the samples as described
in Section 4.3. Prepare or calculate a linear regression plot of the
standard masses in g (x-axis) versus their responses (y-axis). (Take
peak height measurements with symmetrical peaks; in all other cases,
calculate peak areas.) From this line, or equation, determine the slope,
and calculate its reciprocal which is the calibration factor, S. If any
point deviates from the line by more than 7 percent of the concentration
at that point, remake and reanalyze that standard. This deviation can
be determined by multiplying S times the response for each standard.
The resultant concentrations must not differ by more than 7 percent from
each known standard mass (i.e., 25, 50, 100, 150, and 250 g).
5.2 Conductivity Detector. Calibrate according to manufacturer's
specifications prior to initial use.
6. Calculations.
Calculations are the same as Method 5, Section 6, with the following
additions:
6.1 Nomenclature.
Cw=Water blank residue concentration, mg/ml.
F=Dilution factor (required only if sample dilution was needed to
reduce the concentration into the range of calibration).
Hs=Sample response, mm for height or mm /2/ for area.
Hb=Filter blank response, mm for height or mm /2/ for area.
mb=Mass of beaker used to dry sample, mg.
mf=Mass of sample filter, mg.
mn=Mass of nonsulfate particulate matter, mg.
ms=Mass of ammonium sulfate in the sample, mg.
mt=Mass of beaker, filter, and dried sample, mg.
mw=Mass of residue after evaporation of water blank, mg.
S=Calibration factor, g/mm.
Vb=Volume of water blank, ml.
Vs=Volume of sample evaporated, 495 ml.
6.2 Water Blank Concentration.
Eq. 5F-1
6.3 Mass of Ammonium Sulfate.
Eq. 5F-2
6.4 Mass of Nonsulfate Particulate Matter.
mn=mt^mb^ms^mf^VsCw
Eq. 5F-3
7.1 The following procedure may be used as an alternative to the
procedure in Section 4.3.
7.1.1 Apparatus. Same as for Method 6, Sections 2.3.3 to 2.3.6 with
the following additions.
7.1.1.1 Beakers. 250-ml, one for each sample, and 600-ml.
7.1.1.2 Oven. Capable of maintaining temperatures of 75 5 C and
105 5 C.
7.1.1.3 Buchner Funnel.
7.1.14 Glass Columns. 25-mm 305-mm (1-in. 12-in.) with Teflon
stopcock.
7.1.1.5 Volumetric Flasks. 50-ml and 500-ml, one set for each
sample, and 100-ml, 200-ml, and 1000-ml.
7.1.1.6 Pipettes. Two 20-ml and one 200-ml, one set for each sample,
and 5-ml.
7.1.1.7 Filter Flasks. 500-ml.
7.1.1.8 Polyethylene Bottle. 500-ml, one for each sample.
7.1.2 Reagents. Same as Method 6, Sections 3.3.2 to 3.3.5 with the
following additions:
7.1.2.1 Water, Ammonium Hydroxide, and Phenolphthalein. Same as
Sections 3.2.1, 3.2.5, and 3.2.6 of this method, respectively.
7.1.2.2 Filter. Glass fiber to fit Buchner funnel.
7.1.2.3 Hydrochloric Acid (HCl), 1 M. Add 8.3 ml of concentrated HCl
(12 M) to 50 ml of water in a 100-ml volumetric flask. Dilute to 100 ml
with water.
7.1.2.4 Glass Wool.
7.1.2.5 Ion Exchange Resin. Strong cation exchange resin, hydrogen
form, analytical grade.
7.1.2.6 pH Paper. Range of 1 to 7.
7.1.3 Analysis.
7.1.3.1 Ion Exchange Column Preparation. Slurry the resin with 1 M
HCl in a 250-ml beaker, and allow to stand overnight. Place 2.5 cm (1
in.) of glass wool in the bottom of the glass column. Rinse the
slurried resin twice with water. Resuspend the resin in water, and pour
sufficent resin into the column to make a bed 5.1 cm (2 in.) deep. Do
not allow air bubbles to become entrapped in the resin or glass wool to
avoid channeling, which may produce erratic results. If necessary, stir
the resin with a glass rod to remove air bubbles. after the column has
been prepared, never let the liquid level fall below the top of the
upper glass wool plug. Place a 2.5-cm (1-in.) plug of glass wool on top
of the resin. Rinse the column with water until the eluate gives a pH
of 5 or greater as measured with pH paper.
7.1.3.2 Sample Extraction. Follow the procedure given in Section
4.3.1 except do not dilute the sample to 500 ml.
7.1.3.3 Sample Residue. Place at least one clean glass fiber filter
for each sample in a Buchner funnel, and rinse the filters with water.
Remove the filters from the funnel, and dry them in an oven at 105 5
C; then cool in a desiccator. Weigh each filter to constant weight
according to the procedure in Method 5, Section 4.3. Record the weight
of each filter to the nearest 0.1 mg.
Assemble the vacuum filter apparatus, and place one of the clean,
tared glass fiber filters in the Buchner funnel. Decant the liquid
portion of the extracted sample (Section 7.1.3.2) through the tared
glass fiber filter into a clean, dry, 500-ml filter flask. Rinse all
the particulate matter remaining in the volumetric flask onto the glass
fiber filter with water. Rinse the particulate matter with additional
water. Transfer the filtrate to a 500-ml volumetric flask, and dilute
to 500 ml with water. Dry the filter overnight at 105 5 C, cool in a
desiccator, and weigh to the nearest 0.1 mg.
Dry a 250-ml beaker at 75 5 C, and cool in a desiccator; then
weigh to constant weight to the nearest 0.1 mg. Pipette 200 ml of the
filtrate that was saved into a tared 250-ml beaker; add five drops of
phenolphtahalein indicator and sufficient concentrated ammonium
hydroxide to turn the solution pink. Carefully evaporate the contents
of the beaker to dryness at 75 5 C. Check for dryness every 30
minutes. Do not continue to bake the sample once it has dried. Cool
the sample in a desiccator, and weigh to constant weight to the nearest
0.1 mg.
7.1.3.4 Sulfate Analysis. Adjust the flow rate through the ion
exchange column to 3 ml/min. Pipette a 20-ml aliquot of the filtrate
onto the top of the ion exchange column, and collect the eluate in a
50-ml volumetric flask. Rinse the column with two 15-ml portions of
water. Stop collection of the eluate when the volume in the flask
reaches 50-ml. Pipette a 20-ml aliquot of the eluate into a 250-ml
Erlenmeyer flask, add 80 ml of 100 percent isopropanol and two to four
drops of thorin indicator, and titrate to a pink end point using 0.0100
N barium perchlorate. Repeat and average the titration volumes. Run a
blank with each series of samples. Replicate titrations must agree
within 1 percent or 0.2 ml, whichever is larger. Perform the ion
exchange and titration procedures on duplicate portions of the filtrate.
Results should agree within 5 percent. Regenerate or replace the ion
exchange resin after 20 sample aliquotes have been analyzed or if the
end point of the titration becomes unclear.
Note: Protect the 0.0100 N barium perchlorate solution from
evaporation at all times.
7.1.3.5 Blank Determination. Begin with a sample of water of the
same volume as the samples being processed and carry it through the
analysis steps described in Sections 7.1.3.3 and 7.1.3.4. A blank value
larger that 5 mg should not be subtracted from the final particulate
matter mass. Causes for large blank values should be investigated and
any problems resolved before proceeding with further analyses.
7.1.4 Calibration. Calibrate the barium perchlorate solutions as in
Method 6, Section 5.5.
7.1.5 Calculations.
7.1.5.1 Nomenclature. Same as Section 6.1 with the following
additions:
ma = Mass of clean analytical filter, mg.
md = Mass of dissolved particulate matter, mg.
me = Mass of beaker and dissolved particulate matter after
evaporation of filtrate, mg.
mp = Mass of insoluble particulate matter, mg.
mr = Mass of analytical filter, sample filter, and insoluble
particulate matter, mg.
mbk = Mass of nonsulfate particulate matter in blank sample, mg.
N = Normality of Ba(Cl04)2 titrant, meq/ml.
Va = Volume of aliquot taken for titration, 20 ml.
Vc = Volume of titrant used for titration blank, ml.
Vd = Volume of filtrate evaporated, 200ml.
Ve = Volume of eluate collected, 50 ml.
Vf = Volume of extracted sample, 500 ml.
Vi = Volume of filtrate added to ion exchange column, 20 ml.
Vt = Volume of Ba(Cl04)2 titrant, ml.
W = Equivalent weight of ammonium sulfate, 66.07 mg/meq.
7.1.5.2 Mass of Insoluble Particulate Matter.
7.1.5.3 Mass of Dissolved Particulate Matter.
md = (me ^ (Vf/Vd) mb) Eq. 5F-5
7.1.5.4 Mass of Ammonium Sulfate.
7.1.5.5 Mass of Nonsulfate Particulate Matter.
8. Bibliography.
1. Mulik, J.D. and E. Sawicki. Ion Chromatographic Analysis of
Environmental Pollutants. Ann Arbor, Ann Arbor Science Publishers, Inc.
Vol. 2. 1979.
2. Sawicki, E., J.D. Mulik, and E. Wittgenstein. Ion Chromatographic
Analysis of Environmental Pollutants. Ann Arbor, Ann Arbor Science
Publishers, Inc. Vol. 1. 1978.
3. Siemer, D.D. Separation of Chloride and Bromide From Complex
Matrices Prior to Ion Chromatographic Determination. Analytical
Chemistry. 52(12):1874-1877. October 1980.
4. Small, H., T.S. Stevens, and W.C. Bauman. Novel Ion Exchange
Chromatographic Method Using Conductimetric Determination. Analytical
Chemistry. 47(11):1801. 1975.
40 CFR 60.748 Pt. 60, App. A, Meth. 5G
1.1 Applicability. This method is applicable for the determination of
particulate matter emissions from wood heaters.
1.2 Principle. Particulate matter is withdrawn proportionally at a
single point from a total collection hood and sampling tunnel that
combines the wood heater exhaust with ambient dilution air. The
particulate matter is collected on two glass fiber filters in series.
The filters are maintained at a temperature of no greater than 32 C (90
F). The particulate mass is determined gravimetrically after removal
of uncombined water.
There are three sampling train approaches described in this method:
(1) One dual-filter dry sampling train operated at about 0.015 m /3/
/min, (2) One dual-filter plus impingers sampling train operated at
about 0.015 m /3/ /min, and (3) two dual-filter dry sampling trains
operated simultaneously at any flow rate. Options (2) and (3) are
referenced in Section 7 of this method. The dual-filter sampling train
equipment and operation, option (1), are described in detail in this
method.
2.1 Sampling Train. The sampling train configuration is shown in
Figure 5G-1 and consists of the following components:
2.1.1 Probe. Stainless steel (e.g., 316 or grade more corrosion
resistant) or glass about 95 mm ( 3/8 in.) I.D., 0.6 m (24 in.) in
length. If made of stainless steel, the probe shall be constructed from
seamless tubing.
2.1.2 Pitot Tube. Type S, as described in Section 2.1 of Method 2.
The Type S pitot tube assembly shall have a known coefficient,
determined as outlined in Method 2, Section 4.
Alternatively, a standard pitot may be used as described in Method 2,
Section 2.1.
2.1.3 Differential Pressure Gauge. Inclined manometer or equivalent
device, as described in Method 2, Section 2.2. One manometer shall be
used for velocity head (Dp) readings and another (optional) for orifice
differential pressure readings (DH).
2.1.4 Filter Holders. Two each made of borosilicate glass, stainless
steel, or Teflon, with a glass frit or stainless steel filter support
and a silicone rubber, Teflon, or Viton gasket. The holder design shall
provide a positive seal against leakage from the outside or around the
filters. The filter holders shall be placed in series with the backup
filter holder located 25 to 100 mm (1 to 4 in.) downstream from the
primary filter holder. The filter holder shall be capable of holding a
filter with a 100 mm (4 in.) diameter, except as noted in Section 7.
Note: Mention of trade names or specific product does not constitute
endorsement by the Environmental Protection Agency.
2.1.5 Filter Temperature Monitoring System. A temperature gauge
capable of measuring temperature to within 1.5 percent of absolute
temperature. The gauge shall be installed at the exit side of the front
filter holder so that the sensing tip of the temperature gauge is in
direct contact with the sample gas or in a thermowell as shown in Figure
5G-1. The temperature gauge shall comply with the calibration
specifications in Method 2, Section 4. Alternatively, the sensing tip
of the temperature gauge may be installed at the inlet side of the front
filter holder.
2.1.6 Dryer. Any system capable of removing water from the sample gas
to less than 1.5 percent moisture (volume percent) prior to the metering
system. System includes monitor for demonstrating that sample gas
temperature is less than 20 C (68 F).
2.1.7 Metering System. Same as Method 5, Section 2.1.8.
2.1.8 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg).
2.1.9 Dilution Tunnel Gas Temperature Measurement. A temperature
gauge capable of measuring temperature to within 1.5 percent of absolute
temperature.
2.2 Dilution Tunnel. The dilution tunnel apparatus is shown in
Figure 5G-2 and consists of the following components:
2.2.1 Hood. Constructed of steel with a minimum diameter of 0.3 m (1
ft) on the large end and a standard 0.15 to 0.3 m (0.5 to 1 ft) coupling
capable of connecting to standard 0.15 to 0.3 m (0.5 to 1 ft) stove pipe
on the small end.
2.2.2 90 Elbows. Steel 90 elbows, 0.15 to 0.3 m (0.5 to 1 ft) in
diameter for connecting mixing duct, straight duct and damper (optional)
assembly. There shall be at least two 90 elbows upstream of the
sampling section (see Figure 5G-2).
2.2.3 Straight Duct. Steel, 0.15 to 0.3 m (0.5 to 1 ft) in diameter
to provide the ducting for the dilution apparatus upstream of the
sampling section. Steel duct, 0.15 m (0.5 ft) in diameter shall be used
for the sampling section. In the sampling section, at least 1.2 m (4
ft) downstream of the elbow, shall be two holes (velocity traverse
ports) at 90 to each other of sufficient size to allow entry of the
pitot for traverse measurements. At least 1.2 m (4 ft) downstream of
the velocity traverse ports, shall be one hole (sampling port) of
sufficient size to allow entry of the sampling probe. Ducts of larger
diameter may be used for the sampling section, provided the
specifications for minimum gas velocity and the dilution rate range
shown in Section 4 are maintained. The length of duct from the hood
inlet to the sampling ports shall not exceed 9.1 m (30 ft).
2.2.4 Mixing Baffles. Steel semicircles (two) attached at 90 to the
duct axis on opposite sides of the duct midway between the two elbows
upstream of sampling section. The space between the baffles shall be
about 0.3 m (12 in.).
2.2.5 Blower. Squirrel cage or other fan capable of extracting gas
from the dilution tunnel of sufficient flow to maintain the velocity and
dilution rate specifications in Section 4 and exhausting the gas to the
atmosphere.
2.3 Sample Recovery. Probe brushes, wash bottles, sample storage
containers, petri dishes, and a funnel as described in Method 5, Section
2.2.1 through 2.2.4, and 2.2.8, respectively, are needed.
2.4 Analysis. Glass weighing dishes, desiccator, analytical balance,
beakers (250 ml or smaller), hygrometer, and temperature gauge as
described in Method 5, Sections 2.3.1 through 2.3.3 and 2.3.5 through
2.3.7, respectively, are needed.
3.1 Sampling. The reagents used in sampling are as follows:
3.1.1 Filters. Glass fiber filters with a minimum diameter of 100 mm
(4 in.), without organic binder, exhibiting at least 99.95 percent
efficiency (<0.05 percent penetration) on 0.3-micron dioctyl phthalate
smoke particles. Gelman A/E 61631 has been found acceptable for this
purpose.
3.1.2 Stopcock Grease. Same as Method 5, Section 3.1.5.
3.2 Sample Recovery. Acetone-reagent grade, same as Method 5,
Section 3.2.
3.3 Analysis. Two reagents are required for the analysis:
3.3.1 Acetone. As in Section 3.2.
3.3.2 Desiccant. Anhydrous calcium sulfate, calcium chloride, or
silica gel, indicating type.
4.1 Dilution Tunnel. A schematic of a dilution tunnel is shown in
Figure 5G-2. The dilution tunnel dimensions and other features are
described in Section 2.2. Assemble the dilution tunnel sealing joints
and seams to prevent air leakage. Clean the dilution tunnel with an
appropriately sized, wire chimney brush before each certification test.
4.1.1 Draft Determination. Prepare the wood heater as in Method 28,
Section 6.2.1. Locate the dilution tunnel hood centrally over the wood
heater stack exhaust. Operate the dilution tunnel blower at the flow
rate to be used during the test run. Measure the draft imposed on the
wood heater by the dilution tunnel (i.e., the difference in draft
measured with and without the dilution tunnel operating) as described in
Method 28, Section 6.2.3. Adjust the distance between the top of the
wood heater stack exhaust and the dilution tunnel hood so that the
dilution tunnel induced draft is less than 1.25 Pa (0.005 in. H2O).
Have no fire in the wood heater, close the wood heater doors, and open
fully the air supply controls during this check and adjustment.
4.1.2 Smoke Capture. During the pretest ignition period described in
Method 28, Section 6.3, operate the dilution tunnel and visually monitor
the wood heater stack exhaust. Operate the wood heater with the doors
closed and determine that 100 percent of the exhaust gas is collected by
the dilution tunnel hood. If less than 100 percent of the wood heater
exhaust gas is collected, adjust the distance between the wood heater
stack and the dilution tunnel hood until no visible exhaust gas is
escaping. Stop the pretest ignition period, and repeat the draft
determination procedure described in Section 4.1.1.
4.2 Velocity Measurements. During the pretest ignition period
described in Method 28, Section 6.3, conduct a velocity traverse to
identify the point of average velocity. This single point shall be used
for measuring velocity during the test run.
4.2.1 Velocity Traverse. Measure the diameter of the duct at the
velocity traverse port location through both ports. Calculate the duct
area using the average of the two diameters. A pretest leak-check of
pitot lines as in Method 2, Section 3.1, is recommended. Place the
calibrated pitot tube at the centroid of the stack in either of the
velocity traverse ports. Adjust the damper or similar device on the
blower inlet until the velocity indicated by the pitot is approximately
220 m/min (715 fpm). Continue to read the Dp and temperature until the
velocity has remained constant (less than 5 percent change) for 1
minute. Once a constant velocity is obtained at the centroid of the
duct, perform a velocity traverse as outlined in Method 2, Section 3.3
using four points per traverse as outlined in Method 1. Measure the Dp
and tunnel temperature at each traverse point and record the readings.
Calculate the total gas flow rate using calculations contained in Method
2, Section 5. Verify that the flow rate is 4 0.45 sm /3/ /min (140
14 scfm); if not, readjust the damper, and repeat the velocity
traverse. The moisture may be assumed to be 4 percent (100 percent
relative humidity at 85 F). Direct moisture measurements such as
outlined in EPA Method 4 are also permissible.
Note: If burn rates exceed 3 kg/hr (6.6 lb/hr), dilution tunnel duct
flow rates greater than 4 sm /3/ /min (140 scfm) and sampling section
duct diameters larger than 150 mm (6 in.) are allowed. If larger ducts
or flow rates are used, the sampling section velocity shall be at least
220 m/min (715 fpm). In order to ensure measurable particulate mass
catch, it is recommended that the ratio of the average mass flow rate in
the dilution tunnel to the average fuel burn rate be less than 150:1 if
larger duct sizes or flow rates are used.
4.2.2 Testing Velocity Measurements. After obtaining velocity
traverse results that meet the flow rate requirements, choose a point of
average velocity and place the pitot and thermocouple at that location
in the duct. Alternatively, locate the pitot and thermocouple at the
duct centroid and calculate a velocity correction factor for the
centroidal position. Mount the pitot to ensure no movement during the
test run and seal the port holes to prevent any air leakage. Align the
pitot to be parallel with the duct axis, at the measurement point.
Check that this condition is maintained during the test run (about
30-minute interva1s). Monitor the temperature and velocity during the
pretest ignition period to ensure the proper flow rate is maintained.
Make adjustments to the dilution tunnel flow rate as necessary.
4.3 Sampling.
4.3.1 Pretest Preparation. It is suggested that sampling equipment
be maintained and calibrated according to the procedure described in
APTD-0576.
Check and desiccate filters as described in Method 5, Section 4.1.1.
4.3.2 Preparation of Collection Train. During preparation and
assembly of the sampling train, keep all openings where contamination
can occur covered until just prior to assembly or until sampling is
about to begin.
Using a tweezer or clean disposable surgical gloves, place one
labeled (identified) and weighed filter in each of the filter holders.
Be sure that each of the filters is properly centered and the gasket
properly placed so as to prevent the sample gas stream from
circumventing the filter. Check each of the filters for tears after
assembly is completed.
Mark the probe with heat resistant tape or by some other method to
denote the proper distance into the stack or duct.
Set up the train as in Figure 5G-1.
4.3.3 Leak-Check Procedures.
4.3.3.1 Pretest Leak-Check. A pretest leak-check is recommended, but
not required. If the tester opts to conduct the pretest leak-check,
conduct the leak-check as described in Method 5, Section 4.1.4.1. A
vacuum 130 mm Hg (5 in. Hg) may be used instead of 380 mm Hg (15 in.
Hg).
4.3.3.2 Post-Test Leak-Check. A leak-check is mandatory at the
conclusion of each test run. The leak-check shall be done in accordance
with the procedures described in Method 5, Section 4.1.4.1. A vacuum of
130 mm Hg (5 in. Hg) or the greatest vacuum measured during the test
run, whichever is greater, may be used instead of 380 mm Hg (15 in. Hg).
4.3.4 Preliminary Determinations. Determine the pressure,
temperature and the average velocity of the tunnel gases as in Section
4.2. Moisture content of diluted tunnel gases is assumed to be 4 percent
for making flow rate calculations; the moisture content may be measured
directly as in Method 4.
4.3.5 Sampling Train Operation. Position the probe inlet at the
stack centroid, and block off the openings around the probe and porthole
to prevent unrepresentative dilution of the gas stream. Be careful not
to bump the probe into the stack wall when removing or inserting the
probe through the porthole; this minimizes the chance of extracting
deposited material.
Begin sampling at the start of the test run as defined in Method 28,
Section 6.4.1. During the test run, maintain a sample flow rate
proportional to the dilution tunnel flow rate (within 10 percent of the
initial proportionality ratio) and a filter holder temperature of no
greater than 32 C (90 F). The initial sample flow rate shall be
approximately 0.015 m /3/ /min (0.5 cfm).
For each test run, record the data required on a data sheet such as
the one shown in Figure 5G-3. Be sure to record the initial dry gas
meter reading. Record the dry gas meter readings at the beginning and
end of each sampling time increment and when sampling is halted. Take
other readings as indicated on Figure 5G-3 at least once each 10 minutes
during the test run. Since the manometer level and zero may drift
because of vibrations and temperature changes, make periodic checks
during the test run.
For the purposes of proportional sampling rate determinations, data
from calibrated flow rate devices, such as glass rotameters, may be used
in lieu of incremental dry gas meter readings. Proportional rate
calculation procedures must be revised, but acceptability limits remain
the same.
During the test run, make periodic adjustments to keep the
temperature between (or upstream of) the filters at the proper level.
Do not change sampling trains during the test run.
At the end of the test run (see Method 28, Section 6.4.6), turn off
the coarse adjust valve, remove the probe from the stack, turn off the
pump, record the final dry gas meter reading, and conduct a post-test
leak-check, as outlined in Section 4.3.3. Also, leak-check the pitot
lines as described in Method 2, Section 3.1; the lines must pass this
leak-check in order to validate the velocity head data.
4.3.6 Calculation of Proportional Sampling Rate. Calculate percent
proportionality (see Calculations, Section 6) to determine whether the
run was valid or another test run should be made.
4.4 Sample Recovery. Begin recovery of the probe and filter samples
as described in Method 5, Section 4.2, except that an acetone blank
volume of about 50 ml or more may be used.
Treat the samples as follows:
Container No. 1. Carefully remove the filter from the primary filter
holder and place it in its identified (labeled) petri dish container.
Use a pair of tweezers and/or clean disposable surgical gloves to handle
the filter. If it is necessary to fold the filter, do so such that the
particulate cake is inside the fold. Carefully transfer to the petri
dish any particulate matter and/or filter fibers which adhere to the
filter holder gasket, by using a dry Nylon bristle brush and/or a
sharp-edged blade. Seal the container.
Container No. 2. Remove the filter from the second filter holder
using the same procedures as described above.
Note: The two filters may be placed in the same container for
desiccation and weighing. Use the sum of the filter tare weights to
determine the sample mass collected.
Container No. 3. Taking care to see that dust on the outside of the
probe or other exterior surfaces does not get into the sample,
quantitatively recover particulate matter or any condensate from the
probe and filter holders by washing and brushing these components with
acetone and placing the wash in a labeled (No. 3) glass container. At
least three cycles of brushing and rinsing are necessary.
Between sampling runs, keep brushes clean and protected from
contamination.
After all acetone washings and particulate matter have been collected
in the sample containers, tighten the lids on the sample containers so
that the acetone will not leak out when transferred to the laboratory
weighing area. Mark the height of the fluid levels to determine whether
leakage occurs during transport. Label the containers clearly to
identify contents. Requirements for capping and transport of sample
containers are not applicable if sample recovery and analysis occur in
the same room.
4.5 Analysis. Record the data required on a sheet such as the one
shown in Figure 5G-4. Use the same analytical balance for determining
tare weight and final sample weights. Handle each sample container as
follows:
Containers No. 1 and 2. Leave the contents in the sample containers
or transfer the filters and loose particulate to tared glass weighing
dishes. Desiccate for no more than 36 hours before the initial
weighing, weigh to a constant weight, and report the results to the
nearest 0.1 mg. For purposes of this section, the term ''constant
weight'' means a difference of no more than 0.5 mg or 1 percent of total
sample weight (less tare weight), whichever is greater, between two
consecutive weighings, with no less than 2 hours between weighings.
Container No. 3. Note the level of liquid in the container, and
confirm on the analysis sheet whether leakage occurred during transport.
If a noticeable amount of leakage has occurred, either void the sample
or use methods, subject to the approval of the Administrator, to correct
the final results. Determination of sample leakage is not applicable if
sample recovery and analysis occur in the same room. Measure the liquid
in this container either volumetrically to within 1 ml or
gravimetrically to within 0.5 g. Transfer the contents to a tared 250 ml
or smaller beaker and evaporate to dryness at ambient temperature and
pressure. Desiccate and weigh to a constant weight. Report the results
to the nearest 0.1 mg.
''Acetone Blank'' Container. Measure acetone in this container
either volumetrically or gravimetrically. Transfer the acetone to a
tared 250 ml or smaller beaker and evaporate to dryness at ambient
temperature and pressure. Desiccate and weigh to a constant weight.
Report the results to the nearest 0.1 mg.
Maintain a laboratory record of all calibrations.
5.1 Pitot Tube. The Type S pitot tube assembly shall be calibrated
according to the procedure outlined in Method 2, Section 4, prior to the
first certification test and checked semiannually, thereafter. A
standard pitot need not be calibrated but shall be inspected and
cleaned, if necessary, prior to each certification test.
5.2 Volume Metering System.
5.2.1 Initial and Periodic Calibration. Before its initial use and
at least semiannually thereafter, calibrate the volume metering system
as described in Method 5, Section 5.3.1, except that the wet test meter
with a capacity of 3.0 liters/rev (0.1 ft /3/ /rev) may be used. Other
liquid displacement systems accurate to within 1 percent, may be used as
calibration standards.
Procedures and equipment specified in Method 5, Section 7, for
alternative calibration standards, including calibrated dry gas meters
and critical orifices, are allowed for calibrating the dry gas meter in
the sampling train. A dry gas meter used as a calibration standard
shall be recalibrated at least once annually.
5.2.2 Calibration After Use. After each certification or audit test
(four or more test runs conducted on a wood heater at the four burn
rates specified in Method 28), check calibration of the metering system
by performing three calibration runs at a single, intermediate flow rate
as described in Method 5, Section 5.3.2.
Procedures and equipment specified in Method 5, Section 7, for
alternative calibration standards are allowed for the post-test dry gas
meter calibration check.
5.2.3 Acceptable Variation in Calibration. If the dry gas meter
coefficient values obtained before and after a certification test differ
by more than 5 percent, the certification test shall either be voided
and repeated, or calculations for the certification test shall be
performed using whichever meter coefficient value (i.e., before or
after) gives the lower value of total sample volume.
5.3 Temperature Gauges. Use the procedure in Method 2, Section 4.3,
to calibrate temperature gauges before the first certification or audit
test and at least semiannually, thereafter.
5.4 Leak-Check of Metering System Shown in Figure 5G-1. That portion
of the sampling train from the pump to the orifice meter shall be
leak-checked prior to initial use and after each certification or audit
test. Leakage after the pump will result in less volume being recorded
than is actually sampled. Use the procedure described in Method 5,
Section 5.6.
Similar leak-checks shall be conducted for other types of metering
systems (i.e., without orifice meters).
5.5 Barometer. Calibrate against a mercury barometer before the first
certification test and at least semiannually, thereafter. If a mercury
barometer is used, no calibration is necessary. Follow the
manufacturer's instructions for operation.
5.6 Analytical Balance. Perform a multipoint calibration (at least
five points spanning the operational range) of the analytical balance
before the first certification test and semiannually, thereafter.
Before each certification test, audit the balance by weighing at least
one calibration weight (class F) that corresponds to 50 to 150 percent
of the weight of one filter. If the scale cannot reproduce the value of
the calibration weight to within 0.1 mg, conduct the multipoint
calibration before use.
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after the final
calculation. Other forms of the equations may be used as long as they
give equivalent results.
6.1 Nomenclature.
Bws=Water vapor in the gas stream, proportion by volume (assumed to
be 0.04).
cs=Concentration of particulate matter in stack gas, dry basis,
corrected to standard conditions, g/dsm /3/ (g/dscf).
E=Particulate emission rate, g/hr.
La=Maximum acceptable leakage rate for either a pretest or post-test
leak-check, equal to 0.00057 m /3/ /min (0.02 cfm) or 4 percent of the
average sampling rate, whichever is less.
Lp=Leakage rate observed during the post-test leak-check, m /3/ /min
(cfm).
ma=Mass of residue of acetone blank after evaporation, mg.
maw=Mass of residue from acetone wash after evaporation, mg.
mn=Total amount of particulate matter collected, mg.
Mw=Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb-mole).
Pbar=Barometric pressure at the sampling site, mm Hg (in. Hg).
PR=Percent of proportional sampling rate.
Ps=Absolute gas pressure in dilution tunnel, mm Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
Qsd=Average gas flow rate in dilution tunnel, calculated as in Method
2, Equation 2-10, dsm /3/ /hr (dscf/hr).
Tm=Absolute average dry gas meter temperature (see Figure 5G-3), oK
(oR).
Tmi=Absolute average dry gas meter temperature during each 10-minute
interval, i, of the test run, oK (oR).
Ts=Absolute average gas temperature in the dilution tunnel (see
Figure 5G 3), oK (oR).
Tsi=Absolute average gas temperature in the dilution tunnel during
each 10 minute interval, i, of the test run, oK (oR).
Tstd=Standard absolute temperature, 293 oK (528 oR).
Va=Volume of acetone blank, ml.
Vaw=Volume of acetone used in wash, ml.
Vm=Volume of gas sample as measured by dry gas meter, dm /3/ (dcf).
Vmi=Volume of gas sample as measured by dry gas meter during each
10-minute interval, i, of the test run, dm /3/ (dcf).
Vm(std)=Volume of gas sample measured by the dry gas meter, corrected
to standard conditions, dsm /3/ (dscf).
Vs=Average gas velocity in dilution tunnel, calculated by Method 2,
Equation 2-9, m/sec (ft/sec). The dilution tunnel dry gas molecular
weight may be assumed to be 29 g/g mole (lb/lb mole).
Vsi=Average gas velocity in dilution tunnel during each 10-minute
interval, i, of the test run, calculated by Method 2, Equation 2-9,
m/sec (ft/sec).
Y=Dry gas meter calibration factor.
DH=Average pressure differential across the orifice meter, if used
(see Figure 5G-2), mm H2O (in. H2O).
U=Total sampling time, min.
10=10 minutes, length of first sampling period.
13.6=Specific gravity of mercury.
100=Conversion to percent.
6.2 Dry Gas Volume. Correct the sample volume measured by the dry
gas meter to standard conditions (20 C, 760 mm Hg or 68 F, 29.92 in.
Hg) by using Equation 5G-1. (If no orifice meter is used in sampling
train, assume DH=O or measure static pressure at dry gas meter outlet.)
where;
Kl=0.3858 oK/mm Hg for metric units.
=17.64 oR/in. Hg for English units.
Note: If Lp exceeds La, Equation 5G-1 must be modified as
follows:Replace Vm in Equation 5G-1 with the expression:
(Vm^(Lp^La)U)
6.3 Solvent Wash Blank.
Eq. 5G-2
6.4 Total Particulate Weight. Determine the total particulate catch,
mn, from the sum of the weights obtained from Containers 1, 2, and 3,
less the acetone blank (see Figure 5G-4).
6.5 Particulate Concentration.
cs=(0.001 g/mg) (mn/Vm(std))
Eq. 5G-3
6.6 Particulate Emission Rate.
E=csQsd
Eq. 5G-4
Note: Particulate emission rate results produced using the sampling
train described in Section 2 and shown in Figure 5G-1 shall be adjusted
for reporting purposes by the following methods adjustment factor:
Eadj=1.82 (E)0.83
Eq. 5G-5
6.7 Proportional Rate Variation. Calculate PR for each 10-minute
interval, i, of the test run.
Eq. 5G-6
Alternate calculation procedures for proportional rate variation may
be used if other sample flow rate data (e.g., orifice flow meters or
rotameters) are monitored to maintain proportional sampling rates. The
proportional rate variations shall be calculated for each 10-minute
interval by comparing the stack to nozzle velocity ratio for each
10-minute interval to the average stack to nozzle velocity ratio for the
test run. Proportional rate variation may be calculated for intervals
shorter than 10 minutes with appropriate revisions to Equation 5G-6.
6.8 Acceptable Results. If no more than 10 percent of the PR values
for all the intervals exceed 90 percent >PR >110 percent, and if no PR
value for any interval exceeds 80 percent >PR >120 percent, the results
are acceptable. If the PR values for the test run are judged to be
unacceptable, report the test run emission results, but do not include
the results in calculating the weighted average emission rate, and
repeat the test run.
7.1 Method 5H Sampling Train. The sampling and analysis train and
procedures described in Method 5H, Sections 2.1, 3.1, 3.2, 5.1, 5.2.3,
5.3, and 5.6 may be used in lieu of similar sections in Method 5G.
Operation of the Method 5H sampling train in the dilution tunnel is as
described in Section 4.3.5 of this method. Filter temperatures and
condenser conditions are as described in Method 5H. No methods
adjustment factor as described in Equation 5G-5, Section 6.6, is to be
applied to the particulate emission rate data produced by this
alternative method.
7.2 Dual Sampling Trains. The tester may operate two sampling trains
simultaneously at sample flow rates other than that specified in Section
4.3.5 provided the following specifications are met.
7.2.1 Sampling Train. The sampling train configuration shall be the
same as specified in Section 2.1, except the probe, filter, and filter
holder need not be the same sizes as specified in the applicable
sections. Filter holders of plastic materials such as Nalgene or
polycarbonate materials may be used (the Gelman 1119 filter holder has
been found suitable for this purpose). With such materials, it is
recommended not to use solvents in sample recovery. The filter face
velocity shall not exceed 150 mm/sec (30 ft/min) during the test run.
The dry gas meter shall be calibrated for the same flow rate range as
encountered during the test runs. Two separate, complete sampling
trains are required for each test run.
7.2.2 Probe Location. Locate the two probes in the dilution tunnel
at the same level (see Section 2.2.3). Two sample ports are necessary.
Locate the probe inlets within the 50 mm (2 in.) diameter centroidal
area of the dilution tunnel no closer than 25 mm (1 in.) apart.
7.2.3 Sampling Train Operation. Operate the sampling trains as
specified in Section 4.3.5, maintaining proportional sampling rates and
starting and stopping the two sampling trains simultaneously. The pitot
values as described in Section 4.2.2 shall be used to adjust sampling
rates in both sampling trains.
7.2.4 Recovery and Analysis of Sample. Recover and analyze the
samples from the two sampling trains separately, as specified in
Sections 4.4 and 4.5.
For this alternative procedure, the probe and filter holder assembly
may be weighed without sample recovery (use no solvents) described above
in order to determine the sample weight gains. For this approach, weigh
the clean, dry probe and filter holder assembly upstream of the front
filter (without filters) to the nearest 0.1 mg to establish the tare
weights. The filter holder section between the front and second filter
need not be weighed. At the end of the test run, carefully clean the
outside of the probe, cap the ends, and identify the sample (label).
Remove the filters from the filter holder assemblies as described for
containers Nos. 1 and 2 above. Reassemble the filter holder assembly,
cap the ends, identify the sample (label), and transfer all the samples
to the laboratory weighing area for final weighing. Descriptions of
capping and transport of samples are not applicable if sample recovery
and analysis occur in the same room.
For this alternative procedure, filters may be weighed directly
without a petri dish. If the probe and filter holder assemb1y are to be
weighed to determine the sample weight, rinse the probe with acetone to
remove moisture before desiccating prior to the test run. Following the
test run, transport the probe and fi1ter ho1der to the dessicator, and
uncap the openings of the probe and the filter holder assembly.
Desiccate no more than 36 hours and weigh to a constant weight. Report
the results to the nearest 0.l mg.
7.2.5 Calculations. Calculate an emission rate (Section 6.6) for the
sample from each sampling train separately and determine the average
emission rate for the two values. The two emission rates shall not
differ by more than 7.5 percent from the average emission rate, or 7.5
percent of the weighted average emission rate limit in the applicable
standard, whichever is greater. If this specification is not met, the
results are unacceptable. Report the results, but do not include the
results in calculating the weighted average emission rate. Repeat the
test run until acceptable results are achieved, report the average
emission rate for the acceptable test run, and use the average in
calculating the weighted average emission rate.
1. Same as for Method 5, citations 1 through 11, with the addition of
the following:
2. Oregon Department of Environmental Quality Standard Method for
Measuring the Emissions and Efficiencies of Woodstoves, June 8, 1984.
Pursuant to Oregon Administrative Rules Chapter 340, Division 21.
3. American Society for Testing Materials. Proposed Test Methods for
Heating Performance and Emissions of Residential Wood-fired Closed
Combustion-Chamber Heating Appliances. E-6 Proposal P 180. August
1986.
Insert illus 0138
Insert illus 0139
Insert illus 0140
Stove
Date
Run No.
Filter Nos.
Liquid lost during
transport, ml
Acetone blank volume, ml
Acetone wash volume, ml
Acetone blank
concentration, mg/mg
Acetone wash blank, mg
Figure 5G-4. Analysis data sheet.
40 CFR 60.748 Pt. 60, App. A, Meth. 5H
1.1 Applicability. This method is applicable for the determination of
particulate matter and condensible emissions from wood heaters.
1.2 Principle. Particulate matter is withdrawn proportionally from
the wood heater exhaust and is collected on two glass fiber filters
separated by impingers immersed in an ice bath. The first filter is
maintained at a temperature of no greater than 120 C (248 F). The
second filter and the impinger system are cooled such that the exiting
temperature of the gas is no greater than 20 C (68 F). The
particulate mass collected in the probe, on the filters, and in the
impingers is determined gravimetrically after removal of uncombined
water.
2.1 Sampling Train. The sampling train configuration is shown in
Figure 5H-1. APTD-0576 is suggested for operating and maintenance
procedures. The train consists of the following components:
2.1.1 Probe Nozzle. (Optional) Same as Method 5, Section 2.1.1. A
straight sampling probe without a nozzle is an acceptable alternative.
2.1.2 Probe Liner. Same as Method 5, Section 2.1.2, except that the
maximum length of the sample probe shall be 0.6 m (2 ft) and probe
heating is optional.
2.1.3 Differential Pressure Gauge. Same as Method 5, Section 2.1.4.
2.1.4 Filter Holders. Two each of borosilicate glass, with a glass
frit or stainless steel filter support and a silicone rubber, Teflon, or
Viton gasket. The holder design shall provide a positive seal against
leakage from the outside or around the filter. The front filter holder
shall be attached immediately at the outlet of the probe and prior to
the first impinger. The second filter holder shall be attached on the
outlet of the third impinger and prior to the inlet of the fourth
(silica gel) impinger.
Note: Mention of trade names or specific product does not constitute
endorsement by the Environmental Protection Agency.
2.1.5 Filter Heating System. Same as Method 5, Section 2.1.6.
2.1.6 Condenser. Same as Method 5, Section 2.1.7, used to collect
condensible materials and determine the stack gas moisture content.
2.1.7 Metering System. Same as Method 5, Section 2.1.8.
2.1.8 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg).
2.2 Stack Flow Rate Measurement System. A schematic of an example
test system is shown in Figure 5H-2. The flow rate measurement system
consists of the following components:
2.2.1 Sample Probe. A glass or stainless steel sampling probe.
2.2.2 Gas Conditioning System. A high density filter to remove
particulate matter and a condenser capable of lowering the dew point of
the gas to less than 5 C (40 F). Desiccant, such as Drierite, may be
used to dry the sample gas. Do not use silica gel.
2.2.3 Pump. An inert (i.e., Teflon or stainless steel heads) sampling
pump capable of delivering more than the total amount of sample required
in the manufacturer's instructions for the individual instruments. A
means of controlling the analyzer flow rate and a device for determining
proper sample flow rate (e.g., precision rotameter, pressure gauge
downstream of all flow controls) shall be provided at the analyzer. The
requirements for measuring and controlling the analyzer flow rate are
not applicable if data are presented that demonstrate the analyzer is
insensitive to flow variations over the range encountered during the
test.
2.2.4 CO Analyzer. Any analyzer capable of providing a measure of CO
in the range of 0 to 10 percent by volume at least once every 10
minutes.
2.2.5 CO2 Analyzer. Any analyzer capable of providing a measure of
CO2 in the range of 0 to 25 percent by volume at least once every 10
minutes.
Note: Analyzers with ranges less than those specified above may be
used provided actual concentrations do not exceed the range of the
analyzer.
2.2.6 Manifold. A sampling tube capable of delivering the sample gas
to two analyzers and handling an excess of the total amount used by the
analyzers. The excess gas is exhausted through a separate port.
2.2.7 Recorders (optional). To provide a permanent record of the
analyzer outputs.
2.3 Proportional Gas Flow Rate System. To monitor stack flow rate
changes and provide a measurement that can be used to adjust and
maintain particulate sampling flow rates proportional to the stack flow
rate. A schematic of the proportional flow rate system is shown in
Figure 5H-2 and consists of the following components:
2.3.1 Tracer Gas Injection System. To inject a known concentration
of SO2 into the flue. The tracer gas injection system consists of a
cylinder of SO2, a gas cylinder regulator, a stainless steel needle
valve or flow controller, a nonreactive (stainless steel and glass)
rotameter, and an injection loop to disperse the SO2 evenly in the flue.
2.3.2 Sample Probe. A glass or stainless steel sampling probe.
2.3.3 Gas Conditioning System. A combustor as described in Method
16A, Sections 2.1.5 and 2.1.6, followed by a high density filter to
remove particulate matter, and a condenser capable of lowering the dew
point of the gas to less than 5 C (40 F). Desiccant, such as
Drierite, may be used to dry the sample gas. Do not use silica gel.
2.3.4 Pump. As described in Section 2.2.3.
2.3.5 SO2 Analyzer. Any analyzer capable of providing a measure of
the SO2 concentration in the range of 0 to 1,000 ppm by volume (or other
range necessary to measure the SO2 concentration) at least once every 10
minutes.
2.3.6 Recorder (optional). To provide a permanent record of the
analyzer outputs.
Note: Other tracer gas systems, including helium gas systems, are
allowed for determining instantaneous proportional sampling rates.
2.4 Sample Recovery. Probe liner and probe nozzle brushes, wash
bottles, sample storage containers, petri dishes, graduated cylinder or
balance, plastic storage containers, funnel and rubber policeman, as
described in Method 5, Sections 2.2.1 through 2.2.8, respectively, are
needed.
2.5 Analysis. Weighing dishes, desiccator, analytical balance,
beakers (250 ml or less), hygrometer or psychrometer, and temperature
gauge as described in Method 5, Sections 2.3.1 through 2.3.7,
respectively, are needed. In addition, a separatory funnel, glass or
Teflon, 500 ml or greater, is needed.
3.1 Sampling. The reagents used in sampling are as follows:
3.1.1 Filters. Glass fiber filters, without organic binder,
exhibiting at least 99.95 percent efficiency (<0.05 percent penetration)
on 0.3-micron dioctyl phthalate smoke particles. Gelman A/E 61631
filters have been found acceptable for this purpose.
3.1.2 Silica Gel. Same as Method 5, Section 3.1.2.
3.1.3 Water. Deionized distilled to conform to ASTM Specification
D1193-77, Type 3 (incorporated by reference -- see 60.17). Run blanks
prior to field use to eliminate a high blank on test samples.
3.1.4 Crushed Ice.
3.1.5 Stopcock Grease. Same as Method 5, Section 3.1.5.
3.2 Sample Recovery. Same as Method 5, Section 3.2.
3.3 Cylinder Gases. For the purposes of this procedure, span value
is defined as the upper limit of the range specified for each analyzer
as described in Section 2.2 or 2.3. If an analyzer with a range
different from that specified in this method is used, the span value
shall be equal to the upper limit of the range for the analyzer used
(see Note in Section 2.2.5).
3.3.1 Calibration Gases. The calibration gases for the CO2, CO and
SO2 analyzers shall be CO2, CO, or SO2, as appropriate, in N2. CO2 and
CO calibration gases may be combined in a single cylinder.
There are two alternatives for checking the concentrations of the
calibration gases. (a) The first is to use calibration gases that are
documented traceable to National Bureau of Standards Reference
Materials. Use Tracebility Protocol for Establishing True
Concentrations of Gases Used for Calibrations and Audits of Continuous
Source Emission Monitors (Protocol Number 1) that is available from the
Environmental Monitoring and Support Laboratory, Quality Assurance
Branch, Mail Drop 77, Environmental Protection Agency, Research Triangle
Park, North Carolina 27711. Obtain a certification from the gas
manufacturer that the protocol was followed. These calibration gases
are not to be analyzed with the test methods. (b) The second
alternative is to use calibration gases not prepared according to the
protocol. If this alternative is chosen, within 6 months prior to the
certification test, analyze each of the CO2 and CO calibration gas
mixtures in triplicate using Method 3, and within 1 month prior to the
certification test, analyze SO2 calibration gas mixtures using Method 6.
For the low-level, mid-level, or high-level gas mixtures, each of the
individual SO2 analytical results must be within 10 percent (or 10 ppm,
whichever is greater) of the triplicate set average; CO2 and CO test
results must be within 0.5 percent CO2 and CO; otherwise, discard the
entire set and repeat the triplicate analyses. If the average of the
triplicate test method results is within 5 percent for SO2 gas (or 0.5
percent CO2 and CO for the CO2 and CO gases) of the calibration gas
manufacturer's tag values, use the tag value; otherwise, conduct at
least three additional test method analyses until the results of six
individual SO2 runs (the three original plus three additional) agree
within 10 percent (or 10 ppm, whichever is greater) of the average (CO2
and CO test results must be within 0.5 percent). Then use this average
for the cylinder value. Four calibration gas levels are required as
specified below:
3.3.1.1 High-level Gas. A gas concentration that is equivalent to 80
to 90 percent of the span value.
3.3.1.2 Mid-level Gas. A gas concentration that is equivalent to 45
to 55 percent of the span value.
3.3.1.3 Low-level Gas. A gas concentration that is equivalent to 20
to 30 percent of the span value.
3.3.1.4 Zero Gas. A gas concentration of less than 0.25 percent of
the span value. Purified air may be used as zero gas for the CO2, CO,
and SO2 analyzers.
3.3.2 SO2 Injection Gas. A known concentration of SO2 in N2. The
concentration must be at least 2 percent SO2 with a maximum of 100
percent SO2. The cylinder concentration shall be certified by the
manufacturer to be within 2 percent of the specified concentration.
3.4 Analysis. Three reagents are required for the analysis:
3.4.1 Acetone. Same as 3.2.
3.4.2 Dichloromethane (Methylene Chloride). Reagent grade, <0.001
percent residue in glass bottles.
3.4.3 Desiccant. Anhydrous calcium sulfate, calcium chloride, or
silica gel, indicating type.
4.1 Response Time. The amount of time required for the measurement
system to display 95 percent of a step change in gas concentration. The
response time for each analyzer and gas conditioning system shall be no
more than 2 minutes.
4.2 Zero Drift. The zero drift value for each analyzer shall be less
than 2.5 percent of the span value over the period of the test run.
4.3 Calibration Drift. The calibration drift value measured with the
mid-level calibration gas for each analyzer shall be less than 2.5
percent of the span value over the period of the test run.
4.4 Resolution. The resolution of the output for each analyzer shall
be 0.5 percent of span value or less.
4.5 Calibration Error. The linear calibration curve produced using
the zero and mid-level calibration gases shall predict the actual
response to the low-level and high-level calibration gases within 2
percent of the span value.
5.1 Pretest Preparation.
5.1.1 Filter and Desiccant. Same as Method 5, Section 4.1.1.
5.1.2 Sampling Probe and Nozzle. The sampling location for the
particulate sampling probe shall be 2.45 0.15 m (8 0.5 ft) above the
platform upon which the wood heater is placed (i.e., the top of the
scale).
Select a nozzle, if used, sized for the range of velocity heads, such
that it is not necessary to change the nozzle size in order to maintain
proportional sampling rates. During the run, do not change the nozzle
size.
Select a suitable probe liner and probe length to effect minimum
blockage.
5.1.3 Preparation of Particulate Sampling Train. During preparation
and assembly of the particulate sampling train, keep all openings where
contamination can occur covered until just prior to assembly or until
sampling is about to begin.
Place 100 ml of water in each of the first two impingers, leave the
third impinger empty, and transfer approximately 200 to 300 g of
preweighed silica gel from its container to the fourth impinger. More
silica gel may be used, but care should be taken to ensure that it is
not entrained and carried out from the impinger during sampling. Place
the container in a clean place for later use in the sample recovery.
Alternatively, the weight of the silica gel plus impinger may be
determined to the nearest 0.5 g and recorded.
Using a tweezer or clean surgical gloves, place one labeled
(identified) and weighed filter in each of the filter holders. Be sure
that each of the filters is properly centered and the gasket properly
placed so as to prevent the sample gas stream from circumventing the
filter. Check the filters for tears after assembly is completed.
When glass liners are used, install the selected nozzle using a Viton
A O-ring. Other connecting systems using either 316 stainless steel or
Teflon ferrules may be used. Mark the probe with heat resistant tape or
by some other method to denote the proper distance into the stack or
duct.
Set up the train as in Figure 5H 1, using (if necessary) a very light
coat of silicone grease on all ground glass joints, greasing only the
outer portion (see APTD-0576) to avoid possibility of contamination by
the silicone grease.
Place crushed ice around the impingers.
5.1.4 Leak-Check Procedures.
5.1.4.1 Pretest Leak-Check. A pretest leak-check is recommended, but
not required. If the tester opts to conduct the pretest leak-check,
conduct the leak-check as described in Method 5, Section 4.1.4.1, except
that a vacuum of 130 mm Hg (5 in. Hg) may be used instead of 380 mm Hg
(15 in. Hg).
5.1.4.2 Leak-Checks During Sample Run. If, during the sampling run,
a component (e.g., filter assembly or impinger) change becomes
necessary, conduct a leak-check as described in Method 5, Section
4.1.4.2.
5.1.4.3 Post-Test Leak-Check. A leak-check is mandatory at the
conclusion of each sampling run. The leak-check shall be done in
accordance with the procedures described in Method 5, Section 4.1.4.3,
except that a vacuum of 130 mm Hg (5 in. Hg) or the greatest vacuum
measured during the test run, whichever is greater, may be used instead
of 380 mm Hg (15 in. Hg).
5.1.5 Tracer Gas Procedure. A schematic of the tracer gas injection
and sampling systems is shown in Figure 5H-2.
5.1.5.1 SO2 Injection Probe. Install the SO2 injection probe and
dispersion loop in the stack at a location 2.8 0.15 m (9.5 0.5 ft) above
the sampling platform.
5.1.5.2 SO2 Sampling Probe. Install the SO2 sampling probe at the
centroid of the stack at a location 4 0.15 m (13.5 0.5 ft) above the
sampling platform.
5.1.6 Flow Rate Measurement System. A schematic of the flow rate
measurement system is shown in Figure 5H-2. Locate the flow rate
measurement sampling probe at the centroid of the stack at a location
2.3 0.3 m (7.5 1 ft) above the sampling platform.
5.2 Test Run Procedures. The start of the test run is defined as in
Method 28, Section 6.4.1.
5.2.1 Tracer Gas Procedure. Within 1 minute after closing the wood
heater door at the start of the test run, meter a known concentration of
SO2 tracer gas at a constant flow rate into the wood heater stack.
Monitor the SO2 concentration in the stack, and record the SO2
concentrations at 10-minute intervals or more often at the option of the
tester. Adjust the particulate sampling flow rate proportionally to the
SO2 concentration changes using Equation 5H-6 (e.g., the SO2
concentration at the first 10-minute reading is measured to be 100 ppm;
the next 10 minute SO2 concentration is measured to be 75 ppm: the
particulate sample flow rate is adjusted from the initial 0.15 cfm to
0.20 cfm). A check for proportional rate variation shall be made at the
completion of the test run using Equation 5H-10.
5.2.2 Volumetric Flow Rate Procedure. Apply stoichiometric
relationships to the wood combustion process in determining the exhaust
gas flow rate as follows:
5.2.2.1 Test Fuel Charge Weight. Record the test fuel charge weight
in kilograms (wet) as specified in Method 28, Section 6.4.2. The wood
is assumed to have the following weight percent composition: 51 percent
carbon, 7.3 percent hydrogen, 41 percent oxygen. Record the wood
moisture for each wood charge as described in Method 28, Section 6.2.5.
The ash is assumed to have negligible effect on associated C, H, O
concentrations after the test burn.
5.2.2.2 Measured Values. Record the CO and CO2 concentrations in the
stack on a dry basis every 10 minutes during the test run or more often
at the option of the tester. Average these values for the test run.
Use as a mole fraction (e.g., 10 percent CO2 is recorded as 0.10) in the
calculations to express total flow Equation 5H-7.
5.2.3 Particulate Train Operation. For each run, record the data
required on a data sheet such as the one shown in Figure 5H-3. Be sure
to record the initial dry gas meter reading. Record the dry gas meter
readings at the beginning and end of each sampling time increment, when
changes in flow rates are made, before and after each leak-check, and
when sampling is halted. Take other readings as indicated on Figure
5H-3 at least once each 10 minutes during the test run.
Remove the nozzle cap, verify that the filter and probe heating
systems are up to temperature, and that the probe is properly
positioned. Position the nozzle, if used, facing into gas stream, or
the probe tip in the 50 mm (2 in.) centroidal area of the stack.
Be careful not to bump the probe tip into the stack wall when
removing or inserting the probe through the porthole; this minimizes
the chance of extracting deposited material.
When the probe is in position, block off the openings around the
probe and porthole to prevent unrepresentative dilution of the gas
stream.
Begin sampling at the start of the test run as defined in Method 28,
Section 6.4.1, start the sample pump, and adjust the sample flow rate to
between 0.003 and 0.015 m /3/ /min (0.1 and 0.5 cfm). Adjust the sample
flow rate proportionally to the stack flow during the test run (Section
5.2.1), and maintain a proportional sampling rate (within 10 percent of
the desired value) and a filter holder temperature no greater than 120
C (248 F).
During the test run, make periodic adjustments to keep the
temperature around the filter holder at the proper level. Add more ice
to the impinger box and, if necessary, salt to maintain a temperature of
less than 20 C (68 F) at the condenser/silica gel outlet.
If the pressure drop across the filter becomes too high, making
sampling difficult to maintain, either filter may be replaced during a
sample run. It is recommended that another complete filter assembly be
used rather than attempting to change the filter itself. Before a new
filter assembly is installed, conduct a leak-check (see Section
5.1.4.2). The total particulate weight shall include the summation of
all filter assembly catches. The total time for changing sample train
components shall not exceed 10 minutes. No more than one component
change is allowed for any test run.
At the end of the test run, turn off the coarse adjust valve, remove
the probe and nozzle from the stack, turn off the pump, record the final
dry gas meter reading, and conduct a post-test leak-check, as outlined
in Section 5.1.4.3.
5.3 Sample Recovery. Begin recovery of the probe and filter sample
as described in Method 5, Section 4.2, except that an acetone blank
volume of about 50 ml may be used. Treat the samples as follows:
Container No. 1. Carefully remove the filter from the front filter
holder and place it in its identified petri dish container. Use a pair
of tweezers and/or clean disposable surgical gloves to handle the
filter. If it is necessary to fold the filter, do so such that the
particulate cake is inside the fold. Carefully transfer to the petri
dish any particulate matter and/or filter fibers which adhere to the
filter holder gasket, by using a dry Nylon bristle brush and/or a
sharp-edged blade. Seal and label the container.
Container No. 2. Remove the filter from the back filter holder using
the same procedures as described above.
Container No. 3. Same as Method 5, Section 4.2 for Container No. 2.
except that descriptions of capping and sample transport are not
applicable if sample recovery and analysis occur in the same room.
Container No. 4. Treat the impingers as follows: Measure the liquid
which is in the first three impingers to within 1 ml by using a
graduated cylinder or by weighing it to within 0.5 g by using a balance
(if one is available). Record the volume or weight of liquid present.
This information is required to calculate the moisture content of the
effluent gas.
Transfer the water from the first, second and third impingers to a
glass container. Tighten the lid on the sample container so that water
will not leak out. Rinse impingers and graduated cylinder, if used,
with acetone three times or more. Avoid direct contact between the
acetone and any stopcock grease or collection of any stopcock grease in
the rinse solutions. Add these rinse solutions to sample Container No.
3.
Whenever possible, containers should be transferred in such a way
that they remain upright at all times. Descriptions of capping and
transport of samples are not applicable if sample recovery and analysis
occur in the same room.
Container No. 5. Transfer the silica gel from the fourth impinger to
its original container and seal. A funnel may make it easier to pour
the silica gel without spilling. A rubber policeman may be used as an
aid in removing the silica gel from the impinger. It is not necessary
to remove the small amount of dust particles that may adhere to the
impinger wall and are difficult to remove. Since the gain in weight is
to be used for moisture calculations, do not use any water or other
liquids to transfer the silica gel. If a balance is available, follow
the procedure for Container No. 5 in Section 5.4.
5.4 Analysis. Record the data required on a sheet such as the one
shown in Figure 5H-4. Handle each sample container as follows:
Containers No. 1 and 2. Leave the contents in the shipping
container or transfer both of the filters and any loose particulate from
the sample container to a tared glass weighing dish. Desiccate for no
more than 36 hours. Weigh to a constant weight and report the results
to the nearest 0.1 mg. For purposes of this Section, 5.6, the term
''constant weight'' means a difference of no more than 0.5 mg or 1
percent of total weight less tare weight, whichever is greater, between
two consecutive weighings, with no less than 2 hours between weighings.
Container No. 3. Note the level of liquid in the container and
confirm on the analysis sheet whether leakage occurred during transport.
If a noticeable amount of leakage has occurred, either void the sample
or use methods, subject to the approval of the Administrator, to correct
the final results. Determination of sample leakage is not applicable if
sample recovery and analysis occur in the same room. Measure the liquid
in this container either volumetrically to within 1 ml or
gravimetrically to within 0.5 g. Transfer the contents to a tared 250-ml
or smaller beaker, and evaporate to dryness at ambient temperature and
pressure. Desiccate and weigh to a constant weight. Report the results
to the nearest 0.1 mg.
Container No. 4. Note the level of liquid in the container and
confirm on the analysis sheet whether leakage occurred during transport.
If a noticeable amount of leakage has occurred, either void the sample
or use methods, subject to the approval of the Administrator, to correct
the final results. Determination of sample leakage is not applicable if
sample recovery and analysis occur in the same room. Measure the liquid
in this container either volumetrically to within 1 ml or
gravimetrically to within 0.5 g. Transfer the contents to a 500 ml or
larger separatory funnel. Rinse the container with water, and add to
the separatory funnel. Add 25 ml of dichloromethane to the separatory
funnel, stopper and vigorously shake 1 minute, let separate and transfer
the dichloromethane (lower layer) into a tared beaker or evaporating
dish. Repeat twice more. It is necessary to rinse the Container No. 4
with dichloromethane. This rinse is added to the impinger extract
container. Transfer the remaining water from the separatory funnel to a
tared beaker or evaporating dish and evaporate to dryness at 220 F (105
C). Desiccate and weigh to a constant weight. Evaporate the combined
impinger water extracts at ambient temperature and pressure. Desiccate
and weigh to a constant weight. Report both results to the nearest 0.1
mg.
Container No. 5. Weigh the spent silica gel (or silica gel plus
impinger) to the nearest 0.5 g using a balance.
''Acetone Blank'' Container. Measure acetone in this container
either volumetrically or gravimetrically. Transfer the acetone to a
tared 250-ml or smaller beaker, and evaporate to dryness at ambient
temperature and pressure. Desiccate and weigh to a constant weight.
Report the results to the nearest 0.1 mg.
''Dichloromethane'' Container. Measure 75 ml of dichloromethane in
this container and treat it the same as the ''acetone blank.''
''Water Blank'' Container. Measure 200 ml water into this container
either volumetrically or gravemetrically. Transfer the water to a tared
250-ml beaker and evaporate to dryness at 105 C (221 F). Desiccate
and weigh to a constant weight.
Maintain a laboratory record of all calibrations.
6.1 Volume Metering System.
6.1.1 Initial and Periodic Calibration. Before the first
certification or audit test and at least semiannually, thereafter,
calibrate the volume metering system as described in Method 5G, Section
5.2.1.
6.1.2 Calibration After Use. Same as Method 5G, Section 5.2.2.
6.1.3 Acceptable Variation in Calibration. Same as Method 5G,
Section 5.2.3.
6.2 Probe Heater Calibration. (Optional) The probe heating system
shall be calibrated before the first certification or audit test. Use
the procedure described in Method 5, Section 5.4.
6.3 Temperature Gauges. Use the procedure in Method 2, Section 4.3,
to calibrate in-stack temperature gauges before the first certification
or audit test and semiannually, thereafter.
6.4 Leak-Check of Metering System Shown in Figure 5H-1. That portion
of the sampling train from the pump to the orifice meter shall be
leak-checked after each certification or audit test. Use the procedure
described in Method 5, Section 5.6.
6.5 Barometer. Calibrate against a mercury barometer before the first
certification test and semiannually, thereafter. If a mercury barometer
is used, no calibration is necessary. Follow the manufacturer's
instructions for operation.
6.6 SO2 Injection Rotameter. Calibrate the SO2 injection rotameter
system with a soap film flowmeter or similar direct volume measuring
device with an accuracy of 2 percent. Operate the rotameter at a
single reading for at least three calibration runs for 10 minutes each.
When three consecutive calibration flow rates agree within 5 percent,
average the three flow rates, mark the rotameter at the calibrated
setting, and use the calibration flow rate as the SO2 injection flow
rate during the test run. Repeat the rotameter calibration before the
first certification test and semiannually, thereafter.
6.7 Analyzer Calibration Error Check. Conduct the analyzer
calibration error check prior to each certification test.
6.7.1 Calibration Gas Injection. After the flow rate measurement
system and the tracer gas measurement system have been prepared for use
(Sections 5.1.5.2 and 5.1.6), introduce zero gases and then the
mid-level calibration gases for each analyzer. Set the analyzers'
output responses to the appropriate levels. Then introduce the
low-level and high-level calibration gases, one at a time, for each
analyzer. Record the analyzer responses.
6.7.2 Acceptability Values. If the linear curve for any analyzer
determined from the zero and mid-level calibration gases' responses does
not predict the actual responses of the low-level and high-level gases
within 2 percent of the span value, the calibration of that analyzer
shall be considered invalid. Take corrective measures on the
measurement system before repeating the calibration error check and
proceeding with the test runs.
6.8 Measurement System Response Time. Introduce zero gas at the
calibration gas valve into the flow rate measurement system and the
tracer gas measurement system until all readings are stable. Then,
quickly switch to introduce the mid-level calibration gas at the
calibration value until a stable value is obtained. A stable value is
equivalent to a change of less than 1 percent of span value for 30
seconds. Record the response time. Repeat the procedure three times.
Conduct the response time check for each analyzer separately before its
initial use and at least semiannually thereafter.
6.9 Measurement System Drift Checks. Immediately prior to the start
of each test run (within 1 hour of the test run start), introduce zero
and mid-level calibration gases, one at a time, to each analyzer through
the calibration valve. Adjust the analyzers to respond appropriately.
Immediately following each test run (within 1 hour of the end of the
test run), or if adjustments to the analyzers or measurement systems are
required during the test run, reintroduce the zero- and mid-level
calibration gases and record the responses, as described above. Make no
adjustments to the analyzers or the measurement system until after the
drift checks are made.
If the difference between the analyzer responses and the known
calibration gas values exceed the specified limits (Sections 4.2 and
4.3), the test run will be considered invalid and shall be repeated
following corrections to the measurement system. Alternatively,
recalibrate the measurement system and recalculate the measurement data.
Report the test run results using both the initial and final
calibration data.
6.10 Analytical Balance. Perform a multipoint calibration (at least
five points spanning the operational range) of the analytical balance
before the first certification test and semiannually, thereafter.
Before each certification test, audit the balance by weighing at least
one calibration weight (class F) that corresponds to 50 to 150 percent
of the weight of one filter. If the scale cannot reproduce the value of
the calibration weight to within 0.1 mg, conduct the multipoint
calibration before use.
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after the final
calculation. Other forms of the equations may be used as long as they
give equivalent results.
7.1 Nomenclature.
a=Sample flow rate adjustment factor.
BR=dry wood burn rate, kg/hr (lb/hr), from Method 28, Section 8.3.
Bws=Water vapor in the gas stream, proportion by volume.
cs=Concentration of particulate matter in stack gas, dry basis,
corrected to standard conditions, g/dsm /3/ (g/dscf).
E=Particulate emission rate, g/hr.
DH=Average pressure differential across the orifice meter (see Figure
5H-1), mm H2O (in. H2O).
La=Maximum acceptable leakage rate for either a post-test leak check
or for a leak-check following a component change; equal to 0.00057 m
/3/ /min (0.02 cfm) or 4 percent of the average sampling rate, whichever
is less.
L1=Individual leakage rate observed during the leak-check conducted
before a component change, m /3/ /min (cfm).
Lp=Leakage rate observed during the post-test leak-check, m /3/ /min
(cfm).
mn=Total amount of particulate matter collected, mg.
ma=Mass of residue of solvent after evaporation, mg.
NC=Gram atoms of carbon/gram of dry fuel (lb/lb), equal to 0.0425.
NT=Total dry moles of exhaust gas/Kg of dry wood burned, g-moles/kg
(lb-moles/lb).
PR=Percent of proportional sampling rate.
Pbar=Barometric pressure at the sampling site, mm Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
Qsd=Total gas flow rate, dsm /3/ /hr (dscf/hr).
QT=Flow of tracer gas, liters/min.
Si=Concentration measured at the SO2 analyzer for the ''ith'' 10
minute interval, ppm.
S1=Concentration measured at the SO2 analyzer for the first 10-minute
interval, ppm.
T1=Absolute average stack gas temperature for the first 10-minute
interval, K ( R).
Ti=Absolute average stack gas temperature at the ''ith'' 10-minute
interval, K ( R).
Tm=Absolute average dry gas meter temperature (see Figure 5H-3), K (
R).
Tstd=Standard absolute temperature, 293 K (528 R).
Va=volume of solvent blank, ml.
Vaw=Volume of solvent used in wash, ml.
Vlc=Total volume of liquid collected in impingers and silica gel (see
Figure 5H-4), ml.
Vm=Volume of gas sample as measured by dry gas meter, dm /3/ (dcf).
Vm(std)=Volume of gas sample measured by the dry gas meter, corrected
to standard conditions, dsm /3/ (dscf).
Vml(std)=Volume of gas sample measured by the dry gas meter during
the first 10-minute interval, corrected to standard conditions, dsm /3/
(dscf).
Vmi(std)=Volume of gas sample measured by the dry gas meter during
the ''ith'' 10-minute interval, dsm /3/ (dscf).
Vw(std)=Volume of water vapor in the gas sample, corrected to
standard conditions, sm /3/ (scf).
Wa=Weight of residue in solvent wash, mg.
Y=Dry gas meter calibration factor.
YCO=Measured mole fraction of CO (dry), average from Section 5.2.2.2,
g/g-mole (lb/lb-mole).
YCO2=Measured mole fraction of CO2 (dry), average from Section
5.2.2.2, g/g-mole (lb/lb-mole).
YHC=Assumed mole fraction of HC (dry), g/g-mole (lb/lb-mole);
=0.0088 for catalytic wood heaters; =0.0132 for non-catalytic
wood heaters; =0.0080 for pellet-fired wood heaters.
10=Length of first sampling period, minutes.
13.6=Specific gravity of mercury.
100=Conversion to percent.
u=Total sampling time, min.
u1=Sampling time interval, from the beginning of a run until the
first component change, min.
7.2 Average dry gas meter temperature and average orifice pressure
drop. See data sheet (Figure 5H-3).
7.3 Dry Gas Volume. Correct the sample volume measured by the dry
gas meter to standard conditions (20 C, 760 mm Hg or 68 F, 29.92 in.
Hg) by using Equation 5H-1.
40 CFR 60.748
where;
K1=0.3858 0K/m. Hg for metric units.
=17.64 0R/in. Hg for English units.
Note: Equation 5H-1 can be used as written unless the leakage rate
observed during any of the mandatory leak-checks (i.e., the post-test
leak-check or leak-check conducted before a component change) exceeds
La.
If Lp exceeds La, Equation 5H-1 must be modified as follows:
(a) Case I. No component changes made during sampling run. In this
case, replace Vm in Equation 5H-1 with the expression:
(Vm^(Lp^La)u)
(b) Case II. One component change made during the sampling run. In
this case, replace Vm in Equation 5H-1 by the expression:
Vm^(L1^La)u1
and substitute only for those leakage rates (L1 or Lp) which exceed
La.
7.4 Volume of Water Vapor.
Vw(std)=K2Vlc Eq. 5H-2
where:
K2=0.001333 m /3/ /ml for metric units
=0.04707 ft /3/ /ml for English units.
7.5 Moisture Content.
7.6 Solvent Wash Blank.
7.7 Total Particulate Weight. Determine the total particulate catch
from the sum of the weights obtained from containers 1, 2, 3, and 4 less
the appropriate solvent blanks (see Figure 5H-4).
Note: Refer to Method 5, Section 4.1.5 to assist in calculation of
results involving two filter assemblies.
7.8 Particulate Concentration.
cs=(0.001 g/mg) (mn/Vm(std))
Eq. 5H-5
7.9 Sample Flow Rate Adjustment.
7.10 Carbon Balance for Total Moles of Exhaust Gas (dry)/Kg of Wood
Burned in the Exhaust Gas.
where:
K3=1000 g/kg for metric units.
K3=1.0 lb/lb for English units.
Note: The NOx/SOx portion of the gas is assumed to be negligible.
7.11 Total Stack Gas Flow Rate.
Qsd=K4 NT BR
Eq. 5H-8
where:
K4=0.02406 for metric units, dsm /3/ /g-mole.
=384.8 for English units, dscf/lb-mole.
7.12 Particulate Emission Rate.
E=csQsd
Eq. 5H-9
7.13 Proportional Rate Variation. Calculate PR for each 10-minute
interval, i, of the test run.
7.14 Acceptable Results. If no more than 15 percent of the PR values
for all the intervals exceed 90 percent > PR > 110 percent, and if no PR
value for any interval exceeds 75 > PR > 125 percent, the results are
acceptable. If the PR values for the test runs are judged to be
unacceptable, report the test run emission results, but do not include
the test run results in calculating the weighted average emission rate,
and repeat the test.
1. Same as for Method 5, citations 1 through 11, with the addition of
the following:
2. Oregon Department of Environmental Quality Standard Method for
Measuring the emissions and efficiencies of Woodstoves, July 8, 1984.
Pursuant to Oregon Administrative Rules Chapter 340, Division 21.
3. American Society for Testing Materials. Proposed Test Methods for
Heating Performance and Emissions of Residential Wood-fired Closed
Combustion-Chamber Heating Appliances. E-6 Proposal P 180. August
1986.
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40 CFR 60.748 Pt. 60, App. A, Meth. 6
1. Principle and Applicability
1.1 Principle. A gas sample is extracted from the sampling point in
the stack. The sulfuric acid mist (including sulfur trioxide) and the
sulfur dioxide are separated. The sulfur dioxide fraction is measured
by the barium-thorin titration method.
1.2 Applicability. This method is applicable for the determination of
sulfur dioxide emissions from stationary sources. The minimum
detectable limit of the method has been determined to be 3.4 milligrams
(mg) of SO2/m3 (2.12 10^7 lb/ft3). Although no upper limit has been
established, tests have shown that concentrations as high as 80,000
mg/m3 of SO2 can be collected efficiently in two midget impingers, each
containing 15 milliliters of 3 percent hydrogen peroxide, at a rate of
1.0 lpm for 20 minutes. Based on theoretical calculations, the upper
concentration limit in a 20-liter sample is about 93,300 mg/m3.
Possible interferents are free ammonia, water-soluble cations, and
fluorides. The cations and fluorides are removed by glass wool filters
and an isopropanol bubbler, and hence do not affect the SO2 analysis.
When samples are being taken from a gas stream with high concentrations
of very fine metallic fumes (such as in inlets to control devices), a
high-efficiency glass fiber filter must be used in place of the glass
wool plug (i.e., the one in the probe) to remove the cation
interferents.
Free ammonia interferes by reacting with SO2 to form particulate
sulfite and by reacting with the indicator. If free ammonia is present
(this can be determined by knowledge of the process and the presence of
white particulate matter in the probe and isopropanol bubbler), the
alternative procedures in Section 7.2 shall be used.
Insert illus. 246A
2. Apparatus
2.1 Sampling. The sampling train is shown in Figure 6-1, and
component parts are discussed below. The tester has the option of
substituting sampling equipment described in Method 8 in place of the
midget impinger equipment of Method 6. However, the Method 8 train must
be modified to include a heated filter between the probe and isopropanol
impinger, and the operation of the sampling train and sample analysis
must be at the flow rates and solution volumes defined in Method 8.
The tester also has the option of determining SO2 simultaneously with
particulate matter and moisture determinations by (1) replacing the
water in a Method 5 impinger system with 3 percent peroxide solution, or
(2) by replacing the Method 5 water impinger system with a Method 8
isopropanol-filter-peroxide system. The analysis for SO2 must be
consistent with the procedure in Method 8.
2.1.1 Probe. Borosilicate glass, or stainless steel (other materials
of construction may be used, subject to the approval of the
Administrator), approximately 6-mm inside diameter, with a heating
system to prevent water condensation and a filter (either in-stack or
heated out-stack) to remove particulate matter, including sulfuric acid
mist. A plug of glass wool is a satisfactory filter.
2.1.2 Bubbler and Impingers. One midget bubbler, with medium-coarse
glass frit and borosilicate or quartz glass wool packed in top (see
Figure 6-1) to prevent sulfuric acid mist carryover, and three 30-ml
midget impingers. The bubbler and midget impingers must be connected in
series with leak-free glass connectors. silicone grease may be used, if
necessary, to prevent leakage.
At the option of the tester, a midget impinger may be used in place
of the midget bubbler.
Other collection absorbers and flow rates may be used, but are
subject to the approval of the Administrator. Also, collection
efficiency must be shown to be at least 99 percent for each test run and
must be documented in the report. If the efficiency is found to be
acceptable after a series of three tests, further documentation is not
required. To conduct the efficiency test, an extra absorber must be
added and analyzed separately. This extra absorber must not contain
more than 1 percent of the total SO2.
2.1.3 Glass Wool. Borosilicate or quartz.
2.1.4 Stopcock Grease. Acetone-insoluble, heatstable silicone grease
may be used, if necessary.
2.1.5 Temperature Gauge. Dial thermometer, or equivalent, to measure
temperature of gas leaving impinger train to within 1 C (2 F.)
2.1.6 Drying Tube. Tube packed with 6- to 16-mesh indicating type
silica gel, or equivalent, to dry the gas sample and to protect the
meter and pump. If the silica gel has been used previously, dry at 175
C (350 F) for 2 hours. New silica gel may be used as received.
Alternatively, other types of desiccants (equivalent or better) may be
used, subject to approval of the Administrator.
2.1.7 Valve. Needle valve, to regulate sample gas flow rate.
2.1.8 Pump. Leak-free diaphragm pump, or equivalent, to pull gas
through the train. Install a small surge tank between the pump and rate
meter to eliminate the pulsation effect of the diaphragm pump on the
rotameter.
2.1.9. Rate Meter. Rotameter, or equivalent, capable of measuring
flow rate to within 2 percent of the selected flow rate of about 1000
cc/min.
2.1.10 Volume Meter. Dry gas meter, sufficiently accurate to measure
the sample volume within 2 percent, calibrated at the selected flow rate
and conditions actually encountered during sampling, and equipped with a
temperature gauge (dial thermometer, or equivalent) capable of measuring
temperature to within 3 C (5.4 F).
2.1.11 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg). In many
cases, the barometric reading may be obtained from a nearby National
Weather Service station, in which case the station value (which is the
absolute barometric pressure) shall be requested and an adjustment for
elevation differences between the weather station and sampling point
shall be applied at a rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 m
(100 ft) elevation increase or vice versa for elevation decrease.
2.1.12 Vacuum Gauge and Rotameter. At least 760 mm Hg (30 in. Hg)
gauge and 0-40 cc/min rotameter, to be used for leak check of the
sampling train.
2.2 Sample Recovery.
2.2.1 Wash Bottles. Polyethylene or glass, 500 ml, two.
2.2.2 Storage Bottles. Polyethylene, 100 ml, to store impinger
samples (one per sample).
2.3 Analysis.
2.3.1 Pipettes. Volumetric type, 5-ml, 20-ml (one per sample), and
25-ml sizes.
2.3.2 Volumetric Flasks. 100-ml size (one per sample) and 1000 ml
size.
2.3.3 Burettes. 5- and 50-ml sizes.
2.3.4 Erlenmeyer Flasks. 250 ml-size (one for each sample, blank,
and standard).
2.3.5 Dropping Bottle. 125-ml size, to add indicator.
2.3.6 Graduated Cylinder. 100-ml size.
2.3.7 Spectrophotometer. To measure absorbance at 352 nanometers.
3. Reagents
Unless otherwise indicated, all reagents must conform to the
specifications established by the Committee on Analytical Reagents of
the American Chemical Society. Where such specifications are not
available, use the best available grade.
3.1 Sampling.
3.1.1 Water. Deionized distilled to conform to ASTM Specification
D1193-77, Type 3 (incorporated by reference -- see 60.17). At the
option of the analyst, the KMnO4 test for oxidizable organic matter may
be omitted when high concentrations of organic matter are not expected
to be present. Unless otherwise specified, this water shall be used
throughout this method.
3.1.2 Isopropanol, 80 percent. Mix 80 ml of isopropanol with 20 ml
of water. Check each lot of isopropanol for peroxide impurities as
follows: shake 10 ml of isopropanol with 10 ml of freshly prepared 10
percent potassium iodide solution. Prepare a blank by similarly
treating 10 ml of water. After 1 minute, read the absorbance at 352
nanometers on a spectrophotometer. If absorbance exceeds 0.1, reject
alcohol for use.
Peroxides may be removed from isopropanol by redistilling or by
passage through a column of activated alumina; however, reagent grade
isopropanol with suitably low peroxide levels may be obtained from
commercial sources. Rejection of contaminated lots may, therefore, be a
more efficient procedure.
3.1.3 Hydrogen Peroxide, 3 Percent. Dilute 30 percent hydrogen
peroxide 1:9 (v/v) with water (30 ml is needed per sample). Prepare
fresh daily.
3.1.4 Potassium Iodide Solution, 10 Percent. Dissolve 10.0 grams KI
in water and dilute to 100 ml. Prepare when needed.
3.2 Sample Recovery.
3.2.1 Water. Same as in Section 3.1.1.
3.2.2 Isopropanol, 80 Percent. Mix 80 ml of isopropanol with 20 ml
of water.
3.3 Analysis.
3.3.1 Water. Same as in Section 3.1.1.
3.3.2 Isopropanol, 100 Percent.
3.3.3 Thorin Indicator.
1-(o-arsonophenylazo)-2-naphthol-3,6-disfonic acid, disodium salt, or
equivalent. Dissolve 0.20 g in 100 ml of water.
3.3.4 Barium Perchlorate Solution, 0.0100 N. Dissolve 1.95 g of
barium perchlorate trihydrate (Ba(ClO4)2 3H2O) in 200 ml water and
dilute to 1 liter with isopropanol. Alternatively, 1.22 g of (BaCl2
2H2O) may be used instead of the perchlorate. Standardize as in Section
5.5.
3.3.5 Sulfuric Acid Standard, 0.0100 N. Purchase or standardize to
0.0002 N against 0.0100 N NaOH which has previously been standardized
against potassium acid phthalate (primary standard grade).
3.3.6 Quality Assurance Audit Samples. Sulfate samples in glass
vials prepared by EPA's Environmental Monitoring Systems Laboratory,
Quality Assurance Division, Source Branch, Mail Drop 77A, Research
Triangle Park, North Carolina 27711. Each set will consist of two vials
having solutions of unknown concentrations. Only when making compliance
determinations, obtain an audit sample set from the Quality Assurance
Management office at each EPA regional Office or the responsible
enforcement agency. (Note: The tester should notify the quality
assurance office or the responsible enforcement agency at least 30 days
prior to the test date to allow sufficient time for sample delivery.)
3.3.7 Hydrochloric Acid (HCl) Solution, 0.1 N (for use in Section
7.2). Carefully pipette 8.6 ml of concentrated HCl into a 1-liter
volumetric flask containing water. Dilute to volume with mixing.
4. Procedure
4.1 Sampling.
4.1.1 Preparation of Collection Train. Measure 15 ml of 80 percent
isopropanol into the midget bubbler and 15 ml of 3 percent hydrogen
peroxide into each of the first two midget impingers. Leave the final
midget impinger dry. Assemble the train as shown in Figure 6-1. Adjust
probe heater to a temperature sufficient to prevent water condensation.
Place crushed ice and water around the impingers.
4.1.2 Leak-Check Procedure. A leak check prior to the sampling run
is optional; however, a leak check after the sampling run is mandatory.
The leak-check procedure is as follows:
Temporarily attach a suitable (e.g., 0-40 cc/min) rotameter to the
outlet of the dry gas meter and place a vacuum gauge at or near the
probe inlet. Plug the probe inlet, pull a vaccum of at least 250 mm Hg
(10 in. Hg), and note the flow rate as indicated by the rotameter. A
leakage rate not in excess of 2 percent of the average sampling rate is
acceptable.
Note: Carefully release the probe inlet plug before turning off the
pump.
It is suggested (not mandatory) that the pump be leak-checked
separately, either prior to or after the sampling run. If done prior to
the sampling run, the pump leak-check shall precede the leak check of
the sampling train described immediately above; if done after the
sampling run, the pump leak-check shall follow the train leak-check. To
leak check the pump, proceed as follows: Disconnect the drying tube
from the probe-impinger assembly. Place a vacuum gauge at the inlet to
either the drying tube or the pump, pull a vacuum of 250 mm (10 in.) Hg,
plug or pinch off the outlet of the flow meter and then turn off the
pump. The vacuum should remain stable for at least 30 seconds.
Other leak-check procedures may be used, subject to the approval of
the Adminstrator, U.S. Environmental Protection Agency.
4.1.3 Sample Collection. Record the initial dry gas meter reading
and barometric pressure. To begin sampling, position the tip of the
probe at the sampling point, connect the probe to the bubbler, and start
the pump. Adjust the sample flow to a constant rate of approximately
1.0 liter/min as indicated by the rotameter. Maintain this constant
rate ( 10 percent) during the entire sampling run. Take readings (dry
gas meter, temperatures at dry gas meter and at impinger outlet, and
rate meter) at least every 5 minutes. Add more ice during the run to
keep the temperature of the gases leaving the last impinger at 20 C (68
F) or less. At the conclusion of each run, turn off the pump, remove
probe from the stack, and record the final readings. Conduct a leak
check as in Section 4.1.2 (This leak check is mandatory.) If a leak is
found, void the test run, or use procedures acceptable to the
Administrator to adjust the sample volume for the leakage. Drain the
ice bath, and purge the remaining part of the train by drawing clean
ambient air through the system for 15 minutes at the sampling rate.
Clean ambient air can be provided by passing air through a charcoal
filter or through an extra midget impinger with 15 ml of 3 percent H2O2.
The tester may opt to simply use ambient air, without purification.
4.2 Sample Recovery. Disconnect the impingers after purging.
Discard the contents of the midget bubbler. Pour the contents of the
midget impingers into a leak-free polyethylene bottle for shipment.
Rinse the three midget impingers and the connecting tubes with water,
and add the washings to the same storage container. Mark the fluid
level. Seal and identify the sample container.
4.3 Sample Analysis. Note level of liquid in container, and confirm
whether any sample was lost during shipment; note this on analytical
data sheet. If a noticeable amount of leakage has occurred, either void
the sample or use methods, subject to the approval of the Administrator,
to correct the final results.
Transfer the contents of the storage container to a 100-ml volumetric
flask and dilute to exactly 100 ml with water. Pipette a 20-ml aliquot
of this solution into a 250-ml Erlenmeyer flask, add 80 ml of 100
percent isopropanol and two to four drops of thorin indicator, and
titrate to a pink endpoint using 0.0100 N barium perchlorate. Repeat
and average the titration volumes. Run a blank with each series of
samples. Replicate titrations must agree within 1 percent or 0.2 ml,
whichever is larger.
Note: Protect the 0.0100 N barium perchlorate solution from
evaporation at all times.
4.4 Audit Sample Analysis. Concurrently analyze the two audit
samples and a set of compliance samples (Section 4.3) in the same manner
to evaluate the technique of the analyst and the standards preparation.
(Note: It is recommended that known quality control samples be analyzed
prior to the compliance and audit sample analysis to optimize the system
accuracy and precision. One source of these samples is the Source Branch
listed in Section 3.3.6.) The same analysts, analytical reagents, and
analytical system shall be used both for compliance samples and the EPA
audit samples; if this condition is met, auditing of subsequent
compliance analyses for the same enforcement agency within 30 days is
not required. An audit sample set may not be used to validate different
sets of compliance samples under the jurisdiction of different
enforcement agencies, unless prior arrangements are made with both
enforcement agencies.
Calculate the concentrations in mg/dscm using the specified sample
volume in the audit instructions. (Note: Indication of acceptable
results may be obtained immediately by reporting the audit results in
mg/dscm and compliance results in total mg SO2/sample by telephone to
the responsible enforcement agency.) Include the results of both audit
samples, their identification numbers, and the analyst's name with the
results of the compliance determination samples in appropriate reports
to the EPA regional office or the appropriate enforcement agency.
Include this information with subsequent compliance analyses for the
same enforcement agency during the 30-day period.
The concentrations of the audit samples obtained by the analyst shall
agree within 5 percent of the actual concentrations. If the 5-percent
specification is not met, reanalyze the compliance samples and audit
samples, and include initial and reanalysis values in the test report
(see Note in first paragraph of this section).
Failure to meet the 5-percent specification may require retests until
the audit problems are resolved. However, if the audit results do not
affect the compliance or noncompliance status of the affected facility,
the Administrator may waive the reanalysis requirement, further audits,
or retests and accept the results of the compliance test. While steps
are being taken to resolve audit analysis problems, the Administrator
may also choose to use the data to determine the compliance or
noncompliance status of the affected facility.
5. Calibration
5.1 Metering System.
5.1.1 Initial Calibration. Before its initial use in the field,
first leak check the metering system (drying tube, needle valve, pump,
rotameter, and dry gas meter) as follows: place a vacuum gauge at the
inlet to the drying tube and pull a vaccum of 250 mm (10 in.) Hg; plug
or pinch off the outlet of the flow meter, and then turn off the pump.
The vaccum shall remain stable for at least 30 seconds. Carefully
release the vaccum gauge before releasing the flow meter end.
Next, remove the drying tube and calibrate the metering system (at
the sampling flow rate specified by the method) as follows: connect an
appropriately sized wet test meter (e.g., 1 liter per revolution) to the
inlet of the drying tube. Make three independent calibration runs,
using at least five revolutions of the dry gas meter per run. Calculate
the calibration factor, Y (wet test meter calibration volume divided by
the dry gas meter volume, both volumes adjusted to the same reference
temperature and pressure), for each run, and average the results. If
any Y value deviates by more than 2 percent from the average, the
metering system is unacceptable for use. Otherwise, use the average as
the calibration factor for subsequent test runs.
5.1.2 Post-Test Calibration Check. After each field test series,
conduct a calibration check as in Section 5.1.1 above, except for the
following variations: (a) the leak check is not to be conducted, (b)
three, or more revolutions of the dry gas meter may be used, and (c)
only two independent runs need be made. If the calibration factor does
not deviate by more than 5 percent from the initial calibration factor
(determined in Section 5.1.1), then the dry gas meter volumes obtained
during the test series are acceptable. If the calibration factor
deviates by more than 5 percent, recalibrate the metering system as in
Section 5.1.1, and for the calculations, use the calibration factor
(initial or recalibration) that yields the lower gas volume for each
test run.
5.2 Thermometers. Calibrate against mercury-in-glass thermometers.
5.3 Rotameter. The rotameter need not be calibrated but should be
cleaned and maintained according to the manufactuturer's instruction.
5.4 Barometer. Calibrate against a mercury barometer.
5.5 Barium Perchlorate Solution. Standardize the barium perchlorate
solution against 25 ml of standard sulfuric acid to which 100 ml of 100
percent isopropanol has been added.
Run duplicate analyses. Calculate the normality using the average of
a pair of duplicate analyses where the titrations agree within 1 percent
or 0.2 ml, whichever is larger.
6. Calculations
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after final
calculation.
6.1 Nomenclature.
Cso2=Concentration of sulfur dioxide, dry basis corrected to standard
conditions, mg/dscm (lb/dscf).
N=Normality of barium perchlorate titrant, milliequivalents/ml.
Pbar=Barometric pressure at the exit orifice of the dry gas meter, mm
Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
Tm=Average dry gas meter absolute temperature, K ( R).
Tstd=Standard absolute temperature, 293 K (528 R).
Va=Volume of sample aliquot titrated, ml.
Vm=Dry gas volume as measured by the dry gas meter, dcm (dcf).
Vm(std)=Dry gas volume measured by the dry gas meter, corrected to
standard conditions, dscm (dscf).
Vsoln=Total volume of solution in which the sulfur dioxide sample is
contained, 100 ml.
Vt=Volume of barium perchlorate titrant used for the sample, ml
(average or replicate titrations).
Vtb=Volume of barium perchlorate titrant used for the blank, ml.
Y=Dry gas meter calibration factor.
32.03=Equivalent weight of sulfur dioxide.
6.2 Dry Sample Gas Volume, Corrected to Standard Conditions.
Insert illus. 247A
Where:
K1=0.3858 K/mm Hg for metric units.
=17.64 R/in. Hg for English units.
6.3 Sulfur Dioxide Concentration.
Insert illus. 248A
Where:
K3=32.03 mg/meq. for metric units.
=7.061 10^5 lb/meq. for English units.
6.4 Relative Error (RE) for QA Audit Samples, Percent.
Where:
Cd=Determined audit sample concentration, mg/dscm.
Ca=Actual audit sample concentration, mg/dscm.
7. Alternative Procedures
7.1 Dry Gas Meter as a Calibration Standard. A dry gas meter may be
used as a calibration standard for volume measurements in place of the
wet test meter specified in Section 5.1, provided that it is calibrated
initially and recalibrated periodically according to the same procedures
outlined in Method 5, Section 7.1, with the following exception: (1)
the dry gas meter is calibrated against a wet test meter having a
capacity of 1 liter/rev or 3 liters/rev and having the capability of
measuring volume to within 1 percent; (2) the dry gas meter is
calibrated at 1 liter/min (2 cfh); and (3) the meter box of the Method
6 sampling train is calibrated at the same flow rate.
7.2 Critical Orifices for Volume and Rate Measurements. A critical
orifice may be used in place of the dry gas meter specified in Section
2.1.10, provided that it is selected, calibrated, and used as follows:
7.2.1 Preparation of Collection Train. Prepare the sampling train as
shown in Figure 6-2. The rotameter and surge tank are optional but are
recommended in order to detect changes in the flow rate.
Note: The critical orifices can be adapted to a Method 6 type
sampling train as follows: Insert sleeve type, serum bottle stoppers
into two reducing unions. Insert the needle into the stoppers as shown
in Figure 6-3.
Insert illus. 0 583
Insert illus. 0 584
7.2.2 Selection of Critical Orifices. The procedure that follows
describes the use of hypodermic needles and stainless steel needle
tubings, which have been found suitable for use as critical orifices.
Other materials and critical orifice designs may be used provided the
orifices act as true critical orifices, i.e., a critical vacuum can be
obtained, as described in this section. Select a critical orifice that
is sized to operate at the desired flow rate. The needle sizes and
tubing lengths shown below give the following approximate flow rates.
Determine the suitability and the appropriate operating vaccum of the
critical orifice as follows: If applicable, temporarily attach a
rotameter and surge tank to the outlet of the sampling train. Turn on
the pump, and adjust the valve to give an outlet vacuum reading
corresponding to about half of the atmospheric pressure. Observe the
rotameter reading. Slowly increase the vacuum until a stable reading is
obtained on the rotameter. Record the critical vacuum, which is the
outlet vacuum when the rotameter first reaches a stable value. Orifices
that do not reach a critical value shall not be used.
7.2.3 Field Procedure.
7.2.3.1 Leak-Check Procedure. A leak-check before the sampling run
is recommended, but is optional. The leak-check procedure is as
follows:
Temporarily attach a suitable (e.g., 0-40 cc/min) rotameter and surge
tank, or a soap bubble meter and surge tank to the outlet of the pump.
Plug the probe inlet, pull an outlet vacuum of at least 254 mm Hg (10
in. Hg), and note the flow rate as indicated by the rotameter or bubble
meter. A leakage rate not in excess of 2 percent of the average
sampling rate (Q8std) is acceptable. Carefully release the probe inlet
plug before turning off the pump.
7.2.3.2 Moisture Determination. At the sampling location, prior to
testing, determine the percent moisture of the ambient air using the wet
and dry bulb temperatures or, if appropriate, a relative-humidity meter.
7.2.3.3 Critical Orifice Calibration. Prior to testing, at the
sampling location, calibrate the entire sampling train using a 500-cc
soap bubble meter which is attached to the inlet of the probe and an
outlet vacuum of 25 to 50 mm Hg (1 to 2 in. Hg) above the critical
vacuum. Record the information listed in Figure 6-4.
Calculate the standard volume of air measured by the soap bubble
meter and the volumetric flow rate, using the equations below:
insert illus. 0587
where:
Pbar=Barometric pressure, mm Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
Qstd=Volumetric flow rate through critical orifice, scm/min
(scf/min).
Tamb=Ambient absolute temperature of air, K ( R).
Tstd=Standard absolute temperature, 273 K (528 R).
Vsb=Volume of gas as measured by the soap bubble meter, m3 (ft3).
Vsb(std)=Volume of gas as measured by the soap bubble meter,
corrected to standard conditions, scm (scf).
U=Time, min.
insert illus 0588
7.2.3.4 Sampling. Operate the sampling train for sample collection at
the same vacuum used during the calibration run. Start the watch and
pump simultaneously. Take readings (temperature, rate meter, inlet
vacuum, and outlet vacuum) at least every 5 minutes. At the end of the
sampling run, stop the watch and pump simultaneously.
Conduct a post-test calibration run using the calibration procedure
outlined in Section 7.2.3.3. If the Qstd obtained before and after the
test differ by more than 5 pecent, void the test run; if not, calculate
the volume of the gas measured with the critical orifice, Vm(std), using
Equation 6-6 and the average of Qstd of both runs, as follows:
insert illus 0589
where:
Vm(std)=Dry gas volume measured with the critical orifice, corrected
to standard conditions, dscm (dscf).
Qstd=Average flow rate of pretest and post-test calibration runs,
scm/min (scf/min).
Bwa=Water vapor in ambient air, proportion by volume.
us=Sampling time, min.
Pc=Inlet vacuum reading obtained during the calibration run, mm Hg
(in. Hg).
Psr=Inlet vacuum reading obtained during the sampling run, mm Hg (in.
Hg).
If the percent difference between the molecular weight of the ambient
air at saturated conditions and the sample gas is more than 3 percent,
then the molecular weight of the gas sample must be considered in the
calculations using the following equation:
insert illus 0590
where:
Ma=Molecular weight of the ambient air saturated at impinger
temperature, g/g-mole (lb/lb-mole).
Ms=Molecular weight of the sample gas saturated at impinger
temperature, g/g-mole (lb/lb-mole).
Note: A post-test leak-check is not necessary because the post-test
calibration run results will indicate whether there is any leakage.
Drain the ice bath, and purge the sampling train using the procedure
described in Section 4.1.3.
7.3 Elimination of Ammonia Interference. The following alternative
procedures shall be used in addition to those specified in the method
when sampling at sources having ammonia emissions.
7.3.1 Sampling. The probe shall be maintained at 275 C and equipped
with a high-efficiency in-stack filter (glass fiber) to remove
particulate matter. The filter material shall be unreactive to SO2.
Whatman 934AH (formerly Reeve Angel 934AH) filters treated as described
in Citation 10 of the Method 5 bibliography is an example of a filter
that has been shown to work. Where alkaline particulate matter and
condensed moisture are present in the gas stream, the filter shall be
heated above the moisture dew point but below 225 C.
7.3.2 Sample Recovery. Recover the sample according to Section 4.2
except for discarding the contents of the midget bubbler. Add the
bubbler contents, including the rinsings of the bubbler with water, to
the polyethylene bottle containing the rest of the sample. Under normal
testing conditions where sulfur trioxide will not be present
significantly, the tester may opt to delete the midget bubbler from the
sampling train. If an approximation of the sulfur trioxide
concentration is desired, transfer the contents of the midget bubbler to
a separate polyethylene bottle.
7.3.3 Sample Analysis. Follow the procedures in Section 4.3, except
add 0.5 ml of 0.1 N HC1 to the Erlenmeyer flask and mix before adding
the indicator. The following analysis procedure may be used for an
approximation of the sulfur trioxide concentration. The accuracy of the
calculated concentration will depend upon the ammonia to SO2 ratio and
the level of oxygen present in the gas stream. A fraction of the SO2
will be counted as sulfur trioxide as the ammonia to SO2 ratio and the
sample oxygen content increases. Generally, when this ratio is 1 or
less and the oxygen content is in the range of 5 percent, less than 10
percent of the SO2 will be counted as sulfur trioxide. Analyze the
peroxide and isopropanol sample portions separately. Analyze the
peroxide portion as described above. Sulfur trioxide is determined by
difference using sequential titration of the isopropanol portion of the
sample. Transfer the contents of the isopropanol storage container to a
100-ml volumetric flask, and dilute to exactly 100 ml with water.
Pipette a 20-ml aliquot of this solution into a 250-ml Erlenmeyer flask,
add 0.5 ml of 0.1 N HC1, 80 ml of 100 percent isopropanol, and two to
four drops of thorin indicator. Titrate to a pink endpoint using 0.0100
N barium perchlorate. Repeat and average the titration volumes that
agree within 1 percent or 0.2 ml, whichever is larger. Use this volume
in Equation 6-2 to determine the sulfur trioxide concentration. From
the flask containing the remainder of the isopropanol sample, determine
the fraction of SO2 collected in the bubbler by pipetting 20-ml aliquots
into 250-ml Erlenmeyer flasks. Add 5 ml of 3 percent hydrogen peroxide,
100 ml of 100 percent isopropanol, and two to four drops of thorin
indicator, and titrate as before. From this titration volume, subtract
the titrant volume determined for sulfur trioxide, and add the titrant
volume determined for the peroxide portion. This final volume
constitutes Vt, the volume of barium perchlorate used for the SO2
sample.
8. Bibliography
1. Atmospheric Emissions from Sulfuric Acid Manufacturing Processes.
U.S. DHEW, PHS, Division of Air Pollution. Public Health Service
Publication No. 999-AP-13. Cincinnati, OH. 1965.
2. Corbett, P. F. The Determination of SO2 and SO3 in Flue Gases.
Journal of the Institute of Fuel. 24: 237-243, 1961.
3. Matty, R. E. and E. K. Diehl. Measuring Flue-Gas SO2 and SO3.
Power. 101: 94-97. November 1957.
4. Patton, W. F. and J. A. Brink, Jr. New Equipment and Techniques
for Sampling Chemical Process Gases. J. Air Pollution Control
Association. 13: 162. 1963.
5. Rom, J. J. Maintenance, Calibration, and Operation of Isokinetic
Source-sampling Equipment. Office of Air Programs, Environmental
Protection Agency. Research Triangle Park, NC. APTD-0576. March 1972.
6. Hamil, H. F. and D. E. Camann. Collaborative Study of Method for
the Determination of Sulfur Dioxide Emissions from Stationary Sources
(Fossil-Fuel Fired Steam Generators). Environmental Protection Agency,
Research Triangle Park, NC. EPA-650/4-74-024. December 1973.
7. Annual Book of ASTM Standards. Part 31; Water, Atmospheric
Analysis. American Society for Testing and Materials. Philadelphia,
PA. 1974. pp. 40-42.
8. Knoll, J. E. and M. R. Midgett. The Application of EPA Method 6
to High Sulfur Dioxide Concentrations. Environmental Protection Agency.
Research Triangle Park, NC. EPA-600/4-76-038. July 1976.
9. Westlin, P. R. and R. T. Shigehara. Procedure for Calibrating
and Using Dry Gas Meter Volume Meters as Calibration Standards. Source
Evaluation Society Newsletter. 3(1):17-30. February 1978.
10. Yu, K. K. Evaluation of Moisture Effect on Dry Gas Meter
Calibration. Source Evaluation Society Newsletter. 5(1):24-28.
February 1980.
11. Lodge, J.P., Jr., J.B. Pate, B.E. Ammons, and G.A. Swanson. The
Use of Hypodermic Needles as Critical Orifices in Air Sampling. J. Air
Pollution Control Association. 16:197-200. 1966.
12. Shigehara, R.T., and Candace B. Sorrell. Using Critical Orifices
as Method 5 Calibration Standards. Source Evaluation Society
Newsletter. 10(3):4-15. August 1985.
40 CFR 60.748 Pt. 60, App. A, Meth. 6A
1. Principle and Applicability
1.1 Applicability. This method applies to the determination of sulfur
dioxide (SO2) emissions from fossil fuel combustion sources in terms of
concentration (mg/m /3/ ) and in terms of emission rate (ng/J) and to
the determination of carbon dioxide (CO2) concentration (percent).
Moisture, if desired, may also be determined by this method.
The minimum detectable limit, the upper limit, and the interferences
of the method for the measurement of SO2 are the same as for Method 6.
For a 20-liter sample, the method has a precision of 0.5 percent CO2 for
concentrations between 2.5 and 25 percent CO2 and 1.0 percent moisture
for moisture concentrations greater than 5 percent.
1.2 Principle. The principle of sample collection is the same as for
Method 6 except that moisture and CO2 are collected in addition to SO2
in the same sampling train. Moisture and CO2 fractions are determined
gravimetrically.
2. Apparatus
2.1 Sampling. The sampling train is shown in Figure 6A-1; the
equipment required is the same as for Method 6, Section 2.1, except as
specified below:
2.1.1 SO2 Absorbers. Two 30-ml midget impingers with a 1-mm
restricted tip and two 30-ml midget bubblers with an unrestricted tip.
Other types of impingers and bubblers, such as Mae West for SO2
collection and rigid cylinders for moisture absorbers containing
Drierite, may be used with proper attention to reagent volumes and
levels, subject to the Administrator's approval.
2.1.2 CO2 Absorber. A sealable rigid cylinder or bottle with an
inside diameter between 30 and 90 mm and a length between 125 and 250 mm
and with appropriate connections at both ends.
Note: For applications downstream of wet scrubbers, a heated
out-of-stack filter (either borosilicate glass wool or glass fiber mat)
is necessary. The filter may be a separate heated unit or may be within
the heated portion of the probe. If the filter is within the sampling
probe, the filter should not be within 15 cm of the probe inlet or any
unheated section of the probe, such as the connection to the first SO2
absorber. The probe and filter should be heated to at least 20 C above
the source temperature, but not greater than 120 C. The filter
temperature (i.e., the sample gas temperature) should be monitored to
assure the desired temperature is maintained. A heated Teflon connector
may be used to connect the filter holder or probe to the first impinger.
Note: Mention of a brand name does not constitute endorsement by the
Environmental Protection Agency.
2.2 Sample Recovery and Analysis. The equipment needed for sample
recovery and analysis is the same as required for Method 6. In
addition, a balance to measure within 0.05 g is needed for analysis.
3. Reagents
Unless otherwise indicated, all reagents must conform to the
specifications established by the committee on analytical reagents of
the American Chemical Society. Where such specifications are not
available, use the best available grade.
3.1 Sampling. The reagents required for sampling are the same as
specified in Method 6. In addition, the following reagents are
required:
Insert illus. 517A
3.1.1 Drierite. Anhydrous calcium sulfate (CaSO4) desiccant, 8 mesh,
indicating type is recommended. (Do not use silica gel or similar
desiccant in the application.)
3.1.2 CO2 Absorbing Material. Ascarite II. Sodium hydroxide coated
silica, 8 to 20 mesh.
3.2 Sample Recovery and Analysis. The reagents needed for sample
recovery and analysis are the same as for Method 6, Sections 3.2 and
3.3, respectively.
4. Procedure
4.1 Sampling.
4.1.1 Preparation of Collection Train. Measure 15 ml of 80 percent
isopropanol into the first midget bubbler and 15 ml of 3 percent
hydrogen peroxide into each of the first two midget impingers as
described in Method 6. Insert the glass wool into the top of the
isopropanol bubbler as shown in Figure 6A-1. Into the fourth vessel in
the train, the second midget bubbler, place about 25 g of Drierite.
Clean the outsides of the bubblers and impingers, and weigh at room
temperature ( 20 C) to the nearest 0.1 g. Weigh the four vessels
simultaneously, and record this initial mass.
With one end of the CO2 absorber sealed, place glass wool in the
cylinder to a depth of about 1 cm. Place about 150 g of CO2 absorbing
material in the cylinder on top of the glass wool, and fill the
remaining space in the cylinder with glass wool. Assemble the cylinder
as shown in Figure 6A-2. With the cylinder in a horizontal position,
rotate it around the horizontal axis. The CO2 absorbing material should
remain in position during the rotation, and no open spaces or channels
should be formed. If necessary, pack more glass wool into the cylinder
to make the CO2 absorbing material stable. Clean the outside of the
cylinder of loose dirt and moisture and weigh at room temperature to the
nearest 0.1 g. Record this initial mass.
Assemble the train as shown in Figure 6A-1. Adjust the probe heater
to a temperature sufficient to prevent condensation (see Note in section
2.1.1). Place crushed ice and water around the impingers and bubblers.
Mount the CO2 absorber outside the water bath in a vertical flow
position with the sample gas inlet at the bottom. Flexible tubing,
e.g., Tygon, may be used to connect the last SO2 absorbing bubbler to
the Drierite absorber and to connect the Drierite absorber to the CO2
absorber. A second, smaller CO2 absorber containing Ascarite II may be
added in line downstream of the primary CO2 absorber as a breakthrough
indicator. Ascarite II turns white when CO2 is absorbed.
Insert illus. 517B
4.1.2 Leak-Check Procedure and Sample Collection. The leak-check
procedure and sample collection procedure are the same as specified in
Method 6, Sections 4.1.2 and 4.1.3, respectively.
4.2 Sample Recovery.
4.2.1 Moisture Measurement. Disconnect the isopropanol bubbler, the
SO2 impingers, and the moisture absorber from the sample train. Allow
about 10 minutes for them to reach room temperature, clean the outsides
of loose dirt and moisture, and weigh them simultaneously in the same
manner as in Section 4.1.1. Record this final mass.
4.2.2 Peroxide Solution. Discard the contents of the isopropanol
bubbler and pour the contents of the midget impingers into a leak-free
polyethylene bottle for shipping, Rinse the two midget impingers and
connecting tubes with deionized distilled water, and add the washings to
the same storage container.
4.2.3 CO2 Absorber. Allow the CO2 absorber to warm to room
temperature (about 10 minutes), clean the outside of loose dirt and
moisture, and weigh to the nearest 0.1 g in the same manner as in
Section 4.1.1. Record this final mass. Discard used Ascarite II
material.
4.3 Sample Analysis. The sample analysis procedure for SO2 is the
same as specified in Method 6, Section 4.3.
4.4 Quality Assurance (QA) Audit Samples. Only when this method is
used for compliance determinations, obtain an audit sample set as
directed in Section 3.3.6 of Method 6. Analyze the audit samples, and
report the results as directed in Section 4.4 of Method 6. Acceptance
criteria for the audit results are the same as in Method 6.
5. Calibration
The calibrations and checks are the same as required in Method 6,
Section 5.
6. Calculations
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after final
calculations. The calculations, nomenclature, and procedures are the
same as specified in Method 6 with the addition of the following:
6.1 Nomenclature.
Cw= Concentration of moisture, percent.
CCO2=Concentration of CO2, dry basis, percent.
mwi=Initial mass of impingers, bubblers, and moisture absorber, g.
mwf=Final mass of impingers, bubblers, and moisture absorber, g.
mai=Initial mass of CO2 absorber, g.
maf=Final mass of CO2 absorber, g.
VCO2(std)=Equivalent volume of CO2 collected at standard conditions,
dsm3.
Vw(std)=Equivalent volume of moisture collected at standard
conditions, sm3.
5.467 10^4=Equivalent volume of gaseous CO2 at standard conditions
per gram, sm3/g.
1.336 10^3=Equivalent volume of water vapor at standard conditions
per gram, sm3/g.
6.2 CO2 Volume Collected, Corrected to Standard Conditions.
VCO2(std)=5.467 x 10^4 (maf^ mai) Eq. 6A-1
6.3 Moisture Volume Collected, Corrected to Standard Conditions.
Eq. 6A-2
6.4 SO2 Concentration.
Insert illus. 0320A
6.5 CO2 Concentration.
insert illus. 0320B
6.6 Moisture Concentration.
Eq. 6A-5
7. Emission Rate Procedure
If the only emission measurement desired is in terms of emission rate
of SO (ng/J), an abbreviated procedure may be used. The differences
between Method 6A and the abbreviated procedure are described below.
7.1 Sample Train. The sample train is the same as shown in Figure
6A-1 and as described in Section 4, except that the dry gas meter is not
needed.
7.2 Preparation of the Collection Train. Follow the same procedure
as in Section 4.1.1, except do not weigh the isopropanol bubbler, the
SO2 absorbing impingers or the moisture absorber.
7.3 Sampling. Operate the train as described in Section 4.1.3, except
that dry gas meter readings, barometric pressure, and dry gas meter
temperatures need not be recorded.
7.4 Sample Recovery. Follow the procedure in Section 4.2, except do
not weigh the isopropanol bubbler, the SO2 absorbing impingers, or the
moisture absorber.
7.5 Sample Analysis. Analysis of the peroxide solution is the same
as described in Section 4.3. Only when making compliance determinations,
conduct an audit of the SO2 analysis procedure as described in Section
4.4.
7.6 Calculations.
7.6.1 SO Mass Collected.
Insert illus. 321B
Where:
mSO2=Mass of SO2 collected, mg.
7.6.2 Sulfur Dioxide Emission Rate.
Insert illus. 321C
Where:
ESO2=Emission rate of SO2 (ng/J).
Fc=Carbon F Factor for the fuel burned, m3/J, from Method 19.
8. Bibliography
1. Same as for Method 6, Citations 1 through 8, with the addition of
the following:
2. Stanley, Jon and P.R. Westlin. An Alternate Method for Stack Gas
Moisture Determination. Source Evaluation Society Newsletter. Vol. 3,
No. 4. November 1978.
3. Whittle, Richard N. and P.R. Westlin. Air Pollution Test Report:
Development and Evaluation of an Intermittent Integrated SO2/CO2
Emission Sampling Procedure. Environmental Protection Agency, Emission
Standard and Engineering Division, Emission Measurement Branch.
Research Triangle Park, NC. December 1979. 14 pages.
40 CFR 60.748 Pt. 60, App. A, Meth. 6B
1. Principle and Applicability
1.1 Applicability. This method applies to the determination of sulfur
dioxide (SO2) emissions from combustion sources in terms of
concentration (ng/m3) and emission rate (ng/J), and for the
determination of carbon dioxide (CO2) concentration (percent) on a daily
(24 hours) basis.
The minimum detectable limits, upper limit, and the interferences for
SO2 measurements are the same as for Method 6. EPA-sponsored
collaborative studies were undertaken to determine the magnitude of
repeatability and reproducibility achievable by qualified testers
following the procedures in this method. The results of the studies
evolve from 145 field tests including comparisons with Methods 3 and 6.
For measurements of emission rates from wet, flue gas desulfurization
units in (ng/J), the repeatability (within laboratory precision) is 8.0
percent and the reproducibility (between laboratory precision) is 11.1
percent.
1.2 Principle. A gas sample is extracted from the sampling point in
the stack intermittently over a 24-hour or other specified time period.
Sampling may also be conducted continuously if the apparatus and
procedures are appropriately modified (see Note in Section 4.1.1). The
SO2 and CO2 are separated and collected in the sampling train. The SO2
fraction is measured by the barium-thorin titration method, and CO2 is
determined gravimetrically.
2. Apparatus
The equipment required for this method is the same as specified for
Method 6A, Section 2, except the isopropanol bubbler is not used. An
empty bubbler for the collection of liquid droplets and does not allow
direct contact between the collected liquid and the gas sample may be
included in the train. For intermittent operation, include an
industrial timer-switch designed to operate in the ''on'' position at
least 2 minutes continuously and ''off'' the remaining period over a
repeating cycle. The cycle of operation in designated in the applicable
regulation. At a minimum, the sampling operation should include at
least 12, equal, evenly-spaced periods per 24 hours.
For applications downstream of wet scrubbers, a heated out-of-stack
filter (either borosilicate glass wool or glass fiber mat) is necessary.
The probe and filter should be heated continuously to at least 20 C
above the source temperature, but not greater than 120 C. The filter
(i.e., sample gas) temperature should be monitored to assure the desired
temperature is maintained.
Stainless steel sampling probes, type 316, are not recommended for
use with Method 6B because of potential corrosion and contamination of
sample. Glass probes or other types of stainless steel, e.g., Hasteloy
or Carpenter 20, are recommended for long-term use.
Other sampling equipment, such as Mae West bubblers and rigid
cylinders for moisture absorption, which requires sample or reagent
volumes other than those specified in this procedure for full
effectiveness may be used, subject to the approval of the Administrator.
3. Reagents
All reagents for sampling and analysis are the same as described in
Method 6A, Section 3, except isopropanol is not used for sampling. The
hydrogen peroxide absorbing solution shall be diluted to no less than 6
percent by volume, instead of 3 percent as specified in Method 6. If
Method 6B is to be operated in a low sample flow condition (less than
100 ml/min), molecular sieve material may be substituted for Ascarite II
as the CO2 absorbing material. The recommended molecular sieve material
is Union Carbide 1/16 inch pellets, 5A , or equivalent. Molecular sieve
material need not be discarded following the sampling run provided it is
regenerated as per the manufacturer's instruction. Use of molecular
sieve material at flow rates higher than 100 ml/min may cause erroneous
CO2 results.
4. Procedure
4.1 Sampling.
4.1.1 Preparation of Collection Train. Preparation of the sample
train is the same as described in Method 6A, Section 4.1.4, with the
addition of the following:
The sampling train is assembled as shown in Figure 6A-1, except the
isopropanol bubbler is not included. The probe must be heated to a
temperature sufficient to prevent water condensation and must include a
filter (either in-stack, out-of-stack, or both) to prevent particulate
entrainment in the peroxide impingers. The electric supply for the
probe heat should be continuous and separate from the timed operation of
the sample pump.
Adjust the timer-switch to operate in the ''on'' position from 2 to 4
minutes on a 2-hour repeating cycle or other cycle specified in the
applicable regulation. Other timer sequences may be used with the
restriction that the total sample volume collected is between 25 and 60
liters for the amounts of sampling reagents prescribed in this method.
Add cold water to the tank until the impingers and bubblers are
covered at least two-thirds of their length. The impingers and bubbler
tank must be covered and protected from intense heat and direct
sunlight. If freezing conditions exist, the impinger solution and the
water bath must be protected.
Note: Sampling may be conducted continuously if a low flow-rate
sample pump (20 to 40 ml/min for the reagent volumes described in this
method) is used. Then the timer-switch is not necessary. In addition,
if the sample pump is designed for constant rate sampling, the rate
meter may be deleted. The total gas volume collected should be between
25 and 60 liters for the amounts of sampling reagents prescribed in this
method.
4.1.2 Leak-Check Procedure. The leak-check procedure is the same as
described in Method 6, Section 4.1.2.
4.1.3 Sample Collection. Record the initial dry gas meter reading.
To begin sampling, position the tip of the probe at the sampling point,
connect the probe to the first impinger (or filter), and start the timer
and the sample pump. Adjust the sample flow to a constant rate of
approximately 1.0 liter/min as indicated by the rotameter. Assure that
the timer is operating as intended, i.e., in the ''on'' position for the
desired period and the cycle repeats as required.
During the 24-hour sampling period, record the dry gas meter
temperature one time between 9:00 a.m. and 11:00 a.m., and the
barometric pressure.
At the conclusion of the run, turn off the timer and the sample pump,
remove the probe from the stack, and record the final gas meter volume
reading. Conduct a leak check as described in Section 4.1.2. If a leak
is found, void the test run or use procedures acceptable to the
Administrator to adjust the sample volume for leakage. Repeat the steps
in this section (4.1.3) for successive runs.
4.2 Sample Recovery. The procedures for sample recovery (moisture
measurement, peroxide solution, and CO2 absorber) are the same as in
Method 6A, Section 4.2.
4.3 Sample Analysis. Analysis of the peroxide impinger solutions is
the same as in Method 6, Section 4.3.
4.4 Quality Assurance (QA) Audit Samples. Only when this method is
used for compliance determinations, obtain an audit sample set as
directed in Section 3.3.6 of Method 6. Analyze the audit samples at
least once for every 30 days of sample collection, and report the
results as directed in Section 4.4 of Method 6. The analyst performing
the sample analyses shall perform the audit analyses. If more than one
analyst performed the sample analyses during the 30-day sampling period,
each analyst shall perform the audit analyses and all audit results
shall be reported. Acceptance criteria for the audit results are the
same as in Method 6.
5. Calibration
5.1 Metering System.
5.1.1 Initial Calibration. The initial calibration for the volume
metering system is the same as for Method 6, Section 5.1.1.
5.1.2 Periodic Calibration Check. After 30 days of operation of the
test train, conduct a calibration check as in Section 5.1.1 above,
except for the following variations: (1) The leak check is not to be
conducted, (2) three or more revolutions of the dry gas meter must be
used, and (3) only two independent runs need be made. If the
calibration factor does not deviate by more than 5 percent from the
initial calibration factor determined in Section 5.1.1, then the dry gas
meter volumes obtained during the test series are acceptable and use of
the train can continue. If the calibration factor deviates by more than
5 percent, recalibrate the metering system as in Section 5.1.1; and for
the calculations for the preceding 30 days of data, use the calibration
factor (initial or recalibration) that yields the lower gas volume for
each test run. Use the latest calibration factor for succeeding tests.
5.2 Thermometers. Calibrate against mercury-in-glass thermometers
initially and at 30-day intervals.
5.3 Rotameter. The rotameter need not be calibrated, but should be
cleaned and maintained according to the manufacturer's instructions.
5.4 Barometer. Calibrate against a mercury barometer initially and at
30-day intervals.
5.5 Barium Perchlorate Solution. Standardize the barium perchlorate
solution against 25 ml of standard sulfuric acid to which 100 ml of 100
percent isopropanol has been added.
6. Calculations
The nomenclature and calculation procedures are the same as in Method
6A with the following exceptions:
Pbar=Initial barometric pressure for the test period, mm Hg.
Tm=Absolute meter temperature for the test period, K.
7. Emission Rate Procedure
The emission rate procedure is the same as described in Method 6A,
Section 7, except that the timer is needed and is operated as described
in this method. Only when this method is used for compliance
determinations, perform the QA audit analyses as described in Section
4.4.
8. Bibliography
The bibliography is the same as described in Method 6A, with the
addition of the following:
1. Butler, Frank E; J.E. Knoll, J.C. Suggs, M.R. Midgett, and W.
Mason. The Collaborative Test of Method 6B: Twenty-Four-Hour Analysis
of SO2 and CO2. JAPCA. Vol. 33, No. 10. October 1983.
40 CFR 60.748 Pt. 60, App. A, Meth. 6C
1. Applicability and Principle
1.1 Applicability. This method is applicable to the determination of
sulfur dioxide (SO2) concentrations in controlled and uncontrolled
emissions from stationary sources only when specified within the
regulations.
1.2 Principle. A gas sample is continuously extracted from a stack,
and a portion of the sample is conveyed to an instrumental analyzer for
determination of SO2 gas concentration using an ultraviolet (UV),
nondispersive infrared (NDIR), or fluorescence analyzer. Performance
specifications and test procedures are provided to ensure reliable data.
2. Range and Sensitivity
2.1 Analytical Range. The analytical range is determined by the
instrumental design. For this method, a portion of the analytical range
is selected by choosing the span of the monitoring system. The span of
the monitoring system shall be selected such that the pollutant gas
concentration equivalent to the emission standard is not less than 30
percent of the span. If at any time during a run the measured gas
concentration exceeds the span, the run shall be considered invalid.
2.2 Sensitivity. The minimum detectable limit depends on the
analytical range, span, and signal-to-noise ratio of the measurement
system. For a well designed system, the minimum detectable limit should
be less than 2 percent of the span.
3. Definitions
3.1 Measurement System. The total equipment required for the
determination of gas concentration. The measurement system consists of
the following major subsystems:
3.1.1 Sample Interface. That portion of a system used for one or
more of the following: sample acquisition, sample transport, sample
conditioning, or protection of the analyzers from the effects of the
stack effluent.
3.1.2 Gas Analyzer. That portion of the system that senses the gas
to be measured and generates an output proportional to its
concentration.
3.1.3 Data Recorder. A strip chart recorder, analog computer, or
digital recorder for recording measurement data from the analyzer
output.
3.2 Span. The upper limit of the gas concentration measurement range
displayed on the data recorder.
3.3 Calibration Gas. A known concentration of a gas in an
appropriate diluent gas.
3.4 Analyzer Calibration Error. The difference between the gas
concentration exhibited by the gas analyzer and the known concentration
of the calibration gas when the calibration gas is introduced directly
to the analyzer.
3.5 Sampling System Bias. The difference between the gas
concentrations exhibited by the measurement system when a known
concentration gas is introduced at the outlet of the sampling probe and
when the same gas is introduced directly to the analyzer.
3.6 Zero Drift. The difference in the measurement system output
reading from the initial calibration response at the zero concentration
level after a stated period of operation during which no unscheduled
maintenance, repair, or adjustment took place.
3.7 Calibration Drift. The difference in the measurement system
output reading from the initial calibration response at a mid-range
calibration value after a stated period of operation during which no
unscheduled maintenance, repair, or adjustment took place.
3.8 Response Time. The amount of time required for the measurement
system to display 95 percent of a step change in gas concentration on
the data recorder.
3.9 Interference Check. A method for detecting analytical
interferences and excessive biases through direct comparison of gas
concentrations provided by the measurement system and by a modified
Method 6 procedure. For this check, the modified Method 6 samples are
acquired at the sample by-pass discharge vent.
3.10 Calibration Curve. A graph or other systematic method of
establishing the relationship between the analyzer response and the
actual gas concentration introduced to the analyzer.
4. Measurement System Performance Specifications
4.1 Analyzer Calibration Error. Less than 2 percent of the span for
the zero, mid-range, and high-range calibration gases.
4.2 Sampling System Bias. Less than 5 percent of the span for the
zero, and mid- or high-range calibration gases.
4.3 Zero Drift. Less than 3 percent of the span over the period of
each run.
4.4 Calibration Drift. Less than 3 percent of the span over the
period of each run.
4.5 Interference Check. Less than 7 percent of the modified Method
6 result for each run.
5. Apparatus and Reagents
5.1 Measurement System. Any measurement system for SO2 that meets
the specifications of this method. A schematic of an acceptable
measurement system is shown in Figure 6C-1. The essential components of
the measurement system are described below:
5.1.1 Sample Probe. Glass, stainless steel, or equivalent, of
sufficient length to traverse the sample points. The sampling probe
shall be heated to prevent condensation.
5.1.2 Sample Line. Heated (sufficient to prevent condensation)
stainless steel or Teflon tubing, to transport the sample gas to the
moisture removal system.
5.1.3 Sample Transport Lines. Stainless steel or Teflon tubing, to
transport the sample from the moisture removal system to the sample
pump, sample flow rate control, and sample gas manifold.
5.1.4 Calibration Valve Assembly. A three-way valve assembly, or
equivalent, for blocking the sample gas flow and introducing calibration
gases to the measurement system at the outlet of the sampling probe when
in the calibration mode.
5.1.5 Moisture Removal System. A refrigerator-type condenser or
similar device (e.g., permeation dryer), to remove condensate
continuously from the sample gas while maintaining minimal contact
between the condensate and the sample gas. The moisture removal system
is not necessary for analyzers that can measure gas concentrations on a
wet basis; for these analyzers, (1) heat the sample line and all
interface components up to the inlet of the analyzer sufficiently to
prevent condensation, and (2) determine the moisture content and correct
the measured gas concentrations to a dry basis using appropriate
methods, subject to the approval of the Administrator. The
determination of sample moisture content is not necessary for pollutant
analyzers that measure concentrations on a wet basis when (1) a wet
basis CO2 analyzer operated according to Method 3A is used to obtain
simultaneous measurements, and (2) the pollutant/CO2 measurements are
used to determine emissions in units of the standard.
5.1.6 Particulate Filter. An in-stack or heated (sufficient to
prevent water condensation) out-of-stack filter. The filter shall be
borosilicate or quartz glass wool, or glass fiber mat. Additional
filters at the inlet or outlet of the moisture removal system and inlet
of the analyzer may be used to prevent accumulation of particulate
material in the measurement system and extend the useful life of the
components. All filters shall be fabricated of materials that are
nonreactive to the gas being sampled.
5.1.7 Sample Pump. A leak-free pump, to pull the sample gas through
the system at a flow rate sufficient to minimize the response time of
the measurement system. The pump may be constructed of any material
that is nonreactive to the gas being sampled.
5.1.8 Sample Flow Rate Control. A sample flow rate control valve and
rotameter, or equivalent, to maintain a constant sampling rate within 10
percent.
(Note: The tester may elect to install a back-pressure regulator to
maintain the sample gas manifold at a constant pressure in order to
protect the analyzer(s) from overpressurization, and to minimize the
need for flow rate adjustments.)
5.1.9 Sample Gas Manifold. A sample gas manifold, to divert a
portion of the sample gas stream to the analyzer, and the remainder to
the by-pass discharge vent. The sample gas manifold should also include
provisions for introducing calibration gases directly to the analyzer.
The manifold may be constructed of any material that is nonreactive to
the gas being sampled.
5.1.10 Gas Analyzer. A UV or NDIR absorption or fluorescence
analyzer, to determine continuously the SO2 concentration in the sample
gas stream. The analyzer shall meet the applicable performance
specifications of Section 4. A means of controlling the analyzer flow
rate and a device for determining proper sample flow rate (e.g.,
precision rotameter, pressure gauge downstream of all flow controls,
etc.) shall be provided at the analyzer.
(Note: Housing the analyzer(s) in a clean, thermally-stable,
vibration-free environment will minimize drift in the analyzer
calibration.)
5.1.11 Data Recorder. A strip chart recorder, analog computer, or
digital recorder, for recording measurement data. The data recorder
resolution (i.e., readability) shall be 0.5 percent of span.
Alternatively, a digital or analog meter having a resolution of 0.5
percent of span may be used to obtain the analyzer responses and the
readings may be recorded manually. If this alternative is used, the
readings shall be obtained at equally spaced intervals over the duration
of the sampling run. For sampling run durations of less than 1 hour,
measurements at 1-minute intervals or a minimum of 30 measurements,
whichever is less restrictive, shall be obtained. For sampling run
durations greater than 1 hour, measurements at 2-minute intervals or a
minimum of 96 measurements, whichever is less restrictive, shall be
obtained.
5.2 Method 6 Apparatus and Reagents. The apparatus and reagents
described in Method 6, and shown by the schematic of the sampling train
in Figure 6C-2, to conduct the interference check.
5.3 SO2 Calibration Gases. The calibration gases for the gas
analyzer shall be SO2 in N2 or SO2 in air. Alternatively, SO2/CO2,
SO2/O2, or SO2/CO2/O2 gas mixtures in N2 may be used. For
fluorescence-based analyzers, the O2 and CO2 concentrations of the
calibration gases as introduced to the analyzer shall be within 1
percent (absolute) O2 and 1 percent (absolute) CO2 of the O2 and Co2
concentrations of the effluent samples as introduced to the analyzer.
Alternatively, for fluorescence-based analyzers, use calibration blends
of SO2 in air and the nomographs provided by the vendor to determine the
quenching correction factor (the effluent O2 and CO2 concentrations must
be known). Use three calibration gases as specified below:
5.3.1 High-Range Gas. Concentration equivalent to 80 to 100 percent
of the span.
5.3.2 Mid-Range Gas. Concentration equivalent to 40 to 60 percent of
the span.
5.3.3 Zero Gas. Concentration of less than 0.25 percent of the span.
Purified ambient air may be used for the zero gas by passing air
through a charcoal filter, or through one or more impingers containing a
solution of 3 percent H2O2.
6. Measurement System Performance Test Procedures
Perform the following procedures before measurement of emissions
(Section 7).
6.1 Calibration Gas Concentration Verification. There are two
alternatives for establishing the concentrations of calibration gases.
Alternative Number 1 is preferred.
6.1.1 Alternative Number 1 -- Use of calibration gases that are
analyzed following the Environmental Protection Agency Traceability
Protocol Number 1 (see Citation 1 in the Bibliography). Obtain a
certification from the gas manufacturer that Protocol Number 1 was
followed.
6.1.2 Alternative Number 2 -- Use of calibration gases not prepared
according to Protocol Number 1. If this alternative is chosen, obtain
gas mixtures with a manufacturer's tolerance not to exceed 2 percent of
the tag value. Within 6 months before the emission test, analyze each
of the calibration gases in triplicate using Method 6. Citation 2 in
the Bibliography describes procedures and techniques that may be used
for this analysis. Record the results on a data sheet (example is shown
in Figure 6C-3). Each of the individual SO2 analytical results for each
calibration gas shall be within 5 percent (or 5 ppm, whichever is
greater) of the triplicate set average; otherwise, discard the entire
set, and repeat the triplicate analyses. If the average of the
triplicate analyses is within 5 percent of the calibration gas
manufacturer's cylinder tag value, use the tag value; otherwise,
conduct at least three additional analyses until the results of six
consecutive runs agree with 5 percent (or 5 ppm, whichever is greater)
of their average. Then use this average for the cylinder value.
6.2 Measurement System Preparation. Assemble the measurement system
by following the manufacturer's written instructions for preparing and
preconditioning the gas analyzer and, as applicable, the other system
components. Introduce the calibration gases in any sequence, and make
all necessary adjustments to calibrate the analyzer and the data
recorder. Adjust system components to achieve correct sampling rates.
6.3 Analyzer Calibration Error. Conduct the analyzer calibration
error check by introducing calibration gases to the measurement system
at any point upstream of the gas analyzer as follows:
6.3.1 After the measurement system has been prepared for use,
introduce the zero, mid-range, and high-range gases to the analyzer.
During this check, make no adjustments to the system except those
necessary to achieve the correct calibration gas flow rate at the
analyzer. Record the analyzer responses to each calibration gas on a
form similar to Figure 6C-4.
Note: A calibration curve established prior to the analyzer
calibration error check may be used to convert the analyzer response to
the equivalent gas concentration introduced to the analyzer. However,
the same correction procedure shall be used for all effluent and
calibration measurements obtained during the test.
6.3.2 The analyzer calibration error check shall be considered
invalid if the gas concentration displayed by the analyzer exceeds 2
percent of the span for any of the calibration gases. If an invalid
calibration is exhibited, take corrective action, and repeat the
analyzer calibration error check until acceptable performance is
achieved.
6.4 Sampling System Bias Check. Perform the sampling system bias
check by introducing calibration gases at the calibration valve
installed at the outlet of the sampling probe. A zero gas and either
the mid-range or high-range gas, whichever most closely approximates the
effluent concentrations, shall be used for this check as follows:
6.4.1 Introduce the upscale calibration gas, and record the gas
concentration displayed by the analyzer on a form similar to Figure
6C-5. Then introduce zero gas, and record the gas concentration
displayed by the analyzer. During the sampling system bias check,
operate the system at the normal sampling rate, and make no adjustments
to the measurement system other than those necessary to achieve proper
calibration gas flow rates at the analyzer. Alternately introduce the
zero and upscale gases until a stable response is achieved. The tester
shall determine the measurement system response time by observing the
times required to achieve a stable response for both the zero and
upscale gases. Note the longer of the two times as the response time.
6.4.2 The sampling system bias check shall be considered invalid if
the difference between the gas concentrations displayed by the
measurement system for the analyzer calibration error check and for the
sampling system bias check exceeds 5 percent of the span for either the
zero or upscale calibration gas. If an invalid calibration is
exhibited, take corrective action, and repeat the sampling system bias
check until acceptable performance is achieved. If adjustment to the
analyzer is required, first repeat the analyzer calibration error check,
then repeat the sampling system bias check.
7. Emission Test Procedure
7.1 Selection of Sampling Site and Sampling Points. Select a
measurement site and sampling points using the same criteria that are
applicable to Method 6.
7.2 Interference Check Preparation. For each individual analyzer,
conduct an interference check for at least three runs during the initial
field test on a particular source category. Retain the results, and
report them with each test performed on that source category.
If an interference check is being performed, assemble the modified
Method 6 train (flow control valve, two midget impingers containing 3
percent H2O2, and dry gas meter) as shown in Figure 6C-2. Install the
sampling train to obtain a sample at the measurement system sample
by-pass discharge vent. Record the initial dry gas meter reading.
7.3 Sample Collection. Position the sampling probe at the first
measurement point, and begin sampling at the same rate as used during
the sampling system bias check. Maintain constant rate sampling (i.e.,
10 percent) during the entire run. The sampling time per run shall be
the same as for Method 6 plus twice the system response time. For each
run, use only those measurements obtained after twice response time of
the measurement system has elapsed, to determine the average effluent
concentration. If an interference check is being performed, open the
flow control valve on the modified Method 6 train concurrent with the
initiation of the sampling period, and adjust the flow to 1 liter per
minute ( 10 percent).
(Note: If a pump is not used in the modified Method 6 train, caution
should be exercised in adjusting the flow rate since overpressurization
of the impingers may cause leakage in the impinger train, resulting in
positively biased results).
7.4 Zero and Calibration Drift Tests. Immediately preceding and
following each run, or if adjustments are necessary for the measurement
system during the run, repeat the sampling system bias check procedure
described in Section 6.4 (Make no adjustments to the measurement system
until after the drift checks are completed.) Record and analyzer's
responses on a form similar to Figure 6C-5.
7.4.1 If either the zero or upscale calibration value exceeds the
sampling system bias specification, then the run is considered invalid.
Repeat both the analyzer calibration error check procedure (Section 6.3)
and the sampling system bias check procedure (Section 6.4) before
repeating the run.
7.4.2 If both the zero and upscale calibration values are within the
sampling system bias specification, then use the average of the initial
and final bias check values to calculate the gas concentration for the
run. If the zero or upscale calibration drift value exceeds the drift
limits, based on the difference between the sampling system bias check
responses immediately before and after the run, repeat both the analyzer
calibration error check procedure (Section 6.3) and the sampling system
bias check procedure (Section 6.4) before conducting additional runs.
7.5 Interference Check (if performed). After completing the run,
record the final dry gas meter reading, meter temperature, and
barometric pressure. Recover and analyze the contents of the midget
impingers, and determine the SO2 gas concentration using the procedures
of Method 6. (It is not necessary to analyze EPA performance audit
samples for Method 6.) Determine the average gas concentration exhibited
by the analyzer for the run. If the gas concentrations provided by the
analyzer and the modified Method 6 differ by more than 7 percent of the
modified Method 6 result, the run is invalidated.
8. Emission Calculation
The average gas effluent concentration is determined from the average
gas concentration displayed by the gas analyzer, and is adjusted for the
zero and upscale sampling system bias checks, as determined in
accordance with Section 7.4. The average gas concentration displayed by
the analyzer may be determined by integration of the area under the
curve for chart recorders, or by averaging all of the effluent
measurements. Alternatively, the average may be calculated from
measurements recorded at equally spaced intervals over the entire
duration of the run. For sampling run durations of less than 1 hour,
measurements at 1-minute intervals or a minimum of 30 measurements,
whichever is less restrictive, shall be used. For sampling run
durations greater than 1 hour, measurements at 2-minute intervals or a
minimum of 96 measurements, whichever is less restrictive, shall be
used. Calculate the effluent gas concentration using Equation 6C-1.
Eq. 6C-1
Where:
Cgas = Effluent gas concentration, dry basis, ppm.
C8 = Average gas concentration indicated by gas analyzer, dry basis,
ppm.
Co = Average of initial and final system calibration bias check
responses for the zero gas, ppm.
Cm = Average of initial and final system calibration bias check
responses for the upscale calibration gas, ppm.
Cma = Actual concentration of the upscale calibration gas, ppm.
9. Bibliography
1. Traceability Protocol for Establishing True Concentrations of
Gases Used for Calibrations and Audits of Continuous Source Emission
Monitors: Protocol Number 1. U.S. Environmental Protection Agency,
Quality Assurance Division. Research Triangle Park, NC. June 1978.
2. Westlin, Peter R. and J. W. Brown. Methods for Collecting and
Analyzing Gas Cylinder Samples. Source Evaluation Society Newsletter.
3(3):5-15. September 1978.
Insert illus.
OMITT500000000 ED
Insert illus. 0810
Date
Analytic method used
Source identification:
Test personnel:
Date:
Analyzer calibration data for sampling
runs:
Span:
Source identification:
Test personnel:
Date:
Run number:
Span:
40 CFR 60.748 Pt. 60, App. A, Meth. 7
1. Principle and Applicability
1.1 Principle. A grab sample is collected in an evacuated flask
containing a dilute sulfuric acid-hydrogen peroxide absorbing solution,
and the nitrogen oxides, except nitrous oxide, are measured
colorimetrically using the phenoldisulfonic acid (PDS) procedure.
1.2 Applicability. This method is applicable to the measurement of
nitrogen oxides emitted from stationary sources. The range of the
method has been determined to be 2 to 400 milligrams NOx (as NO2) per
dry standard cubic meter, without having to dilute the sample.
2. Apparatus
2.1 Sampling (see Figure 7-1). Other grab sampling systems or
equipment, capable of measuring sample volume to within 2.0 percent and
collecting a sufficient sample volume to allow analytical
reproducibility to within 5 percent, will be considered acceptable
alternatives, subject to approval of the Administrator, U.S.
Environmental Protection Agency. The following equipment is used in
sampling:
2.1.1 Probe. Borosilicate glass tubing, sufficiently heated to
prevent water condensation and equipped with an in-stack or out-stack
filter to remove particulate matter (a plug of glass wool is
satisfactory for this purpose). Stainless steel or Teflon3 tubing may
also be used for the probe. Heating is not necessary if the probe
remains dry during the purging period.
Insert illus 249
2.1.2 Collection Flask. Two-liter borosilicate, round bottom flask,
with short neck and 24/40 standard taper opening, protected against
implosion or breakage.
2.1.3 Flask Valve. T-bore stopcock connected to a 24/40 standard
taper joint.
2.1.4 Temperature Gauge. Dial-type thermometer, or other temperature
gauge, capable of measuring 1 C (2 F) intervals from ^5 to 50 C (25
to 125 F).
2.1.5 Vacuum Line. Tubing capable of withstanding a vacuum of 75 mm
Hg (3 in. Hg) absolute pressure, with ''T'' connection and T-bore
stopcock.
2.1.6 Vacuum Gauge. U-tube manometer, 1 meter (36 in.), with 1-mm
(0.1-in.) divisions, or other gauge capable of measuring pressure to
within 2.5 mm Hg (0.10 in. Hg).
2.1.7 Pump. Capable of evacuating the collection flask to a pressure
equal to or less than 75 mm Hg (3 in. Hg) absolute.
2.1.8 Squeeze Bulb. One-way.
2.1.9 Volumetric Pipette. 25 ml.
2.1.10 Stopcock and Ground Joint Grease. A high-vacuum,
high-temperature chlorofluorocarbon grease is required. Halocarbon
25-5S has been found to be effective.
2.1.11 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg). In many
cases, the barometric reading may be obtained from a nearby National
Weather Service station, in which case the station value (which is the
absolute barometric pressure) shall be requested and an adjustment for
elevation differences between the weather station and sampling point
shall be applied at a rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 m
(100 ft) elevation increase, or vice versa for elevation decrease.
2.2 Sample Recovery. The following equipment is required for sample
recovery:
2.2.1 Graduated Cylinder. 50 ml with 1-ml divisions.
2.2.2 Storage Containers. Leak-free polyethylene bottles.
2.2.3 Wash Bottle. Polyethylene or glass.
2.2.4 Glass Stirring Rod.
2.2.5 Test Paper for Indicating pH. To cover the pH range of 7 to
14.
2.3 Analysis. For the analysis, the following equipment is needed:
2.3.1 Volumetric Pipettes. Two 1 ml, two 2 ml, one 3 ml, one 4 ml,
two 10 ml, and one 25 ml for each sample and standard.
2.3.2 Porcelain Evaporating Dishes. 175- to 250-ml capacity with lip
for pouring, one for each sample and each standard. The Coors No.
45006 (shallow-form, 195 ml) has been found to be satisfactory.
Alternatively, polymethyl pentene beakers (Nalge No. 1203, 150 ml), or
glass beakers (150 ml) may be used. When glass beakers are used,
etching of the beakers may cause solid matter to be present in the
analytical step; the solids should be removed by filtration (see
Section 4.3).
2.3.3 Steam Bath. Low-temperature ovens or thermostatically
controlled hot plates kept below 70 C (160 F) are acceptable
alternatives.
2.3.4 Dropping Pipette or Dropper. Three required.
2.3.5 Polyethylene Policeman. One for each sample and each standard.
2.3.6 Graduated Cylinder. 100 ml with 1-ml divisions.
2.3.7 Volumetric Flasks. 50 ml (one for each sample and each
standard), 100 ml (one for each sample and each standard, and one for
the working standard KNO3 solution), and 1000 ml (one).
2.3.8 Spectrophotometer. To measure absorbance at 410 nm.
2.3.9 Graduated Pipette. 10 ml with 0.1-ml divisions.
2.3.10 Test Paper for Indicating pH. To cover the pH range of 7 to
14.
2.3.11 Analytical Balance. To measure to within 0.1 mg.
3. Reagents
Unless otherwise indicated, it is intended that all reagents conform
to the specifications established by the Committee on Analytical
Reagents of the American Chemical Society, where such specifications are
available; otherwise, use the best available grade.
3.1 Sampling. To prepare the absorbing solution, cautiously add 2.8
ml concentrated H2SO4 to 1 liter of deionized, distilled water. Mix
well and add 6 ml of 3 percent hydrogen peroxide, freshly prepared from
30 percent hydrogen peroxide solution. The absorbing solution should be
used within 1 week of its preparation. Do not expose to extreme heat or
direct sunlight.
3.2 Sample Recovery. Two reagents are required for sample recovery:
3.2.1 Sodium Hydroxide (1N). Dissolve 40 g NaOH in deionized,
distilled water and dilute to 1 liter.
3.2.2 Water. Deionized, distilled to conform to ASTM Specification
D1193-77, Type 3 (incorporated by reference -- see 60.17). At the
option of the analyst, the KMnO4 test for oxidizable organic matter may
be omitted when high concentrations of organic matter are not expected
to be present.
3.3 Analysis. For the analysis, the following reagents are required:
3.3.1 Fuming Sulfuric Acid. 15 to 18 percent by weight free sulfur
trioxide. HANDLE WITH CAUTION.
3.3.2 Phenol. White solid.
3.3.3 Sulfuric Acid. Concentrated, 95 percent minimum assay. HANDLE
WITH CAUTION.
3.3.4 Potassium Nitrate. Dried at 105 to 110 C (220 to 230 F) for
a minimum of 2 hours just prior to preparation of standard solution.
3.3.5 Standard KNO3 Solution. Dissolve exactly 2.198 g of dried
potassium nitrate (KNO3) in deionized, distilled water and dilute to 1
liter with deionized, distilled water in a 1,000-ml volumetric flask.
3.3.6 Working Standard KNO3 Solution. Dilute 10 ml of the standard
solution to 100 ml with deionized distilled water. One milliter of the
working standard solution is equivalent to 100 g nitrogen dioxide
(NO2).
3.3.7 Water. Deionized, distilled as in Section 3.2.2.
3.3.8 Phenoldisulfonic Acid Solution. Dissolve 25 g of pure white
phenol in 150 ml concentrated sulfuric acid on a steam bath. Cool, add
75 ml fuming sulfuric acid, and heat at 100 C (212 F) for 2 hours.
Store in a dark, stoppered bottle.
3.3.9 Quality Assurance Audit Samples. Nitrate samples in glass
vials prepared by EPA's Environmental Monitoring Systems Laboratory,
Quality Assurance Division, Source Branch, Mail Drop 77A, Research
Triangle Park, North Carolina 27711. Each set will consist of two vials
having solutions of unknown concentrations. Only when making compliance
determinations, obtain an audit sample set from the quality assurance
management office at each EPA regional office or the responsible
enforcement agency. (Note: The tester should notify the quality
assurance office or the responsible enforcement agency at least 30 days
prior to the test date to allow sufficient time for sample delivery.)
4. Procedures
4.1 Sampling.
4.1.1 Pipette 25 ml of absorbing solution into a sample flask,
retaining a sufficient quantity for use in preparing the calibration
standards. Insert the flask valve stopper into the flask with the valve
in the ''purge'' position. Assemble the sampling train as shown in
Figure 7-1 and place the probe at the sampling point. Make sure that
all fitings are tight and leak-free, and that all ground glass joints
have been properly greased with a high-vacuum, high-temperature
chlorofluorocarbon-based stopcock grease. Turn the flask valve and the
pump valve to their ''evacuate'' positions. Evacuate the flask to 75 mm
Hg (3 in. Hg) absolute pressure, or less. Evacuation to a pressure
approaching the vapor pressure of water at the existing temperature is
desirable. Turn the pump valve to its ''vent'' position and turn the
off the pump. Check for leakage by observing the manometer for any
pressure fluctuation. (Any variation greater than 10 mm Hg (0.4 in. Hg)
over a period of 1 minute is not acceptable, and the flask is not to be
used until the leakage problem is corrected. Pressure in the flask is
not to exceed 75 mm Hg (3 in. Hg) absolute at the time sampling is
commenced.) Record the volume of the flask and valve (Vf), the flask
temperature (Ti), and the barometric pressure. Turn the flask valve
counterclockwise to its ''purge'' position and do the same with the pump
valve. Purge the probe and the vacuum tube using the squeeze bulb. If
condensation occurs in the probe and the flask valve area, heat the
probe and purge until the condensation disappears. Next, turn the pump
valve to its ''vent'' position. Turn the flask valve clockwise to its
''evacuate'' position and record the difference in the mercury levels in
the manometer. The absolute internal pressure in the flask (Pi) is
equal to the barometric pressure less the manometer reading.
Immediately turn the flask valve to the ''sample'' position and permit
the gas to enter the flask until pressures in the flask and sample line
(i.e., duct, stack) are equal. This will usually require about 15
seconds; a longer period indicates a ''plug'' in the probe, which must
be corrected before sampling is continued. After collecting the sample,
turn the flask valve to its ''purge'' position and disconnect the flask
from the sampling train. Shake the flask for at least 5 minutes.
4.1.2 If the gas being sampled contains insufficient oxygen for the
conversion of NO to NO2 (e.g., an applicable subpart of the standard may
require taking a sample of a calibration gas mixture of NO in N2), then
oxygen shall be introduced into the flask to permit this conversion.
Oxygen may be introduced into the flask by one of three methods; (1)
Before evacuating the sampling flask, flush with pure cylinder oxygen,
then evacuate flask to 75 mm Hg (3 in. Hg) absolute pressure or less;
or (2) inject oxygen into the flask after sampling; or (3) terminate
sampling with a minimum of 50 mm Hg (2 in. Hg) vacuum remaining in the
flask, record this final pressure, and then vent the flask to the
atmosphere until the flask pressure is almost equal to atmospheric
pressure.
4.2 Sample Recovery. Let the flask set for a minimum of 16 hours and
then shake the contents for 2 minutes. Connect the flask to a mercury
filled U-tube manometer. Open the valve from the flask to the manometer
and record the flask temperature (Tf), the barometric pressure, and the
difference between the mercury levels in the manometer. The absolute
internal pressure in the flask (Pf) is the barometric pressure less the
manometer reading. Transfer the contents of the flask to a leak-free
polyethylene bottle. Rinse the flask twice with 5-ml portions of
deionized, distilled water and add the rinse water to the bottle.
Adjust the pH to between 9 and 12 by adding sodium hydroxide (1 N),
dropwise (about 25 to 35 drops). Check the pH by dipping a stirring rod
into the solution and then touching the rod to the pH test paper.
Remove as little material as possible during this step. Mark the height
of the liquid level so that the container can be checked for leakage
after transport. Label the container to clearly identify its contents.
Seal the container for shipping.
4.3 Analysis. Note the level of the liquid in container and confirm
whether or not any sample was lost during shipment; note this on the
analytical data sheet. If a noticeable amount of leakage has occurred,
either void the sample or use methods, subject to the approval of the
Administrator, to correct the final results. Immediately prior to
analysis, transfer the contents of the shipping container to a 50-ml
volumetric flask, and rinse the container twice with 5-ml portions of
deionized, distilled water. Add the rinse water to the flask and dilute
to the mark with deionized, distilled water; mix thoroughly. Pipette a
25-ml aliquot into the procelain evaporating dish. Return any unused
portion of the sample to the polyethylene storage bottle. Evaporate the
25-ml aliquot to dryness on a steam bath and allow to cool. Add 2 ml
phenoldisulfonic acid solution to the dried residue and triturate
thoroughly with a polyethylene policeman. Make sure the solution
contacts all the residue. Add 1 ml deionized, distilled water and four
drops of concentrated sulfuric acid. Heat the solution on a steam bath
for 3 minutes with occasional stirring. Allow the solution to cool, add
20 ml deionized, distilled water, mix well by stirring, and add
concentrated ammonium hydroxide, dropwise, with constant stirring, until
the pH is 10 (as determined by pH paper). If the sample contains
solids, these must be removed by filtration (centrifugation is an
acceptable alternative, subject to the approval of the Administrator),
as follows: filter through Whatman No. 41 filter paper into a 100-ml
volumetric flask; rinse the evaporating dish with three 5-ml portions
of deionized, distilled water; filter these three rinses. Wash the
filter with at least three 15-ml portions of deionized, distilled water.
Add the filter washings to the contents of the volumetric flask and
dilute to the mark with deionized, distilled water. If solids are
absent, the solution can be transferred directly to the 100-ml
volumetric flask and diluted to the mark with deionized, distilled
water. Mix the contents of the flask thoroughly, and measure the
absorbance at the optimum wavelength used for the standards (Section
5.2.1), using the blank solution as a zero reference. Dilute the sample
and the blank with equal volumes of deionized, distilled water if the
absorbance exceeds A4, the absorbance of the 400 g NO2 standard (see
Section 5.2.2).
4.4 Audit Sample Analysis. Concurrently analyze the two audit
samples and a set of compliance samples (Section 4.3) in the same manner
to evaluate the technique of the analyst and the standards preparation.
(Note: It is recommended that known quality control samples be analyzed
prior to the compliance and audit sample analysis to optimize the system
accuracy and precision. One source of these samples is the Source Branch
listed in Section 3.3.9.) The same analysts, analytical reagents, and
analytical system shall be used both for the compliance samples and the
EPA audit samples; if this condition is met, auditing of subsequent
compliance analyses for the same enforcement agency within 30 days is
not required. An audit sample set may not be used to validate different
sets of compliance samples under the jurisdiction of different
enforcement agencies, unless prior arrangements are made with both
enforcement agencies.
Calculate the concentrations in mg/dscm using the specified sample
volume in the audit instructions. (Note: Indication of acceptable
results may be obtained immediately by reporting the audit results in
mg/dscm and compliance results in total mg NO2/sample by telephone to
the responsible enforcement agency.) Include the results of both audit
samples, their identification numbers, and the analyst's name with the
results of the compliance determination samples in appropriate reports
to the EPA regional office or the appropriate enforcement agency.
Include this information with subsequent compliance analyses for the
same enforcement agency during the 30-day period.
The concentrations of the audit samples obtained by the analyst shall
agree within 10 percent of the actual audit concentrations. If the
10-percent specification is not met, reanalyze the compliance samples
and audit samples and include initial and reanalysis values in the test
report (see Note in the first paragraph of this section).
Failure to meet the 10-percent specification may require retests
until the audit problems are resolved. However, it the audit results do
not affect the compliance or noncompliance status of the affected
facility, the Administrator may waive the reanalysis requirement,
further audits, or retests and accept the results of the compliance
test. While steps are being taken to resolve audit analysis problems,
the Administrator may also choose to use the data to determine the
compliance or noncompliance status of the affected facility.
5. Calibration
5.1 Flask Volume. The volume of the collection flask-flask valve
combination must be known prior to sampling. Assemble the flask and
flask valve and fill with water, to the stopcock. Measure the volume of
water to 10 ml. Record this volume on the flask.
5.2 Spectrophotometer Calibration.
5.2.1 Optimum Wavelength Determination. Calibrate the wavelength
scale of the spectrophotometer every 6 months. The calibration may be
accomplished by using an energy source with an intense line emission
such as a mercury lamp, or by using a series of glass filters spanning
the measuring range of the spectrophotometer. Calibration materials are
available commercially and from the National Bureau of Standards.
Specific details on the use of such materials should be supplied by the
vendor; general information about calibration techniques can be
obtained from general reference books on analytical chemistry. The
wavelength scale of the spectrophotometer must read correctly within 5
nm at all calibration points; otherwise, the spectrophotometer shall be
repaired and recalibrated. Once the wavelength scale of the
spectrophotometer is in proper calibration, use 410 nm as the optimum
wavelength for the measurement of the absorbance of the standards and
samples.
Alternatively, a scanning procedure may be employed to determine the
proper measuring wavelength. If the instrument is a double-beam
spectrophotometer, scan the spectrum between 400 and 415 nm using a 200
g NO2 standard solution in the sample cell and a blank solution in the
reference cell. If a peak does not occur, the spectrophotometer is
probably malfunctioning and should be repaired. When a peak is obtained
within the 400 to 415 nm range, the wavelength at which this peak occurs
shall be the optimum wavelength for the measurement of absorbance of
both the standards and the samples. For a single-beam
spectrophotometer, follow the scanning procedure described above, except
that the blank and standard solutions shall be scanned separately. The
optimum wavelength shall be the wavelength at which the maximum
difference in absorbance between the standard and the blank occurs.
5.2.2 Determination of Spectrophotometer Calibration Factor Kc. Add
0.0 ml, 2 ml, 4 ml, 6 ml., and 8 ml of the KNO3 working standard
solution (1 ml=100 g NO2) to a series of five 50-ml volumetric flasks.
To each flask, add 25 ml of absorbing solution, 10 ml deionized,
distilled water, and sodium hydroxide (1 N) dropwise until the pH is
between 9 and 12 (about 25 to 35 drops each). Dilute to the mark with
deionized, distilled water. Mix thoroughly and pipette a 25-ml aliquot
of each solution into a separate porcelain evaporating dish. Beginning
with the evaporation step, follow the analysis procedure of Section 4.3
until the solution has been transferred to the 100 ml volumetric flask
and diluted to the mark. Measure the absorbance of each solution, at
the optimum wavelength, as determined in Section 5.2.1. This calibration
procedure must be repeated on each day that samples are analyzed.
Calculate the spectrophotometer calibration factor as follows:
Eq. 7-1
Where:
Kc=Calibration factor, mg.
A1=Absorbance of the 100- g NO2 standard.
A2=Absorbance of the 200- g NO2 standard.
A3=Absorbance of the 300- g NO2 standard.
A4=Absorbance of the 400- g NO2 standard.
5.2.3 Spectrophotometer Calibration Quality Control. Multiply the
absorbance value obtained for each standard by the Kc factor (least
squares slope) to determine the distance each calibration point lies
from the theoretical calibration line. These calculated concentration
values should not differ from the actual concentrations (i.e., 100, 200,
300, and 400 mg NO2) by more than 7 percent for three of the four
standards.
5.3 Barometer. Calibrate against a mercury barometer.
5.4 Temperature Gauge. Calibrate dial thermometers against
mercury-in-glass thermometers.
5.5 Vacuum Gauge. Calibrate mechanical gauges, if used, against a
mercury manometer such as that specified in 2.1.6.
5.6 Analytical Balance. Calibrate against standard weights.
6. Calculations
Carry out the calculations, retaining at least one extra decimal
figure beyond that of the acquired data. Round off figures after final
calculations.
6.1 Nomenclature.
A=Absorbance of sample.
C=Concentration of NOx as NO2, dry basis, corrected to standard
conditions, mg/dscm (lb/dscf).
F=Dilution factor (i.e., 25/5, 25/10, etc., required only if sample
dilution was needed to reduce the absorbance into the range of
calibration).
Kc=Spectrophotometer calibration factor.
m=Mass of NOx as NO2 in gas sample, g.
Pf=Final absolute pressure of flask, mm Hg (in. Hg).
Pi=Initial absolute pressure of flask, mm Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
Tf=Final absolute temperature of flask, K ( R).
Ti=Initial absolute temperature of flask, K ( R).
Tstd=Standard absolute temperature 293 K (528 R).
Vsc=Sample volume at standard conditions (dry basis), ml.
Vf=Volume of flask and valve, ml.
Va=Volume of absorbing soluton, 25 ml.
2=50/25, the aliquot factor. (If other than a 25-ml aliquot was used
for analysis, the corresponding factor must be substituted).
6.2 Sample Volume, Dry Basis, Corrected to Standard Conditions.
Vsc= (Tstd/Pstd)(Vf ^Va)(Pf/Tf^Pi/Ti)
=K1 (Vf ^25 ml)(Pf/Tf^ Pi/Ti) Eq. 7-2
Where:
K1=0.3858 K/mm Hg for metric units
=17.64 R/in. Hg for English units.
6.3 Total mg NO2 Per Sample.
m= 2Kc A F Eq. 7-3
Note: If other than a 25-ml aliquot is used for analysis, the factor
2 must be replaced by a corresponding factor.
6.4 Sample Concentration, Dry Basis, Corrected to Standard
Conditions.
Insert illus. 252
Where:
K2=10 /3/ (mg/scm)/( g/ml) for metric units.
=6.242 10^5 (lb/scf)/( g/ml) for English units.
To convert from mg/dscm to g/dscm, divide C by 1,000.
6.5 Relative Error (RE) for QA Audit Samples, Percent.
Where:
Cd=Determined audit sample concentration, mg/dscm.
Ca=Actual audit sample concentration, mg/dscm.
7. Bibliography
1. Standard Methods of Chemical Analysis 6th ed. New York, D. Van
Nostrand Co., Inc. 1962. Vol. 1, p. 329-330.
2. Standard Method of Test for Oxides of Nitrogen in Gaseous
Combustion Products (Phenoldisulfonic Acid Procedure). In: 1968 Book
of ASTM Standards, Part 26. Philadephia, PA. 1968. ASTM Designation
D-1608-60, p. 725-729.
3. Jacob, M. B. The Chemical Analysis of Air Pollutants. New York.
Interscience Publisher, Inc. 1960. Vol. 10, p. 351-356.
4. Beatty, R. L., L. B. Berger, and H. H. Schrenk. Determination of
Oxides of Nitrogen by the Phenoldisulfonic Acid Method. Bureau of
Mines, U.S. Dept. of Interior. RI. 3687. February 1943.
5. Hamil, H. F. and D. E. Camann. Collaborative Study of method for
the Determination of Nitrogen Oxide Emissions from Stationary Sources
(Fossil Fuel-Fired Steam Generators). Southwest Research Institute
report for Environmental Protection Agency. Research Triangle Park, NC.
October 5, 1973.
6. Hamil, H. F. and R. E. Thomas. Collaborative Study of Method for
the Determination of Nitrogen Oxide Emissions from Stationary Sources
(Nitric Acid Plants). Southwest Research Institute report for
Environmental Protection Agency. Research Triangle Park, NC. May 8,
1974.
3Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
40 CFR 60.748 Pt. 60, App. A, Meth. 7A
1. Applicability and Principle
1.1 Applicability. This method applies to the measurement of nitrogen
oxides emitted from stationary sources; it may be used as an
alternative to Method 7 (as defined in 40 CFR Part 60.8(b)) to determine
compliance if the stack concentration is within the analytical range.
The analytical range of the method is from 125 to 1,250 mg NOx/m3 as NO2
(65 to 655 ppm), and higher concentrations may be analyzed by diluting
the sample. The lower detection limit is approximately 19 mg/m3 (10
ppm), but may vary among instruments.
1.2 Principle. A grab sample is collected in an evacuated flask
containing a diluted sulfuric acid-hydrogen peroxide absorbing solution.
The nitrogen oxides, except nitrous oxide, are oxidized to nitrate and
measured by ion chromatography.
2. Apparatus
2.1 Sampling. Same as in Method 7, Section 2.1.
2.2 Sampling Recovery. Same as in Method 7, Section 2.2, except the
stirring rod and pH paper are not needed.
2.3 Analysis. For the analysis, the following equipment is needed.
Alternative instrumentation and procedures will be allowed provided the
calibration precision in Section 5.2 and acceptable audit accuracy can
be met.
2.3.1 Volumetric Pipets. Class A; 1-, 2-, 4-, 5-ml (two for the set
of standards and one per sample), 6-, 10-, and graduated 5-ml sizes.
2.3.2 Volumetric Flasks. 50-ml (two per sample and one per
standard), 200-ml, and 1-liter sizes.
2.3.3 Analytical Balance. To measure to within 0.1 mg.
2.3.4 Ion Chromatograph. The ion chromatograph should have at least
the following components:
2.3.4.1 Columns. An anion separation or other column capable of
resolving the nitrate ion from sulfate and other species present and a
standard anion suppressor column (optional). Suppressor columns are
produced as proprietary items; however, one can be produced in the
laboratory using the resin available from BioRad Company, 32nd and
Griffin Streets, Richmond, CA. Peak resolution can be optimized by
varying the eluent strength or column flow rate, or by experimenting
with alternative columns that may offer more efficient separation. When
using guard columns with the stronger reagent to protect the separation
column, the analyst should allow rest periods between injection
intervals to purge possible sulfate buildup in the guard column.
2.3.4.2 Pump. Capable of maintaining a steady flow as required by the
system.
2.3.4.3 Flow Gauges. Capable of measuring the specified system flow
rate.
2.3.4.4 Conductivity Detector.
2.3.4.5 Recorder. Compatible with the output voltage range of the
detector.
3. Reagents
Unless otherwise indicated, it is intended that all reagents conform
to the specifications established by the Committee on Analytical
Reagents of the American Chemical Society, where such specifications are
available; otherwise, use the best available grade.
3.1 Sampling. An absorbing solution consisting of sulfuric acid
(H2SO4) and hydrogen peroxide (H2O2) is required for sampling. To
prepare the absorbing solution, cautiously add 2.8 ml concentrated H2SO4
to a 1-liter flask containing water (same as Section 3.2). Add 6 ml of 3
percent H2O2 that has been freshly prepared from 30 percent solution.
Dilute to volume with water, and mix well. This absorbing solution
should be used within 1 week of its preparation. Do not expose to
extreme heat or direct sunlight.
Note: Biased testing results have been observed when sampling under
conditions of high sulfur dioxide concentrations (above 2000 ppm).
3.2 Sample Recovery. Deionized distilled water that conforms to
American Society for Testing and Materials Specification D 1193-74, Type
3, is required for sample recovery. At the option of the analyst, the
KMnO4 test for oxidizable organic matter may be omitted when high
concentrations of organic matter are not expected to be present.
3.3 Analysis. For the analysis, the following reagents are required:
3.3.1 Water. Same as in Section 3.2.
3.3.2 Stock Standard Solution, 1 mg NO2/ml. Dry an adequate amount
of sodium nitrate (NaNO3) at 105 to 110 C for a minimum of 2 hours just
before preparing the standard solution. Then dissolve exactly 1.847 g
of dried NaNO3 in water, and dilute to 1 liter in a volumetric flask.
Mix well. This solution is stable for 1 month and should not be used
beyond this time.
3.3.3 Working Standard Solution, 25 mg/ml. Dilute 5 ml of the
standard solution to 200 ml with water in a volumetric flask, and mix
well.
3.3.4 Eluent Solution. Weight 1.018 g of sodium carbonate (Na2CO3)
and 1.008 g of sodium bicarbonate (NaHCO3), and dissolve in 4 liters of
water. This solution is 0.0024 M Na2CO3/0.003 M NaHCO3. Other eluents
appropriate to the column type and capable of resolving nitrate ion from
sulfate and other species present may be used.
3.3.5 Quality Assurance Audit Samples. Same as required in Method 7.
4. Procedure
4.1 Sampling. Same as in Method 7, Section 4.1.
4.2 Sample Recovery. Same as in Method 7, Section 4.2, except delete
the steps on adjusting and checking the pH of the sample. Do not store
the samples more than 4 days between collection and recovery.
4.3 Sample. Preparation. Note the level of the liquid in the
container and confirm whether any sample was lost during shipment; note
this on the analytical data sheet. If a noticeable amount of leakage
has occurred, either void the sample or use methods, subject to the
approval of the Administrator, to correct the final results.
Immediately before analysis, transfer the contents of the shipping
container to a 50-ml volumetric flask, and rinse the container twice
with 5-ml portions of water. Add the rinse water to the flask, and
dilute to the mark with water. Mix thoroughly.
Pipet a 5-ml aliquot of the sample into a 50-ml volumetric flask, and
dilute to the mark with water. Mix thoroughly. For each set of
determinations, prepare a reagent blank by diluting 5 ml of absorbing
solution to 50 ml with water. (Alternatively, eluent solution may be
used in all sample, standard, and blank dilutions.)
4.4 Analysis. Prepare a standard calibration curve according to
Section 5.2. Analyze the set of standards followed by the set of samples
using the same injection volume for both standards and samples. Repeat
this analysis sequence followed by a final analysis of the standard set.
Average the results. The two sample values must agree within 5 percent
of their mean for the analysis to be valid. Perform this duplicate
analysis sequence on the same day. Dilute any sample and the blank with
equal volumes of water if the concentration exceeds that of the highest
standard.
Document each sample chromatogram by listing the following analytical
parameters: injection point, injection volume, nitrate and sulfate
retention times, flow rate, detector sensitivity setting, and recorder
chart speed.
4.5 Audit Sample Analysis. Same as required in Method 7.
5. Calibration
5.1 Flask Volume. Same as in Method 7, Section 5.1.
5.2 Standard Calibration Curve. Prepare a series of five standards
by adding 1.0, 2.0, 4.0, 6.0, and 10.0 ml of working standard solution
(25 mg/ml) to a series of five 50-ml volumetric flasks. (The standard
masses will equal 25, 50, 100, 150, and 250 mg.) Dilute each flask to
volume with water, and mix well. Analyze with the samples as described
in Section 4.4 and subtract the blank from each value. Prepare or
calculate a linear regression plot to the standard masses in mg (x-axis)
versus their peak height responses in millimeters (y-axis). (Take peak
height measurements with symmetrical peaks; in all other cases,
calculate peak areas.) From this curve, or equation, determine the
slope, and calculate its reciprocal to denote as the calibration factor,
S. If any point deviates from the line by more than 7 percent of the
concentration at that point, remake and reanalyze that standard. This
deviation can be determined by multiplying S times the peak height
response for each standard. The resultant concentrations must not
differ by more than 7 percent from each known standard mass (i.e., 25,
50, 100, 150, and 250 mg).
5.3 Conductivity Detector. Calibrate according to manufacturer's
specifications prior to initial use.
5.4 Barometer. Calibrate against a mercury barometer.
5.5 Temperature Gauge. Calibrate dial thermometers against
mercury-in-glass thermometers.
5.6 Vacuum Gauge. Calibrate mechanical gauges, if used, against a
mercury manometer such as that specified in Section 2.1.6 of Method 7.
5.7 Analytical Balance. Calibrate against standard weights.
6. Calculations
Carry out the calculations, retaining at least one extra decimal
figure beyond that of the acquired data. Round off figures after final
calculations.
6.1 Sample Volume. Calculate the sample volume Vsc (in ml) on a dry
basis, corrected to standard conditions, using Equation 7-2 of Method 7.
6.2 Sample Concentration of NOx as NO2. Calculate the sample
concentration C (in mg/dscm) as follows:
Where:
H =Sample peak height, mm.
S =Calibration factor, g/mm.
F =Dilution factor (required only if sample dilution was needed to
reduce the concentration into the range of calibration)
104 = 1:10 dilution times conversion factor of
To convert from mg/dscm to g/dscm, divide C by 1000.
If desired, the concentration of NO2 may be calculated as ppm NO2 at
standard conditions as follows:
Where:
0.5228 = ml/mg NO2.
7. Bibliography
1. Mulik, J. D. and E. Sawicki. Ion Chromatographic Analysis of
Environmental Pollutants. Ann Arbor, Ann Arbor Science Publishers, Inc.
Vol. 2, 1979.
2. Sawicki, E., J. D. Mulik, and E. Wittgenstein. Ion
Chromatographic Analysis of Environmental Pollutants. Ann Arbor, Ann
Arbor Science Publishers, Inc. Vol. 1. 1978.
3. Siemer, D. D. Separation of Chloride and Bromide from Complex
Matrices Prior to Ion Chromatographic Determination. Analytical
Chemistry 52(12:1874-1877). October 1980.
4. Small, H., T. S. Stevens, and W. C. Bauman. Novel Ion Exchange
Chromatographic Method Using Conductimetric Determination. Analytical
Chemistry. 47(11:1801). 1975.
5. Yu, King K. and Peter R. Westlin. Evaluation of Reference Method
7 Flask Reaction Time. Source Evaluation Society Newsletter. 4(4).
November 1979. 10 p.
40 CFR 60.748 Pt. 60, App., A, Meth. 7B
1. Applicability and Principle
1.1 Applicability. This method is applicable to the measurement of
nitrogen oxides emitted from nitric acid plants. The range of the
method as outlined has been determined to be 57 to 1,500 milligrams NOx
(as NO2) per dry standard cubic meter, or 30 to 786 ppm NOx (as NO2),
assuming corresponding standards are prepared.
1.2 Principle. A grab sample is collected in an evacuated flask
containing a dilute sulfuric acid-hydrogen peroxide absorbing solution;
and the nitrogen oxides, except nitrous oxide, are measured by
ultraviolet absorption.
2. Apparatus
2.1 Sampling. Same as Method 7, Section 2.1.1 through Section 2.1.11.
2.2 Sample Recovery. The following equipment is required for sample
recovery:
2.2.1 Wash Bottle. Polyethylene or glass.
2.2.2 Volumetric Flasks. 100-ml (one for each sample).
2.3 Analysis. The following equipment is needed for analysis:
2.3.1 Volumetric Pipettes. 5-, 10-, 15-, and 20-ml to make standards
and sample dilutions.
2.3.2 Volumetric Flasks. 1000- and 100-ml for preparing standards
and dilution of samples.
2.3.3 Spectrophotometer. To measure ultraviolet absorbance at 210 nm.
2.3.4 Analytical Balance. To measure to within 0.1 mg.
3. Reagents
Unless otherwise indicated, all reagents are to conform to the
specifications established by the committee on analytical reagents of
the American Chemical Society, where such specifications are available.
Otherwise, use the best available grade.
3.1 Sampling. Same as Method 7, Section 3.1. It is important that the
amount of hydrogen peroxide in the absorbing solution not be increased.
Higher concentrations of peroxide may interfere with sample analysis.
3.2 Sample Recovery. Same as for Method 7, Section 3.2.2.
3.3 Analysis. Same as for Method 7, Sections 3.3.4, 3.3.5, and 3.3.7
with the addition of the following:
3.3.1 Working Standard KNO3 Solution. Dilute 10 ml of the standard
solution to 1000 ml with water. One milliliter of the working standard
is equivalent to 10 mg nitrogen dioxide (NO2).
3.3.2 Absorbing Solution. Same as in Section 3.1.
3.3.3 Quality Assurance Audit Samples. Nitrate samples are prepared
in glass vials by the Environmental Protection Agency (EPA),
Environmental Monitoring Systems Laboratory, Research Triangle Park,
North Carolina. Each set will consist of two vials with two unknown
concentrations. When making compliance determinations, obtain the audit
samples from the quality assurance management office at each EPA
regional office.
4. Procedures
4.1 Sampling. Same as Method 7, Sections 4.1.1 and 4.1.2.
4.2 Sample Recovery. Let the flask sit for a minimum of 16 hours,
and then shake the contents for 2 minutes. Connect the flask to a
mercury filled U-tube manometer. Open the valve from the flask to the
manometer, and record the flask temperature (Tf), the barometric
pressure, and the difference between the mercury levels in the
manometer. The absolute internal pressure in the flask (Pf) is the
barometric pressure less the manometer reading.
Transfer the contents of the flask to a 100-ml volumetric flask.
Rinse the flask three times with 10-ml portions of water, and add to the
volumetric flask. Dilute to 100 ml with water. Mix thoroughly. The
sample is now ready for analysis.
4.3 Analysis. Pipette a 20-ml aliquot of sample into a 100-ml
volumetric flask. Dilute to 100 ml with water. The sample is now ready
to be read by ultraviolet spectrophotometry. Using the blank as zero
reference, read the absorbance of the sample at 210 nm.
4.4 Audit Analysis. With each set of compliance samples or once per
analysis day, or once per week when averaging continuous samples,
analyze each performance audit in the same manner as the sample to
evaluate the analyst's technique and standard preparation. The same
person, the same reagents, and the same analytical system must be used
both for compliance determination samples and the EPA audit samples.
Report the results of all audit samples with the results of the
compliance determination samples. The relative error will be determined
by the regional office or the appropriate enforcement agency.
5. Calibration
Same as Method 7, Section 5.1 and Sections 5.3 through 5.6 with the
addition of the following:
5.1 Determination of Spectrophotometer Standard Curve. Add 0.0 ml, 5
ml, 10 ml, 15 ml, and 20 ml of the KNO3 working standard solution (1 ml=
10 g NO2) to a series to five 100-ml volumetric flasks. To each flask,
add 5 ml of absorbing solution. Dilute to the mark with water. The
resulting solutions contain 0.0, 50, 100, 150, and 200 g NO2,
respectively. Measure the absorbance by ultraviolet spectrophotometry
at 210 nm, using the blank as a zero reference. Prepare a standard
curve plotting absorbance vs. g NO2.
Note: If other than a 20-ml aliquot of sample is used for analysis,
then the amount of absorbing solution in the blank and standards must be
adjusted such that the same amount of absorbing solution is in the blank
and standards as is in the aliquot of sample used. Calculate the
spectrophotometer calibration factor Kc as follows:
insert illus. 0422A
Where:
mi=Mass of NO2 in standard i, g.
Ai=Absorbance of NO2 standard i.
N=Total number of calibration standards.
For the set of calibration standards specified here, Equation 7-1
simplifies to the following:
6. Calculations
Same as Method 7, Sections 6.1, 6.2, and 6.4 with the addition of the
following:
6.1 Total g NO2 Per Sample:
Where:
5=100/20, the aliquot factor.
Note: If other than a 20-ml aliquot is used for analysis, the factor
5 must be replaced by a corresponding factor.
6.2 Relative Error (RE) for Quality Assurance Audits.
Where:
Cd=Determined audit concentration.
Ca=Actual audit concentration.
7. Bibliography
1. National Institute for Occupational Safety and Health
Recommendations for Occupational Exposure to Nitric Acid. In:
Occupational Safety and Health Reporter. Washington, DC. Bureau of
National Affairs, Inc. 1976. p. 149.
2. Rennie, P.J., A.M. Sumner, and F.B. Basketter. ''Determination of
Nitrate in Raw, Potable, and Waste Waters by Ultraviolet
Spectrophotometry.'' ''Analyst.'' Vol. 104. September 1979. p. 837.
40 CFR 60.748 Pt. 60, App. A, Meth. 7C
1. Applicability, Principle, Interferences, Precision, Bias, and
Stability
1.1 Applicability. The method is applicable to the determination of
NOx emissions from fossil-fuel fired steam generators, electric utility
plants, nitric acid plants, or other sources as specified in the
regulations. The lower detectable limit is 13 mg NOx/m3, as NO2 (7 ppm
NOx) when sampling at 500 cc/min for 1 hour. No upper limit has been
established; however, when using the recommended sampling conditions,
the method has been found to collect NOx emissions quantitatively up to
1,782 mg NOx/m3, as NO2 (932 ppm NOx).
1.2 Principle. An integrated gas sample is extracted from the stack
and collected in alkaline-potassium permanganate solution; NOx (NO+NO2)
emissions are oxidized to NO2- and NO3-. The NO3- is reduced to NO2-
with cadmium, and the NO2- is analyzed colorimetrically.
1.3 Interferences. Possible interferences are SO2 and NH3. High
concentrations of SO2 could interfere because SO2 consumes MnO4- (as
does NOx) and, therefore, could reduce the NOx collection efficiency.
However, when sampling emissions from a coal-fired electric utility
plant burning 2.1-percent sulfur coal with no control of SO2 emissions,
collection efficiency was not reduced. In fact, calculations show that
sampling 3000 ppm SO2 will reduce the MnO4- concentration by only 5
percent if all the SO2 is consumed in the first impinger.
NH3 is slowly oxidized to NO3- by the absorbing solution. At 100 ppm
NH3 in the gas stream, an interference of 6 ppm NOx (11 mg NO2/m3) was
observed when the sample was analyzed 10 days after collection.
Therefore, the method may not be applicable to plants using NH3
injection to control NOx emissions unless means are taken to correct the
results. An equation has been developed to allow quantitation of the
interference and is discussed in Citation 5 of the Bibliography.
1.4 Precision and Bias. The method does not exhibit any bias
relative to Method 7. The within-laboratory relative standard deviation
for a single measurement is 2.8 and 2.9 percent at 201 and 268 ppm NOx,
respectively.
1.5 Stability. Collected samples are stable for at least 4 weeks.
2. Apparatus
2.1 Sampling and Sample Recovery. The sampling train is shown in
Figure 7C-1, and component parts are discussed below. Alternative
apparatus and procedures are allowed provided acceptable accuracy and
precision can be demonstrated.
insert illus 0253
2.1.1 Probe. Borosilicate glass tubing, sufficiently heated to
prevent water condensation and equipped with an in-stack or out-stack
filter to remove particulate matter (a plug of glass wool is
satisfactory for this purpose). Stainless steel or Teflon tubing may
also be used for the probe. (Note: Mention of trade names or specific
products does not constitute endorsement by the U.S. Environmental
Protection Agency.)
2.1.2 Impingers. Three restricted-orifice glass impingers, having the
specifications given in Figure 7C-2, are required for each sampling
train. The impingers must be connected in series with leak-free glass
connectors. Stopcock grease may be used, if necessary, to prevent
leakage. (The impingers can be fabricated by a glass blower until they
become available commercially.)
Insert illus 0255
2.1.3 Glass Wool, Stopcock Grease, Drying Tube, Valve, Pump,
Barometer, and Vacuum Gauge and Rotameter. Same as in Method 6,
Sections 2.1.3, 2.1.4, 2.1.6, 2.1.7, 2.1.8, 2.1.11, and 2.1.12,
respectively.
2.1.4 Rate Meter. Rotameter, or equivalent, accurate to within 2
percent at the selected flow rate between 400 and 500 cc/min. For
rotameters, a range of 0 to 1 liter/min is recommended.
2.1.5 Volume Meter. Dry gas meter capable of measuring the sample
volume, under the sampling conditions of 400 to 500 cc/min for 60
minutes within an accuracy of 2 percent.
2.1.6 Filter. To remove NOx from ambient air, prepared by adding 20 g
of a 5-angstrom molecular sieve to a cylindrical tube, e.g., a
polyethylene drying tube.
2.1.7 Polyethylene Bottles. 1-liter, for sample recovery.
2.1.8 Funnel and Stirring Rods. For sample recovery.
2.2 Sample Preparation and Analysis.
2.2.1 Hot Plate. Stirring type with 50- by 10-mm Teflon-coated
stirring bars.
2.2.2 Beakers. 400-, 600-, and 1000-ml capacities.
2.2.3 Filtering Flask. 500-ml capacity with side arm.
2.2.4 Buchner Funnel. 75-mm ID, with spout equipped with a 13-mm ID
by 90-mm long piece of Teflon tubing to minimize possibility of
aspirating sample solution during filtration.
2.2.5 Filter Paper. Whatman GF/C, 7.0-cm diameter.
2.2.6 Stirring Rods.
2.2.7 Volumetric Flasks. 100-, 200- or 250-, 500-, and 1000-ml
capacity.
2.2.8 Watch Glasses. To cover 600- and 1,000-ml beakers.
2.2.9 Graduated Cylinders. 50- and 250-ml capacities.
2.2.10 Pipettes. Class A
2.2.11 pH Meter. To measure pH from 0.5 to 12.0
2.2.12 Burette. 50-ml with a micrometer type stopcock. (The stopcock
is Catalogue No. 8225-t-05, Ace Glass, Inc., Post Office Box 996,
Louisville, Kentucky 50201.) Place a glass wool plug in bottom of
burette. Cut off burette at a height of 43 cm from the top of plug, and
have a glass blower attach a glass funnel to top of burette such that
the diameter of the burette remains essentially unchanged. Other means
of attaching the funnel are acceptable.
2.2.13 Glass Funnel. 75-mm ID at the top.
2.2.14 Spectrophotometer. Capable of measuring absorbance at 540 nm.
One-cm cells are adequate.
2.2.15 Metal Thermometers. Bimetallic thermometers, range 0 to 150
C.
2.2.16 Culture Tubes. 20- by 150-mm, Kimax No. 45048.
2.2.17 Parafilm ''M.'' Obtained from American Can Company, Greenwich,
Connecticut 06830.
2.2.18 CO2 Measurement Equipment. Same as in Method 3.
3. Reagents
Unless otherwise indicated, all reagents should conform to the
specifications established by the Committee on Analytical Reagents of
the American Chemical Society, where such specifications are available;
otherwise, use the best available grade.
3.1 Sampling.
3.1.1 Water. Deionized distilled to conform to ASTM Specification D
1193-74, Type 3 (incorporated by reference -- see 60.17).
3.1.2 Potassium Permanganate, 4.0 percent (w/w), Sodium Hydroxide,
2.0 percent (w/w). Dissolve 40.0 g of KMnO4 and 20.0 g of NaOH in 940
ml of water.
3.2 Sample Preparation and Analysis.
3.2.1 Water. Same as in Section 3.1.1.
3.2.2 Sulfuric Acid. Concentrated H2SO4.
3.2.3 Oxalic Acid Solution. Dissolve 48 g of oxalic acid ((COOH)2
2H2O) in water, and dilute to 500 ml. Do not heat the solution.
3.2.4 Sodium Hydroxide, 0.5 N. Dissolve 20 g of NaOH in water, and
dilute to 1 liter.
3.2.5 Sodium Hydroxide, 10 N. Dissolve
40 g of NaOH in water and dilute to 100 ml.
3.2.6 Ethylenediamine Tetraacetic Acid (EDTA) Solution, 6.5 Percent.
Dissolve 6.5 g of EDTA (disodium salt) in water, and dilute to 100 ml.
Solution is best accomplished by using a magnetic stirrer.
3.2.7 Column Rinse Solution. Add 20 ml of 6.5 percent EDTA solution
to 960 ml of water, and adjust the pH to 11.7 to 12.0 with 0.5 N NaOH.
3.2.8 Hydrochloric Acid (HCl), 2 N. Add 86 ml of concentrated HCl to
a 500-ml volumetric flask containing water, dilute to volume, and mix
well. Store in a glass-stoppered bottle.
3.2.9 Sulfanilamide Solution. Add 20 g of sulfanilamide (melting
point 165 to 167 C) to 700 ml of water. Add, with mixing, 50 ml
concentrated phosphoric acid (85 percent), and dilute to 1000 ml. This
solution is stable for at least 1 month, if refrigerated.
3.2.10 N-(1-Naphthyl)-Ethylenediamine Dihydrochloride (NEDA)
Solution. Dissolve 0.5 g of NEDA in 500 ml of water. An aqueous
solution should have one absorption peak at 320 nm over the range of 260
to 400 nm. NEDA, showing more than one absorption peak over this range,
is impure and should not be used. This solution is stable for at least
1 month if protected from light and refrigerated.
3.2.11 Cadmium. Obtained from Matheson Coleman and Bell, 2909
Highland Avenue, Norwood, Ohio 45212, as EM Laboratories Catalogue No.
2001. Prepare by rinsing in 2 N HCl for 5 minutes until the color is
silver-grey. Then rinse the cadmium with water until the rinsings are
neutral when tested with pH paper. CAUTION: H2 is liberated during
preparation. Prepare in an exhaust hood away from any flame.
3.2.12 NaNO2 Standard Solution, Nominal Concentration, 1000 mg
NO2-/ml. Desiccate NaNO2 overnight. Accurately weigh 1.4 to 1.6 g of
NaNO2 (assay of 97 percent NaNO2 or greater), dissolve in water, and
dilute to 1 liter. Calculate the exact NO2- concentration from the
following relationship:
This solution is stable for at least 6 months under laboratory
conditions.
3.2.13 KNO3 Standard Solution. Dry KNO3 at 110 C for 2 hours, and
cool in a desiccator. Accurately weigh 9 to 10 g of KNO3 to within 0.1
mg, dissolve in water, and dilute to 1 liter. Calculate the exact NO3-
concentration from the following relationship:
This solution is stable for 2 months without preservative under
laboratory conditions.
3.2.14 Spiking Solution. Pipette 7 ml of the KNO3 standard into a
100-ml volumetric flask, and dilute to volume.
3.2.15 Blank Solution. Dissolve 2.4 g of KMnO4 and 1.2 g of NaOH in
96 ml of water. Alternatively, dilute 60 ml of KMnO4/NaOH solution to
100 ml.
3.2.16 Quality Assurance Audit Samples. Same as in Method 7, Section
3.3.9. When requesting audit samples, specify that they be in the
appropriate concentration range for Method 7C.
4. Procedure
4.1 Sampling.
4.1.1 Preparation of Collection Train. Add 200 ml of KMnO4/NaOH
solution (3.1.2) to each of three impingers, and assemble the train as
shown in Figure 7C-1. Adjust probe heater to a temperature sufficient
to prevent water condensation.
4.1.2 Leak-Check Procedure. A leak-check prior to the sampling run
should be carried out; a leak-check after the sampling run is
mandatory. Carry out the leak-check(s) according to Method 6, Section
4.1.2.
4.1.3 Check of Rotameter Calibration Accuracy (Optional). Disconnect
the probe from the first impinger, and connect the filter (2.1.6). Start
the pump, and adjust the rotameter to read between 400 and 500 cc/min.
After the flow rate has stabilized, start measuring the volume sampled,
as recorded by the dry gas meter (DGM), and the sampling time. Collect
enough volume to measure accurately the flow rate, and calculate the
flow rate. This average flow rate must be less than 500 cc/min for the
sample to be valid; therefore, it is recommended that the flow rate be
checked as above prior to each test.
4.1.4 Sample Collection. Record the initial DGM reading and
barometric pressure. Determine the sampling point or points according
to the appropriate regulations, e.g., 60.46(c) of 40 CFR Part 60.
Position the tip of the probe at the sampling point, connect the probe
to the first impinger, and start the pump. Adjust the sample flow to a
value between 400 and 500 cc/min. CAUTION: HIGHER FLOW RATES WILL
PRODUCE LOW RESULTS. Once adjusted, maintain a constant flow rate
during the entire sampling run. Sample for 60 minutes. For relative
accuracy (RA) testing of continuous emission monitors, the minimum
sampling time is 1 hour, sampling 20 minutes at each traverse point.
(Note. -- When the SO2 concentration is greater than 1200 ppm, the
sampling time may have to be reduced to 30 minutes to eliminate plugging
of the impinger orifice with MnO2. For RA tests with SO2 greater than
1200 ppm, sample for 30 minutes (10 minutes at each point)). Record the
DGM temperature, and check the flow rate at least every 5 minutes. At
the conclusion of each run, turn off the pump, remove probe from the
stack, and record the final readings. Divide the sample volume by the
sampling time to determine the average flow rate. Conduct a leak-check
as in Section 4.1.2. If a leak is found, void the test run, or use
procedures acceptable to the Administrator to adjust the sample volume
for the leakage.
4.1.5 CO2 Measurement. During sampling, measure the CO2 content of
the stack gas near the sampling point using Method 3. The single-point
grab sampling procedure is adequate, provided the measurements are made
at least three times -- near the start, midway, and before the end of a
run and the average CO2 concentration is computed. The Orsat or Fyrite
analyzer may be used for this analysis.
4.2 Sample Recovery. Disconnect the impingers. Pour the contents of
the impingers into a 1-liter polyethylene bottle using a funnel and a
stirring rod (or other means) to prevent spillage. Complete the
quantitative transfer by rinsing the impingers and connecting tubes with
water until the rinsings are clear to light pink, and add the rinsings
to the bottle. Mix the sample, and mark the solution level. Seal and
identify the sample container.
4.3 Sample Preparation for Analysis. Prepare a cadmium reduction
column as follows: Fill the burette (2.2.12) with water. Add freshly
prepared cadmium slowly with tapping until no further settling occurs.
The height of the cadmium column should be 39 cm. When not in use,
store the column under rinse solution (3.2.7). (Note. -- The column
should not contain any bands of cadmium fines. This may occur if
regenerated column is used and will greatly reduce the column lifetime.)
Note the level of liquid in the sample container, and determine
whether any sample was lost during shipment. If a noticeable amount of
leakage has occurred, the volume lost can be determined from the
difference between initial and final solution levels, and this value can
then be used to correct the analytical result. Quantitatively transfer
the contents to a 1-liter volumetric flask, and dilute to volume.
Take a 100-ml aliquot of the sample and blank (unexposed KMnO4/NaOH)
solutions, and transfer to 400-ml beakers containing magnetic stirring
bars. Using a pH meter, add concentrated H2SO4 with stirring until a pH
of 0.7 is obtained. Allow the solutions to stand for 15 minutes. Cover
the beakers with watch glasses, and bring the temperature of the
solutions to 50 C. Keep the temperature below 60 C. Dissolve 4.8 g
of oxalic acid in a minimum volume of water, approximately 50 ml, at
room temperature. Do not heat the solution. Add this solution slowly,
in increments, until the KMnO4 solution becomes colorless. If the color
is not completely removed, prepare some more of the above oxalic acid
solution, and add until a colorless solution is obtained. Add an excess
of oxalic acid by dissolving 1.6 g of oxalic acid in 50 ml of water, and
add 6 ml of this solution to the colorless solution. If suspended
matter is present, add concentrated H2SO4 until a clear solution is
obtained.
Allow the samples to cool to near room temperature, being sure that
the samples are still clear. Adjust the pH to 11.7 to 12.0 with 10 N
NaOH. Quantitatively transfer the mixture to a Buchner funnel
containing GF/C filter paper, and filter the precipitate. Filter the
mixture into a 500-ml filtering flask. Wash the solid material four
times with water. When filtration is complete, wash the Teflon tubing,
quantitatively transfer the filtrate to a 500-ml volumetric flask, and
dilute to volume. The samples are now ready for cadmium reduction.
Pipette a 50-ml aliquot of the sample into a 150-ml beaker, and add a
magnetic stirring bar. Pipette in 1.0 ml of 6.5 percent EDTA solution,
and mix.
Determine the correct stopcock setting to establish a flow rate of 7
to 9 ml/min of column rinse solution through the cadmium reduction
column. Use a 50-ml graduated cylinder to collect and measure the
solution volume. After the last of the rinse solution has passed from
the funnel into the burette, but before air entrapment can occur, start
adding the sample, and collect it in a 250-ml graduated cylinder.
Complete the quantitative transfer of the sample to the column as the
sample passes through the column. After the last of the sample has
passed from the funnel into the burette, start adding 60 ml of column
rinse solution, and collect the rinse solution until the solution just
disappears from the funnel. Quantitatively transfer the sample to a
200-ml volumetric flask (250-ml may be required), and dilute to volume.
The samples are now ready for NO2- analysis. (Note. -- Both the sample
and blank should go through this procedure. Additionally, two spiked
samples should be run with every group of samples passed through the
column. To do this, prepare two additional 50-ml aliquots of the sample
suspected to have the highest NO3- concentration, and add 1 ml of the
spiking solution to these aliquots. If the spike recovery or column
efficiency (see 6.2.1) is below 95 percent, prepare a new column, and
repeat the cadmium reduction).
4.4 Sample Analysis. Pipette 10 ml of sample into a culture tube.
(Note. -- Some test tubes give a high blank NO2- value but culture tubes
do not.) Pipette in 10 ml of sulfanilamide solution and 1.4 ml of NEDA
solution. Cover the culture tube with parafilm, and mix the solution.
Prepare a blank in the same manner using the sample from treatment of
the unexposed KMnO4/NaOH solution (3.1.2). Also, prepare a calibration
standard to check the slope of the calibration curve. After a 10-minute
color development interval, measure the absorbance at 540 nm against
water. Read g NO2-/ml from the calibration curve. If the absorbance
is greater than that of the highest calibration standard, pipette less
than 10 ml of sample and enough water to make the total sample volume 10
ml, and repeat the analysis. Determine the NO2 concentration using the
calibration curve obtained in Section 5.3.
4.5 Audit Analysis. This is the same as in Method 7, Section 4.4.
5. Calibration
5.1 Dry Gas Metering System (DGM).
5.1.1 Initial Calibration. Same as in Method 6, Section 5.1.1. For
detailed instructions on carrying out this calibration, it is suggested
that Section 3.5.2 of Citation 4 in the Bibiography be consulted.
5.1.2 Post-Test Calibration Check. Same as in Method 6, Section
5.1.2.
5.2 Thermometers for DGM and Barometer. Same as in Method 6,
Sections 5.2 and 5.4, respectively.
5.3 Calibration Curve for Spectrophotometer. Dilute 5.0 ml of the
NaNO2 standard solution to 200 ml with water. This solution nominally
contains 25 g NO2-/ml. Use this solution to prepare calibration
standards to cover the range of 0.25 to 3.00 g NO2-/ml. Prepare a
minimum of three standards each for the linear and slightly nonlinear
(described below) range of the curve. Use pipettes for all additions.
Run standards and a water blank as instructed in Section 4.4. Plot
the net absorbance vs gNO2-/ml. Draw a smooth curve through the
points. The curve should be linear up to an absorbance of approximately
1.2 with a slope of approximately 0.53 absorbance units/ g NO2-/ml. The
curve should pass through the origin. The curve is slightly nonlinear
from an absorbance of 1.2 to 1.6.
6. Calculations
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after final
calculation.
6.1 Sample volume, dry basis, corrected to standard conditions.
Where:
Vm(std)=Dry gas volume measured by the dry gas meter, corrected to
standard conditions, dscm.
Vm=Dry gas volume as measured by the dry gas meter, dcm.
Y=Dry gas meter calibration factor.
X=Correction factor for CO2 collection.
Pbar=Barometric pressure, mm Hg.
Pstd=Standard absolute pressure, 760 mm Hg.
Tm=Average dry gas meter absolute temperature, K.
Tstd=Standard absolute temperature, 293 K.
K1=0.3858 K/mm Hg.
6.2 Total mg NO2 Per Sample.
6.2.1 Efficiency of Cadmium Reduction Column. Calculate this value
as follows:
Insert illus 0266A
Where:
E=Column efficiency, unitless.
x=Analysis of spiked sample, mg NO2-/ml.
y=Analysis of unspiked sample, mg NO2-/ml.
200=Final volume of sample and blank after passing through the
column, ml
s=Concentration of spiking solution, mg NO3^/ml.
1.0=Volume of spiking solution added, ml.
46.01=mg NO2-/mmole.
62.01=mg NO3-/mmole.
6.2.2 Total mg NO2.
Where:
m=Mass of NOx, as NO2, in sample, mg.
S=Analysis of sample, mg NO2-/ml.
B=Analysis of blank, mg NO2-/ml.
500=Total volume of prepared sample, ml.
50=Aliquot of prepared sample processed through cadmium column, ml.
100=Aliquot of KMnO4/NaOH solution, ml.
1000=Total volume of KMnO4/NaOH solution ml.
6.3 Sample Concentration.
Where:
C=Concentration of NOx as NO2, dry basis, mg/dscm.
K2=10^3 mg/mg.
6.4 Conversion Factors.
1.0 ppm NO=1.247 mg NO/m3 at STP.
1.0 ppm NO2=1.912 mg NO2/m3 at STP.
1 ft3=2.832 10^2 m3.
1000 mg=1 g.
7. Quality Control
Quality control procedures are specified in Sections 4.1.3 (flow rate
accuracy); 4.3 (cadmium column efficiency); 4.4 (calibration curve
accuracy); and 4.5 (audit analysis accuracy).
8. Bibliography
1. Margeson, J.H., W.J. Mitchell, J.C. Suggs, and M.R. Midgett.
Integrated Sampling and Analysis Methods for Determining NOx Emissions
at Electric Utility Plants. U.S. Environmental Protection Agency,
Research Triangle Park, NC. Journal of the Air Pollution Control
Association. 32:1210-1215. 1982.
2. Memorandum and attachment from J.H. Margeson, Source Branch,
Quality Assurance Division, Environmental Monitoring Systems Laboratory,
to The Record, EPA. March 30, 1983. NH3 Interference in Methods 7C and
7D.
3. Margeson, J.H., J.C. Suggs, and M.R. Midgett. Reduction of Nitrate
to Nitrite with Cadmium. Anal. Chem. 52:1955-57. 1980.
4. Quality Assurance Handbook for Air Pollution Measurement Systems.
Volume III -- Stationary Source Specific Methods. August 1977. U.S.
Environmental Protection Agency. Research Triangle Park, NC.
Publication No. EPA-600/4-77-027b. August 1977.
5. Margeson, J.H., et al. An Integrated Method for Determining NOx
Emissions at Nitric Acid Plants. Manuscript submitted to Analytical
Chemistry. April 1984.
40 CFR 60.748 Pt. 60, App. A, Meth. 7D
1. Applicability, Principle, Interferences, Precision, Bias, and
Stability
1.1 Applicability. The method is applicable to the determination of
NOx emissions from fossil-fuel fired steam generators, electric utility
plants, nitric acid plants, or other sources as specified in the
regulations. The lower detectable limit is similar to that for Method
7C. No upper limit has been established; however, when using the
recommended sampling conditions, the method has been found to collect
NOx emissions quantitatively up to 1782 mg NOx/m3, as NO2 (932 pm NOx).
1.2 Principle. An integrated gas sample is extracted from the stack
and collected in alkaline-potassium permanganate solution; NOx (NO+NO2)
emissions are oxidized to NO3-. Then NO3- is analyzed by ion
chromatography.
1.3 Interferences. Possible interferences are SO2 and NH3. High
concentrations of SO2 could interfere because SO2 consumes MnO4- (as
does NOx) and, therefore, could reduce the NOx collection efficiency.
However, when sampling emissions from a coal-fired electric utility
plant burning 2.1-percent sulfur coal with no control of SO2 emissions,
collection efficiency was not reduced. In fact, calculations show that
sampling 3000 ppm SO2 will reduce the MnO4- concentration by only 5
percent if all the SO2 is consumed in the first impinger.
NH3 is slowly oxidized to NO3- by the absorbing solution. At 100 ppm
NH3 in the gas stream, an interference of 6 ppm NOx (11 mg NO2/m3) was
observed when the sample was analyzed 10 days after collection.
Therefore, the method may not be applicable to plants using NH3
injection to control NOx emissions unless means are taken to correct the
results. An equation has been developed to allow quantitation of the
interference and is discussed in Citation 4 of the Bibliography.
1.4 Precision and Bias. The method does not exhibit any bias
relative to Method 7. The within-laboratory relative standard deviation
for a single measurement was approximately 6 percent at 200 to 270 ppm
NOx.
1.5 Stability. Collected samples are stable for at least 4 weeks.
2. Apparatus
2.1 Sampling and Sample Recovery. The sampling train is the same as
in Figure 7C-1 of Method 7C. Component parts are the same as in Method
7C, Section 2.1.
2.2 Sample Preparation and Analysis.
2.2.1 Magnetic Stirrer. With 25- by 10-mm Teflon-coated stirring
bars.
2.2.2 Filtering Flask. 500-ml capacity with sidearm.
2.2.3 Buchner Funnel. 75-mm ID. The spout equipped with a 13-mm ID
by 90-mm long piece of Teflon tubing to minimize possibility of
aspirating sample solution during filtration.
2.2.4 Filter Paper. Whatman GF/C, 7.0-cm diameter.
2.2.5 Stirring Rods.
2.2.6 Volumetric Flask. 250-ml.
2.2.7 Pipettes. Class A.
2.2.8 Erlenmeyer Flasks. 250-ml.
2.2.9 Ion Chromatograph. Equipped with an anion separator column to
separate NO3-, a H+ suppressor, and necessary auxiliary equipment.
Nonsuppressed and other forms of ion chromatography may also be used
provided that adequate resolution of NO3- is obtained. The system must
also be able to resolve and detect NO2-.
3. Reagents
Unless otherwise indicated, all reagents should conform to the
specifications established by the Committee on Analytical Reagents of
the American Chemical Society, where such specifications are available;
otherwise, use the best available grade.
3.1 Sampling.
3.1.1 Water. Deionized distilled to conform to ASTM Specification D
1193-74, Type 3 (incorporated by reference -- see 60.17).
3.1.2 Potassium Permanganate, 4.0 Percent (w/w), Sodium Hydroxide,
2.0 Percent (w/w). Dissolve 40.0 g of KMnO4 and 20.0 g of NaOH in 940
ml of water.
3.2 Sample Preparation and Analysis.
3.2.1 Water. Same as in Section 3.1.1.
3.2.2 Hydrogen Peroxide, 5 Percent. Dilute 30 percent H2O2 1:5 (v/v)
with water.
3.2.3 Blank Solution. Dissolve 2.4 g of KMnO4and 1.2 g of NaOH in 96
ml of water. Alternatively, dilute 60 ml of KMnO4/NaOH solution to 100
ml.
3.2.4 KNO3 Standard Solution. Dry KNO3at 110 C for 2 hours, and
cool in a desiccator. Accurately weigh 9 to 10 g of KNO3to within 0.1
mg, dissolve in water, and dilute to 1 liter. Calculate the exact NO3-
concentration from the following relationship:
This solution is stable for 2 months without preservative under
laboratory conditions.
3.2.5 Eluent, 0.003 M NaHCO3/0.0024 M Na2CO3. Dissolve 1.008 g
NaHCO3and 1.018 g Na2CO3in water, and dilute to 4 liters. Other eluents
capable of resolving nitrate ion from sulfate and other species present
may be used.
3.2.6 Quality Assurance Audit Samples. This is the same as in Method
7, Section 3.3.9. When requesting audit samples, specify that they be in
the appropriate concentration range for Method 7D.
4. Procedure
4.1 Sampling. This is the same as in Method 7C, Section 4.1.
4.2 Sample Recovery. This is the same as in Method 7C, Section 4.2.
4.3 Sample Preparation for Analysis. Note the level of liquid in the
sample container, and determine whether any sample was lost during
shipment. If a noticeable amount of leakage has occurred, the volume
lost can be determined from the difference between initial and final
solution levels, and this value can then be used to correct the
analytical result. Quantitatively transfer the contents to a 1-liter
volumetric flask, and dilute to volume.
Sample preparation can be started 36 hours after collection. This
time is necessary to ensure that all NO2- is converted to NO3- Take a
50-ml aliquot of the sample and blank, and transfer to 250-ml Erlenmeyer
flasks. Add a magnetic stirring bar. Adjust the stirring rate to as
fast a rate as possible without loss of solution. Add 5 percent H2O2in
increments of approximately 5 ml using a 5-ml pipette. When the
KMnO4color appears to have been removed, allow the precipitate to
settle, and examine the supernatant liquid. If the liquid is clear, the
H2O2addition is complete. If the KMnO4color persists, add more H2O2,
with stirring, until the supernatant liquid is clear. (Note: The
faster the stirring rate, the less volume of H2O2that will be required
to remove the KMnO4.) Quantitatively transfer the mixture to a Buchner
funnel containing GF/C filter paper, and filter the precipitate. The
spout of the Buchner funnel should be equipped with a 13-mm ID by 90-mm
long piece of Teflon tubing. This modification minimizes the
possibility of aspirating sample solution during filtration. Filter the
mixture into a 500-ml filtering flask. Wash the solid material four
times with water. When filtration is complete, wash the Teflon tubing,
quantitatively transfer the filtrate to a 250-ml volumetric flask, and
dilute to volume. The sample and blank are now ready for NO3^analysis.
4.4 Sample Analysis. The following chromatographic conditions are
recommended: 0.003 M NaHCO3/0.0024 M Na2CO3 eluent solution. (3.2.5),
full scale range 3 MHO; sample loop, 0.5 ml; flow rate, 2.5 ml/min.
These conditions should give a NO3^ retention time of approximately 15
minutes (Figure 7D-1).
insert illus. 0276
Establish a stable baseline. Inject a sample of water, and determine
if any NO3^ appears in the chromatogram. If NO3^ is present, repeat the
water load/injection procedure approximately five times; then re-inject
a water sample, and observe the chromatogram. When no NO3^ is present,
the instrument is ready for use. Inject calibration standards. Then
inject samples and a blank. Repeat the injection of the calibration
standards (to compensate for any drift in response of the instrument).
Measure the NO3^peak height or peak area, and determine the sample
concentration from the calibration curve.
4.5 Audit analysis. This is the same as in Method 7, Section 4.4.
5. Calibration
5.1 Dry Gas Metering System (DGM).
5.1.1 Initial Calibration. Same as in Method 6, Section 5.1.1. For
detailed instructions on carrying out this calibration, it is suggested
that Section 3.5.2 of Citation 3 in the Bibliography be consulted.
5.1.2 Post-Test Calibration Check. Same as in Method 6, Section
5.1.2.
5.2 Thermometers for DGM and Barometer. Same as in Method 6, Section
5.2 and 5.4, respectively.
5.3 Calibration Curve for Ion Chromatograph. Dilute a given volume
(1.0 ml or greater) of the KNO3 standard solution to a convenient volume
with water, and use this solution to prepare calibration standards.
Prepare at least four standards to cover the range of the samples being
analyzed. Use pipettes for all additions. Run standards as instructed
in Section 4.4. Determine peak height or area, and plot the individual
values versus concentration in gNO3-/ml. Do not force the curve
through zero. Draw a smooth curve through the points. The curve should
be linear. With the linear curve, use linear regression to determine
the calibration equation.
6. Calculations
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after final
calculation.
6.1 Sample Volume, Dry Basis, Corrected to Standard Conditions. Same
as in Method 7C, Section 6.1.
6.2 Total g NO2 Per Sample.
Where:
m=Mass of NOx, as NO2, in sample, g.
S=Analysis of sample, g NO3-/ml.
B=Analysis of blank, g NO3-/ml.
250=Volume of prepared sample, ml.
46.01=Molecular weight of NO2-.
62.01=Molecular weight of NO3-.
1000=Total volume of KMnO4 solution, ml.
50=Aliquot KMnO4/NaOH solution, ml.
6.3 Sample Concentration.
Where:
C=Concentration of NOx as NO2, dry basis, mg/dscm.
K2=10^3 mg/ g.
Vm(std)=Dry gas volume measured by the dry gas meter, corrected to
standard conditions, dscm.
6.4 Conversion Factors.
1.0 ppm NO=1.247 mg NO/m3 at STP.
1.0 ppm NO2=1.912 mg NO2/m3 at STP.
1 ft3=2.832 10^2 m3.
1000 mg=1 g.
7. Quality Control
Quality control procedures are specified in Sections 4.1.3 (flow rate
accuracy) and 4.5 (audit analysis accuracy) of Method 7C.
8. Bibliography
1. Margeson, J.H., W.J. Mitchell, J.C. Suggs, and M.R. Midgett.
Integrated Sampling and Analysis Methods for Determining NOx Emissions
at Electric Utility Plants. U.S. Environmental Protection Agency,
Research Triangle Park, NC. Journal of the Air Pollution Control
Association. 32: 1210-1215. 1982.
2. Memorandum and attachment from J.H. Margeson, Source Branch,
Quality Assurance Division, Environmental Monitoring Systems Laboratory,
to The Record, EPA. March 30, 1983. NH3 Interference in Methods 7C and
7D.
3. Quality Assurance Handbook for Air Pollution Measurement Systems.
Volume III -- Stationary Source Specific Methods. U.S. Environmental
Protection Agency, Research Triangle Park, NC. Publication No.
EPA-600/4-77-027b. August 1977.
4. Margeson, J.H., et al. An Integrated Method for determining NOx
Emissions at Nitric Acid Plants. Manuscript submitted to Analytical
Chemistry. April 1984.
40 CFR 60.748 Pt. 60, App. A, Meth. 7E
1. Applicability and Principle
1.1 Applicability. This method is applicable to the determination of
nitrogen oxides (NOx) concentrations in emissions from stationary
sources only when specified within the regulations.
1.2 Principle. A gas simple is continuously extracted from a stack,
and a portion of the sample is conveyed to an instrumental
chemiluminescent analyzer for determination of NOx concentration.
Performance specifications and test procedures are provided to ensure
reliable data.
2. Range and Sensitivity
Same as Method 6C, Sections 2.1 and 2.2.
3. Definitions
3.1 Measurement System. The total equipment required for the
determination of NOx concentration. The measurement system consists of
the following major subsystems:
3.1.1 Sample Interface, Gas Analyzer, and Data Recorder. Same as
Method 6C, Sections 3.1.1, 3.1.2, and 3.1.3.
3.1.2 NO2 to NO Converter. A device that converts the nitrogen
dioxide (NO2) in the sample gas to nitrogen oxide (NO).
3.2 Span, Calibration Gas, Analyzer Calibration Error, Sampling
System Bias, Zero Drift, Calibration Drift, and Response Time. Same as
Method 6C, Sections 3.2 through 3.8.
3.3 Interference Response. The output response of the measurement
system to a component in the sample gas, other than the gas component
being measured.
4. Measurement System Performance Specifications
Same as Method 6C, Sections 4.1 through 4.4.
5. Apparatus and Reagents
5.1 Measurement System. Any measurement system for NOx that meets
the specifications of this method. A schematic of an acceptable
measurement system is shown in Figure 6C-1 of Method 6C. The essential
components of the measurement system are described below:
5.1.1 Sample Probe, Sample Line, Calibration Valve Assembly, Moisture
Removal System, Particulate Filter, Sample Pump, Sample Flow Rate
Control, Sample Gas Manifold, and Data Recorder. Same as Method 6C,
Sections 5.1.1 through 5.1.9, and 5.1.11.
5.1.2 NO2 to NO Converter. That portion of the system that converts
the nitrogen dioxide (NO2) in the sample gas to nitrogen oxide (NO). An
NO2 to NO converter is not necessary if data are presented to
demonstrate that the NO2 portion of the exhaust gas is less than 5
percent of the total NOx concentration.
5.1.3 NOx Analyzer. An analyzer based on the principles of
chemiluminescence, to determine continuously the NOx concentration in
the sample gas stream. The analyzer shall meet the applicable
performance specifications of Section 4. A means of controlling the
analyzer flow rate and a device for determining proper sample flow rate
(e.g., precision rotameter, pressure gauge downstream of all flow
controls, etc.) shall be provided at the analyzer.
5.2 NOx Calibration Gases. The calibration gases for the NOx
analyzer shall be NO in N2. Three calibration gases, as specified in
Sections 5.3.1 through 5.3.3. of Method 6C, shall be used. Ambient air
may be used for the zero gas.
6. Measurement System Performance Test Procedures
Perform the following procedures before measurement of emissions
(Section 7).
6.1 Calibration Gas Concentration Verification. Follow Section 6.1
of Method 6C, except if calibration gas analysis is required, use Method
7, and change all 5 percent performance values to 10 percent (or 10 ppm,
whichever is greater).
6.2 Interference Response. Conduct an interference response test of
the analyzer prior to its initial use in the field. Thereafter, recheck
the measurement system if changes are made in the instrumentation that
could alter the interference response (e.g., changes in the gas
detector). Conduct the interference response in accordance with Section
5.4 of Method 20.
6.3 Measurement System Preparation, Analyzer Calibration Error, and
Sample System Bias Check. Follow Sections 6.2 through 6.4 of Method 6C.
6.4 NO2 to NO Conversion Efficiency. Unless data are presented to
demonstrate that the NO2 concentration within the sample stream is not
greater than 5 percent of the NOx concentration, conduct an NO2 to NO
conversion efficiency test in accordance with Section 5.6 of Method 20.
7. Emission Test Procedure
7.1 Selection of Sampling Site and Sampling Points. Select a
measurement site and sampling points using the same criteria that are
applicable to tests performed using Method 7.
7.2 Sample Collection. Position the sampling probe at the first
measurement point, and begin sampling at the same rate as used during
the system calibration drift test. Maintain constant rate sampling
(i.e., 10 percent) during the entire run. The sampling time per run
shall be the same as the total time required to perform a run using
Method 7, plus twice the system response time. For each run, use only
those measurements obtained after twice the response time of the
measurement system has elapsed, to determine the average effluent
concentration.
7.3 Zero and Calibration Drift Test. Follow Section 7.4 of Method
6C.
8. Emission Calculation
Follow Section 8 of Method 6C.
9. Bibliography
Same as bibliography of Method 6C.
40 CFR 60.748 Pt. 60, App. A, Meth. 8
1. Principle and Applicability
1.1 Principle. A gas sample is extracted isokinetically from the
stack. The sulfuric acid mist (including sulfur trioxide) and the
sulfur dioxide are separated, and both fractions are measured separately
by the barium-thorin titration method.
1.2 Applicability. This method is applicable for the determination of
sulfuric acid mist (including sulfur trioxide, and in the absence of
other particulate matter) and sulfur dioxide emissions from stationary
sources. Collaborative tests have shown that the minimum detectable
limits of the method are 0.05 milligrams/cubic meter (0.03 10^7
pounds/cubic foot) for sulfur trioxide and 1.2 mg/m3 (0.74 10^7 lb/ft3)
for sulfur dioxide. No upper limits have been established. Based on
theoretical calculations for 200 milliters of 3 percent hydrogen
peroxide solution, the upper concentration limit for sulfur dioxide in a
1.0 m3 (35.3 ft3) gas sample is about 12,500 mg/m3 (7.7 10^4 lb/ft3).
The upper limit can be extended by increasing the quantity of peroxide
solution in the impingers.
Possible interfering agents of this method are fluorides, free
ammonia, and dimethyl aniline. If any of these interfering agents are
present (this can be determined by knowledge of the process),
alternative methods, subject to the approval of the Administrator, U.
S. E. P.A., are required.
Filterable particulate matter may be determined along with SO3 and
SO2 (subject to the approval of the Administrator) by inserting a heated
glass fiber filter between the probe and isopropanol impinger (see
Section 2.1 of Method 6.) If this option is chosen, particulate analysis
is gravimetric only; H2SO4 acid mist is not determined separately.
2. Apparatus
2.1 Sampling. A schematic of the sampling train used in this method
is shown in Figure 8-1; it is similiar to the Method 5 train except
that the filter position is different and the filter holder does not
have to be heated. Commercial models of this train are available. For
those who desire to build their own, however, complete construction
details are described in APTD-0581. Changes from the APTD-0581 document
and allowable modifications to Figure 8-1 are discussed in the following
subsections.
The operating and maintenance procedures for the sampling train are
described in APTD-0576. Since correct usage is important in obtaining
valid results, all users should read the APTD-0576 document and adopt
the operating and maintenance procedures outlined in it, unless
otherwise specified herein. Further details and guidelines on operation
and maintenance are given in Method 5 and should be read and followed
whenever they are applicable.
2.1.1 Probe Nozzle. Same as Method 5, Section 2.1.1.
2.1.2 Probe Liner. Borosilicate or quartz glass, with a heating
system to prevent visible condensation during sampling. Do not use
metal probe liners.
2.1.3 Pitot Tube. Same as Method 5, Section 2.1.3.
Insert illus. 253
2.1.4 Differential Pressure Gauge. Same as Method 5, Section 2.1.4.
2.1.5 Filter Holder. Borosilicate glass, with a glass frit filter
support and a silicone rubber gasket. Other gasket materials, e.g.,
Teflon or Viton, may be used subject to the approval of the
Administrator. The holder design shall provide a positive seal against
leakage from the outside or around the filter. The filter holder shall
be placed between the first and second impingers. Note: Do not heat
the filter holder.
2.1.6 Impingers. Four, as shown in Figure 8-1. The first and third
shall be of the Greenburg-Smith design with standard tips. The second
and fourth shall be of the Greenburg-Smith design, modified by replacing
the insert with an approximately 13 millimeter (0.5 in.) ID glass tube,
having an unconstricted tip located 13 mm (0.5 in.) from the bottom of
the flask. Similar collection systems, which have been approved by the
Administrator, may be used.
2.1.7 Metering System. Same as Method 5, Section 2.1.8.
2.1.8 Barometer. Same as Method 5, Section 2.1.9.
2.1.9 Gas Density Determination Equipment. Same as Method 5, Section
2.1.10.
2.1.10 Temperature Gauge. Thermometer, or equivalent, to measure the
temperature of the gas leaving the impinger train to within 1 C (2 F).
2.2 Sample Recovery.
2.2.1 Wash Bottles. Polyethylene or glass, 500 ml. (two).
2.2.2 Graduated Cylinders. 250 ml, 1 liter. (Volumetric flasks may
also be used.
2.2.3 Storage Bottles. Leak-free polyethlene bottles, 1000 ml size
(two for each sampling run).
2.2.4 Trip Balance. 500-gram capacity, to measure to 0.5 g
(necessary only if a moisture content analysis is to be done).
2.3 Analysis.
2.3.1 Pipettes. Volumetric 25 ml, 100 ml.
2.3.2 Burette, 50 ml.
2.3.3 Erlenmeyer Flask. 250 ml. (one for each sample, blank, and
standard).
2.3.4 Graduated Cylinder. 100 ml.
2.3.5 Trip Balance. 500 g capacity, to measure to 0.5 g.
2.3.6 Dropping Bottle. To add indicator solution, 125-ml size.
3. Reagents
Unless otherwise indicated, all reagents are to conform to the
specifications established by the Committee on Analytical Reagents of
the American Chemical Society, where such specifications are available.
Otherwise, use the best available grade.
3.1 Sampling.
3.1.1 Filters. Same as Method 5, Section 3.1.1.
3.1.2 Silica Gel. Same as Method 5, Section 3.1.2.
3.1.3 Water. Deionized, distilled to conform to ASTM Specification
D1193-77, Type 3 (incorporated by reference -- see 60.17). At the
option of the analyst, the KMnO4 test for oxidizable organic matter may
be omitted when high concentrations of organic matter are not expected
to be present.
3.1.4 Isopropanol. 80 Percent. Mix 800 ml of isopropanol with 200 ml
of deionized, distilled water.
Note: Experience has shown that only A.C.S. grade isopropanol is
satisfactory. Tests have shown that isopropanol obtained from
commercial sources occasionally has peroxide impurities that will cause
erroneously high sulfuric acid mist measurement. Use the following test
for detecting peroxides in each lot of isopropanol: Shake 10 ml of the
isopropanol with 10 ml of freshly prepared 10 percent potassium iodide
solution. Prepare a blank by similarly treating 10 ml of distilled
water. After 1 minute, read the absorbance on a spectrophotometer at
352 nanometers. If the absorbance exceeds 0.1, the isopropanol shall
not be used. Peroxides may be removed from isopropanol by redistilling,
or by passage through a column of activated alumina. However, reagent
grade isopropanol with suitably low peroxide levels is readily available
from commercial sources; therefore, rejection of contaminated lots may
be more efficient than following the peroxide removal procedure.
3.1.5 Hydrogen Peroxide, 3 Percent. Dilute 100 ml of 30 percent
hydrogen peroxide to 1 liter with deionized, distilled water. Prepare
fresh daily.
3.1.6 Crushed Ice.
3.2 Sample Recovery.
3.2.1 Water. Same as 3.1.3.
3.2.2 Isopropanol, 80 Percent. Same as 3.1.4.
3.3 Analysis.
3.3.1 Water. Same as 3.1.3.
3.3.2 Isopropanol, 100 Percent.
3.3.3 Thorin Indicator. 1-(o-arsonophenylazo) 2-naphthol-3,
6-disulfonic acid, disodium salt, or equivalent. Dissolve 0.20 g in 100
ml of deionized, distilled water.
3.3.4 Barium Perchlorate (0.0100 Normal). Dissolve 1.95 g of barium
perchlorate trihydrate (Ba(C104)2 3H2O) in 200 ml deionized, distilled
water, and dilute to 1 liter with isopropanol; 1.22 g of barium
chloride dihydrate (BaC12 2H2O) may be used instead of the barium
perchlorate. Standardize with sulfuric acid as in Section 5.2. This
solution must be protected against evaporation at all times.
3.3.5 Sulfuric Acid Standard (0.0100 N). Purchase or standardize to
0.0002 N against 0.0100 N NaOH that has previously been standardized
against primary standard potassium acid phthalate.
3.3.6 Quality Assurance Audit Samples. Same as in Method 6, Section
3.3.6.
4. Procedure
4.1 Sampling.
4.1.1 Pretest Preparation. Follow the procedure outlined in Method
5, Section 4.1.1; filters should be inspected, but need not be
desiccated, weighed, or identified. If the effluent gas can be
considered dry, i.e., moisture free, the silica gel need not be weighed.
4.1.2 Preliminary Determinations. Follow the procedure outlined in
Method 5, Section 4.1.2.
4.1.3 Preparation of Collection Train. Follow the procedure outlined
in Method 5, Section 4.1.3 (except for the second paragraph and other
obviously inapplicable parts) and use Figure 8-1 instead of Figure 5-1.
Replace the second paragraph with: Place 100 ml of 80 percent
isopropanol in the first impinger, 100 ml of 3 percent hydrogen peroxide
in both the second and third impingers; retain a portion of each
reagent for use as a blank solution. Place about 200 g of silica gel in
the fourth impinger.
Note: If moisture content is to be determined by impinger analysis,
weigh each of the first three impingers (plus absorbing solution) to the
nearest 0.5 g and record these weights. The weight of the silica gel
(or silica gel plus container) must also be determined to the nearest
0.5 g and recorded.
4.1.4 Pretest Leak-Check Procedure. Follow the basic procedure
outlined in Method 5, Section 4.1.4.1, noting that the probe heater
shall be adjusted to the minimum temperature required to prevent
condensation, and also that verbage such as, ''. . . plugging the inlet
to the filter holder . . .,'' shall be replaced by, ''. . . plugging
the inlet to the first impinger . . .'' The pretest leak-check is
optional.
4.1.5 Train Operation. Follow the basic procedures outlined in
Method 5, Section 4.1.5, in conjunction with the following special
instructions. Data shall be recorded on a sheet similar to the one in
Figure 8-2. The sampling rate shall not exceed 0.030 m3/min (1.0 cfm)
during the run. Periodically during the test, observe the connecting
line between the probe and first impinger for signs of condensation. If
it does occur, adjust the probe heater setting upward to the minimum
temperature required to prevent condensation. If component changes
become necessary during a run, a leak-check shall be done immediately
before each change, according to the procedure outlined in Section
4.1.4.2 of Method 5 (with appropriate modifications, as mentioned in
Section 4.1.4 of this method); record all leak rates. If the leakage
rate(s) exceed the specified rate, the tester shall either void the run
or shall plan to correct the sample volume as outlined in Section 6.3 of
Method 5. Immediately after component changes, leak-checks are
optional. If these leak-checks are done, the procedure outlined in
Section 4.1.4.1 of Method 5 (with appropriate modifications) shall be
used.
After turning off the pump and recording the final readings at the
conclusion of each run, remove the probe from the stack. Conduct a
post-test (mandatory) leak-check as in Section 4.1.4.3 of Method 5 (with
appropriate modification) and record the leak rate. If the post-test
leakage rate exceeds the specified acceptable rate, the tester shall
either correct the sample volume, as outlined in Section 6.3 of Method
5, or shall void the run.
Drain the ice bath and, with the probe disconnected, purge the
remaining part of the train, by drawing clean ambient air through the
system for 15 minutes at the average flow rate used for sampling.
Note: Clean ambient air can be provided by passing air through a
charcoal filter. At the option of the tester, ambient air (without
cleaning) may be used.
4.1.6 Calculation of Percent Isokinetic. Follow the procedure
outlined in Method 5, Section 4.1.6.
4.2 Sample Recovery.
4.2.1 Container No. 1. If a moisture content analysis is to be done,
weigh the first impinger plus contents to the nearest 0.5 g and record
this weight.
Transfer the contents of the first impinger to a 250-ml graduated
cylinder. Rinse the probe, first impinger, all connecting glassware
before the filter, and the front half of the filter holder with 80
percent isopropanol. Add the rinse solution to the cylinder. Dilute to
250 ml with 80 percent isopropanol. Add the filter to the solution,
mix, and transfer to the storage container. Protect the solution
against evaporation. Mark the level of liquid on the container and
identify the sample container.
4.2.2 Container No. 2. If a moisture content analysis is to be done,
weigh the second and third impingers (plus contents) to the nearest 0.5
g and record these weights. Also, weigh the spent silica gel (or silica
gel plus impinger) to the nearest 0.5 g.
Transfer the solutions from the second and third impingers to a
1000-ml graduated cylinder. Rinse all connecting glassware (including
back half of filter holder) between the filter and silica gel impinger
with deionized, distilled water, and add this rinse water to the
cylinder. Dilute to a volume of 1000 ml with deionized, distilled
water. Transfer the solution to a storage container. Mark the level of
liquid on the container. Seal and identify the sample container.
4.3 Analysis.
Note the level of liquid in Containers 1 and 2, and confirm whether
or not any sample was lost during shipment; note this on the analytical
data sheet. If a noticeable amount of leakage has occured, either void
the sample or use methods, subject to the approval of the Administrator,
to correct the final results.
4.3.1 Container No. 1. Shake the container holding the isopropanol
solution and the filter. If the filter breaks up, allow the fragments
to settle for a few minutes before removing a sample. Pipette a 100-ml
aliquot of this solution into a 250-ml Erlenmeyer flask, add 2 to 4
drops of thorin indicator, and titrate to a pink endpoint using 0.0100 N
barium perchlorate. Repeat the titration with a second aliquot of
sample and average the titration values. Replicate titrations must
agree within 1 percent or 0.2 ml, whichever is greater.
4.3.2 Container No. 2. Thoroughly mix the solution in the container
holding the contents of the second and third impingers. Pipette a 10-ml
aliquot of sample into a 250-ml Erlenmeyer flask. Add 40 ml of
isopropanol, 2 to 4 drops of thorin indicator, and titrate to a pink
endpoint using 0.0100 N barium perchlorate. Repeat the titration with a
second aliquot of sample and average the titration values. Replicate
titrations must agree within 1 percent or 0.2 ml, whichever is greater.
4.3.3 Blanks. Prepare blanks by adding 2 to 4 drops of thorin
indicator to 100 ml of 80 percent isopropanol. Titrate the blanks in
the same manner as the samples.
4.4 Quality Control Procedures. Same as in Method 5, Section 4.4.
4.5 Audit Sample Analysis. Same as in Method 6, Section 4.4.
5. Calibration
5.1 Calibrate equipment using the procedures specified in the
following sections of Method 5: Section 5.3 (metering system); Section
5.5 (temperature gauges); Section 5.7 (barometer). Note that the
recommended leak-check of the metering system, described in Section 5.6
of Method 5, also applies to this method.
5.2 Standardize the barium perchlorate solution with 25 ml of
standard sulfuric acid, to which 100 ml of 100 percent isopropanol has
been added.
6. Calculations
Note: Carry out calculations retaining at least one extra decimal
figure beyond that of the acquired data. Round off figures after final
calculation.
6.1 Nomenclature.
An=Cross-sectional area of nozzle, m2 (ft2).
Bws=Water vapor in the gas stream, proportion by volume.
CH2SO4=Sulfuric acid (including SO3) concentration, g/dscm (lb/dscf).
CSO2=Sulfur dioxide concentration, g/dscm (lb/dscf).
I=Percent of isokinetic sampling.
N=Normality of barium perchlorate titrant, meq/ml.
Pbar=Barometric pressure at the sampling site, mm Hg (in. Hg).
Ps=Absolute stack gas pressure, mm Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
Tm=Average absolute dry gas meter temperature (see Figure 8-2), K (
R).
Ts=Average absolute stack gas temperature (see Figure 8-2), K ( R).
Tstd=Standard absolute temperature, 293 K (528 R).
Va=Volume of sample aliquot titrated, 100 ml for H2SO4 and 10 ml for
SO2.
Vlc=Total volume of liquid collected in impingers and silica gel, ml.
Vm=Volume of gas sample as measured by dry gas meter, dcm (dcf).
Vm(std)=Volume of gas sample measured by the dry gas meter corrected
to standard conditions, dscm (dscf).
vs=Average stack gas velocity, calculated by Method 2, Equation 2-9,
using data obtained from Method 8, m/sec (ft/sec).
Vsoln=Total volume of solution in which the sulfuric acid or sulfur
dioxide sample is contained, 250 ml or 1,000 ml, respectively.
Vt=Volume of barium perchlorate titrant used for the sample, ml.
Vtb=Volume of barium perchlorate titrant used for the blank, ml.
Y=Dry gas meter calibration factor.
H=Average pressure drop across orifice meter, mm (in.) H2O.
=Total sampling time, min.
13.6=Specific gravity of mercury.
60=sec/min.
100=Conversion to percent.
6.2 Average Dry Gas Meter Temperature and Average Orifice Pressure
Drop. See data sheet (Figure 8-2).
6.3 Dry Gas Volume. Correct the sample volume measured by the dry
gas meter to standard conditions (20 C and 760 mm Hg or 68 F and 29.92
in. Hg) by using Equation 8-1.
Insert illus. 255
Where:
K1=0.3858 K/mm Hg for metric units.
=17.64 R/in., Hg for English units.
Note: If the leak rate observed during any mandatory leak-checks
exceeds the specified acceptable rate, the tester shall either correct
the value of Vm in Equation 8-1 (as described in Section 6.3 of Method
5), or shall invalidate the test run.
6.4 Volume of Water Vapor and Moisture Content. Calculate the volume
of water vapor using Equation 5-2 of Method 5; the weight of water
collected in the impingers and silica gel can be directly converted to
milliliters (the specific gravity of water is 1 g/ml). Calculate the
moisture content of the stack gas, using Equation 5-3 of Method 5. The
''Note'' in Section 6.5 of Method 5 also applies to this method. Note
that if the effluent gas stream can be considered dry, the volume of
water vapor and moisture content need not be calculated.
6.5 Sulfuric Acid Mist (including SO3) Concentration.
Insert illus. 256
Where:
K2=0.04904 g/milliequivalent for metric units.
=1.081 10^4 lb/meq for English units.
6.6 Sulfur Dioxide Concentration.
Insert illus. 257
Where:
K3=0.03203 g/meq for metric units.
=7.061 10^5 lb/meq for English units.
6.7 Isokinetic Variation.
6.7.1 Calculation from Raw Data.
Where:
K4=0.003464 mm Hg-m3/ml- K for metric units.
=0.002676 in. Hg-ft3/ml- R for English units.
6.7.2 Calculation from Intermediate Values.
Insert illus. 259
where:
K5=4.320 for metric units.
=0.09450 for English units
6.8 Acceptable Results. If I is greater than 90 percent and less
than 110 percent, the results are acceptable. If the results are low
in comparison to the standards and I is beyond the acceptable range,
the Administrator may opt to accept the results. Use Citation 4 in the
Bibliography of Method 5 to make judgments. Otherwise, reject the
results and repeat the test.
6.9 Stack Gas Velocity and Volumetric Flow Rate. Calculate the
average stack gas velocity and volumetric flow rate, if needed, using
data obtained in this method and equations in Sections 5.2 and 5.3 of
Method 2.
6.10 Relative Error (RE) for QA Audit Samples. Same as in Method 6,
Section 6.4.
7. Bibliography
1. Atmospheric Emissions from Sulfuric Acid Manufacturing Processes.
U.S. DHEW, PHS, Division of Air Pollution. Public Health Service
Publication No. 999-AP-13. Cincinnati, OH. 1965.
2. Corbett, P. F. The Determination of SO2 and SO3 in Flue Gases.
Journal of the Institute of Fuel. 24: 237-243. 1961.
3. Martin, Robert M. Construction Details of Isokinetic Source
Sampling Equipment. Environmental Protection Agency. Research Triangle
Park, NC. Air Pollution Control Office Publication No. APTD-0581.
April, 1971.
4. Patton, W. F. and J. A. Brink, Jr. New Equipment and Techniques
for Sampling Chemical Process Gases. Journal of Air Pollution Control
Association. 13: 162. 1963.
5. Rom, J. J. Maintenance, Calibration, and Operation of Isokinetic
Source-Sampling Equipment. Office of Air Programs, Environmental
Protection Agency. Research Triangle Park, NC. APTD-0576. March, 1972.
6. Hamil, H. F. and D. E. Camann. Collaborative Study of Method for
Determination of Sulfur Dioxide Emissions from Stationary Sources
(Fossil Fuel-Fired Steam Generators). Environmental Protection Agency.
Research Triangle Park, NC. EPA-650/4-74-024. December, 1973.
7. Annual Book of ASTM Standards. Part 31; Water, Atmospheric
Analysis. pp. 40-42. American Society for Testing and Materials.
Philadelphia, Pa. 1974.
40 CFR 60.748 Pt. 60, App. A, Meth. 9
Many stationary sources discharge visible emissions into the
atmosphere; these emissions are usually in the shape of a plume. This
method involves the determination of plume opacity by qualified
observers. The method includes procedures for the training and
certification of observers, and procedures to be used in the field for
determination of plume opacity. The appearance of a plume as viewed by
an observer depends upon a number of variables, some of which may be
controllable and some of which may not be controllable in the field.
Variables which can be controlled to an extent to which they no longer
exert a significant influence upon plume appearance include: Angle of
the observer with respect to the plume; angle of the observer with
respect to the sun; point of observation of attached and detached steam
plume; and angle of the observer with respect to a plume emitted from a
rectangular stack with a large length to width ratio. The method
includes specific criteria applicable to these variables.
Other variables which may not be controllable in the field are
luminescence and color contrast between the plume and the background
against which the plume is viewed. These variables exert an influence
upon the appearance of a plume as viewed by an observer, and can affect
the ability of the observer to accurately assign opacity values to the
observed plume. Studies of the theory of plume opacity and field
studies have demonstrated that a plume is most visible and presents the
greatest apparent opacity when viewed against a contrasting background.
It follows from this, and is confirmed by field trials, that the opacity
of a plume, viewed under conditions where a contrasting background is
present can be assigned with the greatest degree of accuracy. However,
the potential for a positive error is also the greatest when a plume is
viewed under such contrasting conditions. Under conditions presenting a
less contrasting background, the apparent opacity of a plume is less and
approaches zero as the color and luminescence contrast decrease toward
zero. As a result, significant negative bias and negative errors can be
made when a plume is viewed under less contrasting conditions. A
negative bias decreases rather than increases the possibility that a
plant operator will be cited for a violation of opacity standards due to
observer error.
Studies have been undertaken to determine the magnitude of positive
errors which can be made by qualified observers while reading plumes
under contrasting conditions and using the procedures set forth in this
method. The results of these studies (field trials) which involve a
total of 769 sets of 25 readings each are as follows:
(1) For black plumes (133 sets at a smoke generator), 100 percent of
the sets were read with a positive error /1/ of less than 7.5 percent
opacity; 99 percent were read with a positive error of less than 5
percent opacity.
(2) For white plumes (170 sets at a smoke generator, 168 sets at a
coal-fired power plant, 298 sets at a sulfuric acid plant), 99 percent
of the sets were read with a positive error of less than 7.5 percent
opacity; 95 percent were read with a positive error of less than 5
percent opacity.
The positive observational error associated with an average of
twenty-five readings is therefore established. The accuracy of the
method must be taken into account when determining possible violations
of applicable opacity standards.
1. Principle and Applicability
1.1 Principle. The opacity of emissions from stationary sources is
determined visually by a qualified observer.
1.2 Applicability. This method is applicable for the determination of
the opacity of emissions from stationary sources pursuant to 60.11(b)
and for qualifying observers for visually determining opacity of
emissions.
2. Procedures
The observer qualified in accordance with section 3 of this method
shall use the following procedures for visually determining the opacity
of emissions:
2.1 Position. The qualified observer shall stand at a distance
sufficient to provide a clear view of the emissions with the sun
oriented in the 140 sector to his back. Consistent with maintaining
the above requirement, the observer shall, as much as possible, make his
observations from a position such that his line of vision is
approximately perpendicular to the plume direction, and when observing
opacity of emissions from rectangular outlets (e.g., roof monitors, open
baghouses, noncircular stacks), approximately perpendicular to the
longer axis of the outlet. The observer's line of sight should not
include more than one plume at a time when multiple stacks are involved,
and in any case the observer should make his observations with his line
of sight perpendicular to the longer axis of such a set of multiple
stacks (e.g., stub stacks on baghouses).
2.2 Field Records. The observer shall record the name of the plant,
emission location, type facility, observer's name and affiliation, a
sketch of the observer's position relative to the source, and the date
on a field data sheet (Figure 9-1). The time, estimated distance to the
emission location, approximate wind direction, estimated wind speed,
description of the sky condition (presence and color of clouds), and
plume background are recorded on a field data sheet at the time opacity
readings are initiated and completed.
2.3 Observations. Opacity observations shall be made at the point of
greatest opacity in that portion of the plume where condensed water
vapor is not present. The observer shall not look continuously at the
plume, but instead shall observe the plume momentarily at 15-second
intervals.
2.3.1 Attached Steam Plumes. When condensed water vapor is present
within the plume as it emerges from the emission outlet, opacity
observations shall be made beyond the point in the plume at which
condensed water vapor is no longer visible. The observer shall record
the approximate distance from the emission outlet to the point in the
plume at which the observations are made.
2.3.2 Detached Steam Plume. When water vapor in the plume condenses
and becomes visible at a distinct distance from the emission outlet, the
opacity of emissions should be evaluated at the emission outlet prior to
the condensation of water vapor and the formation of the steam plume.
2.4 Recording Observations. Opacity observations shall be recorded
to the nearest 5 percent at 15-second intervals on an observational
record sheet. (See Figure 9-2 for an example.) A minimum of 24
observations shall be recorded. Each momentary observation recorded
shall be deemed to represent the average opacity of emissions for a
15-second period.
2.5 Data Reduction. Opacity shall be determined as an average of 24
consecutive observations recorded at 15-second intervals. Divide the
observations recorded on the record sheet into sets of 24 consecutive
observations. A set is composed of any 24 consecutive observations.
Sets need not be consecutive in time and in no case shall two sets
overlap. For each set of 24 observations, calculate the average by
summing the opacity of the 24 observations and dividing this sum by 24.
If an applicable standard specifies an averaging time requiring more
than 24 observations, calculate the average for all observations made
during the specified time period. Record the average opacity on a
record sheet. (See Figure 9-1 for an example.)
3. Qualifications and Testing
3.1 Certification Requirements. To receive certification as a
qualified observer, a candidate must be tested and demonstrate the
ability to assign opacity readings in 5 percent increments to 25
different black plumes and 25 different white plumes, with an error not
to exceed 15 percent opacity on any one reading and an average error not
to exceed 7.5 percent opacity in each category. Candidates shall be
tested according to the procedures described in section 3.2. Smoke
generators used pursuant to section 3.2 shall be equipped with a smoke
meter which meets the requirements of section 3.3.
The certification shall be valid for a period of 6 months, at which
time the qualification procedure must be repeated by any observer in
order to retain certification.
3.2 Certification Procedure. The certification test consists of
showing the candidate a complete run of 50 plumes -- 25 black plumes and
25 white plumes -- generated by a smoke generator. Plumes within each
set of 25 black and 25 white runs shall be presented in random order.
The candidate assigns an opacity value to each plume and records his
observation on a suitable form. At the completion of each run of 50
readings, the score of the candidate is determined. If a candidate
fails to qualify, the complete run of 50 readings must be repeated in
any retest. The smoke test may be administered as part of a smoke
school or training program, and may be preceded by training or
familiarization runs of the smoke generator during which candidates are
shown black and white plumes of known opacity.
3.3 Smoke Generator Specifications. Any smoke generator used for the
purposes of section 3.2 shall be equipped with a smoke meter installed
to measure opacity across the diameter of the smoke generator stack.
The smoke meter output shall display instack opacity based upon a
pathlength equal to the stack exit diameter, on a full 0 to 100 percent
chart recorder scale. The smoke meter optical design and performance
shall meet the specifications shown in Table 9-1. The smoke meter shall
be calibrated as prescribed in section 3.3.1 prior to the conduct of
each smoke reading test. At the completion of each test, the zero and
span drift shall be checked and if the drift exceeds 1 percent opacity,
the condition shall be corrected prior to conducting any subsequent test
runs. The smoke meter shall be demonstrated, at the time of
installation, to meet the specifications listed in Table 9-1. This
demonstration shall be repeated following any subsequent repair or
replacement of the photocell or associated electronic circuitry
including the chart recorder or output meter, or every 6 months,
whichever occurs first.
3.3.1 Calibration. The smoke meter is calibrated after allowing a
minimum of 30 minutes warmup by alternately producing simulated opacity
of 0 percent and 100 percent. When stable response at 0 percent or 100
percent is noted, the smoke meter is adjusted to produce an output of 0
percent or 100 percent, as appropriate. This calibration shall be
repeated until stable 0 percent and 100 percent readings are produced
without adjustment. Simulated 0 percent and 100 percent opacity values
may be produced by alternately switching the power to the light source
on and off while the smoke generator is not producing smoke.
3.3.2 Smoke Meter Evaluation. The smoke meter design and performance
are to be evaluated as follows:
3.3.2.1 Light Source. Verify from manufacturer's data and from
voltage measurements made at the lamp, as installed, that the lamp is
operated within 5 percent of the nominal rated voltage.
3.3.2.2 Spectral Response of Photocell. Verify from manufacturer's
data that the photocell has a photopic response; i.e., the spectral
sensitivity of the cell shall closely approximate the standard
spectral-luminosity curve for photopic vision which is referenced in (b)
of Table 9-1.
Insert illus. 15A
3.3.2.3 Angle of View. Check construction geometry to ensure that
the total angle of view of the smoke plume, as seen by the photocell,
does not exceed 15 . The total angle of view may be calculated from:
=2 tan^1d/2L, where =total angle of view; d=the sum of the photocell
diameter+the diameter of the limiting aperture; and L=the distance from
the photocell to the limiting aperture. The limiting aperture is the
point in the path between the photocell and the smoke plume where the
angle of view is most restricted. In smoke generator smoke meters this
is normally an orifice plate.
3.3.2.4 Angle of Projection. Check construction geometry to ensure
that the total angle of projection of the lamp on the smoke plume does
not exceed 15 . The total angle of projection may be calculated from:
=2 tan^1d/2L, where = total angle of projection; d= the sum of the
length of the lamp filament + the diameter of the limiting aperture;
and L= the distance from the lamp to the limiting aperture.
3.3.2.5 Calibration Error. Using neutral-density filters of known
opacity, check the error between the actual response and the theoretical
linear response of the smoke meter. This check is accomplished by first
calibrating the smoke meter according to 3.3.1 and then inserting a
series of three neutral-density filters of nominal opacity of 20, 50,
and 75 percent in the smoke meter pathlength. Filters calibrated within
2 percent shall be used. Care should be taken when inserting the
filters to prevent stray light from affecting the meter. Make a total
of five nonconsecutive readings for each filter. The maximum error on
any one reading shall be 3 percent opacity.
3.3.2.6 Zero and Span Drift. Determine the zero and span drift by
calibrating and operating the smoke generator in a normal manner over a
1-hour period. The drift is measured by checking the zero and span at
the end of this period.
3.3.2.7 Response Time. Determine the response time by producing the
series of five simulated 0 percent and 100 percent opacity values and
observing the time required to reach stable response. Opacity values of
0 percent and 100 percent may be simulated by alternately switching the
power to the light source off and on while the smoke generator is not
operating.
4. Bibliography.
1. Air Pollution Control District Rules and Regulations, Los Angeles
County Air Pollution Control District, Regulation IV, Prohibitions, Rule
50.
2. Weisburd, Melvin I., Field Operations and Enforcement Manual for
Air, U.S. Environmental Protection Agency, Research Triangle Park, NC.
APTD-1100, August 1972, pp. 4.1-4.36.
3. Condon, E.U., and Odishaw, H., Handbook of Physics, McGraw-Hill
Co., New York, NY, 1958, Table 3.1, p. 6-52.
/1/ For a set, positive error = average opacity determined by
observers' 25 observations -- average opacity determined from
transmissometer's 25 recordings.
40 CFR 60.748 Pt. 60, App. A, Alt. Meth.
This alternate method provides the quantitative determination of the
opacity of an emissions plume remotely by a mobile lidar system (laser
radar; Light Detection and Ranging). The method includes procedures
for the calibration of the lidar and procedures to be used in the field
for the lidar determination of plume opacity. The lidar is used to
measure plume opacity during either day or nighttime hours because it
contains its own pulsed light source or transmitter. The operation of
the lidar is not dependent upon ambient lighting conditions (light,
dark, sunny or cloudy).
The lidar mechanism or technique is applicable to measuring plume
opacity at numerous wavelengths of laser radiation. However, the
performance evaluation and calibration test results given in support of
this method apply only to a lidar that employs a ruby (red light) laser
(Reference 5.1).
1. Principle and Applicability
1.1 Principle. The opacity of visible emissions from stationary
sources (stacks, roof vents, etc.) is measured remotely by a mobile
lidar (laser radar).
1.2 Applicability. This method is applicable for the remote
measurement of the opacity of visible emissions from stationary sources
during both nighttime and daylight conditions, pursuant to 40 CFR
60.11(b). It is also applicable for the calibration and performance
verification of the mobile lidar for the measurement of the opacity of
emissions. A performance/design specification for a basic lidar system
is also incorporated into this method.
1.3 Definitions.
Azimuth angle: The angle in the horizontal plane that designates
where the laser beam is pointed. It is measured from an arbitrary fixed
reference line in that plane.
Backscatter: The scattering of laser light in a direction opposite
to that of the incident laser beam due to reflection from particulates
along the beam's atmospheric path which may include a smoke plume.
Backscatter signal: The general term for the lidar return signal
which results from laser light being backscattered by atmospheric and
smoke plume particulates.
Convergence distance: The distance from the lidar to the point of
overlap of the lidar receiver's field-of-view and the laser beam.
Elevation angle: The angle of inclination of the laser beam
referenced to the horizontal plane.
Far region: The region of the atmosphere's path along the lidar
line-of-sight beyond or behind the plume being measured.
Lidar: Acronym for Light Detection and Ranging.
Lidar range: The range or distance from the lidar to a point of
interest along the lidar line-of-sight.
Near region: The region of the atmospheric path along the lidar
line-of-sight between the lidar's convergence distance and the plume
being measured.
Opacity: One minus the optical transmittance of a smoke plume,
screen target, etc.
Pick interval: The time or range intervals in the lidar backscatter
signal whose minimum average amplitude is used to calculate opacity.
Two pick intervals are required, one in the near region and one in the
far region.
Plume: The plume being measured by lidar.
Plume signal: The backscatter signal resulting from the laser light
pulse passing through a plume.
1/R2 correction: The correction made for the systematic decrease in
lidar backscatter signal amplitude with range.
Reference signal: The backscatter signal resulting from the laser
light pulse passing through ambient air.
Sample interval: The time period between successive samples for a
digital signal or between successive measurements for an analog signal.
Signal spike: An abrupt, momentary increase and decrease in signal
amplitude.
Source: The source being tested by lidar.
Time reference: The time (to) when the laser pulse emerges from the
laser, used as the reference in all lidar time or range measurements.
2. Procedures
The mobile lidar calibrated in accordance with Paragraph 3 of this
method shall use the following procedures for remotely measuring the
opacity of stationary source emissions:
2.1 Lidar Position. The lidar shall be positioned at a distance from
the plume sufficient to provide an unobstructed view of the source
emissions. The plume must be at a range of at least 50 meters or three
consecutive pick intervals (whichever is greater) from the lidar's
transmitter/receiver convergence distance along the line-of-sight. The
maximum effective opacity measurement distance of the lidar is a
function of local atmospheric conditions, laser beam diameter, and plume
diameter. The test position of the lidar shall be selected so that the
diameter of the laser beam at the measurement point within the plume
shall be no larger than three-fourths the plume diameter. The beam
diameter is calculated by Equation (AM1-1):
D(lidar)=A+R 0.75 D(Plume) (AM1-1)
Where:
D(Plume)=diameter of the plume (cm),
=laser beam divergence measured in radians
R=range from the lidar to the source (cm)
D(Lidar)=diameter of the laser beam at range R (cm),
A=diameter of the laser beam or pulse where it leaves the laser.
The lidar range, R, is obtained by aiming and firing the laser at the
emissions source structure immediately below the outlet. The range
value is then determined from the backscatter signal which consists of a
signal spike (return from source structure) and the atmospheric
backscatter signal (Reference 5.1). This backscatter signal should be
recorded.
When there is more than one source of emissions in the immediate
vicinity of the plume, the lidar shall be positioned so that the laser
beam passes through only a single plume, free from any interference of
the other plumes for a minimum of 50 meters or three consecutive pick
intervals (whichever is greater) in each region before and beyond the
plume along the line-of-sight (determined from the backscatter signals).
The lidar shall initially be positioned so that its line-of-sight is
approximately perpendicular to the plume.
When measuring the opacity of emissions from rectangular outlets
(e.g., roof monitors, open baghouses, noncircular stacks, etc.), the
lidar shall be placed in a position so that its line-of-sight is
approximately perpendicular to the longer (major) axis of the outlet.
2.2 Lidar Operational Restrictions. The lidar receiver shall not be
aimed within an angle of 15 (cone angle) of the sun.
This method shall not be used to make opacity measurements if
thunderstorms, snowstorms, hail storms, high wind, high-ambient dust
levels, fog or other atmospheric conditions cause the reference signals
to consistently exceed the limits specified in Section 2.3.
2.3 Reference Signal Requirements. Once placed in its proper
position for opacity measurement, the laser is aimed and fired with the
line-of-sight near the outlet height and rotated horizontally to a
position clear of the source structure and the associated plume. The
backscatter signal obtained from this position is called the ambient-air
or reference signal. The lidar operator shall inspect this signal
(Section V of Reference 5.1) to: (1) determine if the lidar
line-of-sight is free from interference from other plumes and from
physical obstructions such as cables, power lines, etc., for a minimum
of 50 meters or three consecutive pick intervals (whichever is greater)
in each region before and beyond the plume, and (2) obtain a qualitative
measure of the homogeneity of the ambient air by noting any signal
spikes.
Should there be any signal spikes on the reference signal within a
minimum of 50 meters or three consecutive pick intervals (whichever is
greater) in each region before and beyond the plume, the laser shall be
fired three more times and the operator shall inspect the reference
signals on the display. If the spike(s) remains, the azimuth angle
shall be changed and the above procedures conducted again. If the
spike(s) disappears in all three reference signals, the lidar
line-of-sight is acceptable if there is shot-to-shot consistency and
there is no interference from other plumes.
Shot-to-shot consistency of a series of reference signals over a
period of twenty seconds is verified in either of two ways. (1) The
lidar operator shall observe the reference signal amplitudes. For
shot-to-shot consistency the ratio of Rf to Rn (amplitudes of the near
and far region pick intervals (Section 2.6.1)) shall vary by not more
than 6% between shots; or (2) the lidar operator shall accept any one
of the reference signals and treat the other two as plume signals; then
the opacity for each of the subsequent reference signals is calculated
(Equation AM1-2). For shot-to-shot consistency, the opacity values
shall be within 3% of 0% opacity and the associated So values less
than or equal to 8% (full scale) (Section 2.6).
If a set of reference signals fails to meet the requirements of this
section, then all plume signals (Section 2.4) from the last set of
acceptable reference signals to the failed set shall be discarded.
2.3.1 Initial and Final Reference Signals. Three reference signals
shall be obtained within a 90-second time period prior to any data run.
A final set of three reference signals shall be obtained within three
(3) minutes after the completion of the same data run.
2.3.2 Temporal Criterion for Additional Reference Signals. An
additional set of reference signals shall be obtained during a data run
if there is a change in wind direction or plume drift of 30 or more
from the direction that was prevalent when the last set of reference
signals was obtained. An additional set of reference signals shall also
be obtained if there is an increase in value of SIn (near region
standard deviation, Equation AM1-5) or SIf (far region standard
deviation, Equation AM1-6) that is greater than 6% (full scale) over the
respective values calculated from the immediately previous plume signal,
and this increase in value remains for 30 seconds or longer.An
additional set of reference signals shall also be obtained if there is a
change in amplitude in either the near or the far region of the plume
signal, that is greater than 6% of the near signal amplitude and this
change in amplitude remains for 30 seconds or more.
2.4 Plume Signal Requirements. Once properly aimed, the lidar is
placed in operation with the nominal pulse or firing rate of six
pulses/minute (1 pulse/10 seconds). The lidar operator shall observe
the plume backscatter signals to determine the need for additional
reference signals as required by Section 2.3.2. The plume signals are
recorded from lidar start to stop and are called a data run. The length
of a data run is determined by operator discretion. Short-term stops of
the lidar to record additional reference signals do not constitute the
end of a data run if plume signals are resumed within 90 seconds after
the reference signals have been recorded, and the total stop or
interrupt time does not exceed 3 minutes.
2.4.1 Non-hydrated Plumes. The laser shall be aimed at the region of
the plume which displays the greatest opacity. The lidar operator must
visually verify that the laser is aimed clearly above the source exit
structure.
2.4.2 Hydrated Plumes. The lidar will be used to measure the opacity
of hydrated or so-called steam plumes. As listed in the reference
method, there are two types, i.e., attached and detached steam plumes.
2.4.2.1 Attached Steam Plumes. When condensed water vapor is present
within a plume, lidar opacity measurements shall be made at a point
within the residual plume where the condensed water vapor is no longer
visible. The laser shall be aimed into the most dense region (region of
highest opacity) of the residual plume.
During daylight hours the lidar operator locates the most dense
portion of the residual plume visually. During nighttime hours a
high-intensity spotlight, night vision scope, or low light level TV,
etc., can be used as an aid to locate the residual plume. If visual
determination is ineffective, the lidar may be used to locate the most
dense region of the residual plume by repeatedly measuring opacity,
along the longitudinal axis or center of the plume from the emissions
outlet to a point just beyond the steam plume, The lidar operator should
also observe color differences and plume reflectivity to ensure that the
lidar is aimed completely within the residual plume. If the operator
does not obtain a clear indication of the location of the residual
plume, this method shall not be used.
Once the region of highest opacity of the residual plume has been
located, aiming adjustments shall be made to the laser line-of-sight to
correct for the following: movement to the region of highest opacity
out of the lidar line-of-sight (away from the laser beam) for more than
15 seconds, expansion of the steam plume (air temperature lowers and/or
relative humidity increases) so that it just begins to encroach on the
field-of-view of the lidar's optical telescope receiver, or a decrease
in the size of the steam plume (air temperature higher and/or relative
humidity decreases) so that regions within the residual plume whose
opacity is higher than the one being monitored, are present.
2.4.2.2 Detached Steam Plumes. When the water vapor in a hydrated
plume condenses and becomes visible at a finite distance from the stack
or source emissions outlet, the opacity of the emissions shall be
measured in the region of the plume clearly above the emissions outlet
and below condensation of the water vapor.
During daylight hours the lidar operators can visually determine if
the steam plume is detached from the stack outlet. During nighttime
hours a high-intensity spotlight, night vision scope, low light level
TV, etc., can be used as an aid in determining if the steam plume is
detached. If visual determination is ineffective, the lidar may be used
to determine if the steam plume is detached by repeatedly measuring
plume opacity from the outlet to the steam plume along the plume's
longitudinal axis or center line. The lidar operator should also
observe color differences and plume reflectivity to detect a detached
plume. If the operator does not obtain a clear indication of the
location of the detached plume, this method shall not be used to make
opacity measurements between the outlet and the detached plume.
Once the determination of a detached steam plume has been confirmed,
the laser shall be aimed into the region of highest opacity in the plume
between the outlet and the formation of the steam plume. Aiming
adjustments shall be made to the lidar's line-of-sight within the plume
to correct for changes in the location of the most dense region of the
plume due to changes in wind direction and speed or if the detached
steam plume moves closer to the source outlet encroaching on the most
dense region of the plume. If the detached steam plume should move too
close to the source outlet for the lidar to make interference-free
opacity measurements, this method shall not be used.
2.5 Field Records. In addition to the recording recommendations
listed in other sections of this method the following records should be
maintained. Each plume measured should be uniquely identified. The
name of the facility, type of facility, emission source type, geographic
location of the lidar with respect to the plume, and plume
characteristics should be recorded. The date of the test, the time
period that a source was monitored, the time (to the nearest second) of
each opacity measurement, and the sample interval should also be
recorded. The wind speed, wind direction, air temperature, relative
humidity, visibility (measured at the lidar's position), and cloud cover
should be recorded at the beginning and end of each time period for a
given source. A small sketch depicting the location of the laser beam
within the plume should be recorded.
If a detached or attached steam plume is present at the emissions
source, this fact should be recorded. Figures AM1-I and AM1-II are
examples of logbook forms that may be used to record this type of data.
Magnetic tape or paper tape may also be used to record data.
Insert illus. 0809
Insert illus. 0810
Insert illus. 0811
2.6 Opacity Calculation and Data Analysis. Referring to the
reference signal and plume signal in Figure AM1-III, the measured
opacity (Op) in percent for each lidar measurement is calculated using
Equation AM1-2. (Op=1^Tp; Tp is the plume transmittance.)
Insert illus 0808
Where:
In=near-region pick interval signal amplitude, plume signal, 1/R2
corrected,
If=far-region pick interval signal amplitude, plume signal, 1/R2
corrected,
Rn=near-region pick interval signal amplitude, reference signal, 1/R2
corrected, and
Rf=far-region pick interval signal amplitude, reference signal, 1/R2
corrected.
The 1/R2 correction to the plume and reference signal amplitudes is
made by multiplying the amplitude for each successive sample interval
from the time reference, by the square of the lidar time (or range)
associated with that sample interval (Reference 5.1).
The first step in selecting the pick intervals for Equation AM1-2 is
to divide the plume signal amplitude by the reference signal amplitude
at the same respective ranges to obtain a ''normalized'' signal. The
pick intervals selected using this normalized signal, are a minimum of
15 m (100 nanoseconds) in length and consist of at least 5 contiguous
sample intervals. In addition, the following criteria, listed in order
of importance, govern pick interval selection. (1) The intervals shall
be in a region of the normalized signal where the reference signal meets
the requirements of Section 2.3 and is everywhere greater than zero.
(2) The intervals (near and far) with the minimum average amplitude are
chosen. (3) If more than one interval with the same minimum average
amplitude is found, the interval closest to the plume is chosen. (4)
The standard deviation, So, for the calculated opacity shall be 8% or
less. (So is calculated by Equation AM1-7).
If So is greater than 8%, then the far pick interval shall be changed
to the next interval of minimal average amplitude. If So is still
greater than 8%, then this procedure is repeated for the far pick
interval. This procedure may be repeated once again for the near pick
interval, but if So remains greater than 8%, the plume signal shall be
discarded.
The reference signal pick intervals, Rn and Rf, must be chosen over
the same time interval as the plume signal pick intervals, In and If,
respectively (Figure AM1-III). Other methods of selecting pick
intervals may be used if they give equivalent results. Field-oriented
examples of pick interval selection are available in Reference 5.1.
The average amplitudes for each of the pick intervals, In, If, Rn,
Rf, shall be calculated by averaging the respective individual
amplitudes of the sample intervals from the plume signal and the
associated reference signal each corrected for 1/R2. The amplitude of
In shall be calculated according to Equation (AM-3).
Insert illus 0813A
Where:
Ini=the amplitude of the ith sample interval (near-region),
=sum of the individual amplitudes for the sample intervals,
m=number of sample intervals in the pick interval, and
In=average amplitude of the near-region pick interval.
Similarly, the amplitudes for If, Rn, and Rf are calculated with the
three expressions in Equation (AM1-4).
Insert illus. 0813B
The standard deviation, SIn, of the set of amplitudes for the
near-region pick interval, In, shall be calculated using Equation
(AM1-5).
Insert illus. 0813C
Similarly, the standard deviations SIf, SRn, and SRf are calculated
with the three expressions in Equation (AM1-6).
Insert illus. 0814A
The standard deviation, So, for each associated opacity value, Op,
shall be calculated using Equation (AM1-7).
insert illus 01223
The calculated values of In, If, Rn, Rf, SIn, SIf, SRn, SRf, Op, and
So should be recorded. Any plume signal with an So greater than 8%
shall be discarded.
2.6.1 Azimuth Angle Correction. If the azimuth angle correction to
opacity specified in this section is performed, then the elevation angle
correction specified in Section 2.6.2 shall not be performed. When
opacity is measured in the residual region of an attached steam plume,
and the lidar line-of-sight is not perpendicular to the plume, it may be
necessary to correct the opacity measured by the lidar to obtain the
opacity that would be measured on a path perpendicular to the plume.
The following method, or any other method which produces equivalent
results, shall be used to determine the need for a correction, to
calculate the correction, and to document the point within the plume at
which the opacity was measured.
Figure AM1-IV(b) shows the geometry of the opacity correction. L' is
the path through the plume along which the opacity measurement is made.
P' is the path perpendicular to the plume at the same point. The angle
is the angle between L' and the plume center line. The angle (p/2- ),
is the angle between the L' and P'. The measured opacity, Op, measured
along the path L' shall be corrected to obtain the corrected opacity,
Opc, for the path P', using Equation (AM1-8).
insert illus. 01224A
The correction in Equation (AM1-8) shall be performed if the
inequality in Equation (AM1-9) is true.
insert illus. 01224B
Figure AM1-IV(a) shows the geometry used to calculate and the
position in the plume at which the lidar measurement is made. This
analysis assumes that for a given lidar measurement, the range from the
lidar to the plume, the elevation angle of the lidar from the horizontal
plane, and the azimuth angle of the lidar from an arbitrary fixed
reference in the horizontal plane can all be obtained directly.
Insert illus. 0816
Rs=range from lidar to source*
s=elevation angle of Rs*
Rp=range from lidar to plume at the opacity measurement point*
p=elevation angle of Rp*
Ra=range from lidar to plume at some arbitrary point, Pa, so the
drift angle of the plume can be determined*
a=elevation angle of Ra*
=angle between Rp and Ra
R's=projection of Rs in the horizontal plane
R'p=projection of Rp in the horizontal plane
R'a=projection of Ra in the horizontal plane
'=angle between R's and R'p*
'=angle between R'p and R'a*
R =distance from the source to the opacity measurement point
projected in the horizontal plane
R =distance from opacity measurement point Pp to the point in the
plume Pa.
insert illus. 0815A
The correction angle shall be determined using Equation AM1-10.
Where:
=Cos^1 (Cos p Cos a Cos '+Sin p Sin a),
and
R =(Rp2+Ra2^2 Rp Ra Cos )1/2
R , the distance from the source to the opacity measurement point
projected in the horizontal plane, shall be determined using Equation
AM1-11.
insert illus 0817B
Where:
R's=Rs Cos s, and
R'p=Rp Cos p.
In the special case where the plume centerline at the opacity
measurement point is horizontal, parallel to the ground, Equation AM1-12
may be used to determine instead of Equation AM1-10.
insert illus. 01224E
Where:
R''s=(R'2s+Rp2 Sin2 p)1/2.
If the angle is such that 30 or 150 , the azimuth angle
correction shall not be performed and the associated opacity value shall
be discarded.
2.6.2 Elevation Angle Correction. An individual lidar-measured
opacity, Op, shall be corrected for elevation angle if the laser
elevation or inclination angle, p (Figure AM1-V), is greater than or
equal to the value calculated in Equation AM1-13.
insert illus. 01224F
The measured opacity, Op, along the lidar path L, is adjusted to
obtain the corrected opacity, Opc, for the actual plume (horizontal)
path, P, by using Equation (AM1-14).
insert illus. 01224G
Where:
p=lidar elevation or inclination angle,
Op=measured opacity along path L, and
Opc=corrected opacity for the actual plume thickness P.
The values for p, Op and Opc should be recorded.
Insert illus. 0819
2.6.3 Determination of Actual Plume Opacity. Actual opacity of the
plume shall be determined by Equation AM1-15.
insert illus. 0820A
2.6.4 Calculation of Average Actual Plume Opacity. The average of
the actual plume opacity, Opa, shall be calculated as the average of the
consecutive individual actual opacity values, Opa, by Equation AM1-16.
insert illus 0820B
Where:
(Opa)k=the kth actual opacity value in an averaging interval
containing n opacity values; k is a summing index.
=the sum of the individual actual opacity values.
n=the number of individual actual opacity values contained in the
averaging interval.
Opa=average actual opacity calculated over the averaging interval.
3. Lidar Performance Verification
The lidar shall be subjected to two types of performance
verifications that shall be peformed in the field. The annual
calibration, conducted at least once a year, shall be used to directly
verify operation and performance of the entire lidar system. The
routine verification, conducted for each emission source measured, shall
be used to insure proper performance of the optical receiver and
associated electronics.
3.1 Annual Calibration Procedures. Either a plume from a smoke
generator or screen targets shall be used to conduct this calibration.
If the screen target method is selected, five screens shall be
fabricated by placing an opaque mesh material over a narrow frame (wood,
metal extrusion, etc.). The screen shall have a surface area of at least
one square meter. The screen material should be chosen for precise
optical opacities of about 10, 20, 40, 60, and 80%. Opacity of each
target shall be optically determined and should be recorded. If a smoke
generator plume is selected, it shall meet the requirements of Section
3.3 of Reference Method 9. This calibration shall be performed in the
field during calm (as practical) atmospheric conditions. The lidar
shall be positioned in accordance with Section 2.1.
The screen targets must be placed perpendicular to and coincident
with the lidar line-of-sight at sufficient height above the ground
(suggest about 30 ft) to avoid ground-level dust contamination.
Reference signals shall be obtained just prior to conducting the
calibration test.
The lidar shall be aimed through the center of the plume within 1
stack diameter of the exit, or through the geometric center of the
screen target selected. The lidar shall be set in operation for a
6-minute data run at a nominal pulse rate of 1 pulse every 10 seconds.
Each backscatter return signal and each respective opacity value
obtained from the smoke generator transmissometer, shall be obtained in
temporal coincidence. The data shall be analyzed and reduced in
accordance with Section 2.6 of this method. This calibration shall be
performed for 0% (clean air), and at least five other opacities
(nominally 10, 20, 40, 60, and 80%).
The average of the lidar opacity values obtained during a 6-minute
calibration run shall be calculated and should be recorded. Also the
average of the opacity values obtained from the smoke generator
transmissometer for the same 6-minute run shall be calculated and should
be recorded.
Alternate calibration procedures that do not meet the above
requirements but produce equivalent results may be used.
3.2 Routine Verification Procedures. Either one of two techniques
shall be used to conduct this verification. It shall be performed at
least once every 4 hours for each emission source measured. The
following parameters shall be directly verified.
1) The opacity value of 0% plus a minimum of 5 (nominally 10, 20, 40,
60, and 80%) opacity values shall be verified through the PMT detector
and data processing electronics.
2) The zero-signal level (receiver signal with no optical signal from
the source present) shall be inspected to insure that no spurious noise
is present in the signal. With the entire lidar receiver and
analog/digital electronics turned on and adjusted for normal operating
performance, the following procedures shall be used for Techniques 1 and
2, respectively.
3.2.1 Procedure for Technique 1. This test shall be performed with
no ambient or stray light reaching the PMT detector. The narrow band
filter (694.3 nanometers peak) shall be removed from its position in
front of the PMT detector. Neutral density filters of nominal opacities
of 10, 20, 40, 60, and 80% shall be used. The recommended test
configuration is depicted in Figure AM1-VI.
Insert illus. 0823
The zero-signal level shall be measured and should be recorded, as
indicated in Figure AM1-VI(a). This simulated clear-air or 0% opacity
value shall be tested in using the selected light source depicted in
Figure AM1-VI(b).
The light source either shall be a continuous wave (CW) laser with
the beam mechanically chopped or a light emitting diode controlled with
a pulse generator (rectangular pulse). (A laser beam may have to be
attenuated so as not to saturate the PMT detector). This signal level
shall be measured and should be recorded. The opacity value is
calculated by taking two pick intervals (Section 2.6) about 1
microsecond apart in time and using Equation (AM1-2) setting the ratio
Rn/Rf=1. This calculated value should be recorded.
The simulated clear-air signal level is also employed in the optical
test using the neutral density filters. Using the test configuration in
Figure AM1-VI(c), each neutral density filter shall be separately placed
into the light path from the light source to the PMT detector. The
signal level shall be measured and should be recorded. The opacity
value for each filter is calculated by taking the signal level for that
respective filter (If), dividing it by the 0% opacity signal level (In)
and performing the remainder of the calculation by Equation (AM1-2) with
Rn/Rf=1. The calculated opacity value for each filter should be
recorded.
The neutral density filters used for Technique 1 shall be calibrated
for actual opacity with accuracy of 2% or better. This calibration
shall be done monthly while the filters are in use and the calibrated
values should be recorded.
3.2.2 Procedure for Technique 2. An optical generator (built-in
calibration mechanism) that contains a light-emitting diode (red light
for a lidar containing a ruby laser) is used. By injecting an optical
signal into the lidar receiver immediately ahead of the PMT detector, a
backscatter signal is simulated. With the entire lidar receiver
electronics turned on and adjusted for normal operating performance, the
optical generator is turned on and the simulation signal (corrected for
1/R /2/ ) is selected with no plume spike signal and with the opacity
value equal to 0%. This simulated clear-air atmospheric return signal
is displayed on the system's video display. The lidar operator then
makes any fine adjustments that may be necessary to maintain the
system's normal operating range.
The opacity values of 0% and the other five values are selected one
at a time in any order. The simulated return signal data should be
recorded. The opacity value shall be calculated. This
measurement/calculation shall be performed at least three times for each
selected opacity value. While the order is not important, each of the
opacity values from the optical generator shall be verified. The
calibrated optical generator opacity value for each selection should be
recorded.
The optical generator used for Technique 2 shall be calibrated for
actual opacity with an accuracy of 1% or better. This calibration
shall be done monthly while the generator is in use and calibrated value
should be recorded.
Alternate verification procedures that do not meet the above
requirements but produce equivalent results may be used.
3.3 Deviation. The permissible error for the annual calibration and
routine verification are:
3.3.1 Annual Calibration Deviation.
3.3.1.1 Smoke Generator. If the lidar-measured average opacity for
each data run is not within 5% (full scale) of the respective smoke
generator's average opacity over the range of 0% through 80%, then the
lidar shall be considered out of calibration.
3.3.1.2 Screens. If the lidar-measured average opacity for each data
run is not within 3% (full scale) of the laboratory-determined opacity
for each respective simulation screen target over the range of 0%
through 80%, then the lidar shall be considered out of calibration.
3.3.2 Routine Verification Error. If the lidar-measured average
opacity for each neutral density filter (Technique 1) or optical
generator selection (Technique 2) is not within 3% (full scale) of the
respective laboratory calibration value then the lidar shall be
considered non-operational.
4. Performance/Design Specification for Basic Lidar System
4.1 Lidar Design Specification. The essential components of the
basic lidar system are a pulsed laser (transmitter), optical receiver,
detector, signal processor, recorder, and an aiming device that is used
in aiming the lidar transmitter and receiver. Figure AM1-VII shows a
functional block diagram of a basic lidar system.
Insert illus. 0827
4.2 Performance Evaluation Tests. The owner of a lidar system shall
subject such a lidar system to the performance verification tests
described in Section 3, prior to first use of this method. The annual
calibration shall be performed for three separate, complete runs and the
results of each should be recorded. The requirements of Section 3.3.1
must be fulfilled for each of the three runs.
Once the conditions of the annual calibration are fulfilled the lidar
shall be subjected to the routine verification for three separate
complete runs. The requirements of Section 3.3.2 must be fulfilled for
each of the three runs and the results should be recorded. The
Administrator may request that the results of the performance evaluation
be submitted for review.
5. References
5.1 The Use of Lidar for Emissions Source Opacity Determination, U.S.
Environmental Protection Agency, National Enforcement Investigations
Center, Denver, CO. EPA-330/1-79-003-R, Arthur W. Dybdahl, current
edition (NTIS No. PB81-246662).
5.2 Field Evaluation of Mobile Lidar for the Measurement of Smoke
Plume Opacity, U.S. Environmental Protection Agency, National
Enforcement Investigations Center, Denver, CO. EPA/NEIC-TS-128,
February 1976.
5.3 Remote Measurement of Smoke Plume Transmittance Using Lidar, C.
S. Cook, G. W. Bethke, W. D. Conner (EPA/RTP). Applied Optics 11, pg
1742. August 1972.
5.4 Lidar Studies of Stack Plumes in Rural and Urban Environments,
EPA-650/4-73-002, October 1973.
5.5 American National Standard for the Safe Use of Lasers ANSI Z
136.1-176, March 8, 1976.
5.6 U.S. Army Technical Manual TB MED 279, Control of Hazards to
Health from Laser Radiation, February 1969.
5.7 Laser Institute of America Laser Safety Manual, 4th Edition.
5.8 U.S. Department of Health, Education and Welfare, Regulations for
the Administration and Enforcement of the Radiation Control for Health
and Safety Act of 1968, January 1976.
5.9 Laser Safety Handbook, Alex Mallow, Leon Chabot, Van Nostrand
Reinhold Co., 1978.
*Obtained directly from lidar. These values should be recorded.
40 CFR 60.748 Pt. 60, App. A, Meth. 10
1. Principle and Applicability
1.1 Principle. An integrated or continuous gas sample is extracted
from a sampling point and analyzed for carbon monoxide (CO) content
using a Luft-type nondispersive infrared analyzer (NDIR) or equivalent.
1.2 Applicability. This method is applicable for the determination of
carbon monoxide emissions from stationary sources only when specified by
the test procedures for determining compliance with new source
performance standards. The test procedure will indicate whether a
continuous or an integrated sample is to be used.
2. Range and Sensitivity
2.1 Range. 0 to 1,000 ppm.
2.2 Sensitivity. Minimum detectable concentration is 20 ppm for a 0
to 1,000 ppm span.
3. Interferences
Any substance having a strong absorption of infrared energy will
interfere to some extent. For example, discrimination ratios for water
(H2O) and carbon dioxide (CO2) are 3.5 percent H2O per 7 ppm CO and 10
percent CO2 per 10 ppm CO, respectively, for devices measuring in the
1,500 to 3,000 ppm range. For devices measuring in the 0 to 100 ppm
range, interference ratios can be as high as 3.5 percent H2O per 25 ppm
CO and 10 percent CO2 per 50 ppm CO. The use of silica gel and ascarite
traps will alleviate the major interference problems. The measured gas
volume must be corrected if these traps are used.
4. Precision and Accuracy
4.1 Precision. The precision of most NDIR analyzers is approximately
2 percent of span.
4.2 Accuracy. The accuracy of most NDIR analyzers is approximately 5
percent of span after calibration.
5. Apparatus
5.1 Continuous Sample (Figure 10-1).
5.1.1 Probe. Stainless steel or sheathed Pyrex /1/ glass, equipped
with a filter to remove particulate matter.
5.1.2 Air-Cooled Condenser or Equivalent. To remove any excess
moisture.
5.2 Integrated Sample (Figure 10-2).
5.2.1 Probe. Stainless steel or sheathed Pyrex glass, equipped with a
filter to remove particulate matter.
5.2.2 Air-Cooled Condenser or Equivalent. To remove any excess
moisture.
5.2.3 Valve. Needle valve, or equivalent, to to adjust flow rate.
5.2.4 Pump. Leak-free diaphragm type, or equivalent, to transport
gas.
5.2.5 Rate Meter. Rotameter, or equivalent, to measure a flow range
from 0 to 1.0 liter per min (0.035 cfm).
5.2.6 Flexible Bag. Tedlar, or equivalent, with a capacity of 60 to
90 liters (2 to 3 ft /3/ ). Leak-test the bag in the laboratory before
using by evacuating bag with a pump followed by a dry gas meter. When
evacuation is complete, there should be no flow through the meter.
5.2.7 Pitot Tube. Type S, or equivalent, attached to the probe so
that the sampling rate can be regulated proportional to the stack gas
velocity when velocity is varying with the time or a sample traverse is
conducted.
5.3 Analysis (Figure 10-3).
5.3.1 Carbon Monoxide Analyzer. Nondispersive infrared spectrometer,
or equivalent. This instrument should be demonstrated, preferably by
the manufacturer, to meet or exceed manufacturer's specifications and
those described in this method.
5.3.2 Drying Tube. To contain approximately 200 g of silica gel.
5.3.3 Calibration Gas. Refer to section 6.1.
5.3.4 Filter. As recommended by NDIR manufacturer.
Insert illus. 18A
5.3.5 CO2 Removal Tube. To contain approximately 500 g of ascarite.
5.3.6 Ice Water Bath. For ascarite and silica gel tubes.
5.3.7 Valve. Needle valve, or equivalent, to adjust flow rate
5.3.8 Rate Meter. Rotameter or equivalent to measure gas flow rate
of 0 to 1.0 liter per min (0.035 cfm) through NDIR.
5.3.9 Recorder (optional). To provide permanent record of NDIR
readings.
6. Reagents
6.1 Calibration Gases. Known concentration of CO in nitrogen (N2)
for instrument span, prepurified grade of N2 for zero, and two
additional concentrations corresponding approximately to 60 percent and
30 percent span. The span concentration shall not exceed 1.5 times the
applicable source performance standard. The calibration gases shall be
certified by the manufacturer to be within 2 percent of the specified
concentration.
Insert illus. 19A
6.2 Silica Gel. Indicating type, 6 to 16 mesh, dried at 175 C (347
F) for 2 hours.
6.3 Ascarite. Commercially available.
7. Procedure
7.1 Sampling.
7.1.1 Continuous Sampling. Set up the equipment as shown in Figure
10-1 making sure all connections are leak free. Place the probe in the
stack at a sampling point and purge the sampling line. Connect the
analyzer and begin drawing sample into the analyzer. Allow 5 minutes
for the system to stabilize, then record the analyzer reading as
required by the test procedure. (See section7.2 and 8). CO2 content of
the gas may be determined by using the Method 3 integrated sample
procedure, or by weighing the ascarite CO2 removal tube and computing
CO2 concentration from the gas volume sampled and the weight gain of the
tube.
7.1.2 Integrated Sampling. Evacuate the flexible bag. Set up the
equipment as shown in Figure 10-2 with the bag disconnected. Place the
probe in the stack and purge the sampling line. Connect the bag, making
sure that all connections are leak free. Sample at a rate proportional
to the stack velocity. CO2 content of the gas may be determined by
using the Method 3 integrated sample procedures, or by weighing the
ascarite CO2 removal tube and computing CO2 concentration from the gas
volume sampled and the weight gain of the tube.
7.2 CO Analysis. Assemble the apparatus as shown in Figure 10-3,
calibrate the instrument, and perform other required operations as
described in section 8. Purge analyzer with N2 prior to introduction of
each sample. Direct the sample stream through the instrument for the
test period, recording the readings. Check the zero and span again
after the test to assure that any drift or malfunction is detected.
Record the sample data on Table 10-1.
8. Calibration
Assemble the apparatus according to Figure 10-3. Generally an
instrument requires a warm-up period before stability is obtained.
Follow the manufacturer's instructions for specific procedure. Allow a
minimum time of 1 hour for warm-up. During this time check the sample
conditioning apparatus, i.e., filter, condenser, drying tube, and CO2
removal tube, to ensure that each component is in good operating
condition. Zero and calibrate the instrument according to the
manufacturer's procedures using, respectively, nitrogen and the
calibration gases.
9. Calculation
Calculate the concentration of carbon monoxide in the stack using
Equation 10-1.
Eq. 10-1
Where:
CCO stack=Concentration of CO in stack, ppm by volume (dry basis).
CCO NDIR=Concentration of CO measured by NDIR analyzer, ppm by volume
(dry basis).
FCO2=Volume fraction of CO2 in sample, i.e., percent CO2 from Orsat
analysis divided by 100.
10.1 Interference Trap. The sample conditioning system described in
Method 10A, sections 2.1.2 and 4.2, may be used as an alternative to the
silica gel and ascarite traps.
11. Bibliography
1. McElroy, Frank, The Intertech NDIR-CO Analyzer, Presented at 11th
Methods Conference on Air Pollution, University of California, Berkeley,
CA. April 1, 1970.
2. Jacobs, M. B., et al., Continuous Determination of Carbon
Monoxide and Hydrocarbons in Air by a Modified Infrared Analyzer, J.
Air Pollution Control Association, 9(2): 110-114. August 1959.
3. MSA LIRA Infrared Gas and Liquid Analyzer Instruction Book, Mine
Safety Appliances Co., Technical Products Division, Pittsburgh, PA.
4. Models 215A, 315A, and 415A Infrared Analyzers, Beckman
Instruments, Inc., Beckman Instructions 1635-B, Fullerton, CA. October
1967.
5. Continuous CO Monitoring System, Model A5611, Intertech Corp.,
Princeton, NJ.
6. UNOR Infrared Gas Analyzers, Bendix Corp., Ronceverte, WV
Analyzers
B. Definitions of Performance Specifications.
Range -- The minimum and maximum measurement limits.
Output -- Electrical signal which is proportional to the measurement;
intended for connection to readout or data processing devices. Usually
expressed as millivolts or milliamps full scale at a given impedance.
Full scale -- The maximum measuring limit for a given range.
Minimum detectable sensitivity -- The smallest amount of input
concentration that can be detected as the concentration approaches zero.
Accuracy -- The degree of agreement between a measured value and the
true value; usually expressed as percent of full scale.
Time to 90 percent response -- The time interval from a step change
in the input concentration at the instrument inlet to a reading of 90
percent of the ultimate recorded concentration.
Rise Time (90 percent) -- The interval between initial response time
and time to 90 percent response after a step increase in the inlet
concentration.
Fall Time (90 percent) -- The interval between initial response time
and time to 90 percent response after a step decrease in the inlet
concentration.
Zero Drift -- The change in instrument output over a stated time
period, usually 24 hours, of unadjusted continuous operation when the
input concentration is zero; usually expressed as percent full scale.
Span Drift -- The change in instrument output over a stated time
period, usually 24 hours, of unadjusted continuous operation when the
input concentration is a stated upscale value; usually expressed as
percent full scale.
Precision -- The degree of agreement between repeated measurements of
the same concentration, expressed as the average deviation of the single
results from the mean.
Noise -- Spontaneous deviations from a mean output not caused by
input concentration changes.
Linearity -- The maximum deviation between an actual instrument
reading and the reading predicted by a straight line drawn between upper
and lower calibration points.
/1/ Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
40 CFR 60.748 Pt. 60, App. A, Meth. 10A
Petroleum Refineries
1.1 Applicability. This method applies to the measurement of carbon
monoxide (CO) at petroleum refineries. This method serves as the
reference method in the relative accuracy test for nondispersive
infrared (NDIR) CO continuous emission monitoring systems (CEMS's) that
are required to be installed in petroleum refineries on fluid catalytic
cracking unit catalyst regenerators (40 CFR Part 60.105(a)(2)).
1.2 Principle. An integrated gas sample is extracted from the stack,
passed through an alkaline permanganate solution to remove sulfur and
nitrogen oxides, and collected in a Tedlar bag. The CO concentration in
the sample is measured spectrophotometrically using the reaction of CO
with p-sulfaminobenzoic acid.
1.3. Range and Sensitivity.
1.3.1 Range. Approximately 3 to 1800 ppm CO. Samples having
concentrations below 400 ppm are analyzed at 425 nm, and samples having
concentrations above 400 ppm are analyzed at 600 nm.
1.3.2 Sensitivity. The detection limit is 3 ppm based on three times
the standard deviation of the mean reagent blank values.
1.4 Interferences. Sulfur oxides, nitric oxide, and other acid gases
interfere with the colorimetric reaction. They are removed by passing
the sampled gas through an alkaline potassium permanganate scrubbing
solution. Carbon dioxide (CO2) does not interfere, but, because it is
removed by the scrubbing solution, its concentration must be measured
independently and an appropriate volume correction made to the sampled
gas.
1.5 Precision, Accuracy, and Stability.
1.5.1 Precision. The estimated intralaboratory standard deviation of
the method is 3 percent of the mean for gas samples analyzed in
duplicate in the concentration range of 39 to 412 ppm. The
interlaboratory precision has not been established.
1.5.2 Accuracy. The method contains no significant biases when
compared to an NDIR analyzer calibrated with National Bureau of
Standards (NBS) standards.
1.5.3 Stability. The individual components of the colorimetric
reagent are stable for at least 1 month. The colorimetric reagent must
be used within 2 days after preparation to avoid excessive blank
correction. The samples in the Tedlar /1/ bag should be stable for at
least 1 week if the bags are leak-free.
2.1 Sampling. The sampling train is shown in Figure 10A-1, and
component parts are discussed below:
2.1.1 Probe. Stainless steel, sheathed Pyrex glass, or equivalent,
equipped with a glass wool plug to remove particulate matter.
2.1.2 Sample Conditioning System. Three Greenburg-Smith impingers
connected in series with leak-free connections.
2.1.3 Pump. Leak-free pump with stainless steel and Teflon parts to
transport sample at a flow rate of 300 ml/min to the flexible bag.
2.1.4 Surge Tank. Installed between the pump and the rate meter to
eliminate the pulsation effect of the pump on the rate meter.
2.1.5 Rate Meter. Rotameter, or equivalent, to measure flow rate at
300 ml/min. Calibrate according to Section 5.2.
2.1.6 Flexible Bag. Tedlar, or equivalent, with a capacity of 10
liters and equipped with a sealing quick-connect plug. The bag must be
leak-free according to Section 4.1. For protection, it is recommened
that the bag be enclosed with a rigid container.
2.1.7 Valves. Stainless-steel needle valve to adjust flow rate, and
stainless-steel three-way valve, or equivalent.
2.1.8 CO2 Analyzer. Method 3 or its approved alternative to measure
CO2 concentration to within 0.5 percent.
2.1.9 Volume Meter. Dry gas meter, calibrated and capable of
measuring the sample volume under rotameter calibration conditions of
300 ml/min for 10 minutes
2.1.10 Pressure Gauge. A water filled U-tube manometer, or
equivalent, of about 28 cm (12 in.) to leak-check the flexible bag.
2.2 Analysis.
2.2.1 Spectrophotometer. Single- or double-beam to measure absorbance
at 425 and 600 nm. Slit width should not exceed 20 nm.
2.2.2 Spectrophotometer Cells. 1-cm pathlength.
2.2.3 Vacuum Gauge. U-tube mercury manometer, 1 meter (39 in.), with
1-mm divisions, or other gauge capable of measuring pressure to within 1
mm Hg.
2.2.4 Pump. Capable of evacuating the gas reaction bulb to a pressure
equal to or less than 40 mm Hg absolute, equipped with coarse and fine
flow control valves.
2.2.5 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 1 mm Hg.
2.2.6 Reaction Bulbs. Pyrex glass, 100.ml with Teflon stopcock
(Figure 10A-2), leak-free at 40 mm Hg, designed so that 10 ml of the
colorimetric reagent can be added and removed easily and accurately.
Commercially available gas sample bulbs such as Supelco Catalog No.
2-2161 may also be used.
Insert Illus 100
2.2.7 Manifold. Stainless steel, with connections for three reaction
bulbs and the appropriate connections for the manometer and sampling bag
as shown in Figure 10A-3.
2.2.8 Pipets. Class A, 10-ml size.
2.2.9 Shaker Table. Reciprocating-stroke type such as Eberbach
Corporation, Model 6015. A rocking arm or rotary-motion type shaker may
also be used. The shaker must be large enough to accommodate at least
six gas sample bulbs simultaneously. It may be necessary to construct a
table top extension for most commercial shakers to provide sufficient
space for the needed bulbs (Figure 10A-4).
2.2.10 Valve. Stainless steel shut-off valve.
2.2.11 Analytical Balance. Capable of accurately weighing to 0.1 mg.
Unless otherwise indicated, all reagents shall conform to the
specifications established by the Committee on Analytical Reagents of
the American Chemical Society, where such specifications are available,
otherwise, the best available grade shall be used.
3.1 Sampling.
3.1.1 Water. Deionized distilled, as described in Method 6, Section
3.1.1.
3.1.2 Alkaline Permanganate Solution, 0.25 M KMn04/1.5 M NaOH.
Dissolve 40 g KMn04 and 60 g NaOH in water, and dilute to 1 liter.
3.2 Analysis.
3.2.1 Water. Same as in Section 3.1.1.
3.2.2 1 M Sodium Hydroxide (NaOH) Solution. Dissolve 40 g NaOH in
approximately 900 ml of water, cool, and dilute to 1 liter.
3.2.3 0.1 M Silver Nitrate (AgNO3) Solution. Dissolve 8.5 g AgNO3 in
water, and dilute to 500 ml.
3.2.4 0.1 M Para-Sulfaminobenzoic Acid (p-SABA) Solution. Dissolve
10.0 g p-SABA in 0.1 M NaOH (prepared by diluting 50 ml of 1 M NaOH to
500 ml), and dilute to 500 ml with 0.1 M NaOH.
3.2.5 Colorimetric Solution. To a flask, add 100 ml of p-SABA
solution and 100 ml of AgNO3 solution. Mix, and add 50 ml of 1 M NaOH
with shaking. The resultant solution should be clear and colorless.
This solution is acceptable for use for a period of 2 days.
3.2.6 Standard Gas Mixtures. Traceable to NBS standards and
containing between 50 and 1000 ppm CO in nitrogen. At least two
concentrations are needed to span each calibration range used (Section
5.3).
The calibration gases shall be certified by the manufacturer to be
within 2 percent of the specified concentrations.
4.1 Sample Bag Leak-checks. While a bag leak-check is required after
bag use, it should also be done before the bag is used for sample
collection. The bag should be leak-checked in the inflated and deflated
condition according to the following procedures.
Connect the bag to a water manometer, and pressurize the bag to 5 to
10 cm H20 (2 to 4 in. H20). Allow the bag to stand for 60 minutes. Any
displacement in the water manometer indicates a leak. Now, evacuate the
bag with a leakless pump that is connected on the downstream side of a
flow-indicating device such as a 0-to 100-ml/min rotameter or an
impinger containing water. When the bag is completely evacuated, no
flow should be evident if the bag is leak-free.
4.2 Sampling. Evacuate the Tedlar bag completely using a vacuum pump.
Assemble the apparatus as shown in Figure 10A-1. Loosely pack glass
wool in the tip of the probe. Place 400 ml of alkaline permanganate
solution in the first two impingers and 250 ml in the third. Connect
the pump to the third impinger, and follow this with the surge tank,
rate meter, and three-way valve. Do not connect the Tedlar bag to the
system at this time.
Leak-check the sampling system by placing a vacuum gauge at or near
the probe inlet, plugging the probe inlet, opening the three-way valve,
and pulling a vacuum of approximately 250 mm Hg on the system while
observing the rate meter for flow. If flow is indicated on the rate
meter, do not proceed further until the leak is found and corrected.
Purge the system with sample gas by inserting the probe into the
stack and drawing sample through the system at 300 ml/min 10 percent
for 5 minutes. Connect the evacuated Tedlar bag to the system, record
the starting time, and sample at a rate of 300 ml/min for 30 minutes, or
until the Tedlar bag is nearly full. Record the sampling time, the
barometric pressure, and the ambient temperature. Purge the system as
described above immediately before each sample.
The scrubbing solution is adequate for removing sulfur and nitrogen
oxides from 50 liters of stack gas when the concentration of each is
less than 1,000 ppm and the CO2 concentration is less than 15 percent.
Replace the scrubber solution after every fifth sample.
4.3 Carbon Dioxide Measurement. Measure the CO2 content in the stack
to the nearest 0.5 percent each time a CO sample is collected. A
simultaneous grab sample analyzed by the Fyrite analyzer is acceptable.
4.4 Analysis. Assemble the system shown in Figure 10A-3, and record
the information required in Table 10A-1 as it is obtained. Pipet 10.0
ml of the colorimetric reagent into each gas reaction bulb, and attach
the bulbs to the system. Open the stopcocks to the reaction bulbs, but
leave the valve to the Tedlar bag closed. Turn on the pump, fully open
the coarse-adjust flow valve, and slowly open the fine-adjust valve
until the pressure is reduced to at least 40 mm Hg. Now close the
coarse adjust valve, and observe the manometer to be certain that the
system is leak-free. Wait a minimum of 2 minutes. If the pressure has
increased less than 1 mm, proceed as described below. If a leak is
present, find and correct it before proceeding further.
Record the vacuum pressure (Pv) to the nearest 1 mm Hg, and close the
reaction bulb stopcocks. Open the Tedlar bag valve, and allow the
system to come to atmospheric pressure. Close the bag valve, open the
pump coarse adjust valve, and evacuate the system again. Repeat this
fill/evacuation procedure at least twice to flush the manifold
completely. Close the pump coarse adjust valve, open the Tedlar bag
valve, and let the system fill to atmospheric pressure. Open the
stopcocks to the reaction bulbs, and let the entire system come to
atmospheric pressure. Close the bulb stopcocks, remove the bulbs,
record the room temperature and barametric pressure (Pbar, to nearest mm
Hg), and place the bulbs on the shaker table with their main axis either
parallel to or perpendicular to the plane of the table top. Purge the
bulb-filling system with ambient air for several minutes between
samples. Shake the samples for exactly 2 hours.
Immediately after shaking, measure the absorbance (A) of each bulb
sample at 425 nm if the concentration is less than or equal to 400 ppm
CO or at 600 nm if the concentration is above 400 ppm. This may be
accomplished with multiple bulb sets by sequentially collecting sets and
adding to the shaker at staggered intervals, followed by sequentially
removing sets from the shaker for absorbance measurement after the
two-hour designated intervals have elapsed.
Use a small portion of the sample to rinse a spectrophotometer cell
several times before taking an aliquot for analysis. If one cell is
used to analyze multiple samples, rinse the cell several times between
samples with water.
Prepare and analyze standards and a reagent blank as described in
Section 5.3. Use water as the reference. Reject the analysis if the
blank absorbance is greater than 0.1. All conditions should be the same
for analysis of samples and standards. Measure the absorbances as soon
as possible after shaking is completed. Determine the CO concentration
of each bag sample using the calibration curve for the appropriate
concentration range as discussed in Section 5.3.
5.1 Bulb Calibration. Weigh the empty bulb to the nearest 0.1 g.
Fill the bulb to the stopcock with water, and again weigh to the nearest
0.1 g. Subtract the tare weight, and calculate the volume in liters to
three significant figures using the density of water (at the measurement
temperature). Record the volume on the bulb; alternatively, mark an
identification number on the bulb, and record the volume in a notebook.
5.2 Rate Meter Calibration. Assemble the system as shown in Figure
10A-1 (the impingers may be removed), and attach a volume meter to the
probe inlet. Set the rotameter at 300 ml/min, record the volume meter
reading, start the pump, and pull gas through the system for 10 minutes.
Record the final volume meter reading. Repeat the procedure and
average the results to determine the volume of gas that passed through
the system.
5.3 Spectrophotometer Calibration Curve. The calibration curve is
established by taking at least two sets of three bulbs of known CO
collected from Tedlar bags through the analysis procedure. Reject the
standard set where any of the individual bulb absorbances differ from
the set mean by more than 10 percent. Collect the standards as
described in Section 4.2. Prepare standards to span the 0- to 400- or
400- to 1000-ppm range. If any samples span both concentration ranges,
prepare a calibration curve for each range. A set of three bulbs
containing colorimetric reagent but no CO should serve as a reagent
blank and be taken through the analysis procedure.
Calculate the average absorbance for each set (3 bulbs) of standards
using Equation 10A-1 and Table 10A-1. Construct a graph of average
absorbance for each standard against its corresponding concentration in
ppm. Draw a smooth curve through the points. The curve should be
linear over the two concentration ranges discussed in Section 1.3.1.
Carry out calculations retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after final
calculation.
A=Sample absorbance, uncorrected for the reagent blank.
Ar=Aborbance of the reagent blank.
As=Average sample absorbance per liter, units/liter.
Bw=Moisture content in the bag sample.
C=CO concentration in the stack gas, dry basis, ppm.
Cb=CO concentration of the bag sample, dry basis, ppm.
Cg=CO concentration from the calibration curve, ppm.
F=Volume fraction of CO2 in the stack.
n=Number of reaction bulbs used per bag sample.
Pbar=Barometric pressure, mm Hg.
Pv=Residual pressure in the sample bulb after evacuation, mm Hg.
Pw=Vapor pressure of H20 in the bag (from Table 10A-2), mm Hg.
Vb=Volume of the sample bulb, liters.
Vr=Volume of reagent added to the sample bulb, 0.0100 liter.
Average the three absorbance values for each bulb set. Then
calculate As for each set of gas bulbs using Equation 10A-1. Use As to
determine the CO concentration from the calibration curve (Cg).
Eq. 10A-1
Note: A and Ar must be at the same wavelength.
Calculate Cb using Equations 10A-2 and 10A-3. If condensate is
visible in the Tedlar bag, calculate Bw using Table 10A-2 and the
temperature and barometric pressure in the analysis room. If condensate
is not visible, calculate Bw using the temperature and barometric
pressure recorded at the sampling site.
6.4 CO Concentration in the Stack.
C = Cb (1^F)
Eq. 10A-4
1. Butler, F.E., J.E. Knoll, and M.R. Midgett. Development and
Evaluation of Methods for Determining Carbon Monoxide Emissions.
Quality Assurance Division, Environmental Monitoring Systems Laboratory,
U.S. Environmental Protection Agency, Research Triangle Park, NC 27711.
June 1985. 33 p.
2. Ferguson, B.B., R.E. Lester, and W.J. Mitchell. Field Evaluation
of Carbon Monoxide and Hydrogen Sulfide Continuous Emission Monitors at
an Oil Refinery. U.S. Environmental Protection Agency. Research
Triangle Park, NC. Publication No. EPA-600/4-82-054. August 1982. 100
p.
3. Lambert, J.L., and R.E. Weins. Induced Colorimetric Method for
Carbon Monoxide. Analytical Chemistry. 46(7):929-930. June 1974.
4. Levaggi, D.A., and M. Feldstein. The Colorimetric Determination
of Low Concentrations of Carbon Monoxide. Industrial Hygiene Journal.
25:64-66. January-February 1964.
5. Repp, M. Evaluation of Continuous Monitors for Carbon Monoxide in
Stationary Sources. U.S. Environmental Protection Agency. Research
Triangle Park, NC. Publication No. EPA-600/2-77-063. March 1977. 155
p.
6. Smith, F., D.E. Wagoner, and R.P. Donovan. Guidelines for
Development of a Quality Assurance Program: Volume VIII --
Determination of CO Emissions from Stationary Sources by NDIR
Spectrometry. U.S. Environmental Protection Agency. Research Triangle
Park, NC. Publication No. EPA-650/4-74-005-h. Febraury 1975. 96 p.
/1/ Mention of trade names or commercial products in this publication
does not constitute the endorsement or recommendation for use by the
Environmental Protection Agency.
40 CFR 60.748 Pt. 60, App. A, Meth. 10B
1.1 Applicability. This method applies to the measurement of carbon
monoxide (CO) emissions at petroleum refineries and from other sources
when specified in an applicable subpart of the regulations.
1.2 Principle. An integrated gas sample is extracted from the
sampling point and analyzed for CO. The sample is passed through a
conditioning system to remove interferences and collected in a Tedlar
bag. The CO is separated from the sample by gas chromatography (GC) and
catalytically reduced to methane (CH4) prior to analysis by flame
ionization detection FID. The analytical portion of this method is
identical to applicable sections in Method 25 detailing CO measurement.
The oxidation catalyst required in Method 25 is not needed for sample
analysis. Complete Method 25 analytical systems are acceptable
alternatives when calibrated for CO and operated by the Method 25
analytical procedures.
Note: Mention of trade names or commercial products in this method
does not constitute the endorsement or recommendation for use by the
Environmental Protection Agency.
1.3 Interferences. Carbon dioxide (CO2) and organics potentially can
interfere with the analysis. Carbon dioxide is primarily removed from
the sample by the alkaline permanganate conditioning system; any
residual CO2 and organics are separated from the CO by GC.
2.1 Sampling. Same as in Method 10A, section 2.1.
2.2 Analysis.
2.2.1 Gas Chromatographic (GC) Analyzer. A semicontinuous GC/FID
analyzer capable of quantifying CO in the sample and containing at least
the following major components.
2.2.1.1 Separation Column. A column that separates CO from CO2 and
organic compounds that may be present. A 1/8-in. OD stainless-steel
column packed with 5.5 ft of 60/80 mesh Carbosieve S-II (available from
Supelco) has been used successfully for this purpose. The column listed
in Addendum 1 of Method 25 is also acceptable.
2.2.1.2 Reduction Catalyst. Same as in Method 25, section 2.3.2.
2.2.1.3 Sample Injection System. Same as in Method 25, section
2.3.4, equipped to accept a sample line from the Tedlar bag.
2.2.1.4 Flame Ionization Detector. Linearity meeting the
specifications in section 2.3.5.1 of Method 25 where the linearity check
is carried out using standard gases containing 20-, 200-, and 1,000-ppm
CO. The minimal instrument range shall span 10 to 1,000 ppm CO.
2.2.1.5 Data Recording System. Same as in Method 25, section 2.3.6.
3. Reagents
3.1 Sampling. Same as in Method 10A, section 3.1.
3.2 Analysis.
3.2.1 Carrier, Fuel, and Combustion Gases. Same as in Method 25,
sections 3.2.1, 3.2.2, and 3.2.3.
3.2.2 Linearity and Calibration Gases. Three standard gases with
nominal CO concentrations of 20-, 200-, and 1,000-ppm CO in nitrogen.
3.2.3 Reduction Catalyst Efficiency Check Calibration Gas. Standard
CH4 gas with a concentration of 1,000 ppm in air.
4.1 Sample Bag Leak-checks, Sampling, and CO2 Measurement. Same as
in Method 10A, sections 4.1, 4.2, and 4.3.
4.2 Preparation for Analysis. Before putting the GC analyzer into
routine operation, conduct the calibration procedures listed in section
5. Establish an appropriate carrier flow rate and detector temperature
for the specific instrument used.
4.3 Sample Analysis. Purge the sample loop with sample, and then
inject the sample. Analyze each sample in triplicate, and calculate the
average sample area (A). Determine the bag CO concentration according
to section 6.2.
5.1 Carrier Gas Blank Check. Analyze each new tank of carrier gas
with the GC analyzer according to section 4.3 to check for
contamination. The corresponding concentration must be less than 5 ppm
for the tank to be acceptable for use.
5.2 Reduction Catalyst Efficiency Check. Prior to initial use, the
reduction catalyst shall be tested for reduction efficiency. With the
heated reduction catalyst bypassed, make triplicate injections of the
1,000-ppm CH4 gas (section 3.2.3) to calibrate the analyzer. Repeat the
procedure using 1,000-ppm CO (section 3.2.2) with the catalyst in
operation. The reduction catalyst operation is acceptable if the CO
response is within 5 percent of the certified gas value.
5.3 Analyzer Linearity Check and Calibration. Perform this test
before the system is first placed into operation. With the reduction
catalyst in operation, conduct a linearity check of the analyzer using
the standards specified in section 3.2.2. Make triplicate injections of
each calibration gas, and then calculate the average response factor
(area/ppm) for each gas, as well as the overall mean of the response
factor values. The instrument linearity is acceptable if the average
response factor of each calibration gas is within 2.5 percent of the
overall mean value and if the relative standard deviation (calculated in
section 6.9 of Method 25) for each set of triplicate injections is less
than 2 percent. Record the overall mean of the response factor values
as the calibration response factor (R).
Carry out calculations retaining at least one extra decimal figure
beyond that of the acquired data. Round off results only after the
final calculation.
6.1 Nomenclature.
A=Average sample area.
Bw=Moisture content in the bag sample, fraction.
C=CO concentration in the stack gas, dry basis, ppm.
Cb=CO concentration in the bag sample, dry basis, ppm.
F=Volume fraction of CO2 in the stack, fraction.
Pbar=Barometric pressure, mm Hg.
Pw=Vapor pressure H2O in the bag (from Table 10-2, Method 10A), mm
Hg.
R=Mean calibration response factor, area/ppm.
6.2 CO Concentration in the Bag. Calculate Cb using Equations 10B-1
and 10B-2. If condensate is visible in the Tedlar bag, calculate Bw
using Table 10A-1 of Method 10A and the temperature and barometric
pressure in the analysis room. If condensate is not visible, calculate
Bw using the temperature and barometric pressure at the sampling site.
Eq. 10B-1
Eq. 10B-2
6.3 CO Concentration in the Stack.
C=Cb (1^F)
Eq. 10B-3
1. Butler, F.E, J.E. Knoll, and M.R. Midgett. Development and
Evaluation of Methods for Determining Carbon Monoxide Emissions.
Quality Assurance Division, Environmental Monitoring Systems Laboratory,
U.S. Environmental Protection Agency, Research Triangle Park, NC 27711.
June 1985. 33p.
2. Salo, A.E., S. Witz, and R.D. MacPhee. Determination of Solvent
Vapor Concentrations by Total Combustion Analysis: A Comparison of
Infrared with Flame Ionization Detectors. Paper No. 75-33.2.
(Presented at the 68th Annual Meeting of the Air Pollution Control
Association. Boston, MA. June 15, 1975.) 14 p.
3. Salo, A.E., W.L. Oaks, and R.D. MacPhee. Measuring the Organic
Carbon Content of Source Emissions for Air Pollution Control. Paper No.
74-190. (Presented at the 67th Annual Meeting of the Air Pollution
Control Association. Denver, CO. June 9, 1974.) 25 p.
40 CFR 60.748 Pt. 60, App. A, Meth. 11
1. Principle and Applicability
1.1 Principle. Hydrogen sulfide (H2S) is collected from a source in a
series of midget impingers and absorbed in pH 3.0 cadmium sulfate
(CdSO4) solution to form cadmium sulfide (CdS). The latter compound is
then measured iodometrically. An impinger containing hydrogen peroxide
is included to remove SO2 as an interfering species. This method is a
revision of the H2S method originally published in the Federal Register,
Volume 39, No. 47, dated Friday, March 8, 1974.
1.2 Applicability. This method is applicable for the determination of
the hydrogen sulfide content of fuel gas streams at petroleum
refineries.
2. Range and Sensitivity
The lower limit of detection is approximately 8 mg/m3 (6 ppm). The
maximum of the range is 740 mg/m3 (520 ppm).
3. Interferences
Any compound that reduces iodine or oxidizes iodide ion will
interfere in this procedure, provided it is collected in the cadmium
sulfate impingers. Sulfur dioxide in concentrations of up to 2,600
mg/m3 is eliminated by the hydrogen peroxide solution. Thiols
precipitate with hydrogen sulfide. In the absence of H2S, only
co-traces of thiols are collected. When methane- and ethane-thiols at a
total level of 300 mg/m3 are present in addition to H2S, the results
vary from 2 percent low at an H2S concentration of 400 mg/m3 to 14
percent high at an H2S concentration of 100 mg/m3. Carbon oxysulfide at
a concentration of 20 percent does not interfere. Certain
carbonyl-containing compounds react with iodine and produce recurring
end points. However, acetaldehyde and acetone at concentrations of 1
and 3 percent, respectively, do not interfere.
Entrained hydrogen peroxide produces a negative interference
equivalent to 100 percent of that of an equimolar quantity of hydrogen
sulfide. Avoid the ejection of hydrogen peroxide into the cadmium
sulfate impingers.
4. Precision and Accuracy
Collaborative testing has shown the within-laboratory coefficient of
variation to be 2.2 percent and the overall coefficient of variation to
be 5 percent. The method bias was shown to be ^4.8 percent when only
H2S was present. In the presence of the interferences cited in section
3, the bias was positive at low H2S concentration and negative at higher
concentrations. At 230 mg H2S/m3, the level of the compliance standard,
the bias was +2.7 percent. Thiols had no effect on the precision.
5. Apparatus
5.1 Sampling Apparatus.
5.1.1 Sampling Line. Six to 7 mm ( 1/4 in.) Teflon 1 tubing to
connect the sampling train to the sampling valve.
5.1.2 Impingers. Five midget impingers, each with 30 ml capacity.
The internal diameter of the impinger tip must be 1 mm 0.05 mm. The
impinger tip must be positioned 4 to 6 mm from the bottom of the
impinger.
5.1.3 Tubing. Glass or Teflon connecting tubing for the impingers.
5.1.4 Ice Bath Container. To maintain absorbing solution at a low
temperature.
5.1.5 Drying Tube. Tube packed with 6- to 16-mesh indicating-type
silica gel, or equivalent, to dry the gas sample and protect the meter
and pump. If the silica gel has been used previously, dry at 175 C
(350 F) for 2 hours. New silica gel may be used as received.
Alternatively, other types of desiccants (equivalent or better) may be
used, subject to approval of the Administrator.
Note: Do not use more than 30 g of silica gel. Silica gel absorbs
gases such as propane from the fuel gas stream, and use of excessive
amounts of silica gel could result in errors in the determination of
sample volume.
5.1.6 Sampling Valve. Needle valve or equivalent to adjust gas flow
rate. Stainless steel or other corrosion-resistant material.
5.1.7 Volume Meter. Dry gas meter, sufficiently accurate to measure
the sample volume within 2 percent, calibrated at the selected flow rate
( 1.0 liter/min) and conditions actually encountered during sampling.
The meter shall be equipped with a temperature gauge (dial thermometer
or equivalent) capable of measuring temperature to within 3 C (5.4 F).
The gas meter should have a petcock, or equivalent, on the outlet
connector which can be closed during the leak check. Gas volume for one
revolution of the meter must not be more than 10 liters.
5.1.8 Flow Meter. Rotameter or equivalent, to measure flow rates in
the range from 0.5 to 2 liters/min (1 to 4 cfh).
5.1.9 Graduated Cylinder, 25 ml size.
5.1.10 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg). In many
cases, the barometric reading may be obtained from a nearby National
Weather Service station, in which case, the station value (which is the
absolute barometric pressure) shall be requested and an adjustment for
elevation differences between the weather station and the sampling point
shall be applied at a rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 m (100
ft) elevation increase or vice-versa for elevation decrease.
5.1.11 U-tube Manometer. 0-30 cm water column. For leak check
procedure.
5.1.12 Rubber Squeeze Bulb. To pressurize train for leak check.
5.1.13 Tee, Pinchclamp, and Connecting Tubing. For leak check.
5.1.14 Pump. Diaphragm pump, or equivalent. Insert a small surge
tank between the pump and rate meter to eliminate the pulsation effect
of the diaphragm pump on the rotameter. The pump is used for the air
purge at the end of the sample run; the pump is not ordinarily used
during sampling, because fuel gas streams are usually sufficiently
pressurized to force sample gas through the train at the required flow
rate. The pump need not be leak-free unless it is used for sampling.
5.1.15 Needle Valve or Critical Orifice. To set air purge flow to 1
liter/min.
5.1.16 Tube Packed With Active Carbon. To filter air during purge.
5.1.17 Volumetric Flask. One 1,000 ml.
5.1.18 Volumetric Pipette. One 15 ml.
5.1.19 Pressure-Reduction Regulator. Depending on the sampling
stream pressure, a pressure-reduction regulator may be needed to reduce
the pressure of the gas stream entering the Teflon sample line to a safe
level.
5.1.20 Cold Trap. If condensed water or amine is present in the
sample stream, a corrosion-resistant cold trap shall be used immediately
after the sample tap. The trap shall not be operated below 0 C (32 F)
to avoid condensation of C3 or C4 hydrocarbons.
5.2 Sample Recovery.
5.2.1 Sample Container. Iodine flask, glass-stoppered: 500 ml size.
5.2.2 Pipette. 50 ml volumetric type.
5.2.3 Graduated Cylinders. One each 25 and 250 ml.
5.2.4 Flasks. 125 ml, Erlenmeyer.
5.2.5 Wash Bottle.
5.2.6 Volumetric Flasks. Three 1,000 ml.
5.3 Analysis.
5.3.1 Flask. 500 ml glass-stoppered iodine flask.
5.3.2 Burette. 50 ml.
5.3.3 Flask. 125 ml, Erlenmeyer.
5.3.4 Pipettes, Volumetric. One 25 ml; two each 50 and 100 ml.
5.3.5 Volumetric Flasks. One 1,000 ml; two 500 ml.
5.3.6 Graduated Cylinders. One each 10 and 100 ml.
6. Reagents
Unless otherwise indicated, it is intended that all reagents conform
to the specifications established by the Committee on Analytical
Reagents of the American Chemical Society, where such specifications are
available. Otherwise, use best available grade.
6.1 Sampling.
6.1.1 Cadmium Sulfate Absorbing Solution. Dissolve 41 g of 3CdSO4
8H2O and 15 ml of 0.1 M sulfuric acid in a 1-liter volumetric flask that
contains approximately 3/4 liter of deionized distilled water. Dilute
to volume with deionized water. Mix thoroughly. pH should be 3 0.1.
Add 10 drops of Dow-Corning Antifoam B. Shake well before use. If
Antifoam B is not used, the alternative acidified iodine extraction
procedure (Section 7.2.2) must be used.
6.1.2 Hydrogen Peroxide, 3 Percent. Dilute 30 percent hydrogen
peroxide to 3 percent as needed. Prepare fresh daily.
6.1.3 Water. Deionized, distilled to conform to ASTM specifications
D1193-72, Type 3. At the option of the analyst, the KMnO4 test for
oxidizable organic matter may be omitted when high concentrations of
organic matter are not expected to be present.
6.2 Sample Recovery.
6.2.1 Hydrochloric Acid Solution (HCl), 3M. Add 240 ml of
concentrated HCl (specific gravity 1.19) to 500 ml of deionized,
distilled water in a 1-liter volumetric flask. Dilute to 1 liter with
deionized water. Mix thoroughly.
6.2.2 Iodine Solution 0.1 N. Dissolve 24 g of potassium iodide (KI)
in 30 ml of deionized, distilled water. Add 12.7 g of resublimed iodine
(I2) to the potassium iodide solution. Shake the mixture until the
iodine is completely dissolved. If possible, let the solution stand
overnight in the dark. Slowly dilute the solution to 1 liter with
deionized, distilled water, with swirling. Filter the solution if it is
cloudy. Store solution in a brown-glass reagent bottle.
6.2.3 Standard Iodine Solution, 0.01 N. Pipette 100.0 ml of the 0.1 N
iodine solution into a 1-liter volumetric flask and dilute to volume
with deionized, distilled water. Standardize daily as in Section 8.1.1.
This solution must be protected from light. Reagent bottles and flasks
must be kept tightly stoppered.
6.3 Analysis.
6.3.1 Sodium Thiosulfate Solution, Standard 0.1 N. Dissolve 24.8 g of
sodium thiosulfate pentahydrate (Na2S2O3 5H2O) or 15.8 g of anhydrous
sodium thiosulfate (Na2S2O3) in 1 liter of deionized, distilled water
and add 0.01 g of anhydrous sodium carbonate (Na2CO3) and 0.4 ml of
chloroform (CHCl3) to stabilize. Mix thoroughly by shaking or by
aerating with nitrogen for approximately 15 minutes and store in a
glass-stoppered, reagent bottle. Standardize as in Section 8.1.2.
6.3.2 Sodium Thiosulfate Solution, Standard 0.01 N. Pipette 50.0 ml
of the standard 0.1 N thiosulfate solution into a volumetric flask and
dilute to 500 ml with distilled water.
Note: A 0.01 N phenylarsine oxide solution may be prepared instead
of 0.01 N thiosulfate (see Section 6.3.3).
6.3.3 Phenylarsine Oxide Solution, Standard 0.01 N. Dissolve 1.80 g
of phenylarsine oxide (C6H5AsO) in 150 ml of 0.3 N sodium hydroxide.
After settling, decant 140 ml of this solution into 800 ml of distilled
water. Bring the solution to pH 6-7 with 6N hydrochloric acid and
dilute to 1 liter. Standardize as in Section 8.1.3.
6.3.4 Starch Indicator Solution. Suspend 10 g of soluble starch in
100 ml of deionized, distilled water and add 15 g of potassium hydroxide
(KOH) pellets. Stir until dissolved, dilute with 900 ml of deionized
distilled water and let stand for 1 hour. Neutralize the alkali with
concentrated hydrochloric acid, using an indicator paper similar to
Alkacid test ribbon, then add 2 ml of glacial acetic acid as a
preservative.
Note: Test starch indicator solution for decomposition by titrating,
with 0.01 N iodine solution, 4 ml of starch solution in 200 ml of
distilled water that contains 1 g potassium iodide. If more than 4
drops of the 0.01 N iodine solution are required to obtain the blue
color, a fresh solution must be prepared.
7. Procedure
7.1 Sampling.
7.1.1 Assemble the sampling train as shown in Figure 11-1, connecting
the five midget impingers in series. Place 15 ml of 3 percent hydrogen
peroxide solution in the first impinger. Leave the second impinger
empty. Place 15 ml of the cadmium sulfate absorbing solution in the
third, fourth, and fifth impingers. Place the impinger assembly in an
ice bath container and place crushed ice around the impingers. Add more
ice during the run, if needed.
7.1.2 Connect the rubber bulb and manometer to first impinger, as
shown in Figure 11-1. Close the petcock on the dry gas meter outlet.
Pressurize the train to 25-cm water pressure with the bulb and close off
tubing connected to rubber bulb. The train must hold a 25-cm water
pressure with not more than a 1-cm drop in pressure in a 1-minute
interval. Stopcock grease is acceptable for sealing ground glass
joints.
Note: This leak check procedure is optional at the beginning of the
sample run, but is mandatory at the conclusion. Note also that if the
pump is used for sampling, it is recommended (but not required) that the
pump be leak-checked separately, using a method consistent with the
leak-check procedure for diaphragm pumps outlined in Section 4.1.2 of
Method 6, 40 CFR part 60, appendix A.
7.1.3 Purge the connecting line between the sampling valve and first
impinger, by disconnecting the line from the first impinger, opening the
sampling valve, and allowing process gas to flow through the line for a
minute or two. Then, close the sampling valve and reconnect the line to
the impinger train. Open the petcock on the dry gas meter outlet.
Record the initial dry gas meter reading.
Insert illus. 0153
7.1.4 Open the sampling valve and then adjust the valve to obtain a
rate of approximately 1 liter/min. Maintain a constant ( 10 percent)
flow rate during the test. Record the meter temperature.
7.1.5 Sample for at least 10 min. At the end of the sampling time,
close the sampling valve and record the final volume and temperature
readings. Conduct a leak check as described in Section 7.1.2 above.
7.1.6 Disconnect the impinger train from the sampling line. Connect
the charcoal tube and the pump, as shown in Figure 11-1. Purge the
train (at a rate of 1 liter/min) with clean ambient air for 15 minutes
to ensure that all H2S is removed from the hydrogen peroxide. For
sample recovery, cap the open ends and remove the impinger train to a
clean area that is away from sources of heat. The area should be well
lighted, but not exposed to direct sunlight.
7.2 Sample Recovery.
7.2.1 Discard the contents of the hydrogen peroxide impinger.
Carefully rinse the contents of the third, fourth, and fifth impingers
into a 500 ml iodine flask.
Note: The impingers normally have only a thin film of cadmium
sulfide remaining after a water rinse. If Antifoam B was not used or if
significant quantities of yellow cadmium sulfide remain in the
impingers, the alternative recovery procedure described below must be
used.
7.2.2 Pipette exactly 50 ml of 0.01 N iodine solution into a 125 ml
Erlenmeyer flask. Add 10 ml of 3 M HCl to the solution. Quantitatively
rinse the acidified iodine into the iodine flask. Stopper the flask
immediately and shake briefly.
7.2.2 (Alternative). Extract the remaining cadmium sulfide from the
third, fourth, and fifth impingers using the acidified iodine solution.
Immediately after pouring the acidified iodine into an impinger, stopper
it and shake for a few moments, then transfer the liquid to the iodine
flask. Do not transfer any rinse portion from one impinger to another;
transfer it directly to the iodine flask. Once the acidified iodine
solution has been poured into any glassware containing cadmium sulfide,
the container must be tightly stoppered at all times except when adding
more solution, and this must be done as quickly and carefully as
possible. After adding any acidified iodine solution to the iodine
flask, allow a few minutes for absorption of the H2S before adding any
further rinses. Repeat the iodine extraction until all cadmium sulfide
is removed from the impingers. Extract that part of the connecting
glassware that contains visible cadmium sulfide.
Quantitatively rinse all of the iodine from the impingers,
connectors, and the beaker into the iodine flask using deionized,
distilled water. Stopper the flask and shake briefly.
7.2.3 Allow the iodine flask to stand about 30 minutes in the dark
for absorption of the H2S into the iodine, then complete the titration
analysis as in Section 7.3.
Note: Caution! Iodine evaporates from acidified iodine solutions.
Samples to which acidified iodine have been added may not be stored, but
must be analyzed in the time schedule stated in Section 7.2.3.
7.2.4 Prepare a blank by adding 45 ml of cadmium sulfate absorbing
solution to an iodine flask. Pipette exactly 50 ml of 0.01 N iodine
solution into a 125-ml Erlenmeyer flask. Add 10 ml of 3 M HCl. Follow
the same impinger extracting and quantitative rinsing procedure carried
out in sample analysis. Stopper the flask, shake briefly, let stand 30
minutes in the dark, and titrate with the samples.
Note: The blank must be handled by exactly the same procedure as
that used for the samples.
7.3 Analysis.
Note: Titration analyses should be conducted at the sample-cleanup
area in order to prevent loss of iodine from the sample. Titration
should never be made in direct sunlight.
7.3.1 Using 0.01 N sodium thiosulfate solution (or 0.01 N
phenylarsine oxide, if applicable), rapidly titrate each sample in an
iodine flask using gentle mixing, until solution is light yellow. Add 4
ml of starch indicator solution and continue titrating slowly until the
blue color just disappears. Record VTT, the volume of sodium
thiosulfate solution used, or VAT, the volume of phenylarsine oxide
solution used (ml).
7.3.2 Titrate the blanks in the same manner as the samples. Run
blanks each day until replicate values agree within 0.05 ml. Average the
replicate titration values which agree within 0.05 ml.
8. Calibration and Standards
8.1 Standardizations.
8.1.1 Standardize the 0.01 N iodine solution daily as follows:
Pipette 25 ml of the iodine solution into a 125 ml Erlenmeyer flask.
Add 2 ml of 3 M HCl. Titrate rapidly with standard 0.01 N thiosulfate
solution or with 0.01 N phenylarsine oxide until the solution is light
yellow, using gentle mixing. Add four drops of starch indicator
solution and continue titrating slowly until the blue color just
disappears. Record VT, the volume of thiosulfate solution used, or VAS,
the volume of phenylarsine oxide solution used (ml). Repeat until
replicate values agree within 0.05 ml. Average the replicate titration
values which agree within 0.05 ml and calculate the exact normality of
the iodine solution using Equation 11-3. Repeat the standardization
daily.
8.1.2 Standardize the 0.1 N thiosulfate solution as follows:
Oven-dry potassium dichromate (K2Cr2O7) at 180 to 200 C (360 to 390
F). Weigh to the nearest milligram, 2 g of potassium dichromate.
Transfer the dichromate to a 500 ml volumetric flask, dissolve in
deionized, distilled water and dilute to exactly 500 ml. In a 500 ml
iodine flask, dissolve approximately 3 g of potassium iodide (KI) in 45
ml of deionized, distilled water, then add 10 ml of 3 M hydrochloric
acid solution. Pipette 50 ml of the dichromate solution into this
mixture. Gently swirl the solution once and allow it to stand in the
dark for 5 minutes. Dilute the solution with 100 to 200 ml of deionized
distilled water, washing down the sides of the flask with part of the
water. Titrate with 0.1 N thiosulfate until the solution is light
yellow. Add 4 ml of starch indicator and continue titrating slowly to a
green end point. Record VS, the volume of thiosulfate solution used
(ml). Repeat until replicate analyses agree within 0.05 ml. Calculate
the normality using Equation 11-1. Repeat the standardization each
week, or after each test series, whichever time is shorter.
8.1.3 Standardize the 0.01 N Phenylarsine oxide (if applicable) as
follows: oven dry potassium dichromate (K2Cr2O7) at 180 to 200 C (360
to 390 F). Weigh to the nearest milligram, 2 g of the K2Cr2O7;
transfer the dichromate to a 500 ml volumetric flask, dissolve in
deionized, distilled water, and dilute to exactly 500 ml. In a 500 ml
iodine flask, dissolve approximately 0.3 g of potassium iodide (KI) in
45 ml of deionized, distilled water; add 10 ml of 3M hydrochloric acid.
Pipette 5 ml of the K2Cr2O7 solution into the iodine flask. Gently
swirl the contents of the flask once and allow to stand in the dark for
5 minutes. Dilute the solution with 100 to 200 ml of deionized,
distilled water, washing down the sides of the flask with part of the
water. Titrate with 0.01 N phenylarsine oxide until the solution is
light yellow. Add 4 ml of starch indicator and continue titrating
slowly to a green end point. Record VA, the volume of phenylarsine
oxide used (ml). Repeat until replicate analyses agree within 0.05 ml.
Calculate the normality using Equation 11-2. Repeat the standardization
each week or after each test series, whichever time is shorter.
8.2 Sampling Train Calibration. Calibrate the sampling train
components as follows:
8.2.1 Dry Gas Meter.
8.2.1.1 Initial Calibration. The dry gas meter shall be calibrated
before its initial use in the field. Proceed as follows: First,
assemble the following components in series: Drying tube, needle valve,
pump, rotameter, and dry gas meter. Then, leak-check the system as
follows: Place a vacuum gauge (at least 760 mm Hg) at the inlet to the
drying tube and pull a vacuum of 250 mm (10 in.) Hg; plug or pinch off
the outlet of the flow meter, and then turn off the pump. The vacuum
shall remain stable for at least 30 seconds. Carefully release the
vacuum gauge before releasing the flow meter end.
Next, calibrate the dry gas meter (at the sampling flow rate
specified by the method) as follows: Connect an appropriately sized wet
test meter (e.g., 1 liter per revolution) to the inlet of the drying
tube. Make three independent calibration runs, using at least five
revolutions of the dry gas meter per run. Calculate the calibration
factor, Y (wet test meter calibration volume divided by the dry gas
meter volume, both volumes adjusted to the same reference temperature
and pressure), for each run, and average the results. If any Y value
deviates by more than 2 percent from the average, the dry gas meter is
unacceptable for use. Otherwise, use the average as the calibration
factor for subsequent test runs.
8.2.1.2 Post-test Calibration Check. After each field test series,
conduct a calibration check as in Section 8.2.1.1. above, except for the
following variations: (a) The leak check is not to be conducted, (b)
three or more revolutions of the dry gas meter may be used, and (c) only
two independent runs need be made. If the calibration factor does not
deviate by more than 5 percent from the initial calibration factor
(determined in Section 8.2.1.1.), then the dry gas meter volumes
obtained during the test series are acceptable. If the calibration
factor deviates by more than 5 percent, recalibrate the dry gas meter as
in Section 8.2.1.1, and for the calculations, use the calibration factor
(initial or recalibration) that yields the lower gas volume for each
test run.
8.2.2 Thermometers. Calibrate against mercury-in-glass thermometers.
8.2.3 Rotameter. The rotameter need not be calibrated, but should be
cleaned and maintained according to the manufacturer's instruction.
8.2.4 Barometer. Calibrate against a mercury barometer.
9. Calculations
Carry out calculations retaining at least one extra decimal figure
beyond that of the acquired data. Round off results only after the
final calculation.
9.1 Normality of the Standard ( 0.1 N) Thiosulfate Solution.
Eq. 11-1
where:
W=Weight of K2Cr2O7 used, g.
VS=Volume of Na2S2O3 solution used, ml.
NS=Normality of standard thiosulfate solution, g-eq/liter.
2.039=Conversion factor
9.2 Normality of Standard Phenylarsine Oxide Solution (if
applicable).
Eq. 11-2
where:
W=Weight of K2Cr2O7 used, g.
VA=Volume of C6H5AsO used, ml.
NA=Normality of standard phenylarsine oxide solution, g-eq/liter.
0.2039=Conversion factor
9.3 Normality of Standard Iodine Solution.
11-3
where:
NI=Normality of standard iodine solution, g-eq/liter.
VI=Volume of standard iodine solution used, ml.
NT=Normality of standard ( 0.01 N) thiosulfate solution; assumed to
be 0.1 NS, g-eq/liter.
VT=Volume of thiosulfate solution used, ml.
Note: If phenylarsine oxide is used instead of thiosulfate, replace
NT and VT in Equation 11-3 with NA and VAS, respectively (see Sections
8.1.1 and 8.1.3).
9.4 Dry Gas Volume. Correct the sample volume measured by the dry
gas meter to standard conditions (20 C and 760 mm Hg.)
Eq. 11-4
Where:
Vm(std)=Volume at standard conditions of gas sample through the dry
gas meter, standard liters.
Vm=Volume of gas sample through the dry gas meter (meter conditions),
liters.
Tstd=Absolute temperature at standard conditions, 293 K.
Tm=Average dry gas meter temperature, K.
Pbar=Barometric pressure at the sampling site, mm Hg.
Pstd=Absolute pressure at standard conditions, 760 mm Hg.
Y=Dry gas meter calibration factor.
9.5 Concentration of H2S. Calculate the concentration of H2S in the
gas stream at standard conditions using the following equation:
CH2S=K((VITNI^VTTNT) sample --
(VITNI^VTTNT))/Vm(std)
Eq. 11-5
Where (metric units):
CH2S=Concentration of H2S at standard conditions, mg/dscm.
K=Conversion factor 17.04 103
VIT=Volume of standard iodine solution=50.0 ml.
NI=Normality of standard iodine solution, g-eq/liter.
VTT=Volume of standard ( 0.01 N) sodium thiosulfate solution, ml.
NT=Normality of standard sodium thiosulfate solution, g-eq/liter.
Vm(std)=Dry gas volume at standard conditions, liters.
Note: If phenylarsine oxide is used instead of thiosulfate, replace
NT and VTT in Equation 11-5 with NA and VAT, respectively (see Sections
7.3.1 and 8.1.3).
10. Stability
The absorbing solution is stable for at least 1 month. Sample
recovery and analysis should begin within 1 hour of sampling to minimize
oxidation of the acidified cadmium sulfide. Once iodine has been added
to the sample, the remainder of the analysis procedure must be completed
according to Sections 7.2.2 through 7.3.2.
11. Bibliography
1. Determination of Hydrogen Sulfide, Ammoniacal Cadmium Chloride
Method. API Method 772-54. In: Manual on Disposal of Refinery Wastes,
Vol. V: Sampling and Analysis of Waste Gases and Particulate Matter,
American Petroleum Institute, Washington, DC. 1954.
2. Tentative Method of Determination of Hydrogen Sulfide and
Mercaptan Sulfur in Natural Gas, Natural Gas Processors Association,
Tulsa, OK. NGPA Publication No. 2265-65. 1965.
3. Knoll, J. E., and M. R. Midgett. Determination of Hydrogen
Sulfide in Refinery Fuel Gases, Environmental Monitoring Series, Office
of Research and Development, USEPA, Research Triangle Park, NC 27711,
EPA 600/4-77-007.
4. Scheil, G. W., and M. C. Sharp. Standardization of Method 11 at
a Petroleum Refinery, Midwest Research Institute Draft Report for USEPA,
Office of Research and Development, Research Triangle Park, NC 27711,
EPA Contract No. 68-02-1098. August 1976, EPA 600/4-77-088a (Volume 1)
and EPA 600/4-77-088b (Volume 2).
/1/ Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
40 CFR 60.748 Pt. 60, App. A, Meth. 12
1. Principle and Applicability
1.1 Applicability. This method applies to the determination of
inorganic lead (Pb) emissions from specified stationary sources only.
1.2 Principle. Particulate and gaseous Pb emissions are withdrawn
isokinetically from the source and collected on a filter and in dilute
nitric acid. The collected samples are digested in acid solution and
analyzed by atomic absorption spectrometry using an air acetylene flame.
2. Range, Sensitivity, Precision, and Interferences
2.1 Range. For a minimum analytical accuracy of 10 percent, the
lower limit of the range is 100 g. The upper limit can be considerably
extended by dilution.
2.2 Analytical Sensitivity. Typical sensitivities for a 1-percent
change in absorption (0.0044 absorbance units) are 0.2 and 0.5 g Pb/ml
for the 217.0 and 283.3 nm lines, respectively.
2.3 Precision. The within-laboratory precision, as measured by the
coefficient of variation ranges from 0.2 to 9.5 percent relative to a
run-mean concentration. These values were based on tests conducted at a
gray iron foundry, a lead storage battery manufacturing plant, a
secondary lead smelter, and a lead recovery furnace of an alkyl lead
manufacturing plant. The concentrations encountered during these tests
ranged from 0.61 to 123.3 mg Pb/m3.
2.4 Interferences. Sample matrix effects may interfere with the
analysis for Pb by flame atomic absorption. If this interference is
suspected, the analyst may confirm the presence of these matrix effects
and frequently eliminate the interference by using the Method of
Standard Additions.
High concentrations of copper may interfere with the analysis of Pb
at 217.0 nm. This interference can be avoided by analyzing the samples
at 283.3 nm.
3. Apparatus
3.1 Sampling Train. A schematic of the sampling train is shown in
Figure 12-1; it is similar to the Method 5 train. The sampling train
consists of the following components:
3.1.1 Probe Nozzle, Probe Liner, Pitot Tube, Differential Pressure
Gauge, Filter Holder, Filter Heating System, Metering System, Barometer,
and Gas Density Determination Equipment. Same as Method 5, Sections
2.1.1 to 2.1.6 and 2.1.8 to 2.1.10, respectively.
3.1.2 Impingers. Four impingers connected in series with leak-free
ground glass fittings or any similar leak-free noncontaminating
fittings. For the first, third, and fourth impingers, use the
Greenburg-Smith design, modified by replacing the tip with a 1.3 cm (
1/2 in.) ID glass tube extending to about 1.3 cm ( 1/2 in.) from the
bottom of the flask. For the second impinger, use the Greenburg-Smith
design with the standard tip. Place a thermometer, capable of measuring
temperature to within 1 C (2 F) at the outlet of the fourth impinger for
monitoring purposes.
Insert illus. 0715
3.2 Sample Recovery. The following items are needed:
3.2.1 Probe-Liner and Probe-Nozzle Brushes, Petri Dishes, Plastic
Storage Containers, and Funnel and Rubber Policeman. Same as Method 5,
Sections 2.2.1, 2.2.4, 2.2.6, and 2.2.7, respectively.
3.2.2 Wash Bottles. Glass (2).
3.2.3 Sample Storage Containers. Chemically resistant, borosilicate
glass bottles, for 0.1 N nitric acid (HNO3) impinger and probe solutions
and washes, 1000-ml. Use screw-cap liners that are either rubber-backed
Teflon* or leak-free and resistant to chemical attack by 0.1 N HNO3.
(Narrow mouth glass bottles have been found to be less prone to
leakage.)
3.2.4 Graduated Cylinder and/or Balance. To measure condensed water
to within 2 ml or 1 g. Use a graduated cylinder that has a minimum
capacity of 500 ml, and subdivisions no greater than 5 ml. (Most
laboratory balances are capable of weighing to the nearest 0.5 g or
less.)
3.2.5 Funnel. Glass, to aid in sample recovery.
3.3 Analysis. The following equipment is needed:
3.3.1 Atomic Absorption Spectrophotometer. With lead hollow cathode
lamp and burner for air/acetylene flame.
3.3.2 Hot Plate.
3.3.3 Erlenmeyer Flasks. 125-ml, 24/40 $8.
3.3.4 Membrane Filters. Millipore SCWPO 4700 or equivalent.
3.3.5 Filtration Apparatus. Millipore vacuum filtration unit, or
equivalent, for use with the above membrane filter.
3.3.6 Volumetric Flasks. 100-ml, 250-ml, and 1000-ml.
4. Reagents
4.1 Sampling. The reagents used in sampling are as follows:
4.1.1 Filter. Gelman Spectro Grade, Reeve Angel 934 AH, MSA 1106 BH,
all with lot assay for Pb, or other high-purity glass fiber filters,
without organic binder, exhibiting at least 99.95 percent efficiency
(<0.05 percent penetration) on 0.3 micron dioctyl phthalate smoke
particles. Conduct the filter efficiency test using ASTM Standard
Method D2986-71 (incorporated by reference -- see 60.17) or use test
data from the supplier's quality control program.
4.1.2 Silica Gel, Crushed Ice, and Stopcock Grease. Same as Method
5, Sections 3.1.2, 3.1.4, and 3.1.5, respectively.
4.1.3 Water. Deionized distilled, to conform to ASTM Specification
D1192-77 (incorporated by reference -- see 60.17), Type 3. If high
concentrations of organic matter are not expected to be present, the
analyst may delete the potassium permanganate test for oxidizable
organic matter.
4.1.4 Nitric Acid, 0.1 N. Dilute 6.5 ml of concentrated HNO3 to 1
liter with deionized distilled water. (It may be desirable to run
blanks before field use to eliminate a high blank on test samples.)
4.2 Pretest Preparation. 6 N HNO3 is needed. Dilute 390 ml of
concentrated HNO3 to 1 liter with deionized distilled water.
4.3 Sample Recovery. 0.1 N HNO3 (same as 4.1.4 above) is needed for
sample recovery.
4.4 Analysis. The following reagents are needed for analysis (use ACS
reagent grade chemicals or equivalent, unless otherwise specified):
4.4.1 Water. Same as 4.1.3 above.
4.4.2 Nitric Acid. Concentrated.
4.4.3 Nitric Acid, 50 percent (V/V). Dilute 500 ml of concentrated
HNO3 to 1 liter with deionized distilled water.
4.4.4 Stock Lead Standard Solution, 1000 g Pb/ml. Dissolve 0.1598 g
of lead nitrate (Pb(NO3)2) in about 60 ml of deionized distilled water,
add 2 ml concentrated HNO3, and dilute to 100 ml with deionized
distilled water.
4.4.5 Working Lead Standards. Pipet 0.0, 1.0, 2.0, 3.0, 4.0, and 5.0
ml of the stock lead standard solution (4.4.4) into 250-ml volumetric
flasks. Add 5 ml of concentrated HNO3 to each flask and dilute to
volume with deionized distilled water. These working standards contain
0.0, 4.0, 8.0, 12.0, 16.0, and 20.0 g Pb/ml, respectively. Prepare, as
needed, additional standards at other concentrations in a similar
manner.
4.4.6 Air. Suitable quality for atomic absorption analysis.
4.4.7 Acetylene. Suitable quality for atomic absorption analysis.
4.4.8 Hydrogen Peroxide, 3 percent (V/V). Dilute 10 ml of 30 percent
H2O2 to 100 ml with deionized distilled water.
5. Procedure
5.1 Sampling. The complexity of this method is such that, in order to
obtain reliable results, testers should be trained and experienced with
the test procedures.
5.1.1 Pretest Preparation. Follow the same general procedure given
in Method 5, Section 4.1.1, except the filter need not be weighed.
5.1.2 Preliminary Determinations. Follow the same general procedure
given in Method 5, Section 4.1.2.
5.1.3 Preparation of Collection Train. Follow the same general
procedure given in Method 5, Section 4.1.3, except place 100 ml of 0.1 N
HNO3 in each of the first two impingers, leave the third impinger empty,
and transfer approximately 200 to 300 g of preweighed silica gel from
its container to the fourth impinger. Set up the train as shown in
Figure 12-1.
5.1.4 Leak-Check Procedures. Follow the general leak-check
procedures given in Method 5, Sections 4.1.4.1. (Pretest Leak-Check),
4.1.4.2 (Leak-Checks During the Sample Run), and 4.1.4.3 (Post-Test
Leak-Check).
5.1.5 Sampling Train Operation. Follow the same general procedure
given in Method 5, Section 4.1.5. For each run, record the data required
on a data sheet such as the one shown in EPA Method 5, Figure 5-2.
5.1.6 Calculation of Percent Isokinetic. Same as Method 5, Section
4.1.6.
5.2 Sample Recovery. Begin proper cleanup procedure as soon as the
probe is removed from the stack at the end of the sampling period.
Allow the probe to cool. When it can be safely handled, wipe off all
external particulate matter near the tip of the probe nozzle and place a
cap over it. Do not cap off the probe tip tightly while the sampling
train is cooling down as this would create a vacuum in the filter
holder, thus drawing liquid from the impingers into the filter.
Before moving the sampling train to the cleanup site, remove the
probe from the sampling train, wipe off the silicone grease, and cap the
open outlet of the probe. Be careful not to lose any condensate that
might be present. Wipe off the silicone grease from the glassware inlet
where the probe was fastened and cap the inlet. Remove the umbilical
cord from the last impinger and cap the impinger. The tester may use
ground-glass stoppers, plastic caps, or serum caps to close these
openings.
Transfer the probe and filter-impinger assembly to a cleanup area,
which is clean and protected from the wind so that the chances of
contaminating or losing the sample are minimized.
Inspect the train prior to and during disassembly and note any
abnormal conditions. Treat the samples as follows:
5.2.1 Container No. 1 (Filter), Carefully remove the filter from the
filter holder and place it in its identified petri dish container. If
it is necessary to fold the filter, do so such that the sample-exposed
side is inside the fold. Carefully transfer to the petri dish any
visible sample matter and/or filter fibers that adhere to the filter
holder gasket by using a dry Nylon bristle brush and/or a sharp-edged
blade. Seal the container.
5.2.2 Container No. 2 (Probe). Taking care that dust on the outside
of the probe or other exterior surfaces does not get into the sample,
quantitatively recover sample matter or any condensate from the probe
nozzle, probe fitting, probe liner, and front half of the filter holder
by washing these components with 0.1 N HNO3 and placing the wash into a
glass sample storage container. Measure and record (to the nearest
2-ml) the total amount of 0.1 N HNO3 used for each rinse. Perform the
0.1 N HNO3 rinses as follows:
Carefully remove the probe nozzle and rinse the inside surfaces with
0.1 N HNO3 from a wash bottle while brushing with a stainless steel,
Nylon-bristle brush. Brush until the 0.1 N HNO3 rinse shows no visible
particles, then make a final rinse of the inside surface.
Brush and rinse with 0.1 N HNO3 the inside parts of the Swagelok
fitting in a similar way until no visible particles remain.
Rinse the probe liner with 0.1 N HNO3. While rotating the probe so
that all inside surfaces will be rinsed with 0.1 N HNO3, tilt the probe
and squirt 0.1 N HNO3 into its upper end. Let the 0.1 N HNO3 drain from
the lower end into the sample container. The tester may use a glass
funnel to aid in transferring liquid washes to the container. Follow
the rinse with a probe brush. Hold the probe in an inclined position,
squirt 0.1 N HNO3 into the upper end of the probe as the probe brush is
being pushed with a twisting action through the probe; hold the sample
container underneath the lower end of the probe and catch any 0.1 N HNO3
and sample matter that is brushed from the probe. Run the brush through
the probe three times or more until no visible sample matter is carried
out with the 0.1 N HNO3 and none remains on the probe liner on visual
inspection. With stainless steel or other metal probes, run the brush
through in the above prescribed manner at least six times, since metal
probes have small crevices in which sample matter can be entrapped.
Rinse the brush with 0.1 N HNO3 and quantitatively collect these
washings in the sample container. After the brushing make a final rinse
of the probe as described above.
It is recommended that two people clean the probe to minimize loss of
sample. Between sampling runs, keep brushes clean and protected from
contamination.
After insuring that all joints are wiped clean of silicone grease,
brush and rinse with 0.1 N HNO3 the inside of the front half of the
filter holder. Brush and rinse each surface three times or more, if
needed, to remove visible sample matter. Make a final rinse of the
brush and filter holder. After all 0.1 N HNO3 washings and sample
matter are collected in the sample container, tighten the lid on the
sample container so that the fluid will not leak out when it is shipped
to the laboratory. Mark the height of the fluid level to determine
whether leakage occurs during transport. Label the container to clearly
identify its contents.
5.2.3 Container No. 3 (Silica Gel). Check the color of the
indicating silica gel to determine if it has been completely spent and
make a notation of its condition. Transfer the silica gel from the
fourth impinger to the original container and seal. The tester may use
a funnel to pour the silica gel and a rubber policeman to remove the
silica gel from the impinger. It is not necessary to remove the small
amount of particles that may adhere to the walls and are difficult to
remove. Since the gain in weight is to be used for moisture
calculations, do not use any water or other liquids to transfer the
silica gel. If a balance is available in the field, the tester may
follow procedure for Container No. 3 under Section 5.4 (Analysis).
5.2.4 Container No. 4 (Impingers). Due to the large quantity of
liquid involved, the tester may place the impinger solutions in several
containers. Clean each of the first three impingers and connecting
glassware in the following manner:
1. Wipe the impinger ball joints free of silicone grease and cap the
joints.
2. Rotate and agitate each impinger, so that the impinger contents
might serve as a rinse solution.
3. Transfer the contents of the impingers to a 500-ml graduated
cylinder. Remove the outlet ball joint cap and drain the contents
through this opening. Do not separate the impinger parts (inner and
outer tubes) while transferring their contents to the cylinder. Measure
the liquid volume to within 2 ml. Alternatively, determine the weight
of the liquid to within 0.5 g. Record in the log the volume or weight
of the liquid present, along with a notation of any color or film
observed in the impinger catch. The liquid volume or weight is needed,
along with the silica gel data, to calculate the stack gas moisture
content (see Method 5, Figure 5-3).
4. Transfer the contents to Container No. 4.
5. Note: In steps 5 and 6 below, measure and record the total amount
of 0.1 N HNO3 used for rinsing. Pour approximately 30 ml of 0.1 N HNO3
into each of the first three impingers and agitate the impingers. Drain
the 0.1 N HNO3 through the outlet arm of each impinger into Container
No. 4. Repeat this operation a second time; inspect the impingers for
any abnormal conditions.
6. Wipe the ball joints of the glassware connecting the impingers
free of silicone grease and rinse each piece of glassware twice with 0.1
N HNO3; transfer this rinse into Container No. 4. (Do not rinse or
brush the glass-fritted filter support.) Mark the height of the fluid
level to determine whether leakage occurs during transport. Label the
container to clearly identify its contents.
5.2.5 Blanks. Save 200 ml of the 0.1 N HNO3 used for sampling and
cleanup as a blank. Take the solution directly from the bottle being
used and place into a glass sample container labeled ''0.1 N HNO3
blank.''
5.3 Sample Preparation.
5.3.1 Container No. 1 (Filter). Cut the filter into strips and
transfer the strips and all loose particulate matter into a 125-ml
Erlenmeyer flask. Rinse the petri dish with 10 ml of 50 percent HNO3 to
insure a quantitative transfer and add to the flask. (Note: If the
total volume required in Section 5.3.3 is expected to exceed 80 ml, use
a 250-ml Erlenmeyer flask in place of the 125-ml flask.)
5.3.2 Containers No. 2 and No. 4 (Probe and Impingers). (Check the
liquid level in Containers No. 2 and/or No. 4 and confirm as to whether
or not leakage occurred during transport; note observation on the
analysis sheet. If a noticeable amount of leakage had occurred, either
void the sample or take steps, subject to the approval of the
Administrator, to adjust the final results.) Combine the contents of
Containers No. 2 and No. 4 and take to dryness on a hot plate.
5.3.3 Sample Extraction for Lead. Based on the approximate stack gas
particulate concentration and the total volume of stack gas sampled,
estimate the total weight of particulate sample collected. Then
transfer the residue from Containers No. 2 and No. 4 to the 125-ml
Erlenmeyer flask that contains the filter using rubber policeman and 10
ml of 50 percent HNO3 for every 100 mg of sample collected in the train
or a minimum of 30 ml of 50 percent HNO3 whichever is larger.
Place the Erlenmeyer flask on a hot plate and heat with periodic
stirring for 30 min at a temperature just below boiling. If the sample
volume falls below 15 ml, add more 50 percent HNO3. Add 10 ml of 3
percent H2O2 and continue heating for 10 min. Add 50 ml of hot (80 C)
deionized distilled water and heat for 20 min. Remove the flask from
the hot plate and allow to cool. Filter the sample through a Millipore
membrane filter or equivalent and transfer the filtrate to a 250-ml
volumetric flask. Dilute to volume with deionized distilled water.
5.3.4 Filter Blank. Determine a filter blank using two filters from
each lot of filters used in the sampling train. Cut each filter into
strips and place each filter in a separate 125-ml Erlenmeyer flask. Add
15 ml of 50 percent HNO3 and treat as described in Section 5.3.3 using
10 ml of 3 percent H2O2 and 50 ml of hot, deionized distilled water.
Filter and dilute to a total volume of 100 ml using deionized distilled
water.
5.3.5 0.1 N HNO3 Blank. Take the entire 200 ml of 0.1 N HNO3 to
dryness on a steam bath, add 15 ml of 50 percent HNO3, and treat as
described in Section 5.3.3 using 10 ml of 3 percent H2O2 and 50 ml of
hot, deionized distilled water. Dilute to a total volume of 100 ml
using deionized distilled water.
5.4 Analysis.
5.4.1 Lead Determination. Calibrate the spectrophotometer as
described in Section 6.2 and determine the absorbance for each source
sample, the filter blank, and 0.1 N HNO3 blank. Analyze each sample
three times in this manner. Make appropriate dilutions, as required, to
bring all sample Pb concentrations into the linear absorbance range of
the spectrophotometer.
If the Pb concentration of a sample is at the low end of the
calibration curve and high accuracy is required, the sample can be taken
to dryness on a hot plate and the residue dissolved in the appropriate
volume of water to bring it into the optimum range of the calibration
curve.
5.4.2 Check for Matrix Effects on the Lead Results. Since the
analysis for Pb by atomic absorption is sensitive to the chemical
composition and to the physical properties (viscosity, pH) of the sample
(matrix effects), the analyst shall check at least one sample from each
source using the method of additions as follows:
Add or spike an equal volume of standard solution to an aliquot of
the sample solution, then measure the absorbance of the resulting
solution and the absorbance of an aliquot of unspiked sample.
Next, calculate the Pb concentration Cs in mg/ml of the sample
solution by using the following equation:
Where:
Ca=Pb concentration of the standard solution, mg/ml.
As=Absorbance of the sample solution.
At=Absorbance of the spiked sample solution.
Volume corrections will not be required if the solutions as analyzed
have been made to the same final volume. Therefore, Cs and Ca represent
Pb concentration before dilutions.
Method of additions procedures described on pages 9-4 and 9-5 of the
section entitled ''General Information'' of the Perkin Elmer Corporation
Atomic Absorption Spectrophotometry Manual, Number 303-0152 (see
Citation 1 of Bibliography) may also be used. In any event, if the
results of the method of additions procedure used on the single source
sample do not agree to within 5 percent of the value obtained by the
routine atomic absorption analysis, then reanalyze all samples from the
source using a method of additions procedure.
5.4.3 Container No. 3 (Silica Gel). The tester may conduct this
step in the field. Weigh the spent silica gel (or silica gel plus
impinger) to the nearest 0.5 g; record this weight.
6. Calibration
Maintain a laboratory log of all calibrations.
6.1 Sampling Train Calibration. Calibrate the sampling train
components according to the indicated sections of Method 5: Probe
Nozzle (Section 5.1); Pitot Tube (Section 5.2); Metering System
(Section 5.3); Probe Heater (Section 5.4); Temperature Gauges (Section
5.5); Leak-Check of the Metering System (Section 5.6); and Barometer
(Section 5.7).
6.2 Spectrophotometer. Measure the absorbance of the standard
solutions using the instrument settings recommended by the
spectrophotometer manufacturer. Repeat until good agreement ( 3
percent) is obtained between two consecutive readings. Plot the
absorbance (y-axis) versus concentration in g Pb/ml (x-axis). Draw or
compute a straight line through the linear portion of the curve. Do not
force the calibration curve through zero, but if the curve does not pass
through the origin or at least lie closer to the origin than 0.003
absorbance units, check for incorrectly prepared standards and for
curvature in the calibration curve.
To determine stability of the calibration curve, run a blank and a
standard after every five samples and recalibrate, as necessary.
7. Calculations
7.1 Dry Gas Volume. Using the data from this test, calculate
Vm(std), the total volume of dry gas metered corrected to standard
conditions (20 C and 760 mm Hg), by using Equation 5-1 of Method 5. If
necessary, adjust Vw(std) for leakages as outlined in Section 6.3 of
Method 5. See the field data sheet for the average dry gas meter
temperature and average orifice pressure drop.
7.2 Volume of Water Vapor and Moisture Content. Using data obtained
in this test and Equations 5-2 and 5-3 of Method 5, calculate the volume
of water vapor Vw(std) and the moisture content Bws of the stack gas.
7.3 Total Lead in Source Sample. For each source sample correct the
average absorbance for the contribution of the filter blank and the 0.1
N HNO3 blank. Use the calibration curve and this corrected absorbance
to determine the g Pb concentration in the sample aspirated into the
spectrophotometer. Calculate the total Pb content C Pb (in g) in the
original source sample; correct for all the dilutions that were made to
bring the Pb concentration of the sample into the linear range of the
spectrophotometer.
7.4 Lead Concentration. Calculate the stack gas Pb concentration CPb
in mg/dscm as follows:
Where:
K=0.001 mg/ g for metric units.
=2.205 lb/ g 10^9 for English units.
7.5 Isokinetic Variation and Acceptable Results. Same as Method 5,
Sections 6.11 and 6.12, respectively. To calculate vs, the average stack
gas velocity, use Equation 2-9 of Method 2 and the data from this field
test.
8. Alternative Test Methods for Inorganic Lead
8.1 Simultaneous Determination of Particulate and Lead Emissions.
The tester may use Method 5 to simultaneously determine Pb provided that
(1) he uses acetone to remove particulate from the probe and inside of
the filter holder as specified by Method 5, (2) he uses 0.1 N HNO3 in
the impingers, (3) he uses a glass fiber filter with a low Pb
background, and (4) he treats and analyzes the entire train contents,
including the impingers, for Pb as described in Section 5 of this
method.
8.2 Filter Location. The tester may use a filter between the third
and fourth impinger provided that he includes the filter in the analysis
for Pb.
8.3 In-stack Filter. The tester may use an in-stack filter provided
that (1) he uses a glass-lined probe and at least two impingers, each
containing 100 ml of 0.1 N HNO3, after the in-stack filter and (2) he
recovers and analyzes the probe and impinger contents for Pb. Recover
sample from the nozzle with acetone if a particulate analysis is to be
made.
9. Bibliography
1. Perkin Elmer Corporation. Analytical Methods for Atomic
Absorption Spectrophotometry. Norwalk, CT. September 1976.
2. American Society for Testing and Materials. Annual Book of ASTM
Standards. Part 31; Water, Atmospheric Analysis. Philadelphia, PA.
1974. p. 40-42.
3. Klein, R. and C. Hach. Standard Additions -- Uses and
Limitations in Spectrophotometric Analysis. Amer. Lab. 9:21-27. 1977.
4. Mitchell, W.J. and M.R. Midgett. Determining Inorganic and Alkyl
Lead Emissions from Stationary Sources. U.S. Environmental Protection
Agency, Emission Monitoring and Support Laboratory. Research Triangle
Park, NC. (Presented at National APCA Meeting. Houston. June 26,
1978).
5. Same as Method 5, Citations 2 to 5 and 7 of bibliography.
*Mention of trade names or specific products does not constitute
endorsement by the U.S. Environmental Protection Agency.
40 CFR 60.748 Pt. 60, App. A, Meth. 13A
1. Principle and Applicability
1.1 Applicability. This method applies to the determination of
fluoride (F) emissions from sources as specified in the regulations. It
does not measure fluorocarbons, such as freons.
1.2 Principle. Gaseous and particulate F are withdrawn isokinetically
from the source and collected in water and on a filter. The total F is
then determined by the SPADNS Zirconium Lake Colorimetric Method.
2. Range and Sensitivity
The range of this method is 0 to 1.4 g F/ml. Sensitivity has not
been determined.
3. Interferences
Large quantities of chloride will interfere with the analysis, but
this interference can be prevented by adding silver sulfate into the
distillation flask (see Section 7.3.4). If chloride ion is present, it
may be easier to use the Specific Ion Electrode Method (Method 13B).
Grease on sample-exposed surfaces may cause low F results due to
adsorption.
4. Precision, Accuracy, and Stability
4.1 Precision. The following estimates are based on a collaborative
test done at a primary aluminum smelter. In the test, six laboratories
each sampled the stack simultaneously using two sampling trains for a
total of 12 samples per sampling run. Fluoride concentrations
encountered during the test ranged from 0.1 to 1.4 mg F/m3. The
within-laboratory and between-laboratory standard deviations, which
include sampling and analysis errors, were 0.044 mg F/m3 with 60 degrees
of freedom and 0.064 mg F/m3 with five degrees of freedom, respectively.
4.2 Accuracy. The collaborative test did not find any bias in the
analytical method.
4.3 Stability. After the sample and colorimetric reagent are mixed,
the color formed is stable for approximately 2 hours. A 3 C temperature
difference between the sample and standard solutions produces an error
of approximately 0.005 mg F/liter. To avoid this error, the absorbances
of the sample and standard solutions must be measured at the same
temperature.
5. Apparatus
5.1 Sampling Train. A schematic of the sampling train is shown in
Figure 13A-1; it is similar to the Method 5 train except the filter
position is interchangeable. The sampling train consists of the
following components:
5.1.1 Probe Nozzle, Pitot Tube, Differential Pressure Gauge, Filter
Heating System, Metering System, Barometer, and Gas Density
Determination Equipment. Same as Method 5, Sections 2.1.1, 2.1.3, 2.1.4,
2.1.6, 2.1.8, 2.1.9, and 2.1.10. When moisture condensation is a
problem, the filter heating system is used.
5.1.2 Probe Liner. Borosilicate glass or 316 stainless steel. When
the filter is located immediately after the probe, the tester may use a
probe heating system to prevent filter plugging resulting from moisture
condensation, but the tester shall not allow the temperature in the
probe to exceed 120 14 C (248 25 F).
5.1.3 Filter Holder. With positive seal against leakage from the
outside or around the filter. If the filter is located between the
probe and first impinger, use borosilicate glass or stainless steel with
a 20-mesh stainless steel screen filter support and a silicone rubber
gasket; do not use a glass frit or a sintered metal filter support. If
the filter is located between the third and fourth impingers, the tester
may use borosilicate glass with a glass frit filter support and a
silicone rubber gasket. The tester may also use other materials of
construction with approval from the Administrator.
5.1.4 Impingers. Four impingers connected as shown in Figure 13A-1
with ground-glass (or equivalent), vacuum-tight fittings. For the
first, third, and fourth impingers, use the Greenburg-Smith design,
modified by replacing the tip with a 1.3-cm-inside-diameter ( 1/2 in.)
glass tube extending to 1.3 cm ( 1/2 in.) from the bottom of the flask.
For the second impinger, use a Greenburg-Smith impinger with the
standard tip. The tester may use modifications (e.g., flexible
connections between the impingers or materials other than glass),
subject to the approval of the Administrator. Place a thermometer,
capable of measuring temperature to within 1 C (2 F), at the outlet of
the fourth impinger for monitoring purposes.
5.2 Sample Recovery. The following items are needed:
5.2.1 Probe-Liner and Probe-Nozzle Brushes, Wash Bottles, Graduated
Cylinder and/or Balance, Plastic Storage Containers, Rubber Policeman,
Funnel. Same as Method 5, Sections 2.2.1 to 2.2.2 and 2.2.5 to 2.2.8,
respectively.
5.2.2 Sample Storage Container. Wide-mouth, high-density-polyethylene
bottles for impinger water samples, 1-liter.
5.3 Analysis. The following equipment is needed:
5.3.1 Distillation Apparatus. Glass distillation apparatus assembled
as shown in Figure 13A-2.
5.3.2 Bunsen Burner.
5.3.3 Electric Muffle Furnace. Capable of heating to 600 C.
5.3.4 Crucibles. Nickel, 75- to 100-ml.
5.3.5 Beakers. 500-ml and 1500-ml.
5.3.6 Volumetric Flasks. 50-ml.
5.3.7 Erlenmeyer Flasks or Plastic Bottles. 500-ml.
5.3.8 Constant Temperature Bath. Capable of maintaining a constant
temperature of 1.0 C at room temperature conditions.
5.3.9 Balance. 300-g capacity to measure to 0.5 g.
5.3.10 Spectrophotometer. Instrument that measures absorbance at 570
nm and provides at least a 1-cm light path.
5.3.11 Spectrophotometer Cells. 1-cm pathlength.
6. Reagents
6.1 Sampling. Use ACS reagent-grade chemicals or equivalent, unless
otherwise specified. The reagents used in sampling are as follows:
6.1.1 Filters.
6.1.1.1 If the filter is located between the third and fourth
impingers, use a Whatman /1/ No. 1 filter, or equivalent, sized to fit
the filter holder.
Insert illus. 0501
Insert illus. 0502
6.1.1.2 If the filter is located between the probe and first
impinger, use any suitable medium (e.g., paper, organic membrane) that
conforms to the following specifications: (1) The filter can withstand
prolonged exposure to temperatures up to 135 C (275 F). (2) The filter
has at least 95 percent collection efficiency ( 5 percent penetration)
for 0.3 m dioctyl phthalate smoke particles. Conduct the filter
efficiency test before the test series, using ASTM Standard Method D
2986-71, or use test data from the supplier's quality control program.
(3) The filter has a low F blank value ( 0.015 mg F/cm2 of filter area).
Before the test series, determine the average F blank value of at least
three filters (from the lot to be used for sampling) using the
applicable procedures described in Sections 7.3 and 7.4 of this method.
In general, glass fiber filters have high and/or variable F blank
values, and will not be acceptable for use.
6.1.2 Water. Deionized distilled, to conform to ASTM Specification D
1193-74, Type 3. If high concentrations of organic matter are not
expected to be present, the analyst may delete the potassium
permanganate test for oxidizable organic matter.
6.1.3 Silica Gel, Crushed Ice, and Stopcock Grease. Same as Method 5,
Sections 3.1.2, 3.1.4, and 3.1.5, respectively.
6.2 Sample Recovery. Water, from same container as described in
Section 6.1.2, is needed for sample recovery.
6.3 Sample Preparation and Analysis. The reagents needed for sample
preparation and analysis are as follows:
6.3.1 Calcium Oxide (CaO). Certified grade containing 0.005 percent F
or less.
6.3.2 Phenolphthalein Indicator. Dissolve 0.1 g of phenolphthalein in
a mixture of 50 ml of 90 percent ethanol and 50 ml of deionized
distilled water.
6.3.3 Silver Sulfate (Ag2SO4).
6.3.4 Sodium Hydroxide (NaOH). Pellets.
6.3.5 Sulfuric Acid (H2SO4), Concentrated.
6.3.6 Sulfuric Acid, 25 percent (V/V). Mix 1 part of concentrated
H2SO4 with 3 parts of deionized distilled water.
6.3.7 Filters. Whatman No. 541, or equivalent.
6.3.8 Hydrochloric Acid (HCl), Concentrated.
6.3.9 Water. From same container as described in Section 6.1.2.
6.3.10 Fluoride Standard Solution, 0.01 mg F/ml. Dry in an oven at
110 C for at least 2 hours. Dissolve 0.2210 g of NaF in 1 liter of
deionized distilled water. Dilute 100 ml of this solution to 1 liter
with deionized distilled water.
6.3.11 SPADNS Solution (4, 5
dihydroxy-3-(p-sulfophenylazo)-2,7-naphthalene-disulfonic acid trisodium
salt). Dissolve 0.960 0.010 g of SPADNS reagent in 500 ml deionized
distilled water. If stored in a well-sealed bottle protected from the
sunlight, this solution is stable for at least 1 month.
6.3.12 Spectrophotometer Zero Reference Solution. Prepare daily. Add
10 ml of SPADNS solution (6.3.11) to 100 ml deionized distilled water,
and acidify with a solution prepared by diluting 7 ml of concentrated
HCl to 10 ml with deionized distilled water.
6.3.13 SPADNS Mixed Reagent. Dissolve 0.135 0.005 g of zirconyl
chloride octahydrate (ZrOCl2.8H2O) in 25 ml of deionized distilled
water. Add 350 ml of concentrated HCl, and dilute to 500 ml with
deionized distilled water. Mix equal volumes of this solution and
SPADNS solution to form a single reagent. This reagent is stable for at
least 2 months.
7. Procedure
7.1 Sampling. Because of the complexity of this method, testers
should be trained and experienced with the test procedures to assure
reliable results.
7.1.1 Pretest Preparation. Follow the general procedure given in
Method 5, Section 4.1.1, except the filter need not be weighed.
7.1.2 Preliminary Determinations. Follow the general procedure given
in Method 5, Section 4.1.2., except the nozzle size selected must
maintain isokinetic sampling rates below 28 liters/min (1.0 cfm).
7.1.3 Preparation of Collection Train. Follow the general procedure
given in Method 5, Section 4.1.3, except for the following variations:
Place 100 ml of deionized distilled water in each of the first two
impingers, and leave the third impinger empty. Transfer approximately
200 to 300 g of preweighed silica gel from its container to the fourth
impinger.
Assemble the train as shown in Figure 13A-1 with the filter between
the third and fourth impingers. Alternatively, if a 20-mesh stainless
steel screen is used for the filter support, the tester may place the
filter between the probe and first impinger. The tester may also use a
filter heating system to prevent moisture condensation, but shall not
allow the temperature around the filter holder to exceed 120 14 C (248
25 F). Record the filter location on the data sheet.
7.1.4 Leak-Check Procedures. Follow the leak-check procedures given
in Method 5, Sections 4.1.4.1 (Pretest Leak-Check), 4.1.4.2 (Leak-Checks
During the Sample Run), and 4.1.4.3 (Post-Test Leak-Check).
7.1.5 Fluoride Train Operation. Follow the general procedure given in
Method 5, Section 4.1.5, keeping the filter and probe temperatures (if
applicable) at 120 14 C (248 25 F) and isokinetic sampling rates below
28 liters/min (1.0 cfm). For each run, record the data required on a
data sheet such as the one shown in Method 5, Figure 5-2.
7.2 Sample Recovery. Begin proper cleanup procedure as soon as the
probe is removed from the stack at the end of the sampling period.
Allow the probe to cool. When it can be safely handled, wipe off all
external particulate matter near the tip of the probe nozzle and place a
cap over it to keep from losing part of the sample. Do not cap off the
probe tip tightly while the sampling train is cooling down, because a
vacuum would form in the filter holder, thus drawing impinger water
backwards.
Before moving the sample train to the cleanup site, remove the probe
from the sample train, wipe off the silicone grease, and cap the open
outlet of the probe. Be careful not to lose any condensate, if present.
Remove the filter assembly, wipe off the silicone grease from the
filter holder inlet, and cap this inlet. Remove the umbilical cord from
the last impinger, and cap the impinger. After wiping off the silicone
grease, cap off the filter holder outlet and any open impinger inlets
and outlets. The tester may use ground-glass stoppers, plastic caps, or
serum caps to close these openings.
Transfer the probe and filter-impinger assembly to an area that is
clean and protected from the wind so that the chances of contaminating
or losing the sample is minimized.
Inspect the train before and during disassembly, and note any
abnormal conditions. Treat the samples as follows:
7.2.1 Container No. 1 (Probe, Filter, and Impinger Catches). Using
a graduated cylinder, measure to the nearest ml, and record the volume
of the water in the first three impingers; include any condensate in
the probe in this determination. Transfer the impinger water from the
graduated cylinder into this polyethylene container. Add the filter to
this container. (The filter may be handled separately using procedures
subject to the Administrator's approval.) Taking care that dust on the
outside of the probe or other exterior surfaces does not get into the
sample, clean all sample-exposed surfaces (including the probe nozzle,
probe fitting, probe liner, first three impingers, impinger connectors,
and filter holder) with deionized distilled water. Use less than 500 ml
for the entire wash. Add the washings to the sampler container.
Perform the deionized distilled water rinses as follows:
Carefully remove the probe nozzle and rinse the inside surface with
deionized distilled water from a wash bottle. Brush with a Nylon
bristle brush, and rinse until the rinse shows no visible particles,
after which make a final rinse of the inside surface. Brush and rinse
the inside parts of the Swagelok fitting with deionized distilled water
in a similar way.
Rinse the probe liner with deionized distilled water. While
squirting the water into the upper end of the probe, tilt and rotate the
probe so that all inside surfaces will be wetted with water. Let the
water drain from the lower end into the sample container. The tester
may use a funnel (glass or polyethylene) to aid in transferring the
liquid washes to the container. Follow the rinse with a probe brush.
Hold the probe in an inclined position, and squirt deionized distilled
water into the upper end as the probe brush is being pushed with a
twisting action through the probe. Hold the sample container underneath
the lower end of the probe, and catch any water and particulate matter
that is brushed from the probe. Run the brush through the probe three
times or more. With stainless steel or other metal probes, run the
brush through in the above prescribed manner at least six times since
metal probes have small crevices in which particulate matter can be
entrapped. Rinse the brush with deionized distilled water, and
quantitatively collect these washings in the sample container. After
the brushing, make a final rinse of the probe as described above.
It is recommended that two people clean the probe to minimize sample
losses. Between sampling runs, keep brushes clean and protected from
contamination.
Rinse the inside surface of each of the first three impingers (and
connecting glassware) three separate times. Use a small portion of
deionized distilled water for each rinse, and brush each sample-exposed
surface with a Nylon bristle brush, to ensure recovery of fine
particulate matter. Make a final rinse of each surface and of the
brush.
After ensuring that all joints have been wiped clean of the silicone
grease, brush and rinse with deionized distilled water the inside of the
filter holder (front-half only, if filter is positioned between the
third and fourth impingers). Brush and rinse each surface three times
or more if needed. Make a final rinse of the brush and filter holder.
After all water washings and particulate matter have been collected
in the sample container, tighten the lid so that water will not leak out
when it is shipped to the laboratory. Mark the height of the fluid
level to determine whether leakage occurs during transport. Label the
container clearly to identify its contents.
7.2.2 Container No. 2 (Sample Blank). Prepare a blank by placing an
unused filter in a polyethylene container and adding a volume of water
equal to the total volume in Container No. 1. Process the blank in the
same manner as for Container No. 1.
7.2.3 Container No. 3 (Silica Gel). Note the color of the indicating
silica gel to determine whether it has been completely spent and make a
notation of its condition. Transfer the silica gel from the fourth
impinger to its original container and seal. The tester may use a
funnel to pour the silica gel and a rubber policeman to remove the
silica gel from the impinger. It is not necessary to remove the small
amount of dust particles that may adhere to the impinger wall and are
difficult to remove. Since the gain in weight is to be used for
moisture calculations, do not use any water or other liquids to transfer
the silica gel. If a balance is available in the field, the tester may
follow the analytical procedure for Container No. 3 in Section 7.4.2.
7.3 Sample Preparation and Distillation. (Note the liquid levels in
Containers No. 1 and No. 2 and confirm on the analysis sheet whether or
not leakage occurred during transport. If noticeable leakage had
occurred, either void the sample or use methods, subject to the approval
of the Administrator, to correct the final results.) Treat the contents
of each sample container as described below:
7.3.1 Container No. 1 (Probe, Filter, and Impinger Catches). Filter
this container's contents, including the sampling filter, through
Whatman No. 541 filter paper, or equivalent, into a 1500-ml beaker.
7.3.1.1 If the filtrate volume exceeds 900 ml, make the filtrate
basic (red to phenolphthalein) with NaOH, and evaporate to less than 900
ml.
7.3.1.2 Place the filtered material (including sampling filter) in a
nickel crucible, add a few ml of deionized distilled water, and macerate
the filters with a glass rod.
Add 100 mg CaO to the crucible, and mix the contents thoroughly to
form a slurry. Add two drops of phenolphthalein indicator. Place the
crucible in a hood under infrared lamps or on a hot plate at low heat.
Evaporate the water completely. During the evaporation of the water,
keep the slurry basic (red to phenolphthalein) to avoid loss of F. If
the indicator turns colorless (acidic) during the evaporation, add CaO
until the color turns red again.
After evaporation of the water, place the crucible on a hot plate
under a hood and slowly increase the temperature until the Whatman No.
541 and sampling filters char. It may take several hours to completely
char the filters.
Place the crucible in a cold muffle furnace. Gradually (to prevent
smoking) increase the temperature to 600 C, and maintain until the
contents are reduced to an ash. Remove the crucible from the furnace
and allow to cool.
Add approximately 4 g of crushed NaOH to the crucible and mix.
Return the crucible to the muffle furnace, and fuse the sample for 10
minutes at 600 C.
Remove the sample from the furnace, and cool to ambient temperature.
Using several rinsings of warm deionized distilled water, transfer the
contents of the crucible to the beaker containing the filtrate. To
assure complete sample removal, rinse finally with two 20-ml portions of
25 percent H2SO4, and carefully add to the beaker. Mix well, and
transfer to a 1-liter volumetric flask. Dilute to volume with deionized
distilled water, and mix thoroughly. Allow any undissolved solids to
settle.
7.3.2 Container No. 2 (Sample Blank). Treat in the same manner as
described in Section 7.3.1 above.
7.3.3 Adjustment of Acid/Water Ratio in Distillation Flask. (Use a
protective shield when carrying out this procedure.) Place 400 ml of
deionized distilled water in the distillation flask, and add 200 ml of
concentrated H2SO4. (Caution: Observe standard precautions when mixing
H2SO4 with water. Slowly add the acid to the flask with constant
swirling.) Add some soft glass beads and several small pieces of broken
glass tubing, and assemble the apparatus as shown in Figure 13A-2. Heat
the flask until it reaches a temperature of 175 C to adjust the
acid/water ratio for subsequent distillations. Discard the distillate.
7.3.4 Distillation. Cool the contents of the distillation flask to
below 80 C. Pipet an aliquot of sample containing less than 10.0 mg F
directly into the distillation flask, and add deionized distilled water
to make a total volume of 220 ml added to the distillation flask. (To
estimate the appropriate aliquot size, select an aliquot of the solution
and treat as described in Section 7.4.1. This will be an approximation
of the F content because of possible interfering ions.)
Note: If the sample contains chloride, add 5 mg of Ag2SO4 to the
flask for every mg of chloride.
Place a 250-ml volumetric flask at the condenser exit. Heat the
flask as rapidly as possible with a Bunsen burner, and collect all the
distillate up to 175 C. During heatup, play the burner flame up and
down the side of the flask to prevent bumping. Conduct the distillation
as rapidly as possible (15 minutes or less). Slow distillations have
been found to produce low F recoveries. Caution: Be careful not to
exceed 175 C to avoid causing H2SO4 to distill over.
If F distillation in the mg range is to be followed by a distillation
in the fractional mg range, add 220 ml of deionized distilled water and
distill it over as in the acid adjustment step to remove residual F from
the distillation system.
The tester may use the acid in the distillation flask until there is
carry-over of interferences or poor F recovery. Check for these every
tenth distillation using a deionized distilled water blank and a
standard solution. Change the acid whenever the F recovery is less than
90 percent or the blank value exceeds 0.1 g/ml.
7.4 Analysis.
7.4.1 Containers No. 1 and No. 2. After distilling suitable
aliquots from Containers No. 1 and No. 2 according to Section 7.3.4,
dilute the distillate in the volumetric flasks to exactly 250 ml with
deionized distilled water, and mix thoroughly. Pipet a suitable aliquot
of each sample distillate (containing 10 to 40 g F/ml) into a beaker,
and dilute to 50 ml with deionized distilled water. Use the same
aliquot size for the blank. Add 10 ml of SPADNS mixed reagent (6.3.13),
and mix thoroughly.
After mixing, place the sample in a constant-temperature bath
containing the standard solutions (see Section 8.2) for 30 minutes
before reading the absorbance on the spectrophotometer.
Set the spectrophotometer to zero absorbance at 570 nm with the
reference solution (6.3.12), and check the spectrophotometer calibration
with the standard solution. Determine the absorbance of the samples,
and determine the concentration from the calibration curve. If the
concentration does not fall within the range of the calibration curve,
repeat the procedure using a different size aliquot.
7.4.2 Container No. 3 (Silica Gel). Weigh the spent silica gel (or
silica gel plus impinger) to the nearest 0.5 g using a balance. The
tester may conduct this step in the field.
8. Calibration
Maintain a laboratory log of all calibrations.
8.1 Sampling Train. Calibrate the sampling train components according
to the indicated sections in Method 5: Probe Nozzle (Section 5.1);
Pitot Tube (Section 5.2); Metering System (Section 5.3); Probe Heater
(Section 5.4); Temperature Gauges (Section 5.5); Leak Check of
Metering System (Section 5.6); and Barometer (Section 5.7).
8.2 Spectrophotometer. Prepare the blank standard by adding 10 ml of
SPADNS mixed reagent to 50 ml of deionized distilled water. Accurately
prepare a series of standards from the 0.01 mg F/ml standard fluoride
solution (6.3.10) by diluting 0, 2, 4, 6, 8, 10, 12, and 14 ml to 100 ml
with deionized distilled water. Pipet 50 ml from each solution and
transfer each to a separate 100-ml beaker. Then add 10 ml of SPADNS
mixed reagent to each. These standards will contain 0, 10, 20, 30, 40
50, 60, and 70 g F (0 to 1.4 g/ml), respectively.
After mixing, place the reference standards and reference solution in
a constant temperature bath for 30 minutes before reading the absorbance
with the spectrophotometer. Adjust all samples to this same temperature
before analyzing.
With the spectrophotometer at 570 nm, use the reference solution
(6.3.12) to set the absorbance to zero.
Determine the absorbance of the standards. Prepare a calibration
curve by plotting g F/50 ml versus absorbance on linear graph paper.
Prepare the standard curve initially and thereafter whenever the SPADNS
mixed reagent is newly made. Also, run a calibration standard with each
set of samples and if it differs from the calibration curve by 2
percent, prepare a new standard curve.
9. Calculations
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after final
calculation. Other forms of the equations may be used, provided that
they yield equivalent results.
9.1 Nomenclature
Ad = Aliquot of distillate taken for color development, ml.
At = Aliquot of total sample added to still, ml.
Bws = Water vapor in the gas stream, proportion by volume.
Cs = Concentration of F in stack gas, mg/m3 (mg/ft3), dry basis,
corrected to standard conditions of 760 mm Hg (29.92 in. Hg) and 293 K
(528 R).
Ft = Total F in sample, mg.
g F = Concentration from the calibration curve, g.
Tm = Absolute average dry gas meter temperature (see Figure 5-2 of
Method 5), K ( R).
Ts = Absolute average stack gas temperature (see Figure 5-2 of Method
5), K ( R).
Vd = Volume of distillate as diluted, ml.
Vm(std) = Volume of gas sample as measured by dry gas meter,
corrected to standard conditions, dscm (dscf).
Vt = Total volume of F sample, after final dilution, ml.
Vw(std) = Volume of water vapor in the gas sample, corrected to
standard conditions, scm (scf).
9.2 Average Dry Gas Meter Temperature and Average Orifice Pressure
Drop. See data sheet (Figure 5-2 of Method 5).
9.3 Dry Gas Volume. Calculate Vm(std) and adjust for leakage, if
necessary, using the equation in Section 6.3 of Method 5.
9.4 Volume of Water Vapor and Moisture Content. Calculate the volume
of water vapor Vw(std) and moisture content Bws from the data obtained
in this method (Figure 13A-1); use Equations 5-2 and 5-3 of Method 5.
9.5 Concentration.
9.5.1 Total Fluoride in Sample. Calculate the amount of F in the
sample using the following equation:
9.5.2 Fluoride Concentration in Stack Gas. Determine the F
concentration in the stack gas using the following equation:
9.6 Isokinetic Variation and Acceptable Results. Use Method 5,
Sections 6.11 and 6.12.
10. Bibliography
1. Bellack, Ervin, Simplified Fluoride Distillation Method. Journal
of the American Water Works Association. 50: 5306. 1958.
2. Mitchell, W. J., J. C. Suggs, and F. J. Bergman. Collaborative
Study of EPA Method 13A and Method 13B. Publication No.
EPA-600/4-77-050. Environmental Protection Agency. Research Triangle
Park, NC. December 1977.
3. Mitchell, W. J. and M. R. Midgett. Adequacy of Sampling Trains
and Analytical Procedures Used for Fluoride. Atm. Environ. 10:
865-872. 1976.
1Mention of company or product names does not constitute endorsement
by the U.S. Environmental Protection Agency.
40 CFR 60.748 Pt. 60, App. A, Meth. 13B
1. Principle and Applicability
1.1 Applicability. This method applies to the determination of
fluoride (F) emissions from stationary sources as specified in the
regulations. It does not measure fluorocarbons, such as freons.
1.2 Principle. Gaseous and particulate F are withdrawn isokinetically
from the source and collected in water and on a filter. The total F is
then determined by the specific ion electrode method.
2. Range and Sensitivity
The range of this method is 0.02 to 2,000 g F/ml; however,
measurements of less than 0.1 g F/ml require extra care. Sensitivity
has not been determined.
3. Interferences
Grease on sample-exposed surfaces may cause low F results because of
adsorption.
4. Precision and Accuracy
4.1 Precision. The following estimates are based on a collaborative
test done at a primary aluminum smelter. In the test, six laboratories
each sampled the stack simultaneously using two sampling trains for a
total of 12 samples per sampling run. Fluoride concentrations
encountered during the test ranged from 0.1 to 1.4 mg F/m3. The
within-laboratory and between-laboratory standard deviations, which
include sampling and analysis errors, are 0.037 mg F/m3 with 60 degrees
of freedom and 0.056 mg F/m3 with five degrees of freedom, respectively.
4.2 Accuracy. The collaborative test did not find any bias in the
analytical method.
5. Apparatus
5.1 Sampling Train and Sample Recovery. Same as Method 13A, Sections
5.1 and 5.2, respectively.
5.2 Analysis. The following items are needed:
5.2.1 Distillation Apparatus, Bunsen Burner, Electric Muffle Furnace,
Crucibles, Beakers, Volumetric Flasks, Erlenmeyer Flasks or Plastic
Bottles, Constant Temperature Bath, and Balance. Same as Method 13A,
Sections 5.3.1 to 5.3.9, respectively, except include also 100-ml
polyethylene beakers.
5.2.2 Fluoride Ion Activity Sensing Electrode.
5.2.3 Reference Electrode. Single junction, sleeve type.
5.2.4 Electrometer. A pH meter with millivolt-scale capable of
0.1-mv resolution, or a specific ion meter made specifically for
specific ion use.
5.2.5 Magnetic Stirrer and TFE2 Fluorocarbon-Coated Stirring Bars.
6. Reagents
6.1 Sampling and Sample Recovery. Same as Method 13A, Sections 6.1
and 6.2, respectively.
6.2 Analysis. Use ACS reagent grade chemicals (or equivalent), unless
otherwise specified. The reagents needed for analysis are as follows:
6.2.1 Calcium Oxide (CaO). Certified grade containing 0.005 percent F
or less.
6.2.2 Phenolphthalein Indicator. Dissolve 0.1 g of phenolphthalein in
a mixture of 50 ml of 90 percent ethanol and 50 ml deionized distilled
water.
6.2.3 Sodium Hydroxide (NaOH). Pellets.
6.2.4 Sulfuric Acid (H2SO4), Concentrated.
6.2.5 Filters. Whatman No. 541, or equivalent.
6.2.6 Water. From same container as 6.1.2 of Method 13A.
6.2.7 Sodium Hydroxide, 5 M. Dissolve 20 g of NaOH in 100 ml of
deionized distilled water.
6.2.8 Sulfuric Acid, 25 percent (V/V). Mix 1 part of concentrated
H2SO4 with 3 parts of deionized distilled water.
6.2.9 Total Ionic Strength Adjustment Buffer (TISAB). Place
approximately 500 ml of deionized distilled water in a 1-liter beaker.
Add 57 ml of glacial acetic acid, 58 g of sodium chloride, and 4 g of
cyclohexylene dinitrilo tetraacetic acid. Stir to dissolve. Place the
beaker in a water bath to cool it. Slowly add 5 M NaOH to the solution,
measuring the pH continuously with a calibrated pH/reference electrode
pair, until the pH is 5.3. Cool to room temperature. Pour into a
1-liter volumetric flask, and dilute to volume with deionized distilled
water. Commercially prepared TISAB may be substituted for the above.
6.2.10 Fluoride Standard Solution, 0.1 M. Oven dry some sodium
fluoride (NaF) for a minimum of 2 hours at 110 C, and store in a
desiccator. Then add 4.2 g of NaF to a 1-liter volumetric flask, and
add enough deionized distilled water to dissolve. Dilute to volume with
deionized distilled water.
7. Procedure
7.1 Sampling, Sample Recovery, and Sample Preparation and
Distillation. Same as Method 13A, Sections 7.1, 7.2, and 7.3,
respectively, except the notes concerning chloride and sulfate
interferences are not applicable.
7.2 Analysis.
7.2.1 Containers No. 1 and No. 2. Distill suitable aliquots from
Containers No. 1 and No. 2. Dilute the distillate in the volumetric
flasks to exactly 250 ml with deionized distilled water and mix
thoroughly. Pipet a 25-ml aliquot from each of the distillate and
separate beakers. Add an equal volume of TISAB, and mix. The sample
should be at the same temperature as the calibration standards when
measurements are made. If ambient laboratory temperature fluctuates
more than 2 C from the temperature at which the calibration standards
were measured, condition samples and standards in a constant-temperature
bath before measurement. Stir the sample with a magnetic stirrer during
measurement to minimize electrode response time. If the stirrer
generates enough heat to change solution temperature, place a piece of
temperature insulating material such as cork, between the stirrer and
the beaker. Hold dilute samples (below 10^4 M fluoride ion content) in
polyethylene beakers during measurement.
Insert the fluoride and reference electrodes into the solution. When
a steady millivolt reading is obtained, record it. This may take
several minutes. Determine concentration from the calibration curve.
Between electrode measurements, rinse the electrode with deionized
distilled water.
7.2.2 Container No. 3 (Silica Gel). Same as Method 13A, Section
7.4.2.
8. Calibration
Maintain a laboratory log of all calibrations.
8.1 Sampling Train. Same as Method 13A.
8.2 Fluoride Electrode. Prepare fluoride standardizing solutions by
serial dilution of the 0.1 M fluoride standard solution. Pipet 10 ml of
0.1 M fluoride standard solution into a 100-ml volumetric flask, and
make up to the mark with deionized distilled water for a 10^2 M standard
solution. Use 10 ml of 10^2 M solution to make a 10^3 M solution in the
same manner. Repeat the dilution procedure and make 10^4 and 10^5
solutions.
Pipet 50 ml of each standard into a separate beaker. Add 50 ml of
TISAB to each beaker. Place the electrode in the most dilute standard
solution. When a steady millivolt reading is obtained, plot the value
on the linear axis of semilog graph paper versus concentration on the
log axis. Plot the nominal value for concentration of the standard on
the log axis, e.g., when 50 ml of 10^2 M standard is diluted with 50 ml
of TISAB, the concentration is still designated ''10^2 M.''
Between measurements soak the fluoride sensing electrode in deionized
distilled water for 30 seconds, and then remove and blot dry. Analyze
the standards going from dilute to concentrated standards. A
straight-line calibration curve will be obtained, with nominal
concentrations of 10^4, 10^3, 10^2, and 10^1 fluoride molarity on the
log axis plotted versus electrode potential (in mv) on the linear scale.
Some electrodes may be slightly nonlinear between 10^5 and 10^4 M. If
this occurs, use additional standards between these two concentrations.
Calibrate the fluoride electrode daily, and check it hourly. Prepare
fresh fluoride standardizing solutions daily (10^2 M or less). Store
fluoride standardizing solutions in polyethylene or polypropylene
containers.
Note: Certain specific ion meters have been designed specifically
for fluoride electrode use and give a direct readout of fluoride ion
concentration. These meters may be used in lieu of calibration curves
for fluoride measurements over narrow concentration ranges. Calibrate
the meter according to the manufacturer's instructions.)
9. Calculations
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after final
calculation.
9.1 Nomenclature. Same as Method 13A, Section 9.1. In addition:
M=F concentration from calibration curve, molarity.
9.2 Average Dry Gas Meter Temperature and Average Orifice Pressure
Drop, Dry Gas Volume, Volume of Water Vapor and Moisture Content,
Fluoride Concentration in Stack Gas, and Isokinetic Variation and
Acceptable Results. Same as Method 13A, Sections 9.2 to 9.4, 9.5.2, and
9.6, respectively.
9.3 Fluoride in Sample. Calculate the amount of F in the sample using
the following:
Where:
K=19 mg/millimole.
10. Bibliography
1. Same as Method 13A, Citations 1 and 2 of Bibliography.
2. MacLeod, Kathryn E. and Howard L. Crist. Comparison of the
SPADNS -- Zirconium Lake and Specific Ion Electrode Methods of Fluoride
Determination in Stack Emission Samples. Analytical Chemistry.
45:1272-1273. 1973.
2Mention of any trade name or specific product does not constitute
endorsement by the U.S. Environmental Protection Agency.
40 CFR 60.748 Pt. 60, App. A, Meth. 14
1. Applicability and Principle
1.1 Applicability. This method is applicable for the determination of
fluoride emissions from stationary sources only when specified by the
test procedures for determining compliance with new source performance
standards.
1.2 Principle. Gaseous and particulate fluoride roof monitor
emissions are drawn into a permanent sampling manifold through several
large nozzles. The sample is transported from the sampling manifold to
ground level through a duct. The gas in the duct is sampled using
Method 13A or 13B -- Determination of Total Fluoride Emissions from
Stationary Sources. Effluent velocity and volumetric flow rate are
determined with anemometers located in the roof monitor.
2. Apparatus
2.1 Velocity Measurement Apparatus.
2.1.1 Anemometers. Propeller anemometers, or equivalent. Each
anemometer shall meet the following specifications: (1) Its propeller
shall be made of polystyrene, or similar material of uniform density.
To insure uniformity of performance among propellers, it is desirable
that all propellers be made from the same mold; (2) The propeller shall
be properly balanced, to optimize performance; (3) When the anemometer
is mounted horizontally, its threshold velocity shall not exceed 15
m/min (50 fpm); (4) The measurement range of the anemometer shall
extend to at least 600 m/min (2,000 fpm); (5) The anemometer shall be
able to withstand prolonged exposure to dusty and corrosive
environments; one way of achieving this is to continuously purge the
bearings of the anemometer with filtered air during operation; (6) All
anemometer components shall be properly shielded or encased, such that
the performance of the anemometer is uninfluenced by potroom magnetic
field effects; (7) A known relationship shall exist between the
electrical output signal from the anemometer generator and the propeller
shaft rpm, at a minimum of three evenly spaced rpm settings between 60
and 1800 rpm; for the 3 settings, use 60 15, 900 100, and 1800 100 rpm.
Anemometers having other types of output signals (e.g., optical) may be
used, subject to the approval of the Administrator. If other types of
anemometers are used, there must be a known relationship (as described
above) between output signal and shaft rpm; also, each anemometer must
be equipped with a suitable readout system (See Section 2.1.3).
2.1.2 Installation of Anemometers.
2.1.2.1 If the affected facility consists of a single, isolated
potroom (or potroom segment), install at least one anemometer for every
85 m of roof monitor length. If the length of the roof monitor divided
by 85 m is not a whole number, round the fraction to the nearest whole
number to determine the number of anemometers needed. For monitors that
are less than 130 m in length, use at least two anemometers. Divide the
monitor cross-section into as many equal areas as anemometers and locate
an anemometer at the centroid of each equal area. See exception in
Section 2.1.2.3.
2.1.2.2 If the affected facility consists of two or more potrooms (or
potroom segments) ducted to a common control device, install anemometers
in each potroom (or segment) that contains a sampling manifold. Install
at least one anemometer for every 85 m of roof monitor length of the
potroom (or segment). If the potroom (or segment) length divided by 85
is not a whole number, round the fraction to the nearest whole number to
determine the number of anemometers needed. If the potroom (or segment)
length is less than 130 m, use at least two anemometers. Divide the
potroom (or segment) monitor cross-section into as many equal areas as
anemometers and locate an anemometer at the centroid of each equal area.
See exception in Section 2.1.2.3.
2.1.2.3 At least one anemometer shall be installed in the immediate
vicinity (i.e., within 10 m) of the center of the manifold (See Section
2.2.1). For its placement in relation to the width of the monitor, there
are two alternatives. The first is to make a velocity traverse of the
width of the roof monitor where an anemometer is to be placed and
install the anemometer at a point of average velocity along this
traverse. The traverse may be made with any suitable low velocity
measuring device, and shall be made during normal process operating
conditions.
The second alternative, at the option of the tester, is to install
the anemometer halfway across the width of the roof monitor. In this
latter case, the velocity traverse need not be conducted.
2.1.3 Recorders. Recorders, equipped with suitable auxiliary
equipment (e.g. transducers) for converting the output signal from each
anemometer to a continuous recording of air flow velocity, or to an
integrated measure of volumetric flowrate. A suitable recorder is one
that allows the output signal from the propeller anemometer to be read
to within 1 percent when the velocity is between 100 and 120 m/min (350
and 400 fpm). For the purpose of recording velocity, ''continuous''
shall mean one readout per 15-minute or shorter time interval. A
constant amount of time shall elapse between readings. Volumetric flow
rate may be determined by an electrical count of anemometer revolutions.
The recorders or counters shall permit identification of the velocities
or flowrate measured by each individual anemometer.
2.1.4 Pitot Tube. Standard-type pitot tube, as described in Section
2.7 of Method 2, and having a coefficient of 0.99 0.01.
2.1.5 Pitot Tube (Optional). Isolated, Type S pitot, as described in
Section 2.1 of Method 2. The pitot tube shall have a known coefficient,
determined as outlined in Section 4.1 of Method 2.
2.1.6 Differential Pressure Gauge. Inclined manometer or equivalent,
as described in Section 2.1.2 of Method 2.
2.2 Roof Monitor Air Sampling System.
2.2.1 Sampling Ductwork. A minimum of one manifold system shall be
installed for each potroom group (as defined in Subpart S, Section
60.191). The manifold system and connecting duct shall be permanently
installed to draw an air sample from the roof monitor to ground level.
A typical installation of a duct for drawing a sample from a roof
monitor to ground level is shown in Figure 14-1. A plan of a manifold
system that is located in a roof monitor is shown in Figure 14.2. These
drawings represent a typical installation for a generalized roof
monitor. The dimensions on these figures may be altered slightly to
make the manifold system fit into a particular roof monitor, but the
general configuration shall be followed. There shall be eight nozzles,
each having a diameter of 0.40 to 0.50 m. Unless otherwise specified by
the Administrator, the length of the manifold system from the first
nozzle to the eighth shall be 35 m or eight percent of the length of the
potroom (or potroom segment) roof monitor, whichever is greater. The
duct leading from the roof monitor manifold shall be round with a
diameter of 0.30 to 0.40 m. As shown in Figure 14-2, each of the sample
legs of the manifold shall have a device, such as a blast gate or valve,
to enable adjustment of the flow into each sample nozzle.
Insert illus. 01389
Insert illus. 01390
The manifold shall be located in the immediate vicinity of one of the
propeller anemometers (see Section 2.1.2.3) and as close as possible to
the midsection of the potroom (or potroom segment). Avoid locating the
manifold near the end of a potroom or in a section where the aluminum
reduction pot arrangement is not typical of the rest of the potroom (or
potroom segment). Center the sample nozzles in the throat of the roof
monitor (see Figure 14-1). Construct all sample-exposed surfaces within
the nozzles, manifold and sample duct of 316 stainless steel. Aluminum
may be used if a new ductwork system is conditioned with fluoride-laden
roof monitor air for a period of six weeks prior to initial testing.
Other materials of construction may be used if it is demonstrated
through comparative testing that there is no loss of fluorides in the
system. All connections in the ductwork shall be leak free.
Locate two sample ports in a vertical section of the duct between the
roof monitor and exhaust fan. The sample ports shall be at least 10
duct diameters downstream and three diameters upstream from any flow
disturbance such as a bend or contraction. The two sample ports shall
be situated 90 apart. One of the sample ports shall be situated so
that the duct can be traversed in the plane of the nearest upstream duct
bend.
2.2.2 Exhaust Fan. An industrial fan or blower shall be attached to
the sample duct at ground level (see Figure 14-1). This exhaust fan
shall have a capacity such that a large enough volume of air can be
pulled through the ductwork to maintain an isokinetic sampling rate in
all the sample nozzles for all flow rates normally encountered in the
roof monitor.
The exhaust fan volumetric flow rate shall be adjustable so that the
roof monitor air can be drawn isokinetically into the sample nozzles.
This control of flow may be achieved by a damper on the inlet to the
exhauster or by any other workable method.
2.3 Temperature Measurement Apparatus.
2.3.1 Thermocouple. Install a thermocouple in the roof monitor near
the sample duct. The thermocouple shall conform to the specifications
outlined in Section 2.3 of Method 2.
2.3.2 Signal Transducer. Transducer, to change the thermocouple
voltage output to a temperature readout.
2.3.3 Thermocouple Wire. To reach from roof monitor to signal
transducer and recorder.
2.3.4 Recorder. Suitable recorder to monitor the output from the
thermocouple signal transducer.
2.4 Fluoride Sampling Train. Use the train described in Method 13A
or 13B.
3. Reagents
3.1 Sampling and Analysis. Use reagents described in Method 13A or
13B.
4. Calibration
4.1 Initial Performance Checks. Conduct these checks within 60 days
prior to the first performance test.
4.1.1 Propeller Anemometers. Anemometers which meet the
specifications outlined in Section 2.1.1 need not be calibrated,
provided that a reference performance curve relating anemometer signal
output to air velocity (covering the velocity range of interest) is
available from the manufacturer. For the purpose of this method, a
''reference'' performance curve is defined as one that has been derived
from primary standard calibration data, with the anemometer mounted
vertically. ''Primary standard'' data are obtainable by: (1) Direct
calibration of one or more of the anemometers by the National Bureau of
Standards (NBS); (2) NBS-traceable calibration; or (3) Calibration by
direct measurement of fundamental parameters such as length and time
(e.g., by moving the anemometers through still air at measured rates of
speed, and recording the output signals). If a reference performance
curve is not available from the manufacturer, such a curve shall be
generated, using one of the three methods described as above. Conduct a
performance-check as outlined in Sections 4.1.1.1 through 4.1.1.3,
below. Alternatively, the tester may use any other suitable method,
subject to the approval of the Administrator, that takes into account
the signal output, propeller condition and threshold velocity of the
anemometer.
4.1.1.1 Check the signal output of the anemometer by using an
accurate rpm generator (see Figure 14-3) or synchronous motors to spin
the propeller shaft at each of the three rpm settings described in
Section 2.1.1 above (specification No. 7), and measuring the output
signal at each setting. If, at each setting, the output signal is
within 5 percent of the manufacturer's value, the anemometer can be
used. If the anemometer performance is unsatisfactory, the anemometer
shall either be replaced or repaired.
4.1.1.2 Check the propeller condition, by visually inspecting the
propeller, making note of any significant damage or warpage; damaged or
deformed propellers shall be replaced.
4.1.1.3 Check the anemometer threshold velocity as follows: With the
anemometer mounted as shown in Figure 14-4(A), fasten a known weight (a
straight-pin will suffice) to the anemometer propeller at a fixed
distance from the center of the propeller shaft. This will generate a
known torque; for example, a 0.1 g weight, placed 10 cm from the center
of the shaft, will generate a torque of 1.0 g-cm. If the known torque
causes the propeller to rotate downward, approximately 90 (see Figure
14-4(B)), then the known torque is greater than or equal to the starting
torque; if the propeller fails to rotate approximately 90 , the known
torque is less than the starting torque. By trying different
combinations of weight and distance, the starting torque of a particular
anemometer can be satisfactorily estimated. Once an estimate of the
starting torque has been obtained, the threshold velocity of the
anemometer (for horizontal mounting) can be estimated from a graph such
as Figure 14-5 (obtained from the manufacturer). If the horizontal
threshold velocity is acceptable (<15 m/min (50 fpm), when this
technique is used), the anemometer can be used. If the threshold
velocity of an anemometer is found to be unacceptably high, the
anemometer shall either be replaced or repaired.
Insert illus. 01396
Insert illus. 01397
Insert illus. 01398
4.1.2 Thermocouple. Check the calibration of the
thermocouple-potentiometer system, using the procedures outlined in
Section 4.3 of Method 2, at temperatures of 0, 100, and 150 C. If the
calibration is off by more than 5 C at any of the temperatures, repair
or replace the system; otherwise, the system can be used.
4.1.3 Recorders and/or Counters. Check the calibration of each
recorder and/or counter (see Section 2.1.3) at a minimum of three
points, approximately spanning the expected range of velocities. Use
the calibration procedures recommended by the manufacturer, or other
suitable procedures (subject to the approval of the Administrator). If
a recorder or counter is found to be out of calibration, by an average
amount greater than 5 percent for the three calibration points, replace
or repair the system; otherwise, the system can be used.
4.1.4 Manifold Intake Nozzles. In order to balance the flow rates in
the eight individual nozzles, proceed as follows: Adjust the exhaust
fan to draw a volumetric flow rate (refer to Equation 14-1) such that
the entrance velocity into each manifold nozzle approximates the average
effluent velocity in the roof monitor. Measure the velocity of the air
entering each nozzle by inserting a standard pitot tube into a 2.5 cm or
less diameter hole (see Figure 14-2) located in the manifold between
each blast gate (or valve) and nozzle. Note that a standard pitot tube
is used, rather than a type S, to eliminate possible velocity
measurement errors due to cross-section blockage in the small (0.13 m
diameter) manifold leg ducts. The pitot tube tip shall be positioned at
the center of each manifold leg duct. Take care to insure that there is
no leakage around the pitot tube, which could affect the indicated
velocity in the manifold leg. If the velocity of air being drawn into
each nozzle is not the same, open or close each blast gate (or valve)
until the velocity in each nozzle is the same. Fasten each blast gate
(or valve) so that it will remain in this position and close the pitot
port holes. This calibration shall be performed when the manifold
system is installed. Alternatively, the manifold may be preassembled
and the flow rates balanced on the ground, before being installed.
4.2 Periodical Performance Checks. Twelve months after their initial
installation, check the calibration of the propeller anemometers,
thermocouple-potentiometer system, and the recorders and/or counters as
in Section 4.1. If the above systems pass the performance checks, (i.e.,
if no repair or replacement of any component is necessary), continue
with the performance checks on a 12-month interval basis. However, if
any of the above systems fail the performance checks, repair or replace
the system(s) that failed and conduct the periodical performance checks
on a 3-month interval basis, until sufficient information (consult with
the Administrator) is obtained to establish a modified performance check
schedule and calculation procedure.
Note: If any of the above systems fail the initial performance
checks, the data for the past year need not be recalculated.
5. Procedure
5.1 Roof Monitor Velocity Determination.
5.1.1 Velocity Estimate(s) for Setting Isokinetic Flow. To assist in
setting isokinetic flow in the manifold sample nozzles, the anticipated
average velocity in the section of the roof monitor containing the
sampling manifold shall be estimated prior to each test run. The tester
may use any convenient means to make this estimate (e.g., the velocity
indicated by the anemometer in the section of the roof monitor
containing the sampling manifold may be continuously monitored during
the 24-hour period prior to the test run).
If there is question as to whether a single estimate of average
velocity is adequate for an entire test run (e.g., if velocities are
anticipated to be significantly different during different potroom
operations), the tester may opt to divide the test run into two or more
''sub-runs,'' and to use a different estimated average velocity for each
sub-run (see Section 5.3.2.2.)
5.1.2 Velocity Determination During a Test Run. During the actual
test run, record the velocity or volumetric flowrate readings of each
propeller anemometer in the roof monitor. Readings shall be taken for
each anemometer every 15 minutes or at shorter equal time intervals (or
continuously).
5.2 Temperature Recording. Record the temperature of the roof
monitor every 2 hours during the test run.
5.3 Sampling.
5.3.1 Preliminary Air Flow in Duct. During 24 hours preceding the
test, turn on the exhaust fan and draw roof monitor air through the
manifold duct to condition the ductwork. Adjust the fan to draw a
volumetric flow through the duct such that the velocity of gas entering
the manifold nozzles approximates the average velocity of the air
exiting the roof monitor in the vicinity of the sampling manifold.
5.3.2 Manifold Isokinetic Sample Rate Adjustment(s).
5.3.2.1 Initial Adjustment. Prior to the test run (or first sub-run,
if applicable; see Sections 5.1.1 and 5.3.2.2), adjust the fan to
provide the necessary volumetric flowrate in the sampling duct, so that
air enters the manifold sample nozzles at a velocity equal to the
appropriate estimated average velocity determined under Section 5.1.1.
Equation 14-1 gives the correct stream velocity needed in the duct at
the sampling location, in order for sample gas to be drawn
isokinetically into the manifold nozzles. Next, verify that the correct
stream velocity has been achieved, by performing a pitot tube traverse
of the sample duct (using either a standard or type S pitot tube); use
the procedure outlined in Method 2.
Where:
vd=Desired velocity in duct at sampling location, m/sec.
Dn=Diameter of a roof monitor manifold nozzle, m.
Dd=Diameter of duct at sampling location, m.
vm=Average velocity of the air stream in the roof monitor, m/min, as
determined under Section 5.1.1.
5.3.2.2 Adjustments During Run. If the test run is divided into two
or more ''sub-runs'' (see Section 5.1.1), additional isokinetic rate
adjustment(s) may become necessary during the run. Any such adjustment
shall be made just before the start of a sub-run, using the procedure
outlined in Section 5.3.2.1 above.
Note: Isokinetic rate adjustments are not permissible during a
sub-run.
5.3.3 Sample Train Operation. Sample the duct using the standard
fluoride train and methods described in Methods 13A and 13B. Determine
the number and location of the sampling points in accordance with Method
1. A single train shall be used for the entire sampling run.
Alternatively, if two or more sub-runs are performed, a separate train
may be used for each sub-run; note, however, that if this option is
chosen, the area of the sampling nozzle shall be the same ( 2 percent)
for each train. If the test run is divided into sub-runs, a complete
traverse of the duct shall be performed during each sub-run.
5.3.4 Time Per Run. Each test run shall last 8 hours or more; if
more than one run is to be performed, all runs shall be of approximately
the same ( 10 percent) length. If question exists as to the
representativeness of an 8-hour test, a longer period should be
selected. Conduct each run during a period when all normal operations
are performed underneath the sampling manifold. For most
recently-constructed plants, 24 hours are required for all potroom
operations and events to occur in the area beneath the sampling
manifold. During the test period, all pots in the potroom group shall
be operated such that emissions are representative of normal operating
conditions in the potroom group.
5.3.5 Sample Recovery. Use the sample recovery procedure described
in Method 13A or 13B.
5.4 Analysis. Use the analysis procedures described in Method 13A or
13B.
6. Calculations
6.1 Isokinetic Sampling Check.
6.1.1 Calculate the mean velocity (vm) for the sampling run, as
measured by the anemometer in the section of the roof monitor containing
the sampling manifold. If two or more sub-runs have been performed, the
tester may opt to calculate the mean velocity for each sub-run.
6.1.2 Using Equation 14-1, calculate the expected average velocity
(vd) in the sampling duct, corresponding to each value of vm obtained
under Section 6.1.1.
6.1.3 Calculate the actual average velocity (vs) in the sampling duct
for each run or sub-run, according to Equation 2-9 of Method 2, and
using data obtained from Method 13.
6.1.4 Express each value vs from Section 6.1.3 as a percentage of the
corresponding vd value from Section 6.1.2.
6.1.4.1 If vs is less than or equal to 120 percent of vd, the results
are acceptable (note that in cases where the above calculations have
been performed for each sub-run, the results are acceptable if the
average percentage for all sub-runs is less than or equal to 120
percent).
6.1.4.2 If vs is more than 120 percent of vd, multiply the reported
emission rate by the following factor.
6.2 Average Velocity of Roof Monitor Gases. Calculate the average
roof monitor velocity using all the velocity or volumetric flow readings
from Section 5.1.2.
6.3 Roof Monitor Temperature. Calculate the mean value of the
temperatures recorded in Section 5.2.
6.4 Concentration of Fluorides in Roof Monitor Air.
6.4.1 If a single sampling train was used throughout the run,
calculate the average fluoride concentration for the roof monitor using
Equation 13A-2 of Method 13A.
6.4.2 If two or more sampling trains were used (i.e., one per
sub-run), calculate the average fluoride concentration for the run, as
follows:
Where:
C8s=Average fluoride concentration in roof monitor air, mg F/dscm (mg
F/dscf).
Ft=Total fluoride mass collected during a particular sub-run, mg F
(from Equation 13A-1 of Method 13A or Equation 13B-1 of Method 13B).
Vm(std)=Total volume of sample gas passing through the dry gas meter
during a particular sub-run, dscm (dscf) (see Equation 5-1 of Method 5).
n=Total number of sub-runs.
6.5 Average volumetric flow from the roof monitor of the potroom(s)
(or potroom segment(s)) containing the anemometers is given in Equation
14-3.
Eq. 14-3
Where:
Qsd=Average volumetric flow from roof monitor at standard conditions
on a dry basis, m3/min.
A=Roof monitor open area, m2.
vmt=Average velocity of air in the roof monitor, m/min, from Section
6.2.
Pm=Pressure in the roof monitor; equal to barometric pressure for
this application, mm Hg.
tm=Roof monitor temperature, C, from Section 6.3.
Md=Mole fraction of dry gas, which is given by:
Note: Bws is the proportion by volume of water vapor in the gas
stream, from Equation 5-3, Method 5.
6.6 Conversion Factors.
1 ft /3/ =0.02832 m /3/ 1 hr=60 min
7. Bibliography
1. Shigehara, R. T., A Guideline for Evaluating Compliance Test
Results (Isokinetic Sampling Rate Criterion). U.S. Environmental
Protection Agency, Emission Measurement Branch. Research Triangle Park,
NC. August 1977.
40 CFR 60.748 Pt. 60, App. A, Meth. 15
Introduction
The method described below uses the principle of gas chromatographic
separation and flame photometric detection (FPD). Since there are many
systems or sets of operating conditions that represent useable methods
of determining sulfur emissions, all systems which employ this
principle, but differ only in details of equipment and operation, may be
used as alternative methods, provided that the calibration precision and
sample-line loss criteria are met.
1. Principle and Applicability
1.1 Principle. A gas sample is extracted from the emission source and
diluted with clean dry air. An aliquot of the diluted sample is then
analyzed for hydrogen sulfide (H2S), carbonyl sulfide (COS), and carbon
disulfide (CS2) by gas chromatographic (GC) separation and flame
photometric detection (FPD).
1.2 Applicability. This method is applicable for determination of the
above sulfur compounds from tail gas control units of sulfur recovery
plants.
2. Range and Sensitivity
2.1 Range. Coupled with a gas chromtographic system utilizing a
1-milliliter sample size, the maximum limit of the FPD for each sulfur
compound is approximately 10 ppm. It may be necessary to dilute gas
samples from sulfur recovery plants hundredfold (99:1) resulting in an
upper limit of about 1000 ppm for each compound.
2.2 Sensitivity. The minimum detectable concentration of the FPD is
also dependent on sample size and would be about 0.5 ppm for a 1 ml
sample.
3. Interferences
3.1 Moisture Condensation. Moisture condensation in the sample
delivery system, the analytical column, or the FPD burner block can
cause losses or interferences. This potential is eliminated by heating
the probe, filter box, and conncections, and by maintaining the SO2
scrubber in an ice water bath. Moisture is removed in the SO2 scrubber
and heating the sample beyond this point is not necessary provided the
ambient temperature is above 0 C. Alternatively, moisture may be
eliminated by heating the sample line, and by conditioning the sample
with dry dilution air to lower its dew point below the operating
temperature of the GC/FPD analytical system prior to analysis.
3.2 Carbon Monoxide and Carbon Dioxide. CO and CO2 have substantial
desensitizing effects on the flame photometric detector even after 9:1
dilution. (Acceptable systems must demonstrate that they have eliminated
this interference by some procedure such as eluting CO and CO2 before
any of the sulfur compounds to be measured.) Compliance with this
requirement can be demonstrated by submitting chromatograms of
calibration gases with and without CO2 in the diluent gas. The CO2
level should be approximately 10 percent for the case with CO2 present.
The two chromatograms should show agreement within the precision limits
of Section 4.1.
3.3 Elemental Sulfur. The condensation of sulfur vapor in the
sampling system can lead to blockage of the particulate filter. This
problem can be minimized by observing the filter for buildup and
changing as needed.
3.4 Sulfur Dioxide (SO2). Sulfur dioxide is not a specific
interferent but may be present in such large amounts that it cannot be
effectively separated from the other compounds of interest. The SO2
scrubber described in Section 5.1.3 will effectively remove SO2 from the
sample.
3.5 Alkali Mist. Alkali mist in the emissions of some control
devices may cause a rapid increase in the SO2 scrubber pH to give low
sample recoveries. Replacing the SO2 scrubber contents after each run
will minimize the chances of interference in these cases.
4. Precision
4.1 Calibration Precision. A series of three consecutive injections
of the same calibration gas, at any dilution, shall produce results
which do not vary by more than 13 percent from the mean of the three
injections.
4.2 Calibration Drift. The calibration drift determined from the
mean of three injections made at the beginning and end of any run or
series of runs within a 24-hour period shall not exceed 5 percent.
5. Apparatus
5.1 Sampling (Figure 15-1).
5.1.1 Probe. The probe shall be made of Teflon or Teflon-lined
stainless steel and heated to prevent moisture condensation. It shall
be designed to allow calibration gas to enter the probe at or near the
sample point entry. Any portion of the probe that contacts the stack
gas must be heated to prevent moisture condensation. The probe
described in Section 2.1.1 of Method 16A having a nozzle directed away
from the gas stream is recommended for sources having particulate or
mist emissions. Where very high stack temperatures prohibit the use of
Teflon probe components, glass or quartz-lined probes may serve as
substitutes.
Note. -- Mention of trade names or specific products does not
constitute an endorsement by the Environmental Protection Agency.
5.1.2 Particulate Filter. 50-mm Teflon filter holder and a 1- to
2-micron porosity Teflon filter (available through Savillex Corporation,
5325 Highway 101, Minnetonka, Minnesota 55343). The filter holder must
be maintained in a hot box at a temperature of at least 120 C (248 F).
5.1.3 SO2 Scrubber.
5.1.3.1 Three 300-ml Teflon segment impingers connected in series
with flexible, thick-walled, Teflon tubing. (Impinger parts and tubing
available through Savillex.) The first two impingers contain 100 ml of
citrate buffer, and the third impinger is initially dry. The tip of the
tube inserted into the solution should be constricted to less than 3-mm
( 1/8-in.) ID and should be immersed to a depth of at least 5 cm (2
in.). Immerse the impingers in an ice water bath and maintain near 0 C.
The scrubber solution will normally last for a 3-hour run before
needing replacement. This will depend upon the effects of moisture and
particulate matter on the solution strength and pH.
5.1.3.2 Connections between the probe, particulate filter, and S02
scrubber shall be made of Teflon and as short in length as possible.
All portions of the probe, particulate filter, and connections prior to
the S02 scrubber (or alternative point of moisture removal) shall be
maintained at a temperature of at least 120 C (248 F).
5.1.4 Sample Line. Teflon, no greater than 1.3-cm ( 1/2-in.) ID.
Alternative materials, such as virgin Nylon, may be used provided the
line loss test is acceptable.
5.1.5 Sample Pump. The sample pump shall be a leakless Teflon-coated
diaphragm type or equivalent.
5.2 Dilution System. The dilution system must be constructed such
that all sample contacts are made of Teflon, glass, or stainless-steel.
It must be capable of approximately a 9:1 dilution of the sample.
Insert illustration 0 015
5.3 Gas Chromatograph (Figure 15-2). The gas chromatograph must have
at least the following components:
5.3.1 Oven. Capable of maintaining the separation column at the
proper operating temperature 1 C.
5.3.2 Temperature Gauge. To monitor column oven, detector, and
exhaust temperature 1 C.
5.3.3 Flow System. Gas metering system to measure sample, fuel,
combustion gas, and carrier gas flows.
5.3.4 Flame Photometric Detector.
5.3.4.1 Electrometer. Capable of full scale amplification of linear
ranges of 10^9 to 10^4 amperes full scale.
5.3.4.2 Power Supply. Capable of delivering up to 750 volts.
5.3.4.3 Recorder. Compatible with the output voltage range of the
electrometer.
Insert illustration 0 016
5.3.4.4 Rotary Gas Valves. Multiport Teflon-lined valves equipped
with sample loop. Sample loop volumes shall be chosen to provide the
needed analytical range. Teflon tubing and fittings shall be used
throughout to present an inert surface for sample gas. The gas
chromatograph shall be calibrated with the sample loop used for sample
analysis.
5.4 Gas Chromatograph Columns. The column system must be
demonstrated to be capable of resolving three major reduced sulfur
compounds: H2S, COS, and CS2.
To demonstrate that adequate resolution has been achieved the tester
must submit a chromatogram of a calibration gas containing all three
reduced sulfur compounds in the concentration range of the applicable
standard. Adequate resolution will be defined as base line separation
of adjacent peaks when the amplifier attenuation is set so that the
smaller peak is at least 50 percent of full scale. Base line separation
is defined as a return to zero 5 percent in the interval between peaks.
Systems not meeting this criteria may be considered alternate methods
subject to the approval of the Administrator.
5.5 Calibration System (Figure 15-3). The calibration system must
contain the following components.
5.5.1 Flow System. To measure air flow over permeation tubes within
2 percent. Each flowmeter shall be calibrated after a complete test
series with a wet-test meter. If the flow measuring device differs from
the wet-test meter by more than 5 percent, the completed test shall be
discarded. Alternatively, the tester may elect to use the flow data
that will yield the lowest flow measurement. Calibration with a
wet-test meter before a test is optional. Flow over the permeation
device may also be determined using a soap bubble flowmeter.
5.5.2 Constant Temperature Bath. Device capable of maintaining the
permeation tubes at the calibration temperature within 0.1 C.
5.5.3 Temperature Gauge. Thermometer or equivalent to monitor bath
temperature within 0.1 C.
Insert illustration 0 017
6. Reagents
6.1 Fuel. Hydrogen (H2) prepurified grade or better.
6.2 Combustion Gas. Oxygen (O2) or air, research purity or better.
6.3 Carrier Gas. Prepurified grade or better.
6.4 Diluent. Air containing less than 0.5 ppm total sulfur compounds
and less than 10 ppm each of moisture and total hydrocarbons.
6.5 Calibration Gases. Permeation tubes, one each of H2S, COS, and
CS2, gravimetrically calibrated and certified at some convenient
operating temperature. These tubes consist of hermetically sealed FEP
Teflon tubing in which a liquified gaseous substance is enclosed. The
enclosed gas permeates through the tubing wall at a constant rate. When
the temperature is constant, calibration gases covering a wide range of
known concentrations can be generated by varying and accurately
measuring the flow rate of diluent gas passing over the tubes. These
calibration gases are used to calibrate the GC/FPD system and the
dilution system.
6.6 Citrate Buffer. Dissolve 300 g of potassium citrate and 41 g of
anhydrous citric acid in 1 liter of water. Alternatively, 284 g of
sodium citrate may be substituted for the potassium citrate. Adjust the
pH to between 5.4 and 5.6 with potassium citrate or citric acid, as
required.
6.7 Sample Line Loss Gas (Optional). As an alternative, H2S cylinder
gas may be used for the sample line loss test. The gas shall be
calibrated against permeation devices having known permeation rates or
by the procedure in Section 7 of Method 16A.
7. Pretest Procedures
The following procedures are optional but would be helpful in
preventing any problem which might occur later and invalidate the entire
test.
7.1 After the complete measurement system has been set up at the site
and deemed to be operational, the following procedures should be
completed before sampling is initiated.
7.1.1 Leak Test. Appropriate leak test procedures should be employed
to verify the integrity of all components, sample lines, and
connections. The following leak test procedure is suggested: For
components upstream of the sample pump, attach the probe end of the
sample line to a manometer or vacuum gauge, start the pump and pull
greater than 50 mm (2 in.) Hg vacuum, close off the pump outlet, and
then stop the pump and ascertain that there is no leak for 1 minute.
For components after the pump, apply a slight positive pressure and
check for leaks by applying a liquid (detergent in water, for example)
at each joint. Bubbling indicates the presence of a leak. As an
alternative to the initial leak-test, the sample line loss test
described in Section 10.1 may be performed to verify the integrity of
components.
7.1.2 System Performance. Since the complete system is calibrated
following each test, the precise calibration of each component is not
critical. However, these components should be verified to be operating
properly. This verification can be performed by observing the response
of flowmeters or of the GC output to changes in flow rates or
calibration gas concentrations and ascertaining the response to be
within predicted limits. If any component or the complete system fails
to respond in a normal and predictable manner, the source of the
discrepancy should be identified and corrected before proceeding.
8. Calibration
Prior to any sampling run, calibrate the system using the following
procedures. (If more than one run is performed during any 24-hour
period, a calibration need not be performed prior to the second and any
subsequent runs. The calibration must, however, be verified as
prescribed in Section 10, after the last run made within the 24-hour
period.)
8.1 General Considerations. This section outlines steps to be
followed for use of the GC/FPD and the dilution system. The procedure
does not include detailed instructions because the operation of these
systems is complex, and it requires an understanding of the individual
system being used. Each system should include a written operating
manual describing in detail the operating procedures associated with
each component in the measurement system. In addition, the operator
shuld be familiar with the operating principles of the components;
particularly the GC/FPD. The citations in the Bibliography at the end
of this method are recommended for review for this purpose.
8.2 Calibration Procedure. Insert the permeation tubes into the tube
chamber. Check the bath temperature to assure agreement with the
calibration temperature of the tubes within 0.1 C. Allow 24 hours for
the tubes to equilibrate. Alternatively equilibration may be verified
by injecting samples of calibration gas at 1-hour intervals. The
permeation tubes can be assumed to have reached equilibrium when
consecutive hourly samples agree within the precision limits of Section
4.1.
Vary the amount of air flowing over the tubes to produce the desired
concentrations for calibrating the analytical and dilution systems. The
air flow across the tubes must at all times exceed the flow requirement
of the analytical systems. The concentration in parts per million
generated by a tube containing a specific permeant can be calculated as
follows:
Eq. 15-1
Where:
C=Concentration of permeant produced in ppm.
Pr=Permeation rate of the tube in g/min.
M=Molecular weight of the permeant: g/g-mole.
L=Flow rate, l/min, of air over permeant @ 20 C, 760 mm Hg.
K=Gas constant at 20 C and 760 mm Hg=24.04 l/g mole.
8.3 Calibration of Analysis System. Generate a series of three or
more known concentrations spanning the linear range of the FPD
(approximately 0.5 to 10 ppm for a 1 -- ml sample) for each of the three
major sulfur compounds. Bypassing the dilution system, inject these
standards into the GC/FPD analyzers and monitor the responses. Three
injects for each concentration must yield the precision described in
Section 4.1. Failure to attain this precision is an indication of a
problem in the calibration or analytical system. Any such problem must
be identified and corrected before proceeding.
8.4 Calibration Curves. Plot the GC/FPD response in current
(amperes) versus their causative concentrations in ppm on log-log
coordinate graph paper for each sulfur compound. Alternatively, a least
squares equation may be generated from the calibration data.
Alternatively, a least squares equation may be generated from the
calibration data using concentrations versus the appropriate instrument
response units.
8.5 Calibration of Dilution System. Generate a known concentration
of hydrogen sulfied using the permeation tube system. Adjust the flow
rate of diluent air for the first dilution stage so that the desired
level of dilution is approximated. Inject the diluted calibration gas
into the GC/FPD system and monitor its response. Three injections for
each dilution must yield the precision described in Section 4.1. Failure
to attain this precision in this step is an indication of a problem in
the dilution system. Any such problem must be identified and corrected
before proceeding. Using the calibration data for H2S (developed under
8.3) determine the diluted calibration gas concentration in ppm. Then
calculate the dilution factor as the ratio of the calibration gas
concentration before dilution to the diluted calibration gas
concentration determined under this section. Repeat this procedure for
each stage of dilution required. Alternatively, the GC/FPD system may
be calibrated by generating a series of three or more concentrations of
each sulfur compound and diluting these samples before injecting them
into the GC/FPD system. This data will then serve as the calibration
data for the unknown samples and a separate determination of the
dilution factor will not be necessary. However, the precision
requirements of Section 4.1 are still applicable.
9. Sampling and Analysis Procedure
9.1 Sampling. Insert the sampling probe into the test port making
certain that no dilution air enters the stack through the port. Begin
sampling and dilute the sample approximately 9:1 using the dilution
system. Note that the precise dilution factor is that which is
determined in section 8.5. Condition the entire system with sample for a
minimum of 15 minutes prior to commencing analysis.
9.2 Analysis. Aliquots of diluted sample are injected into the GC/FPD
analyzer for analysis.
9.2.1 Sample Run. A sample run is composed of 16 individual analyses
(injects) performed over a period of not less than 3 hours or more than
6 hours.
9.2.2 Observation for Clogging of Probe or Filter. If reductions in
sample concentrations are observed during a sample run that cannot be
explained by process conditions, the sampling must be interrupted to
determine if the probe or filter is clogged with particulate matter. If
either is found to be clogged, the test must be stopped and the results
up to that point discarded. Testing may resume after cleaning or
replacing the probe and filter. After each run, the probe and filter
shall be inspected and, if necessary, replaced.
10. Post-Test Procedures
10.1 Sample Line Loss. A known concentration of hydrogen sulfide at
the level of the applicable standard, 20 percent, must be introduced
into the sampling system at the opening of the probe in sufficient
quantities to ensure that there is an excess of sample which must be
vented to the atmosphere. The sample must be transported through the
entire sampling system to the measurement system in the normal manner.
The resulting measured concentration should be compared to the known
value to determine the sampling system loss. A sampling system loss of
more than 20 percent is unacceptable. Sampling losses of 0-20 percent
must be corrected by dividing the resulting sample concentration by the
fraction of recovery. The known gas sample may be generated using
permeation tubes. Alternatively, cylinders of hydrogen sulfide mixed in
nitrogen and verified according to Section 6.7 may be used. The
optional pretest procedures provide a good guideline for determining if
there are leaks in the sampling system.
10.2 Recalibration. After each run, or after a series of runs made
within a 24-hour period, perform a partial recalibration using the
procedures in Section 8. Only H2S (or other permeant) need be used to
recalibrate the GC/FPD analysis system (8.3) and the dilution system
(8.5).
10.3 Determination of Calibration Drift. Compare the calibration
curves obtained prior to the runs, to the calibration curves obtained
under Section 10.2. The calibration drift should not exceed the limits
set forth in Section 4.2. If the drift exceeds this limit, the
intervening run or runs should be considered not valid. The tester,
however, may instead have the option of choosing the calibration data
set which would give the highest sample values.
11. Calculations
11.1 Determine the concentrations of each reduced sulfur compound
detected directly from the calibration curves. Alternatively, the
concentrations may be calculated using the equation for the least
squares line.
11.2 Calculation of SO2 Equivalent. SO2 equivalent will be
determined for each analysis made by summing the concentrations of each
reduced sulfur compound resolved during the given analysis.
Eq. 15-2
Where:
SO2 equivalent=The sum of the concentration of each of the measured
compounds (COS, H2S, CS2) expressed as sulfur dioxide in ppm.
H2S=Hydrogen sulfide, ppm.
COS=Carbonyl sulfide, ppm.
CS2=Carbon disulfide, ppm.
d=Dilution factor, dimensionless.
11.3 Average SO2 Equivalent. This is determined using the following
equation. Systems that do not remove moisture from the sample but
conditions the gas to prevent condensation must correct the average SO2
equivalent for the fraction of water vapor present.
where:
Average SO2 equivalent = Average SO2 equivalent in ppm, dry basis.
Average SO2 equivalent i = SO2 in ppm as determined by Equation 15-2.
N = Number of analyses performed.
12. Bibliography
12.1 O'Keeffe, A. E. and G. C. Ortman. ''Primary Standards for
Trace Gas Analysis.'' Anal. Chem. 38,760 (1966).
12.2 Stevens, R. K., A. E. O'Keeffe, and G. C. Ortman. ''Absolute
Calibration of a Flame Photometric Detector to Volatile Sulfur Compounds
at Sub-Part-Per-Million Levels.'' Environmental Science and Technology
3:7 (July 1969).
12.3 Mulik, J. D., R. K. Stevens, and R. Baumgardner. ''An
Analytical System Designed to Measure Multiple Malodorous Compounds
Related to Kraft Mill Activities.'' Presented at the 12th Conference on
Methods in Air Pollution and Industrial Hygiene Studies, University of
Southern California, Los Angeles, CA, April 6-8, 1971.
12.4 Devonald, R. H., R. S. Serenius, and A. D. McIntyre.
''Evaluation of the Flame Photometric Detector for Analysis of Sulfur
Compounds.'' Pulp and Paper Magazine of Canada, 73,3 (March, 1972).
12.5 Grimley, K. W., W. S. Smith, and R. M. Martin. ''The Use of a
Dynamic Dilution System in the Conditioning of Stack Gases for Automated
Analysis by a Mobile Sampling Van.'' Presented at the 63rd Annual APCA
Meeting in St. Louis, MO. June 14-19, 1970.
12.6 General Reference. Standard Methods of Chemical Analysis Volume
III A and B Instrumental Methods. Sixth Edition. Van Nostrand Reinhold
Co.
40 CFR 60.748 Pt. 60, App. A, Meth. 15A
1. Applicability, Principle, Interferences, Precision, and Bias
1.1 Applicability. This method is applicable to the determination of
total reduced sulfur (TRS) emissions from sulfur recovery plants where
the emissions are in a reducing atmosphere, such as in Stretford units.
The lower detectable limit is 0.1 ppm of sulfur dioxide (SO2) when
sampling at 2 liters/min for 3 hours or 0.3 ppm when sampling at 2
liters/min for 1 hour. The upper concentration limit of the method
exceeds TRS levels generally encountered in sulfur recovery plants.
1.2 Principle. An integrated gas sample is extracted from the stack,
and combustion air is added to the oxygen (O2)-deficient gas at a known
rate. The TRS compounds (hydrogen sulfide, carbonyl sulfide, and carbon
disulfide) are thermally oxidized to sulfur dioxide, collected in
hydrogen peroxide as sulfate ion, and then analyzed according to the
Method 6 barium-thorin titration procedure.
1.3 Interferences. Reduced sulfur compounds, other than TRS, that are
present in the emissions will also be oxidized to SO2. For example,
thiophene has been identified in emissions from a Stretford unit and
produced a positive bias of 30 percent in the Method 15A result.
However, these biases may not affect the outcome of the test at units
where emissions are low relative to the standard.
Calcium and aluminum have been shown to interfere in the Method 6
titration procedure. Since these metals have been identified in
particulate matter emissions from Stretford units, a Teflon filter is
required to remove this interference.
Note: Mention of trade name or commercial products in this
publication does not constitute the endorsement or recommendation for
use by the Environmental Protection Agency.
When used to sample emissions containing 7 percent moisture or less,
the midget impingers have sufficient volume to contain the condensate
collected during sampling. Dilution of the H2O2 does not affect the
collection of SO2. At higher moisture contents, the potassium
citrate-citric acid buffer system used with Method 16A should be used to
collect the condensate.
1.4 Precision and bias. Relative standard deviations of 2.8 and 6.9
percent at 41 ppm TRS have been obtained when sampling for 1 and 3
hours, respectively. Results obtained with this method are likely to
contain a positive bias due to the presence of nonregulated sulfur
compounds (that are present in petroleum) in the emissions.
2. Apparatus
2.1 Sampling. The sampling train is shown in Figure 15A-1, and
component parts are discussed below. Modifications to this sampling
train are acceptable provided that the system performance check is met.
Insert illustration 0 031
2.1.1 Probe. 0.6-cm ( 1/4-in.) OD Teflon tubing sequentially wrapped
with heat-resistant fiber strips, a rubberized heating tape (with a plug
at one end), and heat-resistant adhesive tape. A flexible thermocouple
or some other suitable temperature-measuring device shall be placed
between the Teflon tubing and the fiber strips so that the temperature
can be monitored. The probe should be sheathed in stainless steel to
provide in-stack rigidity. A series of bored-out stainless steel
fittings placed at the front of the sheath will prevent flue gas from
entering between the probe and sheath. The sampling probe is depicted
in Figure 15A-2.
insert illus. 0 033
2.1.2 Particulate filter. A 50-mm Teflon filter holder and a 1- to
2-mm porosity Teflon filter (available through Savillex Corporation,
5325 Highway 101, Minnetonka, Minnesota 55345). The filter holder must
be maintained in a hot box at a high enough temperature to prevent
condensation.
2.1.3 Combustion air delivery system. As shown in the schematic
diagram in Figure 15A-3. The rotameter should be selected to measure an
air flow rate of 0.5 liter/min.
insert illus. 0 035
2.1.4 Combustion tube. Quartz glass tubing with an expanded
combustion chamber 2.54 cm (1 in.) in diameter and at least 30.5 cm (12
in.) long. The tube ends should have an outside diameter of 0.6 cm ( 1/4
in.) and be at least 15.3 cm (6 in.) long. This length is necessary to
maintain the quartz-glass connector at ambient temperature and thereby
avoid leaks. Alternatively, the outlet may be constructed with a
90-degree glass elbow and socket that would fit directly onto the inlet
of the first peroxide impinger.
2.1.5 Furnace. Of sufficient size to enclose the combustion tube.
The furnace shall have a temperature regulator capable of maintaining
the temperature at 1100 50 C. The furnace operating temperature shall
be checked with a thermocouple to ensure accuracy. Lindberg furnaces
have been found to be satisfactory.
2.1.6 Peroxide impingers, stopcock grease, thermometer, drying tube,
valve, pump, barometer, and vacuum gauge. Same as in Method 6, Sections
2.1.2, 2.1.4, 2.1.5, 2.1.6, 2.1.7, 2.1.8, 2.1.11, and 2.1.12,
respectively.
2.1.7 Rate meters. Rotameters (or equivalent) capable of measuring
flow rate to within 5 percent of the selected flow rate and calibrated
as in Section 5.2.
2.1.8 Volume meter. Dry gas meter capable of measuring the sample
volume under the particular sampling conditions with an accuracy of 2
percent.
2.1.9 U-tube manometer. To measure the pressure at the exit of the
combustion gas dry gas meter.
2.2 Sample recovery and analysis. Same as in Method 6, Sections 2.2
and 2.3, except a 10-ml buret with 0.05-ml graduations is required for
titrant volumes of less than 10.0 ml, and the spectrophotometer is not
needed.
3. Reagents
Unless otherwise indicated, all reagents must conform to the
specifications established by the Committee on Analytical Reagents of
the American Chemical Society. When such specifications are not
available, the best available grade shall be used.
3.1 Sampling. The following reagents are needed:
3.1.1 Water. Same as in Method 6, Section 3.1.1.
3.1.2 Hydrogen peroxide, 3 percent. Same as in Method 6, Section
3.1.5 (40 ml is needed per sample).
3.1.3 Recovery check gas. Carbonyl sulfide (COS) in nitrogen (100
ppm or greater, if necessary) in an aluminum cylinder. Verify the
concentration by gas chromatography where the instrument is calibrated
with a COS permeation tube.
3.1.4 Combustion gas. Air, contained in a gas cylinder equipped with
a two-stage regulator. The gas should contain less than 50 ppb of
reduced sulfur compounds and less than 10 ppm total hydrocarbons.
3.2 Sample recovery and analysis. Same as in Method 6, Sections 3.2
and 3.3.
4. Procedure
4.1 Sampling. Before any source sampling is done, conduct two
30-minute system performance checks in the field, as detailed in Section
4.3, to validate the sampling train components and procedures
(optional).
4.1.1 Preparation of sampling train. For the Method 6 part of the
train, measure 20 ml of 3 percent hydrogen peroxide into the first and
second midget impingers. Leave the third midget impinger empty and add
silica gel to the fourth impinger. Alternatively, a silica gel drying
tube may be used in place of the fourth impinger. Place crushed ice and
water around all impingers. Maintain the oxidation furnace at 1100 50
C to ensure 100 percent oxidation of COS. Maintain the probe and filter
temperatures at a high enough level (no visible condensation) to prevent
moisture condensation and monitor the temperatures with a thermocouple.
4.1.2 Leak-check procedure. Assemble the sampling train and
leak-check as described in Method 6, Section 4.1.2. Include the
combustion air delivery system from the needle valve forward in the
leak-check.
4.1.3 Sample collection. Adjust the pressure on the second stage of
the regulator on the combustion air cylinder to 10 psig. Adjust the
combustion air flow rate to 0.50 liter/min ( 10 percent) before
injecting combustion air into the sampling train. Then inject
combustion air into the sampling train, start the sample pump, and open
the stack sample gas valve. Carry out these three operations within 15
to 30 seconds to avoid pressurizing the sampling train. Adjust the
total sample flow rate to 2.0 liters/min ( 10 percent). The combustion
air flow rate of 0.50 liter/min and the total sample flow rate of 2.0
liters/min produce an 02 concentration of 5.0 percent in the stack gas.
This 02 concentration must be maintained constantly to allow oxidation
of TRS to SO2. Adjust these flow rates during sampling as necessary.
Monitor and record the combustion air manometer reading at regular
intervals during the sampling period. Sample for 1 or 3 hours. At the
end of sampling, turn off the sample pump and combustion air
simultaneously (within 15 to 30 seconds of each other). All other
procedures are the same as in Method 6, Section 4.1.3, except that the
sampling train should not be purged. After collecting the sample,
remove the probe from the stack and conduct a leak-check (mandatory).
After each 3-hour test run (or after three 1-hour samples), conduct
one system performance check (see Section 4.3). After this system
performance check and before the next test run, it is recommended that
the probe be rinsed and brushed and the filter replaced.
In Method 15, a test run is composed of 16 individual analyses
(injects) performed over a period of not less than 3 hours or more than
6 hours. For Method 15A to be consistent with Method 15, the following
may be used to obtain a test run: (1) Collect three 60-minute samples
or (2) collect one 3-hour sample. (Three test runs constitute a test.)
4.2 Sample recovery. Recover the hydrogen peroxide-containing
impingers as detailed in Method 6, Section 4.2.
4.3 System performance check. A system performance check is done (1)
to validate the sampling train components and procedure (before testing,
optional) and (2) to validate a test run (after a run). Perform a check
in the field before testing consisting of at least two samples
(optional), and perform an additional check after each 3-hour run or
after three 1-hour samples (mandatory).
The checks involve sampling a known concentration of COS and
comparing the analyzed concentration with the known concentration. Mix
the recovery gas with N2 as shown in Figure 15A-4 if dilution is
required. Adjust the flow rates to generate a COS concentration in the
range of the stack gas or within 20 percent of the applicable standard
at a total flow rate of at least 2.5 liters/min. Use Equation 15A-4 to
calculate the concentration of recovery gas generated. Calibrate the
flow rate from both sources with a soap bubble flow tube so that the
diluted concentration of COS can be accurately calculated. Collect
30-minute samples, and analyze in the normal manner. Collect the
samples through the probe of the sampling train using a manifold or some
other suitable device that will ensure extraction of a representative
sample.
Insert illus. 0 041
The recovery check must be performed in the field before replacing
the particulate filter and before cleaning the probe. A sample recovery
of 100 20 percent must be obtained for the data to be valid and should
be reported with the emission data, but should not be used to correct
the data. However, if the performance check results do not affect the
compliance or noncompliance status of the affected facility, the
Administrator may decide to accept the results of the compliance test.
Use Equation 15A-5 to calculate the recovery efficiency.
4.4 Sample analysis. Same as in Method 6, Section 4.3. For
compliance tests only, an EPA SO2 field audit sample shall be analyzed
with each set of samples. Such audit samples are available from the
Quality Assurance Division, Environmental Monitoring Systems Laboratory,
U.S. Environmental Protection Agency, Research Triangle Park, NC 27711.
5. Calibration.
5.1 Metering system, thermometers, barometer, and barium perchlorate
solution. Calibration procedures are presented in Method 6, Sections
5.1, 5.2, 5.4, and 5.5.
5.2 Rotameters. Calibrate with a bubble flow tube.
6. Calculations.
In the calculations, retain at least one extra decimal figure beyond
that of the acquired data. Round off figures after final calculations.
6.1 Nomenclature.
CTRS=Concentration of TRS as SO2, dry basis, corrected to standard
conditions, ppm.
N=Normality of barium perchlorate titrant, milliequivalents/ml.
Pbar=Barometric pressure at exit orifice of the dry gas meter, mm Hg.
Pstd=Standard absolute pressure, 760 mm Hg.
Tm=Average dry gas meter absolute temperature, .
Tstd=Standard absolute temperature, 293 .
Va=Volume of sample aliquot titrated, ml.
Vms=Dry gas volume as measured by the sample train dry gas meter,
liters.
Vmc=Dry gas volume as measured by the combustion air dry gas meter,
liters.
Vms(std)=Dry gas volume measured by the sample train dry gas meter,
corrected to standard conditions, liters.
Vmc(std)=Dry gas volume measured by the combustion air dry gas meter,
corrected to standard conditions, liters.
Vsoln=Total volume of solution in which the sulfur dioxide sample is
contained, 100 ml.
Vt=Volume of barium perchlorate titrant used for the sample (average
of replicate titrations), ml.
Vtb=Volume of barium perchlorate titrant used for the blank, ml.
Y=Calibration factor for sampling train dry gas meter.
Yc=Calibration factor for combustion air dry gas meter.
CRG=Concentration of generated recovery gas, ppm.
CCOS=Concentration of COS recovery gas, ppm.
QCOS=Flow rate of COS recovery gas, liters/min.
QN =Flow rate of diluent N2, liters/min.
R=Recovery efficiency for the system performance check, percent.
32.03=Equivalent weight of sulfur dioxide, mg/meq.
6.2 Dry Sample Gas Volume, Corrected to Standard Conditions.
Eq. 15A-1
where: K1=0.3858 K/mm Hg for metric units.
6.3 Combustion Air Gas Volume, Gorrected to Standard Conditions.
Note: Correct Pbar for the average pressure of the manometer during
the sampling period.
6.4 Concentration of TRS as ppm SO2.
where: K2=12025 ml/meq for metric units.
6.5 Concentration of Generated Recovery Gas.
6.6 Recovery Efficiency.
7. Bibliography
1. American Society for Testing and Materials
Annual Book of ASTM Standards. Part 31: Water, Atmospheric
Analysis. Philadelphia, Pennsylvania. 1974. p. 40-42.
2. Blosser, R.O., H.S. Oglesby, and A.K. Jain
A Study of Alternate SO2 Scrubber Designs Used for TRS Monitoring.
National Council of the Paper Industry for Air and Stream Improvement,
Inc., New York, New York. Special Report 77-05. July 1977.
3. Curtis, F., and G.D. McAlister
Development and Evaluation of an Oxidation/Method 6 TRS Emission
Sampling Procedure. Emission Measurement Branch, Emission Standards and
Engineering Division, U.S. Environmental Protection Agency, Research
Triangle Park, North Carolina 27711. February 1980.
4. Gellman, I.
A Laboratory and Field Study of Reduced Sulfur Sampling and
Monitoring Systems.
National Council of the Paper Industry for Air and Stream
Improvement, Inc., New York, New York. Atmospheric Quality Improvement
Technical Bulletin No. 81. October 1975.
5. Margeson, J.H., J.E. Knoll, M.R. Midgett, B.B. Ferguson, and P.J.
Schworer
A Manual Method for TRS Determination. Journal of Air Pollution
Control Association. 35:1280-1286. December 1985.
40 CFR 60.748 Pt. 60, App. A, Meth. 16
Introduction
The method described below uses the principle of gas chromatographic
separation and flame photometric detection (FPD). Since there are many
systems or sets of operating conditions that represent useable methods
of determining sulfur emissions, all systems which employ this
principle, but differ only in details of equipment and operation, may be
used as alternative methods, provided that the calibration precision and
sample line loss criteria are met.
1. Principle and Applicability
1.1 Principle. A gas sample is extracted from the emission source and
an aliquot is analyzed for hydrogen sulfide (H2S), methyl mercaptan
(MeSH), dimethly sulfide (DMS), and dimethyl disulfide (DMDS) by gas
chromatographic (GC) separation and flame photometric detection (FPD).
These four compounds are know collectively as total reduced sulfur
(TRS).
1.2 Applicability. This method is applicable for determination of TRS
compounds from recovery furnaces, lime kilns, and smelt dissolving tanks
at kraft pulp mills.
2. Range and Sensitivity
2.1 Range. The analytical range will vary with the sample loop size.
Typically, the analytical range may extend from 0.1 to 100 ppm using 10
to 0.1-ml sample loop sizes. This eliminates the need for sample
dilution in most cases.
2.2 Sensitivity. Using the 10-ml sample size, the minimum detectable
concentration is approximately 50 ppb.
3. Interferences
3.1 Moisture Condensation. Moisture condensation in the sample
delivery system, the analytical column, or the FPD burner block can
cause losses or interferences. This is prevented by maintaining the
probe, filter box, and connections at a temperature of at least 120 C
(248 F). Moisture is removed in the SO2 scrubber and heating the sample
beyond this point is not necessary provided the ambient temperature is
above 0 C. Alternatively, moisture may be eliminated by heating the
sample line, and by conditioning the sample with dry dilution air to
lower its dew point below the operating temperature of the GC/FPD
analytical system prior to analysis.
3.2 Carbon Monoxide and Carbon Dioxide. CO and CO2 have a
substantial desensitizing effect on the flame photometric detector even
after dilution. Acceptable systems must demonstrate that they have
eliminated this interference by some procedure such as eluting these
compounds before any of the compounds to be measured. Compliance with
this requirement can be demonstrated by submitting chromatograms of
calibration gases with and without CO2 in the diluent gas. The CO2
level should be approximately 10 percent for the case with CO2 present.
The two chromatograms should show agreement within the precision limits
of Section 4.1.
3.3 Particulate Matter. Particulate matter in gas samples can cause
interference by eventual clogging of the analytical system. This
interference is eliminated by using the Teflon filter after the probe.
3.4 Sulfur Dioxide (SO2). Sulfur dioxide is not a specific
interferent but may be present in such large amounts that it cannot be
effectively separated from the other compounds of interest. The SO2
scrubber described in Section 5.1.3 will effectively remove SO2 from the
sample.
4. Precision and Accuracy
4.1 GC/FPD Calibration Precision. A series of three consecutive
injections of the same calibration gas, at any dilution, shall produce
results which do not vary by more than 5 percent from the mean of the
three injections.
4.2 Calibration Drift. The calibration drift determined from the
mean of three injections made at the beginning and end of any run or
series of runs within a 24-hour period shall not exceed 5 percent.
4.3 System Calibration Accuracy. Losses through the sample transport
system must be measured and a correction factor developed to adjust the
calibration accuracy to 100 percent.
5. Apparatus
5.1. Sampling.
5.1.1 Probe.
Insert illus. 1209
5.1.1.1 Teflon or Teflon-lined stainless steel. The probe must be
heated to prevent moisture condensation. It shall be designed to allow
calibration gas to enter the probe at or near the sample point entry.
Any portion of the probe that contacts the stack gas must be heated to
prevent moisture condensation.
5.1.1.2 Figure 16-1 illustrates the probe used in lime kilns and
other sources where significant amounts of particulate matter are
present. The probe is designed with the deflector shield placed between
the sample and the gas inlet holes to reduce clogging of the filter and
possible adsorption of sample gas. As an alternative, the probe
described in Section 2.1.1 of Methods 16A having a nozzle directed away
from the gas stream may be used at sources having significant amounts of
particulate matter.
5.1.1.3 Note: Mention of trade names or specific products does not
constitute an endorsement by the Environmental Protection Agency.
5.1.2 Particulate Filter. 50-mm Teflon filter holder and a 1- to
2-micron porosity Teflon filter (available through Savillex Corporation,
5325 Highway 101, Minnetonka, Minnesota 55343). The filter holder must
be maintained in a hot box at a temperature of at least 120 C (248 F).
5.1.3 SO2 Scrubber.
5.1.3.1 Three 300-ml Teflon segmented impingers connected in series
with flexible, thick-walled, Teflon tubing. (Impinger parts and tubing
available through Savillex.) The first two impingers contain 100 ml of
citrate buffer and the third impinger is initially dry. The tip of the
tube inserted into the solution should be constricted to less than 3-mm
( 1/8-in.) ID and should be immersed to a depth of at least 5 cm (2
in.). Immerse the impingers in an ice water bath and maintain near 0 C.
The scrubber solution will normally last for a 3-hour run before
needing replacement. This will depend upon the effects of moisture and
particulate matter on the solution strength and pH.
5.1.3.2 Connections between the probe, particulate filter, and SO2
scrubber shall be made of Teflon and as short in length as possible.
All portions of the probe, particulate filter, and connections prior to
the SO2 scrubber (or alternative point of moisture removal) shall be
maintained at a temperature of at least 120 C (248 F).
5.1.4 Sample Line. Teflon, no greater than 1.3-cm ( 1/2-in.) ID.
Alternative materials, such as virgin Nylon, may be used provided the
line loss test is acceptable.
5.1.5 Sample Pump. The sample pump shall be leakless Teflon-coated
diaphragm type or equivalent.
5.2 Dilution System. Needed only for high sample concentrations.
The dilution system must be constructed such that all sample contacts
are made of Teflon, glass, or stainless steel.
5.3 Gas Chromatograph. The gas chromatograph must have at least the
following components:
5.3.1 Oven. Capable of maintaining the separation column at the
proper operating temperature 1 C.
5.3.2 Temperature Gauge. To monitor column oven, detector, and
exhaust temperature 1 C.
5.3.3 Flow System. Gas metering system to measure sample, fuel,
combustion gas, and carrier gas flows.
5.3.4 Flame Photometric Detector.
5.3.4.1 Electrometer. Capable of full scale amplification of linear
ranges of 10^9 to 10^4 amperes full scale.
5.3.4.2 Power Supply. Capable of delivering up to 750 volts.
5.3.4.3 Recorder. Compatible with the output voltage range of the
electrometer.
5.3.4.4 Rotary Gas Valves. Multiport Teflon-lined valves equipped
with sample loop. Sample loop volumes shall be chosen to provide the
needed analytical range. Teflon tubing and fittings shall be used
throughout to present an inert surface for sample gas. The gas
chromatograph shall be calibrated with the sample loop used for sample
analysis.
5.4 Gas Chromatogram Columns. The column system must be demonstrated
to be capable of resolving the four major reduced sulfur compounds:
H2S, MeSH, DMS, and DMDS. It must also demonstrate freedom from known
interferences.
To demonstrate that adequate resolution has been achieved, the tester
must submit a chromatogram of a calibration gas containing all four of
the TRS compounds in the concentration range of the applicable standard.
Adequate resolution will be defined as base line separation of adjacent
peaks when the amplifier attenuation is set so that the smaller peak is
at least 50 percent of full scale. Baseline separation is defined as a
return to zero 5 percent in the interval between peaks. Systems not
meeting this criteria may be considered alternate methods subject to the
approval of the Administrator.
5.5 Calibration System. The calibration system must contain the
following components. (Figure 16-2)
5.5.1 Tube Chamber. Chamber of glass or Teflon of sufficient
dimensions to house permeation tubes.
5.5.2 Flow System. To measure air flow over permeation tubes at 2
percent. Each flowmeter shall be calibrated after a complete test
series with a wet test meter. If the flow measuring device differs from
the wet test meter by 5 percent, the completed test shall be discarded.
Alternatively, the tester may elect to use the flow data that would
yield the lower flow measurement. Calibration with a wet test meter
before a test is optional. Flow over the permeation device may also be
determined using a soap bubble flowmeter.
5.5.3 Constant Temperature Bath. Device capable of maintaining the
permeation tubes at the calibration temperature within 0.1 C.
5.5.4 Temperature Gauge. Thermometer or equivalent to monitor bath
temperature within 1 C.
6. Reagents
6.1 Fuel. Hydrogen (H2), prepurified grade or better.
6.2 Combustion Gas. Oxygen (O2) or air, research purity or better.
6.3 Carrier Gas. Prepurified grade or better.
6.4 Diluent (If required). Air containing less than 50 ppb total
sulfur compounds and less than 10 ppm each of moisture and total
hydrocarbons.
6.5 Calibration Gases. Permeation tubes, one each of H2S, MeSH, DMS,
and DMDS, gravimetrically calibrated and certified at some convenient
operating temperature. These tubes consist of hermetically sealed FEP
Teflon tubing in which a liquified gaseous substance is enclosed. The
enclosed gas permeates through the tubing wall at a constant rate. When
the temperature is constant, calibration gases covering a wide range of
known concentrations can be generated by varying and accurately
measuring the flow rate of diluent gas passing over the tubes. These
calibration gases are used to calibrate the GC/FPD system and the
dilution system.
6.6 Citrate Buffer. Dissolve 300 grams of potassium citrate and 41
grams of anhydrous citric acid in 1 liter of deionized water. 284 grams
of sodium citrate may be substituted for the potassium citrate. Adjust
the pH to between 5.4 and 5.6 with potassium citrate or citric acid, as
required.
6.7 Sample Line Loss Gas (Optional). As an alternative to permeation
gas, H2S cylinder gas may be used for the sample line loss test. The
gas shall be calibrated against permeation devices having known
permeation rates or by the procedure in Section 7 of Method 16A.
7. Pretest Procedures
The following procedures are optional but would be helpful in
preventing any problem which might occur later and invalidate the entire
test.
7.1 After the complete measurement system has been set up at the site
and deemed to be operational, the following procedures should be
completed before sampling is initiated.
7.1.1 Leak Test. Appropriate leak test procedures should be employed
to verify the integrity of all components, sample lines, and
connections. The following leak test procedure is suggested: For
components upstream of the sample pump, attach the probe end of the
sample line to a manometer or vacuum gauge, start the pump and pull
greater than 50 mm (2 in.) Hg vacuum, close off the pump outlet, and
then stop the pump and ascertain that there is no leak for 1 minute.
For components after the pump, apply a slight positive pressure and
check for leaks by applying a liquid (detergent in water, for example)
at each joint. Bubbling indicates the presence of a leak. As an
alternative to the initial leak-test, the sample line loss test
described in Section 10.1 may be performed to verify the integrity of
components.
7.1.2 System Performance. Since the complete system is calibrated
following each test, the precise calibration of each component is not
critical. However, these components should be verified to be operating
properly. This verification can be performed by observing the response
of flowmeters or of the GC output to changes in flow rates or
calibration gas concentrations and ascertaining the response to be
within predicted limits. In any component, or if the complete system
fails to respond in a normal and predictable manner, the source of the
discrepancy should be identified and corrected before proceeding.
8. Calibration
Prior to any sampling run, calibrate the system using the following
procedures. (If more than one run is performed during any 24-hour
period, a calibration need not be performed prior to the second and any
subsequent runs. The calibration must, however, be verified as
prescribed in Section 10, after the last run made within the 24-hour
period.)
8.1 General Considerations. This section outlines steps to be
followed for use of the GC/FPD and the dilution system (if applicable).
The procedure does not include detailed instructions because the
operation of these systems is complex, and it requires an understanding
of the individual system being used. Each system should include a
written operating manual describing in detail the operating procedures
associated with each component in the measurement system. In addition,
the operator should be familiar with the operating principles of the
components, particularly the GC/FPD. The citations in the Bibliography
at the end of this method are recommended for review for this purpose.
8.2 Calibration Procedure. Insert the permeation tubes into the tube
chamber. Check the bath temperature to assure agreement with the
calibration temperature of the tubes within 0.1 C. Allow 24 hours for
the tubes to equilibrate. Alternatively equilibration may be verified
by injecting samples of calibration gas at 1-hour intervals. The
permeation tubes can be assumed to have reached equilibrium when
consecutive hourly samples agree within the precision limits of Section
4.1.
Vary the amount of air flowing over the tubes to produce the desired
concentrations for calibrating the analytical and dilution systems. The
air flow across the tubes must at all times exceed the flow requirement
of the analytical systems. The concentration in parts per million
generated by a tube containing a specific permeant can be calculated as
follows:
Eq. 16-1
Where:
C=Concentration of permeant produced in ppm.
Pr=Permeation rate of the tube in g/min.
M=Molecular weight of the permeant (g/g-mole).
L=Flow rate, 1/min, of air over permeant @ 20 C, 760 mm Hg.
K=Gas constant at 20 C and 760 mm Hg=24.04 1/g mole.
8.3 Calibration of Analysis System. Generate a series of three or
more known concentrations spanning the linear range of the FPD
(approximately 0.5 to 10 ppm for a 1-ml sample) for each of the four
major sulfur compounds. Inject these standards into the GC/FPD analyzer
and monitor the responses. Three injects for each concentration must
not vary by more than 5 percent from the mean of the three injections.
Failure to attain this precision is an indication of a problem in the
calibration or analytical system. Any such problem must be identified
and corrected before proceeding.
8.4 Calibration Curves. Plot the GC/FPD response in current
(amperes) versus their causative concentrations in ppm on log-log
coordinate graph paper for each sulfur compound. Alternatively, a least
squares equation may be generated from the calibration data.
Alternatively, a least squares equation may be generated from the
calibration data using concentrations versus the appropriate instrument
response units.
9. Sampling and Analysis Procedure
9.1 Sampling. Insert the sampling probe into the test port making
certain that no dilution air enters the stack through the port. Begin
sampling. Condition the entire system with sample for a minimum of 15
minutes prior to commencing analysis.
9.2 Analysis. Aliquots of sample are injected into the GC/FPD
analyzer for analysis.
9.2.1 Sample Run. A sample run is composed of 16 individual analyses
(injects) performed over a period of not less than 3 hours or more than
6 hours.
9.2.2 Observation for Clogging of Probe or Filter. If reductions in
sample concentrations are observed during a sample run that cannot be
explained by process conditions, the sampling must be interrupted to
determine if the probe or filter is clogged with particulate matter. If
either is found to be clogged, the test must be stopped and the results
up to that point discarded. Testing may resume after cleaning or
replacing the probe and filter. After each run, the probe and filter
shall be inspected and, if necessary, replaced.
10. Post-Test Procedures
10.1 Sample line loss. A known concentration of hydrogen sulfide at
the level of the applicable standard, 20 percent, must be introduced
into the sampling system at the opening of the probe in sufficient
quantities to ensure that there is an excess of sample which must be
vented to the atmosphere. The sample must be transported through the
entire sampling system to the measurement system in the normal manner.
(See figure 16-1). The resulting measured concentration should be
compared to the known value to determine the sampling system loss.
For sampling losses greater than 20 percent in a sample run, the
sample run is not to be used when determining the arithmetic mean of the
performance test. For sampling losses of 0-20 percent, the sample
concentration must be corrected by dividing the sample concentration by
the fraction of recovery. The fraction of recovery is equal to one
minus the ratio of the measured concentration to the known concentration
of hydrogen sulfide in the sample line loss procedure. The known gas
sample may be generated using permeation tubes. Alternatively,
cylinders of hydrogen sulfide mixed in nitrogen and certified according
to section 6.7 may be used. The optional pretest procedures provide a
good guideline for determining if there are leaks in the sampling
system.
Insert illus. 1210
10.2 Recalibration. After each run, or after a series of runs made
within a 24-hour period, perform a partial recalibration using the
procedures in Section 8. Only H2S (or other calibration gas) need be
used to recalibrate the GC/FPD analysis system (Section 8.3).
10.3 Determination of Calibration Drift. Compare the calibration
curves obtained prior to the runs, to the calibration curves obtained
under Section 10.2. The calibration drift should not exceed the limits
set forth in Section 4.2. If the drift exceeds this limit, the
intervening run or runs should be considered not valid. The tester,
however, may instead have the option of choosing the calibration data
set which would give the highest sample values.
11. Calculations
11.1 Determine the concentrations of each reduced sulfur compound
detected directly from the calibration curves. Alternatively, the
concentrations may be calculated using the equation for the least
squares line.
11.2 Calculation of TRS. Total reduced sulfur will be determined for
each analysis made by summing the concentrations of each reduced sulfur
compound resolved during a given analysis.
Eq. 16-2
Where:
TRS=Total reduced sulfur in ppm, dry basis.
H2S=Hydrogen sulfide, ppm.
MeSH=Methyl mercaptan, ppm.
DMS=Dimethyl sulfide, ppm.
DMDS=Dimethyl disulfide, ppm.
d=Dilution factor, dimensionless.
11.3 Average TRS. The average TRS will be determined as follows:
Where:
Average TRS=Average total reduced sulfur in ppm, dry basis.
TRSi=Total reduced sulfur in ppm as determined by Equation 16-2.
N=Number of samples.
Bwo=Fraction of volume of water vapor in the gas stream as determined
by reference Method 4 -- Determination of Moisture in Stack Gases.
11.4 Average Concentration of Individual Reduced Sulfur Compounds.
Where:
Si=Concentration of any reduced sulfur compound from the ith sample
injection, ppm.
C=Average concentration of any one of the reduced sulfur compounds
for the entire run, ppm.
N=Number of injections in any run period.
12. Bibliography
12.1 O'Keeffe, A. E. and G. C. Ortman. ''Primary Standards for
Trace Gas Analysis.'' Analytical Chemical Journal, 38,760 (1966).
12.2 Stevens, R. K., A. E. O'Keeffe, and G. C. Ortman. ''Absolute
Calibration of a Flame Photometric Detector to Volatile Sulfur Compounds
at Sub-Part-Per-Million Levels.'' Environmental Science and Technology,
3:7 (July, 1969).
12.3 Mulik, J. D., R. K. Stevens, and R. Baumgardner. ''An
Analytical System Designed to Measure Multiple Malodorous Compounds
Related to Kraft Mill Activities.'' Presented at the 12th Conference on
Methods in Air Pollution and Industrial Hygiene Studies, University of
Southern California, Los Angeles, CA. April 6-8, 1971.
12.4 Devonald, R. H., R. S. Serenius, and A. D. McIntyre.
''Evaluation of the Flame Photometric Detector for Analysis of Sulfur
Compounds.'' Pulp and Paper Magazine of Canada, 73,3 (March, 1972).
12.5 Grimley, K. W., W. S. Smith, and R. M. Martin. ''The Use of a
Dynamic Dilution System in the Conditioning of Stack Gases for Automated
Analysis by a Mobile Sampling Van.'' Presented at the 63rd Annual APCA
Meeting in St. Louis, MO. June 14-19, 1970.
12.6 General Reference. Standard Methods of Chemical Analysis Volume
III A and B Instrumental Methods. Sixth Edition. Van Nostrand Reinhold
Co.
40 CFR 60.748 Pt. 60, App. A, Meth. 16A
1. Applicability, Principle, Interferences, Precision, and Bias
1.1 Applicability. This method is applicable to the determination of
total reduced sulfur (TRS) emissions from recovery boilers, lime kilns,
and smelt dissolving tanks at kraft pulp mills, and from other sources
when specified in an applicable subpart of the regulations. The TRS
compounds include hydrogen sulfide, methyl mercaptan, dimethyl sulfide,
and dimethyl disulfide.
The flue gas must contain at least 1 percent oxygen for complete
oxidation of all TRS to sulfur dioxide (SO2). The lower detectable
limit is 0.1 ppm SO2 when sampling at 2 liters/min for 3 hours or 0.3
ppm when sampling at 2 liters/min for 1 hour. The upper concentration
limit of the method exceeds TRS levels generally encountered at kraft
pulp mills.
1.2 Principle. An integrated gas sample is extracted from the stack.
SO2 is removed selectively from the sample using a citrate buffer
solution. TRS compounds are then thermally oxidized to SO2, collected
in hydrogen peroxide as sulfate, and analyzed by the Method 6
barium-thorin titration procedure.
1.3 Interferences. TRS compounds other than those regulated by the
emission standards, if present, may be measured by this method.
Therefore, carbonyl sulfide, which is partially oxidized to SO2 and may
be present in a lime kiln exit stack, would be a positive interferent.
Particulate matter from the lime kiln stack gas (primarily calcium
carbonate) can cause a negative bias if it is allowed to enter the
citrate scrubber; the particulate matter will cause the pH to rise and
H2S to be absorbed prior to oxidation. Furthermore, if the calcium
carbonate enters the hydrogen peroxide impingers, the calcium will
precipitate sulfate ion. Proper use of the particulate filter described
in Section 2.1.3 will eliminate this interference.
1.4 Precision and Bias. Relative standard deviations of 2.0 and 2.6
percent were obtained when sampling a recovery boiler for 1 and 3 hours,
respectively.
In a separate study at a recovery boiler, Method 16A was found to be
unbiased relative to Method 16. Comparison of Method 16A with Method 16
at a lime kiln indicated that there was no bias in Method 16A. However,
instability of the source emissions adversely affected the comparison.
The precision of Method 16A at the lime kiln was similar to that
obtained at the recovery boiler.
Relative standard deviations of 2.7 and 7.7 percent have been
obtained for system performance checks.
2. Apparatus
2.1 Sampling. The sampling train is shown in Figure 16A-1 and
component parts are discussed below. Modifications to this sampling
train are acceptable provided the system performance check (Section 4.3)
is met.
insert illus 0324
2.1.1 Probe. Teflon (mention of trade names or specific products does
not constitute endorsement by the U.S. Environmental Protection Agency)
tubing, 0.6-cm ( 1/4-in.) diameter, sequentially wrapped with
heat-resistant fiber strips, a rubberized heat tape (plug at one end),
and heat-resistant adhesive tape. A flexible thermocouple or other
suitable temperature measuring device should be placed between the
Teflon tubing and the fiber strips so that the temperature can be
monitored to prevent softening of the probe. The probe should be
sheathed in stainless steel to provide in-stack rigidity. A series of
bored-out stainless steel fittings placed at the front of the sheath
will prevent moisture and particulate from entering between the probe
and sheath. A 0.6-cm ( 1/4-in.) Teflon elbow (bored out) should be
attached to the inlet of the probe, and a 2.54-cm (1-in.) piece of
Teflon tubing should be attached at the open end of the elbow to permit
the opening of the probe to be turned away from the particulate stream;
this will reduce the amount of particulate drawn into the sampling
train. The sampling probe is depicted in Figure 16A-2.
insert illus. 0326
2.1.2 Probe Brush. Nylon bristle brush with handle inserted into a
3.2-mm ( 1/8-in.) Teflon tubing. The Teflon tubing should be long
enough to pass the brush through the length of the probe.
2.1.3 Particulate Filter. 50-mm Teflon filter holder and a 1- to 2-m
porosity, Teflon filter (available through Savillex Corporation, 5325
Highway 101, Minnetonka, Minnesota 55343). The filter holder must be
maintained in a hot box at a temperature sufficient to prevent moisture
condensation. A temperature of 121 C (250 F) was found to be
sufficient when testing a lime kiln under sub-freezing ambient
conditions.
2.1.4 SO2 Scrubber. Three 300-ml Teflon segmented impingers
connected in series with flexible, thick-walled, Teflon tubing.
(Impinger parts and tubing available through Savillex.) The first two
impingers contain 100 ml of citrate buffer and the third impinger is
initially dry. The tip of the tube inserted into the solution should be
constricted to less than 3 mm ( 1/8 in.) ID and should be immersed to a
depth of at least 5 cm (2 in.).
2.1.5 Combustion Tube. Quartz glass tubing with an expanded
combustion chamber 2.54 cm (1 in.) in diameter and at least 30.5 cm (12
in.) long. The tube ends should have an outside diameter of 0.6 cm ( 1/4
in.) and be at least 15.3 cm (6 in.) long. This length is necessary to
maintain the quartz-glass connector at ambient temperature and thereby
avoid leaks. Alternatively, the outlet may be constructed with a
90-degree glass elbow and socket that would fit directly onto the inlet
of the first peroxide impinger.
2.1.6 Furnace. A furnace of sufficient size to enclose the combustion
chamber of the combustion tube with a temperature regulator capable of
maintaining the temperature at 800 100 C. The furnace operating
temperature should be checked with a thermocouple to ensure accuracy.
2.1.7 Peroxide Impingers, Stopcock Grease, Thermometer, Drying Tube,
Valve, Pump, Barometer, and Vacuum Gauge. Same as in Method 6, Sections
2.1.2, 2.1.4, 2.1.6, 2.1.7, 2.1.8, 2.1.11, and 2.1.12, respectively.
2.1.8 Rate Meter. Rotameter, or equivalent, accurate to within 5
percent at the selected flow rate of 2 liters/min.
2.1.9 Volume Meter. Dry gas meter capable of measuring the sample
volume under the sampling conditions of 2 liters/min with an accuracy of
2 percent.
2.1.10 Polyethylene Bottles. 250-ml bottles for hydrogen peroxide
solution recovery.
2.2 Sample Preparation and Analysis. Same as in Method 6, Section
2.3, except a 10-ml buret with 0.05-ml graduations is required and the
spectrophotometer is not needed.
3. Reagents
Unless otherwise indicated, all reagents must conform to the
specifications established by the Committee on Analytical Reagents of
the American Chemical Society. When such specifications are not
available, the best available grade shall be used.
3.1 Sampling. The following reagents are needed:
3.1.1 Water. Same as in Method 6, Section 3.1.1.
3.1.2 Citrate Buffer. 300 g of potassium citrate (or 284 g of sodium
citrate) and 41 g of anhydrous citric acid dissolved in 1 liter of water
(200 ml is needed per test). Adjust the pH to between 5.4 and 5.6 with
potassium citrate or citric acid, as required.
3.1.3 Hydrogen Peroxide, 3 percent. Same as in Method 6, Section
3.1.3 (40 ml is needed per sample).
3.1.4 Recovery Check Gas. Hydrogen sulfide (100 ppm or less) in
nitrogen, stored in aluminum cylinders. Verify the concentration by
Method 11 or by gas chromatography where the instrument is calibrated
with an H2S permeation tube as described below. For Method 11, the
standard deviation should not exceed 5 percent on at least three
20-minute runs.
Alternatively, hydrogen sulfide recovery gas generated from a
permeation device gravimetrically calibrated and certified at some
convenient operating temperature may be used. The permeation rate of
the device must be such that at a dilution gas flow rate of 3
liters/min, an H2S concentration in the range of the stack gas or within
20 percent of the standard can be generated.
3.1.5 Combustion Gas. Gas containing less than 50 ppb reduced sulfur
compounds and less than 10 ppm total hydrocarbons. The gas may be
generated from a clean-air system that purifies ambient air and consists
of the following components: Diaphragm pump, silica gel drying tube,
activated charcoal tube, and flow rate measuring device. Flow from a
compressed air cylinder is also acceptable.
3.2 Sample Recovery and Analysis. Same as in Method 6, Sections
3.2.1 and 3.3.
4. Procedure
4.1 Sampling. Before any source sampling is done, conduct two
30-minute system performance checks in the field as detailed in Section
4.3 to validate the sampling train components and procedure (optional).
4.1.1 Preparation of Collection Train. For the SO2 scrubber, measure
100 ml of citrate buffer into the first and second impingers; leave the
third impinger empty. Immerse the impingers in an ice bath, and locate
them as close as possible to the filter heat box. The connecting tubing
should be free of loops. Maintain the probe and filter temperatures
sufficiently high to prevent moisture condensation, and monitor with a
suitable temperature indicator.
For the Method 6 part of the train, measure 20 ml of 3 percent
hydrogen peroxide into the first and second midget impingers. Leave the
third midget impinger empty, and place silica gel in the fourth midget
impinger. Alternatively, a silica gel drying tube may be used in place
of the fourth impinger. Maintain the oxidation furnace at 800 100 C.
Place crushed ice and water around all impingers.
4.1.2 Citrate Scrubber Conditioning Procedure. Condition the citrate
buffer scrubbing solution by pulling stack gas through the Teflon
impingers and bypassing all other sampling train components. A purge
rate of 2 liters/min for 10 minutes has been found to be sufficient to
obtain equilibrium. After the citrate scrubber has been conditioned,
assemble the sampling train, and conduct (optional) a leak-check as
described in Method 6, Section 4.1.2.
4.1.3 Sample Collection. Same as in Method 6, Section 4.1.3, except
the sampling rate is 2 liters/min ( 10 percent) for 1 or 3 hours.
After the sample is collected, remove the probe from the stack, and
conduct (mandatory) a post-test leak check as described in Method 6,
Section 4.1.2. The 15-minute purge of the train following collection
should not be performed. After each 3-hour test run (or after three
1-hour samples), conduct one system performance check (see Section 4.3)
to determine the reduced sulfur recovery efficiency through the sampling
train. After this system performance check and before the next test
run, rinse and brush the probe with water, replace the filter, and
change the citrate scrubber (recommended but optional).
In Method 16, a test run is composed of 16 individual analyses
(injects) performed over a period of not less than 3 hours or more than
6 hours. For Method 16A to be consistent with Method 16, the following
may be used to obtain a test run: (1) collect three 60-minute samples
or (2) collect one 3-hour sample. (Three test runs constitute a test.)
4.2 Sample Recovery. Disconnect the impingers. Quantitatively
transfer the contents of the midget impingers of the Method 6 part of
the train into a leak-free polyethylene bottle for shipment. Rinse the
three midget impingers and the connecting tubes with water and add the
washings to the same storage container. Mark the fluid level. Seal and
identify the sample container.
4.3 System Performance Check. A system performance check is done (1)
to validate the sampling train components and procedure (prior to
testing; optional) and (2) to validate a test run (after a run).
Perform a check in the field prior to testing consisting of a least two
samples (optional), and perform an additional check after each 3-hour
run or after three 1-hour samples (mandatory).
The checks involve sampling a known concentration of H2S and
comparing the analyzed concentration with the known concentration. Mix
the H2S recovery gas (Section 3.1.4) and combustion gas in a dilution
system such as is shown in Figure 16A-3. Adjust the flow rates to
generate an H2S concentration in the range of the stack gas or within 20
percent of the applicable standard and an oxygen concentration greater
than 1 percent at a total flow rate of at least 2.5 liters/min. Use
Equation 16A-3 to calculate the concentration of recovery gas generated.
Calibrate the flow rate from both sources with a soap bubble flow tube
so that the diluted concentration of H2S can be accurately calculated.
Collect 30-minute samples, and analyze in the normal manner (as
discussed in Section 4.1.3). Collect the sample through the probe of the
sampling train using a manifold or some other suitable device that will
ensure extraction of a representative sample.
Insert illus 0332
The recovery check must be performed in the field prior to replacing
the SO2 scrubber and particulate filter and before the probe is cleaned.
A sample recovery of 100 20 percent must be obtained for the data to
be valid and should be reported with the emission data, but should not
be used to correct the data. However, if the performance check results
do not affect the compliance or noncompliance status of the affected
facility, the Administrator may decide to accept the results of the
compliance test. Use Equation 16A-4 to calculate the recovery
efficiency.
4.4 Sample Analysis. Same as in Method 6, Section 4.3, except for
1-hour sampling, take a 40-ml aliquot, add 160 ml of 100 percent
isopropanol, and four drops of thorin. Analyze an EPA SO2 field audit
sample with each set of samples. Such audit samples are available from
the Source Branch, Quality Assurance Division, Environmental Monitoring
Systems Laboratory, U. S. Environmental Protection Agency, Research
Triangle Park, North Carolina 27711.
5. Calibration
5.1 Metering System, Thermometers, Rotameters, Barometers, and Barium
Perchlorate Solution. Calibration procedures are presented in Method 6,
Sections 5.1 through 5.5.
6. Calculations
In the calculations, at least one extra decimal figure should be
retained beyond that of the acquired data. Figures should be rounded
off after final calculations.
6.1 Nomenclature.
CTRS=Concentration of TRS as SO2, dry basis corrected to standard
conditions, ppm.
CRG=Concentration of recovery gas generated, ppm.
CH2S=Verified concentration of H2S recovery gas.
N=Normality of barium perchlorate titrant, milliequivalents/ml.
Pbar=Barometric pressure at exit orifice of the dry gas meter, mm Hg
(in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
QH2S=Calibrated flow rate of H2S recovery gas, liters/min.
QCG=Calibrated flow rate of combustion gas, liters/min.
R=Recovery efficiency for the system performance check, percent.
Tm=Average dry gas meter absolute temperature, K ( R).
Tstd=Standard absolute temperature, 293 K, (528 R).
Va=Volume of sample aliquot titrated, ml.
Vm=Dry gas volume as measured by the dry gas meter, liters (dcf).
Vm(std)=Dry gas volume measured by the dry gas meter, corrected to
standard conditions, liters (dscf).
Vsoln=Total volume of solution in which the sulfur dioxide sample is
contained, 100 ml.
Vt=Volume of barium perchlorate titrant used for the sample, ml
(average of replicate titrations).
Vtb=Volume of barium perchlorate titrant used for the blank, ml.
Y=Dry gas meter calibration factor.
32.03=Equivalent weight of sulfur dioxide, mg/meq.
6.2 Dry Sample Gas Volume, Corrected to Standard Conditions.
Eq. 16A-1
Where: K1=0.3858 K/mm Hg for metric units.
6.3 Concentration of TRS as ppm SO2.
Eq. 16A-2
Where:
6.4 Concentration of Recovery Gas Generated in the System Performance
Check.
6.5 Recovery Efficiency for the System Performance Check.
7. Alternative Procedures
7.1 Determination of H2S Content in Cylinder Gases. As an
alternative to the procedures specified in section 3.1.4, the following
procedure may be used to verify the concentration of the recovery check
gas. The H2S is collected from the calibration gas cylinder and is
absorbed in zinc acetate solution to form zinc sulfide. The latter
compound is then measured iodometrically. The method has been examined
in the range of 5 to 1500 ppm. There are no known interferences to this
method when used to analyze cylinder gases containing H2S in nitrogen.
Laboratory tests have shown a relative standard deviation of less than 3
percent. The method showed no bias when compared to a gas
chromatographic method that used gravimetrically certified permeation
tubes for calibration.
7.1.1 Sampling Apparatus. The sampling train is shown in Figure
16A-4 and consists of the following components:
Insert illustration(s)009
7.1.1.1 Sampling Line. Teflon tubing ( 1/4-in.) to connect the
cylinder regulator to the sampling valve.
7.1.1.2 Needle Valve. Stainless steel or Teflon needle valve to
control the flow rate of gases to the impingers.
7.1.1.3 Impingers. Three impingers of approximately 100-ml capacity,
constructed to permit the addition of reagents through the gas inlet
stem. The impingers shall be connected in series with leak-free glass
or Teflon connectors. The impinger bottoms have a standard 24/25
ground-glass fitting. The stems are from standard 1/4-in. (0.64-cm)
ball joint midget impingers, custom lengthened by about 1 in. When
fitted together, the stem end should be approximately 1/2 in. (1.27-cm)
from the bottom (Southern Scientific, Inc., Micanopy, Florida: Set
Number S6962-048). The third in-line impinger acts as a drop-out
bottle.
7.1.1.4 Drying Tube, Flowmeter, and Barometer. Same as in Method 11,
Sections 5.1.5, 5.1.8, and 5.1.10.
7.1.1.5 Cylinder Gas Regulator. Stainless steel, to reduce the
pressure of the gas stream entering the Teflon sampling line to a safe
level.
7.1.1.6 Soap Bubble Meter. Calibrated for 100 and 500 ml, or two
separate bubble meters.
7.1.1.7 Critical Orifice. For volume and rate measurements. The
critical orifice may be fabricated according to Section 7.1.4.3 and must
be calibrated as specified in Section 7.1.8.4.
7.1.1.8 Graduated Cylinder. 50-ml size.
7.1.1.9 Volumetric Flask. 1-liter size.
7.1.1.10 Volumetric Pipette. 15-ml size.
7.1.1.11 Vacuum Gauge. Minimum 20-in. Hg capacity.
7.1.1.12 Stopwatch.
7.1.2 Sample Recovery and Analysis Apparatus.
7.1.2.1 Erlenmeyer Flasks. 125- and 250-ml sizes.
7.1.2.2 Pipettes. 2-, 10-, 20-, and 100-ml volumetric.
7.1.2.3 Burette. 50-ml size.
7.1.2.4 Volumetric Flask. 1-liter size.
7.1.2.5 Graduated Cylinder. 50-ml size.
7.1.2.6 Wash Bottle.
7.1.2.7 Stirring Plate and Bars.
7.1.3 Reagents. Unless otherwise indicated, all reagents shall
conform to the specifications established by the Committee on Analytical
Reagents of the American Chemical Society, where such specifications are
available. Otherwise, use the best available grade.
7.1.3.1 Water. Same as in Method 11, Section 6.1.3.
7.1.3.2 Zinc Acetate Absorbing Solution. Dissolve 20 g zinc acetate
in water and dilute to 1 liter.
7.1.3.3 Potassium Bi-iodate (KH(IO3)2 Solution, Standard 0.100 N.
Dissolve 3.249 g anhydrous KH(IO3)2 in water, and dilute to 1 liter.
7.1.3.4 Sodium Thiosulfate (Na2S203) Solution, Standard 0.1 N. Same
as in Method 11, Section 6.3.1. Standardize according to Section
7.1.8.2.
7.1.3.5 Na2S203 Solution, Standard 0.01 N. Pipette 100.0 ml of 0.1 N
Na2S203 solution into a 1-liter volumetric flask, and dilute to the mark
with water.
7.1.3.6 Iodine Solution, 0.1 N. Same as in Method 11, Section 6.2.2.
7.1.3.7 Standard Iodine Solution, 0.01 N. Same as in Method 11,
Section 6.2.3. Standardize according to Section 7.1.8.3.
7.1.3.8 Hydrochloric Acid (HCl) Solution, 10 Percent by Weight. Add
230 ml concentrated HCl (specific gravity 1.19) to 770 ml water.
7.1.3.9 Starch Indicator Solution. To 5 g starch (potato, arrowroot,
or soluble), add a little cold water, and grind in a mortar to a thin
paste. Pour into 1 liter of boiling water, stir, and let settle
overnight. Use the clear supernatant. Preserve with 1.25 g salicylic
acid, 4 g zinc chloride, or a combination of 4 g sodium propionate and 2
g sodium azide per liter of starch solution. Some commercial starch
substitutes are satisfactory.
7.1.4 Sampling Procedure.
7.1.4.1 Selection of Gas Sample Volumes. This procedure has been
validated for estimating the volume of cylinder gas sample needed when
the H2S concentration is in the range of 5 to 1500 ppm. The sample
volume ranges were selected in order to ensure a 35 to 60 percent
consumption of the 20 ml of 0.01 N iodine (thus ensuring a 0.01 N
Na2S2O3 titer of approximately 7 to 12 ml). The sample volumes for
various H2S concentrations can be estimated by dividing the approximate
ppm-liters desired for a given concentration range by the H2S
concentration stated by the manufacturer.
For example, for analyzing a cylinder gas containing approximately 10
ppm H2S, the optimum sample volume is 65 liters (650 ppm-liters/10 ppm).
For analyzing a cylinder gas containing approximately 1000 ppm H2S, the
optimum sample volume is 1 liter (1000 ppm-liters/1000 ppm).
7.1.4.2 Critical Orifice Flow Rate Selection. The following table
shows the ranges of sample flow rates that are desirable in order to
ensure capture of H2S in the impinger solution. Slight deviations from
these ranges will not have an impact on measured concentrations.
7.1.4.3 Critical Orifice Fabrication. Critical orifice of desired
flow rates may be fabricated by selecting an orifice tube of desired
length and connecting 1/16-in. x 1/4-in. (0.16-cm x 0.64-cm) reducing
fittings to both ends. The inside diameters and lengths of orifice
tubes needed to obtain specific flow rates are shown below.
7.1.4.4 Determination of Critical Orifice Approximate Flow Rate.
Connect the critical orifice to the sampling system as shown in Figure
16A-4 but without the H2S cylinder. Connect a rotameter in the line to
the first impinger. Turn on the pump, and adjust the valve to give a
reading of about half atmospheric pressure. Observe the rotameter
reading. Slowly increase the vacuum until a stable flow rate is
reached, and record this as the critical vacuum. The measured flow rate
indicates the expected critical flow rate of the orifice. If this flow
rate is in the range shown in Section 7.1.4.2, proceed with the critical
orifice calibration according to Section 7.1.8.4.
7.1.4.5 Determination of Approximate Sampling Time. Determine the
approximate sampling time for a cylinder of known concentration. Use
the optimum sample volume obtained in Section 7.1.4.1.
7.1.4.6 Sample Collection. Connect the Teflon tubing, Teflon tee,
and rotameter to the flow control needle valve as shown in Figure 16A-4.
Vent the rotameter to an exhaust hood. Plug the open end of the tee.
Five to 10 minutes prior to sampling, open the cylinder valve while
keeping the flow control needle valve closed. Adjust the delivery
pressure to 20 psi. Open the needle valve slowly until the rotameter
shows a flow rate approximately 50 to 100 ml above the flow rate of the
critical orifice being used in the system.
Place 50 ml of zinc acetate solution in two of the impingers, connect
them and the empty third impinger (dropout bottle) and the rest of the
equipment as shown in Figure 16A-4. Make sure the ground-glass fittings
are tight. The impingers can be easily stabilized by using a small
cardboard box in which three holes have been cut, to act as a holder.
Connect the Teflon sample line to the first impinger. Cover the
impingers with a dark cloth or piece of plastic to protect the absorbing
solution from light during sampling.
Record the temperature and barometric pressure. Note the gas flow
rate through the rotameter. Open the closed end of the tee. Connect
the sampling tube to the tee, ensuring a tight connection. Start the
sampling pump and stopwatch simultaneously. Note the decrease in flow
rate through the excess flow rotameter. This decrease should equal the
known flow rate of the critical orifice being used. Continue sampling
for the period determined in Section 7.1.4.5.
When sampling is complete, turn off the pump and stopwatch.
Disconnect the sampling line from the tee and plug it. Close the needle
valve followed by the cylinder valve. Record the sampling time.
7.1.5 Blank Analysis. While the sample is being collected, run a
blank as follows: To a 250-ml Erlenmeyer flask, add 100 ml of zinc
acetate solution, 20.0 ml. 0.01 N iodine solution, and 2 ml HCl
solution. Titrate, while stirring, with 0.01 N Na2S203 until the
solution is light yellow. Add starch, and continue titrating until the
blue color disappears. Analyze a blank with each sample, as the blank
titer has been observed to change over the course of a day.
Note: Iodine titration of zinc acetate solutions is difficult to
perform because the solution turns slightly white in color near the end
point, and the disappearance of the blue color is hard to recognize. In
addition, a blue color may reappear in the solution about 30 to 45
seconds after the titration endpoint is reached. This should not be
taken to mean the original endpoint was in error. It is recommended
that persons conducting this test perform several titrations to be able
to correctly identify the endpoint. The importance of this should be
recognized because the results of this analytical procedure are
extremely sensitive to errors in titration.
7.1.6 Sample Analysis. Sample treatment is similar to the blank
treatment. Before detaching the stems from the bottoms of the
impingers, add 20.0 ml of 0.01 N iodine solution through the stems of
the impingers holding the zinc acetate solution, dividing it between the
two (add about 15 ml to the first impinger and the rest to the second).
Add 2 ml HCl solution through the stems, dividing it as with the iodine.
Disconnect the sampling line, and store the impingers for 30 minutes.
At the end of 30 minutes, rinse the impinger stems into the impinger
bottoms. Titrate the impinger contents with 0.01 N Na2S203. Do not
transfer the contents of the impinger to a flask because this may result
in a loss of iodine and cause a positive bias.
7.1.7 Post-test Orifice Calibration. Conduct a post-test critical
orifice calibration run using the calibration procedures outlined in
Section 7.1.8.4. If the Qstd obtained before and after the test differs
by more than 5 percent, void the sample; if not, proceed to perform the
calculations.
7.1.8 Calibrations and Standardizations.
7.1.8.1 Rotameter and Barometer. Same as in Method 11, Sections
8.2.3 and 8.2.4.
7.1.8.2 Na2S2O3 Solution, 0.1 N. Standardize the 0.1 N Na2S2O3
solution as follows: To 80 ml water, stirring constantly, add 1 ml
concentrated H2SO4, 10.0 ml 0.100 N KH(IO3)2 and 1 g potassium iodide.
Titrate immediately with 0.1 N Na2S2O3 until the solution is light
yellow. Add 3 ml starch solution, and titrate until the blue color just
disappears. Repeat the titration until replicate analyses agree within
0.05 ml. Take the average volume of Na2S2O3 consumed to calculate the
normality to three decimal figures using Equation 16A-5.
7.1.8.3 Iodine Solution, 0.01 N. Standardize the 0.01 N iodine
solution as follows: Pipet 20.0 ml of 0.01 N iodine solution into a
125-ml Erlenmeyer flask. Titrate with standard 0.01 N Na2S2O3 solution
until the solution is light yellow. Add 3 ml starch solution, and
continue titrating until the blue color just disappears.
If the normality of the iodine tested is not 0.010, add a few ml of
0.1 N iodine solution if it is low, or a few ml of water if it is high,
and standardize again. Repeat the titration until replicate values
agree within 0.05 ml. Take the average volume to calculate the normality
to three decimal figures using Equation 16A-6.
7.1.8.4 Critical Orifice. Calibrate the critical orifice using the
sampling train shown in Figure 16A-4 but without the H2S cylinder and
vent rotameter. Connect the soap bubble meter to the Teflon line that
is connected to the first impinger. Turn on the pump, and adjust the
needle valve until the vaccum is higher than the critical vacuum
determined in Section 7.1.4.4. Record the time required for gas flow to
equal the soap bubble meter volume (use the 100-ml soap bubble meter for
gas flow rates below 100 ml/min, otherwise use the 500-ml soap bubble
meter). Make three runs, and record the data listed in Table 1. Use
these data to calculate the volumetric flow rate of the orifice.
7.1.9 Calculations.
7.1.9.1 Nomenclature.
Bwa=Fraction of water vapor in ambient air during orifice
calibration.
CH2S=H2S concentration in cylinder gas, ppm.
K=Conversion factor=12025 ml/eq
Ma=Molecular weight of ambient air saturated at impinger temperature,
g/g-mole.
Ms=Molecular weight of sample gas (nitrogen) saturated at impinger
temperature, g/g-mole. (For tests carried out in a laboratory where the
impinger temperature is 25 C, Ma=28.5 g/g-mole and Ms=27.7 g/g-mole.)
NI=Normality of standard iodine solution (0.01 N), g-eq/liter.
NT=Normality of standard Na2S2O3 solution (0.01 N), g-eq/liter.
Pbar=Barometric pressure, mm Hg.
Pstd=Standard absolute pressure, 760 mm Hg.
Qstd=Volumetric flow rate through critical orifice, liters/min.
DateXXXXXXXXXX
Critical orifice IDXXXXXXXXXX
Soap bubble meter volume, Vsb XXX liters
Time, Usb
Run no. 1 XXX min XXX sec
Run no. 2 XXX min XXX sec
Run no. 3 XXX min XXX sec
Average XXX min XXX sec
Convert the seconds to fraction of minute:
Time
= XXX min + XXX Sec/60
= XXX min
Barometric pressure, Pbar = XXX mm Hg
Ambient temperature, tamb = 273 + XXX C
= XXX K
Pump vacuum, = XXX mm Hg. (This should be approximately 0.4 times
barometric pressure.)
= ---------- liters
= ---------- liters/min
Table 1 -- Critical orifice calibration data.
Qstd, average = Average standard flow rate through critical orifice,
liters/min.
Qstd, before = Average standard flow rate through critical orifice
determined before H2S sampling (Section 7.1.4.4), liters/min.
Qstd, after = Average standard flow rate through critical orifice
determined after H2S sampling (Section 7.1.7), liters/min.
Tamb = Absolute ambient temperature, K.
Tstd = Standard absolute temperature, 293 K.
Us = Sampling time, min.
Usb = Time for soap bubble meter flow rate measurement, min.
Vm(std) = Sample gas volume measured by the critical orifice,
corrected to standard conditions, liters.
Vsb = Volume of gas as measured by the soap bubble meter, ml.
Vsb(std) = Volume of gas as measured by the soap bubble meter,
corrected to standard conditions, liters.
VI = Volume of standard iodine solution (0.01 N) used, ml.
VT = Volume of standard Na2S2O3 solution (0.01 N) used, ml.
VTB = Volume of standard Na2S2O3 solution (0.01 N) used for the
blank, ml.
7.1.9.2 Normality of Standard Na2S2O3 Solution (0.1. N).
Eq. 16A-5
7.1.9.3 Normality of Standard Iodine Solution (0.01 N).
Eq. 16A-6
7.1.9.4 Sample Gas Volume.
Eq. 16A-7
7.1.9.5 Concentration of H2S in the Gas Cylinder.
Eq. 16A-8
1. American Public Health Association, American Water Works
Association, and Water Pollution Control Federation. Standard Methods
for the Examination of Water and Wastewater. Washington, DC. American
Public Health Association. 1975. p. 316-317.
2. American Society for Testing and Materials. Annual Book of ASTM
Standards. Part 31: Water, Atmospheric Analysis. Philadelphia, PA.
1974. p. 40-42.
3. Blosser, R.O. A Study of TRS Measurement Methods. National
Council of the Paper Industry for Air and Stream Improvement, Inc., New
York, NY. Technical Bulletin No. 434. May 1984. 14 p.
4. Blosser, R.O., H.S. Oglesby, and A.K. Jain. A Study of Alternate
SO2 Scrubber Designs Used for TRS Monitoring. A Special Report by the
National Council of the Paper Industry for Air and Stream Improvement,
Inc., New York, NY. July 1977.
5. Curtis, F., and G.D. McAlister. Development and Evaluation of an
Oxidation/Method 6 TRS Emission Sampling Procedure. Emission
Measurement Branch, Emission Standards and Engineering Division, U.S.
Environmental Protection Agency, Research Triangle Park, NC 27711.
February 1980.
6. Gellman, I. A Laboratory and Field Study of Reduced Sulfur
Sampling and Monitoring Systems. National Council of the Paper Industry
for Air and Stream Improvement, Inc., New York, NY. Atmospheric Quality
Improvement Technical Bulletin No. 81. October 1975.
7. Margeson, J.H., J.E. Knoll, and M.R. Midgett. A Manual Method for
TRS Determination. Draft Available from the authors. Source Branch,
Quality Assurance Division, U.S. Environmental Protection Agency,
Research Triangle Park, NC 27711.
8. National Council of the Paper Industry for Air and Stream
Improvement. An Investigation of H2S and SO2 Calibration Cylinder Gas
Stability and Their Standardization Using Wet Chemical Techniques.
Special Report 76-06. New York, NY. August 1976.
9. National Council of the Paper Industry for Air and Stream
Improvement. Wet Chemical Method for Determining the H2S Concentration
of Calibration Cylinder Gases. Technical Bulletin Number 450. New
York, NY. January 1985. 23 p.
10. National Council of the Paper Industry for Air and Stream
Improvement. Modified Wet Chemcial Method for Determining the H2S
Concentration of Calibration Cylinder Gases. Draft Report. New York,
NY. March 1987. 29 p.
40 CFR 60.748 Pt. 60, App. A, Meth. 16B
1. Applicability, Principle, Range and Sensitivity, Interferences,
and Precision and Accuracy
1.1 Applicability. This method is applicable to the determination of
total reduced sulfur (TRS) emissions from recovery furnaces, lime kilns,
and smelt dissolving tanks at kraft pulp mills, and from other sources
when specified in an applicable subpart of the regulations. The TRS
compounds include hydrogen sulfide (H2S), methyl mercaptan, dimethyl
sulfide, and dimethyl disulfide.
The flue gas must contain at least 1 percent oxygen for complete
oxidation of all TRS to sulfur dioxide (SO2).
1.2 Principle. An integrated gas sample is extracted from the stack.
The SO2 is removed selectively from the sample using a citrate buffer
solution. The TRS compounds are then thermally oxidized to SO2 and
analyzed as SO2 by gas chromatography (GC) using flame photometric
detection (FPD).
1.3 Range and Sensitivity. Coupled with a GC utilizing a 1-ml sample
size, the maximum limit of the FPD for SO2 is approximately 10 ppm.
This limit is expanded by dilution of the sample gas before analysis or
by reducing the sample aliquot size. For sources with emission levels
between 10 and 100 ppm, the measuring range can be best extended by
reducing the sample size.
1.4 Interferences. The TRS compounds other than those regulated by
the emission standards, if present, may be measured by this method.
Therefore, carbonyl sulfide, which is partially oxidized to SO2 and may
be present in a lime kiln exit stack, would be a positive interferent.
Particulate matter from the lime kiln stack gas (primarily calcium
carbonate) can cause a negative bias if it is allowed to enter the
citrate scrubber; the particulate matter will cause the pH to rise and
H2S to be absorbed before oxidation. Proper use of the particulate
filter, described in Section 2.1.3 of Method 16A, will eliminate this
interference.
Carbon monoxide (CO) and carbon dioxide (CO2) have substantial
desensitizing effects on the FPD even after dilution. Acceptable
systems must demonstrate that they have eliminated this interference by
some procedure such as eluting these compounds before the SO2.
Compliance with this requirement can be demonstrated by submitting
chromatograms of calibration gases with and without CO2 in diluent gas.
The CO2 level should be approximately 10 percent for the case with CO2
present. The two chromatograms should show agreement within the
precision limits of Section 1.5.
1.5 Precision and Accuracy. The GC/FPD and dilution calibration
precision and drift, and the system calibration accuracy are the same as
in Method 16, Sections 4.1 to 4.3.
Field tests between this method and Method 16A showed an average
difference of less than 4.0 percent. This difference was not determined
to be significant.
2. Apparatus
2.1 Sampling. A sampling train is shown in Figure 16B-1.
Modifications to the apparatus are accepted provided the system
performance check is met.
40 CFR 60.748
2.1.1 Probe, Probe Brush, Particulate Filter, SO2 Scrubber,
Combustion Tube, and Furnace. Same as in Method 16A, Sections 2.1.1 to
2.1.6.
2.1.2 Sampling Pump. Leakless Teflon-coated diaphragm type or
equivalent.
2.2 Analysis.
2.2.1 Dilution System (optional), Gas Chromatograph, Oven,
Temperature Gauges, Flow System, Flame Photometric Detector,
Electrometer, Power Supply, Recorder, Calibration System, Tube Chamber,
Flow System, and Constant Temperature Bath. Same as in Method 16,
Sections 5.2, 5.4, and 5.5.
2.2.2 Gas Chromatograph Columns. Same as in Method 16, Section
12.1.4.1.1. Other columns with demonstrated ability to resolve SO2 and
be free from known interferences are acceptable alternatives.
3. Reagents
Same as in Method 16, Section 6, except the following:
3.1 Calibration Gas. SO2 permeation tube gravimetrically calibrated
and certified at some convenient operating temperature. These tubes
consist of hermetically sealed FEP Teflon tubing in which a liquefied
gaseous substance is enclosed. The enclosed gas permeates through the
tubing wall at a constant rate. When the temperature is constant,
calibration gases covering a wide range of known concentrations can be
generated by varying and accurately measuring the flow rate of diluent
gas passing over the tubes. In place of SO2 permeation tubes, National
Bureau of Standards traceable cylinder gases containing SO2 in nitrogen
may be used for calibration. The calibration gas is used to calibrate
the GC/FPD system and the dilution system.
3.2 Recovery Check Gas. Hydrogen sulfide (100 ppm or less) in
nitrogen, stored in aluminum cylinders. Verify the concentration by
Method 11, the procedure discussed in Section 7.1 of Method 16A, or gas
chromatography where the instrument is calibrated with an H2S permeation
tube as described below. For the wet-chemical methods, the standard
deviation should not exceed 5 percent on at least three 20-minute runs.
Hydrogen sulfide recovery gas generated from a permeation device
gravimetically calibrated and certified at some convenient operation
temperature may be used. The permeation rate of the device must be such
that at a dilution gas flow rate of 3 liters/min, an H2S concentration
in the range of the stack gas or within 20 percent of the standard can
be generated.
3.3 Combustion Gas. Gas containing less than 50 ppb reduced sulfur
compounds and less than 10 ppm total hydrocarbons. The gas may be
generated from a clean-air system that purifies ambient air and consists
of the following components: diaphragm pump, silica gel drying tube,
activated charcoal tube, and flow rate measuring device. Gas from a
compressed air cylinder is also acceptable.
4. Pretest Procedures
Same as in Method 16, Section 7.
5. Calibration
Same as in Method 16, Section 8, except SO2 is used instead of H2S.
6. Sampling and Analysis Procedure
6.1 Sampling. Before any source sampling is done, conduct a system
performance check as detailed in Section 7.1 to validate the sampling
train components and procedures. Although this test is optional, it
would significantly reduce the possibility of rejecting tests as a
result of failing the post-test performance check. At the completion of
the pretest system performance check, insert the sampling probe into the
test port making certain that no dilution air enters the stack through
the port. Condition the entire system with sample for a minimum of 15
minutes before beginning analysis. If the sample is diluted, determine
the precise dilution factor as in Section 8.5 of Method 16.
6.2 Analysis. Pass aliquots of diluted sample through the SO2
scrubber and oxidation furnace, and then inject into the GC/FPD analyzer
for analysis. The rest of the analysis is the same as in Method 16,
Sections 9.2.1 and 9.2.2.
7. Post-Test Procedures
7.1 System Performance Check. Same as in Method 16A, Section 4.3.
Sufficient numbers of sample injections should be made so that the
precision requirements of Section 4.1 of Method 16 are satisfied.
7.2 Recalibration. Same as in Method 16, Section 10.2.
7.3 Determination of Calibration Drift. Same as in Method 16,
Section 10.3.
8. Calculations
8.1 Nomenclature.
CSO2 = Sulfur dioxide concentration, ppm.
CTRS = Total reduced sulfur concentration as determined by Equation
16B-1, ppm.
d = Dilution factor, dimensionless.
N = Number of samples.
8.2 SO2 Concentration. Determine the concentration of SO2 (CSO2)
directly from the calibration curves. Alternatively, the concentration
may be calculated using the equation for the least-squares line.
8.3 TRS Concentration.
CTRS = (CSO2) (d)
Eq. 16B-1
8.4 Average TRS Concentration.
9. Example System
Same as in Method 16, Section 12. Single column systems using the
column in Section 12.1.4.1.1 of Method 16 or a 7-ft Carbosorb B HT 100
column have been found satisfactory in resolving SO2 from CO2.
10. Bibliography
1. Same as in Method 16, Sections 13.1 to 13.6.
2. National Council of the Paper Industry for Air and Stream
Improvement, Inc. A Study of TRS Measurement Methods. Technical
Bulletin No. 434. New York, NY. May 1984. 12 p.
3. Margeson, J.H., J.E. Knoll, and M.R. Midgett. A Manual Method for
TRS Determination. Draft available from the authors. Source Branch,
Quality Assurance Division, U.S. Environmental Protection Agency,
Research Triangle Park, NC 27711.
40 CFR 60.748 Pt. 60, App. A, Meth. 17
Introduction
Particulate matter is not an absolute quantity; rather, it is a
function of temperature and pressure. Therefore, to prevent variability
in particulate matter emission regulations and/or associated test
methods, the temperature and pressure at which particulate matter is to
be measured must be carefully defined. Of the two variables (i.e.,
temperature and pressure), temperature has the greater effect upon the
amount of particulate matter in an effluent gas stream; in most
stationary source categories, the effect of pressure appears to be
negligible.
In Method 5, 250 F is established as a nominal reference
temperature. Thus, where Method 5 is specified in an applicable subpart
of the standards, particulate matter is defined with respect to
temperature. In order to maintain a collection temperature of 250 F,
Method 5 employs a heated glass sample probe and a heated filter holder.
This equipment is somewhat cumbersome and requires care in its
operation. Therefore, where particulate matter concentrations (over the
normal range of temperature associated with a specified source category)
are known to be independent of temperature, it is desirable to eliminate
the glass probe and heating systems, and sample at stack temperature.
This method describes an in-stack sampling system and sampling
procedures for use in such cases. It is intended to be used only when
specified by an applicable subpart of the standards, and only within the
applicable temperature limits (if specified), or when otherwise approved
by the Administrator.
1. Principle and Applicability
1.1 Principle. Particulate matter is withdrawn isokinetically from
the source and collected on a glass fiber filter maintained at stack
temperature. The particulate mass is determined gravimetrically after
removal of uncombined water.
1.2 Applicability. This method applies to the determination of
particulate emissions from stationary sources for determining compliance
with new source performance standards, only when specifically provided
for in an applicable subpart of the standards. This method is not
applicable to stacks that contain liquid droplets or are saturated with
water vapor. In addition, this method shall not be used as written if
the projected cross-sectional area of the probe extension-filter holder
assembly covers more than 5 percent of the stack cross-sectional area
(see Section 4.1.2).
2. Apparatus
2.1 Sampling Train. A schematic of the sampling train used in this
method is shown in Figure 17-1. Construction details for many, but not
all, of the train components are given in APTD-0581 (Citation 2 in
Bibliography); for changes from the APTD-0581 document and for
allowable modifications to Figure 17-1, consult with the Administrator.
Insert illus. 1216
The operating and maintenance procedures for many of the sampling
train components are described in APTD-0576 (Citation 3 in
Bibliography). Since correct usage is important in obtaining valid
results, all users should read the APTD-0576 document and adopt the
operating and maintenance procedures outlined in it, unless otherwise
specified herein. The sampling train consists of the following
components:
2.1.1 Probe Nozzle. Stainless steel (316) or glass, with sharp,
tapered leading edge. The angle of taper shall be 30 and the taper
shall be on the outside to preserve a constant internal diameter. The
probe nozzle shall be of the button-hook or elbow design, unless
otherwise specified by the Administrator. If made of stainless steel,
the nozzle shall be constructed from seamless tubing. Other materials
of construction may be used subject to the approval of the
Administrator.
A range of sizes suitable for isokinetic sampling should be
available, e.g., 0.32 to 1.27 cm ( 1/8 to 1/2 in.) -- or larger if
higher volume sampling trains are used -- inside diameter (ID) nozzles
in increments of 0.16 cm ( 1/16 in.). Each nozzle shall be calibrated
according to the procedures outlined in Section 5.1.
2.1.2 Filter Holder. The in-stack filter holder shall be constructed
of borosilicate or quartz glass, or stainless steel; if a gasket is
used, it shall be made of silicone rubber, Teflon, or stainless steel.
Other holder and gasket materials may be used subject to the approval of
the Administrator. The filter holder shall be designed to provide a
positive seal against leakage from the outside or around the filter.
2.1.3 Probe Extension. Any suitable rigid probe extension may be
used after the filter holder.
2.1.4 Pitot Tube. Type S, as described in Section 2.1 of Method 2,
or other device approved by the Administrator; the pitot tube shall be
attached to the probe extension to allow constant monitoring of the
stack gas velocity (see Figure 17-1). The impact (high pressure)
opening plane of the pitot tube shall be even with or above the nozzle
entry plane during sampling (see Method 2, Figure 2-6b). It is
recommended: (1) that the pitot tube have a known baseline coefficient,
determined as outlined in Section 4 of Method 2; and (2) that this
known coefficient be preserved by placing the pitot tube in an
interference-free arrangement with respect to the sampling nozzle,
filter holder, and temperature sensor (see Figure 17-1). Note that the
1.9 cm (0.75 in.) free-space between the nozzle and pitot tube shown in
Figure 17-1, is based on a 1.3 cm (0.5 in.) ID nozzle. If the sampling
train is designed for sampling at higher flow rates than that described
in APTD-0581, thus necessitating the use of larger sized nozzles, the
free-space shall be 1.9 cm (0.75 in.) with the largest sized nozzle in
place.
Source-sampling assemblies that do not meet the minimum spacing
requirements of Figure 17-1 (or the equivalent of these requirements,
e.g., Figure 2-7 of Method 2) may be used; however, the pitot tube
coefficients of such assemblies shall be determined by calibration,
using methods subject to the approval of the Administrator.
2.1.5 Differential Pressure Gauge. Inclined manometer or equivalent
device (two), as described in Section 2.2 of Method 2. One manometer
shall be used for velocity head ( p) readings, and the other, for
orifice differential pressure readings.
2.1.6 Condenser. It is recommended that the impinger system described
in Method 5 be used to determine the moisture content of the stack gas.
Alternatively, any system that allows measurement of both the water
condensed and the moisture leaving the condenser, each to within 1 ml or
1 g, may be used. The moisture leaving the condenser can be measured
either by: (1) monitoring the temperature and pressure at the exit of
the condenser and using Dalton's law of partial pressures; or (2)
passing the sample gas stream through a silica gel trap with exit gases
kept below 20 C (68 F) and determining the weight gain.
Flexible tubing may be used between the probe extension and
condenser. If means other than silica gel are used to determine the
amount of moisture leaving the condenser, it is recommended that silica
gel still be used between the condenser system and pump to prevent
moisture condensation in the pump and metering devices and to avoid the
need to make corrections for moisture in the metered volume.
2.1.7 Metering System. Vacuum gauge, leak-free pump, thermometers
capable of measuring temperature to within 3 C (5.4 F), dry gas meter
capable of measuring volume to within 2 percent, and related equipment,
as shown in Figure 17-1. Other metering systems capable of maintaining
sampling rates within 10 percent of isokinetic and of determining sample
volumes to within 2 percent may be used, subject to the approval of the
Administrator. When the metering system is used in conjunction with a
pitot tube, the system shall enable checks of isokinetic rates.
Sampling trains utilizing metering systems designed for higher flow
rates than that described in APTD-0581 or APTD-0576 may be used provided
that the specifications of this method are met.
2.1.8 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg). In many
cases, the barometric reading may be obtained from a nearby National
Weather Service station, in which case the station value (which is the
absolute barometric pressure) shall be requested and an adjustment for
elevation differences between the weather station and sampling point
shall be applied at a rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 m
(100 ft) elevation increase or vice versa for elevation decrease.
2.1.9 Gas Density Determination Equipment. Temperature sensor and
pressure gauge, as described in Sections 2.3 and 2.4 of Method 2, and
gas analyzer, if necessary, as described in Method 3.
The temperature sensor shall be attached to either the pitot tube or
to the probe extension, in a fixed configuration. If the temperature
sensor is attached in the field, the sensor shall be placed in an
interference-free arrangement with respect to the Type S pitot tube
openings (as shown in Figure 17-1 or in Figure 2-7 of Method 2).
Alternatively, the temperature sensor need not be attached to either the
probe extension or pitot tube during sampling, provided that a
difference of not more than 1 percent in the average velocity
measurement is introduced. This alternative is subject to the approval
of the Administrator.
2.2 Sample Recovery.
2.2.1 Probe Nozzle Brush. Nylon bristle brush with stainless steel
wire handle. The brush shall be properly sized and shaped to brush out
the probe nozzle.
2.2.2 Wash Bottles -- Two. Glass wash bottles are recommended;
polyethylene wash bottles may be used at the option of the tester. It
is recommended that acetone not be stored in polyethylene bottles for
longer than a month.
2.2.3 Glass Sample Storage Containers. Chemically resistant,
borosilicate glass bottles, for acetone washes, 500 ml or 1000 ml.
Screw cap liners shall either be rubber-backed Teflon or shall be
constructed so as to be leak-free and resistant to chemical attack by
acetone. (Narrow mouth glass bottles have been found to be less prone
to leakage.) Alternatively, polyethylene bottles may be used.
2.2.4 Petri Dishes. For filter samples; glass or polyethylene,
unless otherwise specified by the Administrator.
2.2.5 Graduated Cylinder and/or Balance. To measure condensed water
to within 1 ml or 1 g. Graduated cylinders shall have subdivisions no
greater than 2 ml. Most laboratory balances are capable of weighing to
the nearest 0.5 g or less. Any of these balances is suitable for use
here and in Section 2.3.4.
2.2.6 Plastic Storage Containers. Air tight containers to store
silica gel.
2.2.7 Funnel and Rubber Policeman. To aid in transfer of silica gel
to container; not necessary if silica gel is weighed in the field.
2.2.8 Funnel. Glass or polyethylene, to aid in sample recovery.
2.3 Analysis.
2.3.1 Glass Weighing Dishes.
2.3.2 Desiccator.
2.3.3 Analytical Balance. To measure to within 0.1 mg.
2.3.4 Balance. To measure to within 0.5 mg.
2.3.5 Beakers. 250 ml.
2.3.6 Hygrometer. To measure the relative humidity of the laboratory
environment.
2.3.7 Temperature Gauge. To measure the temperature of the
laboratory environment.
3. Reagents
3.1 Sampling.
3.1.1 Filters. The in-stack filters shall be glass mats or thimble
fiber filters, without organic binders, and shall exhibit at least 99.95
percent efficiency (0.05 percent penetration) on 0.3 micron dioctyl
phthalate smoke particles. The filter efficiency tests shall be
conducted in accordance with ASTM Standard Method D2986-71 (Reapproved
1978) (incorporated by reference -- see 60.17). Test data from the
supplier's quality control program are sufficient for this purpose.
3.1.2 Silica Gel. Indicating type, 6- to 16-mesh. If previously
used, dry at 175 C (350 F) for 2 hours. New silica gel may be used as
received. Alternatively, other types of desiccants (equivalent or
better) may be used, subject to the approval of the Administrator.
3.1.3 Crushed Ice.
3.1.4 Stopcock Grease. Acetone-insoluble, heat-stable silicone
grease. This is not necessary if screw-on connectors with Teflon
sleeves, or similar, are used. Alternatively, other types of stopcock
grease may be used, subject to the approval of the Administrator.
3.1.5 Water. Same as in Method 5, section 3.1.3.
3.2 Sample Recovery. Acetone, reagent grade, 0.001 percent residue,
in glass bottles. Acetone from metal containers generally has a high
residue blank and should not be used. Sometimes, suppliers transfer
acetone to glass bottles from metal containers. Thus, acetone blanks
shall be run prior to field use and only acetone with low blank values (
0.001 percent) shall be used. In no case shall a blank value of greater
than 0.001 percent of the weight of acetone used be subtracted from the
sample weight.
3.3 Analysis.
3.3.1 Acetone. Same as 3.2.
3.3.2 Desiccant. Anhydrous calcium sulfate, indicating type.
Alternatively, other types of desiccants may be used, subject to the
approval of the Administrator.
4. Procedure
4.1 Sampling. The complexity of this method is such that, in order to
obtain reliable results, testers should be trained and experienced with
the test procedures.
4.1.1 Pretest Preparation. All components shall be maintained and
calibrated according to the procedure described in APTD-0576, unless
otherwise specified herein.
Weigh several 200 to 300 g portions of silica gel in air-tight
containers to the nearest 0.5 g. Record the total weight of the silica
gel plus container, on each container. As an alternative, the silica
gel need not be preweighed, but may be weighed directly in its impinger
or sampling holder just prior to train assembly.
Check filters visually against light for irregularities and flaws or
pinhole leaks. Label filters of the proper size on the back side near
the edge using numbering machine ink. As an alternative, label the
shipping containers (glass or plastic petri dishes) and keep the filters
in these containers at all times except during sampling and weighing.
Desiccate the filters at 20 5.6 C (68 10 F) and ambient pressure
for at least 24 hours and weigh at intervals of at least 6 hours to a
constant weight, i.e., 0.5 mg change from previous weighing; record
results to the nearest 0.1 mg. During each weighing the filter must not
be exposed to the laboratory atmosphere for a period greater than 2
minutes and a relative humidity above 50 percent. Alternatively (unless
otherwise specified by the Administrator), the filters may be oven dried
at 105 C (220 F) for 2 to 3 hours, desiccated for 2 hours, and
weighed. Procedures other than those described, which account for
relative humidity effects, may be used, subject to the approval of the
Administrator.
4.1.2 Preliminary Determinations. Select the sampling site and the
minimum number of sampling points according to Method 1 or as specified
by the Administrator. Make a projected-area model of the probe
extension-filter holder assembly, with the pitot tube face openings
positioned along the centerline of the stack, as shown in Figure 17-2.
Calculate the estimated cross-section blockage, as shown in Figure 17-2.
If the blockage exceeds 5 percent of the duct cross sectional area, the
tester has the following options: (1) a suitable out-of-stack
filtration method may be used instead of in-stack filtration; or (2) a
special in-stack arrangement, in which the sampling and velocity
measurement sites are separate, may be used; for details concerning
this approach, consult with the Administrator (see also Citation 10 in
Bibliography). Determine the stack pressure, temperature, and the range
of velocity heads using Method 2; it is recommended that a leak-check
of the pitot lines (see Method 2, Section 3.1) be performed. Determine
the moisture content using Approximation Method 4 or its alternatives
for the purpose of making isokinetic sampling rate settings. Determine
the stack gas dry molecular weight, as described in Method 2, Section
3.6; if integrated Method 3 sampling is used for molecular weight
determination, the integrated bag sample shall be taken simultaneously
with, and for the same total length of time as, the particulate sample
run.
Insert illus. 1226
Select a nozzle size based on the range of velocity heads, such that
it is not necessary to change the nozzle size in order to maintain
isokinetic sampling rates. During the run, do not change the nozzle
size. Ensure that the proper differential pressure gauge is chosen for
the range of velocity heads encountered (see Section 2.2 of Method 2).
Select a probe extension length such that all traverse points can be
sampled. For large stacks, consider sampling from opposite sides of the
stack to reduce the length of probes.
Select a total sampling time greater than or equal to the minimum
total sampling time specified in the test procedures for the specific
industry such that (1) the sampling time per point is not less than 2
minutes (or some greater time interval if specified by the
Administrator), and (2) the sample volume taken (corrected to standard
conditions) will exceed the required minimum total gas sample volume.
The latter is based on an approximate average sampling rate.
It is recommended that the number of minutes sampled at each point be
an integer or an integer plus one-half minute, in order to avoid
timekeeping errors.
In some circumstances, e.g., batch cycles, it may be necessary to
sample for shorter times at the traverse points and to obtain smaller
gas sample volumes. In these cases, the Administrator's approval must
first be obtained.
4.1.3 Preparation of Collection Train. During preparation and
assembly of the sampling train, keep all openings where contamination
can occur covered until just prior to assembly or until sampling is
about to begin.
If impingers are used to condense stack gas moisture, prepare them as
follows: place 100 ml of water in each of the first two impingers,
leave the third impinger empty, and transfer approximately 200 to 300 g
of preweighed silica gel from its container to the fourth impinger.
More silica gel may be used, but care should be taken to ensure that it
is not entrained and carried out from the impinger during sampling.
Place the container in a clean place for later use in the sample
recovery. Alternatively, the weight of the silica gel plus impinger may
be determined to the nearest 0.5 g and recorded.
If some means other than impingers is used to condense moisture,
prepare the condenser (and, if appropriate, silica gel for condenser
outlet) for use.
Using a tweezer or clean disposable surgical gloves, place a labeled
(identified) and weighed filter in the filter holder. Be sure that the
filter is properly centered and the gasket properly placed so as not to
allow the sample gas stream to circumvent the filter. Check filter for
tears after assembly is completed. Mark the probe extension with heat
resistant tape or by some other method to denote the proper distance
into the stack or duct for each sampling point.
Assemble the train as in Figure 17-1, using a very light coat of
silicone grease on all ground glass joints and greasing only the outer
portion (see APTD-0576) to avoid possibility of contamination by the
silicone grease. Place crushed ice around the impingers.
4.1.4 Leak Check Procedures.
4.1.4.1 Pretest Leak-Check. A pretest leak-check is recommended, but
not required. If the tester opts to conduct the pretest leak-check, the
following procedure shall be used.
After the sampling train has been assembled, plug the inlet to the
probe nozzle with a material that will be able to withstand the stack
temperature. Insert the filter holder into the stack and wait
approximately 5 minutes (or longer, if necessary) to allow the system to
come to equilibrium with the temperature of the stack gas stream. Turn
on the pump and draw a vacuum of at least 380 mm Hg (15 in. Hg); note
that a lower vacuum may be used, provided that it is not exceeded during
the test. Determine the leakage rate. A leakage rate in excess of 4
percent of the average sampling rate or 0.00057 m3/min. (0.02 cfm),
whichever is less, is unacceptable.
The following leak-check instructions for the sampling train
described in APTD-0576 and APTD-0581 may be helpful. Start the pump
with by-pass valve fully open and coarse adjust valve completely closed.
Partially open the coarse adjust valve and slowly close the by-pass
valve until the desired vacuum is reached. Do not reverse direction of
by-pass valve. If the desired vacuum is exceeded, either leak-check at
this higher vacuum or end the leak-check as shown below and start over.
When the leak-check is completed, first slowly remove the plug from
the inlet to the probe nozzle and immediately turn off the vacuum pump.
This prevents water from being forced backward and keeps silica gel from
being entrained backward.
4.1.4.2 Leak-Checks During Sample Run. If, during the sampling run,
a component (e.g., filter assembly or impinger) change becomes
necessary, a leak-check shall be conducted immediately before the change
is made. The leak-check shall be done according to the procedure
outlined in Section 4.1.4.1 above, except that it shall be done at a
vacuum equal to or greater than the maximum value recorded up to that
point in the test. If the leakage rate is found to be no greater than
0.00057 m3/min (0.02 cfm) or 4 percent of the average sampling rate
(whichever is less), the results are acceptable, and no correction will
need to be applied to the total volume of dry gas metered; if, however,
a higher leakage rate is obtained, the tester shall either record the
leakage rate and plan to correct the sample volume as shown in Section
6.3 of this method, or shall void the sampling run.
Immediately after component changes, leak-checks are optional; if
such leak-checks are done, the procedure outlined in Section 4.1.4.1
above shall be used.
4.1.4.3 Post-Test Leak-Check. A leak-check is mandatory at the
conclusion of each sampling run. The leak-check shall be done in
accordance with the procedures outlined in Section 4.1.4.1, except that
it shall be conducted at a vacuum equal to or greater than the maximum
value reached during the sampling run. If the leakage rate is found to
be no greater than 0.00057 m3/min (0.02 cfm) or 4 percent of the average
sampling rate (whichever is less), the results are acceptable, and no
correction need be applied to the total volume of dry gas metered. If,
however, a higher leakage rate is obtained, the tester shall either
record the leakage rate and correct the sample volume as shown in
Section 6.3 of this method, or shall void the sampling run.
4.1.5 Particulate Train Operation. During the sampling run, maintain
a sampling rate such that sampling is within 10 percent of true
isokinetic, unless otherwise specified by the Administrator.
For each run, record the data required on the example data sheet
shown in Figure 17-3. Be sure to record the initial dry gas meter
reading. Record the dry gas meter readings at the beginning and end of
each sampling time increment, when changes in flow rates are made,
before and after each leak check, and when sampling is halted. Take
other readings required by Figure 17-3 at least once at each sample
point during each time increment and additional readings when
significant changes (20 percent variation in velocity head readings)
necessitate additional adjustments in flow rate. Level and zero the
manometer. Because the manometer level and zero may drift due to
vibrations and temperature changes, make periodic checks during the
traverse.
Clean the portholes prior to the test run to minimize the chance of
sampling the deposited material. To begin sampling, remove the nozzle
cap and verify that the pitot tube and probe extension are properly
positioned. Position the nozzle at the first traverse point with the
tip pointing directly into the gas stream. Immediately start the pump
and adjust the flow to isokinetic conditions. Nomographs are available,
which aid in the rapid adjustment to the isokinetic sampling rate
without excessive computations. These nomographs are designed for use
when the Type S pitot tube coefficient is 0.85 0.02, and the stack gas
equivalent density (dry molecular weight) is equal to 29 4. APTD-0576
details the procedure for using the nomographs. If Cp and Md are
outside the above stated ranges, do not use the nomographs unless
appropriate steps (see Citation 7 in Bibliography) are taken to
compensate for the deviations.
When the stack is under significant negative pressure (height of
impinger stem), take care to close the coarse adjust valve before
inserting the probe extension assembly into the stack to prevent water
from being forced backward. If necessary, the pump may be turned on
with the coarse adjust valve closed.
When the probe is in position, block off the openings around the
probe and porthole to prevent unrepresentative dilution of the gas
stream.
Traverse the stack cross section, as required by Method 1 or as
specified by the Administrator, being careful not to bump the probe
nozzle into the stack walls when sampling near the walls or when
removing or inserting the probe extension through the portholes, to
minimize chance of extracting deposited material.
During the test run, take appropriate steps (e.g., adding crushed ice
to the impinger ice bath) to maintain a temperature of less than 20 C
(68 F) at the condenser outlet; this will prevent excessive moisture
losses. Also, periodically check the level and zero of the manometer.
If the pressure drop across the filter becomes too high, making
isokinetic sampling difficult to maintain, the filter may be replaced in
the midst of a sample run. It is recommended that another complete
filter holder assembly be used rather than attempting to change the
filter itself. Before a new filter holder is installed, conduct a leak
check, as outlined in Section 4.1.4.2. The total particulate weight
shall include the summation of all filter assembly catches.
A single train shall be used for the entire sample run, except in
cases where simultaneous sampling is required in two or more separate
ducts or at two or more different locations within the same duct, or, in
cases where equipment failure necessitates a change of trains. In all
other situations, the use of two or more trains will be subject to the
approval of the Administrator. Note that when two or more trains are
used, a separate analysis of the collected particulate from each train
shall be performed, unless identical nozzle sizes were used on all
trains, in which case the particulate catches from the individual trains
may be combined and a single analysis performed.
At the end of the sample run, turn off the pump, remove the probe
extension assembly from the stack, and record the final dry gas meter
reading. Perform a leak-check, as outlined in Section 4.1.4.3. Also,
leak-check the pitot lines as described in Section 3.1 of Method 2; the
lines must pass this leak-check, in order to validate the velocity head
data.
4.1.6 Calculation of Percent Isokinetic. Calculate percent
isokinetic (see Section 6.11) to determine whether another test run
should be made. If there is difficulty in maintaining isokinetic rates
due to source conditions, consult with the Administrator for possible
variance on the isokinetic rates.
4.2 Sample Recovery. Proper cleanup procedure begins as soon as the
probe extension assembly is removed from the stack at the end of the
sampling period. Allow the assembly to cool.
When the assembly can be safely handled, wipe off all external
particulate matter near the tip of the probe nozzle and place a cap over
it to prevent losing or gaining particulate matter. Do not cap off the
probe tip tightly while the sampling train is cooling down as this would
create a vacuum in the filter holder, forcing condenser water backward.
Before moving the sample train to the cleanup site, disconnect the
filter holder-probe nozzle assembly from the probe extension; cap the
open inlet of the probe extension. Be careful not to lose any
condensate, if present. Remove the umbilical cord from the condenser
outlet and cap the outlet. If a flexible line is used between the first
impinger (or condenser) and the probe extension, disconnect the line at
the probe extension and let any condensed water or liquid drain into the
impingers or condenser. Disconnect the probe extension from the
condenser; cap the probe extension outlet. After wiping off the
silicone grease, cap off the condenser inlet. Ground glass stoppers,
plastic caps, or serum caps (whichever are appropriate) may be used to
close these openings.
Transfer both the filter holder-probe nozzle assembly and the
condenser to the cleanup area. This area should be clean and protected
from the wind so that the chances of contaminating or losing the sample
will be minimized.
Save a portion of the acetone used for cleanup as a blank. Take 200
ml of this acetone directly from the wash bottle being used and place it
in a glass sample container labeled ''acetone blank.''
Inspect the train prior to and during disassembly and note any
abnormal conditions. Treat the samples as follows:
Container No. 1. Carefully remove the filter from the filter holder
and place it in its identified petri dish container. Use a pair of
tweezers and/or clean disposable surgical gloves to handle the filter.
If it is necessary to fold the filter, do so such that the particulate
cake is inside the fold. Carefully transfer to the petri dish any
particulate matter and/or filter fibers which adhere to the filter
holder gasket, by using a dry Nylon bristle brush and/or a sharp-edged
blade. Seal the container.
Container No. 2. Taking care to see that dust on the outside of the
probe nozzle or other exterior surfaces does not get into the sample,
quantitatively recover particulate matter or any condensate from the
probe nozzle, fitting, and front half of the filter holder by washing
these components with acetone and placing the wash in a glass container.
Distilled water may be used instead of acetone when approved by the
Administrator and shall be used when specified by the Administrator; in
these cases, save a water blank and follow Administrator's directions on
analysis. Perform the acetone rinses as follows:
Carefully remove the probe nozzle and clean the inside surface by
rinsing with acetone from a wash bottle and brushing with a Nylon
bristle brush. Brush until acetone rinse shows no visible particles,
after which make a final rinse of the inside surface with acetone.
Brush and rinse with acetone the inside parts of the fitting in a
similar way until no visible particles remain. A funnel (glass or
polyethylene) may be used to aid in transferring liquid washes to the
container. Rinse the brush with acetone and quantitatively collect
these washings in the sample container. Between sampling runs, keep
brushes clean and protected from contamination.
After ensuring that all joints are wiped clean of silicone grease (if
applicable), clean the inside of the front half of the filter holder by
rubbing the surfaces with a Nylon bristle brush and rinsing with
acetone. Rinse each surface three times or more if needed to remove
visible particulate. Make final rinse of the brush and filter holder.
After all acetone washings and particulate matter are collected in the
sample container, tighten the lid on the sample container so that
acetone will not leak out when it is shipped to the laboratory. Mark
the height of the fluid level to determine whether or not leakage
occurred during transport. Label the container to clearly identify its
contents.
Container No. 3. If silica gel is used in the condenser system for
mositure content determination, note the color of the gel to determine
if it has been completely spent; make a notation of its condition.
Transfer the silica gel back to its original container and seal. A
funnel may make it easier to pour the silica gel without spilling, and a
rubber policeman may be used as an aid in removing the silica gel. It
is not necessary to remove the small amount of dust particles that may
adhere to the walls and are difficult to remove. Since the gain in
weight is to be used for moisture calculations, do not use any water or
other liquids to transfer the silica gel. If a balance is available in
the field, follow the procedure for Container No. 3 under ''Analysis.''
Condenser Water. Treat the condenser or impinger water as follows:
make a notation of any color or film in the liquid catch. Measure the
liquid volume to within 1 ml by using a graduated cylinder or, if a
balance is available, determine the liquid weight to within 0.5 g.
Record the total volume or weight of liquid present. This information
is required to calculate the moisture content of the effluent gas.
Discard the liquid after measuring and recording the volume or weight.
4.3 Analysis. Record the data required on the example sheet shown in
Figure 17-4. Handle each sample container as follows:
Container No. 1. Leave the contents in the shipping container or
transfer the filter and any loose particulate from the sample container
to a tared glass weighing dish. Desiccate for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh to a constant weight and
report the results to the nearest 0.1 mg. For purposes of this Section,
4.3, the term ''constant weight'' means a difference of no more than 0.5
mg or 1 percent of total weight less tare weight, whichever is greater,
between two consecutive weighings, with no less than 6 hours of
desiccation time between weighings.
Alternatively, the sample may be oven dried at the average stack
temperature or 105 C (220 F), whichever is less, for 2 to 3 hours,
cooled in the desiccator, and weighed to a constant weight, unless
otherwise specified by the Administrator. The tester may also opt to
oven dry the sample at the average stack temperature or 105 C (220 F),
whichever is less, for 2 to 3 hours, weigh the sample, and use this
weight as a final weight.
Plant
Date
Run No.
Filter No.
Amount liquid lost during transport
Acetone blank volume, ml
Acetone wash volume, ml
Acetone blank concentration, mg/mg (Equation 17-4)
Acetone wash blank, mg (Equation 17-5)
Container No. 2. Note the level of liquid in the container and
confirm on the analysis sheet whether or not leakage occurred during
transport. If a noticeable amount of leakage has occurred, either void
the sample or use methods, subject to the approval of the Administrator,
to correct the final results. Measure the liquid in this container
either volumetrically to 1 ml or gravimetrically to 0.5 g. Transfer
the contents to a tared 250-ml beaker and evaporate to dryness at
ambient temperature and pressure. Desiccate for 24 hours and weigh to a
constant weight. Report the results to the nearest 0.1 mg.
Container No. 3. This step may be conducted in the field. Weigh the
spent silica gel (or silica gel plus impinger) to the nearest 0.5 g
using a balance.
''Acetone Blank'' Container. Measure acetone in this container
either volumetrically or gravimetrically. Transfer the acetone to a
tared 250-ml beaker and evaporate to dryness at ambient temperature and
pressure. Desiccate for 24 hours and weigh to a constant weight.
Report the results to the nearest 0.1 mg.
Note: At the option of the tester, the contents of Container No. 2
as well as the acetone blank container may be evaporated at temperatures
higher than ambient. If evaporation is done at an elevated temperature,
the temperature must be below the boiling point of the solvent; also,
to prevent ''bumping,'' the evaporation process must be closely
supervised, and the contents of the beaker must be swirled occasionally
to maintain an even temperature. Use extreme care, as acetone is highly
flammable and has a low flash point.
5. Calibration
Maintain a laboratory log of all calibrations.
5.1 Probe Nozzle. Probe nozzles shall be calibrated before their
initial use in the field. Using a micrometer, measure the inside
diameter of the nozzle to the nearest 0.025 mm (0.001 in.). Make three
separate measurements using different diameters each time, and obtain
the average of the measurements. The difference between the high and
low numbers shall not exceed 0.1 mm (0.004 in.). When nozzles become
nicked, dented, or corroded, they shall be reshaped, sharpened, and
recalibrated before use. Each nozzle shall be permanently and uniquely
identified.
5.2 Pitot Tube. If the pitot tube is placed in an interference-free
arrangement with respect to the other probe assembly components, its
baseline (isolated tube) coefficient shall be determined as outlined in
Section 4 of Method 2. If the probe assembly is not interference-free,
the pitot tube assembly coefficient shall be determined by calibration,
using methods subject to the approval of the Administrator.
5.3 Metering System. Before its initial use in the field, the
metering system shall be calibrated according to the procedure outlined
in APTD-0576. Instead of physically adjusting the dry gas meter dial
readings to correspond to the wet test meter readings, calibration
factors may be used to mathematically correct the gas meter dial
readings to the proper values.
Before calibrating the metering system, it is suggested that a
leak-check be conducted. For metering systems having diaphragm pumps,
the normal leak-check procedure will not detect leakages within the
pump. For these cases the following leak-check procedure is suggested:
make a 10-minute calibration run at 0.00057 m3/min (0.02 cfm); at the
end of the run, take the difference of the measured wet test meter and
dry gas meter volumes; divide the difference by 10, to get the leak
rate. The leak rate should not exceed 0.00057 m3/min (0.02 cfm).
After each field use, the calibration of the metering system shall be
checked by performing three calibration runs at a single, intermediate
orifice setting (based on the previous field test), with the vacuum set
at the maximum value reached during the test series. To adjust the
vacuum, insert a valve between the wet test meter and the inlet of the
metering system. Calculate the average value of the calibration factor.
If the calibration has changed by more than 5 percent, recalibrate the
meter over the full range of orifice settings, as outlined in APTD-0576.
Alternative procedures, e.g., using the orifice meter coefficients,
may be used, subject to the approval of the Administrator.
Note: If the dry gas meter coefficient values obtained before and
after a test series differ by more than 5 percent, the test series shall
either be voided, or calculations for the test series shall be performed
using whichever meter coefficient value (i.e., before or after) gives
the lower value of total sample volume.
5.4 Temperature Gauges. Use the procedure in Section 4.3 of Method 2
to calibrate in-stack temperature gauges. Dial thermometers, such as
are used for the dry gas meter and condenser outlet, shall be calibrated
against mercury-in-glass thermometers.
5.5 Leak Check of Metering System Shown in Figure 17-1. That portion
of the sampling train from the pump to the orifice meter should be leak
checked prior to initial use and after each shipment. Leakage after the
pump will result in less volume being recorded than is actually sampled.
The following procedure is suggested (see Figure 17-5). Close the main
valve on the meter box. Insert a one-hole rubber stopper with rubber
tubing attached into the orifice exhaust pipe. Disconnect and vent the
low side of the orifice manometer. Close off the low side orifice tap.
Pressurize the system to 13 to 18 cm (5 to 7 in.) water column by
blowing into the rubber tubing. Pinch off the tubing and observe the
manometer for one minute. A loss of pressure on the manometer indicates
a leak in the meter box; leaks, if present, must be corrected.
Insert illus. 1245
5.6 Barometer. Calibrate against a mercury barometer.
6. Calculations
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after the final
calculation. Other forms of the equations may be used as long as they
give equivalent results.
6.1 Nomenclature.
An=Cross-sectional area of nozzle, m2 (ft2).
Bws=Water vapor in the gas stream, proportion by volume.
Ca=Acetone blank residue concentration, mg/mg.
cs=Concentration of particulate matter in stack gas, dry basis,
corrected to standard conditions, g/dscm (g/dscf).
I=Percent of isokinetic sampling.
La=Maximum acceptable leakage rate for either a pretest leak check or
for a leak check following a component change; equal to 0.00057 m3/min
(0.02 cfm) or 4 percent of the average sampling rate, whichever is less.
Li=Individual leakage rate observed during the leak check conducted
prior to the ''ith'' component change (i=1, 2, 3 . . . n), m3/min (cfm).
Lp=Leakage rate observed during the post-test leak check, m3/min
(cfm).
ma=Mass of residue of acetone after evaporation, mg.
mn=Total amount of particulate matter collected, mg.
Mw=Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb-mole).
Pbar=Barometric pressure at the sampling site, mm Hg (in. Hg).
Ps=Absolute stack gas pressure, mm Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
R=Ideal gas constant, 0.06236 mm Hg-m3/ K-g-mole (21.85 in. Hg-ft3/
R-lb-mole).
Tm=Absolute average dry gas meter temperature (see Figure 17-3), K (
R).
Ts=Absolute average stack gas temperature (see Figure 17-3), K ( R).
Tstd=Standard absolute temperature, 293 K (528 R).
Va=Volume of acetone blank, ml.
Vaw=Volume of acetone used in wash, ml.
Vlc=Total volume of liquid collected in impingers and silica gel (see
Figure 17-4), ml.
Vm=Volume of gas sample as measured by dry gas meter, dcm (dcf).
Vm(std)=Volume of gas sample measured by the dry gas meter, corrected
to standard conditions, dscm (dscf).
Vw(std)=Volume of water vapor in the gas sample, corrected to
standard conditions, scm (scf).
vs=Stack gas velocity, calculated by Method 2, Equation 2-9, using
data obtained from Method 17, m/sec (ft/sec).
Wa=Weight of residue in acetone wash, mg.
Y=Dry gas meter calibration coefficient.
H=Average pressure differential across the orifice meter (see Figure
17-3), mm H2O (in. H2O).
a=Density of acetone, mg/ml (see label on bottle).
rw=Density of water, 0.9982 g/ml (0.002201 lb/ml).
=Total sampling time, min.
1=Sampling time interval, from the beginning of a run until the
first component change, min.
i=Sampling time interval, between two successive component changes,
beginning with the interval between the first and second changes, min.
p=Sampling time interval, from the final (nth) component change
until the end of the sampling run, min.
13.6=Specific gravity of mercury.
60=Sec/min.
100=Conversion to percent.
6.2 Average Dry Gas Meter Temperature and Average Orifice Pressure
Drop. See data sheet (Figure 17-3).
6.3 Dry Gas Volume. Correct the sample volume measured by the dry
gas meter to standard conditions (20 C, 760 mm Hg or 68 F, 29.92 in.
Hg) by using Equation 17-1.
Insert illus. 1249
Eq. 17-1
Where:
K1=0.3858 K/mm Hg for metric units; 17.64 R/in. Hg for English
units.
Note: Equation 17-1 can be used as written unless the leakage rate
observed during any of the mandatory leak checks (i.e., the post-test
leak check or leak checks conducted prior to component changes) exceeds
La. If Lp or Li exceeds La, Equation 17-1 must be modified as follows:
(a) Case I. No component changes made during sampling run. In this
case, replace Vm in Equation 17-1 with the expression:
(b) Case II. One or more component changes made during the sampling
run. In this case, replace Vm in Equation 17-1 by the expression:
Insert illus. 1250
and substitute only for those leakage rates (Li or Lp) which exceed
La.
6.4 Volume of Water Vapor.
Insert illus. 1251
Eq. 17-2
Where:
K2=0.001333 m3/ml for metric units; 0.04707 ft3/ml for English
units.
6.5 Moisture Content.
Eq. 17-3
6.6 Acetone Blank Concentration.
Eq. 17-4
6.7 Acetone Wash Blank.
Eq. 17-5
6.8 Total Particulate Weight. Determine the total particulate catch
from the sum of the weights obtained from Containers 1 and 2 less the
acetone blank (see Figure 17-4).
Note: Refer to Section 4.1.5 to assist in calculation of results
involving two or more filter assemblies or two or more sampling trains.
6.9 Particulate Concentration.
Eq. 17-6
6.10 Conversion Factors:
6.11 Isokinetic Variation.
6.11.1 Calculation from Raw Data.
Insert illus. 1254
Eq. 17-7
Where:
K3=0.003454 mm Hg-m3/ml- K for metric units; 0.002669 in.
Hg-ft3/ml- R for English units.
6.11.2 Calculation from Intermediate Values.
Insert illus. 1255
Eq. 17-8
Where:
K4=4.320 for metric units; 0.09450 for English units.
6.12 Acceptable Results. If I is less than 90 percent and greater
than 110 percent, the results are acceptable. If the results are low in
comparison to the standard and I is beyond the acceptable range, or, if
I is less than 90 percent, the Administrator may opt to accept the
results. Use Citation 4 in Bibliography to make judgments. Otherwise,
reject the results and repeat the test.
7. Bibliography
1. Addendum to Specifications for Incinerator Testing at Federal
Facilities. PHS, NCAPC. December 6, 1967.
2. Martin, Robert M., Construction Details of Isokinetic
Source-Sampling Equipment. Environmental Protection Agency. Research
Triangle Park, NC, APTD-0581. April, 1971.
3. Rom, Jerome J., Maintenance, Calibration, and Operation of
Isokinetic Source-Sampling Equipment. Environmental Protection Agency.
Research Triangle Park, NC APTD-0576. March, 1972.
4. Smith, W. S., R. T. Shigehara, and W. F. Todd. A Method of
Interpreting Stack Sampling Data. Paper Presented at the 63rd Annual
Meeting of the Air Pollution Control Association, St. Louis, MO June
14-19, 1970.
5. Smith, W. S., et al., Stack Gas Sampling Improved and Simplified
with New Equipment. APCA Paper No. 67-119. 1967.
6. Specifications for Incinerator Testing at Federal Facilities.
PHS, NCAPC. 1967.
7. Shigehara, R. T., Adjustments in the EPA Nomograph for Different
Pitot Tube Coefficients and Dry Molecular Weights. Stack Sampling News
2:4-11. October, 1974.
8. Vollaro, R. F., A Survey of Commercially Available
Instrumentation for the Measurement of Low-Range Gas Velocities. U.S.
Environmental Protection Agency, Emission Measurement Branch. Research
Triangle Park, NC, November, 1976 (unpublished paper).
9. Annual Book of ASTM Standards. Part 26. Gaseous Fuels; Coal and
Coke; Atmospheric Analysis. American Society for Testing and
Materials. Philadelphia, PA 1974. pp. 617-622.
10. Vollaro, R. F., Recommended Procedure for Sample Traverses in
Ducts Smaller than 12 Inches in Diameter. U.S. Environmental Protection
Agency, Emission Measurement Branch. Research Triangle Park, NC,
November, 1976.
40 CFR 60.748 Pt. 60, App. A, Meth. 18
Introduction
This method should not be attempted by persons unfamiliar with the
performance characteristics of gas chromatography, nor by those persons
who are unfamiliar with source sampling. Particular care should be
exercised in the area of safety concerning choice of equipment and
operation in potentially explosive atmospheres.
1. Applicability and Principle
1.1 Applicability. This method applies to the analysis of
approximately 90 percent of the total gaseous organics emitted from an
industrial source. It does not include techniques to identify and
measure trace amounts of organic compounds, such as those found in
building air and fugitive emission sources.
This method will not determine compounds that (1) are polymeric (high
molecular weight), (2) can polymerize before analysis, or (3) have very
low vapor pressures at stack or instrument conditions.
1.2 Principle.
The major organic components of a gas mixture are separated by gas
chromatography (GC) and individually quantified by flame ionization,
photoionization, electron capture, or other appropriate detection
principles.
The retention times of each separated component are compared with
those of known compounds under identical conditions. Therefore, the
analyst confirms the identity and approximate concentrations of the
organic emission components beforehand. With this information, the
analyst then prepares or purchases commercially available standard
mixtures to calibrate the GC under conditions identical to those of the
samples. The analyst also determines the need for sample dilution to
avoid detector saturation, gas stream filtration to eliminate
particulate matter, and prevention of moisture condensation.
2. Range and Sensitivity
2.1 Range. The range of this method is from about 1 part per million
(ppm) to the upper limit governed by GC detector saturation or column
overloading. The upper limit can be extended by diluting the stack
gases with an inert gas or by using smaller gas sampling loops.
2.2 Sensitivity. The sensitivity limit for a compound is defined as
the minimum detectable concentration of that compound, or the
concentration that produces a signal-to-noise ratio of three to one.
The minimum detectable concentration is determined during the presurvey
calibration for each compound.
3. Precision and Accuracy
Gas chromatographic techniques typically provide a precision of 5 to
10 percent relative standard deviation (RSD), but an experienced GC
operator with a reliable instrument can readily achieve 5 percent RSD.
For this method, the following combined GC/operator values are required.
(a) Precision. Duplicate analyses are within 5 percent of their mean
value.
(b) Accuracy. Analysis results of prepared audit samples are within
10 percent of preparation values.
4. Interferences
Resolution interferences that may occur can be eliminated by
appropriate GC column and detector choice or by shifting the retention
times through changes in the column flow rate and the use of temperature
programming.
The analytical system is demonstrated to be essentially free from
contaminants by periodically analyzing blanks that consist of
hydrocarbon-free air or nitrogen.
Sample cross-contamination that occurs when high-level and low-level
samples or standards are analyzed alternately, is best dealt with by
thorough purging of the GC sample loop between samples.
To assure consistent detector response, calibration gases are
contained in dry air. To adjust gaseous organic concentrations when
water vapor is present in the sample, water vapor concentrations are
determined for those samples, and a correction factor is applied.
5. Presurvey and Presurvey Sampling.
Perform a presurvey for each source to be tested. Refer to Figure
18-1. Some of the information can be collected from literature surveys
and source personnel. Collect gas samples that can be analyzed to
confirm the identities and approximate concentrations of the organic
emissions.
5.1 Apparatus. This apparatus list also applies to Sections 6 and 7.
5.1.1 Teflon Tubing. (Mention of trade names or specific products
does not constitute endorsement by the U.S. Environmental Protection
Agency.) Diameter and length determined by connection requirements of
cylinder regulators and the GC. Additional tubing is necessary to
connect the GC sample loop to the sample.
5.1.2 Gas Chromatograph. GC with suitable detector, columns,
temperature-controlled sample loop and valve assembly, and temperature
programable oven, if necessary. The GC shall achieve sensitivity
requirements for the compounds under study.
5.1.3 Pump. Capable of pumping 100 ml/min. For flushing sample loop.
5.1.4 Flowmeters. To measure flow rates.
5.1.5 Regulators. Used on gas cylinders for GC and for cylinder
standards.
5.1.6 Recorder. Recorder with linear strip chart is minimum
acceptable. Integrator (optional) is recommended.
5.1.7 Syringes. 0.5-ml, 1.0- and 10-microliter sizes, calibrated,
maximum accuracy (gas tight), for preparing calibration standards.
Other appropriate sizes can be used.
5.1.8 Tubing Fittings. To plumb GC and gas cylinders.
5.1.9 Septums. For syringe injections.
5.1.10 Glass Jars. If necessary, clean-colored glass jars with
Teflon-lined lids for condensate sample collection. Size depends on
volume of condensate.
5.1.11 Soap Film Flow Meter. To determine flow rates.
5.1.12 Tedlar Bags. 10- and 50-liter capacity, for preparation of
standards.
5.1.13 Dry Gas Meter with Temperature and Pressure Gauges. Accurate
to 2 percent, for perparation of gas standards.
5.1.14 Midget Impinger/Hot Plate Assembly. For preparation of gas
standards.
5.1.15 Sample Flasks. For presurvey samples, must have gas-tight
seals.
5.1.16 Adsorption Tubes. If necessary, blank tubes filled with
necessary adsorbent (charcoal, Tenax, XAD-2, etc.) for presurvey
samples.
5.1.17 Personnel Sampling Pump. Calibrated, for collecting adsorbent
tube presurvey samples.
5.1.18 Dilution System. Calibrated, the dilution system is to be
constructed following the specifications of an acceptable method.
5.1.19 Sample Probes. Pyrex or stainless steel, of sufficient length
to reach centroid of stack, or a point no closer to the walls than 1 m.
5.1.20 Barometer. To measure barometric pressure.
5.2 Reagents.
5.2.1 Deionized Distilled Water.
5.2.2 Methylene Dichloride.
5.2.3 Calibration Gases. A series of standards prepared for every
compound of interest.
5.2.4 Organic Compound Solutions. Pure (99.9 percent), or as pure as
can reasonably be obtained, liquid samples of all the organic compounds
needed to prepare calibration standards.
5.2.5 Extraction Solvents. For extraction of adsorbent tube samples
in preparation for analysis.
5.2.6 Fuel. As recommended by the manufacturer for operation of the
GC.
5.2.7 Carrier Gas. Hydrocarbon free, as recommended by the
manufacturer for operation of the detector and compatability with the
column.
5.2.8 Zero Gas. Hydrocarbon free air or nitrogen, to be used for
dilutions, blank preparation, and standard preparation.
5.3 Sampling.
5.3.1 Collection of Samples with Glass Sampling Flasks. Presurvey
samples can be collected in precleaned 250-ml double-ended glass
sampling flasks. Teflon stopcocks, without grease, are preferred.
Flasks should be cleaned as follows: Remove the stopcocks from both
ends of the flasks, and wipe the parts to remove any grease. Clean the
stopcocks, barrels, and receivers with methylene dichloride. Clean all
glass ports with a soap solution, then rinse with tap and deionized
distilled water. Place the flask in a cool glass annealing furnace and
apply heat up to 500 C. Maintain at this temperature for 1 hour.
After this time period, shut off and open the furnace to allow the flask
to cool. Grease the stopcocks with stopcock grease and return them to
the flask receivers. Purge the assembly with high-purity nitrogen for 2
to 5 minutes. Close off the stopcocks after purging to maintain a
slight positive nitrogen pressure. Secure the stopcocks with tape.
Presurvey samples can be obtained either by drawing the gases into
the previously evacuated flask or by drawing the gases into and purging
the flask with a rubber suction bulb.
5.3.1.1 Evacuated Flask Procedure. Use a high-vacuum pump to
evacuate the flask to the capacity of the pump; then close off the
stopcock leading to the pump. Attach a 6-mm outside diameter (OD) glass
tee to the flask inlet with a short piece of Teflon tubing. Select a
6-mm OD borosilicate sampling probe, enlarged at one end to a 12-mm OD
and of sufficient length to reach the centroid of the duct to be
sampled. Insert a glass wool plug in the enlarged end of the probe to
remove particulate matter. Attach the other end of the probe to the tee
with a short piece of Teflon tubing. Connect a rubber suction bulb to
the third leg of the tee. Place the filter end of the probe at the
centroid of the duct, or at a point no closer to the walls than 1 m, and
purge the probe with the rubber suction bulb. After the probe is
completely purged and filled with duct gases, open the stopcock to the
grab flask until the pressure in the flask reaches duct pressure. Close
off the stopcock, and remove the probe from the duct. Remove the tee
from the flask and tape the stopcocks to prevent leaks during shipment.
Measure and record the duct temperature and pressure.
5.3.1.2 Purged Flask Procedure. Attach one end of the sampling flask
to a rubber suction bulb. Attach the other end to a 6-mm OD glass probe
as described in Section 5.3.1.1. Place the filter end of the probe at
the centroid of the duct, or at a point no closer to the walls than 1 m,
and apply suction with the bulb to completely purge the probe and flask.
After the flask has been purged, close off the stopcock near the
suction bulb, and then close the stopcock near the probe. Remove the
probe from the duct, and disconnect both the probe and suction bulb.
Tape the stopcocks to prevent leakage during shipment. Measure and
record the duct temperature and pressure.
5.3.2 Flexible Bag Procedure. Tedlar or aluminized Mylar bags can
also be used to obtain the presurvey sample. Use new bags, and leak
check them before field use. In addition, check the bag before use for
contamination by filling it with nitrogen or air, and analyzing the gas
by GC at high sensitivity. Experience indicates that it is desirable to
allow the inert gas to remain in the bag about 24 hours or longer to
check for desorption of organics from the bag. Follow the leak check
and sample collection procedures given in Section 7.1.
5.3.3 Determination of Moisture Content. For combustion or
water-controlled processes, obtain the moisture content from plant
personnel or by measurement during the presurvey. If the source is
below 59 C, measure the wet bulb and dry bulb temperatures, and
calculate the moisture content using a psychrometric chart. At higher
temperatures, use Method 4 to determine the moisture content.
5.4 Determination of Static Pressure. Obtain the static pressure
from the plant personnel or measurement. If a type S pitot tube and an
inclined manometer are used, take care to align the pitot tube 90 from
the direction of the flow. Disconnect one of the tubes to the
manometer, and read the static pressure; note whether the reading is
positive or negative.
5.5 Collection of Presurvey Samples with Adsorption Tube. Follow
Section 7.4 for presurvey sampling.
6. Analysis Development
6.1 Selection of GC Parameters.
6.1.1 Column Choice. Based on the initial contact with plant
personnel concerning the plant process and the anticipated emissions,
choose a column that provides good resolution and rapid analysis time.
The choice of an appropriate column can be aided by a literature search,
contact with manufacturers of GC columns, and discussion with personnel
at the emission source.
Most column manufacturers keep excellent records of their products.
Their technical service departments may be able to recommend appropriate
columns and detector type for separating the anticipated compounds, and
they may be able to provide information on interferences, optimum
operating conditions, and column limitations.
Plants with analytical laboratories may also be able to provide
information on appropriate analytical procedures.
6.1.2 Preliminary GC Adjustment. Using the standards and column
obtained in Section 6.1.1, perform initial tests to determine
appropriate GC conditions that provide good resolution and minimum
analysis time for the compounds of interest.
6.1.3 Preparation of Presurvey Samples. If the samples were
collected on an adsorbent, extract the sample as recommended by the
manufacturer for removal of the compounds with a solvent suitable to the
type of GC analysis. Prepare other samples in an appropriate manner.
6.1.4 Presurvey Sample Analysis. Before analysis, heat the presurvey
sample to the duct temperature to vaporize any condensed material.
Analyze the samples by the GC procedure, and compare the retention times
against those of the calibration samples that contain the components
expected to be in the stream. If any compounds cannot be identified
with certainty by this procedure, identify them by other means such as
GC/mass spectroscopy (GC/MS) or GC/infrared techniques. A GC/MS system
is recommended.
Use the GC conditions determined by the procedures of Section 6.1.2
for the first injection. Vary the GC parameters during subsequent
injections to determine the optimum settings. Once the optimum settings
have been determined, perform repeat injections of the sample to
determine the retention time of each compound. To inject a sample, draw
sample through the loop at a constant rate (100 ml/min for 30 seconds).
Be careful not to pressurize the gas in the loop. Turn off the pump and
allow the gas in the sample loop to come to ambient pressure. Activate
the sample valve, and record injection time, loop temperature, column
temperature, carrier flow rate, chart speed, and attenuator setting.
Calculate the retention time of each peak using the distance from
injection to the peak maximum divided by the chart speed. Retention
times should be repeatable within 0.5 seconds.
If the concentrations are too high for appropriate detector response,
a smaller sample loop or dilutions may be used for gas samples, and, for
liquid samples, dilution with solvent is appropriate. Use the standard
curves (Section 6.3) to obtain an estimate of the concentrations.
Identify all peaks by comparing the known retention times of
compounds expected to be in the retention times of peaks in the sample.
Identify any remaining unidentified peaks which have areas larger than 5
percent of the total using a GC/MS, or estimation of possible compounds
by their retention times compared to known compounds, with confirmation
by further GC analysis.
6.2 Calibration Standards. Prepare or obtain enough calibration
standards so that there are three different concentrations of each
organic compound expected to be measured in the source sample. For each
organic compound, select those concentrations that bracket the
concentrations expected in the source samples. A calibration standard
may contain more than one organic compound. If available, commercial
cylinder gases may be used if their concentrations have been certified
by direct analysis.
If samples are collected in adsorbent tubes (charcoal, XAD-2, Tenax,
etc.), prepare or obtain standards in the same solvent used for the
sample extraction procedure. Refer to Section 7.4.3.
Verify the stability of all standards for the time periods they are
used. If gas standards are prepared in the laboratory, use one or more
of the following procedures.
6.2.1 Preparation of Standards from High Concentration Cylinder
Standards. Obtain enough high concentration cylinder standards to
represent all the organic compounds expected in the source samples.
Use these high concentration standards to prepare lower concentration
standards by dilution, as shown by Figures 18-5 and 18-6.
To prepare the diluted calibration samples, calibrated rotameters are
normally used to meter both the high concentration calibration gas and
the diluent gas. Other types of flowmeters and commercially available
dilution systems can also be used.
Calibrate each flowmeter before use by placing it between the diluent
gas supply and suitably sized bubble meter, spirometer, or wet test
meter. Record all data shown on Figure 18-4. While it is desirable to
calibrate the cylinder gas flowmeter with cylinder gas, the available
quantity and cost may preclude it. The error introduced by using the
diluent gas for calibration is insignificant for gas mixtures of up to
1,000 to 2,000 ppm of each organic component.
Once the flowmeters are calibrated, connect the flowmeters to the
calibration and diluent gas supplies using 6-mm Teflon tubing. Connect
the outlet side of the flowmeters through a connector to a leak-free
Tedlar bag as shown in Figure 18-5. (See Section 7.1 for bag leak-check
procedures.) Adjust the gas flow to provide the desired dilution, and
fill the bag with sufficient gas for GC calibration. Be careful not to
overfill and cause the bag to apply additional pressure on the dilution
system. Record the flow rates of both flowmeters, and the laboratory
temperature and atmospheric pressure. Calculate the concentration Cs in
ppm of each organic in the diluted gas as follows:
Insert illus. 444a
where:
10 /6/ =Conversion to ppm.
X=Mole or volume fraction of the organic in the calibration gas to be
diluted.
qc=Flow rate of the calibration gas to be diluted.
qd=Diluent gas flow rate.
Single-stage dilutions should be used to prepare calibration mixtures
up to about 1:20 dilution factor.
For greater dilutions, a double dilution system is recommended, as
shown in Figure 18-6. Fill the Tedlar bag with the dilute gas from the
second stage. Record the laboratory temperature, barometric pressure,
and static pressure readings. Correct the flow reading for temperature
and pressure. Calculate the concentration Cs in ppm of the organic in
the final gas mixture as follows:
Insert illus. 445a
Where:
10 /6/ =Conversion to ppm.
X=Mole or volume fraction of the organic in the calibration gas to be
diluted.
qc1=Flow rate of the calibration gas to be diluted in stage 1.
qc2=Flow rate of the calibration gas to be diluted in stage 2.
qd1=Flow rate of diluent gas in stage 1.
qd2=Flow rate of diluent gas in stage 2.
Further details of the calibration methods for flowmeters and the
dilution system can be found in Citation 21 in the Bibliography.
6.2.2 Preparation of Standards from Volatile Materials. Record all
data shown on Figure 18-3.
6.2.2.1 Gas Injection Technique. This procedure is applicable to
organic compounds that exist entirely as a gas at ambient conditions.
Evacuate a 10-liter Tedlar bag that has passed a leak-check (see Section
7.1), and meter in 5.0 liters of air or nitrogen through a dry gas meter
that has been calibrated in a manner consistent with the procedure
described in Section 5.1.1 of Method 5. While the bag is filling use a
0.5-ml syringe to inject a known quantity of ''pure'' gas of the organic
compound through the wall of the bag, or through a septum-capped tee at
the bag inlet. Withdraw the syringe needle, and immediately cover the
resulting hole with a piece of masking tape. In a like manner, prepare
dilutions having other concentrations. Prepare a minimum of three
concentrations. Place each bag on a smooth surface, and alternately
depress opposite sides of the bag 50 times to mix the gases Record the
average meter temperature and pressure, the gas volume and the
barometric pressure. Record the syringe temperature and pressure before
injection.
Calculate each organic standard concentration Cs in ppm as follows:
Insert illus. 446a
where:
Gv=Gas volume or organic compound injected, ml.
106=Conversion to ppm.
Ps=Absolute pressure of syringe before injection, mm Hg.
Ts=Absolute temperature of syringe before injection, K.
Vm=Gas volume indicated by dry gas meter, liters.
Y=Dry gas meter calibration factor, dimensionless.
Pm=Absolute pressure of dry gas meter, mm Hg.
Tm=Absolute temperature of dry gas meter, K.
1000=Conversion factor, ml/liter.
6.2.2.2 Liquid Injection Technique. Use the equipment shown in
Figure 18-8. Calibrate the dry gas meter as described in Section
6.2.2.1 with a wet test meter or a spirometer. Use a water manometer
for the pressure gauge and glass, Teflon, brass, or stainless steel for
all connections. Connect a valve to the inlet of the 50-liter Tedlar
bag.
To prepare the standards, assemble the equipment as shown in Figure
18-8, and leak-check the system. Completely evacuate the bag. Fill the
bag with hydrocarbon-free air, and evacuate the bag again. Close the
inlet valve.
Turn on the hot plate, and allow the water to reach boiling, Connect
the bag to the impinger outlet. Record the initial meter reading, open
the bag inlet valve, and open the cylinder. Adjust the rate so that the
bag will be completely filled in approximately 15 minutes. Record meter
pressure and temperature, and local barometric pressure.
Allow the liquid organic to equilibrate to room temperature. Fill
the 1.0- or 10-microliter syringe to the desired liquid volume with the
organic. Place the syringe needle into the impinger inlet using the
septum provided, and inject the liquid into the flowing air stream. Use
a needle of sufficient length to permit injection of the liquid below
the air inlet branch of the tee. Remove the syringe.
When the bag is filled, stop the pump, and close the bag inlet valve.
Record the final meter reading, temperature, and pressure.
Disconnect the bag from the impinger outlet, and either set it aside
for at least 1 hour, or massage the bag to insure complete mixing.
Measure the solvent liquid density at room temperature by accurately
weighing a known volume of the material on an analytical balance to the
nearest 1.0 milligram. A ground-glass stoppered 25-mil volumetric flask
or a glass-stoppered specific gravity bottle is suitable for weighing.
Calculate the result in terms of g/ml. As an alternative, literature
values of the density of the liquid at 20 C may be used.
Calculate each organic standard concentration Cs in ppm as follows:
Insert illus. 448a
where:
Lv=Liquid volume of organic injected, ml.
ml=Liquid organic density as determined, g/ml.
M=Molecular weight of organic, g/g-mole.
24.055=Ideal gas molar volume at 293 K and 760 mm Hg, liters/g-mole.
106=Conversion to ppm.
1000=Conversion factor, ml/ml.
6.3 Preparation of Calibration Curves. Establish proper GC
conditions, then flush the sampling loop for 30 seconds at a rate of 100
ml/min. Allow the sample loop pressure to equilibrate to atmospheric
pressure, and activate the injection valve. Record the standard
concentration, attenuator factor, injection time, chart speed, retention
time, peak area, sample loop temperature, column temperature, and
carrier gas flow rate. Repeat the standard injection until two
consecutive injections give area counts within 5 percent of their
average. The average value multipled by the attenuator factor is then
the calibration area value for the concentration.
Repeat this procedure for each standard. Prepare a graphical plot of
concentration (Cs) versus the calibration area values. Perform a
regression analysis, and draw the least squares line.
6.4 Relative Response Factors. The calibration curve generated from
the standards for a single organic can usually be related to each of the
individual GC response curves that are developed in the laboratory for
all the compounds in the source. In the field, standards for that
single organic can then be used to ''calibrate'' the GC for all the
organics present. This procedure should first be confirmed in the
laboratory by preparing and analyzing calibration standards containing
multiple organic compounds.
6.5 Quality Assurance for Laboratory Procedures. Immediately after
the preparation of the calibration curves and prior to the presurvey
sample analysis, the analysis audit described in 40 CFR Part 61,
Appendix C, Procedure 2: ''Procedure for Field Auditing GC Analysis,''
should be performed. The information required to document the analysis
of the audit samples has been included on the example data sheets shown
in Figures 18-3 and 18-7. The audit analyses should agree with the
audit concentrations within 10 percent. When available, the tester may
obtain audit cylinders by contacting: U.S. Environmental Protection
Agency, Environmental Monitoring Systems Laboratory, Quality Assurance
Division (MD-77), Research Triangle Park, North Carolina 27711. Audit
cylinders obtained from a commercial gas manufacturer may be used
provided that (a) the gas manufacturer certifies the audit cylinder in a
manner similar to the procedure described in 40 CFR Part 61, Appendix B,
Method 106, Section 5.2.3.1, and (b) the gas manufacturer obtains an
independent analysis of the audit cylinders to verify this analysis.
Independent analysis is defined as an analysis performed by an
individual other than the individual who performs the gas manufacturer's
analysis, while using calibration standards and analysis equipment
different from those used for the gas manufacturer's analysis.
Verification is complete and acceptable when the independent analysis
concentration is within 5 percent of the gas manufacturer's
concentration.
7. Final Sampling and Analysis Procedure
Considering safety (flame hazards) and the source conditions, select
an appropriate sampling and analysis procedure (Section 7.1, 7.2, 7.3,
or 7.4). In situations where a hydrogen flame is a hazard and no
intrinsically safe GC is suitable, use the flexible bag collection
technique or an adsorption technique. If the source temperature is
below 100 C, and the organic concentrations are suitable for the
detector to be used, use the direct interface method. If the source
gases require dilution, use a dilution interface and either the bag
sample or adsorption tubes. The choice between these two techniques
will depend on the physical layout of the site, the source temperature,
and the storage stability of the compounds if collected in the bag.
Sample polar compounds by direct interfacing or dilution interfacing to
prevent sample loss by adsorption on the bag.
7.1 Integrated Bag Sampling and Analysis.
7.1.1 Evacuated Container Sampling Procedure. In this procedure, the
bags are filled by evacuating the rigid air-tight containers that hold
the bags. Use a field sample data sheet as shown in Figure 18-10.
Collect triplicate sample from each sample location.
7.1.1.1 Apparatus.
7.1.1.1.1 Probe. Stainless steel, Pyrex glass, or Teflon tubing
probe, according to the duct temperature, with 6.4-mm OD Teflon tubing
of sufficient length to connect to the sample bag. Use stainless steel
or Teflon unions to connect probe and sample line.
7.1.1.1.2 Quick Connects. Male (2) and female (2) of stainless steel
construction.
7.1.1.1.3 Needle Valve. To control gas flow.
7.1.1.1.4 Pump. Leakless Teflon-coated diaphragm-type pump or
equivalent. To deliver at least 1 liter/min.
7.1.1.1.5 Charcoal Adsorption Tube. Tube filled with activated
charcoal, with glass wool plugs at each end, to adsorb organic vapors.
7.1.1.1.6 Flowmeter. 0 to 500-ml flow range; with manufacturer's
calibration curve.
7.1.1.2 Sampling Procedure. To obtain a sample, assemble the sample
train as shown in Figure 18-9. Leak check both the bag and the
container. Connect the vacuum line from the needle valve to the Teflon
sample line from the probe. Place the end of the probe at the centroid
of the stack, or at a point no closer to the walls than 1 m, and start
the pump with the needle valve adjusted to yield a flow of 0.5
liter/minute. After allowing sufficient time to purge the line several
times, connect the vacuum line to the bag, and evacuate until the
rotameter indicates no flow. Then position the sample and vacuum lines
for sampling, and begin the actual sampling, keeping the rate
proportional to the stack velocity. As a precaution, direct the gas
exiting the rotameter away from sampling personnel. At the end of the
sample period, shut off the pump, disconnect the sample line from the
bag, and disconnect the vacuum line from the bag container, Record the
source temperature, barometric pressure, ambient temperature, sampling
flow rate, and initial and final sampling time on the data sheet shown
in Figure 18-10. Protect the Tedlar bag and its container from
sunlight. When possible, perform the analysis within 2 hours of sample
collection.
7.1.2 Direct Pump Sampling Procedure. Follow 7.1.1, except place the
pump and needle valve between the probe and the bag. Use a pump and
needle valve constructed of stainless steel or some other material not
affected by the stack gas. Leak check the system, and then purge with
stack gas before the connecting to the previously evacuated bag.
7.1.3 Explosion Risk Area Bag Sampling Procedure. Follow 7.1.1
except replace the pump with another evacuated can (see Figure 18-9a).
Use this method whenever there is a possibility of an explosion due to
pumps, heated probes, or other flame producing equipment.
7.1.4 Other Modified Bag Sampling Procedures. In the event that
condensation is observed in the bag while collecting the sample and a
direct interface system cannot be used, heat the bag during collection,
and maintain it at a suitably elevated temperature during all subsequent
operations. (Note: Take care to leak check the system prior to the
dilutions so as not to create a potentially explosive atmosphere.) As an
alternative, collect the sample gas, and simultaneously dilute it in the
Tedlar bag.
In the first procedure, heat the box containing the sample bag to the
source temperature, provided the components of the bag and the
surrounding box can withstand this temperature. Then transport the bag
as rapidly as possible to the analytical area while maintaining the
heating, or cover the box with an insulating blanket. In the analytical
area, keep the box heated to source temperature until analysis. Be sure
that the method of heating the box and the control for the heating
circuit are compatible with the safety restrictions required in each
area.
To use the second procedure, prefill the Tedlar bag with a known
quantity of inert gas. Meter the inert gas into the bag according to
the procedure for the preparation of gas concentration standards of
volatile liquid materials (Section 6.2.2.2), but eliminate the midget
impinger section. Take the partly filled bag to the source, and meter
the source gas into the bag through heated sampling lines and a heated
flowmeter, or Teflon positive displacement pump. Verify the dilution
factors periodically through dilution and analysis of gases of known
concentration.
7.1.5 Analysis of Bag Samples.
7.1.5.1 Apparatus. Same as Section 5. A minimum of three gas
standards are required.
7.1.5.2 Procedure. Establish proper GC operating conditions as
described in Section 6.3, and record all data listed in Figure 18-7.
Prepare the GC so that gas can be drawn through the sample valve. Flush
the sample loop with gas from one of the three calibration mixtures, and
activate the valve. Obtain at least two chromatograms for the mixture.
The results are acceptable when the peak areas from two consecutive
injections agree to within 5 percent of their average. If they do not,
run additional analyses or correct the analytical techniques until this
requirement is met. Then analyze the other two calibration mixtures in
the same manner. Prepare a calibration curve as described in the same
manner. Prepare a calibration curve as described in Section 6.3.
Analyze the source gas samples by connecting each bag to the sampling
valve with a piece of Teflon tubing identified for that bag. Follow the
specifications on replicate analyses specified for the calibration
gases. Record the data listed in Figure 18-11. If certain items do not
apply, use the notation ''N.A.'' After all samples have been analyzed,
repeat the analyses of the calibration gas mixtures, and generate a
second calibration curve. Use an average of the two curves to determine
the sample gas concentrations. If the two calibration curves differ by
more than 5 percent from their mean value, then report the final results
by comparison to both calibration curves.
7.1.6 Determination of Bag Water Vapor Content. Measure and record
the ambient temperature and barometric pressure near the bag. From a
water saturation vapor pressure table, determine and record the water
vapor content as a decimal figure. (Assume the relative humidity to be
100 percent unless a lesser value is known.) If the bag has been
maintained at an elevated temperature as described in Section 7.1.4,
determine the stack gas water content by Method 4.
7.1.7 Quality Assurance. Immediately prior to the analysis of the
stack gas samples, perform audit analyses as described in Section 6.5.
The audit analyses must agree with the audit concentrations within 10
percent. If the results are acceptable, proceed with the analyses of
the source samples. If they do not agree within 10 percent, then
determine the reason for the discrepancy, and take corrective action
before proceeding.
7.1.8 Emission Calculations. From the average calibration curve
described in Section 7.1.5., select the value of Cs that corresponds to
the peak area. Calculate the concentration Cc in ppm, dry basis, of
each organic in the sample as follows:
Insert Illus 452a
where:
Cs=Concentration of the organic from the calibration curve, ppm.
Pr=Reference pressure, the barometric pressure or absolute sample
loop pressure recorded during calibration, mm Hg.
Ti=Sample loop temperature at the time of sample analysis, K.
Fr=Relative response factor (if applicable, see Section 6.4).
Pi=Barometric or absolute sample loop pressure at time of sample
analysis, mm Hg.
Tr=Reference temperature, the termperature of the sample loop
recorded during calibration, K.
Bws=Water vapor content of the bag sample or stack gas, proportion by
volume.
7.2 Direct Interface Sampling and Analysis Procedure. The direct
interface procedure can be used provided that the moisture content of
the gas does not interfere with the analysis procedure, the physical
requirements of the equipment can be met at the site, and the source gas
concentration is low enough that detector saturation is not a problem.
Adhere to all safety requirements with this method.
7.2.1 Apparatus.
7.2.1.1 Probe. Constructed of stainless steel, Pyrex glass, or Teflon
tubing as required by duct temperature, 6.4-mm OD, enlarged at duct end
to contain glass wool plug. If necessary, heat the probe with heating
tape or a special heating unit capable of maintaining duct temperature.
7.2.1.2 Sample Lines. 6.4-mm OD Teflon lines, heat-traced to prevent
condensation of material.
7.2.1.3 Quick Connects. To connect sample line to gas sampling valve
on GC instrument and to pump unit used to withdraw source gas. Use a
quick connect or equivalent on the cylinder or bag containing
calibration gas to allow connection of the calibration gas to the gas
sampling valve.
7.2.1.4 Thermocouple Readout Device. Potentiometer or digital
thermometer, to measure source temperature and probe temperature.
7.2.1.5 Heated Gas Sampling Valve. Of two-position, six-port design,
to allow sample loop to be purged with source gas or to direct source
gas into the GC instrument.
7.2.1.6 Needle Valve. To control gas sampling rate from the source.
7.2.1.7 Pump. Leakless Teflon-coated diaphragm-type pump or
equivalent, capable of at least 1 liter/minute sampling rate.
7.2.1.8 Flowmeter. Of suitable range to measure sampling rate.
7.2.1.9 Charcoal Adsorber. To adsorb organic vapor collected from
the source to prevent exposure of personnel to source gas.
7.2.1.10 Gas Cylinders. Carrier gas (helium or nitrogen), and oxygen
and hydrogen for a flame ionization detector (FID) if one is used.
7.2.1.11 Gas Chromatograph. Capable of being moved into the field,
with detector, heated gas sampling valve, column required to complete
separation of desired components, and option for temperature
programming.
7.2.1.12 Recorder/Integrator. To record results.
7.2.2 Procedure. To obtain a sample, assemble the sampling system as
shown in Figure 18-12. Make sure all connections are tight. Turn on
the probe and sample line heaters. As the temperature of the probe and
heated line approaches the source temperature as indicated on the
thermocouple readout device, control the heating to maintain a
temperature of 0 to 3 C above the source temperature. While the probe
and heated line are being heated, disconnect the sample line from the
gas sampling valve, and attach the line from the calibration gas
mixture. Flush the sample loop with calibration gas and analyze a
portion of that gas. Record the results. After the calibration gas
sample has been flushed into the GC instrument, turn the gas sampling
valve to flush position, then reconnect the probe sample line to the
valve. Place the inlet of the probe at the centroid of the duct, or at
a point no closer to the walls than 1 m, and draw source gas into the
probe, heated line, and sample loop. After thorough flushing, analyze
the sample using the same conditions as for the calibration gas mixture.
Repeat the analysis on an additional sample. Measure the peak areas
for the two samples, and if they do not agree to within 5 percent of
their mean value, analyze additional samples until two consecutive
analyses meet this criteria. Record the data. After consistent results
are obtained, remove the probe from the source and analyze a second
calibration gas mixture. Record this calibration data and the other
required data on the data sheet shown in Figure 18-11, deleting the
dilution gas information.
(Note: Take care to draw all samples, calibration mixtures, and
audits through the sample loop at the same pressure.)
7.2.3 Determination of Stack Gas Moisture Content. Use Method 4 to
measure the stack gas moisture content.
7.2.4 Quality Assurance. Same as Section 7.1.7. Introduce the audit
gases in the sample line immediately following the probe.
7.2.5 Emission Calculations. Same as Section 7.1.8.
7.3 Dilution Interface Sampling and Analysis Procedure. Source
samples that contain a high concentration of organic materials may
require dilution prior to analysis to prevent saturating the GC
detector. The apparatus required for this direct interface procedure is
basically the same as that described in the Section 7.2, except a
dilution system is added between the heated sample line and the gas
sampling valve. The apparatus is arranged so that either a 10:1 or
100:1 dilution of the source gas can be directed to the chromatograph.
A pump of larger capacity is also required, and this pump must be heated
and placed in the system between the sample line and the dilution
apparatus.
7.3.1 Apparatus. The equipment required in addition to that specified
for the direct interface system is as follows:
7.3.1.1 Sample Pump. Leakless Teflon-coated diaphragm-type that can
withstand being heated to 120 C and deliver 1.5 liters/minute.
7.3.1.2 Dilution Pumps. Two Model A-150 Komhyr Teflon positive
displacement type delivering 150 cc/minute, or equivalent. As an
option, calibrated flowmeters can be used in conjunction with
Teflon-coated diaphragm pumps.
7.3.1.3 Valves. Two Teflon three-way valves, suitable for connecting
to 6.4-mm OD Teflon tubing.
7.3.1.4 Flowmeters. Two, for measurement of diluent gas, expected
delivery flow rate to be 1,350 cc/min.
7.3.1.5 Diluent Gas with Cylinders and Regulators. Gas can be
nitrogen or clean dry air, depending on the nature of the source gases.
7.3.1.6 Heated Box. Suitable for being heated to 120 C, to contain
the three pumps, three-way valves, and associated connections. The box
should be equipped with quick connect fittings to facilitate connection
of: (1) The heated sample line from the probe, (2) the gas sampling
valve, (3) the calibration gas mixtures, and (4) diluent gas lines. A
schematic diagram of the components and connections is shown in Figure
18-13.
(Note: Care must be taken to leak check the system prior to the
dilutions so as not to create a potentially explosive atmosphere.)
The heated box shown in Figure 18-13 is designed to receive a heated
line from the probe. An optional design is to build a probe unit that
attaches directly to the heated box. In this way, the heated box
contains the controls for the probe heaters, or, if the box is placed
against the duct being sampled, it may be possible to eliminate the
probe heaters. In either case, a heated Teflon line is used to connect
the heated box to the gas sampling valve on the chromatograph.
7.3.2 Procedure. Assemble the apparatus by connecting the heated box,
shown in Figure 18-13, between the heated sample line from the probe and
the gas sampling valve on the chromatograph. Vent the source gas from
the gas sampling valve directly to the charcoal filter, eliminating the
pump and rotameter. Heat the sample probe, sample line, and heated box.
Insert the probe and source thermocouple to the centroid of the duct,
or to a point no closer to the walls than 1 m. Measure the source
temperature, and adjust all heating units to a temperature 0 to 3 C
above this temperature. If this temperature is above the safe operating
temperature of the Teflon components, adjust the heating to maintain a
temperature high enough to prevent condensation of water and organic
compounds. Verify the operation of the dilution system by analyzing a
high concentration gas of known composition through either the 10:1 or
100:1 dilution stages, as appropriate. (If necessary, vary the flow of
the diluent gas to obtain other dilution ratios.) Determine the
concentration of the diluted calibration gas using the dilution factor
and the calibration curves prepared in the laboratory. Record the
pertinent data on the data sheet shown in Figure 18-11. If the data on
the diluted calibration gas are not within 10 percent of the expected
values, determine whether the chromatograph or the dilution system is in
error, and correct it. Verify the GC operation using a low
concentration standard by diverting the gas into the sample loop,
bypassing the dilution system. If these analyses are not within
acceptable limits, correct the dilution system to provide the desired
dilution factors. Make this correction by diluting a high-concentration
standard gas mixture to adjust the dilution ratio as required.
Once the dilution system and GC operations are satisfactory, proceed
with the analysis of source gas, maintaining the same dilution settings
as used for the standards. Repeat the analyses until two consecutive
values do not vary by more than 5 percent from their mean value are
obtained.
Repeat the analysis of the calibration gas mixtures to verify
equipment operation. Analyze the two field audit samples using either
the dilution system, or directly connect to the gas sampling valve as
required. Record all data and report the results to the audit
supervisor.
7.3.3 Determination of Stack Gas Moisture Content. Same as Section
7.2.3.
7.3.4 Quality Assurance. Same as Section 7.2.4.
7.3.5 Emission Calculations. Same as Section 7.2.5, with the
dilution factor applied.
7.4 Adsorption Tube Procedure (Alternative Procedure). It is
suggested that the tester refer to the National Institute of
Occupational Safety and Health (NIOSH) method for the particular
organics to be sampled. The principal interferent will be water vapor.
If water vapor is present at concentrations above 3 percent, silica gel
should be used in front of the charcoal. Where more than one compound
is present in the emissions, then develop relative adsorptive capacity
information.
7.4.1 Additional Apparatus. In addition to the equipment listed in
the NIOSH method for the particular organic(s) to be sampled, the
following items (or equivalent) are suggested.
7.4.1.1 Probe (Optional). Borosilicate glass or stainless steel,
approximately 6-mm ID, with a heating system if water condensation is a
problem, and a filter (either in-stack or out-stack heated to stack
temperature) to remove particulate matter. In most instances, a plug of
glass wool is a satisfactory filter.
7.4.1.2 Flexible Tubing. To connect probe to adsorption tubes. Use
a material that exhibits minimal sample adsorption.
7.4.1.3 Leakless Sample Pump. Flow controlled, constant rate pump,
with a set of limiting (sonic) orifices to provide pumping rates from
approximately 10 to 100 cc/min.
7.4.1.4 Bubble-Tube Flowmeter. Volume accuracy within 1 percent,
to calibrate pump.
7.4.1.5 Stopwatch. To time sampling and pump rate calibration.
7.4.1.6 Adsorption Tubes. Similar to ones specified by NIOSH, except
the amounts of adsorbent per primary/backup sections are 800/200 mg for
charcoal tubes and 1040/260 mg for silica gel tubes. As an alternative,
the tubes may contain a porous polymer adsorbent such as Tenax GC or
XAD-2.
7.4.1.7 Barometer. Accurate to 5 mm Hg, to measure atmospheric
pressure during sampling and pump calibration.
7.4.1.8 Rotameter. 0 to 100 cc/min, to detect changes in flow rate
during sampling.
7.4.2 Sampling and Analysis. It is suggested that the tester follow
the sampling and analysis portion of the respective NIOSH method section
entitled ''Procedure.'' Calibrate the pump and limiting orifice flow
rate through adsorption tubes with the bubble tube flowmeter before
sampling. The sample system can be operated as a ''recirculating loop''
for this operation. Record the ambient temperature and barometric
pressure. Then, during sampling, use the rotameter to verify that the
pump and orifice sampling rate remains constant.
Use a sample probe, if required, to obtain the sample at the centroid
of the duct, or at a point no closer to the walls than 1 m. Minimize
the length of flexible tubing between the probe and adsorption tubes.
Several adsorption tubes can be connected in series, if the extra
adsorptive capacity is needed. Provide the gas sample to the sample
system at a pressure sufficient for the limiting orifice to function as
a sonic orifice. Record the total time and sample flow rate (or the
number of pump strokes), the barometric pressure, and ambient
temperature. Obtain a total sample volume commensurate with the
expected concentration(s) of the volatile organic(s) present, and
recommended sample loading factors (weight sample per weight adsorption
media). Laboratory tests prior to actual sampling may be necessary to
predetermine this volume. When more than one organic is present in the
emissions, then develop relative adsorptive capacity information. If
water vapor is present in the sample at concentrations above 2 to 3
percent, the adsorptive capacity may be severely reduced. Operate the
gas chromatograph according to the manufacture's instructions. After
establishing optimum conditions, verify and document these conditions
during all operations. Analyze the audit samples (see Section 7.4.4.3),
then the emission samples. Repeat the analysis of each sample until the
relative deviation of two consecutive injections does not exceed 5
percent.
7.4.3 Standards and Calibration. The standards can be prepared
according to the respective NIOSH method. Use a minimum of three
different standards; select the concentrations to bracket the expected
average sample concentration. Perform the calibration before and after
each day's sample analyses. Prepare the calibration curve by using the
least squares method.
7.4.4 Quality Assurance.
7.4.4.1 Determination of Desorption Efficiency. During the testing
program, determine the desorption efficiency in the expected sample
concentration range for each batch of adsorption media to be used. Use
an internal standard. A minimum desorption efficiency of 50 percent
shall be obtained. Repeat the desorption determination until the
relative deviation of two consecutive determinations does not exceed 5
percent. Use the average desorption efficiency of these two consecutive
determinations for the correction specified in Section 7.4.4.5. If the
desorption efficiency of the compound(s) of interest is questionable
under actual sampling conditions, use of the Method of Standard
Additions may be helpful to determine this value.
7.4.4.2 Determination of Sample Collection Efficiency. For the
source samples, analyze the primary and backup portions of the
adsorption tubes separately. If the backup portion exceeds 10 percent
of the total amount (primary and backup), repeat the sampling with a
larger sampling portion.
7.4.4.3 Analysis Audit. Immediately before the sample analyses,
analyze the two audits in accordance with Section 7.4.2. The analysis
audit shall agree with the audit concentration within 10 percent.
7.4.4.4 Pump Leak Checks and Volume Flow Rate Checks. Perform both
of these checks immediately after sampling with all sampling train
components in place. Perform all leak checks according to the
manufacturer's instructions, and record the results. Use the
bubble-tube flowmeter to measure the pump volume flow rate with the
orifice used in the test sampling, and the result. If it has changed by
more than 5 but less than 20 percent, calculate an average flow rate for
the test. If the flow rate has changed by more than 20 percent,
recalibrate the pump and repeat the sampling.
7.4.4.5 Calculations. All calculations can be performed according to
the respective NIOSH method. Correct all sample volumes to standard
conditions. If a sample dilution system has been used, multiply the
results by the appropriate dilution ratio. Correct all results by
dividing by the desorption efficiency (decimal value). Report results
as ppm by volume, dry basis.
7.5 Reporting of Results. At the completion of the field analysis
portion of the study, ensure that the data sheets shown in Figure 18-11
have been completed. Summarize this data on the data sheets shown in
Figure 18-15.
8. Bibliography
1. American Society for Testing and Materials. C1 Through C5
Hydrocarbons in the Atmosphere by Gas Chromatography. ASTM D 2820-72,
Part 23. Philadelphia, Pa. 23:950-958. 1973.
2. Corazon, V. V. Methodology for Collecting and Analyzing Organic
Air Pollutants. U.S. Environmental Protection Agency. Publication No.
EPA-600/2-79-042. February 1979.
3. Dravnieks, A., B. K. Krotoszynski, J. Whitfield, A. O'Donnell,
and T. Burgwald. Environmental Science and Technology.
5(12):1200-1222. 1971.
4. Eggertsen, F. T., and F. M. Nelsen. Gas Chromatographic Analysis
of Engine Exhaust and Atmosphere. Analytical Chemistry. 30(6):
1040-1043. 1958.
5. Feairheller, W. R., P. J. Marn, D. H. Harris, and D. L.
Harris. Technical Manual for Process Sampling Strategies for Organic
Materials. U.S. Environmental Protection Agency. Research Triangle
Park, NC. Publication No. EPA 600/2-76-122. April 1976. 172 p.
6. FR, 39 FR 9319-9323. 1974.
7. FR, 39 FR 32857-32860. 1974.
8. FR, 41 FR 23069-23072 and 23076-23090. 1976.
9. FR, 41 FR 46569-46571. 1976.
10. FR, 42 FR 41771-41776. 1977.
11. Fishbein, L. Chromatography of Environmental Hazards, Volume II.
Elsevier Scientific Publishing Company. NY, NY. 1973.
12. Hamersma, J. W., S. L. Reynolds, and R. F. Maddalone.
EPA/IERL-RTP Procedures Manual: Level 1 Environmental Assessment. U.S.
Environmental Protection Agency. Research Triangle Park, NC.
Publication No. EPA 600/276-160a. June 1976. 130 p.
13. Harris, J. C., M. J. Hayes, P. L. Levins, and D. B. Lindsay.
EPA/IERL-RTP Procedures for Level 2 Sampling and Analysis of Organic
Materials. U.S. Environmental Protection Agency. Research Triangle
Park, NC. Publication No. EPA 600/7-79-033. February 1979. 154 p.
14. Harris, W. E., H. W. Habgood. Programmed Temperature Gas
Chromatography. John Wiley & Sons, Inc. New York. 1966.
15. Intersociety Committee. Methods of Air Sampling and Analysis.
American Health Association. Washington, DC. 1972.
16. Jones, P. W., R. D. Grammar, P. E. Strup, and T. B. Stanford.
Environmental Science and Technology. 10:806-810. 1976.
17. McNair Han Bunelli, E. J. Basic Gas Chromatography.
Consolidated Printers. Berkeley. 1969.
18. Nelson, G. O. Controlled Test Atmospheres, Principles and
Techniques. Ann Arbor. Ann Arbor Science Publishers. 1971. 247 p.
19. NIOSH Manual of Analytical Methods, Volumes 1, 2, 3, 4, 5, 6, 7.
U.S. Department of Health and Human Services National Institute for
Occupational Safety and Health. Center for Disease Control. 4676
Columbia Parkway, Cincinnati, Ohio 45226. April 1977-August 1981. May
be available from the Superintendent of Documents, Government Printing
Office, Washington, DC 20402. Stock Number/Price: Volume 1 --
017-033-00267-3/$13, Volume 2 -- 017-033-00260-6/$11, Volume 3 --
017-033-00261-4/$14, Volume 4 -- 017-033-00317-3/$7.25, Volume 5 --
017-033-00349-1/$10, Volume 6 -- 017-033-00369-6/$9, and Volume 7 --
017-033-00396-5/$7. Prices subject to change. Foreign orders add 25
percent.
20. Schuetzle, D., T. J. Prater, and S. R. Ruddell. Sampling and
Analysis of Emissions from Stationary Sources; I. Odor and Total
Hydrocarbons. Journal of the Air Pollution Control Association.
25(9):925-932. 1975.
21. Snyder, A. D., F. N. Hodgson, M. A. Kemmer and J. R.
McKendree. Utility of Solid Sorbents for Sampling Organic Emissions from
Stationary Sources. U.S. Environmental Protection Agency. Research
Triangle Park, NC Publication No. EPA 600/2-76-201. July 1976. 71 p.
22. Tentative Method for Continuous Analysis of Total Hydrocarbons in
the Atmosphere. Intersociety Committee, American Public Health
Association. Washington, DC 1972. p. 184-186.
23. Zwerg, G., CRC Handbook of Chromatography, Volumes I and II.
Sherma, Joseph (ed.). CRC Press. Cleveland. 1972.
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Figure 18-14. Sampling and analysis check.
Plant --
Date --
Location --
Figure 18-14. Sampling and analysis sheet.
40 CFR 60.748 Pt. 60, App. A, Meth. 19
1.1 Applicability. This method is applicable for (a) determining
particulate matter (PM), sulfur dioxide (SO2), and nitrogen oxides (NOx)
emission rates; (b) determining sulfur removal efficiencies of fuel
pretreatment and SO2 control devices; (c) determining overall reduction
of potential SO2 emissions from steam generating units or other sources
as specified in applicable regulations; and (d) determining SO2 rates
based on fuel sampling and analysis procedures.
1.2 Principle.
1.2.1 Pollutant emission rates are determined from concentrations of
PM, SO2, or NOx, and oxygen (O2) or carbon dioxide (CO2) along with F
factors (ratios of combustion gas volumes to heat inputs).
1.2.2 An overall SO2 emission reduction efficiency is computed from
the efficiency of fuel pretreatment systems (optional) and the
efficiency of SO2 control devices.
1.2.3 The sulfur removal efficiency of a fuel pretreatment system is
determined by fuel sampling and analysis of the sulfur and heat contents
of the fuel before and after the pretreatment system.
1.2.4 The SO2 removal efficiency of a control device is determined by
measuring the SO2 rates before and after the control device.
1.2.5 The inlet rates to SO2 control systems and when SO2 control
systems are not used, SO2 emission rates to the atmosphere may be
determined by fuel sampling and analysis (optional).
Select from the following sections the applicable procedure to
compute the PM, SO2, or NOx emission rate (E) in ng/J (lb/million Btu).
The pollutant concentration must be in ng/scm (lb/scf) and the F factor
must be in scm/J (scf/million Btu). If the pollutant concentration (C)
is not in the appropriate units, use the following table to make the
proper conversion:
An F factor is the ratio of the gas volume of the products of
combustion to the heat content of the fuel. The dry F factor (Fd)
includes all components of combustion less water, the wet F factor (Fw)
includes all components of combustion, and the carbon F factor (Fc)
includes only carbon dioxide.
Note: Since Fw factors include water resulting only from the
combustion of hydrogen in the fuel, the procedures using Fw factors are
not applicable for computing E from steam generating units with wet
scrubbers or with other processes that add water (e.g., steam injection)
2.1 Oxygen-Based F Factor, Dry Basis. When measurements are on a dry
basis for both O2 (%O2d) and pollutant (Cd) concentrations, use the
following equation:
E=CdFd (20.9/(20.9^%O2d))
Eq. 19-1
2.2 Oxygen-Based F Factor, Wet Basis. When measurements are on a wet
basis for both O2 (%O2w) and pollutant (Cw) concentrations, use either
of the following:
2.2.1 If the moisture fraction of ambient air (Bwa) is measured:
E=(CwFw20.9)/(20.9(1^Bwa)^%O2w)
Eq. 19-2
Instead of actual measurement, Bwa may be estimated according to the
procedure below. (Note: The estimates are selected to ensure that
negative errors will not be larger than ^1.5 percent. However, positive
errors, or over-estimation of emissions, of as much as 5 percent may be
introduced depending upon the geographic location of the facility and
the associated range of ambient moisture):
2.2.1.1 Bwa=0.027. This value may be used at any location at all
times.
2.2.1.2 Bwa=Highest monthly average of Bwa that occurred within the
previous calendar year at the nearest Weather Service Station. This
value shall be determined annually and may be used as an estimate for
the entire current calendar year.
2.2.1.3 Bwa=Highest daily average of Bwa that occurred within a
calendar month at the nearest Weather Service Station, calculated from
the data from the past 3 years. This value shall be computed for each
month and may be used as an estimate for the current respective calendar
month.
2.2.2 If the moisture fraction (Bws) of the effluent gas is measured:
E=CwFd 20.9/(20.9(1^Bws)^%O2w)
Eq. 19-3
2.3 Oxygen-Based F Factor, Dry/Wet Basis.
2.3.1 When the pollutant concentration is measured on a wet basis
(Cw) and O2 concentration is measured on a dry basis (%O2d), use the
following equation:
E=((CwFd)/(1^Bws))/(20.9/(20.9^%O2d))
Eq. 19-4
2.3.2 When the pollutant concentration is measured on a dry basis
(Cd) and the O2 concentration is measured on a wet basis (%O2w), use the
following equation:
E=(CdFd20.9)/(20.9^O2w/(1^Bws))
Eq. 19-5
2.4 Carbon Dioxide-Based F Factor, Dry Basis. When measurements are
on a dry basis for both CO2 (%CO2d) and pollutant (Cd) concentrations,
use the following equation:
E=CdFc(100/%CO2d)
Eq. 19-6
2.5 Carbon Dioxide-Based F Factor, Wet Basis. When measurements are
on a wet basis for both CO2 (%CO2w) and pollutant (Cw) concentrations,
use the following equation:
E=CwFc (100/%CO2w)
Eq. 19-7
2.6 Carbon Dioxide-Based F Factor, Dry/Wet Basis.
2.6.1 When the pollutant concentration is measured on a wet basis
(Cw) and CO2 concentration is measured on a dry basis (%CO2d), use the
following equation:
E=(CwFc/(1^Bws)) (100/%CO2d)
Eq. 19-8
2.6.2 When the pollutant concentration is measured on a dry basis
(Cd) and CO2 concentration is measured on a wet basis (%CO2w), use the
following equation:
E=Cd(1^Bws)Fc(100/%CO2w)
Eq. 19-9
2.7 Direct-Fired Reheat Fuel Burning. The effect of direct-fired
reheat fuel burning (for the purpose of raising the temperature of the
exhaust effluent from wet scrubbers to above the moisture dew-point) on
emission rates will be less than 1.0 percent and, therefore, may be
ignored.
2.8 Combined Cycle-Gas Turbine Systems. For gas turbine-steam
generator combined cycle systems, determine the emissions from the steam
generating unit or the percent reduction in potential SO2 emissions as
follows:
2.8.1 Compute the emission rate from the steam generating unit using
the following equation:
Ebo=Eco+(Hg/Hb)(Eco^Eg)
Eq. 19-10
where:
Ebo=pollutant emission rate from the steam generating unit, ng/J
(lb/million Btu).
Eco=pollutant emission rate in combined effluent, ng/J (lb/million
Btu).
Eg=pollutant rate from gas turbine, ng/J (lb/million Btu).
Hb=heat input rate to the steam generating unit from fuels fired in
the steam generating unit, J/hr (million Btu/hr).
Hg=heat input rate to gas turbine from all fuels fired in the gas
turbine, J/hr (million Btu/hr).
2.8.1.1 Use the test methods and procedures section of Subpart GG to
obtain Eco and Eg. Do not use Fw factors for determining Eg or Eco. If
an SO2 control device is used, measure Eco after the control device.
2.8.1.2 Suitable methods shall be used to determine the heat input
rates to the steam generating units (Hb) and the gas turbine (Hg).
2.8.2 If a control device is used, compute the percent of potential
SO2 emissions (% Ps) using the following equations:
Ebi=Eci^(Hg/Hb)(Eci^Eg)
Eq. 19-11
% Ps=100 (1^Ebo/Ebi)
Eq. 19-12
where:
Ebi=pollutant rate from the steam generating unit, ng/J (lb/million
Btu)
Eci=pollutant rate in combined effluent, ng/J (lb/million Btu).
Use the test methods and procedures section of Subpart GG to obtain
Eci and Eg. Do not use Fw factors for determining Eg or Eci.
Use an average F factor according to Section 3.1 or determine an
applicable F factor according to Section 3.2. If combined fuels are
fired, prorate the applicable F factors using the procedure in Section
3.3.
3.1 Average F Factors. Average F factors (Fd, Fw, or Fc) from Table
19-1 may be used.
3.2 Determined F Factors. If the fuel burned is not listed in Table
19-1 or if the owner or operator chooses to determine an F factor rather
than use the values in Table 19-1, use the procedure below:
3.2.1 Equations. Use the equations below, as appropriate, to compute
the F factors:
Fd=K((Khd%H)+(Kc%C)+(Ks%S)+(Kn%N)^(Ko%0))/GCV
Eq. 19-13
Fw=K((Khw%H)+(Kc%C)+(Ks%S)+(Kn%N)^(Ko%0)+(Kw%H2O))/GCVw
Eq. 19-14
Fc=K(Kcc%C)/GCV
Eq. 19-15
(Note. -- Omit the %H2O term in the equations for Fw if %H and %0
include the unavailable hydrogen and oxygen in the form of H2O.)
where:
Fd,Fw,Fc=volumes of combustion components per unit of heat content,
scm/J (scf/million Btu).
%H, %C, %S, %N, %0, and %H2O=concentrations of hydrogen, carbon,
sulfur, nitrogen, oxygen, and water from an ultimate analysis of fuel,
weight percent.
GCV=gross calorific value of the fuel consistent with the ultimate
analysis, kJ/kg (Btu/lb).
K=conversion factor, 10^ /5/ (kJ/J)/(%) (10 /6/ Btu/million Btu).
Khd=22.7 (scm/kg))((3.64 (scf/lb)/(%)).
Kc=9.57 (scm/kg)((1.53 (scf/lb)/(%)).
Ks=3.54 (scm/kg) ((0.57 (scf/lb)/(%)).
Kn=0.86 (scm/kg (0.14 (scf/lb)/(%)).
Ko=2.85 (scm/kg) (0.46 (scf/lb)/(%)).
Khw=34.74 (scm/kg) ((5.57 (scf/lb)/(%)).
Kw=1.30 (scm/kg) ((0.21 (scf/lb)/(%)).
Kcc=2.0 (scm/kg) ((0.321 (scf/lb)/(%)).
3.2.2 Use applicable sampling procedures in Section 5.2.1 or 5.2.2 to
obtain samples for analyses.
3.2.3 Use ASTM D3176-74 (incorporated by reference -- see 60.17) for
ultimate analysis of the fuel.
3.2.4 Use applicable methods in Section 5.2.1 or 5.2.2 to determine
the heat content of solid or liquid fuels. For gaseous fuels, use ASTM
D1826-77 (IBR -- see 60.17) to determine the heat content.
3.3 F Factors for Combination of Fuels. If combinations of fuels are
burned, use the following equations, as applicable unless otherwise
specified in applicable subpart:
where:
Xk=fraction of total heat input from each type of fuel k.
n=number of fuels being burned in combination.
4.1 Average Pollutant Rates from Hourly Values. When hourly average
pollutant rates (Eh), inlet or outlet, are obtained (e.g., CEMS values),
compute the average pollutant rate (Ea ) for the performance test period
(e.g., 30 days) specified in the applicable regulation using the
following equation:
where:
Ea=average pollutant rate for the specified performance test period,
ng/J (lb/million Btu).
Eh=hourly average pollutant, ng/J (lb/million Btu).
H=total number of operating hours for which pollutant rates are
determined in the performance test period.
4.2 Average Pollutant Rates from Other than Hourly Averages. When
pollutant rates are determined from measured values representing longer
than 1-hour periods (e.g., daily fuel sampling and analyses or Method 6B
values), or when pollutant rates are determined from combinations of
1-hour and longer than 1-hour periods (e.g., CEMS and Method 6B values),
compute the average pollutant rate (Ea) for the performance test period
(e.g., 30 days) specified in the applicable regulation using the
following equation:
where:
Ed=average pollutant rate for each sampling period (e.g., 24-hr
Method 6B sample or 24-hr fuel sample) or for each fuel lot (e.g.,
amount of fuel bunkered), ng/J (lb/million Btu).
nd=number of operating hours of the affected facility within the
performance test period for each Ed determined.
D=number of sampling periods during the performance test period.
4.3 Daily Geometric Average Pollutant Rates from Hourly Values. The
geometric average pollutant rate (Ega) is computed using the following
equation:
where:
Ega=daily geometric average pollutant rate, ng/J (lbs/million Btu) or
ppm corrected to 7 percent O2.
Ehj=hourly arithmetic average pollutant rate for hour ''j,'' ng/J
(lb/million Btu) or ppm corrected to 7 percent O2.
n=total number of hourly averages for which pollutant rates are
available within the 24 hr midnight to midnight daily period.
ln=natural log of indicated value.
EXP=the natural logarithmic base (2.718) raised to the value enclosed
by brackets.
5.1 Overall Percent Reduction. Compute the overall percent SO2
reduction (%Ro) using the following equation:
%Ro=100 (1.0^(1.0^%Rf/100)(1.0^%Rg/100))
Eq. 19-21
where:
%Rf=SO2 removal efficiency from fuel pretreatment, percent.
%Rg=SO2 removal efficiency of the control device, percent.
5.2 Pretreatment Removal Efficiency (Optional). Compute the SO2
removal efficiency from fuel pretreatment (%Rf) for the averaging period
(e.g., 90 days) as specified in the applicable regulation using the
following equation:
40 CFR 60.748
where:
%Sp, %Sr=sulfur content of the product and raw fuel lots,
respectively, dry basis weight percent.
GCVp, GCVr=gross calorific value for the product and raw fuel lots,
respectively, dry basis, kg/kg (Btu/lb).
Lp, Lr=weight of the product and raw fuel lots, respectively, metric
ton (ton).
n=number of fuel lots during the averaging period.
Note: In calculating %Rf, include %S and GCV values for all fuel
lots that are not pretreated and are used during the averaging period.
5.2.1 Solid Fossil (Including Waste) Fuel -- Sampling and Analysis.
Note: For the purposes of this method, raw fuel (coal or oil) is the
fuel delivered to the desulfurization (pretreatment) facility. For oil,
the input oil to the oil desulfurization process (e.g., hydrotreatment)
is considered to be the raw fuel.
5.2.1.1 Sample Increment Collection. Use ASTM D2234-76 (IBR -- see
60.17), Type I, Conditions A, B, or C, and systematic spacing. As used
in this method, systematic spacing is intended to include evenly spaced
increments in time or increments based on equal weights of coal passing
the collection area.
As a minimum, determine the number and weight of increments required
per gross sample representing each coal lot according to Table 2 or
Paragraph 7.1.5.2 of ASTM D2234-76. Collect one gross sample for each
lot of raw coal and one gross sample for each lot of product coal.
5.2.1.2 ASTM Lot Size. For the purpose of Section 5.2 (fuel
pretreatment), the lot size of product coal is the weight of product
coal from one type of raw coal. The lot size of raw coal is the weight
of raw coal used to produce one lot of product coal. Typically, the lot
size is the weight of coal processed in a 1-day (24-hour) period. If
more than one type of coal is treated and produced in 1 day, then gross
samples must be collected and analyzed for each type of coal. A coal
lot size equaling the 90-day quarterly fuel quantity for a steam
generating unit may be used if representative sampling can be conducted
for each raw coal and product coal.
Note: Alternative definitions of lot sizes may be used, subject to
prior approval of the Administrator.
5.2.1.3 Gross Sample Analysis. Use ASTM D2013-72 to prepare the
sample, ASTM D3177-75 or ASTM D4239-85 to determine sulfur content (%S),
ASTM D3173-73 to determine moisture content, and ASTM D2015-77 or ASTM
D3286-85 to determine gross calorific value (GCV) (all methods cited IBR
-- see 60.17) on a dry basis for each gross sample.
5.2.2 Liquid Fossil Fuel -- Sampling and Analysis. See Note under
Section 5.2.1.
5.2.2.1 Sample Collection. Follow the procedures for continuous
sampling in ASTM D270-65 (Reapproved 1975) (IBR -- see 60.17) for each
gross sample from each fuel lot.
5.2.2.2 Lot Size. For the purpose of Section 5.2 (fuel
pretreatment), the lot size of a product oil is the weight of product
oil from one pretreatment facility and intended as one shipment (ship
load, barge load, etc.). The lot size of raw oil is the weight of each
crude liquid fuel type used to produce a lot of product oil.
Note: Alternative definitions of lot sizes may be used, subject to
prior approval of the Administrator.
5.2.2.3 Sample Analysis. Use ASTM D129-64 (Reapproved 1978), ASTM
D1552-83, or ASTM D4057-81 to determine the sulfur content (%S) and ASTM
D240-76 (all methods cited IBR -- see 60.17) to determine the GCV of
each gross sample. These values may be assumed to be on a dry basis.
The owner or operator of an affected facility may elect to determine the
GCV by sampling the oil combusted on the first steam generating unit
operating day of each calendar month and then using the lowest GCV value
of the three GCV values per quarter for the GCV of all oil combusted in
that calendar quarter.
5.2.3 Use appropriate procedures, subject to the approval of the
Administrator, to determine the fraction of total mass input derived
from each type of fuel.
5.3 Control Device Removal Efficiency. Compute the percent removal
efficiency (%Rg of the control device using the following equation:
%Rg=100(1.0^Eao/Eai)
Eq. 19-23
where:
Eao, Eai=average pollutant rate of the control device, outlet and
inlet, respectively, for the performance test period, ng/J (lb/million
Btu).
5.3.1 Use continuous emission monitoring systems or test methods, as
appropriate, to determine the outlet SO2 rates and, if appropriate, the
inlet SO2 rates. The rates may be determined as hourly (Eh) or other
sampling period averages (Ed). Then, compute the average pollutant
rates for the performance test period (Eao and Eai) using the procedures
in Section 4.
5.3.2 As an alternative, as-fired fuel sampling and analysis may be
used to determine inlet SO2 rates as follows:
5.3.2.1 Compute the average inlet SO2 rate (Edi) for each sampling
period using the following equation:
Edi=K (%S/GCV)
Eq. 19-24
where:
Edi=average inlet SO2 rate for each sampling period d, ng/J
(lb/million Btu)
% S=sulfur content of as-fired fuel lot, dry basis, weight percent.
GCV=gross calorific value of the fuel lot consistent with the sulfur
analysis, kJ/kg (Btu/lb).
K=2 10 /7/ ((kg)(ng)/(%)(J)) 2 10 /4/ (lb)(Btu/(%))(million Btu)
After calculating Edi use the procedures in Section 4.2 to determine
the average inlet SO2 rate for the performance test period (Eai).
5.3.2.2 Collect the fuel samples from a location in the fuel handling
system that provides a sample representative of the fuel bunkered or
consumed during a steam generating unit operating day.
For the purpose of as-fired fuel sampling under Section 5.3.2 or
Section 6, the lot size for coal is the weight of coal bunkered or
consumed during each steam generating unit operating day. The lot size
for oil is the weight of oil supplied to the ''day'' tank or consumed
during each steam generating unit operating day.
For reporting and calculation purposes, the gross sample shall be
identified with the calendar day on which sampling began. For steam
generating unit operating days when a coal-fired steam generating unit
is operated without coal being added to the bunkers, the coal analysis
from the previous ''as bunkered'' coal sample shall be used until coal
is bunkered again. For steam generating unit operating days when an
oil-fired steam generating unit is operated without oil being added to
the oil ''day'' tank, the oil analysis from the previous day shall be
used until the ''day'' tank is filled again.
Alternative definitions of fuel lot size may be used, subject to
prior approval of the Administrator.
5.3.2.3 Use ASTM procedures specified in Section 5.2.1 or 5.2.2 to
determine the sulfur contents (%S) and gross calorific values (GCV).
5.4 Daily Geometric Average Percent Reduction from Hourly Values.
The geometric average percent reduction (%Rga) is computed using the
following equation:
where:
%Rga=daily geometric average percent reduction.
Ejo, Eji=matched pair hourly arithmetic average pollutant rate,
outlet and inlet, respectively, ng/J (lb/million Btu) or ppm corrected
to 7 percent O2.
n=total number of hourly averages for which paired inlet and outlet
pollutant rates are available within the 24-hr midnight to midnight
daily period.
ln=natural log of indicated value.
EXP=the natural logarithmic base (2.718) raised to the value enclosed
by brackets.
Note: The calculation includes only paired data sets (hourly
average) for the inlet and outlet pollutant measurements.
If fuel sampling and analysis procedures in Section 5.2.1 are being
used to determine average SO2 emission rates (Eas) to the atmosphere
from a coal-fired steam generating unit when there is no SO2 control
device, the following equation may be used to adjust the emission rate
for sulfur retention credits (no credits are allowed for oil-fired
systems) (Edi) for each sampling period using the following equation:
Edi=0.97 K (%S/GCV)
Eq. 19-25
where:
Edi=average inlet SO2 rate for each sampling period d, ng/J
(lb/million Btu)
%S=sulfur content of as-fired fuel lot, dry basis, weight percent.
GCV=gross calorific value of the fuel lot consistent with the sulfur
analysis, kJ/kg (Btu/lb).
K=2 10 /7/ ((kg)(ng)/(%)(J)) 2 10 /4/ (lb)(Btu/(%))(million Btu)
After calculating Edi use the procedures in Section 4-2 to determine
the average SO2 emission rate to the atmosphere for the performance test
period (Eao).
7.1 Adjusted Emission Rates and Control Device Removal Efficiency.
When the minimum data requirement is not met, the Administrator may use
the following adjusted emission rates or control device removal
efficiencies to determine compliance with the applicable standards.
7.1.1 Emission Rate. Compliance with the emission rate standard may
be determined by using the lower confidence limit of the emission rate
(Eao*) as follows:
Eao*=Eao^t0.95 So
Eq. 19-26
where:
So=standard deviation of the hourly average emission rates for each
performance test period, ng/J (lb/million Btu).
t0.95=values shown in Table 19-2 for the indicated number of data
points n.
7.1.2 Control Device Removal Efficiency. Compliance with the overall
emission reduction (%Ro) may be determined by using the lower confidence
limit of the emission rate (Eao*) and the upper confidence limit of the
inlet pollutant rate (Eai*) in calculating the control device removal
efficiency (%Rg) as follows:
%Rg=100 (1.0^Eao*/Eai*)
Eq. 19-27
Eai*=Eai+t0.95 Si
Eq. 19-28
where:
Si=standard deviation of the hourly average inlet pollutant rates for
each performance test period, ng/J (lb/million Btu).
7.2 Standard Deviation of Hourly Average Pollutant Rates. Compute
the standard deviation (Se) of the hourly average pollutant rates using
the following equation:
40 CFR 60.748
where:
S=standard deviation of the hourly average pollutant rates for each
performance test period, ng/J (lb/million Btu).
Hr=total numbers of hours in the performance test period (e.g., 720
hours for 30-day performance test period).
Equation 19-29 may be used to compute the standard deviation for both
the outlet (So) and, if applicable, inlet (Si) pollutant rates.
40 CFR 60.748 Pt. 60, App. A, Meth. 20
1. Principle and Applicability
1.1 Applicability. This method is applicable for the determination of
nitrogen oxides (NOx), sulfur dioxide (SO2), and a diluent gas, either
oxygen (O2) or carbon dioxide (CO2), emissions from stationary gas
turbines. For the NOx and diluent concentration determinations, this
method includes: (1) Measurement system design criteria; (2) Analyzer
performance specifications and performance test procedures; and (3)
Procedures for emission testing.
1.2 Principle. A gas sample is continuously extracted from the
exhaust stream of a stationary gas turbine; a portion of the sample
stream is conveyed to instrumental analyzers for determination of NOx
and diluent content. During each NOx and diluent determination, a
separate measurement of SO2 emissions is made, using Method 6, or its
equivalent. The diluent determination is used to adjust the NOx and SO2
concentrations to a reference condition.
2. Definitions
2.1 Measurement System. The total equipment required for the
determination of a gas concentration or a gas emission rate. The system
consists of the following major subsystems:
2.1.1 Sample Interface. That portion of a system that is used for
one or more of the following: sample acquisition, sample
transportation, sample conditioning, or protection of the analyzers from
the effects of the stack effluent.
2.1.2 NOx Analyzer. That portion of the system that senses NOx and
generates an output proportional to the gas concentration.
2.1.3 O2 Analyzer. That portion of the system that senses O2 and
generates an output proportional to the gas concentration.
2.1.4 CO2 Analyzer. That portion of the system that senses CO2 and
generates an output proportional to the gas concentration.
2.1.5 Data Recorder. That portion of the measurement system that
provides a permanent record of the analyzer(s) output. The data
recorder may include automatic data reduction capabilities.
2.2 Span Value. The upper limit of a gas concentration measurement
range that is specified for affected source categories in the applicable
part of the regulations.
2.3 Calibration Gas. A known concentration of a gas in an
appropriate diluent gas.
2.4 Calibration Error. The difference between the gas concentration
indicated by the measurement system and the known concentration of the
calibration gas.
2.5 Zero Drift. The difference in the measurement system output
readings from zero after a stated period of operation during which no
unscheduled maintenance, repair, or adjustment took place and the input
concentration at the time of the measurements was zero.
2.6 Calibration Drift. The difference in the measurement system
output readings from the known concentration of the calibration gas
after a stated period of operation during which no unscheduled
maintenance, repair, or adjustment took place and the input at the time
of the measurements was a high-level value.
2.7 Response Time. The amount of time required for the measurement
system to display on the data output 95 percent of a step change in
pollutant concentration.
2.8 Interference Response. The output response of the measurement
system to a component in the sample gas, other than the gas component
being measured.
3. Measurement System Performance Specifications
3.1 NO2 to NO Converter. Greater than 90 percent conversion
efficiency of NO2 to NO.
3.2 Interference Response. Less than 2 percent of the span value.
3.3 Response Time. No greater than 30 seconds.
3.4 Zero Drift. Less than 2 percent of the span value over the
period of each test run.
3.5 Calibration Drift. Less than 2 percent of the span value over
the period of each test run.
4. Apparatus and Reagents
4.1 Measurement System. Use any measurement system for NOx and
diluent that is expected to meet the specifications in this method. A
schematic of an acceptable measurement system is shown in Figure 20-1.
The essential components of the measurement system are described below:
insert illus. 0256A
4.1.1 Sample Probe. Heated stainless steel, or equivalent,
open-ended, straight tube of sufficient length to traverse the sample
points.
4.1.2 Sample Line. Heated ( 95 C) stainless steel or Teflon tubing
to transport the sample gas to the sample conditioners and analyzers.
4.1.3 Calibration Valve Assembly. A three-way valve assembly to
direct the zero and calibration gases to the sample conditioners and to
the analyzers. The calibration valve assembly shall be capable of
blocking the sample gas flow and of introducing calibration gases to the
measurement system when in the calibration mode.
4.1.4 NO2 to NO Converter. That portion of the system that converts
the nitrogen dioxide (NO2) in the sample gas to nitrogen oxide (NO).
Some analyzers are designed to measure NOx as NO2 on a wet basis and can
be used without an NO2 to NO converter or a moisture removal trap
provided the sample line to the analyzer is heated ( 95 C) to the inlet
of the analyzer. In addition, an NO2 to NO converter is not necessary
if the NO2 portion of the exhaust gas is less than 5 percent of the
total NOx concentration. As a guideline, an NO2 to NO converter is not
necessary if the gas turbine is operated at 90 percent or more of peak
load capacity. A converter is necessary under lower load conditions.
4.1.5 Moisture Removal Trap. A refrigerator-type condenser or other
type device designed to continuously remove condensate from the sample
gas while maintaining minimal contact between any condensate and the
sample gas. The moisture removal trap is not necessary for analyzers
that can measure NOx concentrations on a wet basis; for these
analyzers, (a) heat the sample line up to the inlet of the analyzers,
(b) determine the moisture content using methods subject to the approval
of the Administrator, and (c) correct the NOx and diluent concentrations
to a dry basis.
4.1.6 Particulate Filter. An in-stack or an out-of-stack glass fiber
filter, of the type specified in EPA Method 5; however, an out-of-stack
filter is recommended when the stack gas temperature exceeds 250 to 300
C.
4.1.7 Sample Pump. A nonreactive leak-free sample pump to pull the
sample gas through the system at a flow rate sufficient to minimize
transport delay. The pump shall be made from stainless steel or coated
with Teflon or equivalent.
4.1.8 Sample Gas Manifold. A sample gas manifold to divert portions
of the sample gas stream to the analyzers. The manifold may be
constructed of glass, Teflon, stainless steel, or equivalent.
4.1.9 Diluent Gas Analyzer. An analyzer to determine the percent O2
or CO2 concentration of the sample gas.
4.1.10 Nitrogen Oxides Analyzer. An analyzer to determine the ppm
NOx concentration in the sample gas stream.
4.1.11 Data Recorder. A strip-chart recorder, analog computer, or
digital recorder for recording measurement data.
4.2 Sulfur Dioxide Analysis. EPA Method 6 apparatus and reagents.
4.3 NOx Calibration Gases. The calibration gases for the NOx
analyzer shall be NO in N2. Use four calibration gas mixtures as
specified below:
4.3.1 High-level Gas. A gas concentration that is equivalent to 80
to 90 percent of the span value.
4.3.2 Mid-level Gas. A gas concentration that is equivalent to 45 to
55 percent of the span value.
4.3.3 Low-level Gas. A gas concentration that is equivalent to 20 to
30 percent of the span value.
4.3.4 Zero Gas. A gas concentration of less than 0.25 percent of the
span value. Ambient air may be used for the NOx zero gas.
4.4 Diluent Calibration Gases.
4.4.1 For O2 calibration gases, use purified air at 20.9 percent O2
as the high-level O2 gas. Use a gas concentration between 11 and 15
percent O2 in nitrogen for the mid-level gas, and use purified nitrogen
for the zero gas.
4.4.2 For CO2 calibration gases, use a gas concentration between 8
and 12 percent CO2 in air for the high-level calibration gas. Use a gas
concentration between 2 and 5 percent CO2 in air for the mid-level
calibration gas, and use purified air (<100 ppm CO2) as the zero level
calibration gas.
5. Measurement System Performance Test Procedures
Perform the following procedures prior to measurement of emissions
(Section 6) and only once for each test program, i.e., the series of all
test runs for a given gas turbine engine.
5.1 Calibration Gas Checks. There are two alternatives for checking
the concentrations of the calibration gases. (a) The first is to use
calibration gases that are documented traceable to National Bureau of
Standards Reference Materials. Use Traceability Protocol for
Establishing True Concentrations of Gases Used for Calibrations and
Audits of Continuous Source Emission Monitors (Protocol Number 1) that
is available from the Environmental Monitoring Systems Laboratory,
Quality Assurance Branch, Mail Drop 77, Environmental Protection Agency,
Research Triangle Park, NC 27711. Obtain a certification from the gas
manufacturer that the protocol was followed. These calibration gases
are not to be analyzed with the Reference Methods. (b) The second
alternative is to use calibration gases not prepared according to the
protocol. If this alternative is chosen, within 1 month prior to the
emission test, analyze each of the calibration gas mixtures in
triplicate using Method 7 or the procedure outlined in Citation 1 for
NOx and use Method 3 for O2 or CO2. Record the results on a data sheet
(example is shown in Figure 20-2). For the low-level, mid-level, or
high-level gas mixtures, each of the individual NOx analytical results
must be within 10 percent (or 10 ppm, whichever is greater) of the
triplicate set average (O2 or CO2 test results must be within 0.5
percent O2 or CO2); otherwise, discard the entire set and repeat the
triplicate analyses. If the average of the triplicate reference method
test results is within 5 percent for NOx gas or 0.5 percent O2 or CO2
for the O2 or CO2 gas of the calibration gas manufacturer's tag value,
use the tag value; otherwise, conduct at least three additional
reference method test analyses until the results of six individual NOx
runs (the three original plus three additional) agree within 10 percent
(or 10 ppm, whichever is greater) of the average (O2 or CO2 test results
must be within 0.5 percent O2 or CO2). Then use this average for the
cylinder value.
5.2 Measurement System Preparation. Prior to the emission test,
assemble the measurement system following the manufacturer's written
instructions in preparing and operating the NO2 to NO converter, the NOx
analyzer, the diluent analyzer, and other components.
Date ---------- (Must be within 1 month prior to the test period)
Reference method used
5.3 Calibration Check. Conduct the calibration checks for both the
NOx and the diluent analyzers as follows:
5.3.1 After the measurement system has been prepared for use (Section
5.2), introduce zero gases and the mid-level calibration gases; set the
analyzer output responses to the appropriate levels. Then introduce
each of the remainder of the calibration gases described in Sections 4.3
or 4.4, one at a time, to the measurement system. Record the responses
on a form similar to Figure 20-3.
5.3.2 If the linear curve determined from the zero and mid-level
calibration gas responses does not predict the actual response of the
low-level (not applicable for the diluent analyzer) and high-level gases
within 2 percent of the span value, the calibration shall be considered
invalid. Take corrective measures on the measurement system before
proceeding with the test.
5.4 Interference Response. Introduce the gaseous components listed
in Table 20-1 into the measurement system separately, or as gas
mixtures. Determine the total interference output response of the
system to these components in concentration units; record the values on
a form similar to Figure 20-4. If the sum of the interference responses
of the test gases for either the NOx or diluent analyzers is greater
than 2 percent of the applicable span value, take corrective measure on
the measurement system.
Date of test ----------
Analyzer type
Serial No.
Conduct an interference response test of each analyzer prior to its
initial use in the field. Thereafter, recheck the measurement system if
changes are made in the instrumentation that could alter the
interference response, e.g., changes in the type of gas detector.
In lieu of conducting the interference response test, instrument
vendor data, which demonstrate that for the test gases of Table 20-1 the
interference performance specification is not exceeded, are acceptable.
5.5 Response Time. To determine response time, first introduce zero
gas into the system at the calibration valve until all readings are
stable; then, switch to monitor the stack effluent until a stable
reading can be obtained. Record the upscale response time. Next,
introduce high-level calibration gas into the system. Once the system
has stabilized at the high-level concentration, switch to monitor the
stack effluent and wait until a stable value is reached. Record the
downscale response time. Repeat the procedure three times. A stable
value is equivalent to a change of less than 1 percent of span value for
30 seconds or less than 5 percent of the measured average concentration
for 2 minutes. Record the response time data on a form similar to
Figure 20-5, the readings of the upscale or downscale reponse time, and
report the greater time as the ''response time'' for the analyzer.
Conduct a response time test prior to the initial field use of the
measurement system, and repeat if changes are made in the measurement
system.
Date of test ----------
Analyzer type
S/N
Span gas concentration: -------- ppm.
Analyzer span setting: -------- ppm.
Upscale:
1 -------- seconds.
2 -------- seconds.
3 -------- seconds.
Average upscale response ---- seconds.
Downscale:
1 -------- seconds.
2 -------- seconds.
3 -------- seconds.
Average downscale response ---- seconds.
System response time=
slower average time=
-------- seconds.
5.6 NO2 to NO Conversion Efficiency.
5.6.1 Add gas from the mid-level NO in N2 calibration gas cylinder to
a clean, evacuated, leak-tight Tedlar bag. Dilute this gas
approximately 1:1 with 20.9 percent O2, purified air. Immediately
attach the bag outlet to the calibration valve assembly and begin
operation of the sampling system. Operate the sampling system,
recording the NOx response, for at least 30 minutes. If the NO2 to NO
conversion is 100 percent, the instrument response will be stable at the
highest peak value observed. If the response at the end of 30 minutes
decreases more than 2.0 percent of the highest peak value, the system is
not acceptable and corrections must be made before repeating the check.
5.6.2 Alternatively, the NO2 to NO converter check described in Title
40, Part 86: Certification and Test Procedures for Heavy-duty Engines
for 1979 and Later Model Years may be used. Other alternative
procedures may be used with approval of the Administrator.
6. Emission Measurement Test Procedure
6.1 Preliminaries.
6.1.1 Selection of a Sampling Site. Select a sampling site as close
as practical to the exhaust of the turbine. Turbine geometry, stack
configuration, internal baffling, and point of introduction of dilution
air will vary for different turbine designs. Thus, each of these
factors must be given special consideration in order to obtain a
representative sample. Whenever possible, the sampling site shall be
located upstream of the point of introduction of dilution air into the
duct. Sample ports may be located before or after the upturn elbow, in
order to accommodate the configuration of the turning vanes and baffles
and to permit a complete, unobstructed traverse of the stack. The
sample ports shall not be located within 5 feet or 2 diameters
(whichever is less) of the gas discharge to atmosphere. For
supplementary-fired, combined-cycle plants, the sampling site shall be
located between the gas turbine and the boiler. The diameter of the
sample ports shall be sufficient to allow entry of the sample probe.
6.1.2 A preliminary O2 or CO2 traverse is made for the purpose of
selecting sampling points of low O2 or high CO2 concentrations, as
appropriate for the measurement system. Conduct this test at the
turbine operating condition that is the lowest percentage of peak load
operation included in the test program. Follow the procedure below, or
use an alternative procedure subject to the approval of the
Administrator.
6.1.2.1 Minimum Number of Points. Select a minimum number of points
as follows: (1) Eight, for stacks having cross-sectional areas less
than 1.5 m2 (16.1 ft2); (2) eight plus one additional sample point for
each 0.2 m2 (2.2 ft2 of areas, for stacks of 1.5 m2 to 10.0 m2
(16.1-107.6 ft2) in cross-sectional area; and (3) 49 sample points (48
for circular stacks) for stacks greater than 10.0 m2 (107.6 ft2) in
cross-sectional area. Note that for circular ducts, the number of sample
points must be a multiple of 4, and for rectangular ducts, the number of
points must be one of those listed in Table 20-2; therefore, round off
the number of points (upward), when appropriate.
6.1.2.2 Cross-sectional Layout and Location of Traverse Points.
After the number of traverse points for the preliminary diluent sampling
has been determined, use Method 1 to located the traverse points.
6.1.2.3 Preliminary Diluent Measurement. While the gas turbine is
operating at the lowest percent of peak load, conduct a preliminary
diluent measurement as follows: Position the probe at the first
traverse point and begin sampling. The minimum sampling time at each
point shall be 1 minute plus the average system response time.
Determine the average steady-state concentration of diluent at each
point and record the data on Figure 20-6.
6.1.2.4 Selection of Emission Test Sampling Points. Select the eight
sampling points at which the lowest O2 concentrations or highest CO2
concentrations were obtained. Sample at each of these selected points
during each run at the different turbine load conditions. More than
eight points may be used, if desired, providing that the points selected
as described above are included.
Date ----------
Location:
Plant
City, State
Turbine identification:
Manufacturer
Model, serial number
6.2 NOx and Diluent Measurement. This test is to be conducted at
each of the specified load conditions. Three test runs at each load
condition constitute a complete test.
6.2.1 At the beginning of each NOx test run and, as applicable,
during the run, record turbine data as indicated in Figure 20-7. Also,
record the location and number of the traverse points on a diagram.
6.2.2 Position the probe at the first point determined in the
preceding section and begin sampling. The minimum sampling time at each
point shall be at least 1 minute plus the average system response time.
Determine the average steady-state concentration of diluent and NOx at
each point and record the data on Figure 20-8.
Test operator -------------------- Date
Turbine identification:
Type
Serial No.
Location:
Plant
City
Ambient temperature
Ambient humidity
Test time start
Test time finish
Fuel flow ratea
Water or steam flow ratea
Ambient pressure
Ultimate fuel analysis:
C
H
O
N
S
Ash
H20
Trace metals:
Na
Va
K
etcb
Operating load
aDescribe measurement method, i.e., continuous flow meter, start
finish volumes, etc.
bi.e., additional elements added for smoke suppression.
Turbine identification:
Manufacturer
Model, serial No.
Location:
Plant
City, State
Ambient temperature
Ambient pressure
Date ----------
Test time: start
Test time: finish
Test operator name
Diluent instrument type
Serial No
NOx instrument type
Serial No.
6.2.3 After sampling the last point, conclude the test run by
recording the final turbine operating parameters and by determining the
zero and calibration drift, as follows:
Immediately following the test run at each load condition, or if
adjustments are necessary for the measurement system during the tests,
reintroduce the zero and mid-level calibration gases as described in
Sections 4.3, and 4.4, one at a time, to the measurement system at the
calibration valve assembly. (Make no adjustments to the measurement
system until after the drift checks are made). Record the analyzers'
responses on a form similar to Figure 20-3. If the drift values exceed
the specified limits, the test run preceding the check is considered
invalid and will be repeated following corrections to the measurement
system. Alternatively, recalibrate the measurement system and
recalculate the measurement data. Report the test results based on both
the initial calibration and the recalibration data.
6.3 SO2 Measurement. This test is conducted only at the 100 percent
peak load condition. Determine SO2 using Method 6, or equivalent,
during the test. Select a minimum of six total points from those
required for the NOx measurements; use two points for each sample run.
The sample time at each point shall be at least 10 minutes. Average the
diluent readings taken during the NOx test runs at sample points
corresponding to the SO2 traverse points (see Section 6.2.2) and use
this average diluent concentration to correct the integrated SO2
concentration obtained by Method 6 to 15 percent diluent (see Equation
20-1).
If the applicable regulation allows fuel sampling and analysis for
fuel sulfur content to demonstrate compliance with sulfur emission unit,
emission sampling with Method 6 is not required, provided the fuel
sulfur content meets the limits of the regulation.
7. Emission Calculations
7.1 Moisture Correction. Measurement data used in most of these
calculations must be on a dry basis. If measurements must be corrected
to dry conditions, use the following equation:
Eq. 20-1
where:
Cd=Pollutant or diluent concentration adjusted to dry conditions, ppm
or percent.
Cw=Pollutant or diluent concentration measured under moist sample
conditions, ppm or percent.
Bws=Moisture content of sample gas as measured with Method 4,
reference method, or other approved method, percent/100.
7.2 CO2 Correction Factor. If pollutant concentrations are to be
corrected to 15 percent O2 and CO2 concentration is measured in lieu of
O2 concentration measurement, a CO2 correction factor is needed.
Calculate the CO2 correction factor as follows:
7.2.1 Calculate the fuel-specific F0 value for the fuel burned during
the test using values obtained from Method 19, Section 5.2, and the
following equation.
where:
FO=Fuel factor based on the ratio of oxygen volume to the ultimate
CO2 volume produced by the fuel at zero percent excess air,
dimensionless.
0.209=Fraction of air that is oxygen, percent/100.
Fd=Ratio of the volume of dry effluent gas to the gross calorific
value of the fuel from Method 19, dsm /3/ /J (dscf/10 /6/ Btu).
Fc=Ratio of the volume of carbon dioxide produced to the gross
calorific value of the fuel from Method 19, dsm /3/ /J (dscf /6/ Btu).
7.2.2. Calculate the CO2 correction factor for correcting measurement
data to 15 percent oxygen, as follows:
where:
XCO2=CO2 Correction factor, percent.
5.9=20.9 percent O2^15 percent O2, the defined O2 correction value,
percent.
7.3 Correction of Pollutant Concentrations to 15 percent O2.
Calculate the NOx and SO2 gas concentrations adjusted to 15 percent O2
using Equation 20-4 or 20-5, as appropriate. The correction to 15
percent O2 is very sensitive to the accuracy of the O2 or CO2
concentration measurement. At the level of the analyzer drift specified
in Section 3, the O2 or CO2 correction can exceed 5 percent at the
concentration levels expected in gas turbine exhaust gases. Therefore,
O2 or CO2 analyzer stability and careful calibration are necessary.
7.3.1 Correction of Pollutant Concentration Using O2 Concentration.
Calculate the O2 corrected pollutant concentration, as follows:
where:
Cadj=Pollutant concentration corrected to 15 percent O2 ppm.
Cd=Pollutant concentration measured, dry basis, ppm.
%O2=Measured O2 concentration dry basis, percent.
7.3.2 Correction of Pollutant Concentration Using CO2 Concentration.
Calculate the CO2 corrected pollutant concentration, as follows:
where:
%CO2=Measured CO2 concentration measured, dry basis, percent.
7.4 Average Adjusted NOx Concentration. Calculate the average
adjusted NOx concentration by summing the adjusted values for each
sample point and dividing by the number of points for each run.
7.5 NOx and SO2 Emission Rate Calculations. The emission rates for
NOx and SO2 in units of pollutant mass per quantity of heat input can be
calculated using the pollutant and diluent concentrations and
fuel-specific F-factors based on the fuel combustion characteristics.
The measured concentrations of pollutant in units of parts per million
by volume (ppm) must be converted to mass per unit volume concentration
units for these calculations. Use the following table for such
conversions:
7.5.1 Calculation of Emission Rate Using Oxygen Correction. Both the
O2 concentration and the pollutant concentration must be on a dry basis.
Calculate the pollutant emission rate, as follows:
where:
E=Mass emission rate of pollutant, ng/J (lb/10 /6/ Btu).
7.5.2 Calculation of Emission Rate Using Carbon Dioxide Correction.
The CO2 concentration and the pollutant concentration may be on either a
dry basis or a wet basis, but both concentrations must be on the same
basis for the calculations. Calculate the pollutant emission rate using
Equation 20-7 or 20-8:
where:
Cw=Pollutant concentration measured on a moist sample basis, ng/sm
/3/ (lb/scf).
%CO2w=Measured CO2 concentration measured on a moist sample basis,
percent.
8. Bibliography
1. Curtis, F. A Method for Analyzing NOx Cylinder Gases-Specific Ion
Electrode Procedure, Monograph available from Emission Measurement
Laboratory, ESED, Research Triangle Park, NC 27711, October 1978.
2. Sigsby, John E., F. M. Black, T. A. Bellar, and D. L Klosterman.
Chemiluminescent Method for Analysis of Nitrogen Compounds in Mobile
Source Emissions (NO, NO2, and NH3). ''Environmental Science and
Technology,'' 7:51-54. January 1973.
3. Shigehara, R.T., R.M. Neulicht, and W.S. Smith. Validating Orsat
Analysis Data from Fossil Fuel-Fired Units. Emission Measurement
Branch, Emission Standards and Engineering Division, Office of Air
Quality Planning and Standards, U.S. Environmental Protection Agency,
Research Triangle Park, NC 27711. June 1975.
40 CFR 60.748 Pt. 60, App. A, Meth. 21
1. Applicability and Principle
1.1 Applicability. This method applies to the determination of
volatile organic compound (VOC) leaks from process equipment. These
sources include, but are not limited to, valves, flanges and other
connections, pumps and compressors, pressure relief devices, process
drains, open-ended valves, pump and compressor seal system degassing
vents, accumulator vessel vents, agitator seals, and access door seals.
1.2 Principle. A portable instrument is used to detect VOC leaks from
individual sources. The instrument detector type is not specified, but
it must meet the specifications and performance criteria contained in
Section 3. A leak definition concentration based on a reference
compound is specified in each applicable regulation. This procedure is
intended to locate and classify leaks only, and is not to be used as a
direct measure of mass emission rates from individual sources.
2. Definitions
2.1 Leak Definition Concentration. The local VOC concentration at
the surface of a leak source that indicates that a VOC emission (leak)
is present. The leak definition is an instrument meter reading based on
a reference compound.
2.2 Reference Compound. The VOC species selected as an instrument
calibration basis for specification of the leak definition
concentration. (For example: If a leak definition concentration is
10,000 ppmv as methane, then any source emission that results in a local
concentration that yields a meter reading of 10,000 on an instrument
calibrated with methane would be classified as a leak. In this example,
the leak definition is 10,000 ppmv, and the reference compound is
methane.)
2.3 Calibration Gas. The VOC compound used to adjust the instrument
meter reading to a known value. The calibration gas is usually the
reference compound at a concentration approximately equal to the leak
definition concentration.
2.4 No Detectable Emission. Any VOC concentration at a potential
leak source (adjusted for local VOC ambient concentration) that is less
than a value corresponding to the instrument readability specification
of section 3.1.1(c) indicates that a leak is not present.
2.5 Response Factor. The ratio of the known concentration of a VOC
compound to the observed meter reading when measured using an instrument
calibrated with the reference compound specified in the application
regulation.
2.6 Calibration Precision. The degree of agreement between
measurements of the same known value, expressed as the relative
percentage of the average difference between the meter readings and the
known concentration to the known concentration.
2.7 Response Time. The time interval from a step change in VOC
concentration at the input of the sampling system to the time at which
90 percent of the corresponding final value is reached as displayed on
the instrument readout meter.
3. Apparatus
3.1 Monitoring Instrument.
3.1.1 Specifications.
a. The VOC instrument detector shall respond to the compounds being
processed. Detector types which may meet this requirement include, but
are not limited to, catalytic oxidation, flame ionization, infrared
absorption, and photoionization.
b. Both the linear response range and the measurable range of the
instrument for each of the VOC to be measured, and for the VOC
calibration gas that is used for calibration, shall encompass the leak
definition concentration specified in the regulation. A dilution probe
assembly may be used to bring the VOC concentration within both ranges;
however, the specifications for instrument response time and sample
probe diameter shall still be met.
c. The scale of the instrument meter shall be readable to 2.5
percent of the specified leak definition concentration when performing a
no detectable emission survey.
d. The instrument shall be equipped with an electrically driven pump
to insure that a sample is provided to the detector at a constant flow
rate. The nominal sample flow rate, as measured at the sample probe
tip, shall be 0.10 to 3.0 liters per minute when the probe is fitted
with a glass wool plug or filter that may be used to prevent plugging of
the instrument.
e. The instrument shall be intrinsically safe as defined by the
applicable U.S.A. standards (e.g., National Electric Code by the
National Fire Prevention Association) for operation in any explosive
atmospheres that may be encountered in its use. The instrument shall,
at a minimum, be intrinsically safe for Class 1, Division 1 conditions,
and Class 2, Division 1 conditions, as defined by the example Code. The
instrument shall not be operated with any safety device, such as an
exhaust flame arrestor, removed.
f. The instrument shall be equipped with a probe or probe extension
for sampling not to exceed 1/4 in. in outside diameter, with a single
end opening for admission of sample.
3.1.2 Performance Criteria.
(a) The instrument response factors for each of the VOC to be
measured shall be less than 10. When no instrument is available that
meets this specification when calibrated with the reference VOC
specified in the applicable regulation, the available instrument may be
calibrated with one of the VOC to be measured, or any other VOC, so long
as the instrument then has a response factor of less than 10 for each of
the VOC to be measured.
(b) The instrument response time shall be equal to or less than 30
seconds. The instrument pump, dilution probe (if any), sample probe,
and probe filter, that will be used during testing, shall all be in
place during the response time determination.
c. The calibration precision must be equal to or less than 10 percent
of the calibration gas value.
d. The evaluation procedure for each parameter is given in Section
4.4.
3.1.3 Performance Evaluation Requirements.
a. A response factor must be determined for each compound that is to
be measured, either by testing or from reference sources. The response
factor tests are required before placing the analyzer into service, but
do not have to be repeated at subsequent intervals.
b. The calibration precision test must be completed prior to placing
the analyzer into service, and at subsequent 3-month intervals or at the
next use whichever is later.
c. The response time test is required prior to placing the instrument
into service. If a modification to the sample pumping system or flow
configuration is made that would change the response time, a new test is
required prior to further use.
3.2 Calibration Gases. The monitoring instrument is calibrated in
terms of parts per million by volume (ppmv) of the reference compound
specified in the applicable regulation. The calibration gases required
for monitoring and instrument performance evaluation are a zero gas
(air, less than 10 ppmv VOC) and a calibration gas in air mixture
approximately equal to the leak definition specified in the regulation.
If cylinder calibration gas mixtures are used, they must be analyzed and
certified by the manufacturer to be within 2 percent accuracy, and a
shelf life must be specified. Cylinder standards must be either
reanalyzed or replaced at the end of the specified shelf life.
Alternately, calibration gases may be prepared by the user according to
any accepted gaseous standards preparation procedure that will yield a
mixture accurate to within 2 percent. Prepared standards must be
replaced each day of use unless it can be demonstrated that degradation
does not occur during storage.
Calibrations may be performed using a compound other than the
reference compound if a conversion factor is determined for that
alternative compound so that the resulting meter readings during source
surveys can be converted to reference compound results.
4. Procedures
4.1 Pretest Preparations. Perform the instrument evaluation
procedures given in Section 4.4 if the evaluation requirements of
Section 3.1.3 have not been met.
4.2 Calibration Procedures. Assemble and start up the VOC analyzer
according to the manufacturer's instructions. After the appropriate
warmup period and zero internal calibration procedure, introduce the
calibration gas into the instrument sample probe. Adjust the instrument
meter readout to correspond to the calibration gas value.
Note: If the meter readout cannot be adjusted to the proper value, a
malfunction of the analyzer is indicated and corrective actions are
necessary before use.
4.3 Individual Source Surveys.
4.3.1 Type I -- Leak Definition Based on Concentration. Place the
probe inlet at the surface of the component interface where leakage
could occur. Move the probe along the interface periphery while
observing the instrument readout. If an increased meter reading is
observed, slowly sample the interface where leakage is indicated until
the maximum meter reading is obtained. Leave the probe inlet at this
maximum reading location for approximately two times the instrument
response time. If the maximum observed meter reading is greater than
the leak definition in the applicable regulation, record and report the
results as specified in the regulation reporting requirements. Examples
of the application of this general technique to specific equipment types
are:
a. Valves -- The most common source of leaks from valves is at the
seal between the stem and housing. Place the probe at the interface
where the stem exits the packing gland and sample the stem
circumference. Also, place the probe at the interface of the packing
gland take-up flange seat and sample the periphery. In addition, survey
valve housings of multipart assembly at the surface of all interfaces
where a leak could occur.
b. Flanges and Other Connections -- For welded flanges, place the
probe at the outer edge of the flange-gasket interface and sample the
circumference of the flange. Sample other types of nonpermanent joints
(such as threaded connections) with a similar traverse.
c. Pumps and Compressors -- Conduct a circumferential traverse at the
outer surface of the pump or compressor shaft and seal interface. If
the source is a rotating shaft, position the probe inlet within 1 cm of
the shaft-seal interface for the survey. If the housing configuration
prevents a complete traverse of the shaft periphery, sample all
accessible portions. Sample all other joints on the pump or compressor
housing where leakage could occur.
d. Pressure Relief Devices -- The configuration of most pressure
relief devices prevents sampling at the sealing seat interface. For
those devices equipped with an enclosed extension, or horn, place the
probe inlet at approximately the center of the exhaust area to the
atmosphere.
e. Process Drains -- For open drains, place the probe inlet at
approximately the center of the area open to the atmosphere. For
covered drains, place the probe at the surface of the cover interface
and conduct a peripheral traverse.
f. Open-Ended Lines or Valves -- Place the probe inlet at
approximately the center of the opening to the atmosphere.
g. Seal System Degassing Vents and Accumulator Vents -- Place the
probe inlet at approximately the center of the opening to the
atmosphere.
h. Access Door Seals -- Place the probe inlet at the surface of the
door seal interface and conduct a peripheral traverse.
4.3.2 Type II -- ''No Detectable Emission''.
Determine the local ambient concentration around the source by moving
the probe inlet randomly upwind and downwind at a distance of one to two
meters from the source. If an interference exists with this
determination due to a nearby emission or leak, the local ambient
concentration may be determined at distances closer to the source, but
in no case shall the distance be less than 25 centimeters. Then move
the probe inlet to the surface of the source and determine the
concentration described in 4.3.1. The difference between these
concentrations determines whether there are no detectable emissions.
Record and report the results as specified by the regulation.
For those cases where the regulation requires a specific device
installation, or that specified vents be ducted or piped to a control
device, the existence of these conditions shall be visually confirmed.
When the regulation also requires that no detectable emissions exist,
visual observations and sampling surveys are required. Examples of this
technique are:
(a) Pump or Compressor Seals -- If applicable, determine the type of
shaft seal. Preform a survey of the local area ambient VOC
concentration and determine if detectable emissions exist as described
above.
(b) Seal System Degassing Vents, Accumulator Vessel Vents, Pressure
Relief Devices -- If applicable, observe whether or not the applicable
ducting or piping exists. Also, determine if any sources exist in the
ducting or piping where emissions could occur prior to the control
device. If the required ducting or piping exists and there are no
sources where the emissions could be vented to the atmosphere prior to
the control device, then it is presumed that no detectable emissions are
present. If there are sources in the ducting or piping where emissions
could be vented or sources where leaks could occur, the sampling surveys
described in this paragraph shall be used to determine if detectable
emissions exist.
4.3.3 Alternative Screening Procedure. A screening procedure based
on the formation of bubbles in a soap solution that is sprayed on a
potential leak source may be used for those sources that do not have
continuously moving parts, that do not have surface temperatures greater
than the boiling point or less than the freezing point of the soap
solution, that do not have open areas to the atmosphere that the soap
solution cannot bridge, or that do not exhibit evidence of liquid
leakage. Sources that have these conditions present must be surveyed
using the instrument techniques of 4.3.1 or 4.3.2.
Spray a soap solution over all potential leak sources. The soap
solution may be a commercially available leak detection solution or may
be prepared using concentrated detergent and water. A pressure sprayer
or a squeeze bottle may be used to dispense the solution. Observe the
potential leak sites to determine if any bubbles are formed. If no
bubbles are observed, the source is presumed to have no detectable
emissions or leaks as applicable. If any bubbles are observed, the
instrument techniques of 4.3.1 or 4.3.2 shall be used to determine if a
leak exists, or if the source has detectable emissions, as applicable.
4.4 Instrument Evaluation Procedures. At the beginning of the
instrument performance evaluation test, assemble and start up the
instrument according to the manufacturer's instructions for recommended
warmup period and preliminary adjustments.
4.4.1 Response Factor. Calibrate the instrument with the reference
compound as specified in the applicable regulation. For each organic
species that is to be measured during individual source surveys, obtain
or prepare a known standard in air at a concentration of approximately
80 percent of the applicable leak definition unless limited by
volatility or explosivity. In these cases, prepare a standard at 90
percent of the saturation concentration, or 70 percent of the lower
explosive limit, respectively. Introduce this mixture to the analyzer
and record the observed meter reading. Introduce zero air until a
stable reading is obtained. Make a total of three measurements by
alternating between the known mixture and zero air. Calculate the
response factor for each repetition and the average response factor.
Alternatively, if response factors have been published for the
compounds of interest for the instrument or detector type, the response
factor determination is not required, and existing results may be
referenced. Examples of published response factors for flame ionization
and catalytic oxidation detectors are included in Bibliography.
4.4.2 Calibration Precision. Make a total of three measurements by
alternately using zero gas and the specified calibration gas. Record
the meter readings. Calculate the average algebraic difference between
the meter readings and the known value. Divide this average difference
by the known calibration value and mutiply by 100 to express the
resulting calibration precision as a percentage.
4.4.3 Response Time. Introduce zero gas into the instrument sample
probe. When the meter reading has stabilized, switch quickly to the
specified calibration gas. Measure the time from switching to when 90
percent of the final stable reading is attained. Perform this test
sequence three times and record the results. Calculate the average
response time.
5. Bibliography
1. DuBose, D.A., and G.E. Harris. Response Factors of VOC Analyzers
at a Meter Reading of 10,000 ppmv for Selected Organic Compounds. U.S.
Environmental Protection Agency, Research Triangle Park, NC.
Publication No. EPA 600/2-81-051. September 1981.
2. Brown, G.E., et al. Response Factors of VOC Analyzers Calibrated
with Methane for Selected Organic Compounds. U.S. Environmental
Protection Agency, Research Triangle Park, NC. Publication No. EPA
600/2-81-022. May 1981.
3. DuBose, D.A., et al. Response of Portable VOC Analyzers to
Chemical Mixtures. U.S. Environmental Protection Agency, Research
Triangle Park, NC. Publication No. EPA 600/2-81-110. September 1981.
40 CFR 60.748 Pt. 60, App. A, Meth. 22
1. Introduction
This method involves the visual determination of fugitive emissions,
i.e., emissions not emitted directly from a process stack or duct.
Fugitive emissions include emissions that (1) escape capture by process
equipment exhaust hoods; (2) are emitted during material transfer; (3)
are emitted from buildings housing material processing or handling
equipment; and (4) are emitted directly from process equipment. This
method is used also to determine visible smoke emissions from flares
used for combustion of waste process materials.
This method determines the amount of time that any visible emissions
occur during the observation period, i.e., the accumulated emission
time. This method does not require that the opacity of emissions be
determined. Since this procedure requires only the determination of
whether a visible emission occurs and does not require the determination
of opacity levels, observer certification according to the procedures of
Method 9 are not required. However, it is necessary that the observer
is educated on the general procedures for determining the presence of
visible emissions. As a minimum, the observer must be trained and
knowledgeable regarding the effects on the visibility of emissions
caused by background contrast, ambient lighting, observer position
relative to lighting, wind, and the presence of uncombined water
(condensing water vapor). This training is to be obtained from written
materials found in Citations 1 and 2 of Bibliography or from the lecture
portion of the Method 9 certification course.
2. Applicability and Principle
2.1 Applicability. This method applies to the determination of the
frequency of fugitive emissions from stationary sources (located indoors
or outdoors) when specified as the test method for determining
compliance with new source performance standards.
This method also is applicable for the determination of the frequency
of visible smoke emissions from flares.
2.2 Principle. Fugitive emissions produced during material
processing, handling, and transfer operations or smoke emissions from
flares are visually determined by an observer without the aid of
instruments.
3. Definitions
3.1 Emission Frequency. Percentage of time that emissions are
visible during the observation period.
3.2 Emission Time. Accumulated amount of time that emissions are
visible during the observation period.
3.3 Fugitive Emissions. Pollutant generated by an affected facility
which is not collected by a capture system and is released to the
atmosphere.
3.4 Smoke Emissions. Pollutant generated by combustion in a flare
and occurring immediately downstream of the flame. Smoke occurring
within the flame, but not downstream of the flame, is not considered a
smoke emission.
3.5 Observation Period. Accumulated time period during which
observations are conducted, not to be less than the period specified in
the applicable regulation.
4. Equipment
4.1 Stopwatches. Accumulative type with unit divisions of at least
0.5 seconds; two required.
4.2 Light Meter. Light meter capable of measuring illuminance in the
50- to 200-lux range; required for indoor observations only.
5. Procedure
5.1 Position. Survey the affected facility or building or structure
housing the process to be observed and determine the locations of
potential emissions. If the affected facility is located inside a
building, determine an observation location that is consistent with the
requirements of the applicable regulation (i.e., outside observation of
emissions escaping the building/structure or inside observation of
emissions directly emitted from the affected facility process unit).
Then select a position that enables a clear view of the potential
emission point(s) of the affected facility or of the building or
structure housing the affected facility, as appropriate for the
applicable subpart. A position at least 15 feet, but not more than 0.25
miles, from the emission source is recommended. For outdoor locations,
select a position where the sun is not directly in the observer's eyes.
5.2 Field Records.
5.2.1 Outdoor Location. Record the following information on the
field data sheet (Figure 22-1): company name, industry, process unit,
observer's name, observer's affiliation, and date. Record also the
estimated wind speed, wind direction, and sky condition. Sketch the
process unit being observed and note the observer location relative to
the source and the sun. Indicate the potential and actual emission
points on the sketch.
5.2.2 Indoor Location. Record the following information on the field
data sheet (Figure 22-2): company name, industry, process unit,
observer's name, observer's affiliation, and date. Record as
appropriate the type, location, and intensity of lighting on the data
sheet. Sketch the process unit being observed and note observer
location relative to the source. Indicate the potential and actual
fugitive emission points on the sketch.
5.3 Indoor Lighting Requirements. For indoor locations, use a light
meter to measure the level of illumination at a location as close to the
emission source(s) as is feasible. An illumination of greater than 100
lux (10 foot candles) is considered necessary for proper application of
this method.
5.4 Observations. Record the clock time when observations begin. Use
one stopwatch to monitor the duration of the observation period; start
this stopwatch when the observation period begins. If the observation
period is divided into two or more segments by process shutdowns or
observer rest breaks, stop the stopwatch when a break begins and restart
it without resetting when the break ends. Stop the stopwatch at the end
of the observation period. The accumulated time indicated by this
stopwatch is the duration of the observation period. When the
observation period is completed, record the clock time.
During the observation period, continously watch the emission source.
Upon observing an emission (condensed water vapor is not considered an
emission), start the second accumulative stopwatch; stop the watch when
the emission stops. Continue this procedure for the entire observation
period. The accumulated elapsed time on this stopwatch is the total
time emissions were visible during the observation period, i.e., the
emission time.
5.4.1 Observation Period. Choose an observation period of sufficient
length to meet the requirements for determining compliance with the
emission regulation in the applicable subpart. When the length of the
observation period is specifically stated in the applicable subpart, it
may not be necessary to observe the source for this entire period if the
emission time required to indicate noncompliance (based on the specified
observation period) is observed in a shorter time period. In other
words, if the regulation prohibits emissions for more than 6 minutes in
any hour, then observations may (optional) be stopped after an emission
time of 6 minutes is exceeded. Similarly, when the regulation is
expressed as an emission frequency and the regulation prohibits
emissions for greater than 10 percent of the time in any hour, then
observations may (optional) be terminated after 6 minutes of emissions
are observed since 6 minutes is 10 percent of an hour. In any case, the
observation period shall not be less than 6 minutes in duration. In
some cases, the process operation may be intermittent or cyclic. In
such cases, it may be convenient for the observation period to coincide
with the length of the process cycle.
5.4.2 Observer Rest Breaks. Do not observe emissions continuously
for a period of more than 15 to 20 minutes without taking a rest break.
For sources requiring observation periods of greater than 20 minutes,
the observer shall take a break of not less than 5 minutes and not more
than 10 minutes after every 15 to 20 minutes of observation. If
continuous observations are desired for extended time periods, two
observers can alternate between making observations and taking breaks.
5.4.3 Visual Interference. Occasionally, fugitive emissions from
sources other than the affected facility (e.g., road dust) may prevent a
clear view of the affected facility. This may particularly be a problem
during periods of high wind. If the view of the potential emission
points is obscured to such a degree that the observer questions the
validity of continuing observations, then the observations are
terminated, and the observer clearly notes this fact on the data form.
5.5 Recording Observations. Record the accumulated time of the
observation period on the data sheet as the observation period duration.
Record the accumulated time emissions were observed on the data sheet
as the emission time. Record the clock time the observation period
began and ended, as well as the clock time any observer breaks began and
ended.
6. Calculations
If the applicable subpart requires that the emission rate be
expressed as an emission frequency (in percent), determine this value as
follows: Divide the accumulated emission time (in seconds) by the
duration of the observation period (in seconds) or by any minimum
observation period required in the applicable subpart, if the acutal
observation period is less than the required period and multiply this
quotient by 100.
7. Bibliography
1. Missan, Robert and Arnold Stein. Guidelines for Evaluation of
Visible Emissions Certification, Field Procedures, Legal Aspects, and
Background Material. EPA Publication No. EPA-340/1-75-007. April 1975
2. Wohlschlegel, P. and D. E. Wagoner. Guideline for Development of
a Quality Assurance Program: Volume IX -- Visual Determination of
Opacity Emissions From Stationary Sources. EPA Publication No.
EPA-650/4-74-005-i. November 1975.
Insert illus. O142
Insert illus. O143
40 CFR 60.748 Pt. 60, App. A, Meth. 23
1.1 Applicability. This method is applicable to the determination of
polychlorinated dibenzo-p-dioxins (PCDD's) and polychlorinated
dibenzofurans (PCDF's) from stationary sources.
1.2 Principle. A sample is withdrawn from the gas stream
isokinetically and collected in the sample probe, on a glass fiber
filter, and on a packed column of adsorbent material. The sample cannot
be separated into a particle vapor fraction. The PCDD's and PCDF's are
extracted from the sample, separated by high resolution gas
chromatography, and measured by high resolution mass spectrometry.
2.1 Sampling. A schematic of the sampling train used in this method
is shown in Figure 23-1. Sealing greases may not be used in assembling
the train. The train is identical to that described in section 2.1 of
Method 5 of this appendix with the following additions:
Insert illustration 010
2.1.1 Nozzle. The nozzle shall be made of nickel, nickel-plated
stainless steel, quartz, or borosilicate glass.
2.1.2 Sample Transfer Lines. The sample transfer lines, if needed,
shall be heat traced, heavy walled TFE ( 1/2 in. OD with 1/8 in. wall)
with connecting fittings that are capable of forming leak-free,
vacuum-tight connections without using sealing greases. The line shall
be as short as possible and must be maintained at 120 C.
2.1.1 Filter Support. Teflon or Teflon-coated wire.
2.1.2 Condenser. Glass, coil type with compatible fittings. A
schematic diagram is shown in Figure 23-2.
2.1.3 Water Bath. Thermostatically controlled to maintain the gas
temperature exiting the condenser at >20 C (68 F).
2.1.4 Adsorbent Module. Glass container to hold the solid adsorbent.
A shematic diagram is shown in Figure 23-2. Other physical
configurations of the resin trap/condenser assembly are acceptable. The
connecting fittings shall form leak-free, vacuum tight seals. No
sealant greases shall be used in the sampling train. A coarse glass
frit is included to retain the adsorbent.
2.2 Sample Recovery.
2.2.1 Fitting Caps. Ground glass, Teflon tape, or aluminum foil
(Section 2.2.6) to cap off the sample exposed sections of the train.
2.2.2 Wash Bottles. Teflon, 500-ml.
2.2.3 Probe-Liner Probe-Nozzle, and Filter-Holder Brushes. Inert
bristle brushes with precleaned stainless steel or Teflon handles. The
probe brush shall have extensions of stainless steel or Teflon, at least
as long as the probe. The brushes shall be properly sized and shaped to
brush out the nozzle, probe liner, and transfer line, if used.
Insert illustration 012
2.2.4 Filter Storage Container. Sealed filter holder, wide-mouth
amber glass jar with Teflon-lined cap, or glass petri dish.
2.2.5 Balance. Triple beam.
2.2.6 Aluminum Foil. Heavy duty, hexane-rinsed.
2.2.7 Metal Storage Container. Air tight container to store silica
gel.
2.2.8 Graduated Cylinder. Glass, 250-ml with 2-ml graduation.
2.2.9 Glass Sample Storage Container. Amber glass bottle for sample
glassware washes, 500- or 1000-ml, with leak free Teflon-lined caps.
2.3 Analysis.
2.3.1 Sample Container. 125- and 250-ml flint glass bottles with
Teflon-lined caps.
2.3.2 Test Tube. Glass.
2.3.3 Soxhlet Extraction Apparatus. Capable of holding 43 x 123 mm
extraction thimbles.
2.3.4 Extraction Thimble. Glass, precleaned cellulosic, or glass
fiber.
2.3.5 Pasteur Pipettes. For preparing liquid chromatographic
columns.
2.3.6 Reacti-vials. Amber glass, 2-ml, silanized prior to use.
2.3.7 Rotary Evaporator. Buchi/Brinkman RF-121 or equivalent.
2.3.8 Nitrogen Evaporative Concentrator. N-Evap Analytical
Evaporator Model III or equivalent.
2.3.9 Separatory Funnels. Glass, 2-liter.
2.3.10 Gas Chromatograph. Consisting of the following components:
2.3.10.1 Oven. Capable of maintaining the separation column at the
proper operating temperature C and performing programmed increases in
temperature at rates of at least 40 C/min.
2.3.10.2 Temperature Gauge. To monitor column oven, detector, and
exhaust temperatures 1 C.
2.3.10.3 Flow System. Gas metering system to measure sample, fuel,
combustion gas, and carrier gas flows.
2.3.10.4 Capillary Columns. A fused silica column, 60 0.25 mm
inside diameter (ID), coated with DB-5 and a fused silica column, 30 m
0.25 mm ID coated with DB-225. Other column systems may be used
provided that the user is able to demonstrate using calibration and
performance checks that the column system is able to meet the
specifications of section 6.1.2.2.
2.3.11 Mass Spectrometer. Capable of routine operation at a
resolution of 1:10000 with a stability of 5 ppm.
2.3.12 Data System. Compatible with the mass spectrometer and
capable of monitoring at least five groups of 25 ions.
2.3.13 Analytical Balance. To measure within 0.1 mg.
3.1 Sampling.
3.1.1 Filters. Glass fiber filters, without organic binder,
exhibiting at least 99.95 percent efficiency (<0.05 percent penetration)
on 0.3-micron dioctyl phthalate smoke particles. The filter efficiency
test shall be conducted in accordance with ASTM Standard Method D
2986-71 (Reapproved 1978) (incorporated by reference -- see 60.17).
3.1.1.1 Precleaning. All filters shall be cleaned before their
initial use. Place a glass extraction thimble and 1 g of silica gel and
a plug of glass wool into a Soxhlet apparatus, charge the apparatus with
toluene, and reflux for a minimum of 3 hours. Remove the toluene and
discard it, but retain the silica gel. Place no more than 50 filters in
the thimble onto the silica gel bed and top with the cleaned glass wool.
Charge the Soxhlet with toluene and reflux for 16 hours. After
extraction, allow the Soxhlet to cool, remove the filters, and dry them
under a clean N2 stream. Store the filters in a glass petri dish sealed
with Teflon tape.
3.1.2 Adsorbent Resin. Amberlite XAD-2 resin. Thoroughly cleaned
before initial use.
3.1.2.1 Cleaning Procedure. This procedure may be carried out in a
giant Soxhlet extractor. An all-glass filter thimble containing an
extra-course frit is used for extraction of XAD-2. The frit is recessed
10-15 mm above a crenelated ring at the bottom of the thimble to
facilitate drainage. The resin must be carefully retained in the
extractor cup with a glass wool plug and a stainless steel ring because
it floats on methylene chloride. This process involves sequential
extraction in the following order.
3.1.2.2 Drying.
3.1.2.2.1 Drying Column. Pyrex pipe, 10.2 cm ID by 0.6 m long, with
suitable retainers.
3.1.2.2.2 Procedure. The adsorbent must be dried with clean inert
gas. Liquid nitrogen from a standard commercial liquid nitrogen
cylinder has proven to be a reliable source of large volumes of gas free
from organic contaminants. Connect the liquid nitrogen cylinder to the
column by a length of cleaned copper tubing, 0.95 cm ID, coiled to pass
through a heat source. A convenient heat source is a water-bath heated
from a steam line. The final nitrogen temperature should only be warm
to the touch and not over 40 C. Continue flowing nitrogen through the
adsorbent until all the residual solvent is removed. The flow rate
should be sufficient to gently agitate the particles but not so
excessive as the cause the particles to fracture.
3.1.2.3 Quality Control Check. The adsorbent must be checked for
residual toluene.
3.1.2.3.1 Extraction. Weigh 1.0 g sample of dried resin into a small
vial, add 3 ml of toluene, cap the vial, and shake it well.
3.1.2.3.2 Analysis. Inject a 2 l sample of the extract into a gas
chromatograph operated under the following conditions:
Column: 6 ft 1/8 in stainless steel containing 10 percent OV-101
on 100/120 Supelcoport.
Carrier Gas: Helium at a rate of 30 ml/min.
Detector: Flame ionization detector operated at a sensitivity of 4
10^11 A/mV.
Injection Port Temperature: 250 C.
Detector Temperature: 305 C.
Oven Temperature: 30 C for 4 min; programmed to rise at 40 C/min
until it reaches 250 C; return to 30 C after 17 minutes.
Compare the results of the analysis to the results from the reference
solution. Prepare the reference solution by injection 2.5 l of
methylene chloride into 100 ml of toluene. This corresponds to 100 g
of methylene chloride per g of adsorbent. The maximum acceptable
concentration is 1000 g/g of adsorbent. If the adsorbent exceeds this
level, drying must be continued until the excess methylene chloride is
removed.
3.1.2.4 Storage. The adsorbent must be used within 4 weeks of
cleaning. After cleaning, it may be stored in a wide mouth amber glass
container with a Teflon-lined cap or placed in one of the glass
adsorbent modules tightly sealed with glass stoppers. If precleaned
adsorbent is purchased in sealed containers, it must be used within 4
weeks after the seal is broken.
3.1.3 Glass Wool. Cleaned by sequential immersion in three aliquots
of methylene chloride, dried in a 110 C oven, and stored in a methylene
chloride-washed glass jar with a Teflon-lined screw cap.
3.1.4 Water. Deionized distilled and stored in a methylene
chloride-rinsed glass container with a Teflon-lined screw cap.
3.1.5 Silica Gel. Indicating type, 6 to 16 mesh. If previously
used, dry at 175 C (350 F) for two hours. New silica gel may be used
as received. Alternately other types of desiccants (equivalent or
better) may be used, subject to the approval of the Administrator.
3.1.6 Chromic Acid Cleaning Solution. Dissolve 20 g of sodium
dichromate in 15 ml of water, and then carefully add 400 ml of
concentrated sulfuric acid.
3.2 Sample Recovery.
3.2.2 Acetone. Pesticide quality.
3.2.2 Methylene Chloride. Pesticide qualtity.
3.2.3 Toluene. Pesticide quality.
3.3 Analysis.
3.3.1 Potassium Hydroxide. ACS grade, 2-percent (weight/volume) in
water.
3.3.2 Sodium Sulfate. Granulated, reagent grade. Purify prior to
use by rinsing with methylene chloride and oven drying. Store the
cleaned material in a glass container with a Teflon-lined screw cap.
3.3.3 Sulfuric Acid. Reagent grade.
3.3.4 Sodium Hydroxide. 1.0 N. Weigh 40 g of sodium hydroxide into a
1-liter volumetric flask. Dilute to 1 liter with water.
3.3.5 Hexane. Pesticide grade.
3.3.6 Methylene Chloride. Pesticide grade.
3.3.7 Benzene. Pesticide Grade.
3.3.8 Ethyl Acetate.
3.3.9 Methanol. Pesticide Grade.
3.3.10 Toluene. Pesticide Grade.
3.3.11 Nonane. Pesticide Grade.
3.3.12 Cyclohexane. Pesticide Grade.
3.3.13 Basic Alumina. Activity grade 1, 100-200 mesh. Prior to use,
activate the alumina by heating for 16 hours at 130 C before use.
Store in a desiccator. Pre-activated alumina may be purchased from a
supplier and may be used as received.
3.3.14 Silica Gel. Bio-Sil A, 100-200 mesh. Prior to use, activate
the silica gel by heating for at least 30 minutes at 180 C. After
cooling, rinse the silica gel sequentially with methanol and methylene
chloride. Heat the rinsed silica gel at 50 C for 10 minutes, then
increase the temperature gradually to 180 C over 25 minutes and
maintain it at this temperature for 90 minutes. Cool at room
temperature and store in a glass container with a Teflon-lined screw
cap.
3.3.15 Silica Gel Impregnated with Sulfuric Acid. Combine 100 g of
silica gel with 44 g of concentrated sulfuric acid in a screw capped
glass bottle and agitate thoroughly. Disperse the solids with a
stirring rod until a uniform mixture is obtained. Store the mixture in
a glass container with a Teflon-lined screw cap.
3.3.16 Silica Gel Impregnated with Sodium Hydroxide. Combine 39 g of
1 N sodium hydroxide with 100 g of silica gel in a screw capped glass
bottle and agitate thoroughly. Disperse solids with a stirring rod
until a uniform mixture is obtained. Store the mixture in glass
container with a Teflon-lined screw cap.
3.3.17 Carbon/Celite. Combine 10.7 g of AX-21 carbon with 124 g of
Celite 545 in a 250-ml glass bottle with a Teflon-lined screw cap.
Agitate the mixture thoroughly until a uniform mixture is obtained.
Store in the glass container.
3.3.18 Nitrogen. Ultra high purity.
3.3.19 Hydrogen. Ultra high purity.
3.3.20 Internal Standard Solution. Prepare a stock standard solution
containing the isotopically labelled PCDD's and PCDF's at the
concentrations shown in Table 1 under the heading ''Internal Standards''
in 10 ml of nonane.
3.3.21 Surrogate Standard Solution. Prepare a stock standard
solution containing the isotopically labelled PCDD's and PCDF's at the
concentrations shown in Table 1 under the heading ''Surrogate
Standards'' in 10 ml of nonane.
3.3.22 Recovery Standard Solution. Prepare a stock standard solution
containing the isotopically labelled PCDD's and PCDF's at the
concentrations shown in Table 1 under the heading ''Recovery Standards''
in 10 ml of nonane.
4.1 Sampling. The complexity of this method is such that, in order to
obtain reliable results, testers should be trained and experienced with
the test procedures.
4.1.1 Pretest Preparation.
4.1.1.1 Cleaning Glassware. All glass components of the train
upstream of and including the adsorbent module, shall be cleaned as
described in section 3A of the ''Manual of Analytical Methods for the
Analysis of Pesticides in Human and Environmental Samples.'' Special
care shall be devoted to the removal of residual silicone grease
sealants on ground glass connections of used glassware. Any residue
shall be removed by soaking the glassware for several hours in a chromic
acid cleaning solution prior to cleaning as described above.
4.1.1.2 Adsorbent Trap. The traps must be loaded in a clean area to
avoid contamination. They may not be loaded in the field. Fill a trap
with 20 to 40 g of XAD-2. Follow the XAD-2 with glass wool and tightly
cap both ends of the trap. Add 100 l of the surrogate standard
solution (section 3.3.21) to each trap.
4.1.1.3 Sample Train. It is suggested that all components be
maintained according to the procedure described in APTD-0576.
4.1.1.4 Silica Gel. Weigh several 200 to 300 g portions of silica
gel in an air tight container to the nearest 0.5 g. Record the total
weight of the silica gel plus container, on each container. As an
alternative, the silica gel may be weighed directly in its impinger or
sampling holder just prior to sampling.
4.1.1.5 Filter. Check each filter against light for irregularities
and flaws or pinhole leaks. Pack the filters flat in a clean glass
container.
4.1.2 Preliminary Determinations. Same as section 4.1.2 of Method 5.
4.1.3 Preparation of Collection Train.
4.1.3.1 During preparation and assembly of the sampling train, keep
all train openings where contamination can enter, sealed until just
prior to assembly or until sampling is about to begin.
Note: Do not use sealant grease in assembling the train.
4.1.3.2 Place approximately 100 ml of water in the second and third
impingers, leave the first and fourth impingers empty, and transfer
approximately 200 to 300 g of preweighed silica gel from its container
to the fifth impinger.
4.1.3.3 Place the silica gel container in a clean place for later use
in the sample recovery. Alternatively, the weight of the silica gel
plus impinger may be determined to the nearest 0.5 g and recorded.
4.1.3.4 Assemble the train as shown in Figure 23-1.
4.1.3.5 Turn on the adsorbent module and condenser coil recirculating
pump and begin monitoring the adsorbent module gas entry temperature.
Ensure proper sorbent temperature gas entry temperature before
proceeding and before sampling is initiated. It is extremely important
that the XAD-2 adsorbent resin temperature never exceed 50 C because
thermal decomposition will occur. During testing, the XAD-2 temperature
must not exceed 20 C for efficient capture of the PCDD's and PCDF's.
4.1.4 Leak-Check Procedure. Same as Method 5, section 4.1.4.
4.1.5 Sample Train Operation. Same as Method 5, section 4.1.5.
4.2 Sample Recovery. Proper cleanup procedure begins as soon as the
probe is removed from the stack at the end of the sampling period. Seal
the nozzle end of the sampling probe with Teflon tape or aluminum foil.
When the probe can be safely handled, wipe off all external
particulate matter near the tip of the probe. Remove the probe from the
train and close off both ends with aluminum foil. Seal off the inlet to
the train with Teflon tape, a ground glass cap, or aluminum foil.
Transfer the probe and impinger assembly to the cleanup area. This
area shall be clean and enclosed so that the chances of losing or
contaminating the sample are minimized. Smoking, which could
contaminate the sample, shall not be allowed in the cleanup area.
Inspect the train prior to and during disassembly and note any
abnormal conditions, e.g., broken filters, colored impinger liquid, etc.
Treat the samples as follows:
4.2.1 Container No. 1. Either seal the filter holder or carefully
remove the filter from the filter holder and place it in its identified
container. Use a pair of cleaned tweezers to handle the filter. If it
is necessary to fold the filter, do so such that the particulate cake is
inside the fold. Carefully transfer to the container any particulate
matter and filter fibers which adhere to the filter holder gasket, by
using a dry inert bristle brush and a sharp-edged blade. Seal the
container.
4.2.2 Adsorbent Module. Remove the module from the train, tightly
cap both ends, label it, cover with aluminum foil, and store it on ice
for transport to the laboratory.
4.2.3 Container No. 2. Quantitatively recover material deposited in
the nozzle, probe transfer lines, the front half of the filter holder,
and the cyclone, if used, first, by brushing while rinsing three times
each with acetone and then, by rinsing the probe three times with
methylene chloride. Collect all the rinses in Container No. 2.
Rinse the back half of the filter holder three times with acetone.
Rinse the connecting line between the filter and the condenser three
times with acetone. Soak the connecting line with three separate
portions of methylene chloride for 5 minutes each. If using a separate
condenser and adsorbent trap, rinse the condenser in the same manner as
the connecting line. Collect all the rinses in Container No. 2 and
mark the level of the liquid on the container.
4.2.4 Container No. 3. Repeat the methylene chloride-rinsing
described in Section 4.2.3 using toluene as the rinse solvent. Collect
the rinses in Container No. 3 and mark the level of the liquid on the
container.
4.2.5 Impinger Water. Measure the liquid in the first three
impingers to within 1 ml by using a graduated cylinder or by weighing
it to within 0.5 g by using a balance. Record the volume or weight of
liquid present. This information is required to calculate the moisture
content of the effluent gas.
Discard the liquid after measuring and recording the volume or
weight.
4.2.7 Silica Gel. Note the color of the indicating silica gel to
determine if it has been completely spent and make a mention of its
condition. Transfer the silica gel from the fifth impinger to its
original container and seal.
All glassware shall be cleaned as described in section 3A of the
''Manual of Analytical Methods for the Analysis of Pesticides in Human
and Environmental Samples.'' All samples must be extracted within 30
days of collection and analyzed within 45 days of extraction.
5.1 Sample Extraction.
5.1.1 Extraction System. Place an extraction thimble (section
2.3.4), 1 g of silica gel, and a plug of glass wool into the Soxhlet
apparatus, charge the apparatus with toluene, and reflux for a minimum
of 3 hours. Remove the toluene and discard it, but retain the silica
gel. Remove the extraction thimble from the extraction system and place
it in a glass beaker to catch the solvent rinses.
5.1.2 Container No. 1 (Filter). Transfer the contents directly to
the glass thimble of the extraction system and extract them
simultaneously with the XAD-2 resin.
5.1.3 Adsorbent Cartridge. Suspend the adsorbent module directly
over the extraction thimble in the beaker (See section 5.1.1). The glass
frit of the module should be in the up position. Using a Teflon squeeze
bottle containing toluene, flush the XAD-2 into the thimble onto the bed
of cleaned silica gel. Thoroughly rinse the glass module catching the
rinsings in the beaker containing the thimble. If the resin is wet,
effective extraction can be accomplished by loosely packing the resin in
the thimble. Add the XAD-2 glass wool plug into the thimble.
5.1.4 Container No. 2 (Acetone and Methylene Chloride). Concentrate
the sample to a volume of about 1-5 ml using the rotary evaporator
apparatus, at a temperature of less than 37 C. Rinse the sample
container three times with small portions of methylene chloride and add
these to the concentrated solution and concentrate further to near
dryness. This residue contains particulate matter removed in the rinse
of the train probe and nozzle. Add the concentrate to the filter and
the XAD-2 resin in the Soxhlet apparatus described in section 5.1.1.
5.1.5 Extraction. Add 100 l of the internal standard solution
(Section 3.3.20) to the extraction thimble containing the contents of
the adsorbent cartridge, the contents of Container No. 1, and the
concentrate from section 5.1.4. Cover the contents of the extraction
thimble with the cleaned glass wool plug to prevent the XAD-2 resin from
floating into the solvent reservoir of the extractor. Place the thimble
in the extractor, and add the toluene contained in the beaker to the
solvent reservoir. Pour additional toluene to fill the reservoir
approximately 2/3 full. Add Teflon boiling chips and assemble the
apparatus. Adjust the heat source to cause the extractor to cycle three
times per hour. Extract the sample for 16 hours. After extraction,
allow the Soxhlet to cool. Transfer the toluene extract and three 10-ml
rinses to the rotary evaporator. Concentrate the extract to
approximately 10 ml. At this point the analyst may choose to split the
sample in half. If so, split the sample, store one half for future use,
and analyze the other according to the procedures in sections 5.2 and
5.3. In either case, use a nitrogen evaporative concentrator to reduce
the volume of the sample being analyzed to near dryness. Dissolve the
residue in 5 ml of hexane.
5.1.6 Container No. 3 (Toluene Rinse). Add 100 l of the Internal
Standard solution (section 3.3.2) to the contents of the container.
Concentrate the sample to a volume of about 1-5 ml using the rotary
evaporator apparatus at a temperature of less than 37 C. Rinse the
sample container apparatus at a temperature of less than 37 C. Rinse
the sample container three times with small portions of toluene and add
these to the concentrated solution and concentrate further to near
dryness. Analyze the extract separately according to the procedures in
sections 5.2 and 5.3, but concentrate the solution in a rotary
evaporator apparatus rather than a nitrogen evaporative concentrator.
5.2 Sample Cleanup and Fractionation.
5.2.1 Silica Gel Column. Pack one end of a glass column, 20 mm x 230
mm, with glass wool. Add in sequence, 1 g silica gel, 2 g of sodium
hydroxide impregnated silica gel, 1 g silica gel, 4 g of acid-modified
silica gel, and 1 g of silica gel. Wash the column with 30 ml of hexane
and discard it. Add the sample extract, dissolved in 5 ml of hexane to
the column with two additional 5-ml rinses. Elute the column with an
additional 90 ml of hexane and retain the entire eluate. Concentrate
this solution to a volume of about 1 ml using the nitrogen evaporative
concentrator (section 2.3.7).
5.2.2 Basic Alumina Column. Shorten a 25-ml disposable Pasteur
pipette to about 16 ml. Pack the lower section with glass wool and 12 g
of basic alumina. Transfer the concentrated extract from the silica gel
column to the top of the basic alumina column and elute the column
sequentially with 120 ml of 0.5 percent methylene chloride in hexane
followed by 120 ml of 35 percent methylene chloride in hexane. Discard
the first 120 ml of eluate. Collect the second 120 ml of eluate and
concentrate it to about 0.5 ml using the nitrogen evaporative
concentrator.
5.2.3 AX-21 Carbon/Celite 545 Column. Remove the botton 0.5 in.
from the tip of a 9-ml disposable Pasteur pipette. Insert a glass fiber
filter disk in the top of the pipette 2.5 cm from the constriction. Add
sufficient carbon/celite mixture to form a 2 cm column. Top with a
glass wool plug. In some cases AX-21 carbon fines may wash through the
glass wool plug and enter the sample. This may be prevented by adding a
celite plug to the exit end of the column. Rinse the column in sequence
with 2 ml of 50 percent benzene in ethyl acetate, 1 ml of 50 percent
methylene chloride in cyclohexane, and 2 ml of hexane. Discard these
rinses. Transfer the concentrate in 1 ml of hexane from the basic
alumina column to the carbon/celite column along with 1 ml of hexane
rinse. Elute the column sequentially with 2 ml of 50 percent methylene
chloride in hexane and 2 ml of 50 percent benzene in ethyl acetate and
discard these eluates. Invert the column and elute in the reverse
direction with 13 ml of toluene. Collect this eluate. Concentrate the
eluate in a rotary evaporator at 50 C to about 1 ml. Transfer the
concentrate to a Reacti-vial using a toluene rinse and concentrate to a
volume of 200 l using a stream of N2. Store extracts at room
temperature, shielded from light, until the analysis is performed.
5.3 Analysis. Analyze the sample with a gas chromatograph coupled to
a mass spectrometer (GC/MS) using the instrumental parameters in
sections 5.3.1 and 5.3.2. Immediately prior to analysis, add a 20 l
aliquot of the Recovery Standard solution from Table 1 to each sample.
A 2 l aliquot of the extract is injected into the GC. Sample extracts
are first analyzed using the DB-5 capillary column to determine the
concentration of each isomer of PCDD's and PCDF's (tetra-through octa-).
If tetra-chlorinated dibenzofurans are detected in this analysis, then
analyze another aliquot of the sample in a separate run, using the
DB-225 column to measure the 2,3,7,8 tetra-chloro dibenzofuran isomer.
Other column systems may be used, provided that the user is able to
demonstrate using calibration and performance checks that the column
system is able to meet the specifications of section 6.1.2.2.
5.3.1 Gas Chromatograph Operating Conditions.
5.3.1.1 Injector. Configured for capillary column, splitless, 250 C..
5.3.1.2 Carrier Gas. Helium, 1-2 ml/min.
5.3.1.3 Oven. Initially at 150 C. Raise by at least 40 C/min to 190
C and then at 3 C/min up to 300 C.
5.3.2 High Resolution Mass Spectrometer.
5.3.2.1 Resolution. 10000 m/e.
5.3.2.2 Ionization Mode. Electron impact.
5.3.2.3 Source Temperature 250 C.
5.3.2.4 Monitoring Mode. Selected ion monitoring. A list of the
various ions to be monitored is summarized in Table 3.
5.3.2.5 Identification Criteria. The following identification
criteria shall be used for the characterization of polychlorinated
dibenzodioxins and dibenzofurans.
1. The integrated ion-abundance ratio (M/M+2 or M+2/M+4) shall be
within 15 percent of the theoretical value. The acceptable
ion-abundance ratio ranges for the identification of chlorine-containing
compounds are given in Table 4.
2. The retention time for the analytes must be within 3 seconds of
the corresponding /1/ /3/ C-labeled internal standard, surrogate or
alternate standard.
3. The monitored ions, shown in Table 3 for a given analyte, shall
reach their maximum within 2 seconds of each other.
4. The identification of specific isomers that do not have
corresponding /1/ /3/ C-labeled standards is done by comparison of the
relative retention time (RRT) of the analyte to the nearest internal
standard retention time with reference (i.e., within 0.005 RRT units) to
the comparable RRT's found in the continuing calibration.
5. The signal to noise ratio for all monitored ions must be greater
than 2.5.
6. The confirmation of 2, 3, 7, 8-TCDD and 2, 3, 7, 8-TCDF shall
satisfy all of the above identification criteria.
7. For the identification of PCDF's, no signal may be found in the
corresponding PCDPE channels.
5.3.2.6 Quantification. The peak areas for the two ions monitored for
each analyte are summed to yield the total response for each analyte.
Each internal standard is used to quantify the indigenous PCDD's or
PCDF's in its homologous series. For example, the /1/ /3/
C12-2,3,7,8-tetra chlorinated dibenzodioxin is used to calculate the
concentrations of all other tetra chlorinated isomers. Recoveries of
the tetra- and penta- internal standards are calculated using the /1/
/3/ C12-1,2,3,4-TCDD. Recoveries of the hexa- through octa-
C12-1,2,3,7,8,95-HxCDD. Recoveries of the surrogate standards are
calculated using the corresponding homolog from the internal standard.
Same as Method 5 with the following additions.
6.1 GC/MS System.
6.1.1 Initial Calibration. Calibrate the GC/MS system using the set
of five standards shown in Table 2. The relative standard deviation for
the mean response factor from each of the unlabeled analytes (Table 2)
and of the internal, surrogate, and alternate standards shall be less
than or equal to the values in Table 5. The signal to noise ratio for
the GC signal present in every selected ion current profile shall be
greater than or equal to 2.5. The ion abundance ratios shall be within
the control limits in Table 4.
6.1.2 Daily Performance Check.
6.1.2.1 Calibration Check. Inject on l of solution Number 3 from
Table 2. Calculate the relative response factor (RRF) for each compound
and compare each RRF to the corresponding mean RRF obtained during the
initial calibration. The analyzer performance is acceptable if the
measured RRF's for the labeled and unlabeled compounds for the daily run
are within the limits of the mean values shown in Table 5. In addition,
the ion-abundance ratios shall be within the allowable control limits
shown in Table 4.
6.1.2.2 Column Separation Check. Inject a solution of a mixture of
PCDD's and PCDF's that documents resolution between 2,3,7,8-TCDD and
other TCDD isomers. Resolution is defined as a valley between peaks
that is less than 25 percent of the lower of the two peaks. Identify
and record the retention time windows for each homologous series.
Perform a similar resolution check on the confirmation column to
document the resolution between 2,3,7,8 TCDF and other TCDF isomers.
6.2 Lock Channels. Set mass spectrometer lock channels as specified
in Table 3. Monitor the quality control check channels specified in
Table 3 to verify instrument stability during the analysis.
7.1 Sampling Train Collection Efficiency Check. Add 100 l of the
surrogate standards in Table 1 to the absorbent cartridge of each train
before collecting the field samples.
7.2 Internal Standard Percent Recoveries. A group of nine carbon
labeled PCDD's and PCDF's representing, the tetra-through
octachlorinated homologues, is added to every sample prior to
extraction. The role of the internal standards is to quantify the
native PCDD's and PCDF's present in the sample as well as to determine
the overall method efficiency. Recoveries of the internal standards
must be between 40 to 130 percent for the tetra-through hexachlorinated
compounds while the range is 25 to 130 percent for the higher hepta- and
octachlorinated homologues.
7.3 Surrogate Recoveries. The five surrogate compounds in Table 2
are added to the resin in the adsorbent sampling cartridge before the
sample is collected. The surrogate recoveries are measured relative to
the internal standards and are a measure of collection efficiency. They
are not used to measure native PCDD's and PCDF's. All recoveries shall
be between 70 and 130 percent. Poor recoveries for all the surrogates
may be an indication of breakthrough in the sampling train. If the
recovery of all standards is below 70 percent, the sampling runs must be
repeated. As an alternative, the sampling runs do not have to be
repeated if the final results are divided by the fraction of surrogate
recovery. Poor recoveries of isolated surrogate compounds should not be
grounds for rejecting an entire set of the samples.
7.4 Toluene QA Rinse. Report the results of the toluene QA rinse
separately from the total sample catch. Do not add it to the total
sample.
8.1 Applicability. When the method is used to analyze samples to
demonstrate compliance with a source emission regulation, an audit
sample must be analyzed, subject to availability.
8.2 Audit Procedure. Analyze an audit sample with each set of
compliance samples. The audit sample contains tetra through octa
isomers of PCDD and PCDF. Concurrently, analyze the audit sample and a
set of compliance samples in the same manner to evaluate the technique
of the analyst and the standards preparation. The same analyst,
analytical reagents, and analytical system shall be used both for the
compliance samples and the EPA audit sample.
8.3 Audit Sample Availability. Audit samples will be supplied only
to enforcement agencies for compliance tests. The availability of audit
samples may be obtained by writing: Source Test Audit Coordinator
(MD-77B), Quality Assurance Division, Atmospheric Research and Exposure
Assessment Laboratory, U.S. Environmental Protection Agency, Research
Triangle Park, NC 27711, or by calling the Source Test Audit Coordinator
(STAC) at (919) 541-7834. The request for the audit sample must be made
at least 30 days prior to the scheduled compliance sample analysis.
8.4 Audit Results. Calculate the audit sample concentration
according to the calculation procedure described in the audit
instructions included with the audit sample. Fill in the audit sample
concentration and the analyst's name on the audit response form included
with the audit instructions. Send one copy to the EPA Regional Office
or the appropriate enforcement agency and a second copy to the STAC.
The EPA Regional office or the appropriate enforcement agency will
report the results of the audit to the laboratory being audited.
Include this response with the results of the compliance samples in
relevant reports to the EPA Regional Office or the appropriate
enforcement agency.
Same as Method 5, section 6 with the following additions.
9.1 Nomenclature.
Aai=Integrated ion current of the noise at the retention time of the
analyte.
A*ci=Integrated ion current of the two ions characteristic of the
internal standard i in the calibration standard.
Acij=Integrated ion current of the two ions characteristic of
compound i in the jth calibration standard.
A*cij=Integrated ion current of the two ions characteristic of the
internal standard i in the jth calibration standard.
Acsi=Integrated ion current of the two ions characteristic of
surrogate compound i in the calibration standard.
Ai=Integrated ion current of the two ions characteristic of compound
i in the sample.
A*i=Integrated ion current of the two ions characteristic of internal
standard i in the sample.
Ars=Integrated ion current of the two ions characteristic of the
recovery standard.
Asi=Integrated ion current of the two ions characteristic of
surrogate compound i in the sample.
Ci=Concentration of PCDD or PCDF i in the sample, pg/M /3/ .
CT=Total concentration of PCDD's or PCDF's in the sample, pg/M /3/ .
mci=Mass of compound i in the calibration standard injected into the
analyzer, pg.
mrs=Mass of recovery standard in the calibration standard injected
into the analyzer, pg.
msi=Mass of surrogate compound i in the calibration standard, pg.
RRFi=Relative response factor.
RRFrs=Recovery standard response factor.
RRFs=Surrogate compound response factor.
9.2 Average Relative Response Factor.
9.3 Concentration of the PCDD's and PCDF's.
9.4 Recovery Standard Response Factor.
9.5 Recovery of Internal Standards (R*).
9.6 Surrogate Compound Response Factor.
9.7 Recovery of Surrogate Compounds (Rs).
9.8 Minimum Detectable Limit (MDL).
9.9 Total Concentration of PCDD's and PCDF's in the Sample.
Any PCDD's or PCDF's that are reported as nondetected (below the MDL)
shall be counted as zero for the purpose of calculating the total
concentration of PCDD's and PCDF's in the sample.
1. American Society of Mechanical Engineers. Sampling for the
Determination of Chlorinated Organic Compounds in Stack Emissions.
Prepared for U.S. Department of Energy and U.S. Environmental Protection
Agency. Washington DC. December 1984. 25 p.
2. American Society of Mechanical Engineers. Analytical Procedures
to Assay Stack Effluent Samples and Residual Combustion Products for
Polychlorinated Dibenzo-p-Dioxins (PCDD) and Polychlorinated
Dibenzofurans (PCDF). Prepared for the U.S. Department of Energy and
U.S. Environmental Protection Agency. Washington, DC. December 1984.
23 p.
3. Thompson, J. R. (ed.). Analysis of Pesticide Residues in Human
and Environmental Samples. U.S. Environmental Protection Agency.
Research Triangle Park, NC. 1974.
4. Triangle Laboratories. Case Study: Analysis of Samples for the
Presence of Tetra Through Octachloro-p-Dibenzodioxins and Dibenzofurans.
Research Triangle Park, NC. 1988. 26 p.
5. U.S. Environmental Protection Agency. Method 8290 -- The Analysis
of Polychlorinated Dibenzo-p-dioxin and Polychlorinated Dibenzofurans by
High-Resolution Gas Chromotography/High-Resolution Mass Spectrometry.
In: Test Methods for Evaluating Solid Waste. Washington, DC. SW-846.
1. Applicability and Principle
40 CFR 60.748 Pt. 60, App. A, Meth. 24
1.1 Applicability. This method applies to the determination of
volatile matter content, water content, density, volume solids, and
weight solids of paint, varnish, lacquer, or related surface coatings.
1.2 Principle. Standard methods are used to determine the volatile
matter content, water content, density, volume solids, and weight solids
of the paint, varnish, lacquer, or related surface coatings.
2. Applicable Standard Methods
Use the apparatus, reagents, and procedures specified in the standard
methods below:
2.1 ASTM D1475-60 (Reapproved 1980), Standard Test Method for Density
of Paint, Varnish, Lacquer, and Related Products (incorporated by
reference -- see 60.17).
2.2 ASTM D2369-81, Standard Test Method for Volatile Content of
Coatings (incorporated by reference -- see 60.17).
2.3 ASTM D3792-79, Standard Test Method for Water Content of
Water-Reducible Paints by Direct Injection into a Gas Chromatograph
(incorporated by reference -- see 60.17).
2.4 ASTM D4017-81, Standard Test Method for Water in Paints and Paint
Materials by the Karl Fischer Titration Method (incorporated by
reference -- see 60.17).
3. Procedure
3.1 Volatile Matter Content. Use the procedure in ASTM D2369-81
(incorporated by reference -- see 60.17) to determine the volatile
matter content (may include water) of the coating. Record the following
information:
W1=Weight of dish and sample before heating, g.
W2=Weight of dish and sample after heating, g.
W3=Sample weight, g.
Run analyses in pairs (duplicate sets) for each coating until the
criterion in Section 4.3 is met. Calculate the weight fraction of the
volatile matter (Wv) for each analysis as follows:
Record the arithmetic average (W8v).
3.2 Water Content. For waterborne (water reducible) coatings only,
determine the weight fraction of water (WW) using either ''Standard
Content Method Test for Water of Water-Reducible Paints by Direct
Injection into a Gas Chromatograph'' or ''Standard Test Method for Water
in Paint and Paint Materials by Karl Fischer Method.'' (These two
methods are incorporated by reference -- see 60.17.) A waterborne
coating is any coating which contains more than 5 percent water by
weight in its volatile fraction. Run duplicate sets of determinations
until the criterion in Section 4.3 is met. Record the arithmetic
average (W8w).
3.3 Coating Density. Determine the density (Dc, kg/liter) of the
surface coating using the procedure in ASTM D1475-60 (Reapproved 1980)
(incorporated by reference -- see 60.17).
Run duplicate sets of determinations for each coating until the
criterion in Section 4.3 is met. Record the arithmetic average (D8c).
3.4 Solids Content. Determine the volume fraction (Vs) solids of the
coating by calculation using the manufacturer's formulation.
4. Data Validation Procedure
4.1 Summary. The variety of coatings that may be subject to analysis
makes it necessary to verify the ability of the analyst and the
analytical procedures to obtain reproducible results for the coatings
tested. This is done by running duplicate analyses on each sample
tested and comparing results with the within-laboratory precision
statements for each parameter. Because of the inherent increased
imprecision in the determination of the VOC content of waterborne
coatings as the weight percent water increases, measured parameters for
waterborne coatings are modified by the appropriate confidence limits
based on between-laboratory precision statements.
4.2 Analytical Precision Statements. The within-laboratory and
between-laboratory precision statements are given below:
4.3 Sample Analysis Criteria. For Wv and Ww, run duplicate analyses
until the difference between the two values in a set is less than or
equal to the within-laboratory precision statement for that parameter.
For Dc run duplicate analyses until each value in a set deviates from
the mean of the set by no more than the within-laboratory precision
statement. If after several attempts it is concluded that the ASTM
procedures cannot be used for the specific coating with the established
within-laboratory precision, the Administrator will assume
responsibility for providing the necessary procedures for revising the
method or precision statements upon written request to: Director,
Emission Standards and Engineering Division, (MD-13) Office of Air
Quality Planning and Standards, U.S. Environmental Protection Agency,
Research Triangle Park, NC 27711.
4.4 Confidence Limit Calculations for Waterborne Coatings. Based on
the between-laboratory precision statements, calculate the confidence
limits for waterborne coatings as follows:
To calculate the lower confidence limit, subtract the appropriate
between-laboratory precision value from the measured mean value for that
parameter. To calculate the upper confidence limit, add the appropriate
between-laboratory precision value to the measured mean value for that
parameter. For Wv and Dc, use the lower confidence limits, and for Ww,
use the upper confidence limit. Because Vs is calculated, there is no
adjustment for the parameter.
5. Calculations
5.1 Nonaqueous Volatile Matter.
5.1.1 Solvent-borne Coatings.
Wo=Wv Eq. 24-2
Where:
Wo=Weight fraction nonaqueous volatile matter, g/g.
5.1.2 Waterborne Coatings.
Wo=Wv^Ww Eq. 24-3
5.2 Weight Fraction Solids.
Ws=1^Wv Eq. 24-4
Where:
Ws=Weight solids, g/g.
40 CFR 60.748 Pt. 60, App. A, Meth. 24A
1. Applicability and Principle
1.1 Applicability. This method applies to the determination of the
volatile organic compound (VOC) content and density of solvent-borne
(solvent reducible) printing inks or related coatings.
1.2 Principle. Separate procedures are used to determine the VOC
weight fraction and density of the coating and the density of the
solvent in the coating. The VOC weight fraction is determined by
measuring the weight loss of a known sample quantity which has been
heated for a specified length of time at a specified temperature. The
density of both the coating and solvent are measured by a standard
procedure. From this information, the VOC volume fraction is
calculated.
2. Procedure
2.1 Weight Fraction VOC.
2.1.1 Apparatus.
2.1.1.1 Weighing Dishes. Aluminum foil, 58 mm in diameter by 18 mm
high, with a flat bottom. There must be at least three weighing dishes
per sample.
2.1.1.2 Disposable Syringe. 5 ml.
2.1.1.3 Analytical Balance. To measure to within 0.1 mg.
2.1.1.4 Oven. Vacuum oven capable of maintaining a temperature of 120
2 C and an absolute pressure of 510 51 mm Hg for 4 hours.
Alternatively, a forced draft oven capable of maintaining a temperature
of 120 2 C for 24 hours.
2.1.2 Analysis. Shake or mix the sample thoroughly to assure that all
the solids are completely suspended. Label and weigh to the nearest 0.1
mg a weighing dish and record this weight (Mxl).
Using a 5-ml syringe without a needle remove a sample of the coating.
Weigh the syringe and sample to the nearest 0.1 mg and record this
weight (McYl). Transfer 1 to 3 g of the sample to the tared weighing
dish. Reweigh the syringe and sample to the nearest 0.1 mg and record
this weight (McY2). Heat the weighing dish and sample in a vacuum oven
at an absolute pressure of 510 51 mm Hg and a temperature of 120 2 C
for 4 hours. Alternatively, heat the weighing dish and sample in a
forced draft oven at a temperature of 120 2 C for 24 hours. After the
weighing dish has cooled, reweigh it to the nearest 0.1 mg and record
the weight (Mx2). Repeat this procedure for a total of three
determinations for each sample.
2.2 Coating Density. Determine the density of the ink or related
coating according to the procedure outlined in ASTM D 1475-60
(Reapproved 1980), (incorporated by reference -- see 60.17).
2.3 Solvent Density. Determine the density of the solvent according
to the procedure outlined in ASTM D 1475-60 (reapproved 1980). Make a
total of three determinations for each coating. Report the density Do
as the arithmetic average of the three determinations.
3. Calculations
3.1 Weight Fraction VOC. Calculate the weight fraction volatile
organic content Wo using the following equation:
Eq. 24A-1
Report the weight fraction VOC Wo as the arithmetic average of the
three determinations.
3.2 Volume Fraction VOC. Calculate the volume fraction volatile
organic content Vo using the following equation:
Eq. 24A-2
4. Bibliography
1. Standard Test Method for Density of Paint, Varnish, Lacquer, and
Related Products. ASTM Designation D 1475-60 (Reapproved 1980).
2. Teleconversation. Wright, Chuck, Inmont Corporation with Reich, R.
A., Radian Corporation. September 25, 1979. Gravure Ink Analysis.
3. Teleconversation. Oppenheimer, Robert, Gravure Research Institute
with Burt, Rick, Radian Corporation, November 5, 1979. Gravure Ink
Analysis.
40 CFR 60.748 Pt. 60, App. A, Meth. 25
1.1 Applicability. This method applies to the measurement of volatile
organic compounds (VOC) as total gaseous nonmethane organics (TGNMO) as
carbon in source emissions. Organic particulate matter will interfere
with the analysis and, therefore, a particulate filter is required. The
minimum detectable for the method is 50 ppm as carbon.
When carbon dioxide (CO2) and water vapor are present together in the
stack, they can produce a positive bias in the sample. The magnitude of
the bias depends on the concentrations of CO2 and water vapor. As a
guideline, multiply the CO2 concentration, expressed as volume percent,
times the water vapor concentration. If this product does not exceed
100, the bias can be considered insignificant. For example, the bias is
not significant for a source having 10 percent CO2 and 10 percent water
vapor, but it would be significant for a source near the detection limit
having 10 percent CO2 and 20 percent water vapor.
This method is not the only method that applies to the measurement of
TGNMO. Costs, logistics, and other practicalities of source testing may
make other test methods more desirable for measuring VOC contents of
certain effluent streams. Proper judgment is required in determining
the most applicable VOC test method. For example, depending upon the
molecular weight of the organics in the effluent stream, a totally
automated semicontinuous nonmethane organics (NMO) analyzer interfaced
directly to the source may yield accurate results. This approach has
the advantage of providing emission data semicontinuously over an
extended time period.
Direct measurement of an effluent with a flame ionization detector
(FID) analyzer may be appropriate with prior characterization of the gas
stream and knowledge that the detector responds predictably to the
organic compounds in the stream. If present, methane (CH4) will, of
course, also be measured. The FID can be applied to the determination
of the mass concentration of the total molecular structure of the
organic emissions under any of the following limited conditions: (1)
Where only one compound is known to exist; (2) when the organic
compounds consist of only hydrogen and carbon; (3) where the relative
percentages of the compounds are known or can be determined, and the FID
responses to the compounds are known; (4) where a consistent mixture of
the compounds exists before and after emission control and only the
relative concentrations are to be assessed; or (5) where the FID can be
calibrated against mass standards of the compounds emitted (solvent
emissions, for example).
Another example of the use of a direct FID is as a screening method.
If there is enough information available to provide a rough estimate of
the analyzer accuracy, the FID analyzer can be used to determine the VOC
content of an uncharacterized gas stream. With a sufficient buffer to
account for possible inaccuracies, the direct FID can be a useful tool
to obtain the desired results without costly exact determination.
In situations where a qualitative/quantitative analysis of an
effluent stream is desired or required, a gas chromatographic FID system
may apply. However, for sources emitting numerous organics, the time
and expense of this approach will be formidable.
1.2 Principle. An emission sample is withdrawn from the stack at a
constant rate through a heated filter and a chilled condensate trap by
means of an evacuated sample tank. After sampling is completed, the
TGNMO are determined by independently analyzing the condensate trap and
sample tank fractions and combining the analytical results. The organic
content of the condensate trap fraction is determined by oxidizing the
NMO to CO2 and quantitatively collecting the effluent in an evacuated
vessel; then a portion of the CO2 is reduced to CH4 and measured by an
FID. The organic content of the sample tank fraction is measured by
injecting a portion of the sample into a gas chromatographic column to
separate the NMO from carbon monoxide (CO), CO2, and CH4; the NMO are
oxidized to CO2, reduced to CH4, and measured by an FID. In this
manner, the variable response of the FID associated with different types
of organics is eliminated.
2.1 Sampling. The sampling system consists of a heated probe, heated
filter, condensate trap, flow control system, and sample tank (Figure
25-1). The TGNMO sampling equipment can be constructed from
commercially available components and components fabricated in a machine
shop. The following equipment is required:
2.1.1 Heated Probe. 6.4-mm ( 1/4-in.) OD stainless steel tubing with
a heating system capable of maintaining a gas temperature at the exit
end of at least 129 C (265 F). The probe shall be equipped with a
thermocouple at the exit end to monitor the gas temperature.
A suitable probe is shown in Figure 25-1. The nozzle is an elbow
fitting attached to the front end of the probe while the thermocouple is
inserted in the side arm of a tee fitting attached to the rear of the
probe. The probe is wrapped with a suitable length of high temperature
heating tape, and then covered with two layers of glass cloth insulation
and one layer of aluminum foil.
Note. -- If it is not possible to use a heating system for safety
reasons, an unheated system with an in-stack filter is a suitable
alternative.
2.1.2 Filter Holder. 25-mm ( 15/16-in.) ID Gelman filter holder with
stainless steel body and stainless steel support screen with the Viton
O-ring replaced by a Teflon O-ring.
Note. -- Mention of trade names or specific products does not
constitute endorsement by the Environmental Protection Agency.
2.1.3 Filter Heating System. A metal box consisting of an inner and
an outer shell separated by insulating material with a heating element
in the inner shell capable of maintaining a gas temperature at the
filter of 121 3 C (250 5 F).
A suitable heating box is shown in Figure 25-2. The outer shell is a
metal box that measures 102 mm 280 mm 292 mm (4 in. 11 in. 11 1/2 in.),
while the inner shell is a metal box measuring 76 mm 229 mm 241 mm (3
in. 9 in. 9 1/2 in.). The inner box is supported by 13-mm ( 1/2-in.)
phenolic rods. The void space between the boxes is filled with
fiberfrax insulation which is sealed in place by means of a silicon
rubber bead around the upper sides of the box. A removable lid made in
a similar manner, with a 25-mm (1-in.) gap between the parts, is used to
cover the heating chamber.
The inner box is heated witn a 250-watt cartridge heater, shielded by
a stainless steel shroud. The heater is regulated by a thermostatic
temperature controller which is set to maintain a temperature of 121 C
as measured by a thermocouple in the gas line just before the filter.
An additional thermocouple is used to monitor the temperature of the gas
behind the filter.
2.1.4 Condensate Trap. 9.5-mm ( 3/8-in.) OD 316 stainless steel
tubing bent into a U-shape. Exact dimensions are shown in Figure 25-3.
The tubing shall be packed with coarse quartz wool, to a density of
approximately 0.11 g/cc before bending. While the condensate trap is
packed with dry ice in the Dewar, an ice bridge may form between the
arms of the condensate trap making it difficult to remove the condensate
trap. This problem can be prevented by attaching a steel plate between
the arms of the condensate trap in the same plane as the arms to
completely fill the intervening space.
2.1.5 Valve. Stainless steel shut-off valve for starting and stopping
sample flow.
2.1.6 Metering Valve. Stainless steel control valve for regulating
the sample flow rate through the sample train.
2.1.7 Rotameter. Glass tube with stainless steel fittings, capable of
measuring sample flow in the range of 60 to 100 cc/min.
2.1.8 Sample Tank. Stainless steel or aluminum tank with a minimum
volume of 4 liters.
2.1.9 Mercury Manometer or Absolute Pressure Gauge. Capable of
measuring pressure to within 1 mm Hg in the range of 0 to 900 mm.
2.1.10 Vacuum Pump. Capable of evacuating to an absolute pressure of
10 mm Hg.
2.2. Condensate Recovery Apparatus. The system for the recovery of
the organics captured in the condensate trap consists of a heat source,
oxidation catalyst, nondispersive infrared (NDIR) analyzer and an
intermediate collection vessel (ICV). Figure 25-4 is a schematic of a
typical system. The system shall be capable of proper oxidation and
recovery, as specified in Section 5.1. The following major components
are required:
2.2.1. Heat Source. Sufficient to heat the condensate trap
(including connecting tubing) to a temperature of 200 C. A system
using both a heat gun and an electric tube furnace is recommended.
2.2.2. Heat Tape. Sufficient to heat the connecting tubing between
the water trap and the oxidation catalyst to 100 C.
2.2.3. Oxidation Catalyst. A suitable length of 9.5-mm ( 3/8-in.) OD
Inconel 600 tubing packed with 15 cm (6 in.) of 3.2-mm ( 1/8-1n.)
diameter 19 percent chromia on alumina pellets. The catalyst material
is packed in the center of the catalyst tube with quartz wool packed on
either end to hold it in place. The catalyst tube shall be mounted
vertically in a 650 C tube furnace.
2.2.4 Water Trap. Leak proof, capable of removing moisture from the
gas stream.
2.2.5 Syringe Port. A 6.4-mm ( 1/4-in.) OD stainless steel tee
fitting with a rubber septum placed in the side arm.
2.2.6 NDIR Detector. Capable of indicating CO2 concentration in the
range of zero to 5 percent, to monitor the progress of combustion of the
organic compounds from the condensate trap.
2.2.7 Flow-Control Valve. Stainless steel, to maintain the trap
conditioning system near atmospheric pressure.
2.2.8 Intermediate Collection Vessel. Stainless steel or aluminum,
equipped with a female quick connect. Tanks with nominal volumes of at
least 6 liters are recommended.
2.2.9 Mercury Manometer or Absolute Pressure Gauge. Capable of
measuring pressure to within 1 mm Hg in the range of 0 to 900 mm.
2.2.10 Syringe. 10-ml gas-tight, glass syringe equipped with an
appropriate needle.
2.3 NMO Analyzer. The NMO analyzer is a gas chromatograph (GC) with
backflush capability for NMO analysis and is equipped with an oxidation
catalyst, reduction catalyst, and FID. Figures 25-5 and 25-6 are
schematics of a typical NMO analyzer. This semicontinuous GC/FID
analyzer shall be capable of: (1) Separating CO, CO2, and CH4 from NMO,
(2) reducing the CO2 to CH4 and quantifying as CH4, and (3) oxidizing
the NMO to CO2, reducing the CO2 to CH4 and quantifying as CH4,
according to Section 5.2. The analyzer consists of the following major
components:
2.3.1 Oxidation Catalyst. A suitable length of 9.5-mm ( 3/8-in.) OD
Inconel 600 tubing packed with 5.1 cm (2 in.) of 19 percent chromia on
3.2-mm ( 1/8-in.) alumina pellets. The catalyst material is packed in
the center of the tube supported on either side by quartz wool. The
catalyst tube must be mounted vertically in a 650 C furnace.
2.3.2 Reduction Catalyst. A 7.6-cm (3-in.) length of 6.4-mm (
1/4-in.) OD Inconel tubing fully packed with 100-mesh pure nickel
powder. The catalyst tube must be mounted vertically in a 400 C
furnace.
2.3.3 Separation Column(s). A 30-cm (1-ft) length of 3.2-mm (
1/8-in.) OD stainless steel tubing packed with 60/80 mesh Unibeads 1S
followed by a 61-cm (2-ft) length of 3.2-mm ( 1/8-in.) OD stainless
steel tubing packed with 60/80 mesh Carbosieve G. The Carbosieve and
Unibeads columns must be baked separately at 200 C with carrier gas
flowing through them for 24 hours before initial use.
2.3.4 Sample Injection System. A 10-port GC sample injection valve
fitted with a sample loop properly sized to interface with the NMO
analyzer (1-cc loop recommended).
2.3.5 FID. An FID meeting the following specifications is required:
2.3.5.1 Linearity. A linear response ( 5 percent) over the operating
range as demonstrated by the procedures established in Section 5.2.3.
2.3.5.2 Range. A full scale range of 10 to 50,000 ppm CH4. Signal
attenuators shall be available to produce a minimum signal response of
10 percent of full scale.
2.3.6 Data Recording System. Analog strip chart recorder or digital
integration system compatible with the FID for permanently recording the
analytical results.
2.4 Other Analysis Apparatus.
2.4.1 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 1 mm Hg.
2.4.2 Thermometer. Capable of measuring the laboratory temperature to
within 1 C.
2.4.3 Vacuum Pump. Capable of evacuating to an absolute pressure of
10 mm Hg.
2.4.4 Syringes. 10- l and 50- l liquid injection syringes.
2.4.5 Liquid Sample Injection Unit. 316 SS U-tube fitted with an
injection septum, see Figure 25-7.
3.1 Sampling. The following are required for sampling:
3.1.1 Crushed Dry Ice.
3.1.2 Coarse Quartz Wool. 8 to 15 m.
3.1.3 Filters. Glass fiber filters, without organic binder.
3.2 NMO Analysis. The following gases are needed:
3.2.1 Carrier Gases. Zero grade helium (He) and oxygen (O2
containing less than 1 ppm CO2 and less than 0.1 ppm C as hydrocarbon.
3.2.2 Fuel Gas. Zero grade hydrogen (H2), 99.999 percent pure.
3.2.3 Combustion Gas. Zero grade air or O2 as required by the
detector.
3.3 Condensate Analysis. The following gases are needed:
3.3.1 Carrier Gas. Zero grade air, containing less than 1 ppm C.
3.3.2 Auxiliary O2. Zero grade O2, containing less than 1 ppm C.
3.3.3 Hexane. ACS grade, for liquid injection.
3.3.4 Decane. ACS grade, for liquid injection.
3.4 Calibration. For all calibration gases, the manufacturer must
recommend a maximum shelf life for each cylinder (i.e., the length of
time the gas concentration is not expected to change more than 5
percent from its certified value). The date of gas cylinder
preparation, certified organic concentration, and recommended maximum
shelf life must be affixed to each cylinder before shipment from the gas
manufacturer to the buyer. The following calibration gases are
required:
3.4.1 Oxidation Catalyst Efficiency Check Calibration Gas. Gas
mixture standard with nominal concentration of 1 percent methane in air.
3.4.2 FID Linearity and NMO Calibration Gases. Three gas mixture
standards with nominal propane concentrations of 20 ppm, 200 ppm, and
3000 ppm, in air.
3.4.3 CO2 Calibration Gases. Three gas mixture standards with
nominal CO2 concentrations of 50 ppm, 500 ppm, and 1 percent, in air.
Note. -- Total NMO of less than 1 ppm required for 1 percent mixture.
3.4.4 NMO Analyzer System Check Calibration Gases. Four calibration
gases are needed as follows:
3.4.4.1 Propane Mixture. Gas mixture standard containing (nominal)
50 ppm CO, 50 ppm CH4, 2 percent CO2, and 20 ppm C3H8, prepared in air.
3.4.4.2 Hexane. Gas mixture standard containing (nominal) 50 ppm
hexane in air.
3.4.4.3 Toluene. Gas mixture standard containing (nominal) 20 ppm
toluene in air.
3.4.4.4 Methanol. Gas mixture standard containing (nominal) 100 ppm
methanol in air.
4.1 Sampling.
4.1.1 Cleaning Sampling Equipment. Before its initial use and after
each subsequent use, a condensate trap should be thoroughly cleaned and
checked to ensure that it is not contaminated. Both cleaning and
checking can be accomplished by installing the trap in the condensate
recovery system and treating it as if it were a sample. The trap should
be heated as described in the final paragraph of Section 4.3.3. A trap
may be considered clean when the CO2 concentration in its effluent gas
drops below 10 ppm. This check is optional for traps that have been
used to collect samples which were then recovered according to the
procedure in Section 4.3.3.
4.1.2 Sample Tank Evacuation and Leak Check. Evacuate the sample
tank to 10 mm Hg absolute pressure or less. Then close the sample tank
valve, and allow the tank to sit for 60 minutes. The tank is acceptable
if no change in tank vacuum is noted. The evacuation and leak check may
be conducted either in the laboratory or the field. The results of the
leak check should be included in the test report.
4.1.3 Sample Train Assembly. Just before assembly, measure the tank
vacuum using a mercury U-tube manometer or absolute pressure gauge.
Record this vacuum, the ambient temperature, and the barometric pressure
at this time. Close the sample tank valve and assemble the sampling
system as shown in Figure 25-1. Immerse the condensate trap body in dry
ice. The point where the inlet tube joins the trap body should be 2.5
to 5 cm above the top of the dry ice.
4.1.4 Pretest Leak Check. A pretest leak check is required.
Calculate or measure the approximate volume of the sampling train from
the probe trip to the sample tank valve. After assembling the sampling
train, plug the probe tip, and make certain that the sample tank valve
is closed. Turn on the vacuum pump, and evacuate the sampling system
from the probe tip to the sample tank valve to an absolute pressure of
10 ppm Hg or less. Close the purge valve, turn off the pump, wait a
minimum period of 5 minutes, and recheck the indicated vacuum.
Calculate the maximum allowable pressure change based on a leak rate of
1 percent of the sampling rate using Equation 25-1, Section 6.2. If the
measured pressure change exceeds the calculated limit, correct the
problem before beginning sampling. The results of the leak check should
be included in the test report.
4.1.5 Sample Train Operation. Unplug the probe tip, and place the
probe into the stack such that the probe is perpendicular to the duct or
stack axis; locate the probe tip at a single preselected point of
average velocity facing away from the direction of gas flow. For stacks
having a negative static pressure, seal the sample port sufficiently to
prevent air in-leakage around the probe. Set the probe temperature
controller to 129 C (265 F) and the filter temperature controller to
121 C (250 F). Allow the probe and filter to heat for about 30
minutes before purging the sample train.
Close the sample valve, open the purge valve, and start the vacuum
pump. Set the flow rate between 60 and 100 cc/min, and purge the train
with stack gas for at least 10 minutes. When the temperatures at the
exit ends of the probe and filter are within their specified range,
sampling may begin.
Check the dry ice level around the condensate trap, and add dry ice
if necessary. Record the clock time. To begin sampling, close the
purge valve and stop the pump. Open the sample valve and the sample
tank valve. Using the flow control valve, set the flow through the
sample train to the proper rate. Adjust the flow rate as necessary to
maintain a constant rate ( 10 percent) throughout the duration of the
sampling period. Record the sample tank vacuum and flowmeter setting at
5-minute intervals. (See Figure 25-8.) Select a total sample time
greater than or equal to the minimum sampling time specified in the
applicable subpart of the regulation; end the sampling when this time
period is reached or when a constant flow rate can no longer be
maintained because of reduced sample tank vacuum.
Note: If sampling had to be stopped before obtaining the minimum
sampling time (specified in the applicable subpart) because a constant
flow rate could not be maintained, proceed as follows: After closing
the sample tank valve, remove the used sample tank from the sampling
train (without disconnecting other portions of the sampling train).
Take another evacuated and leak-checked sample tank, measure and record
the tank vacuum, and attach the new tank to the sampling train. After
the new tank is attached to the sample train, proceed with the sampling
until the required minimum sampling time has been exceeded.
4.2 Sample Recovery. After sampling is completed, close the flow
control valve, and record the final tank vacuum; then record the tank
temperature and barometric pressure. Close the sample tank valve, and
disconnect the sample tank from the sample system. Disconnect the
condensate trap at the flowmetering system, and tightly seal both ends
of the condensate trap. Do not include the probe from the stack to the
filter as part of the condensate sample. Keep the trap packed in dry
ice until the samples are returned to the laboratory for analysis.
Ensure that the test run number is properly identified on the condensate
trap and the sample tank(s).
4.3 Condensate Recovery. See Figure 25-9. Set the carrier gas flow
rate, and heat the catalyst to its operating temperature to condition
the apparatus.
4.3.1 Daily Performance Checks. Each day before analyzing any
samples, perform the following tests:
4.3.1.1 Leak Check. With the carrier gas inlets and the flow control
valve closed, install a clean condensate trap in the system, and
evacuate the system to 10 mm Hg absolute pressure or less. Close the
vacuum pump valve and turn off the vacuum pump. Monitor the system
pressure for 10 minutes. The system is acceptable if the pressure
change is less than 2 mm Hg.
4.3.1.2 System Background Test. Adjust the carrier gas and auxiliary
oxygen flow rate to their normal values of 100 cc/min and 150 cc/min,
respectively, with the sample recovery valve in vent position. Using a
10-ml syringe withdraw a sample from the system effluent through the
syringe port. Inject this sample into the NMO analyzer, and measure the
CO2 content. The system background is acceptable if the CO2
concentration is less than 10 ppm.
4.3.1.3 Oxidation Catalyst Efficiency Check. Conduct a catalyst
efficiency test as specified in Section 5.1.2 of this method. If the
criterion of this test cannot be met, make the necessary repairs to the
system before proceeding.
4.3.2 Condensate Trap CO2 Purge and Sample Tank Pressurization.
After sampling is completed, the condensate trap will contain condensed
water and organics and a small volume of sampled gas. This gas from the
stack may contain a significant amount of CO2 which must be removed from
the condensate trap before the sample is recovered. This is
accomplished by purging the condensate trap with zero air and collecting
the purged gas in the original sample tank.
Begin with the sample tank and condensate trap from the test run to
be analyzed. Set the four-port valve of the condensate recovery system
in the CO2 purge position as shown in Figure 25-9. With the sample tank
valve closed, attach the sample tank to the sample recovery system.
With the sample recovery valve in the vent position and the flow control
valve fully open, evacuate the manometer or pressure gauge to the vacuum
of the sample tank. Next, close the vacuum pump valve, open the sample
tank valve, and record the tank pressure.
Attach the dry-ice-cooled condensate trap to the recovery system, and
initiate the purge by switching the sample recovery valve from vent to
collect position. Adjust the flow control valve to maintain atmospheric
pressure in the recovery system. Continue the purge until the CO2
concentration of the trap effluent is less than 5 ppm. CO2
concentration in the trap effluent should be measured by extracting
syringe samples from the recovery system and analyzing the samples with
the NMO analyzer. This procedure should be used only after the NDIR
response has reached a minimum level. Using a 10-ml syringe, extract a
sample from the syringe port prior to the NDIR, and inject this sample
into the NMO analyzer.
After the completion of the CO2 purge, use the carrier gas bypass
valve to pressurize the sample tank to approximately 1060 mm Hg absolute
pressure with zero air.
4.3.3 Recovery of the Condensate Trap Sample. See Figure 25-10.
Attach the ICV to the sample recovery system. With the sample recovery
valve in a closed position, between vent and collect, and the flow
control and ICV valves fully open, evacuate the manometer or gauge, the
connecting tubing, and the ICV to 10 mm Hg absolute pressure. Close the
flow-control and vacuum pump valves.
Begin auxiliary oxygen flow to the oxidation catalyst at a rate of
150 cc/min, then switch the four-way valve to the trap recovery position
and the sample recovery valve to collect position. The system should
now be set up to operate as indicated in Figure 25-10. After the
manometer or pressure gauge begins to register a slight positive
pressure, open the flow control valve. Adjust the flow-control valve to
maintain atmospheric pressure in the system within 10 percent.
Now, remove the condensate trap from the dry ice, and allow it to
warm to ambient temperature while monitoring the NDIR response. If
after 5 minutes, the CO2 concentration of the catalyst effluent is below
10,000 ppm, discontinue the auxiliary oxygen flow to the oxidation
catalyst. Begin heating the trap by placing it in a furnace preheated
to 200 C. Once heating has begun, carefully monitor the NDIR response
to ensure that the catalyst effluent concentration does not exceed
50,000 ppm. Whenever the CO2 concentration exceeds 50,000 ppm, supply
auxiliary oxygen to the catalyst at the rate of 150 cc/min. Begin
heating the tubing that connected the heated sample box to the
condensate trap only after the CO2 concentration falls below 10,000 ppm.
This tubing may be heated in the same oven as the condensate trap or
with an auxiliary heat source such as a heat gun. Heating temperature
must not exceed 200 C. If a heat gun is used, heat the tubing slowly
along its entire length from the upstream end to the downstream end, and
repeat the pattern for a total of three times. Continue the recovery
until the CO2 concentration drops to less than 10 ppm as determined by
syringe injection as described under the condensate trap CO2 purge
Procedure, Section 4.3.2.
After the sample recovery is completed, use the carrier gas bypass
valve to pressurize the ICV to approximately 1060 mm Hg absolute
pressure with zero air.
4.4 Analysis. Before putting the NMO analyzer into routine operation,
conduct an initial performance test. Start the analyzer, and perform
all the necessary functions in order to put the analyzer into proper
working order; then conduct the performance test according to the
procedures established in Section 5.2. Once the performance test has
been successfully completed and the CO2 and NMO calibration response
factors have been determined, proceed with sample analysis as follows:
4.4.1 Daily Operations and Calibration Checks. Before and
immediately after the analysis of each set of samples or on a daily
basis (whichever occurs first), conduct a calibration test according to
the procedures established in Section 5.3. If the criteria of the daily
calibration test cannot be met, repeat the NMO analyzer performance test
(Section 5.2) before proceeding.
4.4.2 Operating Conditions. The carrier gas flow rate is 29.5 cc/min
He and 2.2 cc/min O2. The column oven is heated to 85 C. The order of
elution for the sample from the column is CO, CH4, CO2, and NMO.
4.4.3 Analysis of Recovered Condensate Sample. Purge the sample loop
with sample, and then inject the sample. Under the specified operating
conditions, the CO2 in the sample will elute in approximately 100
seconds. As soon as the detector response returns to baseline following
the CO2 peak, switch the carrier gas flow to backflush, and raise the
column oven temperature to 195 C as rapidly as possible. A rate of 30
C/min has been shown to be adequate. Record the value obtained for the
condensible organic material (Ccm) measured as CO2 and any measured NMO.
Return the column oven temperature to 85 C in preparation for the next
analysis. Analyze each sample in triplicate, and report the average
Ccm.
4.4.4 Analysis of Sample Tank. Perform the analysis as described in
Section 4.4.3, but record only the value measured for NMO (Ctm).
4.5 Audit Samples. Analyze a set of two audit samples concurrently
with any compliance samples and in exactly the same manner to evaluate
the analyst's technique and the instrument calibration. The same
analysts, analytical reagents, and analytical system shall be used for
the compliance samples and the EPA audit samples; if this condition is
met, auditing of subsequent compliance analyses for the same enforcement
agency within 30 days is not required. An audit sample set may not be
used to validate different sets of compliance samples under the
jurisdiction of different enforcement agencies, unless prior
arrangements are made with both enforcement agencies.
Calculate the concentrations of the audit samples in ppm using the
specified sample volume in the audit instructions. (Note. -- Indication
of acceptable results may be obtained immediately by reporting the audit
results in ppm and compliance results in ppm by telephone to the
responsible enforcement agency.) Include the results of both audit
samples, their identification numbers, and the analyst's name with the
results of the compliance determination samples in appropriate reports
to the EPA regional office or the appropriate enforcement agency during
the 30-day period.
The concentration of the audit samples obtained by the analyst shall
agree within 20 percent of the actual concentrations. Failure to meet
the 20-percent specification may require retests until the audit
problems are resolved. However, if the audit results do not affect the
compliance or noncompliance status of the affected facility, the
Administrator may waive the reanalysis requirement, further audits, or
retests and accept the results of the compliance test. While steps are
being taken to resolve audit analysis problems, the Administrator may
also choose to use the data to determine the compliance or noncompliance
of the affected facility.
Maintain a record of performance of each item.
5.1 Initial Performance Check of Condensate Recovery Apparatus.
Perform these tests before the system is first placed in operation,
after any shutdown of 6 months or more, and after any major modification
of the system, or at the specified frequency.
5.1.1 Carrier Gas and Auxiliary O2 Blank Check. Analyze each new
tank of carrier gas or auxiliary O2 with the NMO analyzer to check for
contamination. Treat the gas cylinders as noncondensible gas samples,
and analyze according to the procedure in Section 4.4.3. Add together
any measured CH4, CO, CO2, or NMO. The total concentration must be less
than 5 ppm.
5.1.2 Catalyst Efficiency Check. With a clean condensate trap
installed in the recovery system, replace the carrier gas cylinder with
the high level methane standard gas cylinder (Section 3.4.1). Set the
four-port valve to the recovery position, and attach an ICV to the
recovery system. With the sample recovery valve in vent position and
the flow-control and ICV valves fully open, evacuate the manometer or
gauge, the connecting tubing, and the ICV to 10 mm Hg absolute pressure.
Close the flow-control and vacuum pump valves.
After the NDIR response has stabilized, switch the sample recovery
valve from vent to collect. When the manometer or pressure gauge begins
to register a slight positive pressure, open the flow-control valve.
Keep the flow adjusted so that atmospheric pressure is maintained in the
system within 10 percent. Continue collecting the sample in a normal
manner until the ICV is filled to a nominal gauge pressure of 300 mm Hg.
Close the ICV valve, and remove the ICV from the system. Place the
sample recovery valve in the vent position, and return the recovery
system to its normal carrier gas and normal operating conditions.
Analyze the ICV for CO2 using the NMO analyzer; the catalyst efficiency
is acceptable if the CO2 concentration is within 2 percent of the
methane standard concentration.
5.1.3 System Performance Check. Construct a liquid sample injection
unit similar in design to the unit shown in Figure 25-7. Insert this
unit into the condensate recovery and conditioning system in place of a
condensate trap, and set the carrier gas and auxiliary O2 flow rates to
normal operating levels. Attach an evacuated ICV to the system, and
switch from system vent to collect. With the carrier gas routed through
the injection unit and the oxidation catalyst, inject a liquid sample
(See Sections 5.1.3.1 to 5.1.3.4) into the injection port. Operate the
trap recovery system as described in Section 4.3.3. Measure the final
ICV pressure, and then analyze the vessel to determine the CO2
concentration. For each injection, calculate the percent recovery using
the equation in Section 6.6.
The performance test is acceptable if the average percent recovery is
100 10 percent with a relative standard deviation (Section 6.9) of less
than 5 percent for each set of triplicate injections as follows:
5.1.3.1 50 l Hexane.
5.1.3.2 10 l Hexane.
5.1.3.3 50 l Decane.
5.1.3.4 10 l Decane.
5.2 Initial NMO Analyzer Performance Test. Perform these tests
before the system is first placed in operation, after any shutdown
longer than 6 months, and after any major modification of the system.
5.2.1 Oxidation Catalyst Efficiency Check. Turn off or bypass the
NMO analyzer reduction catalyst. Make triplicate injections of the high
level methane standard (Section 3.4.1). The oxidation catalyst operation
is acceptable if the FID response is less than 1 percent of the injected
methane concentration.
5.2.2 Reduction Catalyst Efficiency Check. With the oxidation
catalyst unheated or bypassed and the heated reduction catalyst
bypassed, make triplicate injections of the high level methane standard
(Section 3.4.1). Repeat this procedure with both catalysts operative.
The reduction catalyst operation is acceptable if the response under
both conditions agree within 5 percent.
5.2.3 Analyzer Linearity Check and NMO Calibration. While operating
both the oxidation and reduction catalysts, conduct a linearity check of
the analyzer using the propane standards specified in Section 3.4.2.
Make triplicate injections of each calibration gas, and then calculate
the average response factor (area/ppm C) for each gas, as well as the
overall mean of the response factor values. The instrument linearity is
acceptable if the average response factor of each calibration gas is
within 2.5 percent of the overall mean value and if the relative
standard deviation (Section 6.9) for each set of triplicate injections
is less than 2 percent. Record the overall mean of the propane response
factor values as the NMO calibration response factor (RFNMO).
Repeat the linearity check using the CO2 standards specified in
Section 3.4.3. Make triplicate injections of each gas, and then
calculate the average response factor (area/ppm C) for each gas, as well
as the overall mean of the response factor values. Record the overall
mean of the response factor values as the CO2 calibration response
factor (RFCO2). Linearity is acceptable if the average response factor
of each calibration gas is within 2.5 percent of the overall mean value
and if the relative standard deviation for each set of triplicate
injections is less than 2 percent. The RFCO2 must be witnin 10 percent
of the RFNMO.
5.2.4 System Peformance Check. Check the column separation and
overall performance of the analyzer by making triplicate injections of
the calibration gases listed in Section 3.4.4. The analyzer performance
is acceptable if the measured NMO value for each gas (average of
triplicate injections) is within 5 percent of the expected value.
5.3 NMO Analyzer Daily Calibration.
5.3.1 CO2 Response Factor. Inject triplicate samples of the high
level CO2 calibration gas (Section 3.4.3), and calculate the average
response factor. The system operation is adequate if the calculated
response factor is within 5 percent of the RFCO2 calculated during the
initial performance test (Section 5.2.3). Use the daily response factor
(DRFCO2) for analyzer calibration and the calculation of measured CO2
concentrations in the ICV samples.
5.3.2 NMO Response Factors. Inject triplicate samples of the mixed
propane calibration cylinder (Section 3.4.4.1), and calculate the
average NMO response factor. The system operation is adequate if the
calculated response factor is within 5 percent of the RFNMO calculated
during the initial performance test (Section 5.2.4). Use the daily
response factor (DRFNMO) for analyzer calibration and calculation of NMO
concentrations in the sample tanks.
5.4 Sample Tank and ICV Volume. The volume of the gas sampling tanks
used must be determined. Determine the tank and ICV volumes by weighing
them empty and then filled with deionized distilled water; weigh to the
nearest 5 g, and record the results. Alternatively, measure the volume
of water used to fill them to the nearest 5 ml.
All equations are written using absolute pressure; absolute
pressures are determined by adding the measured barometric pressure to
the measured gauge or manometer pressure.
6.1 Nomenclature.
C=TGNMO concentration of the effluent, ppm C equivalent.
Cc=Calculated condensible organic (condensate trap) concentration of
the effluent, ppm C equivalent.
Ccm=Measured concentration (NMO analyzer) for the condensate trap
ICV, ppm CO2.
Ct=Calculated noncondensible organic concentration (sample tank) of
the effluent, ppm C equivalent.
Ctm=Measured concentration (NMO analyzer) for the sample tank, ppm
NMO.
F=Sampling flow rate, cc/min.
L=Volume of liquid injected, l.
M=Molecular weight of the liquid injected, g/g-mole.
mC=TGNMO mass concentration of the effluent, mg C/dsm /3/ .
N=Carbon number of the liquid compound injected (N=12 for decane, N=6
for hexane).
Pf=Final pressure of the intermediate collection vessel, mm Hg
absolute.
Pb=Barometric pressure, cm Hg.
Pti=Gas sample tank pressure before sampling, mm Hg absolute.
Pt=Gas sample tank pressure after sampling, but before pressurizing,
mm Hg absolute.
Ptf=Final gas sample tank pressure after pressurizing, mm Hg
absolute.
Tf=Final temperature of intermediate collection vessel, K.
Tti=Sample tank temperature before sampling, K.
Tt=Sample tank temperature at completion of sampling, K.
Ttf=Sample tank temperature after pressurizing, K.
V=Sample tank volume, m /3/ .
Vt=Sample train volume, cc.
Vv=Intermediate collection vessel volume, m /3/ .
Vs=Gas volume sampled, dsm /3/ .
n=Number of data points.
q=Total number of analyzer injections of intermediate collection
vessel during analysis (where k=injection number, 1 . . . q).
r=Total number of analyzer injections of sample tank during analysis
(where j=injection number, 1 . . . r).
xi=Individual measurements.
x8=Mean value.
r=Density of liquid injected, g/cc.
U=Leak check period, min.
DR=Allowable pressure change, cm Hg.
6.2 Allowable Pressure Change. For the pretest leak check, calculate
the allowable pressure change:
insert illus 0210A
6.3 Sample Volume. For each test run, calculate the gas volume
sampled:
insert illus 0210B
6.4 Noncondensible Organics. For each sample tank, determine the
concentration of nonmethane organics (ppm C):
insert illus 0210C
6.5 Condensible Organics. For each condensate trap determine the
concentration of organics (ppm C):
insert illus 0210D
6.6 TGNMO. To determine the TGNMO concentration for each test run,
use the following equation:
C=Ct+Cc
Eq. 25-5
6.7 TGNMO Mass Concentration. To determine the TGNMO mass
concentration as carbon for each test run, use the following equation:
mc=0.4993 C
Eq. 25-6
6.8 Percent Recovery. To calculate the percent recovery for the
liquid injections to the condensate recovery and conditioning system use
the following equation.
6.9 Relative Standard Deviation.
insert illus 0211A
1. Salo, Albert E., Samuel Witz, and Robert D. MacPhee.
Determination of Solvent Vapor Concentrations by Total Combustion
Analysis: A Comparison of Infrared with Flame Ionization Detectors.
Paper No. 75-33.2. (Presented at the 68th Annual Meeting of the Air
Pollution Control Association. Boston, Massachusetts. June 15-20, 1975.)
14 p.
2. Salo, Albert E., William L. Oaks, and Robert D. MacPhee.
Measuring the Organic Carbon Content of Source Emissions for Air
Pollution Control. Paper No. 74-190. (Presented at the 67th Annual
Meeting of the Air Pollution Control Association. Denver, Colorado.
June 9-13, 1974.) 25 p.
Insert illus. 0212A
Insert illus. 0213A
Insert illus. 0214A
Insert illus. 0215A
Insert illus. 0216A
Insert illus. 0217A
Insert illus. 0218A
Insert illus. 0219A
Insert illus. 0220A
Insert illus. 0221A
40 CFR 60.748 Pt. 60, App. A, Meth. 25A
1. Applicability and Principle
1.1 Applicability. This method applies to the measurement of total
gaseous organic concentration of vapors consisting primarily of alkanes,
alkenes, and/or arenes (aromatic hydrocarbons). The concentration is
expressed in terms of propane (or other appropriate organic calibration
gas) or in terms of carbon.
1.2 Principle. A gas sample is extracted from the source through a
heated sample line, if necessary, and glass fiber filter to a flame
ionization analyzer (FIA). Results are reported as volume concentration
equivalents of the calibration gas or as carbon equivalents.
2. Definitions
2.1 Measurement System. The total equipment required for the
determination of the gas concentration. The system consists of the
following major subsystems:
2.1.1 Sample Interface. That portion of the system that is used for
one or more of the following: sample acquisition, sample
transportation, sample conditioning, or protection of the analyzer from
the effects of the stack effluent.
2.1.2 Organic Analyzer. That portion of the system that senses
organic concentration and generates an output proportional to the gas
concentration.
2.2 Span Value. The upper limit of a gas concentration measurement
range that is specified for affected source categories in the applicable
part of the regulations. The span value is established in the
applicable regulation and is usually 1.5 to 2.5 times the applicable
emission limit. If no span value is provided, use a span value
equivalent to 1.5 to 2.5 times the expected concentration. For
convenience, the span value should correspond to 100 percent of the
recorder scale.
2.3 Calibration Gas. A known concentration of a gas in an
appropriate diluent gas.
2.4 Zero Drift. The difference in the measurement system response to
a zero level calibration gas before and after a stated period of
operation during which no unscheduled maintenance, repair, or adjustment
took place.
2.5 Calibration Drift. The difference in the measurement system
response to a mid-level calibration gas before and after a stated period
of operation during which no unscheduled maintenance, repair or
adjustment took place.
2.6 Response Time. The time interval from a step change in pollutant
concentration at the inlet to the emission measurement system to the
time at which 95 percent of the corresponding final value is reached as
displayed on the recorder.
2.7 Calibration Error. The difference between the gas concentration
indicated by the measurement system and the known concentration of the
calibration gas.
3. Apparatus
A schematic of an acceptable measurement system is shown in Figure
25A-1. The essential components of the measurement system are described
below:
Insert illus. 25A
3.1 Organic Concentration Analyzer. A flame ionization analyzer
(FIA) capable of meeting or exceeding the specifications in this method.
3.2 Sample Probe. Stainless steel, or equivalent, three-hole rake
type. Sample holes shall be 4 mm in diameter or smaller and located at
16.7, 50, and 83.3 percent of the equivalent stack diameter.
Alternatively, a single opening probe may be used so that a gas sample
is collected from the centrally located 10 percent area of the stack
cross-section.
3.3 Sample Line. Stainless steel or Teflon* tubing to transport the
sample gas to the analyzer. The sample line should be heated, if
necessary, to prevent condensation in the line.
3.4 Calibration Valve Assembly. A three-way valve assembly to direct
the zero and calibration gases to the analyzers is recommended. Other
methods, such as quick-connect lines, to route calibration gas to the
analyzers are applicable.
3.5 Particulate Filter. An in-stack or an out-of-stack glass fiber
filter is recommended if exhaust gas particulate loading is significant.
An out-of-stack filter should be heated to prevent any condensation.
3.6 Recorder. A strip-chart recorder, analog computer, or digital
recorder for recording measurement data. The minimum data recording
requirement is one measurement value per minute. Note: This method is
often applied in highly explosive areas. Caution and care should be
exercised in choice of equipment and installation.
4. Calibration and Other Gases
Gases used for calibrations, fuel, and combustion air (if required)
are contained in compressed gas cylinders. Preparation of calibration
gases shall be done according to the procedure in Protocol No. 1,
listed in Citation 2 of Bibliography. Additionally, the manufacturer of
the cylinder should provide a recommended shelf life for each
calibration gas cylinder over which the concentration does not change
more than 2 percent from the certified value. For calibration gas
values not generally available (i.e., organics between 1 and 10 percent
by volume), alternative methods for preparing calibration gas mixtures,
such as dilution systems, may be used with prior approval of the
Administrator.
Calibration gases usually consist of propane in air or nitrogen and
are determined in terms of the span value. Organic compounds other than
propane can be used following the above guidelines and making the
appropriate corrections for response factor.
4.1 Fuel. A 40 percent H2/60 percent He or 40 percent H2/60 percent
N2 gas mixture is recommended to avoid an oxygen synergism effect that
reportedly occurs when oxygen concentration varies significantly from a
mean value.
4.2 Zero Gas. High purity air with less than 0.1 parts per million
by volume (ppmv) of organic material (propane or carbon equivalent) or
less than 0.1 percent of the span value, whichever is greater.
4.3 Low-level Calibration Gas. An organic calibration gas with a
concentration equivalent to 25 to 35 percent of the applicable span
value.
4.4 Mid-level Calibration Gas. An organic calibration gas with a
concentration equivalent to 45 to 55 percent of the applicable span
value.
4.5 High-level Calibration Gas. An organic calibration gas with a
concentration equivalent to 80 to 90 percent of the applicable span
value.
5. Measurement System Performance Specifications
5.1 Zero Drift. Less than 3 percent of the span value.
5.2 Calibration Drift. Less than 3 percent of span value.
5.3 Calibration Error. Less than 5 percent of the calibration gas
value.
6. Pretest Preparations
6.1 Selection of Sampling Site. The location of the sampling site is
generally specified by the applicable regulation or purpose of the test;
i.e., exhaust stack, inlet line, etc. The sample port shall be located
at least 1.5 meters or 2 equivalent diameters upstream of the gas
discharge to the atmosphere.
6.2 Location of Sample Probe. Install the sample probe so that the
probe is centrally located in the stack, pipe, or duct and is sealed
tightly at the stack port connection.
6.3 Measurement System Preparation. Prior to the emission test,
assemble the measurement system following the manufacturer's written
instructions in preparing the sample interface and the organic analyzer.
Make the system operable.
FIA equipment can be calibrated for almost any range of total
organics concentrations. For high concentrations of organics (>1.0
percent by volume as propane) modifications to most commonly available
analyzers are necessary. One accepted method of equipment modification
is to decrease the size of the sample to the analyzer through the use of
a smaller diameter sample capillary. Direct and continuous measurement
of organic concentration is a necessary consideration when determining
any modification design.
6.4 Calibration Error Test. Immediately prior to the test series,
(within 2 hours of the start of the test) introduce zero gas and
high-level calibration gas at the calibration valve assembly. Adjust
the analyzer output to the appropriate levels, if necessary. Calculate
the predicted response for the low-level and mid-level gases based on a
linear response line between the zero and high-level responses. Then
introduce low-level and mid-level calibration gases successively to the
measurement system. Record the analyzer responses for low-level and
mid-level calibration gases and determine the differences between the
measurement system responses and the predicted responses. These
differences must be less than 5 percent of the respective calibration
gas value. If not, the measurement system is not acceptable and must be
replaced or repaired prior to testing. No adjustments to the
measurement system shall be conducted after the calibration and before
the drift check (Section 7.3). If adjustments are necessary before the
completion of the test series, perform the drift checks prior to the
required adjustments and repeat the calibration following the
adjustments. If multiple electronic ranges are to be used, each
additional range must be checked with a mid-level calibration gas to
verify the multiplication factor.
6.5 Response Time Test. Introduce zero gas into the measurement
system at the calibration valve assembly. When the system output has
stabilized, switch quickly to the high-level calibration gas. Record
the time from the concentration change to the measurement system
response equivalent to 95 percent of the step change. Repeat the test
three times and average the results.
7. Emission Measurement Test Procedure
7.1 Organic Measurement. Begin sampling at the start of the test
period, recording time and any required process information as
appropriate. In particular, note on the recording chart periods of
process interruption or cyclic operation.
7.2 Drift Determination. Immediately following the completion of the
test period and hourly during the test period, reintroduce the zero and
mid-level calibration gases, one at a time, to the measurement system at
the calibration valve assembly. (Make no adjustments to the measurement
system until after both the zero and calibration drift checks are made.)
Record the analyzer response. If the drift values exceed the specified
limits, invalidate the test results preceding the check and repeat the
test following corrections to the measurement system. Alternatively,
recalibrate the test measurement system as in Section 6.4 and report the
results using both sets of calibration data (i.e., data determined prior
to the test period and data determined following the test period).
8. Organic Concentration Calculations
Determine the average organic concentration in terms of ppmv as
propane or other calibration gas. The average shall be determined by
the integration of the output recording over the period specified in the
applicable regulation.
If results are required in terms of ppmv as carbon, adjust measured
concentrations using Equation 25A-1.
Cc=K Cmeas Eq. 25A-1
Where:
Cc=Organic concentration as carbon, ppmv.
Cmeas=Organic concentration as measured, ppmv.
K=Carbon equivalent correction factor,
K=2 for ethane.
K=3 for propane.
K=4 for butane.
K=Appropriate response factor for other organic calibration gases.
9. Bibliography
1. Measurement of Volatile Organic Compounds -- Guideline Series.
U.S. Environmental Protection Agency. Research Triangle Park, NC.
Publication No. EPA-450/2-78-041. June 1978. p. 46-54.
2. Traceability Protocol for Establishing True Concentrations of
Gases Used for Calibration and Audits of Continuous Source Emission
Monitors (Protocol No. 1). U.S. Environmental Protection Agency,
Environmental Monitoring and Support Laboratory. Research Triangle
Park, NC. June 1978.
3. Gasoline Vapor Emission Laboratory Evaluation -- Part 2. U.S.
Environmental Protection Agency, Office of Air Quality Planning and
Standards. Research Triangle Park, NC. EMB Report No. 75-GAS-6.
August 1975.
*Mention of trade names or specific products does not constitute
endorsement by the Environmental Protection Agency.
40 CFR 60.748 Pt. 60, App. A, Meth. 25B
1. Applicability and Principle
1.1 Applicability. This method applies to the measurement of total
gaseous organic concentration of vapors consisting primarily of alkanes.
(Other organic materials may be measured using the general procedure in
this method, the appropriate calibration gas, and an analyzer set to the
appropriate absorption band.) The concentration is expressed in terms of
propane (or other appropriate organic calibration gas) or in terms of
carbon.
1.2 Principle. A gas sample is extracted from the source through a
heated sample line, if necessary, and glass fiber filter to a
nondispersive infrared analyzer (NDIR). Results are reported as volume
concentration equivalents of the calibration gas or as carbon
equivalents.
2. Definitions
The terms and definitions are the same as for Method 25A.
3. Apparatus
The apparatus is the same as for Method 25A with the exception of the
following:
3.1 Organic Concentration Analyzer. A nondispersive infrared
analyzer designed to measure alkane organics and capable of meeting or
exceeding the specifications in this method.
4. Calibration Gases
The calibration gases are the same as required for Method 25A,
Section 4. No fuel gas is required for an NDIR.
5. Measurement System Performance Specifications
5.1 Zero Drift. Less than 3 percent of the span value.
5.2 Calibration Drift. Less than 3 percent of the span value.
5.3 Calibration Error. Less than 5 percent of the calibration gas
value.
6. Pretest Preparations
6.1 Selection of Sampling Site. Same as in Method 25A, Section 6.1.
6.2 Location of Sample Probe. Same as in Method 25A, Section 6.2.
6.3 Measurement System Preparation. Prior to the emission test,
assemble the measurement system following the manufacturer's written
instructions in preparing the sample interface and the organic analyzer.
Make the system operable.
6.4 Calibration Error Test. Same as in Method 25A, Section 6.4.
6.5 Response Time Test Procedure. Same as in Method 25A, Section
6.5.
7. Emission Measurement Test Procedure
Proceed with the emission measurement immediately upon satisfactory
completion of the calibration.
7.1 Organic Measurement. Same as in Method 25A, Section 7.1.
7.2 Drift Determination. Same as in Method 25A, Section 7.2.
8. Organic Concentration Calculations
The calculations are the same as in Method 25A, Section 8.
9. Bibliography
The bibliography is the same as in Method 25A.
40 CFR 60.748 Pt. 60, App. A, Meth. 26
1.1 Applicability. This method is applicable for determining hydrogen
chloride (HCl) emissions from stationary sources.
1.2 Principle. An integrated sample is extracted from the stack and
passed through dilute sulfuric acid. In the dilute acid, the HCl gas is
dissolved and forms chloride (Cl^) ions. The Cl^ is analyzed by ion
chromatography (IC).
1.3 Interferences. Volatile materials which produce chloride ions
upon dissolution during sampling are obvious interferences. Another
likely interferent is diatomic chlorine (Cl2) gas which reacts to form
HCl and hypochlorous acid (HOCl) upon dissolving in water. However, Cl2
gas exhibits a low solubility in water and the use of acidic, rather
than neutral or basic collection solutions, greatly reduces the chance
of dissolving any chlorine present.
1.4 Precision and Bias. The within-laboratory relative standard
deviations are 6.2 and 3.2 percent at HCl concentrations of 3.9 and 15.3
ppm, respectively. The method does not exhibit a bias to Cl2 when
sampling at concentrations less than 50 ppm.
1.5 Stability. The collected samples can be stored for up to 4 weeks
before analysis.
1.6 Detection Limit. The analytical detection limit of the method is
0.1 g/ml.
2.1 Sampling. The sampling train is shown in Figure 26-1, and
component parts are discussed below.
2.1.1 Probe. Borsilicate glass, approximately 3/8-in. (9-mm) I.D.
with a heating system to prevent moisture condensation. A Teflon-glass
filter in a mat configuration shall be installed behind the probe to
remove particulate matter from the gas stream (see section 2.1.5). A
glass wool plug should not be used to remove particulate matter since a
negative bias in the data could result.
2.1.2 Three-Way Stopcock. A borosilicate glass three-way stopcock
with a heating system to prevent moisturecondensation. The heated
stopcock should connect to the outlet of the heated filter and the inlet
of the first impinger. The heating system shall be capable of
preventing condensation up to the inlet of the first impinger. Silicone
grease may be used, if necessary, to prevent leakage.
Insert illustration 047
2.1.3 Impingers. Four 30-ml midget impingers with leak-free glass
connectors. Silicone grease may be used, if necessary, to prevent
leakage. For sampling at high moisture sources or for sampling times
greater than 1 hour, a midget impinger with a shortened stem (such that
the gas sample does not bubble through the collected condensate) should
be used in front of the first impinger.
2.1.4 Drying Tube or Impinger. Tube or impinger, of Mae West design,
filled with 6- to 16-mesh indicating type silica gel, or equivalent, to
dry the gas sample and to protect the dry gas meter and pump. If the
silica gel has been used previously, dry at 175 C (350 F) for 2 hours.
New silica gel may be used as received. Alternatively, other types of
desiccants (equivalent or better) may be used.
2.1.5 Filter. A 25-mm (or other size) Teflon-glass mat, Pallflex
TX40HI75 (Pallflex Inc., 125 Kennedy Drive, Putnam, CT 06260). This
filter is in a mat configuration to prevent fine particulate matter from
entering the sampling train. Its composition is 75 percent Teflon/25
percent borosilicate glass. Other filters may be used, but they must be
in a mat (as opposed to a laminate) configuration and contain at least
75 percent Teflon.
2.1.6 Filter Holder and Support. The filter holder should be made of
Teflon or quartz. The filter support shall be made of Teflon.
All-Teflon filter holders and supports are available from Savillex
Corp., 5325 Hwy 101, Minnetonka, MN 55345.
2.1.7 Sample Line. Leak-free, with compatible fittings to connect
the last impinger to the needle valve.
2.1.8 Rate Meter. Rotameter, or equivalent, capable of measuring
flow rate to within 2 percent of the selected flow rate of 2 liters/min.
2.1.9 Purge Pump, Purge Line, Drying Tube, Needle Valve, and Rate
Meter. Pump capable of purging the sampling probe at 2 liters/min, with
drying tube, filled with silica gel or equivalent, to protect pump, and
a rate meter capable of measuring 0 to 5 liters/min.
2.1.10 Stopcock Grease, Valve, Pump, Volume Meter, Barometer, and
Vacuum Gauge. Same as in Method 6, Sections 2.1.4, 2.1.7, 2.1.8,
2.1.10, 2.1.11, and 2.1.12.
2.1.11 Temperature Measuring Devices. Temperature measuring device
to monitor the temperature of the probe and a thermometer or other
temperature measuring device to monitor the temperature of the sampling
system from the outlet of the probe to the inlet of the first impinger.
2.1.12 Ice Water Bath. To minimize loss of absorbing solution.
2.2 Sample Recovery.
2.2.1 Wash Bottles. Polyethylene or glass, 500-ml or larger, two.
2.2.2 Storage Bottles. 100-ml glass, with Teflon-lined lids, to
store impinger samples (two per sampling run).
2.3 Sample Preparation and Analysis. The materials required for
volumetric dilution and chromatographic analysis of samples are
described below.
2.3.1 Volumetric Flasks. Class A, 100-ml size.
2.3.2 Volumetric Pipets. Class A, assortment. To dilute samples
into the calibration range of the instrument.
2.3.3 Ion Chromatograph. Suppressed or nonsuppressed, with a
conductivity detector and electronic integrator operating in the peak
area mode. Other detectors, strip chart recorders, and peak height
measurements may be used.
Unless otherwise indicated, all reagents must conform to the
specifications established by the Committee on Analytical Reagents of
the American Chemical Society (ACS reagent grade). When such
specifications are not available, the best available grade shall be
used.
3.1. Sampling.
3.1.1 Water. Deionized, distilled water that conforms to ASTM
Specification D 1193-77, Type 3.
3.1.2 Absorbing solution, 0.1 N Sulfuric Acid (H2SO4). To prepare
100 ml of the absorbing solution for the front impinger pair, slowly add
0.28 ml of concentrated H2SO4 to about 90 ml of water while stirring,
and adjust the final volume to 100 ml using additional water. Shake
well to mix the solution.
3.1.3 Chlorine Scrubber Solution, 0.1 N Sodium Hydroxide (NaOH). To
prepare 100 ml of the scrubber solution for the back pair of impingers,
dissolve 0.40 g of solid NaOH in about 90 ml of water, and adjust the
final solution volume to 100 ml using additional water. Shake well to
mix the solution.
3.2 Sample Preparation and Analysis.
3.2.1 Water. Same as in Section 3.1.1.
3.2.2 Blank Solution. A separate blank solution of the absorbing
reagent should be prepared for analysis with the field samples. Dilute
30 ml of absorbing solution to 100 ml with water in a separate
volumetric flask.
3.2.3 Sodium Chloride (NaCl) Stock Standard Solution. Solutions
containing a nominal certified concentration of 1000 mg/l are
commercially available as convenient stock solutions from which working
standards can be made by appropriate volumetric dilution. Alternately,
concentrated stock solutions may be produced from reagent grade NaCl.
The NaCl should be dried at 110 C for 2 or more hours and cooled to
room temperature in a desiccator immediately before weighing.
Accurately weigh 1.6 to 1.7 g of the dried NaCl to within 0.1 mg,
dissolve in water, and dilute to 1 liter. The exact Cl concentration
can be calculated using Eq. 26-1.
Refrigerate the stock standard solution and store no longer than 1
month.
3.2.4 Chromatographic Eluent. Effective eluents for nonsuppressed IC
using a resin- or silica-based weak ion exchange column are a 4 mM
potassium hydrogen phthalate solution, adjusted to pH 4.0 using a
saturated sodium borate solution, and a 4 mM 4-hydroxy benzoate
solution, adjusted to pH 8.6 using 1 N NaOH. An effective eluent for
suppressed ion chromatography is a solution containing 3 mM sodium
bicarbonate and 2.4 mM sodium carbonate. Other dilute solutions
buffered to a similar pH and containing no interfering ions may be used.
When using suppressed ion chromatography, if the ''water dip''
resulting from sample injection interferes with the chloride peak, use a
2 mM NaOH/2.4 mM sodium bicarbonate eluent.
4.1 Sampling.
4.1.1 Preparation of Collection Train. Prepare the sampling train as
follows: Pour 15 ml of the aborbing solution into each of the first two
impingers, and add 15 ml of scrubber solution to the third and fourth
impingers. Connect the impingers in series with the knockout impinger
first, followed by the two impingers containing absorbing solution and
the two containing the scrubber solution. Place a fresh charge of
silica gel, or equivalent, in the drying tube or Mae West impinger.
4.1.2 Adjust the probe temperature and the temperature of the filter
and the stopcock, i.e., the heated area in Figure 26-1 to a temperature
sufficient to prevent water condensation. This temperature should be at
least 20 C above the source temperature, but not greater than 120 C.
The temperature should be monitored throughout a sampling run to ensure
that the desired temperature is maintained.
4.1.3 Leak-Check Procedure. A leak-check prior to the sampling run
is optional; however, a leak-check after the sampling run is mandatory.
The leak-check procedure is as follows: Temporarily attach a suitable
(e.g., 0-40 cc/min) rotameter to the outlet of the dry gas meter and
place a vacuum gauge at or near the probe inlet. Plug the probe inlet,
pull a vacuum of at least 250 mm Hg (10 in. Hg), and note the flow rate
as indicated by the rotameter. A leakage rate not in excess of 2
percent of the average sampling rate is acceptable. (NOTE: Carefully
release the probe inlet plug before turning off the pump.) It is
suggested (not mandatory) that the pump be leak-checked separately,
either prior to or after the sampling run. If done prior to the
sampling run, the pump leak-check shall precede the leak-check of the
sampling train described immediately above; if done after the sampling
run, the pump leak-check shall follow the train leak-check. To
leak-check the pump, proceed as follows: Disconnect the drying tube
from the probe-impinger assembly. Place a vacuum gauge at the inlet to
either the drying tube or pump, pull a vacuum of 250 mm (10 in.) Hg,
plug or pinch off the outlet of the flowmeter, and then turn off the
pump. The vacuum should remain stable for at least 30 sec. Other
leak-check procedures may be used, subject to the approval of the
Administrator, U.S. Environmental Protection Agency.
4.1.4 Purge Procedure. Immediately before sampling, connect the
purge line to the stopcock, and turn the stopcock to permit the purge
pump to purge the probe (see Figure 1A of Figure 26-1). Turn on the
purge pump, and adjust the purge rate to 2 liters/min. Purge for at
least 5 minutes before sampling.
4.1.5 Sample Collection. Turn on the sampling pump, pull a slight
vacuum of approximately 25 mm Hg (1 in. Hg) on the impinger train, and
turn the stopcock to permit stack gas to be pulled through the impinger
train (see Figure 1C of Figure 26-1). Adjust the sampling rate to 2
liters/min, as indicated by the rate meter, and maintain this rate to
within 10 percent during the entire sampling run. Take readings of the
dry gas meter volume and temperature, rate meter, and vacuum gauge at
least once every 5 minutes during the run. A sampling time of 1 hour is
recommended. Shorter sampling times may introduce a significant
negative bias in the HCl concentration. At the conclusion of the
sampling run, remove the train from the stack, cool, and perform a
leak-check as described in section 4.1.2.
4.2 Sample Recovery. Disconnect the impingers after sampling.
Quantitatively transfer the contents of the first three impingers (the
knockout impinger and the two absorbing solution impingers) to a
leak-free storage bottle. Add the water rinses of each of these
impingers and connecting glassware to the storage bottle. The contents
of the scrubber impingers and connecting glassware rinses may be
discarded. The sample bottle should be sealed, shaken to mix, and
labeled. The fluid level should be marked so that if any sample is lost
during transport, a correction proportional to the lost volume can be
applied.
4.3 Sample Preparation for Analysis. Check the liquid level in each
sample, and determine if any sample was lost during shipment. If a
noticeable amount of leakage has occurred, the volume lost can be
determined from the difference between the initial and final solution
levels, and this value can be used to correct the analytical results.
Quantitatively transfer the sample solution to a 100-ml volumetric
flask, and dilute the solution to 100 ml with water.
4.4 Sample Analysis.
4.4.1 The IC conditions will depend upon analytical column type and
whether suppressed or nonsuppressed IC is used. An example chromatogram
from a nonsuppressed system using a 150-mm Hamilton PRP-X100 anion
column, a 2 ml/min flow rate of 4 mM 4-hydroxy benzoate solution
adjusted to a pH of 8.6 using 1 N NaOH, a 50- l sample loop, and a
conductivity detector set on 1.0 S full scale is shown in Figure 26-2.
4.4.2 Before sample analysis, establish a stable baseline. Next,
inject a sample of water, and determine if any Cl^ appears in the
chromatogram. If Cl^ is present, repeat the load/injection procedure
until no Cl^ is present. At this point, the instrument is ready for
use.
4.4.3 First, inject the calibration standards covering an appropriate
concentration range, starting with the lowest concentration standard.
Next, inject in duplicate, a QC sample followed by a water blank and the
field samples. Finally, repeat the injection of calibration standards
to allow compensation for any drift in the instrument during analysis of
the field samples. Measure the Cl^ peak areas or heights of the
samples. Use the average response from the duplicate injections to
determine the field sample concentrations using a linear calibration
curve generated from the standards.
4.5 Audit Analysis. An audit sample must be analyzed, subject to
availability.
5.1 Dry Gas Metering System, Thermometers, Rate Meter, and Barometer.
Same as in Method 6, sections 5.1, 5.2, 5.3, and 5.4.
5.2 Calibration Curve for Ion Chromatograph. To prepare calibration
standards, dilute given volumes (1.0 ml or greater) of the stock
standard solution, with 0.1 N H2SO4 (section 3.1.2) to convenient
volumes. Prepare at least four standards that are within the linear
range of the instrument and which cover the expected concentration range
of the field samples. Analyze the standards as instructed in section
4.4.3, beginning with the lowest concentration standard. Determine the
peak measurements, and plot individual values versus Cl- concentration
in g/ml. Draw a smooth curve through the points. Use linear
regression to calculate a formula describing the resulting linear curve.
6.1 Applicability. When the method is used to analyze samples to
demonstrate compliance with a source emission regulation, a set of two
audit samples must be analyzed.
6.2 Audit Procedure. The audit sample are chloride solutions.
Concurrently analyze the two audit samples and a set of compliance
samples in the same manner to evaluate the technique of the analyst and
the standards preparation. The same analyst, analytical reagents, and
analytical system shall be used both for compliance samples and the EPA
audit samples. If this condition is met, auditing the subsequent
compliance analyses for the same enforcement agency within 30 days is
not required. An audit sample set may not be used to validate different
sets of compliance samples under the jurisdiction of different
enforcement agencies, unless prior arrangements are made with both
enforcement agencies.
6.3 Audit Sample Availability. The audit samples may be obtained by
writing or calling the EPA Regional Office or the appropriate
enforcement agency. The request for the audit samples must be made at
least 30 days prior to the scheduled compliance sample analyses.
6.4 Audit Results.
6.4.1 Calculate the concentrations in mg/dscm using the specified
sample volume in the audit instructions.
Note: Indication of acceptable results may be obtained immediately
by reporting the audit results in mg/dscm and compliance results in
total g HCl/sample to the responsible enforcement agency. Include the
results of both audit samples, their identification numbers, and the
analyst's name with the results of the compliance determination samples
in appropriate reports to the EPA Regional Office or the appropriate
enforcement agency. Include this information with subsequent analyses
for the same enforcement agency during the 30-day period.
6.4.2 The concentrations of the audit samples obtained by the analyst
shall agree within 10 percent of the actual concentrations. If the 10
percent specification is not met, reanalyze the compliance samples and
audit samples, and include initial and reanalysis values in the test
report.
6.4.3 Failure to meet the 10 percent specification may require
retests until the audit problems are resolved. However, if the audit
results do no affect the compliance or noncompliance status of the
affected facility, the Administrator may waive the reanalysis
requirement, further audits, or retests and accept the results of the
compliance test. While steps are being taken to resolve audit analysis
problems, the Administrator may also choose to use the data to determine
the compliance or noncompliance status of the affected facility.
Retain at least one extra decimal figure beyond those contained in
the available data in intermediate calculations, and round off only the
final answer appropriately.
7.1 Sample Volume, Dry Basis, Corrected to Standard Conditions.
Calculate the sample volume using Eq. 6-1 of Method 6.
7.2 Total g HCl Per Sample.
where:
m = Mass of HCl in sample, g.
S = Concentration of sample, g Cl-/ml.
B = Concentration of blank, g Cl-/ml.
100 = Volume of filtered and diluted sample, ml.
36.46 = Molecular weight of HCl, g/ g-mole.
35.45 = Atomic weight of Cl, g/ g-mole.
7.3 Concentration of HCl in the Flue Gas.
C=K m/Vm(std) Eq. 26-3
where:
C = Concentration of HCl, dry basis, mg/dscm.
K = 10-3 mg/ g.
m = Mass of HCl in sample, g.
Vm(std) = Dry gas volume measured by the dry gas meter, corrected to
standard conditions, dscm.
1. Steinsberger, S.C. and J.H. Margeson, ''Laboratory and Field
Evaluation of a Methodology for Determination of Hydrogen Chloride
Emissions form Municipal and Hazardous Waste Incinerators,'' U.S.
Environmental Protection Agency, Office of Research and Develpment,
Report No. 600/3-89/064, April 1989. Available from the National
Technical Information Service, Springfield, VA 22161 as PB89220586/AS.
2. State of California, Air Resources Board. Method 421.
''Determination of Hydrochloric Acid Emissions from Stationary
Sources.'' March 18, 1987.
3. Cheney, J.L. and C.R. Fortune. Improvements in the Methodology for
Measuring Hydrochloric Acid in Combustion Source Emissions. J.
Environ. Sci. Health. A19(3): 337-350. 1984.
40 CFR 60.748 Pt. 60, App. A, Meth. 27
1. Applicability and Principle
1.1 Applicability. This method is applicable for the determination of
vapor tightness of a gasoline delivery tank which is equipped with vapor
collection equipment.
1.2 Principle. Pressure and vacuum are applied alternately to the
compartments of a gasoline delivery tank and the change in pressure or
vacuum is recorded after a specified period of time.
2. Definitions and Nomenclature
2.1 Gasoline. Any petroleum distillate or petroleum
distillate/alcohol blend having a Reid vapor pressure of 27.6
kilopascals or greater which is used as a fuel for internal combustion
engines.
2.2 Delivery Tank. Any container, including associated pipes and
fittings, that is attached to or forms a part of any truck, trailer, or
railcar used for the transport of gasoline.
2.3 Compartment. A liquid-tight division of a delivery tank.
2.4 Delivery Tank Vapor Collection Equipment. Any piping, hoses, and
devices on the delivery tank used to collect and route gasoline vapors
either from the tank to a bulk terminal vapor control system or from a
bulk plant or service station into the tank.
2.5 Time Period of the Pressure or Vacuum Test (t). The time period
of the test, as specified in the appropriate regulation, during which
the change in pressure or vacuum is monitored, in minutes.
2.6 Initial Pressure (Pi). The pressure applied to the delivery tank
at the beginning of the static pressure test, as specified in the
appropriate regulation, in mm H2O.
2.7 Initial Vacuum (Vi). The vacuum applied to the delivery tank at
the beginning of the static vacuum test, as specified in the appropriate
regulation, in mm H2O.
2.8 Allowable Pressure Change (Dp). The allowable amount of decrease
in pressure during the static pressure test, within the time period t,
as specified in the appropriate regulation, in mm H2O.
2.9 Allowable Vacuum Change (Dv). The allowable amount of decrease
in vacuum during the static vacuum test, within the time period t, as
specified in the appropriate regulation, in mm H2O.
3. Apparatus
3.1 Pressure Source. Pump or compressed gas cylinder of air or inert
gas sufficient to pressurize the delivery tank to 500 mm H2O above
atmospheric pressure.
3.2 Regulator. Low pressure regulator for controlling pressurization
of the delivery tank.
3.3 Vacuum Source. Vacuum pump capable of evacuating the delivery
tank to 250 mm H2O below atmospheric pressure.
3.4 Pressure-Vacuum Supply Hose.
3.5 Manometer. Liquid manometer, or equivalent instrument, capable of
measuring up to 500 mm H2O gauge pressure with 2.5 mm H2O precision.
3.6 Pressure-Vacuum Relief Valves. The test apparatus shall be
equipped with an in-line pressure-vacuum relief valve set to activate at
675 mm H2O above atmospheric pressure or 250 mm H2O below atmospheric
pressure, with a capacity equal to the pressurizing or evacuating pumps.
3.7 Test Cap for Vapor Recovery Hose. This cap shall have a tap for
manometer connection and a fitting with shut-off valve for connection to
the pressure-vacuum supply hose.
3.8 Caps for Liquid Delivery Hoses.
4. Pretest Preparations
4.1 Summary. Testing problems may occur due to the presence of
volatile vapors and/or temperature fluctuations inside the delivery
tank. Under these conditions, it is often difficult to obtain a stable
initial pressure at the beginning of a test, and erroneous test results
may occur. To help prevent this, it is recommended that, prior to
testing, volatile vapors be removed from the tank and the temperature
inside the tank be allowed to stabilize. Because it is not always
possible to attain completely these pretest conditions a provision to
ensure reproducible results is included. The difference in results for
two consecutive runs must meet the criterion in Sections 5.2.5 and
5.3.5.
4.2 Emptying of Tank. The delivery tank shall be emptied of all
liquid.
4.3 Purging of Vapor. As much as possible, the delivery tank shall
be purged of all volatile vapors by any safe, acceptable method. One
method is to carry a load of non-volatile liquid fuel, such as diesel or
heating oil, immediately prior to the test, thus flushing out all the
volatile gasoline vapors. A second method is to remove the volatile
vapors by blowing ambient air into each tank compartment for at least 20
minutes. This second method is usually not as effective and often
causes stabilization problems, requiring a much longer time for
stabilization during the testing.
4.4 Temperature Stabilization. As much as possible, the test shall
be conducted under isothermal conditions. The temperature of the
delivery tank should be allowed to equilibrate in the test environment.
During the test, the tank should be protected from extreme environmental
and temperature variability, such as direct sunlight.
5. Test Procedure
5.1 Preparations.
5.1.1 Open and close each dome cover.
5.1.2 Connect static electrical ground connections to tank. Attach
the liquid delivery and vapor return hoses, remove the liquid delivery
elbows, and plug the liquid delivery fittings.
(Note: The purpose of testing the liquid delivery hoses is to detect
tears or holes that would allow liquid leakage during a delivery. Liquid
delivery hoses are not considered to be possible sources of vapor
leakage, and thus, do not have to be attached for a vapor leakage test.
Instead, a liquid delivery hose could be either visually inspected, or
filled with water to detect any liquid leakage.)
5.1.3 Attach the test cap to the end of the vapor recovery hose.
5.1.4 Connect the pressure-vacuum supply hose and the pressure-vacuum
relief valve to the shut-off valve. Attach a manometer to the pressure
tap.
5.1.5 Connect compartments of the tank internally to each other if
possible. If not possible, each compartment must be tested separately,
as if it were an individual delivery tank.
5.2 Pressure Test.
5.2.1 Connect the pressure source to the pressure-vacuum supply hose.
5.2.2 Open the shut-off valve in the vapor recovery hose cap.
Applying air pressure slowly, pressurize the tank to Pi, the initial
pressure specified in the regulation.
5.2.3 Close the shut-off valve and allow the pressure in the tank to
stabilize, adjusting the pressure if necessary to maintain pressure of
Pi. When the pressure stabilizes, record the time and initial pressure.
5.2.4 At the end of t minutes, record the time and final pressure.
5.2.5 Repeat steps 5.2.2 through 5.2.4 until the change in pressure
for two consecutive runs agrees within 12.5 mm H2O. Calculate the
arithmetic average of the two results.
5.2.6 Compare the average measured change in pressure to the
allowable pressure change, *p, as specified in the regulation. If the
delivery tank does not satisfy the vapor tightness criterion specified
in the regulation, repair the sources of leakage, and repeat the
pressure test until the criterion is met.
5.2.7 Disconnect the pressure source from the pressure-vacuum supply
hose, and slowly open the shut-off valve to bring the tank to
atmospheric pressure.
5.3 Vacuum Test.
5.3.1 Connect the vacuum source to the pressure-vacuum supply hose.
5.3.2 Open the shut-off valve in the vapor recovery hose cap. Slowly
evacuate the tank to Vi, the initial vacuum specified in the regulation.
5.3.3 Close the shut-off valve and allow the pressure in the tank to
stabilize, adjusting the pressure if necessary to maintain a vacuum of
Vi. When the pressure stabilizes, record the time and initial vacuum.
5.3.4 At the end of t minutes, record the time and final vacuum.
5.3.5 Repeat steps 5.3.2 through 5.3.4 until the change in vacuum for
two consecutive runs agrees within 12.5 mm H2O. Calculate the
arithmetic average of the two results.
5.3.6 Compare the average measured change in vacuum to the allowable
vacuum change, *v, as specified in the regulation. If the delivery tank
does not satisfy the vapor tightness criterion specified in the
regulation, repair the sources of leakage, and repeat the vacuum test
until the criterion is met.
5.3.7 Disconnect the vacuum source from the pressure-vacuum supply
hose, and slowly open the shut-off valve to bring the tank to
atmospheric pressure.
5.4 Post-Test Clean-Up. Disconnect all test equipment and return the
delivery tank to its pretest condition.
6. Alternative Procedures
6.1 The pumping of water into the bottom of a delivery tank is an
acceptable alternative to the pressure source described above.
Likewise, the draining of water out of the bottom of a delivery tank may
be substituted for the vacuum source. Note that some of the specific
step-by-step procedures in the method must be altered slightly to
accommodate these different pressure and vacuum sources.
6.2 Techniques other than specified above may be used for purging and
pressurizing a delivery tank, if prior approval is obtained from the
Administrator. Such approval will be based upon demonstrated
equivalency with the above method.
40 CFR 60.748 Pt. 60, App. A, Meth. 28
1.1 Applicability. This method is applicable for the certification
and auditing of wood heaters. This method describes the test facility,
test fuel charge, and wood heater operation as well as procedures for
determining burn rates and particulate emission rates and for reducing
data.
1.2 Principle. Particulate matter emissions are measured from a wood
heater burning a prepared test fuel crib in a test facility maintained
at a set of prescribed conditions.
2.1 Burn Rate. The rate at which test fuel is consumed in a wood
heater. Measured in kilograms of wood (dry basis) per hour (kg/hr).
2.2 Certification or Audit Test. A series of at least four test runs
conducted for certification or audit purposes that meets the burn rate
specifications in Section 5.
2.3 Firebox. The chamber in the wood heater in which the test fuel
charge is placed and combusted.
2.4 Secondary Air Supply. An air supply that introduces air to the
wood heater such that the burn rate is not altered by more than 25
percent when the secondary air supply is adjusted during the test run.
The wood heater manufacturer can document this through design drawings
that show the secondary air is introduced only into a mixing chamber or
secondary chamber outside the firebox.
2.5 Test Facility. The area in which the wood heater is installed,
operated, and sampled for emissions.
2.6 Test Fuel Charge. The collection of test fuel pieces placed in
the wood heater at the start of the emission test run.
2.7 Test Fuel Crib. The arrangement of the test fuel charge with the
proper spacing requirements between adjacent fuel pieces.
2.8 Test Fuel Loading Density. The weight of the as-fired test fuel
charge per unit volume of usable firebox.
2.9 Test Fuel Piece. The 2 x 4 or 4 x 4 wood piece cut to the length
required for the test fuel charge and used to construct the test fuel
crib.
2.10 Test Run. An individual emission test which encompasses the
time required to consume the mass of the test fuel charge.
2.11 Usable Firebox Volume. The volume of the firebox determined
using the following definitions:
2.11.1 Height. The vertical distance extending above the loading
door, if fuel could reasonably occupy that space, but not more than 2
inches above the top (peak height) of the loading door, to the floor of
the firebox (i.e., below a permanent grate) if the grate allows a 1-inch
diameter piece of wood to pass through the grate, or, if not, to the top
of the grate. Firebox height is not necessarily uniform but must
account for variations caused by internal baffles, air channels, or
other permanent obstructions.
2.11.2 Length. The longest horizontal fire chamber dimension that is
parallel to a wall of the chamber.
2.11.3 Width. The shortest horizontal fire chamber dimension that is
parallel to a wall of the chamber.
2.12 Wood Heater. An enclosed, woodburning appliance capable of and
intended for space heating or domestic water heating, as defined in the
applicable regulation.
2.13 Pellet Burning Wood Heater. A wood heater which meets the
following criteria: (1) The manufacturer makes no reference to burning
cord wood in advertising or other literature, (2) the unit is safety
listed for pellet fuel only, (3) the unit operating and instruction
manual must state that the use of cordwood is prohibited by law, and (4)
the unit must be manufactured and sold including the hopper and auger
combination as integral parts.
3.1 Insulated Solid Pack Chimney. For installation of wood heaters.
Solid pack insulated chimneys shall have a minimum of 2.5 cm (1 in.)
solid pack insulating material surrounding the entire flue and possess a
label demonstrating conformance to U.L. Standard 103 (incorporated by
reference. See 60.17).
3.2 Platform Scale and Monitor. For monitoring of fuel load weight
change. The scale shall be capable of measuring weight to within 0.05
kg (0.1 lb) or 1 percent of the initial test fuel charge weight,
whichever is greater.
3.3 Wood Heater Temperature Monitors. Seven, each capable of
measuring temperature to within 1.5 percent of expected absolute
temperatures.
3.4 Test Facility Temperature Monitor. A thermocouple located
centrally in a vertically oriented 150 mm (6 in.) long, 50 mm (2 in.)
diameter pipe shield that is open at both ends, capable of measuring
temperature to within 1.5 percent of expected temperatures.
3.5 Balance (optional). Balance capable of weighing the test fuel
charge to within 0.05 kg (0.1 1b).
3.6 Moisture Meter. Calibrated electrical resistance meter for
measuring test fuel moisture to within 1 percent moisture content.
3.7 Anemometer. Device capable of detecting air velocities less than
0.10 m/sec (20 ft/min), for measuring air velocities near the test
appliance.
3.8 Barometer. Mercury, aneroid or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg).
3.9 Draft Gauge. Electromanometer or other device for the
determination of flue draft or static pressure readable to within 0.50
Pa (0.002 in. H2O).
3.10 Humidity Gauge. Psychrometer or hygrometer for measuring room
humidity.
3.11 Sampling Methods. Use particulate emission measurement Method
5G or Method 5H to determine particulate concentrations, gas flow rates,
and particulate emission rates.
Charge Specifications
4.1 Test Facility.
4.1.1 Wood Heater Flue. Steel flue pipe extending to 2.6 0.15 m (8.5
0.5 ft) above the top of the platform scale, and above this level,
insulated solid pack type chimney extending to 4.6+0.3 m (15 1 ft) above
the platform scale, and of the size specified by the wood heater
manufacturer. This applies to both freestanding and insert type wood
heaters.
Other chimney types (e.g., solid pack insulated pipe) may be used in
place of the steel flue pipe if the wood heater manufacturer's written
appliance specifications require such chimney for home installation
(e.g., zero clearance wood heater inserts). Such alternative chimney or
flue pipe must remain and be sealed with the wood heater following the
certification test.
4.1.2 Test Facility Conditions. The test facility temperature shall
be maintained between 18 and 32 C (65 and 90 F) during each test run.
Air velocities within 0.6 m (2 ft) of the test appliance and exhaust
system shall be less than 0.25 m/sec (50 ft/min) without fire in the
unit.
The flue shall discharge into the same space or into a space freely
communicating with the test facility. Any hood or similar device used
to vent combustion products shall not induce a draft greater than 1.25
Pa (0.005 in. H2O) on the wood heater measured when the wood heater is
not operating.
For test facilities with artificially induced barometric pressures
(e.g., pressurized chambers), the barometric pressure in the test
facility shall not exceed 1,033 mb (30.5 in. Hg) during any test run.
4.2 Test Fuel Properties. The test fuel shall conform to the
following requirements:
4.2.1 Fuel Species. Untreated, air-dried, Douglas fir lumber.
Kiln-dried lumber is not permitted. The lumber shall be certified C
grade (standard) or better Douglas fir by a lumber grader at the mill of
origin as specified in the West Coast Lumber Inspection Bureau standard
No. 16 (incorporated by reference. See 60.17).
4.2.2 Fuel Moisture. The test fuel shall have a moisture content
range between 16 to 20 percent on a wet basis (19 to 25 percent dry
basis).
Addition of moisture to previously dried wood is not allowed. It is
recommended that the test fuel be stored in a temperature and
humidity-controlled room.
4.2.3 Fuel Temperature. The test fuel shall be at the test facility
temperature 18 to 32 C (65 to 90 F).
4.3 Test Fuel Charge Specifications.
4.3.1 Fuel Dimensions. The dimensions of each test fuel piece shall
conform to the nominal measurements of 2 x 4 and 4 x 4 lumber. Each
piece of test fuel (not including spacers) shall be of equal length,
except as necessary to meet requirements in Section 6.2.5, and shall
closely approximate 5/6 the dimensions of the length of the usable
firebox. The fuel piece dimensions shall be determined in relation to
the appliance's firebox volume according to guidelines listed below:
4.3.1.1 If the usable firebox volume is less than or equal to 0.043 m
/3/ (1.5 ft /3/ ), use 2 x 4 lumber.
4.3.1.2 If the usable firebox volume is greater than 0.043 m /3/
(1.5 ft /3/ ) and less than or equal to 0.085 m /3/ (3.0 ft /3/ ),
use 2 x 4 and 4 x 4 lumber. About half the weight of the test fuel
charge shall be 2 x 4 lumber, and the remainder shall be 4 x 4 lumber.
4.3.1.3 If the usable firebox volume is greater than 0.085 m /3/
(3.0 ft /3/ ), use 4 x 4 lumber.
4.3.2 Test Fuel Spacers. Air-dried, Douglas fir lumber meeting the
fuel properties in Section 4.2. The spacers shall be 130 x 40 x 20 mm (5
x 1.5 x 0.75 in.).
4.3.3 Test Fuel Charge Density. The test fuel charge density shall
be 112 11.2 kg/m /3/ (7 0.7 lb/ft /3/ ) of usable firebox volume on
a wet basis.
4.4 Wood Heater Thermal Equilibrium. The average of the wood heater
surface temperatures at the end of the test run shall agree with the
average surface temperature at the start of the test run to within 70 C
(125 F).
5.1 Burn Rate Categories. One emission test run is required in each
of the following burn rate categories:
5.1.1 Maximum Burn Rate. For Category 4, the wood heater shall be
operated with the primary air supply inlet controls fully open (or, if
thermostatically controlled, the thermostat shall be set at maximum heat
output) during the entire test run, or the maximum burn rate setting
specified by the manufacturer's written instructions.
5.1.2 Other Burn Rate Categories. For burn rates in Categories 1
through 3, the wood heater shall be operated with the primary air supply
inlet control, or other mechanical control device, set at a
predetermined position necessary to obtain the average burn rate
required for the category.
5.2 Alternative Burn Rates for Burn Rate Categories 1 and 2. If a
wood heater cannot be operated at a burn rate below 0.80 kg/hr, two test
runs shall be conducted with burn rates within Category 2. If a wood
heater cannot be operated at a burn rate below 1.25 kg/hr, the flue
shall be dampered or the air supply otherwise controlled in order to
achieve two test runs within Category 2.
Evidence that a wood heater cannot be operated at a burn rate less
than 0.80 kg/hr shall include documentation of two or more attempts to
operate the wood heater in burn rate Category 1 and fuel combustion has
stopped, or results of two or more test runs demonstrating that the burn
rates were greater than 0.80 kg/hr when the air supply controls were
adjusted to the lowest possible position or settings. Stopped fuel
combustion is evidenced when an elapsed time of 30 minutes or more has
occurred without a measurable (< 0.05 kg (0.1 lb) or 1.0 percent,
whichever is greater) weight change in the test fuel charge. See also
Section 6.4.3. Report the evidence and the reasoning used to determine
that a test in burn rate Category 1 cannot be achieved; for example,
two attempts to operate at a burn rate of 0.4 kg/hr are not sufficient
evidence that burn rate Category 1 cannot be achieved.
Note: After July 1, 1990, if a wood heater cannot be operated at a
burn rate less than 0.80 kg/hr, at least one test run with an average
burn rate of 1.00 kg/hr or less shall be conducted. Additionally, if
flue dampering must be used to achieve burn rates below 1.25 kg/hr (or
1.0 kg/hr), results from a test run conducted at burn rates below 0.90
kg/hr need not be reported or included in the test run average provided
that such results are replaced with results from a test run meeting the
criteria above.
6.1 Catalytic Combustor and Wood Heater Aging. The catalyst-equipped
wood heater or a wood heater of any type shall be aged before the
certification test begins. The aging procedure shall be conducted and
documented by a testing laboratory accredited according to procedures in
60.535 of 40 CFR Part 60.
6.1.1 Catalyst-equipped Wood Heater. Operate the catalyst-equipped
wood heater using fuel described in Section 4.2 or cordwood with a
moisture content between 15 and 25 percent on a wet basis. Operate the
wood heater at a medium burn rate (Category 2 or 3) with a new catalytic
combustor in place and in operation for at least 50 hours. Record and
report hourly catalyst exit temperature data (Section 6.2.2) and the
hours of operation.
6.1.2 Non-Catalyst Wood Heater. Operate the wood heater using the
fuel described in Section 6.1.1 at a medium burn rate for at least 10
hours. Record and report the hours of operation.
6.2 Pretest Preparation. Record the test fuel charge dimensions and
weights, and wood heater and catalyst descriptions as shown in the
example in Figure 28-3.
6.2.1 Wood Heater Installation. Assemble the wood heater appliance
and parts in conformance with the manufacturer's written installation
instructions. Place the wood heater centrally on the platform scale and
connect the wood heater to the flue described in Section 4.1.1. Clean
the flue with an appropriately sized, wire chimney brush before each
certification test.
6.2.2 Wood Heater Temperature Monitors. For catalyst-equipped wood
heaters, locate a temperature monitor (optional) about 25 mm (1 in.)
upstream of the catalyst at the centroid of the catalyst face area, and
locate a temperature monitor (mandatory) that will indicate the catalyst
exhaust temperature. This temperature monitor is centrally located
within 25 mm (1 in.) downstream at the centroid of catalyst face area.
Record these locations.
Locate wood heater surface temperature monitors at five locations on
the wood heater firebox exterior surface. Position the temperature
monitors centrally on the top surface, on two sidewall surfaces, and on
the bottom and back surfaces. Position the monitor sensing tip on the
firebox exterior surface inside of any heat shield, air circulation
walls, or other wall or shield separated from the firebox exterior
surface. Surface temperature locations for unusual design shapes (e.g.,
spherical, etc.) shall be positioned so that there are four surface
temperature monitors in both the vertical and horizontal planes passing
at right angles through the centroid of the firebox, not including the
fuel loading door (total of five temperature monitors).
6.2.3 Test Facility Conditions. Locate the test facility temperature
monitor on the horizontal plane that includes the primary air intake
opening for the wood heater. Locate the temperature monitor 1 to 2 m (3
to 6 ft) from the front of the wood heater in the 90 sector in front of
the wood heater.
Use an anemometer to measure the air velocity. Measure and record
the room air velocity before the pretest ignition period (Section 6.3)
and once immediately following the test run completion.
Measure and record the test facility's ambient relative humidity,
barometric pressure, and temperature before and after each test run.
Measure and record the flue draft or static pressure in the flue at a
location no greater than 0.3 m (1 ft) above the flue connector at the
wood heater exhaust during the test run at the recording intervals
(Section 6.4.2).
6.2.4 Wood Heater Firebox Volume. Determine the firebox volume using
the definitions for height, width, and length in Section 2. Volume
adjustments due to presence of firebrick and other permanent fixtures
may be necessary. Adjust width and length dimensions to extend to the
metal wall of the wood heater above the firebrick or permanent
obstruction if the firebrick or obstruction extending the length of the
side(s) or back wall extends less than one-third of the usable firebox
height. Use the width or length dimensions inside the firebrick if the
firebrick extends more than one-third of the usable firebox height. If
a log retainer or grate is a permanent fixture and the manufacturer
recommends that no fuel be placed outside the retainer, the area outside
of the retainer is excluded from the firebox volume calculations.
In general, exclude the area above the ash lip if that area is less
than 10 percent of the usable firebox volume. Otherwise, take into
account consumer loading practices. For instance, if fuel is to be
loaded front-to-back, an ash lip may be considered usable firebox
volume.
Include areas adjacent to and above a baffle (up to two inches above
the fuel loading opening) if four inches or more horizontal space exist
between the edge of the baffle and a vertical obstruction (e.g.,
sidewalls or air channels).
6.2.5 Test Fuel Charge. Prepare the test fuel pieces in accordance
with the specifications in Section 4.3. Determine the test fuel moisture
content with a calibrated electrical resistance meter or other
equivalent performance meter. (To convert moisture meter readings from
the dry basis to the wet basis: (100)(percent dry reading) (100 +
percent dry reading) = percent moisture wet basis.) Determine fuel
moisture for each fuel piece (not including spacers) by averaging at
least three moisture meter readings, one from each of three sides,
measured parallel to the wood grain. Average all the readings for all
the fuel pieces in the test fuel charge. If an electrical resistance
type meter is used, penetration of insulated electrodes shall be
one-fourth the thickness of the test fuel piece or 19 mm (0.75 in.),
whichever is greater. Measure the moisture content within a 4-hour
period prior to the test run. Determine the fuel temperature by
measuring the temperature of the room where the wood has been stored for
at least 24 hours prior to the moisture determination.
Attach the spacers to the test fuel pieces with uncoated,
ungalvanized nails or staples as illustrated in Figure 28-1. Attachment
of spacers to the top of the test fuel piece(s) on top of the test fuel
charge is optional.
To avoid stacking difficulties, or when a whole number of test fuel
pieces does not result, all piece lengths shall be adjusted uniformly to
remain within the specified loading density. The shape of the test fuel
crib shall be geometrically similar to the shape of the firebox volume
without resorting to special angular or round cuts on the individual
fuel pieces.
6.2.6 Sampling Method. Prepare the sampling equipment as defined by
the selected method. Collect one particulate emission sample for each
test run.
6.2.7 Secondary Air Adjustment Validation. If design drawings do not
show the introductions of secondary air into a chamber outside the
firebox (Section 2.4), conduct a separate test of the wood heater's
secondary air supply. Operate the wood heater at a burn rate in
Category 1 (Sections 5.1 or 5.2) with the secondary air supply operated
following the manufacturer's written instructions. Start the secondary
air validation test run as described in Section 6.4.1, except no
emission sampling is necessary and burn rate data shall be recorded at
5-minute intervals.
After the start of the test run, operate the wood heater with the
secondary air supply set as per the manufacturer's instructions, but
with no adjustments to this setting. After 25 percent of the test fuel
has been consumed, adjust the secondary air supply controls to another
setting, as per the manufacturer,s instructions. Record the burn rate
data (5-minute intervals) for 20 minutes following the air supply
adjustment.
Adjust the air supply control(s) to the original position(s), operate
at this condition for at least 20 minutes, and repeat the air supply
adjustment procedure above. Repeat the procedure three times at equal
intervals over the entire burn period as defined in Section 6.4. If the
secondary air adjustment results in a burn rate change of more than an
average of 25 percent between the 20-minute periods before and after the
secondary adjustments, the secondary air supply shall be considered a
primary air supply, and no adjustment to this air supply is allowed
during the test run.
6.3 Pretest Ignition. Build a fire in the wood heater in accordance
with the manufacturer's written instructions.
6.3.1 Pretest Fuel Charge. Crumpled newspaper loaded with kindling
may be used to help ignite the pretest fuel. The pretest fuel, used to
sustain the fire, shall meet the same fuel requirements prescribed in
Section 4.2. The pretest fuel charge shall consist of whole 2 x 4's that
are no less than 1/3 the length of the test fuel pieces. Pieces of 4 x
4 lumber in approximately the same weight ratio as for the test fuel
charge may be added to the pretest fuel charge.
6.3.2 Wood Heater Operation and Adjustments. Set the air inlet
supply controls at any position that will maintain combustion of the
pretest fuel load. At least one hour before the start of the test run,
set the air supply controls at the approximate positions necessary to
achieve the burn rate desired for the test run. Adjustment of the air
supply controls, fuel addition or subtractions, and coalbed raking shall
be kept to a minimum but are allowed up to 15 minutes prior to the start
of the test run. For the purposes of this method, coalbed raking is the
use of a metal tool (poker) to stir coals, break burning fuel into
smaller pieces, dislodge fuel pieces from positions of poor combustion,
and check for the condition of uniform charcoalization. Record all
adjustments made to the air supply controls, adjustments to and
additions or subtractions of fuel, and any other changes to wood heater
operations that occur during pretest ignition period. Record fuel
weight data and wood heater temperature measurements at 10-minute
intervals during the hour of the pretest ignition period preceding the
start of the test run. During the 15-minute period prior to the start
of the test run, the wood heater loading door shall not be open more
than a total of 1 minute. Coalbed raking is the only adjustment allowed
during this period.
Note: One purpose of the pretest ignition period is to achieve
uniform charcoalization of the test fuel bed prior to loading the test
fuel charge. Uniform charcoalization is a general condition of the test
fuel bed evidenced by an absence of large pieces of burning wood in the
coal bed and the remaining fuel pieces being brittle enough to be broken
into smaller charcoal pieces with a metal poker. Manipulations to the
fuel bed prior to the start of the test run should be done to achieve
uniform charcoalization while maintaining the desired burn rate. In
addition, some wood heaters (e.g., high mass units) may require extended
pretest burn time and fuel additions to reach an initial average surface
temperature sufficient to meet the thermal equilibrium criteria in
Section 4.4.
The weight of pretest fuel remaining at the start of the test run is
determined as the difference between the weight of the wood heater with
the remaining pretest fuel and the tare weight of the cleaned, dry wood
heater with or without dry ash or sand added consistent with the
manufacturer's instructions and the owner's manual. The tare weight of
the wood heater must be determined with the wood heater (and ash, if
added) in a dry condition.
6.4 Test Run. Complete a test run in each burn rate category, as
follows:
6.4.1 Test Run Start. When the kindling and pretest fuel have been
consumed to leave a fuel weight between 20 and 25 percent of the weight
of the test fuel charge, record the weight of the fuel remaining and
start the test run. Record and report any other criteria, in addition
to those specified in this section, used to determine the moment of the
test run start (e.g., firebox or catalyst temperature), whether such
criteria are specified by the wood heater manufacturer or the testing
laboratory. Record all wood heater individual surface temperatures,
catalyst temperatures, any initial sampling method measurement values,
and begin the particulate emission sampling. Within 1 minute following
the start of the test run, open the wood heater door, load the test fuel
charge, and record the test fuel charge weight. Recording of average,
rather than individual, surface temperatures is acceptable for tests
conducted in accordance with 60.533(o)(3)(i) of 40 CFR Part 60.
Position the fuel charge so that the spacers are parallel to the
floor of the firebox, with the spacer edges abutting each other. If
loading difficulties result, some fuel pieces may be placed on edge. If
the usable firebox volume is between 0.043 and 0.085 m /3/ (1.5 and 3.0
ft /3/ ), alternate the piece sizes in vertical stacking layers to the
extent possible. For example, place 2 x 4's on the bottom layer in
direct contact with the coal bed and 4 x 4's on the next layer, etc.
(See Figure 28-2). Position the fuel pieces parallel to each other and
parallel to the longest wall of the firebox to the extent possible
within the specifications in Section 6.2.5.
Load the test fuel in appliances having unusual or unconventional
firebox design maintaining air space intervals between the test fuel
pieces and in conformance with the manufacturer's written instructions.
For any appliance that will not accommodate the loading arrangement
specified in the paragraph above, the test facility personnel shall
contact the Administrator for an alternative loading arrangement.
The wood heater door may remain open and the air supply controls
adjusted up to five minutes after the start of the test run in order to
make adjustments to the test fuel charge and to ensure ignition of the
test fuel charge has occurred. Within the five minutes after the start
of the test run, close the wood heater door and adjust the air supply
controls to the position determined to produce the desired burn rate.
No other adjustments to the air supply controls or the test fuel charge
are allowed (except as specified in Sections 6.4.3 and 6.4.4) after the
first five minutes of the test run. Record the length of time the wood
heater door remains open, the adjustments to the air supply controls,
and any other operational adjustments.
6.4.2 Data Recording. Record fuel weight data, wood heater
individual surface and catalyst temperature measurements, other wood
heater operational data (e.g., draft), test facility temperature and
sampling method data at 10-minute intervals (or more frequently at the
option of the tester) as shown on example data sheet, Figure 28-4.
6.4.3 Test Fuel Charge Adjustment. The test fuel charge may be
adjusted (i.e., re-positioned) once during a test run if more than 60
percent of the initial test fuel charge weight has been consumed and
more than 10 minutes have elapsed without a measurable (< 0.05 kg (0.1
lb) or 1.0 percent, whichever is greater) weight change. The time used
to make this adjustment shall be less than 15 seconds.
6.4.4 Air Supply Adjustment. Secondary air supply controls may be
adjusted once during the test run following the manufacturer's written
instructions (see Section 6.2.7). No other air supply adjustments are
allowed during the test run.
Recording of wood heater flue draft during the test run is optional
for tests conducted in accordance with 60.533(o)(3)(i) of 40 CFR Part
60.
6.4.5 Auxiliary Wood Heater Equipment Operation. Heat exchange
blowers sold with the wood heater shall be operated during the test run
following the manufacturer's written instructions. If no manufacturer's
written instructions are available, operate the heat exchange blower in
the ''high'' position. (Automatically operated blowers shall be
operated as designed.) Shaker grates, by-pass controls, or other
auxiliary equipment may be adjusted only one time during the test run
following the manufacturer's written instructions.
Record all adjustments on a wood heater operational written record.
Note: If the wood heater is sold with a heat exchange blower as an
option, test the wood heater with the heat exchange blower operating as
described in Sections 5 and 6 and report the results. As an alternative
to repeating all test runs without the heat exchange blower operating,
the tester may conduct one test run without the blower operating as
described in Section 6.4.5 at a burn rate in Category 2 (Section 5.1).
If the emission rate resulting from this test run without the blower
operating is equal to or less than the emission rate plus 1.0 g/hr for
the test run in burn rate Category 2 with the blower operating, the wood
heater may be considered to have the same average emission rate with or
without the blower operating. Additional test runs without the blower
operating are unnecessary.
6.5 Consecutive Test Runs. Test runs on a wood heater may be
conducted consecutively provided that a minimum one-hour interval occurs
between test runs.
6.6 Additional Test Runs. The testing laboratory may conduct more
than one test run in each of the burn rate categories specified in
Section 5.1. If more than one test run is conducted at a specified burn
rate, the results from at least two-thirds of the test runs in that burn
rate category shall be used in calculating the weighted average emission
rate (see Section 8.1). The measurement data and results of all test
runs shall be reported regardless of which values are used in
calculating the weighted average emission rate (see Note: in Section
5.2).
6.7 Pellet Burning Heaters. Certification testing procedures for
pellet burning wood heaters are based on the procedures in this method.
The differences in the procedures from the sections in Method 28 are as
follows:
6.7.1 Test Fuel Properties. The test fuel shall be all wood pellets
with a moisture content no greater than 20 percent on a wet basis (25
percent on a dry basis). Determine the wood moisture content with
either ASTM-D2016-74(82)(Method A) or ASTM D4442-84. (incorporated by
reference. See Section 60.17).
6.7.2 Test Fuel Charge Specifications. The test fuel charge size
shall be as per the manufacturer s written instructions for maintaining
the desired burn rate.
6.7.3 Wood Heater Firebox Volume. The firebox volume need not be
measured or determined for establishing the test fuel charge size. The
firebox dimensions and other heater specifications needed to identify
the heater for certification purposes shall be reported.
6.7.4 Heater Installation. Arrange the heater with the fuel supply
hopper on the platform scale as described in Section 6.2.1.
6.7.5 Pretest Ignition. Start a fire in the heater as directed by
the manufacturer's written instructions, and adjust the heater controls
to achieve the desired burn rate. Operate the heater at the desired
burn rate for at least 1 hour before the start of the test run.
6.7.6 Sampling Method. Method 5G or 5H shall be used for the
certification testing of pellet burners. Prepare the sampling equipment
as described in Method 5G or 5H. Collect one particulate emission
sample for each test run.
6.7.7 Test Run. Complete a test run in each burn rate category as
follows:
6.7.7.1 Test Run Start. When the wood heater has operated for at
least 1 hour at the desired burn rate, add fuel to the supply hopper as
necessary to complete the test run, record the weight of the fuel in the
supply hopper (the wood heater weight), and start the test run. Add no
additional fuel to the hopper during the test run.
Record all the wood heater surface temperatures, the initial sampling
method measurement values, the time at the start of the test, and begin
the emission sampling. Make no adjustments to the wood heater air
supply or wood supply rate during the test run.
6.7.7.2 Data Recording. Record the fuel (wood heater) weight data,
wood heater temperature and operational data, and emission sampling data
as described in Section 6.4.2.
6.7.7.3 Test Run Completion. Continue emission sampling and wood
heater operation for 2 hours. At the end of the test run, stop the
particulate sampling, and record the final fuel weight, the run time,
and all final measurement values.
6.7.8 Calculations. Determine the burn rate using the difference
between the initial and final fuel (wood heater) weights and the
procedures described in Section 8.3. Complete the other calculations as
described in Section 8.
7.1 Platform Scale. Perform a multipoint calibration (at least five
points spanning the operational range) of the platform scale before its
initial use. The scale manufacturer's calibration results are
sufficient for this purpose. Before each certification test, audit the
scale with the wood heater in place by weighing at least one calibration
weight (Class F) that corresponds to 20 percent to 80 percent of the
expected test fuel charge weight. If the scale cannot reproduce the
value of the calibration weight within 0.05 kg (0.1 lbs) or 1 percent of
the expected test fuel charge weight, whichever is greater, recalibrate
the scale before use with at least five calibration weights spanning the
operational range of the scale.
7.2 Balance (optional). Calibrate as described in Section 7.1.
7.3 Temperature Monitor. Calibrate as in Method 2, Section 4.3,
before the first certification test and semiannually thereafter.
7.4 Moisture Meter. Calibrate as per the manufacturer's instructions
before each certification test.
7.5 Anemometer. Calibrate the anemometer as specified by the
manufacturer's instructions before the first certification test and
semiannually thereafter.
7.6 Barometer. Calibrate against a mercury barometer before the first
certification test and semiannually thereafter.
7.7 Draft Gauge. Calibrate as per the manufacturer's instructions;
a liquid manometer does not require calibration.
7.8 Humidity Gauge. Calibrate as per the manufacturer's instructions
before the first certification test and semiannually thereafter.
Carry out calculations retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after the final
calculation.
8.1 Weighted Average Emission Rate.
where:
Ew=Weighted average emission rate, g/hr;
Ei=Emission rate for test run, i, from Method 5G or 5H, g/hr;
ki=Test run weighting factor=Pi+1 -- Pi-1;
n=Total number of test runs;
Pi=Probability for burn rate during test run, i, obtained from Table
28-1. Use linear interpolation to determine probability values for burn
rates between those listed on the table.
Note: Po always equals 0, P(n+1) always equals 1, P1 corresponds to
the probability of the lowest recorded burn rate, P2 corresponds to the
probability of the next lowest burn rate, etc. An example calculation
is shown on Figure 28-5.
8.2 Average Wood Heater Surface Temperatures. Calculate the average
of the wood heater surface temperatures for the start of the test run
(Section 6.3.1) and for the test run completion (Section 6.3.6). If the
two average temperatures do not agree within 70 C (125 F), report the
test run results, but do not include the test run results in the test
average. Replace such test run results with results from another test
run in the same burn rate category.
8.3 Burn Rate.
Where:
BR = Dry wood burn rate, kg/hr (lb/hr)
Wwd = Total mass of wood burned during the test run, kg (lb)
u - Total time of test run, min.
%Mw = Average moisture in test fuel charge, wet basis, percent.
8.4 Reporting Criteria. Submit both raw and reduced test data for
wood heater tests. Specific reporting requirements are as follows:
8.4.1 Wood Heater Identification. Report wood heater identification
information. An example data form is shown on Figure 28-4.
8.4.2 Test Facility Information. Report test facility temperature,
air velocity, and humidity information. An example data form is shown
on Figure 28-4.
8.4.3 Test Equipment Calibration and Audit Information. Report
calibration and audit results for the platform scale, test fuel balance,
test fuel moisture meter, and sampling equipment including volume
metering systems and gaseous analyzers.
8.4.4 Pretest Procedure Description. Report all pretest procedures
including pretest fuel weight, burn rates, wood heater temperatures, and
air supply settings. An example data form is shown on Figure 28-4.
8.4.5 Particulate Emission Data. Report a summary of test results
for all test runs and the weighted average emission rate. Submit copies
of all data sheets and other records collected during the testing.
Submit examples of all calculations.
8.4.6 Suggested Test Report Format.
1. Purpose of test -- certification, audit, efficiency, research and
development.
2. Wood heater identification -- manufacturer, model number,
catalytic/ noncatalytic, options.
3. Laboratory -- name, location (altitude), participants.
4. Test information -- date wood heater received, date of tests,
sampling methods used, number of test runs.
1. Table of results (in order of increasing burn rate) -- test run
number, burn rate, particulate emission rate, efficiency (if
determined), averages (indicate which test runs are used).
2. Summary of other data -- test facility conditions, surface
temperature averages, catalyst temperature averages, pretest fuel
weights, test fuel charge weights, run times.
3. Discussion -- Burn rate categories achieved, test run result
selection, specific test run problems and solutions.
1. Wood heater dimensions -- volume, height, width, lengths (or other
linear dimensions), weight, volume adjustments.
2. Firebox configuration -- air supply locations and operation, air
supply introduction location, refractory location and dimensions,
catalyst location, baffle and by-pass location and operation (include
line drawings or photographs).
3. Process operation during test -- air supply settings and
adjustments, fuel bed adjustments, draft.
4. Test fuel -- test fuel properties (moisture and temperature), test
fuel crib description (include line drawing or photograph), test fuel
charge density.
Describe sampling location relative to wood heater. Include drawing
or photograph.
1. Sampling methods -- brief reference to operational and sampling
procedures and optional and alternative procedures used.
2. Analytical methods -- brief description of sample recovery and
analysis procedures.
1. Calibration procedures and results -- certification procedures,
sampling and analysis procedures.
2. Test method quality control procedures -- leak-checks, volume
meter checks, stratification (velocity) checks, proportionality results.
1. Results and Example Calculations. Complete summary tables and
accompanying examples of all calculations.
2. Raw Data. Copies of all uncorrected data sheets for sampling
measurements, temperature records and sample recovery data. Copies of
all pretest burn rate and wood heater temperature data.
3. Sampling and Analytical Procedures. Detailed description of
procedures followed by laboratory personnel in conducting the
certification test, emphasizing particularly parts of the procedures
differing from the methods (e.g., approved alternatives).
4. Calibration Results. Summary of all calibrations, checks, and
audits pertinent to certification test results with dates.
5. Participants. Test personnel, manufacturer representatives, and
regulatory observers.
6. Sampling And Operation Records. Copies of uncorrected records of
activities not included on raw data sheets (e.g., wood heater door open
times and durations).
7. Additional Information. Wood heater manufacturer's written
instructions for operation during the certification test.
1. Oregon Department of Environmental Quality Standard Method for
Measuring the Emissions and Efficiencies of Woodstoves, June 8, 1984.
Pursuant to Oregon Administrative Rules Chapter 340, Division 21.
2. American Society for Testing Materials. Proposed Test Methods for
Heating Performance and Emissions of Residential Wood-Fired Closed
Combustion-Chamber Heating Appliances. E-6 Proposal P 180. August,
1986.
3. Radian Corporation, OMNI Environmental Services, Inc., Cumulative
Probability for a Given Burn Rate Based on Data Generated in the CONEG
and BPA Studies. Package of materials submitted to the Fifth Session of
the Regulatory Negotiation Committee, July 16-17, 1986.
Insert illus 0199
Insert illus 0200
Insert illus 0201
Insert illus 0202
K1=P2^Po=0.300^0=0.300
K2=P3^P1=0.380^0.121=0.259
K3=P4^P2=0.722^0.300=0.422
K4=P5^P3=0.912^0.380=0.532
K5=P6^P4=1^0.722=0.278
Ew equals (0.3)(5.0)+(0.259)(4.7)+(0.422)(5.3)+(0.(5.1) divided by
1.791
Ew=4.69 g/hr.
40 CFR 60.748 Pt. 60, App. A, Meth. 28A
1.1 Applicability. This method is applicable for the measurement of
air to fuel ratios and minimum achievable burn rates, for determining
whether a wood-fired appliance is an affected facility, as specified in
40 CFR 60.530.
1.2 Principle. A gas sample is extracted from a location in the stack
of a wood-fired appliance while the appliance is operating at a
prescribed set of conditions. The gas sample is analyzed for percent
carbon dioxide (CO2), percent oxygen (O2), and percent carbon monoxide
(CO). These stack gas components are measured for determining dry
molecular weight of exhaust gas. Total moles of exhaust gas are
determined stoichiometrically. Air to fuel ratio is determined by
relating the mass of dry combustion air to the mass of dry fuel
consumed.
2.1 Burn Rate, Firebox, Secondary Air Supply, Test Facility, Test
Fuel Charge, Test Fuel Crib, Test Fuel Loading Density, Test Fuel Piece,
Test Run, Usable Firebox Volume, and Wood Heater. Same as Method 28,
Sections 2.1 and 2.3 to 2.12.
2.2 Air to Fuel Ratio. Ratio of the mass of dry combustion air
introduced into the firebox, to the mass of dry fuel consumed (grams of
dry air per gram of dry wood burned).
3.1 Test Facility. Insulated Solid Pack Chimney, Platform Scale and
Monitor, Room Temperature Monitor, Balance, Moisture Meter, Anemometer,
Barometer, Draft Gauge, and Humidity Gauge. Same as Method 28, Sections
3.1, 3.2, and 3.4 to 3.10, respectively.
3.2 Sampling System. Probe, Condenser, Valve, Pump, Rate Meter,
Flexible Bag, Pressure Gauge, and Vacuum Gauge. Same as Method 3,
Sections 2.2.1 to 2.2.8, respectively. The sampling systems described in
Method 5H, Sections 2.2.1, 2.2.2, and 2.2.3, may be used.
3.3 Analysis. Orsat analyzer, same as Method 3, Section 2.3; or
instrumental analyzers, same as Method 5H, Sections 2.2.4 and 2.2.5, for
CO2 and CO analyzers, except use a CO analyzer with a range of 0 to 5
percent and use a CO2 analyzer with a range of 0 to 5 percent. Use an
O2 analyzer capable of providing a measure of O2 in the range of 0 to 25
percent by volume at least once every 10 minutes. Prepare cylinder
gases for the three analyzers as described in Method 5H, Section 3.3.
4.1 Test Facility, Wood Heater Appliance Installation, and Test
Facility Conditions. Same as Method 28, Sections 4.1.1 and 4.1.2,
respectively, with the exception that barometric dampers or other
devices designed to introduce dilution air downstream of the firebox
shall be sealed.
4.2 Wood Heater Air Supply Adjustments. This section describes how
dampers are to be set or adjusted and air inlet ports closed or sealed
during Method 28A tests. The specifications in this section are
intended to ensure that affected facility determinations are made on the
facility configurations that could reasonably be expected to be employed
by the user. They are also intended to prevent circumvention of the
standard through the addition of an air port that would often be blocked
off in actual use. These specifications are based on the assumption
that consumers will remove such items as dampers or other closure
mechanism stops if this can be done readily with household tools; that
consumers will block air inlet passages not visible during normal
operation of the appliance using aluminum tape or parts generally
available at retail stores; and that consumers will cap off any
threaded or flanged air inlets. They also assume that air leakage
around glass doors, sheet metal joints or through inlet grilles visible
during normal operation of the appliance would not be further blocked or
taped off by a consumer.
It is not the intention of this section to cause an appliance that is
clearly designed, intended, and, in most normal installations, used as a
fireplace to be converted into a wood heater for purposes of
applicability testing. Such a fireplace would be identifiable by such
features as large or multiple glass doors or panels that are not
gasketed, relatively unrestricted air inlets intended, in large part, to
limit smoking and fogging of glass surfaces, and other aesthetic
features not normally included in wood heaters.
4.2.1 Adjustable Air Supply Mechanisms. Any commercially available
flue damper, other adjustment mechanism or other air inlet port that is
designed, intended or otherwise reasonably expected to be adjusted or
closed by consumers, installers, or dealers and which could restrict air
into the firebox shall be set so as to achieve minimum air into the
firebox, i.e., closed off or set in the most closed position.
Flue dampers, mechanisms and air inlet ports which could reasonably
be expected to be adjusted or closed would include:
(a) All internal or externally adjustable mechanisms (including
adjustments that affect the tightness of door fittings) that are
accessible either before and/or after installation.
(b) All mechanisms, other inlet ports, or inlet port stops that are
identified in the owner's manual or in any dealer literature as being
adjustable or alterable. For example, an inlet port that could be used
to provide access to an outside air duct but which is identified as
being closable through use of additional materials whether or not they
are supplied with the facility.
(c) Any combustion air inlet port or commercially available flue
damper or mechanism stop, which would readily lend itself to closure by
consumers who are handy with household tools by the removal of parts or
the addition of parts generally available at retail stores (e.g.,
addition of a pipe cap or plug, addition of a small metal plate to an
inlet hole on a nondecorative sheet metal surface, or removal of riveted
or screwed damper stops).
(d) Any flue damper, other adjustment mechanisms or other air inlet
ports that are found and documented in several (e.g., a number
sufficient to reasonably conclude that the practice is not unique or
uncommon) actual installations as having been adjusted to a more closed
position, or closed by consumers, installers, or dealers.
4.2.2 Air Supply Adjustments During Test. The test shall be
performed with all air inlets identified under this section in the
closed or most closed position or in the configuration which otherwise
achieves the lowest air inlet (e.g., greatest blockage).
For the purposes of this section, air flow shall not be minimized
beyond the point necessary to maintain combustion or beyond the point
that forces smoke into the room.
Notwithstanding Section 4.2.1, any flue damper, adjustment mechanism
or air inlet port (whether or not equipped with flue dampers or
adjusting mechanisms) that is visible during normal operation of the
appliance and which could not reasonably be closed further or blocked
except through means that would significantly degrade the aesthetics of
the facility (e.g., through use of duct tape) will not be closed further
or blocked.
4.3 Test Fuel Properties and Test Fuel Charge Specifications. Same
as Method 28, Sections 4.2 to 4.3, respectively.
4.4 Sampling System.
4.4.1 Sampling Location. Same as Method 5H, Section 5.1.2.
4.4.2 Sampling System Set Up. Set up the sampling equipment as
described in Method 3, Section 3.2, or as in Method 3A, Section 7.
5.1 Pretest Preparation. Same as Method 28, Sections 6.2.1 and 6.2.3
to 6.2.5.
5.2 Pretest Ignition. Same as Method 28, Section 6.3. Set the wood
heater air supply settings to achieve a burn rate in Category 1 or the
lowest achievable burn rate (see Section 4.2).
5.3 Test Run. Same as Method 28, Section 6.4. Begin sample
collection at the start of the test run as defined in Method 28, Section
6.4.1. If Method 3 is used, collect a minimum of two bag samples
simultaneously at a constant sampling rate for the duration of the test
run. A minimum sample volume of 30 1 per bag is recommended. If
instrumental gas concentration measurement procedures are used, conduct
the gas measurement system performance specifications checks as
described in Method 5H, Sections 6.7, 6.8, and 6.9. The zero drift and
calibration drift limits for all three analyzers shall be 0.2 percent
O2, CO2, or CO, as applicable, or less. Other measurement system
performance specifications are as defined in Method 5H, Section 4.
Sample at a constant rate for the duration of the test run.
5.3.1 Data Recording. Record wood heater operational data, test
facility temperature, sample train flow rate, and fuel weight data at
10-minute intervals.
5.3.2 Test Run Completion. Same as Method 28, Section 6.4.6.
5.4 Analysis Procedure.
5.4.1 Method 3 Integrated Bag Samples. Within 4 hours after the
sample collection, analyze each bag sample for percent CO2, O2, and CO
using an Orsat analyzer as described in Method 3, Sections 4.2.5 through
4.2.7.
5.4.2 Instrumental Analyzers. Average the percent CO2, CO, and O2
values for the test run.
5.5 Quality Control Procedures.
5.5.1 Data Validation. The following quality control procedure is
suggested to provide a check on the quality of the data.
5.5.1.1 Calculate a fuel factor, F0, using the following equation:
where:
%O2 Percent O2 by volume (dry basis).
%CO2 Percent CO2 by volume (dry basis).
20.9 Percent O2 by volume in ambient air.
If CO is present in quantities measurable by this method, adjust the
O2 and CO2 values before performing the calculation for F0 as follows:
%CO2 (adj) = %CO2 + %CO
%O2 (adj) = %O2 ^ 0.5 %CO
where:
%CO = Percent CO by volume (dry basis).
5.5.1.2 Compare the calculated F0 factor with the expected F0 range
for wood (1.000 - 1.120). Calculated F0 values beyond this acceptable
range should be investigated before accepting the test results. For
example, the strength of the solutions in the gas analyzer and the
analyzing technique should be checked by sampling and analyzing a known
concentration, such as air. If no detectable or correctable measurement
error can be identified, the test should be repeated. Alternatively,
determine a range of air to fuel ratio results that could include the
correct value by using an F0 value of 1.05 and calculating a potential
range of CO2 and O2 values. Acceptance of such results will be based on
whether the calculated range includes the exemption limit and the
judgment of the administrator.
5.5.1.3 Method 3 Analyses. Compare the results of the analyses of
the two bag samples. If all the gas components (O2, CO, and CO2) values
for the two analyses agree within 0.5 percent (e.g., 6.0 percent O2 for
bag 1 and 6.5 percent O2 for bag 2, agree within 0.5 percent), the
results of the bag analyses may be averaged for the calculations in
Section 6. If the analysis results do not agree within 0.5 percent for
each component, calculate the air-to-fuel ratio using both sets of
analyses and report the results.
Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figure after the final
calculation. Other forms of the equations may be used as long as they
give equivalent results.
6.1 Nomenclature.
Md=Dry molecular weight, g/g-mole(lb/lb-mole).
%CO2=Percent CO2 by volume (dry basis).
%O2=Percent O2 by volume (dry basis).
%CO=Percent CO by volume (dry basis).
%N2=Percent N2 by volume (dry basis).
NT=Total gram-moles of dry exhaust gas per kg of wood burned
(lb-moles/lb).
YCO2=Measured mole fraction of CO2 (e.g., 10 percent CO2=.10 mole
fraction), g/g-mole (lb/lb-mole).
YCO=Measured mole fraction of CO (e.g., 1 percent CO=.01 mole
fraction), g/g-mole (lb/lb-mole).
YHC=Assumed mole fraction of HC (dry as CH4)
=0.0088 for catalytic wood heaters; =0.0132 for noncatalytic wood
heaters. =0.0080 for pellet-fired wood heaters.
0.280=Molecular weight of N2 or CO, divided by 100.
0.320=Molecular weight of O2 divided by 100.
0.440=Molecular weight of CO2 divided by 100.
42.5=Gram-moles of carbon in 1 kg of dry wood assuming 51 percent
carbon by weight dry basis (.0425 lb/lb).
510=Grams of carbon in exhaust gas per kg of wood burned.
1,000=Grams in 1 kg.
6.2 Dry Molecular Weight. Use Equation 28a-1 to calculate the dry
molecular weight of the stack gas.
Md=0.440(%CO2)+0.320(%O)2)+0.280(%N2+%CO) Eq. 28a-1
Note: The above equation does not consider argon in air (about 0.9
percent, molecular weight of 37.7). A negative error of about 0.4
percent is introduced. The tester may opt to include argon in the
analysis using procedures subject to approval of the Administrator.
6.3 Dry Moles of Exhaust Gas. Use Equation 28a-2 to calculate the
total moles of dry exhaust gas produced per kilogram of dry wood burned.
Eq. 28a-2
6.4 Air to Fuel Ratio. Use Equation 28a-3 to calculate the air to
fuel ratio on a dry mass basis.
Eq. 28a-3
6.5 Burn Rate. Calculate the fuel burn rate as in Method 28, Section
8.3.
Same as Method 3, Section 7, and Method 5H, Section 7.
(36 FR 24877, Dec. 23, 1971)
Editorial Note: For Federal Register citations affecting part 60,
appendix A see the List of CFR Sections in the Finding Aids section of
this volume.
40 CFR 60.748 Appendix B -- Performance Specifications
Performance Specification 1 -- Specifications and test procedures for
opacity continuous emission monitoring systems in stationary sources
Performance Specification 2 -- Specifications and test procedures for
SO2 and NOx continuous emission monitoring systems in stationary sources
Performance Specification 3 -- Specifications and test procedures for
O2 and CO2 continuous emission monitoring systems in stationary sources
Performance Specification 4 -- Specifications and test procedures for
carbon monoxide continuous emission monitoring systems in stationary
sources
Performance Specification 4A -- Specifications and test procedures
for carbon monoxide continuous emission monitoring systems in stationary
sources
Performance Specification 5 -- Specifications and test procedures for
TRS continuous emission monitoring systems in stationary sources
Performance Specification 6 -- Specifications and test procedures for
continuous emission rate monitoring systems in stationary sources
Performance Specification 7 -- Specifications and test procedures for
hydrogen sulfide continuous emission monitoring systems in stationary
sources
40 CFR 60.748 Pt. 60, App. B, Spec. 1
1. Applicability and Principle
1.1 Applicability. This specification contains requirements for the
design, performance, and installation of instruments for opacity
continuous emission monitoring systems (CEMS's) and data computation
procedures for evaluating the acceptability of a CEMS. Certain design
requirements and test procedures established in this specification may
not apply to all instrument designs. In such instances, equivalent
design requirements and test procedures may be used with prior approval
of the Administrator.
Performance Specification 1 (PS 1) applies to opacity monitors
installed after March 30, 1983. Opacity monitors installed before March
30, 1983, are required to comply with the provisions and requirements of
PS 1 except for the following:
(a) Section 4. ''Installation Specifications.''
(b) Sections 5.1.4, 5.1.6, 5.1.7, and 5.1.8 of Section 5, ''Design
and Performance Specifications.''
(c) Section 6.4 of Section 6 ''Design Specifications Verification
Procedure.''
An opacity monitor installed before March 30, 1983, need not be
tested to demonstrate compliance with PS 1 unless required by regulatory
action other than the promulgation of PS 1. If an existing monitor is
replaced with a new monitor, PS 1 shall apply except that the new
monitor may be located at the old measurement location regardless of
whether the location meets the requirements of Section 4. If a new
measurement location is to be determined, the new location shall meet
the requirements of Section 4.
1.2 Principle. The opacity of particulate matter in stack emissions
is continuously monitored by a measurement system based upon the
principle of transmissometry. Light having specific spectral
characteristics is projected from a lamp through the effluent in the
stack or duct, and the intensity of the projected light is measured by a
sensor. The projected light is attenuated because of absorption and
scattered by the particulate matter in the effluent; the percentage of
visible light attenuated is defined as the opacity of the emission.
Transparent stack emissions that do not attenuate light will have a
transmittance of 100 percent or an opacity of zero percent. Opaque
stack emissions that attenuate all of the visible light will have a
transmittance of zero percent or an opacity of 100 percent.
This specification establishes specific design criteria for the
transmissometer system. Any opacity CEMS that is expected to meet this
specification is first checked to verify that the design specifications
are met. Then, the opacity CEMS is calibrated, installed, and operated
for a specified length of time. During this specified time period, the
system is evaluated to determine conformance with the established
performance specifications.
2. Definitions
2.1 Continuous Emission Monitoring System. The total equipment
required for the determination of opacity. The system consists of the
following major subsystems:
2.1.1 Sample Interface. That portion of CEMS that protects the
analyzer from the effects of the stack effluent and aids in keeping the
optical surfaces clean.
2.1.2 Analyzer. That portion of the CEMS that senses the pollutant
and generates an output that is a function of the opacity.
2.1.3 Data Recorder. That portion of the CEMS that provides a
permanent record of the analyzer output in terms of opacity. The data
recorder may include automatic data-reduction capabilities.
2.2 Transmissometer. That portion of the CEMS that includes the
sample interface and the analyzer.
2.3 Transmittance. The fraction of incident light that is transmitted
through an optical medium.
2.4 Opacity. The fraction of incident light that is attenuated by an
optical medium. Opacity (Op) and transmittance (Tr) are related by:
Op=1^Tr.
2.5 Optical Density. A logarithmic measure of the amount of incident
light attenuated. Optical density (D) is related to the transmittance
and opacity as follows:
D=^log10 Tr=^log10 (1-Op).
2.6 Peak Spectral Response. The wavelength of maximum sensitivity of
the transmissometer.
2.7 Mean Spectral Response. The wavelength that is the arithmetic
mean value of the wavelength distribution for the effective spectral
response curve of the transmissometer.
2.8 Angle of View. The angle that contains all of the radiation
detected by the photodetector assembly of the analyzer at a level
greater than 2.5 percent of the peak detector response.
2.9 Angle of Projection. The angle that contains all of the
radiation projected from the lamp assembly of the analyzer at a level of
greater than 2.5 percent of the peak illuminance.
2.10 Span Value. The opacity value at which the CEMS is set to
produce the maximum data display output as specified in the applicable
subpart.
2.11 Upscale Calibration Value. The opacity value at which a
calibration check of the CEMS is performed by simulating an upscale
opacity condition as viewed by the receiver.
2.12 Calibration Error. The difference between the opacity values
indicated by the CEMS and the known values of a series of calibration
attenuators (filters or screens).
2.13 Zero Drift. The difference in the CEMS output readings from the
zero calibration value after a stated period of normal continuous
operation during which no unscheduled maintenance, repair, or adjustment
took place. A calibration value of 10 percent opacity or less may be
used in place of the zero calibration value.
2.14 Calibration Drift. The difference in the CEMS output readings
from the upscale calibration value after a stated period of normal
continuous operation during which no unscheduled maintenance, repair, or
adjustment took place.
2.15 Response Time. The amount of time it takes the CEMS to display
on the data recorder 95 percent of a step change in opacity.
2.16 Conditioning Period. A period of time (168 hours minimum)
during which the CEMS is operated without any unscheduled maintenance,
repair, or adjustment prior to initiation of the operational test
period.
2.17 Operational Test Period. A period of time (168 hours) during
which the CEMS is expected to operate within the established performance
specifications without any unscheduled maintenance, repair, or
adjustment.
2.18 Path Length. The depth of effluent in the light beam between
the receiver and the transmitter of a single-pass transmissometer, or
the depth of effluent between the transceiver and reflector of a
double-pass transmissometer. Two path lengths are referenced by this
specification as follows:
2.18.1 Monitor Path Length. The path length (depth of effluent) at
the installed location of the CEMS.
2.18.2 Emission Outlet Path Length. The path length (depth of
effluent) at the location where emissions are released to the
atmosphere. For noncircular outlets, De=(2LW)'(L+W), where L is the
length of the outlet and W is the width of the outlet. Note that this
definition does not apply to pressure baghouse outlets with multiple
stacks, side discharge vents, ridge roof monitors, etc.
3. Apparatus
3.1 Opacity Continuous Emission Monitoring System. Any opacity CEMS
that is expected to meet the design and performance specifications in
Section 5 and a suitable data recorder, such as an analog strip chart
recorder or other suitable device (e.g., digital computer) with an input
signal range compatible with the analyzer output.
3.2 Calibration Attenuators. Minimum of three. These attenuators
must be optical filters or screens with neutral spectral characteristics
selected and calibrated according to the procedures in Sections 7.1.2
and 7.1.3, and of sufficient size to attenuate the entire light beam
received by the detector of the transmissometer.
3.3 Upscale Calibration Value Attenuator. An optical filter with
neutral spectral characteristics, a screen, or other device that
produces an opacity value (corrected for path length, if necessary) that
is greater than or equal to the applicable opacity standard but less
than or equal to one-half the applicable instrument span value.
3.4 Calibration Spectrophotometer. A laboratory spectrophotometer
meeting the following minimum design specifications:
4. Installation Specifications
Install the CEMS at a location where the opacity measurements are
representative of the total emissions from the affected facility. These
requirements can be met as follows:
4.1 Measurement Location. Select a measurement location that is (a)
downstream from all particulate control equipment, (b) where condensed
water vapor is not present, (c) free of interference from ambient light
(applicable only if transmissometer is responsive to ambient light), and
(d) accessible in order to permit routine maintenance. Accessibility is
an important criterion because easy access for lens cleaning, alignment
checks, calibration checks, and blower maintenance will help assure
quality data.
4.2 Measurement Path. The primary concern in locating a
transmissometer is determining a location of well-mixed stack gas. Two
factors contribute to complete mixing of emission gases: turbulence and
sufficient mixing time. The criteria listed below define conditions
under which well-mixed emissions can be expected.
Select a measurement path that passes through a centroidal area equal
to 25 percent of the cross section. Additional requirements or
modifications must be met for certain locations as follows:
4.2.1 If the location is in a straight vertical section of stack or
duct and is less than 4 equivalent diameters downstream from a bend, use
a path that is in the plane defined by the upstream bend (see Figure
1-1).
4.2.2 If the location is in a straight vertical section of stack or
duct and is less than 4 equivalent diameters upstream from a bend, use a
path that is in the plane defined by the bend (see Figure 1-2).
Insert illus.
ITT500000000 ED
Insert illus. 0036
4.2.3 If the location is in a straight vertical section of stack or
duct and is less than 4 diameters downstream and is also less than 1
diameter upstream from a bend, use a path in the plane defined by the
upstream bend (see Figure 1-3).
4.2.4 If the location is in a horizontal section of duct and is at
least 4 diameters downstream from a vertical bend, use a path in the
horizontal plane that is between one-third and one-half the distance up
the vertical axis from the bottom of the duct (see Figure 1-4).
4.2.5 If the location is in a horizontal section of duct and is less
than 4 diameters downstream from a vertical bend, use a path in the
horizontal plane that is between one-half and two-thirds the distance up
the vertical axis from the bottom of the duct for upward flow in the
vertical section, and is between one-third and one-half the distance up
the vertical axis from the bottom of the duct for downward flow (Figure
1-5).
4.3 Alternative Locations and Measurement Paths. Other locations and
measurement paths may be selected by demonstrating to the Administrator
that the average opacity measured at the alternative location or path is
equivalent to the opacity as measured at a location meeting the criteria
of Sections 4.1 and 4.2. The opacity at the alternative location is
considered equivalent if the average value measured at the alternative
location is within the range defined by the average measured opacity 10
percent at the location meeting the installation criteria in Section
4.2, or if the difference between the two average opacity values is less
than 2 percent opacity. To conduct this demonstration, measure the
opacities at the two locations or paths for a minimum period of 2 hours
and compare the results. The opacities of the two locations or paths
may be measured at different times, but must be measured at the same
process operating conditions. Alternative procedures for determining
acceptable locations may be used if approved by the Administrator.
Insert illus. 0 021
Insert illus. 0 022
Insert illus. 0 023
5. Design and Performance Specifications
5.1 Design Specifications. The CEMS for opacity shall comply with
the following design specifications:
5.1.1 Peak and Mean Spectral Responses. The peak and mean spectral
responses must occur between 500 nm and 600 nm. The response at any
wavelength below 400 nm or above 700 nm shall be less than 10 percent of
the peak spectral response.
5.1.2 Angle of View. The total angle of view shall be no greater
than 5 degrees.
5.1.3 Angle of Projection. The total angle of projection shall be no
greater than 5 degrees.
5.1.4 Optical Alignment Sight. Each analyzer must provide some
method for visually determining that the instrument is optically
aligned. The method provided must be capable of indicating that the
unit is misaligned when an error of +2 percent opacity occurs due to
misalignment at a monitor path length of 8 meters. Instruments that are
capable of providing an absolute zero check while in operation on a
stack or duct with effluent present, and while maintaining the same
optical alignment during measurement and calibration, need not meet this
requirement (e.g., some ''zero pipe'' units).
5.1.5 Simulated Zero and Upscale Calibration System. Each analyzer
must include a calibration system for simulating a zero (or no greater
than 10 percent) opacity and an upscale opacity value for the purpose of
performing periodic checks of the transmissometer calibration while on
an operating stack or duct. This calibration system will provide, as a
minimum, a system check of the analyzer internal optics and all
electronic circuitry including the lamp and photodetector assembly.
5.1.6 Access to External Optics. Each analyzer must provide a means
of access to the optical surfaces exposed to the effluent stream in
order to permit the surfaces to be cleaned without requiring removal of
the unit from the source mounting or without requiring optical
realignment of the unit.
5.1.7 Automatic Zero Compensation Indicator. If the CEMS has a
feature that provides automatic zero compensation for dirt accumulation
on exposed optical surfaces, the system must also provide some means of
indicating when a compensation of 4 percent opacity has been exceeded.
This indicator shall be at a location accessible to the operator (e.g.,
the data output terminal). During the operational test period, the
system must provide some means (manual or automated) for determining the
actual amount of zero compensation at the specified 24-hour intervals so
that the actual 24-hour zero drift can be determined (see Section
7.4.1).
5.1.8 Slotted Tube. For transmissometers that use slotted tubes, the
length of the slotted portion(s) must be equal to or greater than 90
percent of the effluent path length (distance between duct or stack
walls). The slotted tube must be of sufficient size and orientation so
as not to interfere with the free flow of effluent through the entire
optical volume of the transmissometer photodetector. The manufacturer
must also show that the transmissometer minimizes light reflections. As
a minimum, this demonstration shall consist of laboratory operation of
the transmissometer both with and without the slotted tube in position.
Should the operator desire to use a slotted tube design with a
slotted portion equal to or less than 90 percent of the monitor path
length, the operator must demonstrate to the Administrator that
acceptable results can be obtained. As a minimum demonstration, the
effluent opacity shall be measured using both the slotted tube
instrument and another instrument meeting the requirement of this
specification but not of the slotted tube design. The measurements must
be made at the same location and at the same process operating
conditions for a minimum period of 2 hours with each instrument. The
shorter slotted tube may be used if the average opacity measured is
equivalent to the opacity measured by the nonslotted tube design. The
average opacity measured is equivalent if it is within the opacity range
defined by the average opacity value 10 percent measured by the
nonslotted tube design, or if the difference between the average
opacities is less than 2 percent opacity.
5.1.9 External Calibration Filter Access (optional). Provisions in
the design of the transmissometer to accommodate an external calibration
filter assembly are recommended. An adequate design would permit
occasional use of external (i.e., not intrinsic to the instrument)
neutral density filters to assess monitor operation.
5.2 Performance Specifications. The opacity CEMS specifications are
listed in Table 1-1.
6. Design Specifications Verification Procedure
These procedures will not apply to all instrument designs and will
require modification in some cases; all procedural modifications are
subject to the approval of the Administrator.
Test each analyzer for conformance with the design specifications of
Sections 5.1.1-5.1.4, or obtain a certificate of conformance from the
analyzer manufacturer as follows:
6.1 Spectral Response. Obtain detector response, lamp emissivity,
and filter transmittance data for the components used in the measurement
system from their respective manufacturers, and develop the effective
spectral response curve of the transmissometer. Then determine and
report the peak spectral response wavelength, the mean spectral response
wavelength, and the maximum response at any wavelength below 400 nm and
above 700 nm expressed as a percentage of the peak response.
Alternatively, conduct a laboratory measurement of the instrument's
spectral response curve. The procedures of this laboratory evaluation
are subject to approval of the Administrator.
6.2 Angle of View. Set up the receiver as specified by the
manufacturer's written instructions. Draw an arc with radius of 3
meters in the horizontal direction. Using a small (less than 3
centimeters) nondirectional light source, measure the receiver response
at 5-centimeter intervals on the arc for 30 centimeters on either side
of the detector centerline. Repeat the test in the vertical direction.
Then for both the horizontal and vertical directions, calculate the
response of the receiver as a function of viewing angle (26 centimeters
of arc with a radius of 3 meters equals 5 degrees), report relative
angle of view curves, and determine and report the angle of view.
6.3 Angle of Projection. Set up the projector as specified by the
manufacturer's written instructions. Draw an arc with a radius of 3
meters in the horizontal direction. Using a small (less than 3
centimeters) photoelectric light detector, measure the light intensity
at 5-centimeter intervals on the arc for 30 centimeters on either side
of the light source centerline of projection. Repeat the test in the
vertical direction. Then for both the horizontal and vertical
directions, calculate the response of the photoelectric detector as a
function of the projection angle (26 centimeters of arc with a radius of
3 meters equals 5 degrees), report the relative angle of projection
curves, and determine and report the angle of projection.
6.4 Optical Alignment Sight. In the laboratory set the instrument up
as specified by the manufacturer's written instructions for a monitor
path length of 8 meters. Align, zero, and span the instrument. Insert
an attenuator of 10 percent (nominal opacity) into the instrument path
length. Slowly misalign the projector unit by rotating it until a
positive or negative shift of 2 percent opacity is obtained by the data
recorder. Then, following the manufacturer's written instructions,
check the alignment. The alignment procedure must indicate that the
instrument is misaligned. Repeat this test for lateral misalignment of
the projector. Realign the instrument and follow the same procedure for
checking misalignment of the receiver or retroreflector unit (lateral
misalignment only).
6.5 Manufacturer's Certificate of Conformance (alternative to above).
Obtain from the manufacturer a certificate of conformance stating that
the first analyzer randomly sampled from each month's production was
tested according to Sections 6.1 through 6.4 and satisfactorily met all
requirements of Section 5 of this specification. If any of the
requirements were not met, the certificate must state that the entire
month's analyzer production was resampled according to the military
standard 105D sampling procedure (MIL-STD-105D) inspection level II;
was retested for each of the applicable requirements under Section 5 of
this specification; and was determined to be acceptable under
MIL-STD-105D procedures, acceptable quality level 1.0. The certificate
of conformance must include the results of each test performed for the
analyzer(s) sampled during the month the analyzer being installed was
produced.
7. Performance Specification Verification Procedure
Test each CEMS that conforms to the design specifications (Section
5.1) using the following procedures to determine conformance with the
specifications of Table 1-1. These tests are to be performed using the
data recording system to be employed during monitoring. Prior approval
from the Administrator is required if different data recording systems
are used during the performance test and monitoring.
7.1 Preliminary Adjustments and Tests. Before installing the system
on the stack, perform these steps or tests at the affected facility or
in the manufacturer's laboratory.
7.1.1 Equipment Preparation. Set up and calibrate the CEMS for the
monitor path length to be used in the installation as specified by the
manufacturer's written instructions. For this specification, the
mounting distance between the transmitter and receiver/reflector unit at
the source must be measured prior to performing the calibrations (do not
use distances from engineering drawings). If the CEMS has automatic
path length adjustment, follow the manufacturer's instructions to adjust
the signal output from the analyzer in order to yield results based on
the emission outlet path length. Set the instrument and data recording
system ranges so that maximum instrument output is within the span range
specified in the applicable subpart.
Align the instrument so that maximum system response is obtained
during a zero (or upscale) check performed across the simulated monitor
path length. As part of this alignment, include rotating the reflector
unit (detector unit for single pass instruments) on its axis until the
point of maximum instrument response is obtained.
Follow the manufacturer's instructions to zero and span the
instrument. Perform the zero alignment adjustment by balancing the
response of the CEMS so that the simulated zero check coincides with the
actual zero check performed across the simulated monitor path length.
At this time, measure and record the indicated upscale calibration
value. The calibration value reading must be within the required
opacity range (Section 3.3).
7.1.2 Calibration Attenuator Selection. Based on the span value
specified in the applicable subpart, select a minimum of three
calibration attenuators (low, mid, and high range) using Table 1-2.
If the system is operating with automatic path length compensation,
calculate the attenuator values required to obtain a system response
equivalent to the applicable values shown in Table 1-2; use Equation
1-1 for the conversion. A series of filters with nominal optical
density (opacity) values of 0.1(20), 0.2(37), 0.3(50), 0.4(60), 0.5(68),
0.6(75), 0.7(80), 0.8(84), 0.9(88), and 1.0(90) are commercially
available. Within this limitation of filter availability, select the
calibration attenuators having the values given in Table 1-2 or having
values closest to those calculated by Equation 1-1.
Where:
D1=Nominal optical density value of required mid, low, or high range
calibration attenuators.
D2=Desired attenuator optical density output value from Table 1-2 at
the span required by the applicable subpart.
L1=Monitor path length.
L2=Emission outlet path length.
7.1.3 Attenuator Calibration. Select a laboratory calibration
spectrophotometer meeting the specifications of Section 3.4. Using this
calibration spectrophotometer, calibrate the required filters or
screens. Make measurements at wavelength intervals of 20 nm or less.
As an alternative procedure, use the calibration spectrophotometer to
measure the C.I.E. DaylightC luminous transmittance of the attenuators.
Check the attenuators several times, at different locations on the
attenuator.
The attenuator manufacturer must specify the period of time over
which the attenuator values can be considered stable, as well as any
special handling and storing procedures required to enhance attenuator
stability. To assure stability, recheck attenuator values at intervals
less than or equal to the period stability guaranteed by the
manufacturer. Recheck at least every 3 months. If desired, perform the
stability checks with an instrument (secondary) other than the
calibration spectrophotometer. This secondary instrument must be a
high-quality laboratory transmissometer or spectrophotometer, and the
same instrument must always be used for the stability checks. If a
secondary instrument is to be used for stability checks, the value of
the calibrated attenuator must be measured on this secondary instrument
immediately following initial calibration. If over a period of time an
attenuator value changes by more than 2 percent opacity, recalibrate
the attenuator on the calibration spectrophotometer or replace it with a
new attenuator.
If this procedure is conducted by the filter or screen manufacturer
or by an independent laboratory, obtain a statement certifying the
values and certifying that the specified procedure, or equivalent, is
used.
7.1.4 Calibration Error Test. Insert the calibration attenuators
(low, mid, and high range) in the transmissometer path at or as near the
midpoint of the path as feasible. Place the attenuator in the
measurement path at a point where the effluent will be measured; i.e.,
do not place the calibration attenuator in the instrument housing. If
the instrument manufacturer recommends a procedure wherein the
attenuators are placed in the instrument housing, the manufacturer must
provide data showing this alternative procedure is acceptable. While
inserting the attenuator, assure that the entire beam received by the
detector will pass through the attenuator and that the attenuator is
inserted in a manner which minimizes interference from reflected light.
Make a total of five nonconsecutive readings for each filter. Record
the monitoring system output readings in percent opacity (see example
Figure 1-6). Then, if the path length is not adjusted by the
measurement system, subtract the actual calibration attenuator value
from the value indicated by the measurement system recorder for each of
the 15 readings obtained. If the path length is adjusted by the
measurement system, subtract the ''path adjusted'' calibration
attenuator values from the values indicated by the measurement system
recorder (the ''path adjusted'' calibration attenuator values are
calculated using Equation 1-6 or 1-7). Calculate the arithmetic mean
difference, standard deviation, and confidence coefficient of the five
tests at each attenuator value using Equations 1-2, 1-3, and 1-4
(Sections 8.1-8.3). Calculate the sum of the absolute value of the mean
difference and the absolute value of the confidence coefficient for each
of the three test attenuators; report these three values as the
calibration error.
Insert illus. 0053
7.1.5 System Response Test. Insert the high-range calibration
attenuator in the transmissometer path five times, and record the time
required for the system to respond to 95 percent of final zero and
high-range filter values (see example Figure 1-7). Then calculate the
mean time of the 10 upscale and downscale tests and report this value as
the system response time.
Insert illus. 0055
7.2 Preliminary Field Adjustments. Install the CEMS on the affected
facility according to the manufacturer's written instructions and the
specifications in Section 4, and perform the following preliminary
adjustments:
7.2.1 Optical and Zero Alignment. When the facility is not in
operation, optically align the light beam of the transmissometer upon
the optical surface located across the duct or stack (i.e., the
retroreflector or photodetector, as applicable) in accordance with the
manufacturer's instructions; verify the alignment with the optical
alignment sight. Under clear stack conditions, verify the zero
alignment (performed in Section 7.1.1) by assuring that the monitoring
system response for the simulated zero check coincides with the actual
zero measured by the transmissometer across the clear stack. Adjust the
zero alignment, if necessary. Then, after the affected facility has
been started up and the effluent stream reaches normal operating
temperature, recheck the optical alignment. If the optical alignment
has shifted, realign the optics. Note: Careful consideration should be
given to whether a ''clear stack'' condition exists. It is suggested
that the stack be monitored and the data output (instantaneous real-time
basis) be examined to determine whether fluctuations from zero opacity
are occurring before a clear stack condition is assumed to exist.
7.2.2 Optical and Zero Alignment (Alternative Procedure). The
procedure given in 7.2.1 is the preferred procedure and should be used
whenever possible; however, if the facility is operating and a zero
stack condition cannot practicably be obtained, use the zero alignment
obtained during the preliminary adjustments (Section 7.1.1) before
installing the transmissometer on the stack. After completing all the
preliminary adjustments and tests required in Section 7.1, install the
system at the source and align the optics, i.e., align the light beam
from the transmissometer upon the optical surface located across the
duct or stack in accordance with the manufacturer's instruction. Verify
the alignment with the optical alignment sight. The zero alignment
conducted in this manner must be verified and adjusted, if necessary,
the first time a clear stack condition is obtained after the operation
test period has been completed.
7.3 Conditioning Period. After completing the preliminary field
adjustments (Section 7.2), operate the CEMS according to the
manufacturer's instructions for an initial conditioning period of not
less than 168 hours while the source is operating. Except during times
of instrument zero and upscale calibration checks, the CEMS must analyze
the effluent gas for opacity and produce a permanent record of the CEMS
output. During this conditioning period there must be no unscheduled
maintenance, repair, or adjustment. Conduct daily zero calibration and
upscale calibration checks; and, when accumulated drift exceeds the
daily operating limits, make adjustments and clean the exposed optical
surfaces. The data recorder must reflect these checks and adjustments.
At the end of the operational test period, verify that the instrument
optical alignment is correct. If the conditioning period is interrupted
because of source breakdown (record the dates and times of process
shutdown), continue the 168-hour period following resumption of source
operation. If the conditioning period is interrupted because of monitor
failure, restart the 168-hour conditioning period when the monitor
becomes operational.
7.4 Operational Test Period. After completing the conditioning
period, operate the system for an additional 168-hour period. The
168-hour operational test period need not follow immediately after the
168-hour conditioning period. Except during times of instrument zero
and upscale calibration checks, the CEMS must analyze the effluent gas
for opacity and must produce a permanent record of the CEMS output.
During this period, there will be no unscheduled maintenance, repair, or
adjustment. Zero and calibration adjustments, optical surface cleaning,
and optical realignment may be performed (optional) only at 24-hour
intervals or at such shorter intervals as the manufacturer's written
instructions specify. Automatic zero and calibration adjustments made
by the CEMS without operator intervention or initiation are allowable at
any time. During the operational test period, record all adjustments,
realignments, and lens cleanings. If the operational test period is
interrupted because of source breakdown, continue the 168-hour period
following resumption of source operation. If the test period is
interrupted because of monitor failure, restart the 168-hour period when
the monitor becomes operational. During the operational test period,
perform the following test procedures:
7.4.1. Zero Drift Test. At the outset of the 168-hour operational
test period, record the initial simulated zero (or no greater than 10
percent) and upscale opacity readings (see example Figure 1-8). After
each 24-hour interval, check and record the final zero reading before
any optional or required cleaning and adjustment. Zero and upscale
calibration adjustments, optical surface cleaning, and optical
realignment may be performed only at 24-hour intervals (or at such
shorter intervals as the manufacturer's written instructions specify),
but are optional. However, adjustments and cleaning must be performed
when the accumulated zero calibration or upscale calibration drift
exceeds the 24-hour drift specification ( 2 percent opacity). If no
adjustments are made after the zero check, record the final zero reading
as the initial zero reading for the next 24-hour period. If adjustments
are made, record the zero value after adjustment as the initial zero
value for the next 24-hour period. If the instrument has an automatic
zero compensation feature for dirt accumulation on exposed lenses and
the zero value cannot be measured before compensation is entered, then
record the amount of automatic zero compensation (as opacity) for the
final zero reading of each 24-hour period. (List the indicated zero
values of the CEMS in parenthesis.) From the initial and final zero
readings, calculate the zero drift for each 24-hour period. Then
calculate the arithmetic mean, standard deviation, and confidence
coefficient of the 24-hour zero drift and the 95 percent confidence
interval using Equations 1-2, 1-3, and 1-4. Calculate the sum of the
absolute value of the mean and the absolute value of the confidence
coefficient, and report this value as the 24-hour zero drift.
Insert illus. 0059
7.4.2 Upscale Drift Test. At each 24-hour interval, after the zero
calibration value has been checked and any optional or required
adjustments have been made, check and record the simulated upscale
calibration value. If no further adjustments are made to the
calibration system at this time, record the final upscale calibration
value as the initial upscale value for the next 24-hour period. If an
instrument span adjustment is made, record the upscale value after
adjustment as the initial upscale value for the next 24-hour period.
From the initial and final upscale readings, calculate the upscale
calibration drift for each 24-hour period. Then calculate the
arithmetic mean, standard deviation, and confidence coefficient of the
24-hour calibration drift and the 95 percent confidence interval using
Equations 1-2, 1-3, and 1-4. Calculate the sum of the absolute value of
the mean and the absolute value of the confidence coefficient, and
report this value as the 24-hour calibration drift.
8. Equations
8.1 Arithmetic Mean. Calculate the mean, x8, of a set of data as
follows:
insert illus 0062A
where:
n=Number of data points.
8.2 Standard Deviation. Calculate the standard deviation Sd as
follows:
insert illus 0062C
8.3 Confidence Coefficient. Calculate the 2.5 percent error
confidence coefficient (one-tailed), CC, as follows:
insert illus 0062D
Where:
t0.975=t-value (see Table 1-3).
8.4 Error. Calculate the error (i.e., calibration error, zero drift,
and calibration drift), Er, as follows:
insert illus 0062E
8.5 Conversion of Opacity Values from Monitor Path Length to Emission
Outlet Path Length. When the monitor path length is different than the
emission outlet path length, use either of the following equations to
convert from one basis to the other (this conversion may be
automatically calculated by the monitoring system):
log(1-Op2)=(L2/L1) log (1-Op1)
(Eq. 1-6)
D2=(L2/L1) D1 (Eq. 1-7)
Where:
Op1 = Opacity of the effluent based upon L1.
Op2 = Opacity of the effluent based upon L2.
L1 = Monitor path length.
L2 = Emission outlet path length.
D1 = Optical density of the effluent based upon L1.
D2 = Optical density of the effluent based upon L2.
9. Reporting
Report the following (summarize in tabular form where appropriate).
9.1 General Information.
a. Facility being monitored.
b. Person(s) responsible for operational and conditioning test
periods and affiliation.
c. Instrument manufacturer.
d. Instrument model number
e. Instrument serial number.
f. Month/year manufactured.
g. Schematic of monitoring system measurement path location.
h. Monitor pathlength, meters.
i. Emission outlet pathlength, meters.
j. System span value, percent opacity.
k. Upscale calibration value, percent opacity.
l. Calibrated Attenuator values (low, mid, and high range), percent
opacity.
9.2 Design Specification Test Results.
a. Peak spectral response, nm.
b. Mean spectral response, nm.
c. Response above 700 nm, percent of peak.
d. Response below 400 nm, percent of peak.
e. Total angle of view, degrees.
f. Total angle of projection, degrees.
g. Results of optical alignment sight test.
h. Serial number, month/year of manufacturer for unit actually tested
to show design conformance.
9.3 Performance Specification Test Results.
a. Calibration error, high-range, percent opacity.
b. Calibration error, mid-range, percent opacity.
c. Calibration error, low-range, percent opacity.
d. Response time, seconds.
e. 24-hour zero drift, percent opacity.
f. 24-hour calibration drift, percent opacity.
g. Lens cleanings, clock time.
h. Optical alignment adjustments, clock time.
9.4 Statements. Provide a statement that the conditioning and
operational test periods were completed according to the requirements of
Sections 7.3 and 7.4. In this statement, include the time periods during
which the conditioning and operational test periods were conducted.
9.5 Appendix. Provide the data tabulations and calculations for the
above tabulated results.
10. Retest
If the CEMS operates within the specified performance parameters of
Table 1-1, the PS tests will be successfully concluded. If the CEMS
fails one of the preliminary tests, make the necessary corrections and
repeat the performance testing for the failed specification prior to
conducting the operational test period. If the CEMS fails to meet the
specifications for the operational test period, make the necessary
corrections and repeat the operational test period; depending on the
correction made, it may be necessary to repeat the design and
preliminary performance tests.
11. Bibliography
1. Experimental Statistics. Department of Commerce. National Bureau
of Standards Handbook 91. Paragraph 3-3.1.4 1963. pp. 3-31.
12. Performance Specifications for Stationary-Source Monitoring
Systems for Gases and Visible Emissions. U.S. Environmental Protection
Agency. Research Triangle Park, NC. EPA-650/2-74-013. January 1974.
1. Applicability and Principle
40 CFR 60.748 Pt. 60, App. B, Spec. 2
1.1 Applicability. This specification is to be used for evaluating
the acceptability of SO2 and NOx continuous emission monitoring systems
(CEMS's) at the time of or soon after installation and whenever
specified in the regulations. The CEMS may include, for certain
stationary sources, a diluent (O2 or CO2 ) monitor.
This specification is not designed to evaluate the installed CEMS
performance over an extended period of time nor does it identify
specific calibration techniques and other auxiliary procedures to assess
the CEMS performance. The source owner or operator, however, is
responsible to properly calibrate, maintain, and operate the CEMS. To
evaluate the CEMS performance, the Administrator may require, under
Section 114 of the Act, the operator to conduct CEMS performance
evaluations at other times besides the initial test. See 60.13(c).
1.2 Principle. Installation and measurement location specifications,
performance and equipment specifications, test procedures, and data
reduction procedures are included in this specification. Reference
method tests and calibration drift tests are conducted to determined
conformance of the CEMS with the specification.
2. Definitions
2.1 Continuous Emission Monitoring System. The total equipment
required for the determination of a gas concentration or emission rate.
The system consists of the following major subsystems:
2.1.1 Sample Interface. That portion of the CEMS used for one or
more of the following: sample acquisition, sample transportation, and
sample conditioning, or protection of the monitor from the effects of
the stack effluent.
2.1.2 Pollutant Analyzer. That portion of the CEMS that senses the
pollutant gas and generates an output proportional to the gas
concentration.
2.1.3 Diluent Analyzer (if applicable). That portion of the CEMS
that senses the diluent gas (e.g., CO2 or O2) and generates an output
proportional to the gas concentration.
2.1.4 Data Recorder. That portion of the CEMS that provides a
permanent record of the analyzer output. The data recorder may include
automatic data reduction capabilities.
2.2 Point CEMS. A CEMS that measures the gas concentration either at
a single point or along a path equal to or less than 10 percent of the
equivalent diameter of the stack or duct cross section.
2.3 Path CEMS. A CEMS that measures the gas concentration along a
path greater than 10 percent of the equivalent diameter of the stack or
duct cross section.
2.4 Span Value. The upper limit of a gas concentration measurement
range specified for affected source categories in the applicable subpart
of the regulations.
2.5 Relative Accuracy (RA). The absolute mean difference between the
gas concentration or emission rate determined by the CEMS and the value
determined by the RM's plus the 2.5 percent error confidence coefficient
of a series of tests divided by the mean of the RM tests or the
applicable emission limit.
2.6 Calibration Drift (CD). The difference in the CEMS output
readings from the established reference value after a stated period of
operation during which no unscheduled maintenance, repair, or adjustment
took place.
2.7 Centroidal Area. A concentric area that is geometrically similar
to the stack or duct cross section and is no greater than 1 percent of
the stack or duct cross-sectional area.
2.8 Representative Results. As defined by the RM test procedure
outlined in this specification.
3. Installation and Measurement Location Specifications
3.1 The CEMS Installation and Measurement Location. Install the CEMS
at an accessible location where the pollutant concentration or emission
rate measurements are directly representative or can be corrected so as
to be representative of the total emissions from the affected facility
or at the measurement location cross section. Then select
representative measurement points or paths for monitoring in locations
that the CEMS will pass the RA test (see Section 7). If the cause of
failure to meet the RA test is determined to be the measurement location
and a satisfactory correction technique cannot be established, the
Administrator may require the CEMS to be relocated.
Suggested measurement locations and points or paths that are most
likely to provide data that will meet the RA requirements are listed
below.
3.1.1 Measurement Location. It is suggested that the measurement
location be (1) at least two equivalent diameters downstream from the
nearest control device, the point of pollutant generation, or other
point at which a change in the pollutant concentration or emission rate
may occur and (2) at least a half equivalent diameter upstream from the
effluent exhaust or control device.
3.1.2. Point CEMS. It is suggested that the measurement point be (1)
no less than 1.0 meter from the stack or duct wall or (2) within or
centrally located over the centroidal area of the stack or duct cross
section.
3.1.3 Path CEMS. It is suggested that the effective measurement path
(1) be totally within the inner area bounded by a line 1.0 meter from
the stack or duct wall, or (2) have at least 70 percent of the path
within the inner 50 percent of the stack or duct cross-sectional area,
or (3) be centrally located over any part of the centroidal area.
3.2 Reference Method (RM) Measurement Location and Traverse Points.
Select, as appropriate, an accessible RM measurement point at least two
equivalent diameters downstream from the nearest control device, the
point of pollutant generation, or other point at which a change in the
pollutant concentration or emission rate may occur, and at least a half
equivalent diameter upstream from the effluent exhaust or control
device. When pollutant concentration changes are due solely to diluent
leakage (e.g., air heater leakages) and pollutants and diluents are
simultaneously measured at the same location, a half diameter may be
used in lieu of two equivalent diameters. The CEMS and RM locations
need not be the same.
Then select traverse points that assure acquisition of representative
samples over the stack or duct cross section. The minimum requirements
are as follows: Establish a ''measurement line'' that passes through
the centroidal area and in the direction of any expected stratification.
If this line interferes with the CEMS measurements, displace the line
up to 30 cm (or 5 percent of the equivalent diameter of the cross
section, whichever is less) from the centroidal area. Locate three
traverse points at 16.7, 50.0, and 83.3 percent of the measurement line.
If the measurement line is longer than 2.4 meters and pollutant
stratification is not expected, the tester may choose to locate the
three traverse points on the line at 0.4, 1.2, and 2.0 meters from the
stack or duct wall. This option must not be used after wet scrubbers or
at points where two streams with different pollutant concentrations are
combined. The tester may select other traverse points, provided that
they can be shown to the satisfaction of the Administrator to provide a
representative sample over the stack or duct cross section. Conduct all
necessary RM tests within 3 cm (but no less than 3 cm from the stack or
duct wall) of the traverse points.
4. Performance and Equipment Specifications
4.1 Data Recorder Scale. The CEMS data recorder response range must
include zero and a high-level value. The high-level value is chosen by
the source owner or operator and is defined as follows:
For a CEMS intended to measure an uncontrolled emission (e.g., SO2
measurements at the inlet of a flue gas desulfurization unit), the
high-level value must be between 1.25 and 2 times the average potential
emission level, unless otherwise specified in an applicable subpart of
the regulations. For a CEMS installed to measure controlled emissions
or emissions that are in compliance with an applicable regulation, the
high-level value must be between 1.5 times the pollutant concentration
corresponding to the emission standard level and the span value. If a
lower high-level value is used, the source must have the capability of
measuring emissions which exceed the full-scale limit of the CEMS in
accordance with the requirements of applicable regulations.
The data recorder output must be established so that the high-level
value is read between 90 and 100 percent of the data recorder full
scale. (This scale requirement may not be applicable to digital data
recorders.) The calibration gas, optical filter, or cell values used to
establish the data recorder scale should produce the zero and high-level
values. Alternatively, a calibration gas, optical filter, or cell value
between 50 and 100 percent of the high-level value may be used in place
of the high-level value provided the data recorder full-scale
requirements as described above are met.
The CEMS design must also allow the determination of calibration
drift at the zero and high-level values. If this is not possible or
practical, the design must allow these determinations to be conducted at
a low-level value (zero to 20 percent of the high-level value) and at a
value between 50 and 100 percent of the high-level value. In special
cases, if not already approved, the Administrator may approve a
single-point calibration-drift determination.
4.2 Calibration Drift. The CEMS calibration must not drift or
deviate from the reference value of the gas cylinder, gas cell, or
optical filter by more than 2.5 percent of the span value. If the CEMS
includes pollutant and diluent monitors, the calibration drift must be
determined separately for each in terms of concentrations (see PS 3 for
the diluent specifications).
4.3 The CEMS RA. The RA of the CEMS must be no greater than 20
percent of the mean value of the RM test data in terms of the units of
the emission standard or 10 percent of the applicable standard,
whichever is greater. For SO2 emission standards between 130 and 86
ng/J (0.30 and 0.20 lb/million Btu), use 15 percent of the applicable
standard; below 86 ng/J (0.20 lb/million Btu), use 20 percent of
emission standard.
5. Performance Specification Test Procedure
5.1 Pretest Preparation. Install the CEMS, prepare the RM test site
according to the specifications in Section 3, and prepare the CEMS for
operation according to the manufacturer's written instructions.
5.2 Calibration Drift Test Period. While the affected facility is
operating at more than 50 percent of normal load, or as specified in an
applicable subpart, determine the magnitude of the calibration drift
(CD) once each day (at 24-hour intervals) for 7 consecutive days
according to the procedure given in Section 6. To meet the requirement
of Section 4.2, none of the CD's must exceed the specification.
5.3 RA Test Period. Conduct the RA test according to the procedure
given in Section 7 while the affected facility is operating at more than
50 percent or normal load, or as specified in an applicable subpart. To
meet the specifications, the RA must be equal to or less than 20 percent
of the mean value of the RM test data in terms of the units of the
emission standard or 10 percent of the applicable standard, whichever is
greater. For instruments that use common components to measure more
than one effluent gas constituent, all channels must simultaneously pass
the RA requirement, unless it can be demonstrated that any adjustments
made to one channel did not affect the others.
The RA test may be conducted during the CD test period.
6. The CEMS Calibration Drift Test Procedure
The CD measurement is to verify the ability of the CEMS to conform to
the established CEMS calibration used for determining the emission
concentration or emission rate. Therefore, if periodic automatic or
manual adjustments are made to the CEMS zero and calibration settings,
conduct the CD test immediately before these adjustments, or conduct it
in such a way that the CD can be determined.
Conduct the CD test at the two points specified in Section 4.1.
Introduce to the CEMS the reference gases, gas cells, or optical filters
(these need not be certified). Record the CEMS response and subtract
this value from the reference value (see example data sheet in Figure
2-1).
7. Relative Accuracy Test Procedure
7.1 Sampling Strategy for RM Tests. Conduct the RM tests in such a
way that they will yield results representative of the emissions from
the source and can be correlated to the CEMS data. Although it is
preferable to conduct the diluent (if applicable), moisture (if needed),
and pollutant measurements simultaneously, the diluent and moisture
measurements that are taken within a 30- to 60-minute period, which
includes the pollutant measurements, may be used to calculate dry
pollutant concentration and emission rate.
In order to correlate the CEMS and RM data properly, mark the
beginning and end of each RM test period of each run (including the
exact time of the day) on the CEMS chart recordings or other permanent
record of output. Use the following strategies for the RM tests:
7.1.1 For integrated samples, e.g., Method 6 and Method 4, make a
sample traverse of at least 21 minutes, sampling for 7 minutes at each
traverse point.
7.1.2 For grab samples, e.g., Method 7, take one sample at each
traverse point, scheduling the grab samples so that they are taken
simultaneously (within a 3-minute period) or are an equal interval of
time apart over a 21-minute (or less) period. A test run for grab
samples must be made up of at least three separate measurements.
Note: At times, CEMS RA tests are conducted during new source
performance standards performance tests. In these cases, RM results
obtained during CEMS RA tests may be used to determine compliance as
long as the source and test conditions are consistent with the
applicable regulations.
7.2 Correlation of RM and CEMS Data. Correlate the CEMS and the RM
test data as to the time and duration by first determining from the CEMS
final output (the one used for reporting) the integrated average
pollutant concentration or emission rate for each pollutant RM test
period. Consider system response time, if important, and confirm that
the pair of results are on a consistent moisture, temperature, and
diluent concentration basis. Then, compare each integrated CEMS value
against the corresponding average RM value. Use the following
guidelines to make these comparisons.
7.2.1 If the RM has an integrated sampling technique, make a direct
comparison of the RM results and CEMS integrated average value.
7.2.2 If the RM has a grab sampling technique, first average the
results from all grab samples taken during the test run and then compare
this average value against the integrated value obtained from the CEMS
chart recording or output during the run. If the pollutant
concentration is varying with time over the run, the tester may choose
to use the arithmetic average of the CEMS value recorded at the time of
each grab sample.
7.3 Number of RM Tests. Conduct a minimum of nine sets of all
necessary RM tests. Conduct each set within a period of 30 to 60
minutes.
Note: The tester may choose to perform more than nine sets of RM
tests. If this option is chosen, the tester may, at his discretion,
reject a maximum of three sets of the test results so long as the total
number of test results used to determine the RA is greater than or equal
to nine, but he must report all data including the rejected data.
7.4 Reference Methods. Unless otherwise specified in an applicable
subpart of the regulations, Methods 3B, 4, 6, and 7, or their approved
alternatives, are the reference methods for diluent (O2 and CO2),
moisture, SO2, and NOx, respectively.
7.5 Calculations. Summarize the results on a data sheet. An example
is shown in Figure 2-2. Calculate the mean of the RM values. Calculate
the arithmetic differences between the RM and the CEMS output sets.
Then calculate the mean of the difference, standard deviation,
confidence coefficient, and CEMS RA, using Equations 2-1, 2-2, 2-3, and
2-4.
8. Equations
8.1 Arithmetic Mean. Calculate the arithmetic mean of the
difference, d, of a data set as follows:
Insert Illus. 1A
Where:
n=Number of data points.
Insert Illus. 2A
When the mean of the differences of pairs of data is calculated, be
sure to correct the data for moisture, if applicable.
8.2 Standard Deviation. Calculate the standard deviation, Sd, as
follows:
Insert Illus. 3A
8.3 Confidence Coefficient. Calculate the 2.5 percent error
confidence coefficient (one-tailed), CC, as follows:
Insert Illus. 4A
Where:
t0.975=t-value (see Table 2-1)
8.4 Relative Accuracy. Calculate the RA of a set of data as follows:
Insert Illus. 5A
Where:
|d8|=Absolute value of the mean of differences (from Equation 2-1).
|CC|=Absolute value of the confidence coefficient (from Equation
2-3).
R8M8=Average RM value or applicable standard.
9. Reporting
At a minimum (check with the appropriate regional office, or State,
or local agency for additional requirements, if any) summarize in
tabular form the results of the CD tests and the relative accuracy tests
or alternative RA procedure as appropriate. Include all data sheets,
calculations, charts (records of CEMS responses), cylinder gas
concentration certifications, and calibration cell response
certifications (if applicable), necessary to substantiate that the
performance of the CEMS met the performance specifications.
10. Alternative Procedures
10.1 Alternative to Relative Accuracy Procedure in section 7.
Paragraphs 60.13(j) (1) and (2) contain criteria for which the reference
method relative accuracy may be waived and the following procedure
substituted.
10.1.1 Conduct a complete CEMS status check following the
manufacturer's written instructions. The check should include operation
of the light source, signal receiver, timing mechanism functions, data
acquisition and data reduction functions, data recorders, mechanically
operated functions (mirror movements, zero pipe operation, calibration
gas valve operations, etc.), sample filters, sample line heaters,
moisture traps, and other related functions of the CEMS, as applicable.
All parts of the CEMS shall be functioning properly before proceeding to
the alternative RA procedure.
10.1.2 Challenge each monitor (both pollutant and diluent, if
applicable) with cylinder gases of known concentrations or calibration
cells that produce known responses at two measurement points within the
following ranges:
Use a separate cylinder gas or calibration cell for measurement
points 1 and 2. Challenge the CEMS and record the responses three times
at each measurement point. Do not dilute gas from a cylinder when
challenging the CEMS. Use the average of the three responses in
determining relative accuracy.
Operate each monitor in its normal sampling mode as nearly as
possible. When using cylinder gases, pass the cylinder gas through all
filters, scrubbers, conditioners, and other monitor components used
during normal sampling and as much of the sampling probe as practical.
When using calibration cells, the CEMS components used in the normal
sampling mode should not be by-passed during the RA determination.
These include light sources, lenses, detectors, and reference cells.
The CEMS should be challenged at each measurement point for a sufficient
period of time to assure adsorption-desorption reactions on the CEMS
surfaces have stabilized.
Use cylinder gases that have been certified by comparison to National
Bureau of Standards (NBS) gaseous standard reference material (SRM) or
NBS/EPA-approved gas manufacturer's certified reference material (CRM)
(See Citation 2 in the Bibliography) following EPA traceability protocol
Number 1 (See Citation 3 in the Bibliography). As an alternative to
protocol Number 1 gases, CRM's may be used directly as alternative RA
cylinder gases. A list of gas manufacturers that have prepared approved
CRM's is available from EPA at the address shown in Citation 2.
Procedures for preparation of CRM are described in Citation 2.
Use calibration cells certified by the manufacturer to produce a
known response in the CEMS. The cell certification procedure shall
include determination of CEMS response produced by the calibration cell
in direct comparison with measurement of gases of known concentration.
This can be accomplished using SRM or CRM gases in a laboratory source
simulator or through extended tests using reference methods at the CEMS
location in the exhaust stack. These procedures are discussed in
Citation 4 in the Bibliography. The calibration cell certification
procedure is subject to approval of the Administrator.
10.1.3 The differences between the known concentrations of the
cylinder gases and the concentrations indicated by the CEMS are used to
assess the accuracy of the CEMS.
The calculations and limits of acceptable relative accuracy (RA) are
as follows:
(a) For pollutant CEMS:
Where:
d=Difference between response and the known concentration/response.
AC=The known concentration/response of the cylinder gas or
calibration cell.
(b) For diluent CEMS:
RA=|d| 0.7 percent O2 or CO2, as applicable.
Note: Waiver of the relative accuracy test in favor of the
alternative RA procedure does not preclude the requirements to complete
the calibration drift (CD) tests nor any other requirements specified in
the applicable regulation(s) for reporting CEMS data and performing CEMS
drift checks or audits.
Insert illus. 0496
Insert illus. 497
11. Bibliography
1. Department of Commerce. Experimental Statistics. Handbook 91.
Washington, DC, p. 3-31, paragraphs 3-3.1.4.
2. ''A Procedure for Establishing Traceability of Gas Mixtures to
Certain National Bureau of Standards Standard Reference Materials.''
Joint publication by NBS and EPA. EPA-600/7-81-010. Available from U.S.
Environmental Protection Agency, Quality Assurance Division (MD-77),
Research Triangle Park, NC 27711.
3. ''Traceability Protocol for Establishing True Concentrations of
Gases Used for Calibration and Audits of Continuous Source Emission
Monitors. (Protocol Number 1).'' June 1978. Protocol Number 1 is
included in the Quality Assurance Handbook for Air Pollution Measurement
Systems, Volume III, Stationary Source Specific Methods.
EPA-600/4-77-027b. August 1977. Volume III is available from the U.S.
EPA, Office of Research and Development Publications, 26 West St. Clair
Street, Cincinnati, OH 45268.
4. ''Gaseous Continuous Emission Monitoring Systems -- Performance
Specification Guidelines for SO2, NOx, CO2, O2, and TRS.''
EPA-450/3-82-026. Available from U.S. Environmental Protection Agency,
Emission Standards and Engineering Division (MD-19), Research Triangle
Park, NC 27711.
1. Applicability and Principle
40 CFR 60.748 Pt. 60, App. B, Spec. 3
1.1 Applicability. This specification is to be used for evaluating
acceptability of O2 and CO2 continuous emission monitoring systems
(CEM's) at the time of or soon after installation and whenever specified
in an applicable subpart of the regulations. The specification applies
to O2 or CO2 monitors that are not included under Performance
Specification 2 (PS 2).
This specification is not designed to evaluate the installed CEMS
performance over an extended period of time, nor does it identify
specific calibration techniques and other auxiliary procedures to assess
the CEMS performance. The source owner or operator, however, is
responsible to calibrate, maintain, and operate the CEMS properly. To
evaluate the CEMS performance, the Administrator may require, under
Section 114 of the Act, the operator to conduct CEMS performance
evaluations in addition to the initial test. See Section 60.13(c).
The definitions, installation and measurement location
specifications, test procedures, data reduction procedures, reporting
requirements, and bibliography are the same as in PS 2, Sections 2, 3,
5, 6, 8, 9, and 10, and also apply to O2 and CO2 CEMS's under this
specification. The performance and equipment specifications and the
relative accuracy (RA) test procedures for O2 and CO2 CEMS do not differ
from those for SO2 and NOx CEMS, except as noted below.
1.2 Principle. Reference method (RM) tests and calibration drift
tests are conducted to determine conformance of the CEMS with the
specification.
2. Performance and Equipment Specifications
2.1 Instrument Zero and Span. This specification is the same as
Section 4.1 of PS 2.
2.2 Calibration Drift. The CEMS calibration must not drift by more
than 0.5 percent O2 or CO2 from the reference value of the gas, gas
cell, or optical filter.
2.3 The CEMS RA. The RA of the CEMS must be no greater than 20
percent of the mean value of the RM test data or 1.0 percent O2 or CO2 ,
whichever is greater.
3. Relative Accuracy Test Procedure
3.1 Sampling Strategy for RM Tests, Correlation of RM and CEMS Data,
Number of RM Tests, and Calculations. This is the same as PS 2,
Sections 7.1, 7.2, 7.3, and 7.5, respectively.
3.2 Reference Method. Unless otherwise specified in an applicable
subpart of the regulations, Method 3B of appendix A or any approved
alternative is the RM for O2 or CO2.
40 CFR 60.748 Pt. 60, App. B, Spec. 4
1. Applicability and Principle
1.1 Applicability. This specification is to be used for evaluating
the acceptability of carbon monoxide (CO) continuous emission monitoring
systems (CEMS) at the time of or soon after installation and whenever
specified in an applicable subpart of the regulations.
This specification is not designed to evaluate the installed CEMS
performance over an extended period of time nor does it identify
specific calibration techniques and other auxiliary procedures to assess
CEMS performance. The source owner or operator, however, is responsible
to calibrate, maintain, and operate the CEMS. To evaluate CEMS
performance, the Administrator may require, under section 114 of the
Act, the source owner or operator to conduct CEMS performance
evaluations at other times besides the initial test. See 60.13(c).
The definitions, installation specifications, test procedures, data
reduction procedures for determining calibration drifts (CD) and
relative accuracy (RA), and reporting of Performance Specification 2 (PS
2), Sections 2, 3, 5, 6, 8, and 9 apply to this specification.
1.2 Principle. Reference method (RM), CD, and RA tests are conducted
to determine that the CEMS conforms to the specification.
2. Performance and Equipment Specifications
2.1 Instrument Zero and Span. This specification is the same as
Section 4.1 of PS 2.
2.2 Calibration Drift. The CEMS calibration must not drift or
deviate from the reference value of the calibration gas, gas cell, or
optical filter by more than 5 percent of the established span value for
6 out of 7 test days (e.g., the established span value is 1000 ppm for
subpart J affected facilities).
2.3 Relative Accuracy. The RA of the CEMS shall be no greater than
10 percent of the mean value of the RM test data in terms of the units
of the emission standard or 5 percent of the applicable standard,
whichever is greater.
3. Relative Accuracy Test Procedure
3.1 Sampling Strategy for RM Tests, Correlation of RM and CEMS Data,
Number of RM Tests, and Calculations. These are the same as PS 2,
Sections 7.1, 7.2, 7.3, and 7.5, respectively.
3.2 Reference Methods. Unless otherwise specified in an applicable
subpart of the regulation, Method 10 is the RM for this PS. When
evaluating nondispersive infrared continuous emission analyzers, Method
10 shall use the alternative interference trap specified in section 10.1
of the method. Method 10A or 10B is an acceptable alternative to method
10.
4. Bibliography
1. Ferguson, B.B., R.E. Lester, and W.J. Mitchell. Field Evaluation
of Carbon Monoxide and Hydrogen Sulfide Continuous Emission Monitors at
an Oil Refinery. U.S. Environmental Protection Agency. Research
Triangle Park, NC. Publication No. EPA-600/4-82-054. August 1982. 100
p.
2. Repp, M. Evaluation of Continuous Monitors for Carbon Monoxide in
Stationary Sources. U.S. Environmental Protection Agency. Research
Triangle Park, NC. Publication No. EPA-600/2-77-063. March 1977/ 155
p.
3. Smith, F., D.E. Wagoner, and R.P. Donovan. Guidelines for
Development of a Quality Assurance Program: Volume VIII --
Determination of CO Emissions from Stationary Sources by NDIR
Spectrometry. U.S. Environmental Protection Agency. Research Triangle
Park, NC. Publication No. EPA-650/4-74-005-h. February 1975. 96 p.
40 CFR 60.748 Pt. 60, App. B, Spec. 4A
1.1 Applicability.
1.1.1 This specification is to be used for evaluating the
acceptability of carbon monoxide (CO) continuous emission monitoring
systems (CEMS's) at the time of or soon after installation and whenever
specified in an applicable subpart of the regulations.
1.1.2 This specification is not designed to evaluate the installed
CEMS performance over an extended period of time nor does it identify
specific calibration techniques and other auxiliary procedures to assess
CEMS performance. The source owner or operator, however, is responsible
to calibrate, maintain, and operate the CEMS. To evaluate CEMS
performance, the Administrator may require, under section 114 of the
Act, the source owner or operator to conduct CEMS performance
evaluations at other times besides the initial test. See 60.13(c).
1.1.3 The definition, installation specifications, test procedures,
data reduction procedures for determining calibration drifts (CD) and
relative accuracy (RA), and reporting of Performance Specification 2 (PS
2), sections 2, 3, 5, 6, 8, and 9 apply to this specification.
1.2 Principle. Reference method (RM), CD and RA tests are conducted
to determine that the CEMS conforms to the specification.
2.1 Data Recorder Scale. This specification is the same as section
4.1 of PS 2. The CEMS shall be capable of measuring emission levels
under normal conditions and under periods of short-duration peaks of
high concentrations. This dual-range capability may be met using two
separate analyzers, one for each range, or by using dual-range units
which have the capability of measuring both levels with a single unit.
In the latter case, when the reading goes above the full-scale
measurement value of the lower range, the higher-range operation shall
be started automatically. The CEMS recorder range must include zero and
a high-level value.
For the low-range scale, the high-level value shall be between 1.5
times the pollutant concentration corresponding to the emission standard
level and the span value. For the high-range scale, the high-level
value shall be set at 2000 ppm, as a minimum, and the range shall
include the level of the span value. There shall be no concentration
gap between the low- and high-range scales.
2.2 Interference Check. The CEMS must be shown to be free from the
effects of any interferences.
2.3 Response Time. The CEMS response time shall not exceed 1.5 min
to achieve 95 percent of the final stable value.
2.4 Calibration Drift. The CEMS calibration must not drift or
deviate from the reference value of the calibration gas, gas cell, or
optical filter by more than 5 percent of the established span value for
6 out of 7 test days.
2.5 Relative Accuracy. The RA of the CEMS shall be no greater than
10 percent of the mean value of the RM test data in terms of the units
of the emission standard or 5 ppm, whichever is greater. Under
conditions where the average CO emissions are less than 10 percent of
the standard, a cylinder gas audit may be performed in place of the RA
test to determine compliance with these limits. In this case, the
cylinder gas shall contain CO in 12 percent carbon dioxide as an
interference check. If this option is exercised, Method 10 must be used
to verify that emission levels are less than 10 percent of the standard.
The response time test applies to all types of CEMS's, but will
generally have significance only for extractive systems. The entire
system is checked with this procedure including applicable sample
extraction and transport, sample conditioning, gas analyses, and data
recording.
Introduce zero gas into the system. For extractive systems, the
calibration gases should be introduced at the probe as near to the
sample location as possible. For in-situ systems, introduce the zero
gas at the sample interface so that all components active in the
analysis are tested. When the system output has stabilized (no change
greater than 1 percent of full scale for 30 sec), switch to monitor
stack effluent and wait for a stable value. Record the time (upscale
response time) required to reach 95 percent of the final stable value.
Next, introduce a high-level calibration gas and repeat the procedure
(stabilize, switch the sample, stabilize, record). Repeat the entire
procedure three times and determine the mean upscale and downscale
response times. The slower or longer of the two means is the system
response time.
4.1 Sampling Strategy for RM Tests, Correlation of RM and CEMS Data,
Number of RM Tests, and Calculations. These are the same as PS 2,
sections 7.1, 7.2, 7.3, and 7.5, respectively.
4.2 Reference Methods. Unless otherwise specified in an applicable
subpart of the regulation, Methods 10 is the RM for this PS. When
evaluating nondispersive infrared continuous emission analyzers, Method
10 shall use the alternative interference trap specified in section 10.1
of the method. Method 10A or 10B is an acceptable alternative to Method
10.
1. Same as in Performance Specification 4, section 4.
2. ''Gaseous Continuous Emission Monitoring Systems -- Performance
Specification Guidelines for SO2, NOx, CO2, O2, and TRS.''
EPA-450/3-82-026. U.S. Environmental Protection Agency, Technical
Support Division (MD-19). Research Triangle Park, NC 27711.
40 CFR 60.748 Pt. 60, App. B, Spec. 5
1. Applicability and Principle
1.1 Applicability. This specification is to be used for evaluating
the acceptability of total reduced sulfur (TRS) and whenever specified
in an applicable subpart of the regulations. (At present, these
performance specifications do not apply to petroleum refineries, subpart
J.) Sources affected by the promulgation of the specification shall be
allowed 1 year beyond the promulgation date to install, operate, and
test the CEMS. The CEMS's may include O2 monitors which are subject to
Performance Specification 3 (PS 3).
The definitions, installation specifications, test procedures, and
data reduction procedures for determining calibration drifts (CD's) and
relative accuracy (RA), and reporting of PS 2, Sections 2, 3, 4, 5, 6,
8, and 9 also apply to this specification and must be consulted. The
performance and equipment specifications do not differ from PS 2 except
as listed below and are included in this specification.
1.2 Principle. The CD and RA tests are conducted to determine
conformance of the CEMS with the specification.
2. Performance and Equipment Specifications
2.1 Instrument Zero and Span. The CEMS recorder span must be set at
90 to 100 percent of recorder full-scale using a span level between 1.5
times the pollutant concentration corresponding to the emission standard
level and the span value. The CEMS design shall also allow the
determination of calibration at the zero level of the calibration curve.
If zero calibration is not possible or is impractical, this
determination may be conducted at a low level (up to 20 percent of span
value) point. The components of an acceptable permeation tube system
are listed on pages 87-94 of Citation 4.2 of the Bibliography.
2.2 Calibration Drift. The CEMS detector calibration must not drift
or deviate from the reference value of the calibration gas by more than
5 percent (1.5 ppm) of the established span value of 30 ppm for 6 out of
7 test days. If the CEMS includes pollutant and diluent monitors, the
CD must be determined separately for each in terms of concentrations
(see PS 3 for the diluent specifications).
2.3 The CEMS Relative Accuracy. The RA of the CEMS shall be no
greater than 20 percent of the mean value of the reference method (RM)
test data in terms of the units of the emission standard or 10 percent
of the applicable standard, whichever is greater.
3. Relative Accuracy Test Procedure
3.1 Sampling Strategy for RM Tests, Correlation of RM and CEMS Data,
Number of RM Tests, and Calculations. This is the same as PS 2,
Sections 7.1, 7.2, 7.3, and 7.5, respectively. Note: For Method 16, a
sample is made up of at least three separate injects equally spaced over
time. For Method 16A, a sample is collected for at least 1 hour.
3.2 Reference Methods. Unless otherwise specified in an applicable
subpart of the regulations, Method 16, Method 16A, or other approved
alternative, shall be the RM for TRS.
4. Bibliography
1. Department of Commerce. Experimental Statistics. National Bureau
of Standards. Handbook 91. 1963. Paragraphs 3-3.1.4, p. 3-31.
2. A Guide to the Design, Maintenance and Operation of TRS Monitoring
Systems. National Council for Air and Stream Improvement Technical
Bulletin No. 89. September 1977.
3. Observation of Field Performance of TRS Monitors on a Kraft
Recovery Furnace. National Council for Air and Stream Improvement
Technical Bulletin No. 91. January 1978.
40 CFR 60.748 Pt. 60, App. B, Spec. 6
1.1 Applicability. The applicability for this specification is the
same as Section 1.1 of Performance Specification 2 (PS 2), except this
specification is to be used for evaluating the acceptability of
continuous emission rate monitoring systems (CERMS's). The installation
and measurement location specifications, performance specification test
procedure, data reduction procedures, and reporting requirements of PS
2, Section 3, 5, 8, and 9, apply to this specification.
1.2 Principle. Reference method (RM), calibration drift (CD), and
relative accuracy (RA) tests are conducted to determine that the CERMS
conforms to the specification.
The definitions are the same as in Section 2 of PS 2, except that
this specification refers to the continuous emission rate monitoring
system rather than the continuous emission monitoring system. The
following definitions are added:
2.1 Continuous Emission Rate Monitoring System (CERMS). The total
equipment required for the determination and recording of the pollutant
mass emission rate (in terms of mass per unit of time).
2.2 Flow Rate Sensor. That portion of the CERMS that senses the
volumetric flow rate and generates an output proportional to flow rate.
The flow rate sensor shall have provisions to check the CD for each flow
rate parameter that it measures individually (e.g., velocity pressure).
3.1 Data Recorder Scale. Same as Section 4.1 of PS 2.
3.2 CD. Since the CERMS includes analyzers for several measurements,
the CD shall be determined separately for each analyzer in terms of its
specific measurement. The calibration for each analyzer used for the
measurement of flow rate except a temperature analyzer shall not drift
or deviate from either of its reference values by more than 3 percent of
1.25 times the average potential absolute value for that measurement.
For a temperature analyzer, the specification is 1.5 percent of 1.25
times the average potential absolute temperature. The CD specification
for each analyzer for which other PS's have been established (e.g., PS 2
for SO2 and NOx), shall be the same as in the applicable PS.
3.3 CERMS RA. The RA of the CERMS shall be no greater than 20
percent of the mean value of the RM's test data in terms of the units of
the emission standard, or 10 percent of the applicable standard,
whichever is greater.
The CD measurements are to verify the ability of the CERMS to conform
to the established CERMS calibrations used for determining the emission
rate. Therefore, if periodic automatic or manual adjustments are made
to the CERMS zero and calibration settings, conduct the CD tests
immediately before these adjustments, or conduct them in such a way what
CD can be determined.
Conduct the CD tests for pollutant concentration at the two values
specified in Section 4.1 of PS 2. For each of the other parameters that
are selectively measured by the CERMS (e.g., velocity pressure), use two
analogous values: one that represents zero to 20 percent of the
high-level value (a value that is between 1.25 and 2 times the average
potential value) for that parameter, and one that represents 50 to 100
percent of the high-level value. Introduce, or activate internally, the
reference signals to the CERMS (these need not be certified). Record
the CERMS response to each, and subtract this value from the respective
reference value (see example data sheet in Figure 6-1).
5.1 Sampling Strategy for RM's Tests, Correlation of RM and CERMS
Data, Number of RM's Tests, and Calculations. These are the same as PS
2, Sections 7.1, 7.2, 7.3, and 7.5, respectively. Summarize the results
on a data sheet. An example is shown in Figure 6-2. The RA test may be
conducted during the CD test period.
5.2 Reference Methods (RM's). Unless otherwise specified in the
applicable subpart of the regulations, the RM for the pollutant gas is
the appendix A method that is cited for compliance test purposes, or its
approved alternatives. Methods 2, 2A, 2B, 2C, or 2D, as applicable are
the RM's for the determination of volumetric flow rate.
1. Brooks, E.F., E.C. Beder, C.A. Flegal, D.J. Luciani, and R.
Williams. Continuous Measurement of Total Gas Flow Rate from Stationary
Sources. U.S. Envionmental Protection Agency. Research Triangle Park,
NC. Publication No. EPA-650/2-75-020. February 1975. 248 p.
40 CFR 60.748 Pt. 60, App. B, Spec. 7
1.1 Applicability. 1.1.1 This specification is to be used for
evaluating the acceptability of hydrogen sulfide (H2S) continuous
emission monitoring systems (CEMS's) at the time of or soon after
installation and whenever specified in an applicable subpart of the
regulations.
1.1.2 This specification is not designed to evaluate the installed
CEMS performance over an extended period of time nor does it identify
specific calibration techniques and other auxiliary procedures to assess
CEMS performance. The source owner or operator, however, is responsible
to calibrate, maintain, and operate the CEMS. To evaluate CEMS
performance, the Administrator may require, under Section 114 of the
Act, the source owner or operator to conduct CEMS performance
evaluations at other times besides the initial test. See 60.13(c).
1.1.3 The definitions, installation specifications, test procedures,
data reduction procedures for determining calibration drifts (CD) and
relative accuracy (RA), and reporting of Performance Specification 2 (PS
2), Sections 2, 3, 5, 6, 8, and 9 apply to this specification.
1.2 Principle. Reference method (RM), CD, and RA tests are conducted
to determine that the CEMS conforms to the specification.
2.1 Instrument zero and span. This specification is the same as
Section 4.1 of PS 2.
2.2 Calibration drift. The CEMS calibration must not drift or
deviate from the reference value of the calibration gas or reference
source by more than 5 percent of the established span value for 6 out of
7 test days (e.g., the established span value is 300 ppm for subpart J
fuel gas combustion devices).
2.3 Relative accuracy. The RA of the CEMS shall be no greater than
20 percent of the mean value of the RM test data in terms of the units
of the emission standard or 10 percent of the applicable standard,
whichever is greater.
3.1 Sampling Strategy for RM Tests, Correlation of RM and CEMS Data
Number of RM Tests, and Calculations. These are the same as that in PS
2, 7.1, 7.2, 7.3, and 7.5, respectively.
3.2 Reference Methods. Unless otherwise specified in an applicable
subpart of the regulation, Method 11 is the RM for this PS.
1. U.S. Environmental Protection Agency. Standards of Performance
for New Stationary Sources; Appendix B; Performance Specifications 2
and 3 for SO2, NOx, CO2, and O2 Continuous Emission Monitoring Systems;
Final Rule. 48 CFR 23608. Washington, DC, U.S. Government Printing
Office. May 25, 1983.
2. U.S. Government Printing Office. Gaseous Continuous Emission
Monitoring Systems -- Performance Specification Guidelines for SO2, NOx,
CO2, O2, and TRS. U.S. Environmental Protection Agency. Washington,
DC, EPA-450/3-82-026. October 1982. 26p.
3. Maines, G.D., W.C. Kelly (Scott Environmental Technology, Inc.),
and J.B. Homolya. Evaluation of Monitors for Measuring H2S in Refinery
Gas. Prepared for the U.S. Environmental Protection Agency. Research
Triangle Park, NC, Contract No. 68-02-2707. 1978. 60 p.
4. Ferguson, B.B., R.E. Lester (Harmon Engineering and Testing), and
W.J. Mitchell. Field Evaluation of Carbon Monoxide and Hydrogen Sulfide
Continuous Emission Monitors at an Oil Refinery. Prepared for the U.S.
Environmental Protection Agency. Research Triangle Park, NC.
Publication No. EPA-600/4-82-054. August 1982. 100 p.
(48 FR 13327, Mar. 30, 1983 and 48 FR 23611, May 25, 1983, as amended
at 48 FR 32986, July 20, 1983; 51 FR 31701, Aug. 5, 1985; 52 FR 17556,
May 11, 1987; 52 FR 30675, Aug. 18, 1987; 52 FR 34650, Sept. 14, 1987;
53 FR 7515, Mar. 9, 1988; 53 FR 41335, Oct. 21, 1988; 55 FR 18876,
May 7, 1990; 55 FR 40178, Oct. 2, 1990; 55 FR 47474, Nov. 14, 1990;
56 FR 5526, Feb. 11, 1991)
40 CFR 60.748 Pt. 60, App. C
40 CFR 60.748 Appendix C -- Determination of Emission Rate Change
1. Introduction.
1.1 The following method shall be used to determine whether a
physical or operational change to an existing facility resulted in an
increase in the emission rate to the atmosphere. The method used is the
Student's t test, commonly used to make inferences from small samples.
2. Data.
2.1 Each emission test shall consist of n runs (usually three) which
produce n emission rates. Thus two sets of emission rates are
generated, one before and one after the change, the two sets being of
equal size.
2.2 When using manual emission tests, except as provided in 60.8(b)
of this part, the reference methods of appendix A to this part shall be
used in accordance with the procedures specified in the applicable
subpart both before and after the change to obtain the data.
2.3 When using continuous monitors, the facility shall be operated as
if a manual emission test were being performed. Valid data using the
averaging time which would be required if a manual emission test were
being conducted shall be used.
3. Procedure.
3.1 Subscripts a and b denote prechange and postchange respectively.
3.2 Calculate the arithmetic mean emission rate, E, for each set of
data using Equation 1.
Insert illus. 137A
Where:
Ei=Emission rate for the i th run.
n=number of runs.
3.3 Calculate the sample variance, S2, for each set of data using
Equation 2.
Insert illus. 138A
3.4 Calculate the pooled estimate, Sp, using Equation 3.
Insert illus. 138B
3.5 Calculate the test statistic, t, using Equation 4.
Insert illus. 138C
4. Results.
4.1 If Eb Ea and t t', where t' is the critical value of t obtained
from Table 1, then with 95% confidence the difference between Eb and Ea
is significant, and an increase in emission rate to the atmosphere has
occurred.
For greater than 8 degrees of
freedom, see any
standard statistical handbook or
text.
5.1 Assume the two performance tests produced the following set of
data:
5.2 Using Equation 1 --
5.3 Using Equation 2 --
Sa2=(100^102)2+(95^102)2+(110^102)2/3^1=58.5
Sb2=(115^120)2+(120^120)2+(125^120)2/3^1=25
5.4 Using Equation 3 --
Sp=((3^1)(58.5)+(3+1)(25)/3+3^2) 1/2=6.46
5.5 Using Equation 4 --
Insert illus. 138D
5.6 Since (n1+n2^2)=4, t'=2.132 (from Table 1). Thus since t t' the
difference in the values of Ea and Eb is significant, and there has been
an increase in emission rate to the atmosphere.
6. Continuous Monitoring Data.
6.1 Hourly averages from continuous monitoring devices, where
available, should be used as data points and the above procedure
followed.
(40 FR 58420, Dec. 16, 1975)
40 CFR 60.748 Pt. 60, App. D
40 CFR 60.748 Appendix D -- Required Emission Inventory Information
(a) Completed NEDS point source form(s) for the entire plant
containing the designated facility, including information on the
applicable criteria pollutants. If data concerning the plant are
already in NEDS, only that information must be submitted which is
necessary to update the existing NEDS record for that plant. Plant and
point identification codes for NEDS records shall correspond to those
previously assigned in NEDS; for plants not in NEDS, these codes shall
be obtained from the appropriate Regional Office.
(b) Accompanying the basic NEDS information shall be the following
information on each designated facility:
(1) The state and county identification codes, as well as the
complete plant and point identification codes of the designated facility
in NEDS. (The codes are needed to match these data with the NEDS data.)
(2) A description of the designated facility including, where
appropriate:
(i) Process name.
(ii) Description and quantity of each product (maximum per hour and
average per year).
(iii) Description and quantity of raw materials handled for each
product (maximum per hour and average per year).
(iv) Types of fuels burned, quantities and characteristics (maximum
and average quantities per hour, average per year).
(v) Description and quantity of solid wastes generated (per year) and
method of disposal.
(3) A description of the air pollution control equipment in use or
proposed to control the designated pollutant, including:
(i) Verbal description of equipment.
(ii) Optimum control efficiency, in percent. This shall be a
combined efficiency when more than one device operates in series. The
method of control efficiency determination shall be indicated (e.g.,
design efficiency, measured efficiency, estimated efficiency).
(iii) Annual average control efficiency, in percent, taking into
account control equipment down time. This shall be a combined
efficiency when more than one device operates in series.
(4) An estimate of the designated pollutant emissions from the
designated facility (maximum per hour and average per year). The method
of emission determination shall also be specified (e.g., stack test,
material balance, emission factor).
(40 FR 53349, Nov. 17, 1975)
40 CFR 60.748 Appendix E -- (Reserved)
40 CFR 60.748 Pt. 60, App. F
40 CFR 60.748 Appendix F -- Quality Assurance Procedures
Continuous Emission Monitoring Systems Used for
Compliance Determination
1. Applicability and Principle
1.1 Applicability. Procedure 1 is used to evaluate the effectiveness
of quality control (QC) and quality assurance (QA) procedures and the
quality of data produced by any continuous emission monitoring system
(CEMS) that is used for determining compliance with the emission
standards on a continuous basis as specified in the applicable
regulation. The CEMS may include pollutant (e.g., S02 and N0x) and
diluent (e.g., 02 or C02) monitors.
This procedure specifies the minimum QA requirements necessary for
the control and assessment of the quality of CEMS data submitted to the
Environmental Protection Agency (EPA). Source owners and operators
responsible for one or more CEMS's used for compliance monitoring must
meet these minimum requirements and are encouraged to develop and
implement a more extensive QA program or to continue such programs where
they already exist.
Data collected as a result of QA and QC measures required in this
procedure are to be submitted to the Agency. These data are to be used
by both the Agency and the CEMS operator in assessing the effectiveness
of the CEMS QC and QA procedures in the maintenance of acceptable CEMS
operation and valid emission data.
Appendix F, Procedure 1 is applicable December 4, 1987. The first
CEMS accuracy assessment shall be a relative accuracy test audit (RATA)
(see section 5) and shall be completed by March 4, 1988 or the date of
the initial performance test required by the applicable regulation,
whichever is later.
1.2 Principle. The QA procedures consist of two distinct and equally
important functions. One function is the assessment of the quality of
the CEMS data by estimating accuracy. The other function is the control
and improvement of the quality of the CEMS data by implementing QC
policies and corrective actions. These two functions form a control
loop: When the assessment function indicates that the data quality is
inadequate, the control effort must be increased until the data quality
is acceptable. In order to provide uniformity in the assessment and
reporting of data quality, this procedure explicitly specifies the
assessment methods for response drift and accuracy. The methods are
based on procedures included in the applicable performance
specifications (PS's) in appendix B of 40 CFR part 60. Procedure 1 also
requires the analysis of the EPA audit samples concurrent with certain
reference method (RM) analyses as specified in the applicable RM's.
Because the control and corrective action function encompasses a
variety of policies, specifications, standards, and corrective measures,
this procedure treats QC requirements in general terms to allow each
source owner or operator to develop a QC system that is most effective
and efficient for the circumstances.
2. Definitions
2.1 Continuous Emission Monitoring System. The total equipment
required for the determination of a gas concentration or emission rate.
2.2 Diluent Gas. A major gaseous constituent in a gaseous pollutant
mixture. For combustion sources, CO2 and O2 are the major gaseous
constituents of interest.
2.3 Span Value. The upper limit of a gas concentration measurement
range that is specified for affected source categories in the applicable
subpart of the regulation.
2.4 Zero, Low-Level, and High-Level Values. The CEMS response values
related to the source specific span value. Determination of zero,
low-level, and high-level values is defined in the appropriate PS in
appendix B of this part.
2.5 Calibration Drift (CD). The difference in the CEMS output
reading from a reference value after a period of operation during which
no unscheduled maintenance, repair or adjustment took place. The
reference value may be supplied by a cylinder gas, gas cell, or optical
filter and need not be certified.
2.6 Relative Accuracy (RA). The absolute mean difference between the
gas concentration or emission rate determined by the CEMS and the value
determined by the RM's plus the 2.5 percent error confidence coefficient
of a series of tests divided by the mean of the RM tests or the
applicable emission limit.
3. QC Requirements
Each source owner or operator must develop and implement a QC
program. As a minimum, each QC program must include written procedures
which should describe in detail, complete, step-by-step procedures and
operations for each of the following activities:
1. Calibration of CEMS.
2. CD determination and adjustment of CEMS.
3. Preventive maintenance of CEMS (including spare parts inventory).
4. Data recording, calculations, and reporting.
5. Accuracy audit procedures including sampling and analysis methods.
6. Program of corrective action for malfunctioning CEMS.
As described in Section 5.2, whenever excessive inaccuracies occur
for two consecutive quarters, the source owner or operator must revise
the current written procedures or modify or replace the CEMS to correct
the deficiency causing the excessive inaccuracies.
These written procedures must be kept on record and available for
inspection by the enforcement agency.
4. CD Assessment
4.1 CD Requirement. As described in 40 CFR 60.13(d), source owners
and operators of CEMS must check, record, and quantify the CD at two
concentration values at least once daily (approximately 24 hours) in
accordance with the method prescribed by the manufacturer. The CEMS
calibration must, as minimum, be adjusted whenever the daily zero (or
low-level) CD or the daily high-level CD exceeds two times the limits of
the applicable PS's in appendix B of this regulation.
4.2 Recording Requirement for Automatic CD Adjusting Monitors.
Monitors that automatically adjust the data to the corrected calibration
values (e.g., microprocessor control) must be programmed to record the
unadjusted concentration measured in the CD prior to resetting the
calibration, if performed, or record the amount of adjustment.
4.3 Criteria for Excessive CD. If either the zero (or low-level) or
high-level CD result exceeds twice the applicable drift specification in
appendix B for five, consecutive, daily periods, the CEMS is
out-of-control. If either the zero (or low-level) or high-level CD
result exceeds four times the applicable drift specification in appendix
B during any CD check, the CEMS is out-of-control. If the CEMS is
out-of-control, take necessary corrective action. Following corrective
action, repeat the CD checks.
4.3.1 Out-Of-Control Period Definition. The beginning of the
out-of-control period is the time corresponding to the completion of the
fifth, consecutive, daily CD check with a CD in excess of two times the
allowable limit, or the time corresponding to the completion of the
daily CD check preceding the daily CD check that results in a CD in
excess of four times the allowable limit. The end of the out-of-control
period is the time corresponding to the completion of the CD check
following corrective action that results in the CD's at both the zero
(or low-level) and high-level measurement points being within the
corresponding allowable CD limit (i.e., either two times or four times
the allowable limit in appendix B).
4.3.2 CEMS Data Status During Out-of-Control Period. During the
period the CEMS is out-of-control, the CEMS data may not be used in
calculating emission compliance nor be counted towards meeting minimum
data availability as required and described in the applicable subpart
(e.g., 60.47a(f)).
4.4 Data Recording and Reporting. As required in 60.7(d) of this
regulation (40 CFR part 60), all measurements from the CEMS must be
retained on file by the source owner for at least 2 years. However,
emission data obtained on each successive day while the CEMS is
out-of-control may not be included as part of the minimum daily data
requirement of the applicable subpart (e.g., 60.47a(f)) nor be used in
the calculation of reported emissions for that period.
5. Data Accuracy Assessment
5.1 Auditing Requirements. Each CEMS must be audited at least once
each calendar quarter. Successive quarterly audits shall occur no
closer than 2 months. The audits shall be conducted as follows:
5.1.1 Relative Accuracy Test Audit (RATA). The RATA must be
conducted at least once every four calendar quarters. Conduct the RATA
as described for the RA test procedure in the applicable PS in appendix
B (e.g., PS 2 for SO2 and NOX). In addition, analyze the appropriate
performance audit samples received from EPA as described in the
applicable sampling methods (e.g., Methods 6 and 7).
5.1.2 Cylinder Gas Audit (CGA). If applicable, a CGA may be
conducted in three of four calendar quarters, but in no more than three
quarters in succession.
To conduct a CGA: (1) Challenge the CEMS (both pollutant and diluent
portions of the CEMS, if applicable) with an audit gas of known
concentration at two points within the following ranges:
Challenge the CEMS three times at each audit point, and use the
average of the three responses in determining accuracy.
Use of separate audit gas cylinder for audit points 1 and 2. Do not
dilute gas from audit cylinder when challenging the CEMS.
The monitor should be challenged at each audit point for a sufficient
period of time to assure adsorption-desorption of the CEMS sample
transport surfaces has stabilized.
(2) Operate each monitor in its normal sampling mode, i.e., pass the
audit gas through all filters, scrubbers, conditioners, and other
monitor components used during normal sampling, and as much of the
sampling probe as is practical. At a minimum, the audit gas should be
introduced at the connection between the probe and the sample line.
(3) Use audit gases that have been certified by comparision to
National Bureau of Standards (NBS) gaseous Standard Reference Materials
(SRM's) or NBS/EPA approved gas manufacturer's Certified Reference
Materials (CRM's) (See Citation 1) following EPA Traceability Protocol
No. 1 (See Citation 2). As an alternative to Protocol No. 1 audit
gases, CRM's may be used directly as audit gases. A list of gas
manufacturers that have prepared approved CRM's is available from EPA at
the address shown in Citation 1. Procedures for preparation of CRM's
are described in Citation 1. Procedures for preparation of EPA
Traceability Protocol 1 materials are described in Citation 2.
The difference between the actual concentration of the audit gas and
the concentration indicated by the monitor is used to assess the
accuracy of the CEMS.
5.1.3 Relative Accuracy Audit (RAA). The RAA may be conducted three
of four calendar quarters, but in no more than three quarters in
succession. To conduct a RAA, follow the procedure described in the
applicable PS in appendix B for the relative accuracy test, except that
only three sets of measurement data are required. Analyses of EPA
performance audit samples are also required.
The relative difference between the mean of the RM values and the
mean of the CEMS responses will be used to assess the accuracy of the
CEMS.
5.1.4 Other Alternative Audits. Other alternative audit procedures
may be used as approved by the Administrator for three of four calendar
quarters. One RATA is required at least once every four calendar
quarters.
5.2 Excessive Audit Inaccuracy. If the RA, using the RATA, CGA, or
RAA exceeds the criteria in section 5.2.3, the CEMS is out-of-control.
If the CEMS is out-of-control, take necessary corrective action to
eliminate the problem. Following corrective action, the source owner or
operator must audit the CEMS with a RATA, CGA, or RAA to determine if
the CEMS is operating within the specifications. A RATA must always be
used following an out-of-control period resulting from a RATA. The
audit following corrective action does not require analysis of EPA
performance audit samples. If audit results show the CEMS to be
out-of-control, the CEMS operator shall report both the audit showing
the CEMS to be out-of-control and the results of the audit following
corrective action showing the CEMS to be operating within
specifications.
5.2.1 Out-Of-Control Period Definition. The beginning of the
out-of-control period is the time corresponding to the completion of the
sampling for the RATA, RAA, or CGA. The end of the out-of-control
period is the time corresponding to the completion of the sampling of
the subsequent successful audit.
5.2.2. CEMS Data Status During Out-Of-Control Period. During the
period the monitor is out-of-control, the CEMS data may not be used in
calculating emission compliance nor be counted towards meeting minimum
data availabilty as required and described in the applicable subpart
(e.g., 60.47a(f)).
5.2.3 Criteria for Excessive Audit Inaccuracy. Unless specified
otherwise in the applicable subpart, the criteria for excessive
inaccuracy are:
(1) For the RATA, the allowable RA in the applicable PS in appendix
B.
(2) For the CGA, 15 percent of the average audit value or 5 ppm,
whichever is greater.
(3) For the RAA, 15 percent of the three run average or 7.5 percent
of the applicable standard, whichever is greater.
5.3 Criteria for Acceptable QC Procedure. Repeated excessive
inaccuracies (i.e., out-of-control conditions resulting from the
quarterly audits) indicates the QC procedures are inadequate or that the
CEMS is incapable of providing quality data. Therefore, whenever
excessive inaccuracies occur for two consective quarters, the source
owner or operator must revise the QC procedures (see Section 3) or
modify or replace the CEMS.
6.Calculations for CEMS Data Accuracy
6.1 RATA RA Calculation. Follow the equations described in Section 8
of appendix B, PS 2 to calculate the RA for the RATA. The RATA must be
calculated in units of the applicable emission standard (e.g., ng/J).
6.2 RAA Accuracy Calculation. Use Equation 1-1 to calculate the
accuracy for the RAA. The RAA must be calculated in units of the
applicable emission standard (e.g., ng/J).
6.3 CGA Accuracy Calculation. Use Equation 1-1 to calculate the
accuracy for the CGA, which is calculated in units of the appropriate
concentration (e.g., ppm SO2 or percent O2). Each component of the CEMS
must meet the acceptable accuracy requirement.
where:
A = Accuracy of the CEMS, percent.
Cm = Average CEMS response during audit in units of applicable
standard or appropriate concentration.
Ca = Average audit value (CGA certified value or three-run average
for RAA) in units of applicable standard or appropriate concentration.
6.4 Example Accuracy Calculations. Example calculations for the
RATA, RAA, and CGA are available in Citation 3.
7. Reporting Requirements
At the reporting interval specified in the applicable regulation,
report for each CEMS the accuracy results from Section 6 and the CD
assessment results from Section 4. Report the drift and accuracy
information as a Data Assessment Report (DAR), and include one copy of
this DAR for each quarterly audit with the report of emissions required
under the applicable subparts of this part.
As a minimum, the DAR must contain the following information:
1. Source owner or operator name and address.
2. Identification and location of monitors in the CEMS.
3. Manufacturer and model number of each monitor in the CEMS.
4. Assessment of CEMS data accuracy and date of assessment as
determined by a RATA, RAA, or CGA described in Section 5 including the
RA for the RATA, the A for the RAA or CGA, the RM results, the cylinder
gases certified values, the CEMS responses, and the calculations results
as defined in Section 6. If the accuracy audit results show the CEMS to
be out-of-control, the CEMS operator shall report both the audit results
showing the CEMS to be out-of-control and the results of the audit
following corrective action showing the CEMS to be operating within
specifications.
5. Results from EPA performance audit samples described in Section 5
and the applicable RM's.
6. Summary of all corrective actions taken when CEMS was determined
out-of-control, as described in Sections 4 and 5.
An example of a DAR format is shown in Figure 1.
8. Biblography
1. ''A Procedure for Establishing Traceability of Gas Mixtures to
Certain National Bureau of Standards Standard Reference Materials.''
Joint publication by NBS and EPA-600/7-81-010. Available from the U.S.
Environmental Protection Agency. Quality Assurance Division (MD-77).
Research Triangle Park, NC 27711.
2. ''Traceability Protocol for Establishing True Concentrations of
Gases Used for Calibration and Audits of Continuous Source Emission
Monitors (Protocol Number 1)'' June 1978. Section 3.0.4 of the Quality
Assurance Handbook for Air Pollution Measurement Systems. Volume III.
Stationary Source Specific Methods. EPA-600/4-77-027b. August 1977.
U.S. Environmental Protection Agency. Office of Research and
Development Publications, 26 West St. Clair Street, Cincinnati, OH
45268.
3. Calculation and Interpretation of Accuracy for Continuous Emission
Monitoring Systems (CEMS). Section 3.0.7 of the Quality Assurance
Handbook for Air Pollution Measurement Systems, Volume III, Stationary
Source Specific Methods. EPA-600/4-77-027b. August 1977. U.S.
Environmental Protection Agency. Office of Research and Development
Publications, 26 West St. Clair Street, Cincinnati, OH 45268.
Period ending date
Year
Company name
Plant name
Source unit no.
CEMS manufacturer
Model no.
CEMS serial no.
CEMS type (e.g., in situ)
CEMS sampling location (e.g., control device outlet)
CEMS span values as per the applicable regulation: XXXXXX (e.g., SO2
XXXX ppm, NOx XXXX ppm).
I. Accuracy assessment results (Complete A, B, or C below for each
CEMS or for each pollutant and diluent analyzer, as applicable.) If the
quarterly audit results show the CEMS to be out-of-control, report the
results of both the quarterly audit and the audit following corrective
action showing the CEMS to be operating properly.
A. Relative accuracy test audit (RATA) for XXXX (e.g., SO2 in ng/J).
1. Date of audit XXXX.
2. Reference methods (RM's) used XXXX (e.g., Methods 3 and 6).
3. Average RM value XXXX (e.g., ng/J, mg/dsm /3/ , or percent
volume).
4. Average CEMS value XXXX.
5. Absolute value of mean difference (d) XXXX.
6. Confidence coefficient (CC) XXXX.
7. Percent relative accuracy (RA) XXXX percent.
8. EPA performance audit results:
a. Audit lot number (1) XXXX (2) XXXX
b. Audit sample number (1) XXXX (2) XXXX
c. Results (mg/dsm /3/ ) (1) XXXX (2) XXXX
d. Actual value (mg/dsm /3/ )* (1) XXXX (2) XXXX
e. Relative error* (1) XXXX (2) XXXX
B. Cylinder gas audit (CGA) for XXXX (e.g., SO2 in ppm).
C. Relative accuracy audit (RAA) for XXXX (e.g., SO2 in ng/J).
1. Date of audit XXXX.
2. Reference methods (RM's) used XXXX (e.g., Methods 3 and 6).
3. Average RM value XXXX (e.g., ng/J).
4. Average CEMS value XXXX.
5. Accuracy XXXX percent.
6. EPA performance audit results:
a. Audit lot number (1) XXXX (2) XXXX
b. Audit sample number (1) XXXX (2) XXXX
c. Results (mg/dsm /3/ ) (1) XXXX (2) XXXX
d. Actual value (mg/dsm /3/ ) *(1) XXXX (2)
e. Relative error* (1) XXXX (2) XXXX
D. Corrective action for excessive inaccuracy.
1. Out-of-control periods.
a. Date(s) XXXX.
b. Number of days XXXX.
2. Corrective action taken --
3. Results of audit following corrective action. (Use format of A,
B, or C above, as applicable.)
II. Calibration drift assessment.
A. Out-of-control periods.
1. Date(s) XXXX.
2. Number of days XXXX.
B. Corrective action taken --
(52 FR 21008, June 4, 1987; 52 FR 27612, July 22, 1987, as amended
at 56 FR 5527, Feb. 11, 1991)
*To be completed by the Agency.
40 CFR 60.748 Pt. 60, App. G
40 CFR 60.748 Appendix G -- Provisions for an Alternative Method of
Demonstrating Compliance With 40 CFR 60.43 for the Newton Power Station
of Central Illinois Public Service Company
1. Designation of Affected Facilities
1.1 The affected facilities to which this alternative compliance
method applies are the Unit 1 and 2 coal-fired steam generating units
located at the Central Illinois Public Service Company's (CIPS) Newton
Power Station in Jasper County, Illinois. Each of these units is
subject to the Standards of Performance for Fossil-Fuel-Fired Steam
Generators for Which Construction Commenced After August 17, 1971
(subpart D).
2. Definitions
2.1 All definitions in subparts D and Da of part 60 apply to this
provision except that:
24-hour period means the period of time between 12:00 midnight and
the following midnight.
CEMS means continuous emission monitoring system.
DAFGDS means the dual alkali flue gas desulfurizaiton system for the
Newton Unit 1 steam generating unit.
Boiler operating day means a 24-hour period during which any fossil
fuel is combusted in either the Unit 1 or Unit 2 steam generating unit
and during which the provisions of 60.43(e) are applicable.
Coal bunker means a single or group of coal trailers, hoppers, silos
or other containers that: (1) are physically attached to the affected
facility; and (2) provide coal to the coal pulverizers.
3. Compliance Provisions
3.1 If the owner or operator of the affected facility elects to
comply with the 470 nanograms per joule (ng/J) (1.1 lb/million Btu) of
combined heat input emission limit under 60.43(e), he shall notify the
Administrator at least 30 days in advance of the date such election is
to take effect, stating the date such operation is to commence. When
the owner or operator elects to comply with this limit after one or more
periods of reverting to the 520 ng/J heat input (1.2 lb/million Btu)
limit of 60.43(a)(2), as provided under 3.4, he shall notify the
Administrator in writing at least ten (10) days in advance of the date
such election is to take effect.
3.2 Compliance with the sulfur dioxide emission limit under 60.43(e)
is determined on a continuous basis by performance testing using CEMS.
Within 60 days after the initial operation subject to the combined
emission limit in 60.43(e), the owner or operator shall conduct an
initial performance test, as required by 60.8, to determine compliance
with the combined emission limit. This initial performance test is to
be scheduled so that the first boiler operating day of the 30 successive
boiler operating days is completed within 60 days after initial
operation subject to the 470 ng/J (1.1 lb/million Btu) combined emission
limit. Following the initial performance test, a separate performance
test is completed at the end of each boiler operating day Unit 1 and
Unit 2 are subject to 60.43(e), and new 30 day average emission rate
calculated.
3.2.1 Following the initial performance test, a new 30 day average
emission rate is calculated each boiler operating day the affected
facility is subject to 60.43(e). If the owner or operator of the
affected facility elects to comply with 60.43(e) after one or more
periods of reverting to the 520 ng/J heat input (1.2 lb/million Btu)
limit under 60.43(a)(2), as provided under 3.4, the 30 day average
emission rate under 60.43(e) is calculated using emissions data of the
current boiler operating day and data for the previous 29 boiler
operating days when the affected facility was subject to 60.43(e).
Operation of the affected facility under 60.43(a)(2) is not considered
a boiler operating day. Emissions data collected during such periods
are considered relative to 4.6 and emissions data are not included in
calculations of emissions under 60.43(e).
3.2.2 When the affected facility is operated under the provisions of
60.43(e), the Unit 1 DAFGDS bypass damper must be fully closed with no
flue gas bypassing the DAFGDS and the full flue gas volume treated by
the DAFGDS. The DAFGDS bypass may be opened only during periods of
DAFGDS startup, shutdown, or malfunction as described under Sections
3.5.1, 3.5.2, 3.5.3, 3.5.4, and 3.5.5.
3.3 Compliance with the sulfur dioxide emission limit set forth in
60.43(e) is based on the average combined hourly emission rate from
Units 1 and 2 for 30 successive boiler operating days determined as
follows:
where
n=the number of available hourly combined emission rate values in the
30 successive boiler operating day period where Unit 1 and Unit 2 are
subject to 60.43(e).
E30=average emission rate for 30 successive boiler operating days
where Unit 1 and Unit 2 are subject to 60.43(e).
EC=the hourly combined emission rate from Units 1 and 2.
3.3.1 The average hourly combined emission rate for Units 1 and 2 for
each hour of operation of either Unit 1 or 2, or both, is determined as
follows:
EC=((E1)(H1)+(E2)(H2))/(H1+H2))
where:
EC=the hourly combined emission rate from Units 1 and 2 where Units 1
and 2 are subject to 60.43(e).
E1=the hourly emission rate from Unit 1 as determined from CEMS data
using the calculation procedures in EPA Method 19 Section 5 and Section
4 of this appendix.
E2=the hourly emission rate from Unit 2 as determined from CEMS data
using the calculation procedures in EPA Method 19 Section 5 and in
Section 4 of this appendix.
H1=the hourly heat input to Unit 1 as determined in Section 4 of this
appendix.
H2=the hourly heat input to Unit 2 as determined by Section 4 of this
appendix.
If data for any of the four hourly parameters (E1, E2, H1, and H2)
under 3.2 are unavailable during an hourly period, the combined emission
rate (EC) is not calculated and the period is counted as missing data
under 4.6.1., except as provided under 3.5.6.
3.4 After the date of initial operation subject to the combined
emission limit, the owner or operator shall remain subject to the
requirements of this appendix unless the owner or operator of the
affected facility elects to revert to the 520 ng/J heat input (1.2 lb/MM
Btu) limit of 60.43(a)(2) separately at each unit. The Administrator
shall be given written notification from CIPS as soon as practical of
their decision to revert to the 520 ng/J heat input (1.2 lb/MM Btu)
limit of 60.43(a)(2) separately at each unit, but no later than 10 days
in advance of the date such election is to take effect.
3.5 Emission monitoring data for Unit 1 may be excluded from
calculations of the 30 day rolling average only during the following
times:
3.5.1 Periods of DAFGDS startup.
3.5.2 Periods of DAFGDS shutdown.
3.5.3 Periods of DAFGDS malfunction during system emergencies as
defined in 60.41a.
3.5.4 The first 250 hours per calendar year of DAFGDS malfunctions of
Unit 1 DAFGDS provided that efforts are made to minimize emissions from
Unit 1 in accordance with 60.11(d) , and if, after 16 hours of DAFGDS
malfunction, the owner or operator of the affected facility begins
loading coal (following the customary loading procedures, but not more
than 24 hours later) with a potential SO2 emission rate equal to or less
than the current emission rate of Unit 2 (E2) into the Unit 1 coal
bunker. Malfunction periods under 3.5.3 are not counted toward the 250
hour/yr limit under this section.
3.5.5 The malfunction exemption in 3.5.4 is limited to the first 250
hours per calendar year of DAFGDS malfunction. During the first 250
hours, except for the initial 16 hours of each Unit 1 DAFGDS
malfunction, the owner or operator shall load coal with a potential SO2
emission rate equal to or less than the current emission rate of Unit 2
(E2) into the Unit 1 coal bunkers. For malfunctions of the DAFGDS after
the 250 hours per calendar year limit (cumulative), other than those
defined in 3.5.3, the owner or operator of the affected facility shall
combust lower sulfur coal or use any other method to comply with the 470
ng/J (1.1 lb/million Btu) combined emission limit.
3.5.6 During the first 250 hours of DAFGDS malfunction per year or
during periods of DAFGDS startup, or DAFGDS shutdown, CEMS emissions
data from Unit 2 shall continue to be included in the daily calculation
of the combined 30 day rolling average emission rate; that is, the load
on Unit 1 is assumed to be zero (H1=0; EC=E2).
3.5.7 The provision for excluding CEMS data from Unit 1 during the
first 250 hours of DAFGDS malfunctions from combined hourly emissions
calculations supercedes the provisions of 60.11(d). However, the
general purpose contained in 60.11(d) (i.e., following good control
practices to minimize air pollution emissions even during malfunctions)
has not been superseded.
4.1 The CEMS required under Section 3.2 are operated and data are
recorded for all periods of operation of the affected facility including
periods of the DAFGDS startup, shutdown and malfunction except for CEMS
breakdowns, repairs, calibration checks, and zero and span adjustment.
All provisions of 60.45 apply except as follows:
4.2 The owner or operator shall install, calibrate, maintain, and
operate CEMS and monitoring devices for measuring the following:
4.2.1 For Unit 1:
4.2.1.1 Sulfur dioxide and oxygen or carbon dioxide for the Unit 1
DAFGDS stack.
4.2.1.2 Sulfur dioxide, oxygen or carbon dioxide, volumetric flow
rate, and static pressure and temperature for the Unit 1 DAFGDS by-pass
stack.
4.2.1.3 Volumetric flow rate, static pressure, and temperature at the
inlet ducts to the Unit 1 DAFGDS.
4.2.2 For Unit 2, sulfur dioxide and oxygen or carbon dioxide.
4.2.3 For Units 1 and 2, the hourly heat input, the hourly steam
production rate, or the hourly gross electrical power output from each
unit.
4.3 For the Unit 1 by-pass stack and the Unit 2 stack, the span value
of the sulfur dioxide monitoring system is 200 percent of the maximum
estimated hourly potential sulfur dioxide emissions of the fuel fired.
For the Unit 1 DAFGDS stack, the span value is 50 percent of the maximum
estimated hourly potential emissions of the fuel fired.
4.3.1 For the Unit 1 DAFGDS stack, an additional SO2 monitor with a
span value of 200 percent of the maximum hourly potential emissions of
the fuel fired is required. During initial application of 60.43(e),
this requirement is considered to be satisfied if:
(1) Within 90 days of initial election to operate under 60.43(e),
the owner or operator of the affected facility submits a monitoring plan
to the Administrator to install, maintain, and operate a CEMS with a
span value of 200 percent or operate an alternative monitoring system
capable of measuring such values;
(2) The plan is approved by the Administrator within 60 days of
receipt of the plan; and
(3) During the period before the plan is approved, the owner or
operator of the affected facility operates Methods 6 and 3, 8 and 3, or
8A on an hourly basis during all periods emissions exceed 50 percent of
the maximum hourly potential emission rate of the fuel fired.
4.3.2 If an alternative monitoring plan under 4.3.1 is not approved
by the Administrator within 150 days of initial election to operate
under 60.43(e), or if a separate CEMS with a span value of 200 percent
has not been installed and made operational, Unit 1 and Unit 2 will
become subject to the requirements of 60.43(a)(2).
4.4 The monitoring devices required in 4.2 shall be installed,
calibrated, and maintained as follows:
4.4.1 The volumetric flow rate monitoring device specified in 4.2.1.2
(DAFGDS bypass stack) shall be installed at the same location as the
sulfur dioxide emission monitor.
4.4.2 The volumetric flow rate monitoring devices shall be calibrated
using Reference Methods 1 and 2 (appendix A). The traverse location for
Method 2 shall be as near as practicable to the monitoring device
location, and such that no gas flow is added or diverted between the
measurement sites. The average gas velocity or volumetric flow rate by
Method 2 shall be used to calculate a calibration coefficient for the
monitoring device. Average gas molecular weight and moisture content
may be used to calculate the gas density for use in the velocity or flow
rate equations of Method 2.
4.4.3 The volumetric flow rate calibrations shall be conducted prior
to the start of the initial performance test required in 3.2, and
annually thereafter.
4.4.4 Temperature and pressure monitoring devices shall be calibrated
and maintained according to manufacturer's specifications.
4.4.5 Hourly steam production rate or hourly electrical power output
monitoring devices for Unit 1 and Unit 2 shall be calibrated and
maintained according to manufacturer's specifications. The data from
either of these devices may be used for the hourly heat input rates used
in the calculation of the combined emission rate in Section 3.3 unless
the hourly heat input to steam production or hourly heat input to
electrical power output efficiency over a given segment of each boiler
or generator operating range, respectively, varies by more than 5
percent within the specified operating range, or the efficiencies of the
boiler/generator units differ by more than 5 percent. The hourly heat
input may also be calculated based on the fuel firing rates and fuel
analysis.
4.5 The Calculation procedures of Method 19, appendix A are combined
with the volumetric flow rate monitoring device results to calculate an
emission rate for Unit 1 when leakage or diversion of any DAFGDS inlet
gas to the bypass stack occurs (such as during conditions under 3.5.3,
3.5.4, and 3.5.6):
For Unit 1, hourly SO2 emission rate (E1) is calculated as follows:
Where
QB=Dry volumetric bypass stack gas flow rate corrected to standard
conditions, dscm/hr (dscf/hr).
QF=Dry volumetric DAFGDS inlet gas flow rate corrected to standard
conditions, dscm/hr (dscf/hr).
EF=Hourly SO2 emission rate measured in DAFGDS stack, ng/J
(lb/million Btu).
EB=Hourly SO2 emission rate measured in bypass stack ng/J (lb/million
Btu),
Other than during conditions under 3.5.1, 3.5.2, 3.5.3, 3.5.4, or
3.5.5, the DAFGDS bypass system is not used and no leakage through the
bypass damper should be indicated by either the bypass stack static
pressure, temperature, or SO2 measurements, and:
E1=EF
4.6 For the CEMS required for Unit 1 and Unit 2, the owner or
operator of the affected facility shall maintain and operate the CEMS
and obtain combined emission data values (EC) for at least 75 percent of
the boiler operating hours per day for at least 26 out of each 30
successive boiler operating days.
4.6.1 When hourly SO2 emission data are not obtained by the CEMS
because of CEMS breakdowns, repairs, calibration checks and zero and
span adjustments, hourly emission data required by 4.6 are obtained by
using Methods 6 and 3, 6A, or 8 and 3, or by other monitoring procedures
approved by the Administrator. Failure to obtain the minimum data
requirements of 4.6 by CEMS, or by CEMS supplemented with alternative
methods of this section, is a violation of performance testing
requirements.
4.6.2 Independent of complying with the minimum data requirements of
4.6, all valid emissions data collected are used to calculate combined
hourly emission rates (EC) and 30-day rolling average emission rates
(E30) are calculated and used to judge compliance with 60.43(e).
4.7 For each continuous emission monitoring system, a quality
assurance plan shall be prepared by CIPS and approved by the
Administrator. The plan is to be submitted to the Administrator 45 days
before initiation of the intial performance test. At a minimum, the
plan shall contain the following quality control elements:
4.7.1 Calibration of continuous emission monitoring systems (CEMS).
4.7.2 Calibration drift determination and adjustment of CEMS.
4.7.3 Periodic CEMS relative accuracy determinations.
4.7.4 Preventive manitenance of CEMS (including spare parts
inventory).
4.7.5 Data recording and reporting.
4.7.6 Program of corrective action for malfunctioning CEMS.
4.7.7 Criteria for determining when the CEMS are not producing valid
data.
4.8 For the purpose of conducting the continuous emission monitoring
system performance specification tests as required by 60.13 and
appendix B, the following conditions apply:
4.8.1 The calibration drift specification of Specification 2,
appendix B shall be determined separately for the Unit 1 SO2/diluent
systems and the Unit 2 SO2/diluent system.
4.8.2 The relative accuracy of Specification 2, appendix B shall
apply to the calculated combined emission rate for Unit 1 and Unit 2.
The required relative accuracy is 20 percent using the procedures in
Specification 2 simultaneously at Unit 1 and Unit 2.
4.8.3 If, during the instrument performance test period, the DAFGDS
bypass stack gas volumetric flow rate monitoring device indicates a
detectable flow or if the temperature or SO2 concentration in the bypass
stack indicates that leakage to the bypass is occurring or if the static
pressures in the DAFGDS inlet ducts are positive, then the relative
accuracy determination for the Unit 1 CEMS must include the DAFGDS
bypass combination. To determine the relative accuracy of the Unit 1
flow combination:
4.8.3.1 Determine the volumetric flow rate using Method 2 at the
bypass stack and the DAFGDS inlet ducts concurrently with the Method 6
tests required at the DAFGDS and bypass stacks.
4.8.3.2 Compute ''E (Unit 1)'' (Section 4.5) using the reference
methods results.
4.8.3.3 Compute ''E (Unit 1)'' using the concurrent CEMS and flow
rate monitoring device results.
4.8.3.4 Compute the relative accuracy as outlined in Specification 2
using the results in 4.8.3.2 and 4.8.3.3. The resulting relative
accuracy for this separate system must be within 20 percent.
5.1 The plant owner or operator shall keep a record of each hourly
emission rate and each hourly Btu heat input rate, hourly steam rate, or
hourly electrical power output for Unit 1 and for Unit 2, and a record
of each hourly weighted average emission rate. These records shall be
kept for all periods of operation of Unit 1 or 2, including emissions of
Unit 1 (E1) during periods of DAFGDS startup, shutdown, and malfunction
when H1 is assumed to be zero (0) (see 4.5).
5.2 The plant owner or operator shall keep a record of each hourly
gas flow rate to the DAFGDS, each hourly stack gas flow rate to the
bypass stack during any periods that the DAFGDS bypass damper is opened,
and reason for bypass operation.
6.1 The owner or operator of any affected facility shall submit the
written reports required under 6.2 of this section and subpart A to the
Administrator for every calendar quarter. All quarterly reports shall
be submitted by the 30th day following the end of each calendar quarter.
6.2 For sulfur dioxide, the following data are submitted to the
Administrator for each 24-hour period:
6.2.1 Calendar date
6.2.2 The combined average sulfur dioxide emission rate (ng/J or
lb/million Btu) for the past 30 successive boiler operating days (ending
with the last 30-day period in the quarter); and, for any noncompliance
periods, reasons for noncompliance with the emission standards and
description of corrective action taken.
6.2.3 Identification of the boiler operating days for which valid
sulfur dioxide emissions data required by 4.6 have not been obtained for
75 percent of the boiler operating hours; reasons for not obtaining
sufficient data; and description of corrective actions taken to prevent
recurrence.
6.2.4 Identification of the time periods (hours) when Unit 1 or Unit
2 were operated but combined hourly emission rates (EC) were not
calculated because of the unavailability of parameters E1, E2, H1, or H2
as described in 3.2.
6.2.5 Identification of the time periods (hours) when Unit 1 and Unit
2 were operated and where the combined hourly emission rate (EC)
equalled Unit 2 (E2) emissions because of the Unit 1 malfunction
provisions under 3.5.3, 3.5.4, and 3.5.5.
6.2.6 Identification of the time periods (hours) when emissions from
the Unit 1 DAFGDS have been excluded from the calculation of average
sulfur dioxide emisison rates because of Unit 1 DAFGDS startup,
shutdown, malfunction, or other reasons; and justification for
excluding data for reasons other than startup or shutdown. Reporting of
hourly emission rate of Unit 1 (E1) during each hour of the DAFGDS
startup, shutdown, or malfunction under 3.5.1, 3.5.2, 3.5.3, 3.5.4, and
3.5.5 (see 4.5).
6.2.7 Identification of the number of days in the calendar quarter
that the affected facility was operated (any fuel fired).
6.2.8 Identify any periods where Unit 1 DAFGDS malfunctions occurred
and the cumulative hours of Unit 1 DAFGDS malfunction for the quarter.
6.2.9 Identify any periods of time that any exhaust gases were
discharged to the DAFGDS bypass stack and the hourly gas flow rate to
the DAFGDS and to the DAFGDS bypass during such periods and reason for
bypass operation.
6.2.10 Identification of each hourly emission rate (E1) and average
heat input rate (H1) for Unit 1, each hourly average emission rate (E2)
and average heat input rate (H2) for Unit 2, and each hourly weighted
average emission rate (EC).
(52 FR 28955, Aug. 4, 1987)
40 CFR 60.748 Appendix H (Reserved)
40 CFR 60.748 Pt. 60, App. I
40 CFR 60.748 Appendix I -- Removable Label and Owner's Manual
The purpose of this appendix is to provide guidance to the
manufacturer for compliance with the temporary labeling and owner's
manual provisions of subpart AAA. Section 2 provides guidance for the
content and presentation of information on the temporary labels.
Section 3 provides guidance for the contents of the owner's manual.
Temporary labels shall be printed on 90 pound bond paper and shall
measure 5 inches wide by 7 inches long. All labels shall be printed in
black ink on one side of the label only. The type font that shall be
used for all printing is helvetica. Specific instructions for drafting
labels are provided below depending upon the compliance status of the
wood heater model. Figures 1 through 7 illustrate the various label
types that may apply.
The design and content of certified wood heaters vary according to
the following:
Catalyst or noncatalyst,
Measured or default thermal efficiency value, and
Compliance with 1988 or 1990 emission limit.
There are five parts of a label. These include:
Identification and compliance status,
Emission value,
Efficiency value,
Heat output value, and
Caveats.
Instructions for drafting each of these five parts are discussed
below in terms of the three variables listed above. Figures 1 and 2
illustrate the variations in label design. Figure 1 is a temporary
label for a hypothetical catalyst wood heater that meets the 1990
standard, has a certification test emission composite value of 3.5 g/h,
and has a default efficiency of 72 percent. The label in Figure 2 is
for a hypothetical noncatalyst wood heater with a certification test
emission composite value of 7.8 g/h and a measured efficiency of 68
percent. It meets the 1988 but not the 1990 standard. All labels for
wood heaters that have been certified and tested should conform as much
as possible to the general layout, the type font and type size
illustrated in Figures 1 and 2.
The top 1.5 inches of the label should contain the following items
(and location on the label):
Manufacturer name (upper left hand corner,
Model name/number (upper left hand corner,
The words ''U.S. ENVIRONMENTAL PROTECTION AGENCY'' (centered at top
and enclosed in a box with rounded edges),
For catalytic wood heaters, in large bold print the words ''CATALYST
EQUIPPED'' (centered below the words ''U.S. ENVIRONMENTAL PROTECTION
AGENCY''),
Text indicating compliance status for catalytic wood heaters. For
those catalytic wood heaters which comply with the 1988 emission limits,
but not the 1990 emission limits, the words: ''Meets EPA particulate
matter (smoke) control requirements for catalytic wood heaters built on
or after July 1, 1988, and before July 1, 1990.'' For those catalytic
wood heaters which comply with the 1990 emission limits, the words:
''Meets EPA particulate matter (smoke) control requirements for
catalytic wood heaters built on or after July 1, 1990.'' Finally, for
all catalytic wood heaters, the following text should be included:
''See catalyst warranty. Illegal to operate when catalyst is not
working. See owner's manual for operation and maintenance.''
Text indicating compliance status for noncatalytic wood heaters. For
those noncatalytic wood heaters that comply with the 1988 emission
limits but not the 1990 emission limits, the words: ''Meets EPA
particulate matter (smoke) control requirements for NONCATALYTIC wood
heaters built on or after July 1, 1988, and before July I, 1990.'' For
those noncatalytic wood heaters that comply with 1990 emission limits,
the words: ''Meets EPA particulate matter (smoke) control requirements
for NONCATALYTIC wood heaters built on or after July 1, 1990.''
Between 1.5 and 3.0 inches down from the top of the label is the part
that graphically illustrates the particulate matter, or smoke, emission
value. This part consists of the word ''SMOKE'' in large bold print and
a 3.0 inch line with words ''(grams per hour)'' centered beneath the
line. A blunt end arrow with a base (blunt end) that spans 2 g/hr shall
be centered over the point on the emissions line that represents the
composite emission value for the model as measured in the certification
test.
For catalyst equipped wood heaters the 3.0 inch line shall be labeled
''0'' on the left end of the line (centered below the end) and ''5.5''
on the right end (centered below the end). To find where to center the
large blunt end arrow, measure 0.55 inches from the left end for each
g/h of the composite emission value. Thus, a 4 g/h value would be 2.2
inches from the left end. The base of the blunt end should always be
1.1 inches wide (2 g/hr). The words ''This Model'' should be centered
above or within the blunt end arrow.
For noncatalyst equipped wood heaters, the 3.0 inch line should be
labeled ''0'' on the left end of the line (centered below the end) and
''8.5'' on the right end of the line (centered below the end). To find
where to center the large blunt end arrow, measure 0.35 inches from the
left end for each g/h of the composite emission value. Thus, a 4 g/h
value would be 1.4 inches from the left end. The base of the blunt end
should always be 0.7 inches wide (2 g/h). The words ''This Model''
should be centered above or within the blunt end arrow.
Between 3.0 and 4.75 inches down from the top of the label is the
part that illustrates overall thermal efficiency value. The efficiency
value may either be a measured value or a calculated or default value as
provided in 60.536(i)(3) of the regulation. Regardless of how the
efficiency is derived, the words ''EFFICIENCY'' shall be centered above
a 4 inch line. The 4 inch line should be divided into 5 equal lengths
(each 0.8 inches) and labeled ''50%,'' ''60%,'' * * * ''100%'' as
indicated in Figures 1 and 2. As with the smoke line in 2.2.2, a blunt
end arrow shall be centered over the point on the line where the
efficiency value would be located. The base of the blunt end arrow
shall be 0.48 inches wide (6 percentage points). To find where to
center the blunt end arrow, measure 0.08 inches for each percentage
point to the right of the nearest labeled value. For example, a value
of 82 percent would be 0.16 inches to the right of the ''80%'' mark.
For default efficiency values, an asterisk shall follow the word
''EFFICIENCY'' as in Figure 1. The asterisk refers to a note in
parentheses that shall say ''Not tested for efficiency. Value indicated
is for similar catalyst equipped (or noncatalytic, as appropriate) wood
heaters.''
For measured efficiency values measured with the method in appendix
J, the words ''Tested Efficiency'' shall be centered above the blunt end
arrow as in Figure 2.
The last item required for this part is a sentence that says ''Wood
heaters with higher efficiencies cost less to operate.''
Between 4.75 and 6.0 inches down from the top of the label is the
heat output part. The words ''HEAT OUTPUT'' in large bold print are
centered above the Heat Output range numbers in Btu/hr, as derived from
the certification test. The words ''Use this to choose the right size
appliance for your needs. ASK DEALER FOR HELP'' should follow the heat
output range numbers as in Figures 1 and 2. (Note that ''ASK DEALER FOR
HELP'' is a single line, centered in the label.) The low end of the burn
rate range indicated on the label should reflect the low end of the burn
rate range achievable by the wood heater as sold and not as tested in
the laboratory (see 60.536(i)(4)).
In the lower 0.75 inch of the label, the following text shall be
presented:
''This wood heater will achieve low smoke output and high efficiency
only if properly operated and maintained. See owner's manual.''
For those heaters which meet the definition of ''coal only heater''
in 60.531, the temporary label should contain the identical material
(same layout and print font and size) as that illustrated in Figure 3,
except that the hypothetical manufacturer and model name should be
replaced with the appropriate actual names.
For those wood heaters exempted under 60.530(d), the small
manufacturer exemption, the temporary label should contain the identical
material (same layout and print font and size) as that illustrated in
Figure 4, except that the hypothetical manufacturer and model name
should be replaced with the appropriate actual names.
For those wood heaters that do not meet applicable emission limits
under 60.532 and are not otherwise exempted, the temporary label should
contain the identical material (same layout and print font and size) as
those illustrated in Figures 5, 6, and 7, as appropriate. The
hypothetical manufacturer and model names should be replaced with the
appropriate actual names.
There are three kinds of wood heaters which fall into this category
of ''not certified.'' Each requires a separate label. If a wood heater
is tested but fails to meet the applicable limits, the label in Figure 5
applies. Such a label should be printed on red rather than white paper.
If a wood heater is tested and does meet the emission limit but is not
subsequently certified, the label in Figure 6 applies. (An example
would be a one-of-a-kind wood heater which is not part of a model line.
Because of the costs of testing, this circumstance is not expected to
arise often, if at all.) If a wood heater is not tested and is not
certified, it should bear the label illustrated in Figure 7. As with
Figure 5, this label should be printed on red paper.
Although the owner's manuals do not require premarket approval, EPA
will monitor the contents to ensure that sufficient information is
included to provide heater operation and maintenance information
affecting emissions to consumers. The purpose of this section is to
provide guidance to manufacturers in complying with the owner's manual
provisions of 60.536(1). A checklist of topics and illustrative
language is provided as a guideline. Owner's manuals should be tailored
to specific wood heater models, as appropriate.
Wood heater description and compliance status,
Tamper warning,
Catalyst information and warranty (if catalyst equipped),
Fuel selection,
Achieving and maintaining catalyst light-off (if catalyst equipped),
Catalyst monitoring (if catalyst equipped),
Troubleshooting catalytic equipped heaters (if catalyst equipped),
Catalyst replacement (if catalyst equipped),
Wood heater operation and maintenance, and
Wood heater installation: achieving proper draft.
The following are example texts and/or further descriptions
illustrating the topics identified above. Although the regulation
requires manufacturers to address (where applicable) the ten topics
identified above, the exact language is not specified. Manuals should
be written specific to the model and design of the wood heater. The
following guidance is composed of generic descriptions and texts. If
manufacturers choose to use the language provided in the example, the
portion in italics should be revised as appropriate. Any manufacturer
electing to use the EPA example language shall be in compliance with
owner's manual requirements provided that the particular language is
printed in full with only such changes as are necessary to ensure
accuracy. Example language is not provided for certain topics, since
these areas are generally heater specific. For these topics,
manufacturers should develop text that is specific to the operation and
maintenance of their particular products.
Owner's Manuals shall include:
A. Manufacturer and model,
B. Compliance status (exempt, 1988 std., 1990 std., etc.), and
C. Heat output range (as indicated on temporary label).
Example Text covering A, B, and C above:
''This manual describes the installation and operation of the Brand
X, Model 0 catalytic equipped wood heater. This heater meets the U.S.
Environmental Protection Agency's emission limits for wood heaters sold
between July 1, 1990, and July 1, 1992. Under specific test conditions
this heater has been shown to deliver heat at rates ranging from 8,000
to 35,000 Btu/hr.''
This consists of the following statement which must be included in
the owner's manual for catalyst equipped units:
Example Text covering legal prohibition on tampering:
''This wood heater contains a catalytic combustor, which needs
periodic inspection and replacement for proper operation. It is against
the law to operate this wood heater in a manner inconsistent with
operating instructions in this manual, or if the catalytic element is
deactivated or removed.''
Included with or supplied in the owner's and warranty manuals shall
be the following information:
A. Catalyst manufacturer, model,
B. Catalyst warranty details, and
C. Instructions for warranty claims.
Example Text covering A, B, and C:
''The combustor supplied with this heater is a Brand Z, Long Life
Combustor. Consult the catalytic combustor warranty also supplied with
this wood heater. Warranty claims should be addressed to:
Stove or Catalyst Manufacturer
Address
Phone
This section should also provide clear guidance on how to exercise
the warranty (how to package for return shipment, etc.).
Owner's manuals shall include:
A. Instructions on acceptable fuels, and
B. Warning against inappropriate fuels.
Example Text covering A and B:
''This heater is designed to burn natural wood only. Higher
efficiencies and lower emissions generally result when burning air dried
seasoned hardwoods, as compared to softwoods or to green or freshly cut
hardwoods.
DO NOT BURN:
Treated Wood.
Coal.
Garbage.
Cardboard.
Solvents.
Colored Paper.
Trash.
Burning treated wood, garbage, solvents, colored paper or trash may
result in release of toxic fumes and may poison or render ineffective
the catalytic combustor.
Burning coal, cardboard, or loose paper can produce soot, or large
flakes of char or fly ash that can coat the combustor, causing smoke
spillage into the room, and rendering the combustor ineffective.''
Owner's manuals shall describe in detail proper procedures for:
A. Operation of catalyst bypass (stove specific),
B. Achieving catalyst light-off from a cold start, and
C. Achieving catalyst light-off when refueling.
No example text is supplied for describing operation of catalyst
bypass mechanisms (Item A) since these are typically stove-specific.
Manufacturers however must provide instructions specific to their model
describing:
1. Bypass position during start-up,
2. Bypass position during normal operation, and
3. Bypass position during reloading.
Example Text for item B:
''The temperature in the stove and the gases entering the combustor
must be raised to between 500 to 700 F for catalytic activity to be
initiated. During the start-up of a cold stove, a medium to high firing
rate must be maintained for about 20 minutes. This ensures that the
stove, catalyst, and fuel are all stabilized at proper operating
temperatures. Even though it is possible to have gas temperatures reach
600 F within two to three minutes after a fire is started, if the fire
is allowed to die down immediately it may go out or the combustor may
stop working. Once the combustor starts working, heat generated in it
by burning the smoke will keep it working.''
Example Text for item C:
REFUELING:
''During the refueling and rekindling of a cool fire, or a fire that
has burned down to the charcoal phase, operate the stove at a medium to
high firing rate for about 10 minutes to ensure that the catalyst
reaches approximately 600 F.''
Owner's manuals shall include:
A. Recommendation to visually inspect combustor at least three times
during the heating season,
B. Discussion on expected combustor temperatures for monitor-equipped
units, and
C. Suggested monitoring and inspection techniques.
Example Text covering A, B, and C:
''It is important to periodically monitor the operation of the
catalytic combustor to ensure that it is functioning properly and to
determine when it needs to be replaced. A non-functioning combustor
will result in a loss of heating efficiency, and an increase in creosote
and emissions. Following is a list of items that should be checked on a
periodic basis.
Combustors should be visually inspected at least three times during
the heating season to determine if physical degradation has occurred.
Actual removal of the combustor is not recommended unless more detailed
inspection is warranted because of decreased performance. If any of
these conditions exist, refer to Catalyst Troubleshooting section of
this owner's manual.
This catalytic heater is equipped with a temperature probe to monitor
catalyst operation. Properly functioning combustors typically maintain
temperatures in excess of 500 F, and often reach temperatures in excess
of 1,000 F. If catalyst temperatures are not in excess of 500 F,
refer to Catalyst Troubleshooting section of this owner's manual.
You can get an indication of whether the catalyst is working by
comparing the amount of smoke leaving the chimney when the smoke is
going through the combustor and catalyst light-off has been achieved, to
the amount of smoke leaving the chimney when the smoke is not routed
through the combustor (bypass mode).
Step 1 -- Light stove in accordance with instructions in 3.3.5.
Step 2 -- With smoke routed through the catalyst, go outside and
observe the emissions leaving the chimney.
Step 3 -- Engage the bypass mechanism and again observe the emissions
leaving the chimney.
Significantly more smoke should be seen when the exhaust is not
routed through the combustor (bypass mode). Be careful not to confuse
smoke with steam from wet wood.''
The owner's manual should provide clear descriptions of symptoms and
remedies to common combustor problems. It is recommended that
photographs of catalyst peeling, plugging, thermal cracking, mechanical
cracking, and masking be included in the manual to aid the consumer in
identifying problems and to provide direction for corrective action.
The owner's manual should provide clear step-by-step instructions on
how to remove and replace the catalytic combustor. The section should
include diagrams and/or photographs.
Owner's manual shall include:
A. Recommendations about building and maintaining a fire,
B. Instruction on proper use of air controls,
C. Ash removal and disposal,
D. Instruction on gasket replacement, and
E. Warning against overfiring.
No example text is supplied for A, B, and D since these items are
model specific. Manufacturers should provide detailed instructions on
building and maintaining a fire including selection of fuel pieces, fuel
quantity, and stacking arrangement. Manufacturers should also provide
instruction on proper air settings (both primary and secondary) for
attaining minimum and maximum heat outputs and any special instructions
for operating thermostatic controls. Step-by-step instructions on
inspection and replacement of gaskets should also be included.
Manufacturers should provide diagrams and/or photographs to assist the
consumer. Gasket type and size should be specified.
Example Text for item C:
''Whenever ashes get 3 to 4 inches deep in your firebox or ash pan,
and when the fire has burned down and cooled, remove excess ashes.
Leave an ash bed approximately 1 inch deep on the firebox bottom to help
maintain a hot charcoal bed.''
''Ashes should be placed in a metal container with a tight-fitting
lid. The closed container of ashes should be placed on a noncombustible
floor or on the ground, away from all combustible materials, pending
final disposal. The ashes should be retained in the closed container
until all cinders have thoroughly cooled.''
Example Text covering item E:
''DO NOT OVERFIRE THIS HEATER''
''Attempts to achieve heat output rates that exceed heater design
specifications can result in permanent damage to the heater and to the
catalytic combustor if so equipped.''
Owner's manual shall include:
A. Importance of proper draft,
B. Conditions indicating inadequate draft, and
C. Conditions indicating excessive draft.
Example Text for Item A:
''Draft is the force which moves air from the appliance up through
the chimney. The amount of draft in your chimney depends on the length
of the chimney, local geography, nearby obstructions, and other factors.
Too much draft may cause excessive temperatures in the appliance and
may damage the catalytic combustor. Inadequate draft may cause
backpuffing into the room and 'plugging' of the chimney or the
catalyst.''
Example text for Item B:
''Inadequate draft will cause the appliance to leak smoke into the
room through appliance and chimney connector joints.''
Example text Item C:
''An uncontrollable burn or a glowing red stove part or chimney
connector indicates excessive draft.''
Insert illus) 0230
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(53 FR 5913, Feb. 26, 1988)
40 CFR 60.748 FINDING AIDS
A list of CFR titles, subtitles, chapters, subchapters and parts and
an alphabetical list of agencies publishing in the CFR are included in
the CFR Index and Finding Aids volume to the Code of Federal Regulations
which is published separately and revised annually.
Material Approved for Incorporation by Reference
Table of CFR Titles and Chapters
Alphabetical List of Agencies Appearing in the CFR
List of CFR Sections Affected
Title 40 -- Protection of Environment
Material Approved for Incorporation by Reference
Material Approved for Incorporation by Reference
The Director of the Federal Register has approved under 5 U.S.C.
552(a) and 1 CFR Part 51 the incorporation by reference of the following
publications. This list contains only those incorporations by reference
effective as of the revision date of this volume. Incorporations by
reference found within a regulation are effective upon the effective
date of that regulation. For more information on incorporation by
reference, see the preliminary pages of this volume.
40 CFR 60.748 40 CFR, CHAPTER I (PARTS 60): SUBCHAPTER C -- AIR
PROGRAMS
ENVIRONMENTAL PROTECTION AGENCY
40 CFR
American Petroleum Institute
1220 L Street, N.W., Washington, D.C. 20005
API Publication 2517, Evaporation Loss from External Floating-Roof
Tanks, Second Edition, February 1980 60.17; 60.111(1); 60.111a(g);
60.111b(g); 60.116b(f)(2)(ii)
American Public Health Association, American Water Works Association,
and Water Pollution Control Federation
1015 Fifteenth Street, N.W., Washigton, D.C. 20005
Standard Methods for the Examination of Waste and Wastewater, 15th
ed. (1980) Method 209A, Total Residue Dried at 103 to 105 C
60.17(e)(1); 60.683(b)
American Society of Mechanical Engineers
United Engineering Center, 345 E. 47th St., New York, NY 10017
ASME Interim Supplement 19.5 on Instruments and Apparatus;
Application, Part II of Fluid Meters, 6th Edition (1971) 60.17;
60.58a(h)
ASME Power Test Code 4.1: Test Code for Steam Generating Units,
August 8, 1972 60.17; 60.46(b); 60.58a(h)
ASME QRO-1-1989 Standard for the Qualification and Certification of
Resource Recovery Facility Operators 60.17; 60.56a(d)
American Society for Testing and Materials
1916 Race Street, Philadelphia, Pennsylvania 19103
ASTM A99-76, Standard Specification for Ferromanganese 60.261
ASTM A100-69 (Reapproved 1974), Standard Specification for
Ferrosilicon 60.261
ASTM A101-73, Standard Specification for Ferrochromium 60.261
ASTM A482-76, Standard Specification for Ferrochromesilicon 60.261
ASTM A483-64 (Reapproved 1974), Standard Specification for
Silicomanganese 60.261
ASTM A495-76, Standard Specification for Calcium-Silicon and Calcium
Manganese-Silicon 60.261
ASTM D86-78, Distillation of Petroleum Products 60.17(a); 60.593(d);
60.633(h)
ASTM D129-64 (Reapproved 1978), Standard Test Method for Sulfur in
Petroleum Products (General Bomb Method) Appendix A to Part 60, Method
19; 60.17(a)(56); 60.106(h)(2)
ASTM D240-76, Standard Test Method for Heat of Combustion of Liquid
Hydrocarbon Fuels by Bomb Calorimeter 60.46(g); 60.296(f); Appendix A
to Part 60, Method 19
ASTM D270-65 (Reapproved 1975), Standard Method of Sampling Petroleum
and Petroleum Products Appendix A to Part 60, Method 19
ASTM D323-82 Test Method for Vapor Pressure of Petroleum Products
(Reid Method) 60.17(a)(13); 60.111(l); 60.111a(g); 60.111b(g);
60.116b(f)(2)(ii)
ASTM D388-77, Standard Specification for Classification of Coals by
Rank 60.17(a); 60.41(f); 60.45(f)(4) (i), (ii), (vi); 60.41a;
60.41b; 60.41c; 60.251 (b), (c)
ASTM D396-78, Standard Specification for Fuel Oils 60.17(a); 60.40b;
60.41b; 60.41c; 60.111(b); 60.111a(b)
ASTM D975-78, Standard Specification for Diesel Fuel Oils 60.111(b);
60.111a(b)
ASTM D1072-56 (Reapproved 1975), Standard Test Method for Total
Sulfur in Fuel Gases 60.335(b)(2)
ASTM D1137-53 (Reapproved 1975), Standard Method for Analysis of
Natural Gases and Related Types of Gaseous Mixtures by the Mass
Spectrometer 60.45(f)(5)(i)
ASTM D1193-77, Standard Specification for Reagent Water 60.17(a)(22);
Appendix A to Part 60, Method 6, par. 3.1.1; Method 7, par. 3.2.2;
Method 7C, par. 3.1.1; Method 7D, par. 3.1.1; Method 8, par. 3.1.3;
Method 12, par. 4.1.3; 61.18(a)(2); Method 101, par. 6.1.1; Method
101A, par. 6.1.1; Method 104, par. 3.1.2
ASTM D1266-87, Standard Test Method for Sulfur in Petroleum Products
(Lamp Method) 60.17(a)(57); 60.106(h)(2)
ASTM D1475-60 (Reapproved 1980), Standard Test Method for Density of
Paint, Varnish, Lacquer, and Related Products 60.435(d)(1); 60.485(d);
Appendix A to Part 60, Method 24, par. 2.1, and Method 24A, par. 2.2
ASTM D1552-83, Standard Test Method for Sulfur in Petroleum Products
(High-Temperature Method) Appendix A to Part 60, Method 19;
60.17(a)(58); 60.106(h)(2)
ASTM D1608-77, Standard Test Method for Oxides of Nitrogen in Gaseous
Combustion Products (Phenol-Disulfonic Acid Procedures) Method 7, par.
3.2.2
ASTM D1826-77, Standard Test Method for Calorific Value of Gases in
Natural Gas Range by Continuous Recording Calorimeter 60.45(f)(5)(ii);
60.46(g); 60.296(f); Appendix A to Part 60, Method 19
ASTM D1835-86, Standard Specification for Liquefied Petroleum (LP)
Gases 60.17(a)(49); 60.41b; 60.41c
ASTM D1945-64 (Reapproved 1976), Standard Method for Analysis of
Natural Gas by Gas Chromatography 60.45(f)(5)(i)
ASTM D1946-77, Standard Method for Analysis of Reformed Gas by Gas
Chromatography 60.17(a)(6); 60.18(f); 60.45(f)(5)(i);
60.614(d)(2)(ii) and (d)(4); 60.664(d)(2)(ii) and (d)(4)
ASTM D2013-72, Standard Method of Preparing Coal Samples for Analysis
Appendix A to Part 60, Method 19
ASTM D2015-77, Standard Test Method for Gross Calorific Value of
Solid Fuel by the Adiabatic Bomb Calorimeter 60.45(f)(5)(ii); 60.46(g);
Appendix to Part 60, Method 19
ASTM D2016-74 (Reapproved 1983), Standard Text Methods for Moisture
Content of Wood 60.17(a)(53); Appendix A to Part 60, Method 28
ASTM D2234-76, Standard Methods for Collection of a Gross Sample of
Coal Appendix A to Part 60, Method 19
ASTM D2369-81, Standard Test Method for Volatile Content of Coatings
Appendix A to Part 60, Method 24
ASTM D2382-76, Heat of Combustion of Hydrocarbon Fuse by Bomb
Calorimeter (High Precision Method) 60.17(a)(38); 60.18(f); 60.485(g);
60.614(d)(4); 60.664(d)(4)
ASTM D2504-67 (Reapproved 1977) Noncondensable Gases in C3 and
Lighter Hydrocarbon Products by Gas Chromatography 60.485(g)
ASTM D2584-68 (Reapproved 1979), Ignition Loss of Cured Reinforced
Resins 60.17(a)(45); 60.685(e)
ASTM D2622-87, Standard Test Method for Sulfur in Petroleum Products
by X-Ray Spectrometry 60.17(a)(59); 60.106(h)(2)
ASTM D2879-83, Test Method for Vapor Pressure-Temperature
Relationship and Initial Decomposition Temperature of Liquids by
Isoteniscope 60.17; 60.111b(f)(3); 60.116b(e)(3)(ii),
60.116b(f)(2)(i); 60.485(e)
ASTM D2880-78, Standard Specification for Gas Turbine Fuel Oils
60.111(b); 60.111a(b); 60.335(b)(2)
ASTM D2908-74, Standard for Measuring Volatile Organic Matter in
Water by Aqueous-Injection Gas Chromatography 60.17(a); 60.564(j)
ASTM D2986-71 (Reapproved 1978), Standard Method for Evaluation of
Air, Assay Media by the Monodisperse DOP (Dioctyl Phthalate) Smoke Test
Appendix A to Part 60, Method 5, par. 3.1.1; Method 12, par. 4.1.1;
Method 17, par. 3.1.1; 61.18(a)(7); Method 103, par. 2.1.3; Method
104, par. 3.1.1
ASTM D3031-81. Standard Test Method for Total Sulfur in Natural gas
by Hydrogenation 60.335(b)(2)
ASTM D3173-73, Standard Test Method for Moisture in the Analysis
Sample of Coal and Coke Appendix A to Part 60, Method 19
ASTM D3176-74, Standard Method for Ultimate Analysis of Coal and Coke
60.45(f)(5)(i); Appendix A to Part 60, Method 19
ASTM D3177-75, Standard Test Methods for Total Sulfur in the Analysis
Sample of Coal and Coke Appendix A to Part 60, Method 19
ASTM D3178-73, Standard Test Methods for Carbon and Hydrogen in the
Analysis Sample of Coal and Coke 60.45(f)(5)(i)
ASTM D3246-81, Standard Method for Sulfur in Petroleum Gas by
Oxidative Microcoulometry 60.335(b)(2)
ASTM D3286-85, Standard Test Method for Gross Calorific Value of Coal
and Coke by the Isothermal-Jacket Bomb calorimeter 60.17(a)(50);
Appendix A to Part 60, Method 19
ASTM D3370-76, Standard Practices for Sampling Water 60.17(a);
60.564(j)
ASTM D3431-80, Standard Test Method for Trace Nitrogen in Liquid
Petroleum Hydrocarbons (Microcoulometric Method) 60.17(a)(46); Appendix
A to Part 60, Method 19
ASTM D3792-79, Standard Test Method for Water Content of
Water-Reducible Paints by Direct Injection Into a Gas Chromatograph
Appendix A to Part 60, Method 24, par. 2.3
ASTM D4017-81, Standard Test Method for Water in Paints and Paint
Materials by the Karl Fischer Titration Method Appendix A to Part 60,
Method 24, par. 2.4
ASTM D4057-81, Standard Practive for Manual Sampling of Petroleum and
Petroleum Products 60.17(a)(51); Appendix A to Part 60, Method 19
ASTM D4084-82, Standard Method for Analysis of Hydrogen Sulfides in
Gaseous Fuels (Lead Acetate Reaction Rate Method) 60.335(b)(2)
ASTM D4239-85, Standard Test Methods for Sulfur in the Analysis
Sample of Coal and Coke Using High Temperature Tube Furnace Combustion
Methods 60.17(a)(52); Appendix A to Part 60, Method 19
ASTM D4442-84, Standard Test Methods for Direct Moisture Content
Measurement of Wood and Wood-base Materials 60.17(a)(54); Appendix A to
Part 60, Method 28
ASTM E168-67 (Reapproved 1977), General Techniques of Infrared
Qualitative Analysis 60.17(a)(35; 60.485(d); 60.593(b); 60.632(f)
ASTM E169-63 (Reapproved 1977), General Techniques of Ultraviolet
Quantitative Analysis 60.17(a)(34); 60.485(d); 60.593(b); 60.632(f)
ASTM E260-73, General Gas Chromatography Procedures 60.17(a)(36);
60.485(d); 60.593(b); 60.632(f)
Association of Official Analytical Chemists
1111 North 19th Street, Suite 210, Arlington, Virginia 22209
AOAC Method 9, Official Methods of Analysis of the Association of
Official Analytical Chemists, Eleventh Edition, 1970, pp. 11-12
60.204(d)(2); 60.214(d)(2); 60.224(d)(2); 60.234(d)(2); 60.244(f)(2)
Technical Association of the Pulp and Paper Industry
Dunwoody Park, Atlanta, Georgia 30341
TAPPI Method T624 os-68 60.285(d)(4)
Underwriter's Laboratories, Inc/
333 Pfingsten Road, Northbrook, IL 60062
UL 103, Sixth Ed., revised as of September 3, 1986, Standard for
Chimneys, Factory-built, Residential Type and Building Heating Appliance
60.17(f)(1)
West Coast Lumber Inspection Bureau
6980 SW. Barnes Road, Portland Oregon 97223
West Coast Lumber Standard Grading Rules, No. 16, pages 5-21, 90,
and 91, September 3, 1970, revised 1984 60.17(g)(1)
Chap.
40 CFR 60.748 Table of CFR Titles and Chapters
40 CFR 60.748 Title 1 -- General Provisions
I Administrative Committee of the Federal Register (Parts 1 -- 49)
II Office of the Federal Register (Parts 50 -- 299)
III Administrative Conference of the United States (Parts 300 -- 399)
IV Miscellaneous Agencies (Parts 400 -- 500)
40 CFR 60.748 Title 2 -- (Reserved)
40 CFR 60.748 Title 3 -- The President
I Executive Office of the President (Parts 100 -- 199)
40 CFR 60.748 Title 4 -- Accounts
I General Accounting Office (Parts 1 -- 99)
II Federal Claims Collection Standards (General Accounting Office --
Department of Justice) (Parts 100 -- 299)
40 CFR 60.748 Title 5 -- Administrative Personnel
I Office of Personnel Management (Parts 1 -- 1199)
II Merit Systems Protection Board (Parts 1200 -- 1299)
III Office of Management and Budget (Parts 1300 -- 1399)
IV Advisory Committee on Federal Pay (Parts 1400 -- 1499)
V The International Organizations Employees Loyalty Board (Parts 1500
-- 1599)
VI Federal Retirement Thrift Investment Board (Parts 1600 -- 1699)
VII Advisory Commission on Intergovernmental Relations (Parts 1700 --
1799)
VIII Office of Special Counsel (Parts 1800 -- 1899)
IX Appalachian Regional Commission (Parts 1900 -- 1999)
XI United States Soldiers' and Airmen's Home (Parts 2100 -- 2199)
XIV Federal Labor Relations Authority, General Counsel of the Federal
Labor Relations Authority and Federal Service Impasses Panel (Parts 2400
-- 2499)
XV Office of Administration, Executive Office of the President (Parts
2500 -- 2599)
XVI Office of Government Ethics (Parts 2600 -- 2699)
40 CFR 60.748 Title 6 -- (Reserved)
40 CFR 60.748 Title 7 -- Agriculture
Subitle A -- Office of the Secretary of Agriculture (Parts 0 -- 26)
Subitle B -- Regulations of the Department of Agriculture
I Agricultural Marketing Service (Standards, Inspections, Marketing
Practices), Department of Agriculture (Parts 27 -- 209)
II Food and Nutrition Service, Department of Agriculture (Parts 210
-- 299)
III Animal and Plant Health Inspection Service, Department of
Agriculture (Parts 300 -- 399)
IV Federal Crop Insurance Corporation, Department of Agriculture
(Parts 400 -- 499)
V Agricultural Research Service, Department of Agriculture (Parts 500
-- 599)
VI Soil Conservation Service, Department of Agriculture (Parts 600 --
699)
VII Agricultural Stabilization and Conservation Service (Agricultural
Adjustment), Department of Agriculture (Parts 700 -- 799)
VIII Federal Grain Inspection Service, Department of Agriculture
(Parts 800 -- 899)
IX Agricultural Marketing Service (Marketing Agreements and Orders;
Fruits, Vegetables, Nuts), Department of Agriculture (Parts 900 -- 999)
X Agricultural Marketing Service (Marketing Agreements and Orders;
Milk), Department of Agriculture (Parts 1000 -- 1199)
XI Agricultural Marketing Service (Marketing Agreements and Orders;
Miscellaneous Commodities), Department of Agriculture (Parts 1200 --
1299)
XIV Commodity Credit Corporation, Department of Agriculture (Parts
1400 -- 1499)
XV Foreign Agricultural Service, Department of Agriculture (Parts
1500 -- 1599)
XVI Rural Telephone Bank, Department of Agriculture (Parts 1600 --
1699)
XVII Rural Electrification Administration, Department of Agriculture
(Parts 1700 -- 1799)
XVIII Farmers Home Administration, Department of Agriculture (Parts
1800 -- 2099)
XXI Foreign Economic Development Service, Department of Agriculture
(Parts 2100 -- 2199)
XXII Office of International Cooperation and Development, Department
of Agriculture (Parts 2200 -- 2299)
XXV Office of the General Sales Manager, Department of Agriculture
(Parts 2500 -- 2599)
XXVI Office of Inspector General, Department of Agriculture (Parts
2600 -- 2699)
XXVII Office of Information Resources Management, Department of
Agriculture (Parts 2700 -- 2799)
XXVIII Office of Operations, Department of Agriculture (Parts 2800 --
2899)
XXIX Office of Energy, Department of Agriculture (Parts 2900 -- 2999)
XXX Office of Finance and Management, Department of Agriculture
(Parts 3000 -- 3099)
XXXI Office of Environmental Quality, Department of Agriculture
(Parts 3100 -- 3199)
XXXII Office of Grants and Program Systems, Department of Agriculture
(Parts 3200 -- 3299)
XXXIII Office of Transportation, Department of Agriculture (Parts
3300 -- 3399)
XXXIV Cooperative State Research Service, Department of Agriculture
(Parts 3400 -- 3499)
XXXVI National Agricultural Statistics Service, Department of
Agriculture (Parts 3600 -- 3699)
XXXVII Economic Research Service, Department of Agriculture (Parts
3700 -- 3799)
XXXVIII World Agricultural Outlook Board, Department of Agriculture
(Parts 3800 -- 3899)
XXXIX Economic Analysis Staff, Department of Agriculture (Parts 3900
-- 3999)
XL Economics Management Staff, Department of Agriculture (Parts 4000
-- 4099)
XLI National Agricultural Library, Department of Agriculture (Part
4100)
40 CFR 60.748 Title 8 -- Aliens and Nationality
I Immigration and Naturalization Service, Department of Justice
(Parts 1 -- 499)
40 CFR 60.748 Title 9 -- Animals and Animal Products
I Animal and Plant Health Inspection Service, Department of
Agriculture (Parts 1 -- 199)
II Packers and Stockyards Administration, Department of Agriculture
(Parts 200 -- 299)
III Food Safety and Inspection Service, Meat and Poultry Inspection,
Department of Agriculture (Parts 300 -- 399)
40 CFR 60.748 Title 10 -- Energy
I Nuclear Regulatory Commission (Parts 0 -- 199)
II Department of Energy (Parts 200 -- 699)
III Department of Energy (Parts 700 -- 999)
X Department of Energy (General Provisions) (Parts 1000 -- 1099)
XV Office of the Federal Inspector for the Alaska Natural Gas
Transportation System (Parts 1500 -- 1599)
XVII Defense Nuclear Facilities Safety Board (Parts 1700 -- 1799)
40 CFR 60.748 Title 11 -- Federal Elections
I Federal Election Commission (Parts 1 -- 9099)
40 CFR 60.748 Title 12 -- Banks and Banking
I Comptroller of the Currency, Department of the Treasury (Parts 1 --
199)
II Federal Reserve System (Parts 200 -- 299)
III Federal Deposit Insurance Corporation (Parts 300 -- 399)
IV Export-Import Bank of the United States (Parts 400 -- 499)
V Office of Thrift Supervision, Department of The Treasury (Parts 500
-- 599)
VI Farm Credit Administration (Parts 600 -- 699)
VII National Credit Union Administration (Parts 700 -- 799)
VIII Federal Financing Bank (Parts 800 -- 899)
IX Federal Housing Finance Board (Parts 900 -- 999)
XI Federal Financial Institutions Examination Council (Parts 1100 --
1199)
XIII Farm Credit System Assistance Board (Parts 1300 -- 1399)
XIV Farm Credit System Insurance Corporation (Parts 1400 -- 1499)
XV Thrift Depositor Protection Oversight Board (Parts 1500 -- 1599)
XVI Resolution Trust Corporation (Parts 1600 -- 1699)
40 CFR 60.748 Title 13 -- Business Credit and Assistance
I Small Business Administration (Parts 1 -- 199)
III Economic Development Administration, Department of Commerce
(Parts 300 -- 399)
40 CFR 60.748 Title 14 -- Aeronautics and Space
I Federal Aviation Administration, Department of Transportation
(Parts 1 -- 199)
II Office of the Secretary, Department of Transportation (Aviation
Proceedings) (Parts 200 -- 399)
III Office of Commercial Space Transportation, Department of
Transportation (Parts 400 -- 499)
V National Aeronautics and Space Administration (Parts 1200 -- 1299)
40 CFR 60.748 Title 15 -- Commerce and Foreign Trade
Subitle A -- Office of the Secretary of Commerce (Parts 0 -- 29)
Subitle B -- Regulations Relating to Commerce and Foreign Trade
I Bureau of the Census, Department of Commerce (Parts 30 -- 199)
II National Institute of Standards and Technology, Department of
Commerce (Parts 200 -- 299)
III International Trade Administration, Department of Commerce (Parts
300 -- 399)
IV Foreign-Trade Zones Board (Parts 400 -- 499)
VII Bureau of Export Administration, Department of Commerce (Parts
700 -- 799)
VIII Bureau of Economic Analysis, Department of Commerce (Parts 800
-- 899)
IX National Oceanic and Atmospheric Administration, Department of
Commerce (Parts 900 -- 999)
XI Technology Administration, Department of Commerce (Parts 1100 --
1199)
XII United States Travel and Tourism Administration, Department of
Commerce (Parts 1200 -- 1299)
XIII East-West Foreign Trade Board (Parts 1300 -- 1399)
XIV Minority Business Development Agency (Parts 1400 -- 1499)
Subitle C -- Regulations Relating to Foreign Trade Agreements
XX Office of the United States Trade Representative (Parts 2000 --
2099)
Subitle D -- Regulations Relating to Telecommunications and
Information
XXIII National Telecommunications and Information Administration,
Department of Commerce (Parts 2300 -- 2399)
40 CFR 60.748 Title 16 -- Commercial Practices
I Federal Trade Commission (Parts 0 -- 999)
II Consumer Product Safety Commission (Parts 1000 -- 1799)
40 CFR 60.748 Title 17 -- Commodity and Securities Exchanges
I Commodity Futures Trading Commission (Parts 1 -- 199)
II Securities and Exchange Commission (Parts 200 -- 399)
IV Department of the Treasury (Parts 400 -- 499)
40 CFR 60.748 Title 18 -- Conservation of Power and Water Resources
I Federal Energy Regulatory Commission, Department of Energy (Parts 1
-- 399)
III Delaware River Basin Commission (Parts 400 -- 499)
VI Water Resources Council (Parts 700 -- 799)
VIII Susquehanna River Basin Commission (Parts 800 -- 899)
XIII Tennessee Valley Authority (Parts 1300 -- 1399)
40 CFR 60.748 Title 19 -- Customs Duties
I United States Customs Service, Department of the Treasury (Parts 1
-- 199)
II United States International Trade Commission (Parts 200 -- 299)
III International Trade Administration, Department of Commerce (Parts
300 -- 399)
40 CFR 60.748 Title 20 -- Employees' Benefits
I Office of Workers' Compensation Programs, Department of Labor
(Parts 1 -- 199)
II Railroad Retirement Board (Parts 200 -- 399)
III Social Security Administration, Department of Health and Human
Services (Parts 400 -- 499)
IV Employees' Compensation Appeals Board, Department of Labor (Parts
500 -- 599)
V Employment and Training Administration, Department of Labor (Parts
600 -- 699)
VI Employment Standards Administration, Department of Labor (Parts
700 -- 799)
VII Benefits Review Board, Department of Labor (Parts 800 -- 899)
VIII Joint Board for the Enrollment of Actuaries (Parts 900 -- 999)
IX Office of the Assistant Secretary for Veterans' Employment and
Training, Department of Labor (Parts 1000 -- 1099)
40 CFR 60.748 Title 21 -- Food and Drugs
I Food and Drug Administration, Department of Health and Human
Services (Parts 1 -- 1299)
II Drug Enforcement Administration, Department of Justice (Parts 1300
-- 1399)
40 CFR 60.748 Title 22 -- Foreign Relations
I Department of State (Parts 1 -- 199)
II Agency for International Development, International Development
Cooperation Agency (Parts 200 -- 299)
III Peace Corps (Parts 300 -- 399)
IV International Joint Commission, United States and Canada (Parts
400 -- 499)
V United States Information Agency (Parts 500 -- 599)
VI United States Arms Control and Disarmament Agency (Parts 600 --
699)
VII Overseas Private Investment Corporation, International
Development Cooperation Agency (Parts 700 -- 799)
IX Foreign Service Grievance Board Regulations (Parts 900 -- 999)
X Inter-American Foundation (Parts 1000 -- 1099)
XI International Boundary and Water Commission, United States and
Mexico, United States Section (Parts 1100 -- 1199)
XII United States International Development Cooperation Agency (Parts
1200 -- 1299)
XIII Board for International Broadcasting (Parts 1300 -- 1399)
XIV Foreign Service Labor Relations Board; Federal Labor Relations
Authority; General Counsel of the Federal Labor Relations Authority;
and the Foreign Service Impasse Disputes Panel (Parts 1400 -- 1499)
XV African Development Foundation (Parts 1500 -- 1599)
XVI Japan-United States Friendship Commission (Parts 1600 -- 1699)
40 CFR 60.748 Title 23 -- Highways
I Federal Highway Administration, Department of Transportation (Parts
1 -- 999)
II National Highway Traffic Safety Administration and Federal Highway
Administration, Department of Transportation (Parts 1200 -- 1299)
III National Highway Traffic Safety Administration, Department of
Transportation (Parts 1300 -- 1399)
40 CFR 60.748 Title 24 -- Housing and Urban Development
Subitle A -- Office of the Secretary, Department of Housing and Urban
Development (Parts 0 -- 99)
Subitle B -- Regulations Relating to Housing and Urban Development
I Office of Assistant Secretary for Equal Opportunity, Department of
Housing and Urban Development (Parts 100 -- 199)
II Office of Assistant Secretary for Housing-Federal Housing
Commissioner, Department of Housing and Urban Development (Parts 200 --
299)
III Government National Mortgage Association, Department of Housing
and Urban Development (Parts 300 -- 399)
V Office of Assistant Secretary for Community Planning and
Development, Department of Housing and Urban Development (Parts 500 --
599)
VI Office of Assistant Secretary for Community Planning and
Development, Department of Housing and Urban Development (Parts 600 --
699)
VII Office of the Secretary, Department of Housing and Urban
Development (Section 8 Housing Assistance Programs and Public and Indian
Housing Programs) (Parts 700 -- 799)
VIII Office of the Assistant Secretary for Housing -- Federal Housing
Commissioner, Department of Housing and Urban Development (Section 8
Housing Assistance Programs and Section 202 Direct Loan Program) (Parts
800 -- 899)
IX Office of Assistant Secretary for Public and Indian Housing,
Department of Housing and Urban Development (Parts 900 -- 999)
X Office of Assistant Secretary for Housing -- Federal Housing
Commissioner, Department of Housing and Urban Development (Interstate
Land Sales Registration Program) (Parts 1700 -- 1799)
XI Solar Energy and Energy Conservation Bank, Department of Housing
and Urban Development (Parts 1800 -- 1899)
XII Office of Inspector General, Department of Housing and Urban
Development (Parts 2000 -- 2099)
XV Mortgage Insurance and Loan Programs under the Emergency
Homeowners' Relief Act, Department of Housing and Urban Development
(Parts 2700 -- 2799)
XX Office of Assistant Secretary for Housing -- Federal Housing
Commissioner, Department of Housing and Urban Development (Parts 3200 --
3699)
XXV Neighborhood Reinvestment Corporation (Parts 4100 -- 4199)
40 CFR 60.748 Title 25 -- Indians
I Bureau of Indian Affairs, Department of the Interior (Parts 1 --
299)
II Indian Arts and Crafts Board, Department of the Interior (Parts
300 -- 399)
III National Indian Gaming Commission (Parts 500 -- 599)
IV Office of Navajo and Hopi Indian Relocation (Parts 700 -- 799)
40 CFR 60.748 Title 26 -- Internal Revenue
I Internal Revenue Service, Department of the Treasury (Parts 1 --
799)
40 CFR 60.748 Title 27 -- Alcohol, Tobacco Products and Firearms
I Bureau of Alcohol, Tobacco and Firearms, Department of the Treasury
(Parts 1 -- 299)
40 CFR 60.748 Title 28 -- Judicial Administration
I Department of Justice (Parts 0 -- 199)
III Federal Prison Industries, Inc., Department of Justice (Parts 300
-- 399)
V Bureau of Prisons, Department of Justice (Parts 500 -- 599)
VI Offices of Independent Counsel, Department of Justice (Parts 600
-- 699)
VII Office of Independent Counsel (Parts 700 -- 799)
40 CFR 60.748 Title 29 -- Labor
Subitle A -- Office of the Secretary of Labor (Parts 0 -- 99)
Subitle B -- Regulations Relating to Labor
I National Labor Relations Board (Parts 100 -- 199)
II Bureau of Labor-Management Relations and Cooperative Programs,
Department of Labor (Parts 200 -- 299)
III National Railroad Adjustment Board (Parts 300 -- 399)
IV Office of Labor-Management Standards, Department of Labor (Parts
400 -- 499)
V Wage and Hour Division, Department of Labor (Parts 500 -- 899)
IX Construction Industry Collective Bargaining Commission (Parts 900
-- 999)
X National Mediation Board (Parts 1200 -- 1299)
XII Federal Mediation and Conciliation Service (Parts 1400 -- 1499)
XIV Equal Employment Opportunity Commission (Parts 1600 -- 1699)
XVII Occupational Safety and Health Administration, Department of
Labor (Parts 1900 -- 1999)
XX Occupational Safety and Health Review Commission (Parts 2200 --
2499)
XXV Pension and Welfare Benefits Administration, Department of Labor
(Parts 2500 -- 2599)
XXVI Pension Benefit Guaranty Corporation (Parts 2600 -- 2699)
XXVII Federal Mine Safety and Health Review Commission (Parts 2700 --
2799)
40 CFR 60.748 Title 30 -- Mineral Resources
I Mine Safety and Health Administration, Department of Labor (Parts 1
-- 199)
II Minerals Management Service, Department of the Interior (Parts 200
-- 299)
III Board of Surface Mining and Reclamation Appeals, Department of
the Interior (Parts 300 -- 399)
IV Geological Survey, Department of the Interior (Parts 400 -- 499)
VI Bureau of Mines, Department of the Interior (Parts 600 -- 699)
VII Office of Surface Mining Reclamation and Enforcement, Department
of the Interior (Parts 700 -- 999)
40 CFR 60.748 Title 31 -- Money and Finance: Treasury
Subitle A -- Office of the Secretary of the Treasury (Parts 0 -- 50)
Subitle B -- Regulations Relating to Money and Finance
I Monetary Offices, Department of the Treasury (Parts 51 -- 199)
II Fiscal Service, Department of the Treasury (Parts 200 -- 399)
IV Secret Service, Department of the Treasury (Parts 400 -- 499)
V Office of Foreign Assets Control, Department of the Treasury (Parts
500 -- 599)
VI Bureau of Engraving and Printing, Department of the Treasury
(Parts 600 -- 699)
VII Federal Law Enforcement Training Center, Department of the
Treasury (Parts 700 -- 799)
VIII Office of International Investment, Department of the Treasury
(Parts 800 -- 899)
40 CFR 60.748 Title 32 -- National Defense
Subitle A -- Department of Defense
I Office of the Secretary of Defense (Parts 1 -- 399)
V Department of the Army (Parts 400 -- 699)
VI Department of the Navy (Parts 700 -- 799)
VII Department of the Air Force (Parts 800 -- 1099)
Subitle B -- Other Regulations Relating to National Defense
XII Defense Logistics Agency (Parts 1200 -- 1299)
XVI Selective Service System (Parts 1600 -- 1699)
XIX Central Intelligence Agency (Parts 1900 -- 1999)
XX Information Security Oversight Office (Parts 2000 -- 2099)
XXI National Security Council (Parts 2100 -- 2199)
XXIV Office of Science and Technology Policy (Parts 2400 -- 2499)
XXVII Office for Micronesian Status Negotiations (Parts 2700 -- 2799)
XXVIII Office of the Vice President of the United States (Parts 2800
-- 2899)
40 CFR 60.748 Title 33 -- Navigation and Navigable Waters
I Coast Guard, Department of Transportation (Parts 1 -- 199)
II Corps of Engineers, Department of the Army (Parts 200 -- 399)
IV Saint Lawrence Seaway Development Corporation, Department of
Transportation (Parts 400 -- 499)
40 CFR 60.748 Title 34 -- Education
Subitle A -- Office of the Secretary, Department of Education (Parts
1 -- 99)
Subitle B -- Regulations of the Offices of the Department of
Education
I Office for Civil Rights, Department of Education (Parts 100 -- 199)
II Office of Elementary and Secondary Education, Department of
Education (Parts 200 -- 299)
III Office of Special Education and Rehabilitative Services,
Department of Education (Parts 300 -- 399)
IV Office of Vocational and Adult Education, Department of Education
(Parts 400 -- 499)
V Office of Bilingual Education and Minority Languages Affairs,
Department of Education (Parts 500 -- 599)
VI Office of Postsecondary Education, Department of Education (Parts
600 -- 699)
VII Office of Educational Research and Improvement, Department of
Education (Parts 700 -- 799)
40 CFR 60.748 Title 35 -- Panama Canal
I Panama Canal Regulations (Parts 1 -- 299)
40 CFR 60.748 Title 36 -- Parks, Forests, and Public Property
I National Park Service, Department of the Interior (Parts 1 -- 199)
II Forest Service, Department of Agriculture (Parts 200 -- 299)
III Corps of Engineers, Department of the Army (Parts 300 -- 399)
IV American Battle Monuments Commission (Parts 400 -- 499)
V Smithsonian Institution (Parts 500 -- 599)
VII Library of Congress (Parts 700 -- 799)
VIII Advisory Council on Historic Preservation (Parts 800 -- 899)
IX Pennsylvania Avenue Development Corporation (Parts 900 -- 999)
XI Architectural and Transportation Barriers Compliance Board (Parts
1100 -- 1199)
XII National Archives and Records Administration (Parts 1200 -- 1299)
40 CFR 60.748 Title 37 -- Patents, Trademarks, and Copyrights
I Patent and Trademark Office, Department of Commerce (Parts 1 --
199)
II Copyright Office, Library of Congress (Parts 200 -- 299)
III Copyright Royalty Tribunal (Parts 300 -- 399)
IV Assistant Secretary for Technology Policy, Department of Commerce
(Parts 400 -- 499)
V Under Secretary for Technology, Department of Commerce (Parts 500
-- 599)
40 CFR 60.748 Title 38 -- Pensions, Bonuses, and Veterans' Relief
I Department of Veterans Affairs (Parts 0 -- 99)
40 CFR 60.748 Title 39 -- Postal Service
I United States Postal Service (Parts 1 -- 999)
III Postal Rate Commission (Parts 3000 -- 3099)
40 CFR 60.748 Title 40 -- Protection of Environment
I Environmental Protection Agency (Parts 1 -- 799)
V Council on Environmental Quality (Parts 1500 -- 1599)
40 CFR 60.748 Title 41 -- Public Contracts and Property Management
Subitle B -- Other Provisions Relating to Public Contracts
50 Public Contracts, Department of Labor (Parts 50-1 -- 50-999)
51 Committee for Purchase from the Blind and Other Severely
Handicapped (Parts 51-1 -- 51-99)
60 Office of Federal Contract Compliance Programs, Equal Employment
Opportunity, Department of Labor (Parts 60-1 -- 60-999)
61 Office of the Assistant Secretary for Veterans Employment and
Training, Department of Labor (Parts 61-1 -- 61-999)
Subitle C -- Federal Property Management Regulations System
101 Federal Property Management Regulations (Parts 101-1 -- 101-99)
105 General Services Administration (Parts 105-1 -- 105-999)
109 Department of Energy Property Management Regulations (Parts 109-1
-- 109-99)
114 Department of the Interior (Parts 114-1 -- 114-99)
115 Environmental Protection Agency (Parts 115-1 -- 115-99)
128 Department of Justice (Parts 128-1 -- 128-99)
132 Department of the Air Force (Parts 132-1 -- 132-99)
Subitle D -- Other Provisions Relating to Property Management
(Reserved)
Subitle E -- Federal Information Resources Management Regulations
System
201 Federal Information Resources Management Regulation (Parts 201-1
-- 201-99)
Subitle F -- Federal Travel Regulation System
301 Travel Allowances (Parts 301-1 -- 301-99)
302 Relocation Allowances (Parts 302-1 -- 302-99)
303 Payment of Expenses Connected with the Death of Certain Employees
(Parts 303-1 -- 303-2)
304 Payment from a non-Federal source for travel expenses (Parts
304-1 -- 304-99)
40 CFR 60.748 Title 42 -- Public Health
I Public Health Service, Department of Health and Human Services
(Parts 1 -- 199)
IV Health Care Financing Administration, Department of Health and
Human Services (Parts 400 -- 499)
V Office of Inspector General-Health Care, Department of Health and
Human Services (Parts 1000 -- 1999)
40 CFR 60.748 Title 43 -- Public Lands: Interior
Subitle A -- Office of the Secretary of the Interior (Parts 1 -- 199)
Subitle B -- Regulations Relating to Public Lands
I Bureau of Reclamation, Department of the Interior (Parts 200 --
499)
II Bureau of Land Management, Department of the Interior (Parts 1000
-- 9999)
40 CFR 60.748 Title 44 -- Emergency Management and Assistance
I Federal Emergency Management Agency (Parts 0 -- 399)
IV Department of Commerce and Department of Transportation (Parts 400
-- 499)
40 CFR 60.748 Title 45 -- Public Welfare
Subitle A -- Department of Health and Human Services, General
Administration (Parts 1 -- 199)
Subitle B -- Regulations Relating to Public Welfare
II Office of Family Assistance (Assistance Programs), Family Support
Administration, Department of Health and Human Services (Parts 200 --
299)
III Office of Child Support Enforcement (Child Support Enforcement
Program), Family Support Administration, Department of Health and Human
Services (Parts 300 -- 399)
IV Office of Refugee Resettlement, Administration for Children and
Families Department of Health and Human Services (Parts 400 -- 499)
V Foreign Claims Settlement Commission of the United States,
Department of Justice (Parts 500 -- 599)
VI National Science Foundation (Parts 600 -- 699)
VII Commission on Civil Rights (Parts 700 -- 799)
VIII Office of Personnel Management (Parts 800 -- 899)
X Office of Community Services, Family Support Administration,
Department of Health and Human Services (Parts 1000 -- 1099)
XI National Foundation on the Arts and the Humanities (Parts 1100 --
1199)
XII ACTION (Parts 1200 -- 1299)
XIII Office of Human Development Services, Department of Health and
Human Services (Parts 1300 -- 1399)
XVI Legal Services Corporation (Parts 1600 -- 1699)
XVII National Commission on Libraries and Information Science (Parts
1700 -- 1799)
XVIII Harry S. Truman Scholarship Foundation (Parts 1800 -- 1899)
XX Commission on the Bicentennial of the United States Constitution
(Parts 2000 -- 2099)
XXI Commission on Fine Arts (Parts 2100 -- 2199)
XXII Christopher Columbus Quincentenary Jubilee Commission (Parts
2200 -- 2299)
XXIV James Madison Memorial Fellowship Foundation (Parts 2400 --
2499)
40 CFR 60.748 Title 46 -- Shipping
I Coast Guard, Department of Transportation (Parts 1 -- 199)
II Maritime Administration, Department of Transportation (Parts 200
-- 399)
III Coast Guard (Great Lakes Pilotage), Department of Transportation
(Parts 400 -- 499)
IV Federal Maritime Commission (Parts 500 -- 599)
40 CFR 60.748 Title 47 -- Telecommunication
I Federal Communications Commission (Parts 0 -- 199)
II Office of Science and Technology Policy and National Security
Council (Parts 200 -- 299)
III National Telecommunications and Information Administration,
Department of Commerce (Parts 300 -- 399)
40 CFR 60.748 Title 48 -- Federal Acquisition Regulations System
1 Federal Acquisition Regulation (Parts 1 -- 99)
2 Department of Defense (Parts 200 -- 299)
3 Department of Health and Human Services (Parts 300 -- 399)
4 Department of Agriculture (Parts 400 -- 499)
5 General Services Administration (Parts 500 -- 599)
6 Department of State (Parts 600 -- 699)
7 Agency for International Development (Parts 700 -- 799)
8 Department of Veterans Affairs (Parts 800 -- 899)
9 Department of Energy (Parts 900 -- 999)
10 Department of the Treasury (Parts 1000 -- 1099)
12 Department of Transportation (Parts 1200 -- 1299)
13 Department of Commerce (Parts 1300 -- 1399)
14 Department of the Interior (Parts 1400 -- 1499)
15 Environmental Protection Agency (Parts 1500 -- 1599)
16 Office of Personnel Management Federal Employees Health Benefits
Acquisition Regulation (Parts 1600 -- 1699)
17 Office of Personnel Management (Parts 1700 -- 1799)
18 National Aeronautics and Space Administration (Parts 1800 -- 1899)
19 United States Information Agency (Parts 1900 -- 1999)
22 Small Business Administration (Parts 2200 -- 2299)
24 Department of Housing and Urban Development (Parts 2400 -- 2499)
25 National Science Foundation (Parts 2500 -- 2599)
28 Department of Justice (Parts 2800 -- 2899)
29 Department of Labor (Parts 2900 -- 2999)
34 Department of Education Acquisition Regulation (Parts 3400 --
3499)
35 Panama Canal Commission (Parts 3500 -- 3599)
44 Federal Emergency Management Agency (Parts 4400 -- 4499)
51 Department of the Army Acquisition Regulations (Parts 5100 --
5199)
52 Department of the Navy Acquisition Regulations (Parts 5200 --
5299)
53 Department of the Air Force Federal Acquisition Regulation
Supplement (Parts 5300 -- 5399)
57 African Development Foundation (Parts 5700 -- 5799)
61 General Services Administration Board of Contract Appeals (Parts
6100 -- 6199)
63 Department of Transportation Board of Contract Appeals (Parts 6300
-- 6399)
99 Cost Accounting Standards Board, Office of Federal Procurement
Policy, Office of Management and Budget (Parts 9900 -- 9999)
40 CFR 60.748 Title 49 -- Transportation
Subitle A -- Office of the Secretary of Transportation (Parts 1 --
99)
Subitle B -- Other Regulations Relating to Transportation
I Research and Special Programs Administration, Department of
Transportation (Parts 100 -- 199)
II Federal Railroad Administration, Department of Transportation
(Parts 200 -- 299)
III Federal Highway Administration, Department of Transportation
(Parts 300 -- 399)
IV Coast Guard, Department of Transportation (Parts 400 -- 499)
V National Highway Traffic Safety Administration, Department of
Transportation (Parts 500 -- 599)
VI Federal Transit Administration, Department of Transportation
(Parts 600 -- 699)
VII National Railroad Passenger Corporation (AMTRAK) (Parts 700 --
799)
VIII National Transportation Safety Board (Parts 800 -- 899)
X Interstate Commerce Commission (Parts 1000 -- 1399)
40 CFR 60.748 Title 50 -- Wildlife and Fisheries
I United States Fish and Wildlife Service, Department of the Interior
(Parts 1 -- 199)
II National Marine Fisheries Service, National Oceanic and
Atmospheric Administration, Department of Commerce (Parts 200 -- 299)
III International Regulatory Agencies (Fishing and Whaling) (Parts
300 -- 399)
IV Joint Regulations (United States Fish and Wildlife Service,
Department of the Interior and National Marine Fisheries Service,
National Oceanic and Atmospheric Administration, Department of
Commerce); Endangered Species Committee Regulations (Parts 400 -- 499)
V Marine Mammal Commission (Parts 500 -- 599)
VI Fishery Conservation and Management, National Oceanic and
Atmospheric Administration, Department of Commerce (Parts 600 -- 699)
40 CFR 60.748 CFR Index and Finding Aids Subject/Agency List of
Agency Prepared Indexes Parallel Tables of Statutory Authorities and
Rules Acts Requiring Publication in the Federal Register List of CFR
Titles, Chapters, Subchapters, and Parts
40 CFR 60.748 Alphabetical List of Agencies Appearing in the CFR
CFR Title, Subtitle or
Agency
Chapter
ACTION 45, XII
Administrative Committee of the Federal Register 1, I
Administrative Conference of the United States 1, III
Advisory Commission on Intergovernmental Relations 5, VII
Advisory Committee on Federal Pay 5, IV
Advisory Council on Historic Preservation 36, VIII
African Development Foundation 22, XV; 48, 57
Agency for International Development 22, II; 48, 7
Agricultural Marketing Service 7, I, IX, X, XI
Agricultural Research Service 7, V
Agricultural Stabilization and Conservation Service 7, VII
Agriculture Department
Agricultural Marketing Service 7, I, IX, X, XI
Agricultural Research Service 7, V
Agricultural Stabilization and Conservation Service 7, VII
Animal and Plant Health Inspection Service 7, III; 9, I
Commodity Credit Corporation 7, XIV
Cooperative State Research Service 7, XXXIV
Economic Analysis Staff 7, XXXIX
Economic Research Service 7, XXXVII
Economics Management Staff 7, XL
Energy, Office of 7, XXIX
Environmental Quality, Office of 7, XXXI
Farmers Home Administration 7, XVIII
Federal Acquisition Regulation 48, 4
Federal Crop Insurance Corporation 7, IV
Federal Grain Inspection Service 7, VIII
Finance and Management, Office of 7, XXX
Food and Nutrition Service 7, II
Food Safety and Inspection Service 9, III
Foreign Agricultural Service 7, XV
Foreign Economic Development Service 7, XXI
Forest Service 36, II
General Sales Manager, Office of 7, XXV
Grants and Program Systems, Office of 7, XXXII
Information Resources Management, Office of 7, XXVII
Inspector General, Office of 7, XXVI
International Cooperation and Development Office 7, XXII
National Agricultural Library 7, XLI
National Agricultural Statistics Service 7, XXXVI
Operations Office 7, XXVIII
Packers and Stockyards Administration 9, II
Rural Electrification Administration 7, XVII
Rural Telephone Bank 7, XVI
Secretary of Agriculture, Office of 7, Subtitle A
Soil Conservation Service 7, VI
Transportation, Office of 7, XXXIII
World Agriculture Outlook Board 7, XXXVIII
Air Force Department 32, VII; 41, Subtitle C, Ch. 132
Federal Acquisition Regulation Supplement 48, 53
Alaska Natural Gas Transportation System, Office of the Federal
Inspector 10, XV
Alcohol, Tobacco and Firearms, Bureau of 27, I
AMTRAK 49, VII
American Battle Monuments Commission 36, IV
Animal and Plant Health Inspection Service 7, III; 9, I
Appalachian Regional Commission 5, IX
Architectural and Transportation Barriers Compliance Board 36, XI
Arms Control and Disarmament Agency, U.S. 22, VI
Army Department 32, V
Engineers, Corps of 33, II; 36, III
Federal Acquisition Regulation 48, 51
Assistant Secretary for Technology Policy, Department of Commerce 37,
IV
Benefits Review Board 20, VII
Bicentennial of the United States Constitution, Commission on the 45,
XX
Bilingual Education and Minority Languages Affairs, Office of 34, V
Blind and Other Severely Handicapped, Committee for Purchase from 41,
51
Board for International Broadcasting 22, XIII
Budget, Office of Management and 5, III
Census Bureau 15, I
Central Intelligence Agency 32, XIX
Child Support Enforcement, Office of 45, III
Christopher Columbus Quincentenary Jubilee Commission 45, XXII
Civil Rights Commission 45, VII
Civil Rights, Office for (Education Department) 34, I
Claims Collection Standards, Federal 4, II
Coast Guard 33, I; 46, I, III; 49, IV
Commerce Department 44, IV
Census Bureau 15, I
Assistant Secretary for Technology Policy 37, IV
Economic Affairs, Under Secretary 37, V
Economic Analysis, Bureau of 15, VIII
Economic Development Administration 13, III
Endangered Species Committee 50, IV
Export Administration Bureau 15, VII
Federal Acquisition Regulation 48, 13
Fishery Conservation and Management 50, VI
International Trade Administration 15, III; 19, III
National Institute of Standards and Technology 15, II
National Marine Fisheries Service 50, II, IV
National Oceanic and Atmospheric Administration 15, IX; 50, II, III,
IV, VI
National Telecommunications and Information Administration 15, XXIII;
47, III
Patent and Trademark Office 37, I
Productivity, Technology and Innovation, Assistant Secretary for 37,
IV
Secretary of Commerce, Office of 15, Subtitle A
Technology Administration 15, XI
Under Secretary for Technology 37, V
United States Travel and Tourism Administration 15, XII
Commercial Space Transportation, Office of, Department of
Transportation 14, III
Commission on the Bicentennial of the United States Constitution 45,
XX
Committee for Purchase from the Blind and Other Severely Handicapped
41, 51
Commodity Credit Corporation 7, XIV
Commodity Futures Trading Commission 17, I
Community Planning and Development, Office of Assistant Secretary for
24, V, VI
Community Services, Office of 45, X
Comptroller of the Currency 12, I
Construction Industry Collective Bargaining Commission 29, IX
Consumer Product Safety Commission 16, II
Cooperative State Research Service 7, XXXIV
Copyright Office 37, II
Copyright Royalty Tribunal 37, III
Cost Accounting Standards Board, Office of Federal Procurement Policy
48, 99
Council on Environmental Quality 40, V
Customs Service, United States 19, I
Defense Department 32, Subtitle A
Air Force Department 32, VII; 41, Subtitle C, Ch. 132
Army Department 32, V; 33, II; 36, III, 48, 51
Engineers, Corps of 33, II; 36, III
Federal Acquisition Regulation 48, 2
Navy Department 32, VI; 48, 52
Secretary of Defense, Office of 32, I
Defense Logistics Agency 32, XII
Defense Nuclear Facilities Safety Board 10, XVII
Delaware River Basin Commission 18, III
Drug Enforcement Administration 21, II
East-West Foreign Trade Board 15, XIII
Economic Affairs, Under Secretary (Commerce) 37, V
Economic Analysis, Bureau of 15, VIII
Economic Analysis Staff, Department of Agriculture 7, XXXIX
Economic Development Administration 13, III
Economics Management Staff 7, XL
Economic Research Service 7, XXXVII
Education, Department of
Bilingual Education and Minority Languages Affairs, Office of 34, V
Civil Rights, Office for 34, I
Educational Research and Improvement, Office of 34, VII
Elementary and Secondary Education, Office of 34, II
Federal Acquisition Regulation 48, 34
Postsecondary Education, Office of 34, VI
Secretary of Education, Office of 34, Subtitle A
Special Education and Rehabilitative Services, Office of 34, III
Vocational and Adult Education, Office of 34, IV
Educational Research and Improvement, Office of 34, VII
Elementary and Secondary Education, Office of 34, II
Employees' Compensation Appeals Board 20, IV
Employees Loyalty Board, International Organizations 5, V
Employment and Training Administration 20, V
Employment Standards Administration 20, VI
Endangered Species Committee 50, IV
Energy, Department of 10, II, III, X; 41, 109
Federal Acquisition Regulation 48, 9
Federal Energy Regulatory Commission 18, I
Energy, Office of, Department of Agriculture 7, XXIX
Engineers, Corps of 33, II; 36, III
Engraving and Printing, Bureau of 31, VI
Environmental Protection Agency 40, I; 41, 115; 48, 15
Environmental Quality, Office of (Agriculture Department) 7, XXXI
Equal Employment Opportunity Commission 29, XIV
Equal Opportunity, Office of Assistant Secretary for 24, I
Executive Office of the President 3, I
Administration, Office of 5, XV
Export Administration Bureau 15, VII
Export-Import Bank of the United States 12, IV
Family Assistance, Office of 45, II
Family Support Administration 45, II, III, IV, X
Farm Credit Administration 12, VI
Farm Credit System Assistance Board 12, XIII
Farm Credit System Insurance Corporation 12, XIV
Farmers Home Administration 7, XVIII
Federal Acquisition Regulation 48, 1
Federal Aviation Administration 14, I
Federal Claims Collection Standards 4, II
Federal Communications Commission 47, I
Federal Contract Compliance Programs, Office of 41, 60
Federal Crop Insurance Corporation 7, IV
Federal Deposit Insurance Corporation 12, III
Federal Election Commission 11, I
Federal Emergency Management Agency 44, I; 48, 44
Federal Energy Regulatory Commission 18, I
Federal Financial Institutions Examination Council 12, XI
Federal Financing Bank 12, VIII
Federal Grain Inspection Service 7, VIII
Federal Highway Administration 23, I, II; 49, III
Federal Home Loan Mortgage Corporation 1, IV
Federal Housing Finance Board 12, IX
Federal Information Resources Management Regulations 41, Subtitle E,
Ch. 201
Federal Inspector for the Alaska Natural Gas Transportation System,
Office of 10, XV
Federal Labor Relations Authority, and General Counsel of the Federal
Labor Relations Authority 5, XIV; 22, XIV
Federal Law Enforcement Training Center 31, VII
Federal Maritime Commission 46, IV
Federal Mediation and Conciliation Service 29, XII
Federal Mine Safety and Health Review Commission 29, XXVII
Federal Pay, Advisory Committee on 5, IV
Federal Prison Industries, Inc. 28, III
Federal Procurement Policy Office 48, 99
Federal Property Management Regulations 41, 101
Federal Property Management Regulations System 41, Subtitle C
Federal Railroad Administration 49, II
Federal Register, Administrative Committee of 1, I
Federal Register, Office of 1, II
Federal Reserve System 12, II
Federal Retirement Thrift Investment Board 5, VI
Federal Service Impasses Panel 5, XIV
Federal Trade Commission 16, I
Federal Travel Regulation System 41, Subtitle F
Finance and Management, Department of Agriculture 7, XXX
Fine Arts Commission 45, XXI
Fiscal Service 31, II
Fish and Wildlife Service, United States 50, I, IV
Fishery Conservation and Management 50, VI
Fishing and Whaling, International Regulatory Agencies 50, III
Food and Drug Administration 21, I
Food and Nutrition Service 7, II
Food Safety and Inspection Service 9, III
Foreign Agricultural Service 7, XV
Foreign Assets Control, Office of 31, V
Foreign Claims Settlement Commission of United States 45, V
Foreign Economic Development Service 7, XXI
Foreign Service Grievance Board 22, IX
Foreign Service Impasse Disputes Panel 22, XIV
Foreign Service Labor Relations Board 22, XIV
Foreign-Trade Zones Board 15, IV
Forest Service 36, II
General Accounting Office 4, I, II, III
General Sales Manager, Office of 7, XXV
General Services Administration
Contract Appeals Board 48, 61
Federal Acquisition Regulation 48, 5
Federal Information Resources Management Regulations 41, Subtitle E,
Ch. 201
Federal Property Management Regulations System 41, 101, 105
Federal Travel Regulation System 41, Subtitle F
Payment from a non-Federal source for travel expenses 41, 304
Payment of Expenses Connected With the Death of Certain Employees 41,
303
Relocation Allowances 41, 302
Travel Allowances 41, 301
Geological Survey 30, IV
Government Ethics, Office of 5, XVI
Government National Mortgage Association 24, III
Grants and Program Systems, Office of 7, XXXII
Great Lakes Pilotage 46, III
Harry S. Truman Scholarship Foundation 45, XVIII
Health and Human Services, Department of 45, Subtitle A
Child Support Enforcement, Office of 45, III
Community Services, Office of 45, X
Family Assistance, Office of 45, II
Family Support Administration 45, II, III, IV, X
Federal Acquisition Regulation 48, 3
Food and Drug Administration 21, I
Health Care Financing Administration 42, IV
Human Development Services Office 45, XIII
Inspector General, Office of 42, V
Public Health Service 42, I
Refugee Resettlement, Office of 45, IV
Social Security Administration 20, III; 45, IV
Health Care Financing Administration 42, IV
Housing and Urban Development, Department of
Community Planning and Development, Office of Assistant Secretary for
24, V, VI
Equal Opportunity, Office of Assistant Secretary for 24, I
Federal Acquisition Regulation 48, 24
Government National Mortgage Association 24, III
Housing -- Federal Housing Commissioner, Office of Assistant
Secretary for 24, II, VIII, X, XX
Inspector General, Office of 24, XII
Mortgage Insurance and Loan Programs Under Emergency Homeowners'
Relief Act 24, XV
Public and Indian Housing, Office of Assistant Secretary for 24, IX
Secretary, Office of 24, Subtitle B, VII
Solar Energy and Energy Conservation Bank 24, XI
Housing -- Federal Housing Commissioner, Office of Assistant
Secretary for 24, II, VIII, X, XX
Human Development Services Office 45, XIII
Immigration and Naturalization Service 8, I
Indian Affairs, Bureau of 25, I
Indian Arts and Crafts Board 25, II
Information Agency, United States 22, V; 48, 19
Information Resources Management, Office of, Agriculture Department
7, XXVII
Information Security Oversight Office 32, XX
Inspector General, Office of, Agriculture Department 7, XXVI
Inspector General, Office of, Health and Human Services Department
42, V
Inspector General, Office of, Housing and Urban Development
Department 24, XII
Inter-American Foundation 22, X
Intergovernmental Relations, Advisory Commission on 5, VII
Interior Department
Endangered Species Committee 50, IV
Federal Acquisition Regulation 48, 14
Federal Property Management Regulations System 41, 114
Fish and Wildlife Service, United States 50, I, IV
Geological Survey 30, IV
Indian Affairs, Bureau of 25, I
Indian Arts and Crafts Board 25, II
Land Management Bureau 43, II
Minerals Management Service 30, II
Mines, Bureau of 30, VI
National Park Service 36, I
Reclamation Bureau 43, I
Secretary of the Interior, Office of 43, Subtitle A
Surface Mining and Reclamation Appeals, Board of 30, III
Surface Mining Reclamation and Enforcement, Office of 30, VII
United States Fish and Wildlife Service 50, I, IV
Internal Revenue Service 26, I
International Boundary and Water Commission, United States and Mexico
22, XI
International Cooperation and Development Office, Department of
Agriculture 7, XXII
International Development, Agency for 22, II
International Development Cooperation Agency 22, XII
International Development, Agency for 22, II
Overseas Private Investment Corporation 22, VII
International Joint Commission, United States and Canada 22, IV
International Organizations Employees Loyalty Board 5, V
International Regulatory Agencies (Fishing and Whaling) 50, III
International Trade Administration 15, III; 19, III
International Trade Commission, United States 19, II
Interstate Commerce Commission 49, X
Japan-United States Friendship Commission 22, XVI
Joint Board for the Enrollment of Actuaries 20, VIII
Justice Department 28, I; 41, 128
Drug Enforcement Administration 21, II
Federal Acquisition Regulation 48, 28
Federal Claims Collection Standards 4, II
Federal Prison Industries, Inc. 28, III
Foreign Claims Settlement Commission of the United States 45, V
Immigration and Naturalization Service 8, I
Offices of Independent Counsel 28, VI
Prisons, Bureau of 28, V
Labor Department
Benefits Review Board 20, VII
Employees' Compensation Appeals Board 20, IV
Employment and Training Administration 20, V
Employment Standards Administration 20, VI
Federal Acquisition Regulation 48, 29
Federal Contract Compliance Programs, Office of 41, 60
Federal Procurement Regulations System 41, 50
Labor-Management Relations and Cooperative Programs, Bureau of 29, II
Labor-Management Standards, Office of 29, IV
Mine Safety and Health Administration 30, I
Occupational Safety and Health Administration 29, XVII
Pension and Welfare Benefits Administration 29, XXV
Public Contracts 41, 50
Secretary of Labor, Office of 29, Subtitle A
Veterans' Employment and Training, Office of the Assistant Secretary
for 41, 61; 20, IX
Wage and Hour Division 29, V
Workers' Compensation Programs, Office of 20, I
Labor-Management Relations and Cooperative Programs, Bureau of 29, II
Labor-Management Standards, Office of 29, IV
Land Management, Bureau of 43, II
Legal Services Corporation 45, XVI
Library of Congress 36, VII
Copyright Office 37, II
Management and Budget, Office of 5, III; 48, 99
Marine Mammal Commission 50, V
Maritime Administration 46, II
Merit Systems Protection Board 5, II
Micronesian Status Negotiations, Office for 32, XXVII
Mine Safety and Health Administration 30, I
Minerals Management Service 30, II
Mines, Bureau of 30, VI
Minority Business Development Agency 15, XIV
Miscellaneous Agencies 1, IV
Monetary Offices 31, I
Mortgage Insurance and Loan Programs Under the Emergency Homeowners'
Relief Act, Department of Housing and Urban Development 24, XV
National Aeronautics and Space Administration 14, V; 48, 18
National Agricultural Library 7, XLI
National Agricultural Statistics Service 7, XXXVI
National Archives and Records Administration 36, XII
National Bureau of Standards 15, II
National Capital Planning Commission 1, IV
National Commission for Employment Policy 1, IV
National Commission on Libraries and Information Science 45, XVII
National Credit Union Administration 12, VII
National Foundation on the Arts and the Humanities 45, XI
National Highway Traffic Safety Administration 23, II, III; 49, V
National Indian Gaming Commission 25, III
National Institute of Standards and Technology 15, II
National Labor Relations Board 29, I
National Marine Fisheries Service 50, II, IV
National Mediation Board 29, X
National Oceanic and Atmospheric Administration 15, IX; 50, II, III,
IV, VI
National Park Service 36, I
National Railroad Adjustment Board 29, III
National Railroad Passenger Corporation (AMTRAK) 49, VII
National Science Foundation 45, VI; 48, 25
National Security Council 32, XXI
National Security Council and Office of Science and Technology Policy
47, II
National Telecommunications and Information Administration 15, XXIII;
47, III
National Transportation Safety Board 49, VIII
Navy Department 32, VI; 48, 52
Neighborhood Reinvestment Corporation 24, XXV
Nuclear Regulatory Commission 10, I
Occupational Safety and Health Administration 29, XVII
Occupational Safety and Health Review Commission 29, XX
Office of Independent Counsel 28, VII
Office of Navajo and Hopi Indian Relocation 25, IV
Offices of Independent Counsel, Department of Justice 28, VI
Operations Office, Department of Agriculture 7, XXVIII
Overseas Private Investment Corporation 22, VII
Oversight Board 12, XV
Packers and Stockyards Administration 9, II
Panama Canal Commission 48, 35
Panama Canal Regulations 35, I
Patent and Trademark Office 37, I
Payment from a non-Federal source for travel expenses 41, 304
Payment of Expenses Connected With the Death of Certain Employees 41,
303
Peace Corps 22, III
Pennsylvania Avenue Development Corporation 36, IX
Pension and Welfare Benefits Administration, Department of Labor 29,
XXV
Pension Benefit Guaranty Corporation 29, XXVI
Personnel Management, Office of 5, I; 45, VIII; 48, 17
Federal Employees Health Benefits Acquisition Regulation 48, 16
Postal Rate Commission 39, III
Postal Service, United States 39, I
Postsecondary Education, Office of 34, VI
President's Commission on White House Fellowships 1, IV
Presidential Documents 3
Prisons, Bureau of 28, V
Productivity, Technology and Innovation, Assistant Secretary
(Commerce) 37, IV
Property Management Regulations System, Federal 41, Subtitle C
Public Contracts, Department of Labor 41, 50
Public Health Service 42, I
Railroad Retirement Board 20, II
Reclamation Bureau 43, I
Refugee Resettlement, Office of 45, IV
Regional Action Planning Commissions 13, V
Relocation Allowances 41, 302
Research and Special Programs Administration 49, I
Resolution Trust Corporation 12, XVI
Rural Electrification Administration 7, XVII
Rural Telephone Bank 7, XVI
Saint Lawrence Seaway Development Corporation 33, IV
Science and Technology Policy, Office of 32, XXIV
Science and Technology Policy, Office of, and National Security
Council 47, II
Secret Service 31, IV
Securities and Exchange Commission 17, II
Selective Service System 32, XVI
Small Business Administration 13, I; 48, 22
Smithsonian Institution 36, V
Social Security Administration 20, III; 45, IV
Soil Conservation Service 7, VI
Solar Energy and Energy Conservation Bank, Department of Housing and
Urban Development 24, XI
Soldiers' and Airmen's Home, United States 5, XI
Special Counsel, Office of 5, VIII
Special Education and Rehabilitative Services, Office of 34, III
State Department 22, I
Federal Acquisition Regulation 48, 6
Surface Mining and Reclamation Appeals, Board of 30, III
Susquehanna River Basin Commission 18, VIII
Technology Administration 15, XI
Tennessee Valley Authority 18, XIII
Thrift Supervision Office, Department of the Treasury 12, V
Trade Representative, United States, Office of 15, XX
Transportation, Department of 44, IV
Coast Guard 33, I; 46, I, III; 49, IV
Commercial Space Transportation, Office of 14, III
Contract Appeals Board 48, 63
Federal Acquisition Regulation 48, 12
Federal Aviation Administration 14, I
Federal Highway Administration 23, I, II; 49, III
Federal Railroad Administration 49, II
Maritime Administration 46, II
National Highway Traffic Safety Administration 23, II, III; 49, V
Research and Special Programs Administration 49, I
Saint Lawrence Seaway Development Corporation 33, IV
Secretary of Transportation, Office of 14, II; 49, Subtitle A
Urban Mass Transportation Administration 49, VI
Transportation, Office of, Department of Agriculture 7, XXXIII
Travel Allowances 41, 301
Travel and Tourism Administration, United States 15, XII
Treasury Department 17, IV
Alcohol, Tobacco and Firearms, Bureau of 27, I
Comptroller of the Currency 12, I
Customs Service, United States 19, I
Engraving and Printing, Bureau of 31, VI
Federal Acquisition Regulation 48, 10
Federal Law Enforcement Training Center 31, VII
Fiscal Service 31, II
Foreign Assets Control, Office of 31, V
Internal Revenue Service 26, I
Monetary Offices 31, I
Secret Service 31, IV
Secretary of the Treasury, Office of 31, Subtitle A
Thrift Supervision Office 12, V
United States Customs Service 19, I
Truman, Harry S. Scholarship Foundation 45, XVIII
Under Secretary for Technology, Department of Commerce 37, V
United States and Canada, International Joint Commission 22, IV
United States Arms Control and Disarmament Agency 22, VI
United States Customs Service 19, I
United States Fish and Wildlife Service 50, I, IV
United States Information Agency 22, V; 48, 19
United States International Development Cooperation Agency 22, XII
United States International Trade Commission 19, II
United States Postal Service 39, I
United States Soldiers' and Airmen's Home 5, XI
United States Trade Representative, Office of 15, XX
United States Travel and Tourism Adminstration 15, XII
Urban Mass Transportation Administration 49, VI
Veterans Affairs Department 38, I; 48, 8
Veterans' Employment and Training, Office of the Assistant Secretary
for 41, 61; 20, IX
Vice President of the United States, Office of 32, XXVIII
Vocational and Adult Education, Office of 34, IV
Wage and Hour Division 29, V
Water Resources Council 18, VI
Workers' Compensation Programs, Office of 20, I
World Agriculture Outlook Board 7, XXXVIII
40 CFR 60.748 40 CFR (7-1-92 Edition)
40 CFR 60.748 List of CFR Sections Affected
40 CFR 60.748 List of CFR Sections Affected
All changes in this volume of the Code of Federal Regulations which
were made by documents published in the Federal Register since January
1, 1986, are enumerated in the following list. Entries indicate the
nature of the changes effected. Page numbers refer to Federal Register
pages. The user should consult the entries for chapters and parts as
well as sections for revisions.
For the period before January 1, 1986, see the ''List of CFR Sections
Affected, 1949-1963, 1964-1972, and 1973-1985'' published in seven
separate volumes.
40 CFR 60.748 1986
40 CFR
51 FR
Page
Chapter I
57.102 (b)(3) corrected 10211
58.1 (s) revised 9586
58.26 (b)(2) removed; (b)(3) redesignated as (b)(2) 9586
58.35 (c)(1) revised 9586
58.36 Added 9586
58.40 (c) revised 9586
58 Appendix A revised 9587
Appendix B amended 9596
Appendixes C and D amended 9597
Appendix E amended 9598
Appendixes F and G amended 9600
60 Authority delegation notices 3171,
3172, 6736, 8673, 9190, 11021, 11727, 12144, 14993, 15886, 20648,
22520 26546, 27033-27037, 27407, 32641, 32642, 33041-33046, 34216,
44984, 46856
Existing regulations unchanged 43572
60.4 (b)(RR) amended 4344,
(b)(FF) revised 15770
(b)(MM) introductory text and (ix) revised 23419
(b)(FF)(1) table amended; (b)(BBB) revised 26547
(b)(Q) and (AA) revised; (b)(R) added 37910
60.11 (e)(4) corrected 1790
60.13 (c) introductory text amended; (c) (1) and (2) added 21765
60.16 Amended 42796
60.17 (a)(38) revised; (a)(46) added 2702
(a) (1) and (10) revised; (a)(47) added 42794
60.18 Added 2701
60.40b -- 60.49b (Subpart Db) Added 42788
60.44 (a) (1) and (2) revised 42797
60.45 (c)(1) revised 21166
60.46 (a) (2), (4), and (5), (f) (2), (3) introductory text and (i)
revised; (c) amended 21166
(a) (2) and (3), (b), (c), and (f)(3)(ii) revised 42841
60.46b (d) (1), (2) introductory text, (i), and (ii), (5), and (6)
revised; (d)(2)(iii) added 42841
60.47a (h) (1) and (4) amended; (i)(1) revised 21166
60.48a (a)(1) revised 21166
(a) (1) through (6) revised; (a)(7) removed 42842
60.90 -- 60.93 (Subpart I) Heading revised (classification corrected
at 51 FR 12325) 3300
Heading correctly republished 12325
60.90 (a) revised (classification corrected at 51 FR 12325) 3300
(a) correctly republished 12325
60.91 Revised (classification corrected at 51 FR 12325) 3300
Correctly republished 12325
60.106 (a)(1)(i) and (2) revised 42842
60.140 -- 60.144 (Subpart N) Heading revised 160
60.141 (a), (b), and (c) revised; (d) added 160
60.142 (a) introductory text revised; (b) and (c) added 161
60.143 (b)(2) and (c) revised; OMB number 161
60.144 (b) revised; OMB number 161
60.140a -- 60.145a (Subpart Na) Added 161
60.280 Revised 18544
60.281 (e) revised 18544
60.283 (a)(1) introductory text, (iv), and (v) and (4) revised 18544
60.284 (a)(2) introductory text and (b)(1) introductory text, (d)
introductory text, (3) introductory text and (ii) revised; (c)(4)
added; OMB number 18545
60.466 (c) revised 22938
60.482-10 (d) revised 2702
60.633 (g) revised 2702
60 Appendix A amended 20288, 21166
Appendix A corrected 29104
Appendix A amended 32455, 42842
Appendix B amended 21766
40 CFR 60.748 1987
40 CFR
52 FR
Page
Chapter I
53 Technical correction 27902
53.1 (j) revised; (m) and (n) added; eff. 7-31-87 24727
53.2 Revised; eff. 7-31-87 24727
53.3 Revised; eff. 7-31-87 24727
53.4 (a) and (b)(3) amended; footnote 1 removed; (b) (4) through
(6) and (c) revised; eff. 7-31-87 24727
53.9 (c) revised; (d), (f), and (g) amended; eff. 7-31-87 24728
53.20 -- 53.23 (Subpart B) Heading revised; eff. 7-31-87 24728
53.30 -- 53.34 (Subpart C) Heading revised; eff. 7-31-87 24728
53.30 (a), (b)(2) heading, (c) and (d)(2) heading, (3) and (4)
revised; (b)(4) added; eff. 7-31-87 24728
53.31 (b) heading revised; (b) text amended; eff. 7-31-87 24728
53.32 Heading revised; (c) (1), (2), (3) (i) and (ii) and (4)
amended; eff. 7-31-87 24728
53.33 Heading and (h) (2) and (3) revised; (b), (e), (h) heading and
(i) amended; eff. 7-31-87 24728
53.34 Added; eff. 7-31-87 24729
53.40 -- 53.43 (Subpart D) Added; eff. 7-31-87 24729
58.1 (t), (u), and (v) added; eff. 7-31-87 24739
58.13 (b) revised; (c) added; eff. 7-31-87 24739
58.20 (e) amended; eff. 7-31-87 24740
58.23 Introductory text revised; eff. 7-31-87 24740
58.30 (a) introductory text amended; eff. 7-31-87 24740
58.34 Introductory text amended; eff. 7-31-87 24740
58.35 (d) amended; eff. 7-31-87 24740
58 Appendix A, B and C amended; eff. 7-31-87 24741
Appendix D amended; eff. 7-31-87 24742
58 Appendices D and E corrected 27286
Appendix E amended; eff. 7-31-87 24744
Appendix F amended; eff. 7-31-87 24748
60 Appendix F corrected 27612
Appendix G amended; eff. 7-31-87 24749
60 Authority delegation notices 8585-8587, 9164, 23178, 28255, 33934,
35083-35085, 35087, 35088, 35090, 35091, 36033, 36417, 36418, 42114
Authority citation corrected 37874
60.4 (b)(FF)(1) revised 19512
60.7 (a)(7) added 9781
60.11 (b) revised; (e)(1) amended; (e) (5), (6), and (7)
redesignated as (e) (6), (7), and (8); new (e)(5) added; new (e)(6)
revised 9781
60.13 (c) revised 9782
(j) correctly added 17555
(a) revised 21007
60.16 Amended 11428
60.17 (a) (1), (3), (7) through (10), (24) through (28), and (47)
revised; (a) (48) through (53) added 47842
60.17 (a) (13) and (37) and (c) introductory text and (1) revised
11429
60.40b -- 60.49b (Subpart Db) Revised 47842
60.43 (a)(2) revised; (e) added 28954
60.45 (c)(1) revised 21007
60.46 (h) added 28955
60.47a (h) introductory text, (1) and (2) and (i)(1) revised 21007
60.106 (d) introductory text amended; (d)(2) revised 20392
60.110 -- 60.113 (Subpart K) Heading revised 11429
60.111 (l) revised 11429
60.110a -- 60.115a (Subpart Ka) Heading revised 11429
60.111a (g) revised 11429
60.113a (a)(1)(i) introductory text revised; (a)(1)(i) (D) and (E)
added 11429
60.114a Revised 11429
60.110b -- 60.117b (Subpart Kb) Added 11429
60.117b (b) correctly revised 22780
60.285 (d) (1) and (3) revised 36409
60.300 (b) correctly revised 42434
60.330 Correctly revised 42434
60.343 (b) revised 4773
60.344 (c) revised 4774
60.540 -- 60.548 (Subpart BBB) Added 34874
60.543 (a) and (h) introductory text corrected 37874
60.546 (c)(2) corrected 37874
60 Appendix A amended 5106, 9658, 20392, 34639, 36410, 36415, 41425,
47853
Appendix A corrected 10852, 19797, 22888, 33316, 42061
Appendixes A and B amended 30675
Appendix B amended 34650
Appendix B corrected 17556
Appendix F added 21007
60 Appendix F corrected 27612
Appendix G added 28955
40 CFR 60.748 1988
40 CFR
53 FR
Page
Chapter I
53 Petition denied 52705
58 Petition denied 52705
60 Authority citation revised 2675
Authority delegation notices 3891,
8182, 12517, 17038, 22172, 23390,
24698, 27685,
45764, 46614
60.4 (b)(G), (BB), (JJ), (QQ), (TT), and (ZZ) revised; (b) Region
VIII table removed; (c) added 12520
(b) (P), (Y), and (KK) revised 18985
(b)(WW)(iii) revised 24449
(c) table revised 50527
60.17 (a) (54) and (55) and (g) added 5872
60.61 (b), (c), and (d) added 50363
60.63 (b), (c), (d), and (e) added 50363
60.64 (a)(5) added 50364
60.65 Added 50364
60.66 Added 50364
60.106 (b) amended 41333
60.153 (a) introductory text republished; (a)(1) revised; (b), (c),
(d), and (e) added 39416
60.154 (d) added 39417
60.155 Added 39417
60.156 Added 39418
60.286 (a)(2) introductory text revised 12009
60.530 -- 60.539a (Subpart January 1, 1988) Added 5873
60.533 (k)(2) introductory text corrected 14889
60.536 (j) introductory text and (3) through (8) correctly removed;
(j)(1) and (2) correctly revised 12009
60.538 (a) corrected 14889
60.690 -- 60.699 (Subpart QQQ) Added 47623
60.710 -- 60.718 (Subpart SSS) Added 38914
60.711 (c) Table 1B corrected 43799
(b)(26) and Table 1A corrected 47955
Correctly designated 49822
60.713 (a)(2) and (b)(1)(iii)(C) and (9)(ii) corrected 43799
(a) introductory text and (3)(i) and (b)(5)(i)(D) corrected 47955
60.715 (d) corrected 43799
60.717 (f) introductory text and (1) corrected 43799
(d)(2), (4)(ii)(C), and (7) and (h) corrected 47955
60.718 (b) corrected 47955
60.720 -- 60.726 (Subpart TTT) Added 2676
60.726 (b) correctly revised 19300
60 Appendix A corrected 2914,
11591, 12498, 14889
Appendix A amended 4142,
5884, 29682
Appendixes A and B amended 41333
Appendix A corrected 41649
Appendix B amended 7515
Appendix I added 5913
40 CFR 60.748 1989
40 CFR
54 FR
Page
Chapter I
58 Appendix D amended 15183
60 Authority delegation notices 5078,
12627, 12910, 18495-18496, 26041, 50754
Determination of status 13385
Petition denied 27166
60.2 Amended 6662
60.4 (a) amended; (b)(E), (T), (GG) and (LL)(i) revised 32445
(b)(I) amended 40664
(b)(GG)(i) added 52032
60.8 (b) and (e)(1) amended 6662
(b) corrected 21344
60.17 (a)(56), (57), (58), and (59) added 34026
(h) added 51825
60.22 (a) revised 52189
60.41b Amended 51819
60.42b (a) amended; (d), (e) and (f) revised; (j) added 51819
60.43a (h) (1) and (2) amended 6663
(h) (1) and (2) corrected 21344
60.43b (b) and (f) revised 51819
60.44a (a)(1) and (c) amended 6664
60.44b (a) and (b) amended; (h) revised; (i), (j), and (k) added
51825
60.45 (c)(1) revised; (f)(3) amended 6662
60.45b (d) introductory text revised; (j) added 51820
(b) revised 51825
60.46 Revised 6662
(b)(1) corrected 21344
60.46a (d)(3) and (h) amended 6664
60.46b (d) introductory text revised 51820
(c) revised; (g) and (h) added 51825
60.47a (f), (h), (i) introductory text, (1) and (2) revised; (j)
added 6664
60.47b (a) amended; (f) added 51820
60.48a (d) redesignated as (f); new (d) added; (a), (b), (c) and
(e) added 6664
60.48b (b) revised; (i) added 51825
60.49b (r) added 51820
(a)(2), (b), (e), (g) introductory text revised; (p) and (q) added
51825
60.54 Revised 6665
60.64 Revised 6666
60.73 (a) revised; (b) amended 6666
60.74 Revised 6666
60.84 (a), (b), and (d) amended 6666
60.85 Revised 6666
60.93 Revised 6667
60.100 Heading and (b) revised; (c), (d), and (e) added 34026
60.101 (m), (n), (o), (p), and (q) added 34027
60.102 Introductory text added; (a) introductory text revised 34027
60.103 Revised 34027
60.104 Heading and (a) introductory text revised; (b), (c), and (d)
added 34027
60.105 Heading and (a) introductory text and (c) revised; (a)(8),
(9), (10), (11), (12), (13), and (14) added; (e)(4) removed 34028
60.106 (a)(7) amended; (e), (f), (g), and (h) added 34028
60.107 Added 34029
60.108 Added 34030
60.109 Added 34031
60.110b (c) revised 32973
60.111b (f) introductory text revised 32973
60.113b (a)(2) and (4) revised 32973
60.123 Revised 6667
60.133 Revised 6667
60.143 (b)(5) and (c) amended 6667
60.144 Revised 6667
60.144a (d) (1) and (2) redesignated as (c) (1) and (2); (a), (b),
(c) introductory text and (d) revised 6667
60.154 Revised 6668
(c) and (d) added 27015
60.165 (b)(2) (i) and (ii) amended 6668
60.166 Revised 6668
60.175 (a)(2) (i) and (ii) amended 6668
60.176 Revised 6669
60.185 (a)(2) (i) and (ii) amended 6668
60.186 Revised 6669
60.194 (c) and (d) redesignated from 60.195 (a) and (b) 6669
60.195 (a) and (b) redesignated as 60.194 (c) and (d); revised 6669
60.203 (b) amended 6669
60.204 Revised 6669
60.213 (b) amended 6670
60.214 Revised 6670
60.223 (b) amended 6670
60.224 Revised 6670
60.233 (b) amended 6670
60.234 Revised 6670
(b)(3)(ii) corrected 21344
60.243 (b) amended 6671
60.244 Revised 6671
60.253 (b) amended 6671
60.254 Revised 6671
60.266 Revised 6671
(c)(1) corrected 21344
60.273 (c) revised 6672
60.275 (c) redesignated as 60.276 (c); (a), (b), (d), (e) (f)
revised; new (c) added 6672
(b) correctly designated; (e)(2) corrected 21344
60.276 (c) redesignated from 60.275 (c); (b) amended 6672
60.273a (c) revised 6672
60.275a (d) redesignated as 60.276a (f); (a), (b), (c), (e) and (f)
revised; new (d) added 6673
(e)(2) corrected 21344
60.276a (f) redesignated from 60.275a (d); (e) amended 6673
60.285 Revised 6673
(c) (1), (2) and (d)(3) corrected 21344
60.292 (a)(2) amended 6674
60.296 Revised 6674
(b)(1) and (d)(1) corrected 21344
60.303 Revised 6674
60.335 Revised 6675
(c)(1) amended 27016
60.343 (e) amended 6675
60.344 Revised 6675
60.374 Revised 6675
60.385 (c) amended 6676
60.386 Revised 6676
60.404 Revised 6676
(b)(1) corrected 21344
60.424 Revised 6676
60.474 Revised 6677
(c)(4) introductory text amended 27016
60.485 Revised 6678
(g)(4) amended 27016
60.502 (h) amended 6678
60.503 Revised 6678
(c)(3) corrected 21344
60.540 (a) and (b) revised 38635
60.542a Added 38635
60.543 (b) (1) and (2) amended; (b)(4), (f)(2)(iv) and (n) added;
(d) and (f)(2) introductory text revised 38635
60.545 (f) added 38637
60.546 (c)(7), (i), and (j) added 38637
60.547 (a)(5) added 38638
60.643 (b) revised 6679
60.644 Revised 6679
60.645 Removed 6679
60.646 (a) (2), (4) and (d) amended 6680
60.675 Revised 6680
60.676 (d) amended 6680
60.685 Revised 6680
60.721 (a) amended 25459
60.740 -- 60.748 (Subpart VVV) Added 37551
60 Appendix A amended 12622, 46235, 46238
Appendix A corrected 51550
40 CFR 60.748 1990
40 CFR
55 FR
Page
Chapter I
60 Authority delegation notices 28,
5990, 19882, 23077
New stationary sources performance standards review 11338
Authority delegation notices 28393, 48233
60.1 Introductory text designated as (a); (b) added 51382
60.2 Amended 51382
60.4 (c) table revised 29016
(c) table revised 39406
60.7 (c) introductory text and (1) revised; (d) through (f)
redesignated as (e) through (g); new (d) and Figure 1 added 51382
60.17 (a)(6) and (38) revised; (a)(46) removed; (a)(47) through
(55) redesignated as (a)(46) through (54) 26922
(a)(6) and (38) amended 26942
(a)(1), (10), and (50) revised 37683
(a)(6), (38), and (40) revised; (a)(60) and (61) added 51053
(a)(56) through (59) amended 40175
60.40c -- 60.48c (Subpart Dc) Added 37683
60.45 (c)(1) amended 18876
(g) introductory text revised 51382
60.46 (b)(2)(ii), (4)(ii), (5)(ii), (d)(1)(ii), (4) and (6) amended;
(d)(7) added 5212
60.46b (d)(1) amended 18876
60.47a (h)(3), (j)(1) and (3) amended; (j)(4) added 5212
(i)(1) amended 18876
60.47b (b)(2) amended 5212
Corrected 18876
60.48a (b)(2)(ii) amended 5212
60.54 (b)(3), (c)(1)(iii) and (2)(ii) amended 5212
60.103 (a) amended 40175
60.104 (a)(1), (2)(i) and (ii) revised 40175
60.105 (a)(1) through (7), (13)(i), (d) and (e) revised; (a)(14)
removed 40175
60.106 (a) through (d) revised; (e) through (h) redesignated as (g)
through (j); new (e), (f) and (k) added 40176
(h)(3) through (5), (i) introductory text, (2)(i) and (7) amended
40178
(j)(3)(ii) amended 40178
60.107 (b)(1)(ii), (2), (c)(1)(i) through (iii) amended 40178
60.108 (d) amended 40178
60.109 (b)(2) amended 40178
60.266 (c)(5) amended 5212
60.285 (b)(2) and (d)(2) amended 5212
60.315 (b) revised; (c) redesignated as (d); new (c) added (OMB
number) 51383
60.395 (b) and (c) revised (OMB number) 51383
60.447 (b) revised; (c) redesignated as (d); new (c) added 51383
60.455 (b) revised; (c) redesignated as (d); new (c) added (OMB
number) 51383
60.465 (c) redesignated as (e); new (c) and (d) added (OMB number)
51383
60.495 (b) revised; (c) and (d) redesignated as (d) and (e); new
(c) added 51384
60.560 -- 60.566 (Subpart DDD) Added 51035
60.604 (a)(2) revised 51384
60.610 -- 60.618 (Subpart III) Added 26922
60.611 Corrected 36932
60.614 (e)(2) table corrected 36932
60.615 (b)(3) corrected 36932
60.660 -- 60.668 (Subpart NNN) Added 26942
60.665 (g)(4) corrected 36932
60 Appendix A amended 5212,
5616, 21753, 25604
Appendix A amended 47472-47474
Appendix A corrected 48208
Appendix B amended 18876
Appendix B amended 40178, 47474
40 CFR 60.748 1991
40 CFR
56 FR
Page
Chapter I
58 Appendix D amended 64483
60 Authority delegation notices 8280, 13079
Authority delegation notices 13589
Authority delegation notices 29182
Authority delegation notices 50518, 55826, 59886, 63875, 65994
60.4 (c) table revised; eff. 8-19-91 28324
(c) table corrected 41391
60.17 (h) revised; eff. 8-12-91 5506
60.30 Revised 5523
60.32 Removed 5525
60.33 Removed 5525
60.34 Removed 5525
60.30a -- 60.39a (Subpart Ca) Added 5523
60.30b -- 60.32b (Subpart Cb) Added 5525
60.50a -- 60.59a (Subpart Ea) Added; eff. 8-12-91 5506
60.106 (b)(2) revised 4176
60.465 (c) corrected 20497
60.495 (c)(2) corrected 20497
60.561 Corrected 9178
60.562-1 (a)(1)(i)(A), (ii) Table 3, (iii) introductory text, (c)
introductory text and (1)(i)(B) corrected 9178
60.564 (e)(1) and (j)(1)(iii) corrected 9178
60.565 (a)(3)(i), (c)(2)(ii), (e)(2), (f)(1)(i), (ii), (2), (3) and
(h) introductory text corrected 9178
60 Appendix B amended 5526
Appendix F amended 5527
Appendix A amended 5760, 5774
40 CFR 60.748 1992
40 CFR
57 FR
Page
Chapter I
57.103 (p) removed; (q) through (x) redesignated as (p) through (w)
5328
57.806 (a)(2) revised 5328
57.809 (c)(2) amended 5328
60 Authority delegation notices 5388, 19262, 22176
60.4 (b)(H), (U), (W), (EE), (OO) and (UU) revised 1226
60.539 (h)(1) and (3) amended; (h)(2) revised 5328
Appendix A corrected 24550
40
Protection of Environment
PARTS 53 TO 60
Revised as of July 1, 1992
CONTAINING
A CODIFICATION OF DOCUMENTS
OF GENERAL APPLICABILITY
AND FUTURE EFFECT
AS OF JULY 1, 1992
With Ancillaries
Published by
the Office of the Federal Register
National Archives and Records
Administration
as a Special Edition of
the Federal Register
Washington, DC 20402-9328
40 CFR 60.748 Table of Contents
Page
Explanation v
Title 40:
Chapter I -- Environmental Protection Agency (Parts 53 to 60) 3
Finding Aids:
Material Approved for Incorporation by Reference
Table of CFR Titles and Chapters
Alphabetical List of Agencies Appearing in the CFR
List of CFR Sections Affected
40 CFR 60.748 Explanation
The Code of Federal Regulations is a codification of the general and
permanent rules published in the Federal Register by the Executive
departments and agencies of the Federal Government. The Code is divided
into 50 titles which represent broad areas subject to Federal
regulation. Each title is divided into chapters which usually bear the
name of the issuing agency. Each chapter is further subdivided into
parts covering specific regulatory areas.
Each volume of the Code is revised at least once each calendar year
and issued on a quarterly basis approximately as follows:
Title 1 through Title 16 as of January 1
Title 17 through Title 27 as of April 1
Title 28 through Title 41 as of July 1
Title 42 through Title 50 as of October 1
The appropriate revision date is printed on the cover of each volume.
LEGAL STATUS
The contents of the Federal Register are required to be judicially
noticed (44 U.S.C. 1507). The Code of Federal Regulations is prima facie
evidence of the text of the original documents (44 U.S.C. 1510).
HOW TO USE THE CODE OF FEDERAL REGULATIONS
The Code of Federal Regulations is kept up to date by the individual
issues of the Federal Register. These two publications must be used
together to determine the latest version of any given rule.
To determine whether a Code volume has been amended since its
revision date (in this case, July 1, 1992), consult the ''List of CFR
Sections Affected (LSA),'' which is issued monthly, and the ''Cumulative
List of Parts Affected,'' which appears in the Reader Aids section of
the daily Federal Register. These two lists will identify the Federal
Register page number of the latest amendment of any given rule.
EFFECTIVE AND EXPIRATION DATES
Each volume of the Code contains amendments published in the Federal
Register since the last revision of that volume of the Code. Source
citations for the regulations are referred to by volume number and page
number of the Federal Register and date of publication. Publication
dates and effective dates are usually not the same and care must be
exercised by the user in determining the actual effective date. In
instances where the effective date is beyond the cut-off date for the
Code a note has been inserted to reflect the future effective date. In
those instances where a regulation published in the Federal Register
states a date certain for expiration, an appropriate note will be
inserted following the text.
OMB CONTROL NUMBERS
The Paperwork Reduction Act of 1980 (Pub. L. 96-511) requires Federal
agencies to display an OMB control number with their information
collection request. Many agencies have begun publishing numerous OMB
control numbers as amendments to existing regulations in the CFR. These
OMB numbers are placed as close as possible to the applicable
recordkeeping or reporting requirements.
OBSOLETE PROVISIONS
Provisions that become obsolete before the revision date stated on
the cover of each volume are not carried. Code users may find the text
of provisions in effect on a given date in the past by using the
appropriate numerical list of sections affected. For the period before
January 1, 1986, consult either the List of CFR Sections Affected,
1949-1963, 1964-1972, or 1973-1985, published in seven separate volumes.
For the period beginning January 1, 1986, a ''List of CFR Sections
Affected'' is published at the end of each CFR volume.
INCORPORATION BY REFERENCE
What is incorporation by reference? Incorporation by reference was
established by statute and allows Federal agencies to meet the
requirement to publish regulations in the Federal Register by referring
to materials already published elsewhere. For an incorporation to be
valid, the Director of the Federal Register must approve it. The legal
effect of incorporation by reference is that the material is treated as
if it were published in full in the Federal Register (5 U.S.C. 552(a)).
This material, like any other properly issued regulation, has the force
of law.
What is a proper incorporation by reference? The Director of the
Federal Register will approve an incorporation by reference only when
the requirements of 1 CFR part 51 are met. Some of the elements on
which approval is based are:
(a) The incorporation will substantially reduce the volume of
material published in the Federal Register.
(b) The matter incorporated is in fact available to the extent
necessary to afford fairness and uniformity in the administrative
process.
(c) The incorporating document is drafted and submitted for
publication in accordance with 1 CFR part 51.
Properly approved incorporations by reference in this volume are
listed in the Finding Aids at the end of this volume.
What if the material incorporated by reference cannot be found? If
you have any problem locating or obtaining a copy of material listed in
the Finding Aids of this volume as an approved incorporation by
reference, please contact the agency that issued the regulation
containing that incorporation. If, after contacting the agency, you
find the material is not available, please notify the Director of the
Federal Register, National Archives and Records Administration,
Washington DC 20408, or call (202) 523-4534.
CFR INDEXES AND TABULAR GUIDES
A subject index to the Code of Federal Regulations is contained in a
separate volume, revised annually as of January 1, entitled CFR Index
and Finding Aids. This volume contains the Parallel Table of Statutory
Authorities and Agency Rules (Table I), and Acts Requiring Publication
in the Federal Register (Table II). A list of CFR titles, chapters, and
parts and an alphabetical list of agencies publishing in the CFR are
also included in this volume.
An index to the text of ''Title 3 -- The President'' is carried
within that volume.
The Federal Register Index is issued monthly in cumulative form.
This index is based on a consolidation of the ''Contents'' entries in
the daily Federal Register.
A List of CFR Sections Affected (LSA) is published monthly, keyed to
the revision dates of the 50 CFR titles.
REPUBLICATION OF MATERIAL
There are no restrictions on the republication of material appearing
in the Code of Federal Regulations.
INQUIRIES AND SALES
For a summary, legal interpretation, or other explanation of any
regulation in this volume, contact the issuing agency. Inquiries
concerning editing procedures and reference assistance with respect to
the Code of Federal Regulations may be addressed to the Director, Office
of the Federal Register, National Archives and Records Administration,
Washington, DC 20408 (telephone 202-512-1557). All mail order sales are
handled exclusively by the Superintendent of Documents, Attn: New
Orders, P.O. Box 371954, Pittsburgh, PA 15250-7954. Charge orders may
be telephoned to the Government Printing Office order desk at
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Martha L. Girard,
Director,
Office of the Federal Register.
July 1, 1992.
40 CFR 60.748 THIS TITLE
Title 40 -- Protection of Environment is composed of fifteen volumes.
The parts in these volumes are arranged in the following order: parts
1-51, part 52, parts 53-60, parts 61-80, parts 81-85, parts 86-99, parts
100-149, parts 150-189, parts 190-259, parts 260-299, parts 300-399,
parts 400-424, parts 425-699, parts 700-789 and part 790 to End. The
contents of these volumes represent all current regulations codified
under this title of the CFR as of July 1, 1992.
Chapter I -- Environmental Protection Agency appears in all fifteen
volumes. A Pesticide Tolerance Commodity/Chemical Index appears in
parts 150-189. A Toxic Substances Chemical -- CAS Number Index appears
in parts 700-789 and part 790 to End. Distribution Tables appear in the
volumes containing parts 100-149, parts 190-259 and parts 260-299.
Redesignation Tables appear in the volumes containing parts 1-51, parts
150-189, and parts 700-789. Regulations issued by the Council on
Environmental Quality appear in the volume containing part 790 to End.
For this volume, Sheli E. Fleming was Chief Editor. The Code of
Federal Regulations publication program is under the direction of
Richard L. Claypoole, assisted by Alomha S. Morris.
40 CFR 0.0 40 CFR Ch. I (7-1-92 Edition)
40 CFR 0.0 Environmental Protection Agency
40 CFR 0.0 Title 40 -- Protection of Environment
40 CFR 0.0 (This book contains parts 61-80)
Part
chapter i -- Environmental Protection Agency (Continued) 61
40 CFR 0.0 40 CFR Ch. I (7-1-92 Edition)
40 CFR 0.0 Environmental Protection Agency
40 CFR 0.0 CHAPTER I -- ENVIRONMENTAL PROTECTION AGENCY
40 CFR 0.0
40 CFR 0.0 SUBCHAPTER C -- AIR PROGRAMS (Continued)
Part
Page
61 National emission standards for hazardous air pollutants
62 Approval and promulgation of State plans for designated facilities
and pollutants
65 Delayed compliance orders
66 Assessment and collection of noncompliance penalties by EPA
67 EPA approval of State noncompliance penalty program
69 Special exemptions from requirements of the Clean Air Act
73 Sulphur dioxide allowance system
79 Registration of fuels and fuel additives
80 Regulation of fuels and fuel additives
Editorial Note: Subchapter C -- Air Programs is continued in the
volumes containing 40 CFR parts 81-85 and 86-99.
40 CFR 0.0 40 CFR Ch. I (7-1-92 Edition)
40 CFR 0.0 Environmental Protection Agency
40 CFR 0.0 SUBCHAPTER C -- AIR PROGRAMS (Continued)
40 CFR 0.0 Pt. 61
40 CFR 0.0 PART 61 -- NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS
40 CFR 0.0 Subpart A -- General Provisions
Sec.
61.01 Lists of pollutants and applicability of part 61.
61.02 Definitions.
61.03 Units and abbreviations.
61.04 Address.
61.05 Prohibited activities.
61.06 Determination of construction or modification.
61.07 Application for approval of construction or modification.
61.08 Approval of construction or modification.
61.09 Notification of startup.
61.10 Source reporting and request for waiver of compliance.
61.11 Waiver of compliance.
61.12 Compliance with standards and maintenance requirements.
61.13 Emission tests and waiver of emission tests.
61.14 Monitoring requirements.
61.15 Modification.
61.16 Availability of information.
61.17 State authority.
61.18 Incorporations by reference.
61.19 Circumvention.
40 CFR 0.0 Subpart B -- National Emission Standards for Radon
Emissions From Underground Uranium Mines
61.20 Designation of facilities.
61.21 Definitions
61.22 Standard.
61.23 Determining compliance.
61.24 Annual reporting requirements.
61.25 Recordkeeping requirements.
61.26 Exemption from the reporting and testing requirements of 40 CFR
61.10
40 CFR 0.0 Subpart C -- National Emission Standard for Beryllium
61.30 Applicability.
61.31 Definitions.
61.32 Emission standard.
61.33 Stack sampling.
61.34 Air sampling.
40 CFR 0.0 Subpart D -- National Emission Standard for Beryllium
Rocket Motor Firing
61.40 Applicability.
61.41 Definitions.
61.42 Emission standard.
61.43 Emission testing -- rocket firing or propellant disposal.
61.44 Stack sampling.
40 CFR 0.0 Subpart E -- National Emission Standard for Mercury
61.50 Applicability.
61.51 Definitions.
61.52 Emission standard.
61.53 Stack sampling.
61.54 Sludge sampling.
61.55 Monitoring of emissions and operations.
61.56 Delegation of authority.
40 CFR 0.0 Subpart F -- National Emission Standard for Vinyl Chloride
61.60 Applicability.
61.61 Definitions.
61.62 Emission standard for ethylene dichloride plants.
61.63 Emission standard for vinyl chloride plants.
61.64 Emission standard for polyvinyl chloride plants.
61.65 Emission standard for ethylene dichloride, vinyl chloride and
polyvinyl chloride plants.
61.66 Equivalent equipment and procedures.
61.67 Emission tests.
61.68 Emission monitoring.
61.69 Initial report.
61.70 Reporting.
61.71 Recordkeeping.
40 CFR 0.0 Subpart G -- (Reserved)
40 CFR 0.0 Subpart H -- National Emission Standards for Emissions of
Radionuclides Other Than Radon From Department of Energy Facilities
61.90 Designation of facilities.
61.91 Definitions.
61.92 Standard.
61.93 Emissions monitoring and test procedures.
61.94 Compliance and reporting.
61.95 Recordkeeping requirements.
61.96 Applications to construct or modify.
61.97 Exemption from the reporting and testing requirements of 40 CFR
61.10.
40 CFR 0.0 Subpart I -- National Emission Standards for Radionuclide
Emissions From Facilities Licensed by the Nuclear Regulatory Commission
and Federal Facilities Not Covered by subpart H
61.100 Applicability.
61.101 Definitions.
61.102 Standard.
61.103 Determining compliance.
61.104 Reporting requirements.
61.105 Recordkeeping requirements.
61.106 Applications to construct or modify.
61.107 Emission determination.
61.108 Exemption from the reporting and testing requirements of 40
CFR 61.10.
61.109 Stay of effective date.
40 CFR 0.0 Subpart J -- National Emission Standard for Equipment Leaks
(Fugitive Emission Sources) of Benzene
61.110 Applicability and designation of sources.
61.111 Definitions.
61.112 Standards.
40 CFR 0.0 Subpart K -- National Emission Standards for Radionuclide
Emissions From Elemental Phosphorus Plants
61.120 Applicability.
61.121 Definitions.
61.122 Emission standard.
61.123 Emission testing.
61.124 Recordkeeping requirements.
61.125 Test methods and procedures.
61.126 Monitoring of operations.
61.127 Exemption from the reporting and testing requirements of 40
CFR 61.10
40 CFR 0.0 Subpart L -- National Emission Standard for Benzene
Emissions from Coke By-Product Recovery Plants
61.130 Applicability, designation of sources, and delegation of
authority.
61.131 Definitions.
61.132 Standard: Process vessels, storage tanks, and
tar-intercepting sumps.
61.133 Standard: Light-oil sumps.
61.134 Standard: Naphthalene processing, final coolers, and
final-cooler cooling towers.
61.135 Standard: Equipment leaks.
61.136 Compliance provisions and alternative means of emission
limitation.
61.137 Test methods and procedures.
61.138 Recordkeeping and reporting requirements.
61.139 Provisions for alternative means for process vessels, storage
tanks, and tar-intercepting sumps.
40 CFR 0.0 Subpart M -- National Emission Standard for Asbestos
61.140 Applicability.
61.141 Definitions.
61.142 Standard for asbestos mills.
61.143 Standard for roadways.
61.144 Standards for manufacturing.
61.145 Standard for demolition and renovation.
61.146 Standard for spraying.
61.147 Standard for fabricating.
61.148 Standard for insulating materials.
61.149 Standard for waste disposal for asbestos mills.
61.150 Standard for waste disposal for manufacturing, fabricating,
demolition, renovation, and spraying operations.
61.151 Standard for inactive waste disposal sites for asbestos mills
and manufacturing and fabricating operations.
61.152 Air-cleaning.
61.153 Reporting.
61.154 Standard for active waste disposal sites.
61.155 Standard for operations that convert asbestos-containing waste
material into nonasbestos (asbestos-free) material.
61.156 Cross-reference to other asbestos regulations.
61.157 Delegation of authority.
40 CFR 0.0 Subpart N -- National Emission Standard for Inorganic
Arsenic Emissions from Glass Manufacturing Plants
61.160 Applicability and designation of source.
61.161 Definitions.
61.162 Emission limits.
61.163 Emission monitoring.
61.164 Test methods and procedures.
61.165 Reporting and recordkeeping requirements.
40 CFR 0.0 Subpart O -- National Emission Standard for Inorganic
Arsenic Emissions from Primary Copper Smelters
61.170 Applicability and designation of source.
61.171 Definitions.
61.172 Standard for new and existing sources.
61.173 Compliance provisions.
61.174 Test methods and procedures.
61.175 Monitoring requirements.
61.176 Recordkeeping requirements.
61.177 Reporting requirements.
40 CFR 0.0 Subpart P -- National Emission Standard for Inorganic
Arsenic Emissions from Arsenic Trioxide and Metallic Arsenic Production
Facilities
61.180 Applicability and designation of sources.
61.181 Definitions.
61.182 Standard for new and existing sources.
61.183 Emission monitoring.
61.184 Ambient air monitoring for inorganic arsenic.
61.185 Recordkeeping requirements.
61.186 Reporting requirements.
40 CFR 0.0 Subpart Q -- National Emission Standards for Radon
Emissions From Department of Energy Facilities
61.190 Designation of facilities.
61.191 Definitions.
61.192 Standard.
61.193 Exemption from the reporting and testing requirements of 40
CFR 61.10.
40 CFR 0.0 Subpart R -- National Emission Standards for Radon
Emissions From Phosphogypsum Stacks
61.200 Designation of facilities.
61.201 Definitions.
61.202 Standard.
61.203 Radon monitoring and compliance procedures.
61.204 Distribution and use of phosphogypsum for agricultural
purposes.
61.205 Distribution and use of phosphogypsum for research and
development.
61.206 Distribution and use of phosphogypsum for other purposes.
61.207 Radium-226 sampling and measurement procedures.
61.208 Certification requirements.
61.209 Required records.
61.210 Exemption from the reporting and testing requirements of 40
CFR 61.10.
40 CFR 0.0 Subpart S -- (Reserved)
40 CFR 0.0 Subpart T -- National Emission Standards for Radon
Emissions From the Disposal of Uranium Mill Tailings
61.220 Designation of facilities.
61.221 Definitions.
61.222 Standard.
61.223 Compliance procedures.
61.224 Recordkeeping requirements.
61.225 Exemption from the reporting and testing requirements of 40
CFR 61.10.
40 CFR 0.0 Subpart U -- (Reserved)
40 CFR 0.0 Subpart V -- National Emission Standard for Equipment Leaks
(Fugitive Emission Sources)
61.240 Applicability and designation of sources.
61.241 Definitions.
61.242-1 Standards: General.
61.242-2 Standards: Pumps.
61.242-3 Standards: Compressors.
61.242-4 Standards: Pressure relief devices in gas/vapor service.
61.242-5 Standards: Sampling connection systems.
61.242-6 Standards: Open-ended valves or lines.
61.242-7 Standards: Valves.
61.242-8 Standards: Pressure relief devices in liquid service and
flanges and other connectors.
61.242-9 Standards: Product accumulator vessels.
61.242-10 Standards: Delay of repair.
61.242-11 Standards: Closed-vent systems and control devices.
61.243-1 Alternative standrds for valves in UHAP Service -- allowable
percentage of valves leaking.
61.243-2 Alternative standards for valves in VHAP service -- skip
period leak detection and repair.
61.244 Alternative means of emission limitation.
61.245 Test methods and procedures.
61.246 Recordkeeping requirements.
61.247 Reporting requirements.
40 CFR 0.0 Subpart W -- National Emission Standards for Radon
Emissions From Operating Mill Tailings
61.250 Designation of facilities.
61.251 Definitions.
61.252 Standard.
61.253 Determining compliance.
61.254 Annual reporting requirements.
61.255 Recordkeeping requirements.
61.256 Exemption from the reporting and testing requirements of 40
CFR 61.10.
40 CFR 0.0 Subpart X -- (Reserved)
40 CFR 0.0 Subpart Y -- National Emission Standard for Benzene
Emissions from Benzene Storage Vessels
61.270 Applicability and designation of sources.
61.271 Emission standard.
61.272 Compliance provisions.
61.273 Alternative means of emission limitation.
61.274 Initial report.
61.275 Periodic report.
61.276 Recordkeeping.
61.277 Delegation of authority.
40 CFR 0.0 Subparts Z-AA -- (Reserved)
40 CFR 0.0 Subpart BB -- National Emission Standard for Benzene
Emissions from Benzene Transfer Operations
61.300 Applicability.
61.301 Definitions.
61.302 Standards.
61.303 Monitoring requirements.
61.304 Test methods and procedures.
61.305 Reporting and recordkeeping.
61.306 Delegation of authority.
40 CFR 0.0 Subparts CC-EE -- (Reserved)
40 CFR 0.0 Subpart FF -- National Emission Standard for Benzene Waste
Operations
61.340 Applicability.
61.341 Definitions.
61.342 Standards: General.
61.343 Standards: Tanks.
61.344 Standards: Surface impoundments.
61.345 Standards: Containers.
61.346 Standards: Individual drain systems.
61.347 Standards: Oil-water separators.
61.348 Standards: Treatment processes.
61.349 Standards: Closed-vent systems and control devices.
61.350 Standards: Delay of repair.
61.351 Alternative standards for tanks.
61.352 Alternative standards for oil-water separators.
61.353 Alternative means of emission limitation.
61.354 Monitoring of operations.
61.355 Test methods, procedures, and compliance provisions.
61.356 Recordkeeping requirements.
61.357 Reporting requirements.
61.358 Delegation of authority.
61.359 Stay of effective date.
Appendix A to Part 61 -- National Emission Standards for Hazardous
Air Pollutants, Compliance Status Information
Appendix B to Part 61 -- Test Methods
Appendix C to Part 61 -- Quality Assurance Procedures
Appendix D to Part 61 -- Methods for Estimating Radionuclide
Emissions
Appendix E to Part 61 -- Compliance Procedures Methods for
Determining Compliance with Subpart I
Authority: Secs. 101, 112, 114, 116, 301, Clean Air Act as amended
(42 U.S.C. 7401, 7412, 7414, 7416, 7601).
Source: 38 FR 8826, Apr. 6, 1973, unless otherwise noted.
40 CFR 0.0 Subpart A -- General Provisions
40 CFR 61.01 Lists of pollutants and applicability of part 61.
(a) The following list presents the substances that, pursuant to
section 112 of the Act, have been designated as hazardous air
pollutants. The Federal Register citations and dates refer to the
publication in which the listing decision was originally published.
Asbestos (36 FR 5931; Mar. 31, 1971)
Benzene (42 FR 29332; June 8, 1977)
Beryllium (36 FR 5931; Mar. 31, 1971)
Coke Oven Emissions (49 FR 36560; Sept. 18, 1984)
Inorganic Arsenic (45 FR 37886; June 5, 1980)
Mercury (36 FR 5931; Mar. 31, 1971)
Radionuclides (44 FR 76738; Dec. 27, 1979)
Vinyl Chloride (40 FR 59532; Dec. 24, 1975)
(b) The following list presents other substances for which a Federal
Register notice has been published that included consideration of the
serious health effects, including cancer, from ambient air exposure to
the substance.
Acrylonitrile (50 FR 24319; June 10, 1985)
1,3-Butadiene (50 FR 41466; Oct. 10, 1985)
Cadmium (50 FR 42000; Oct. 16, 1985)
Carbon Tetrachloride (50 FR 32621; Aug. 13, 1985)
Chlorinated Benzenes (50 FR 32628; Aug. 13, 1985)
Chlorofluorocarbon -- 113 (50 FR 24313; June 10, 1985)
Chloroform (50 FR 39626; Sept. 27, 1985)
Chloroprene (50 FR 39632; Sept. 27, 1985)
Chromium (50 FR 24317; June 10, 1985)
Copper (52 FR 5496; Feb. 23, 1987)
Epichlorohydrin (50 FR 24575; June 11, 1985)
Ethylene Dichloride (50 FR 41994; Oct. 16, 1985)
Ethylene Oxide (50 FR 40286; Oct. 2, 1985)
Hexachlorocyclopentadiene (50 FR 40154; Oct. 1, 1985)
Manganese (50 FR 32627; Aug. 13, 1985)
Methyl Chloroform (50 FR 24314; June 10, 1985)
Methylene Chloride (50 FR 42037; Oct. 17, 1985)
Nickel (51 FR 34135; Sept. 25, 1986)
Perchloroethylene (50 FR 52800; Dec. 26, 1985)
Phenol (51 FR 22854; June 23, 1986)
Polycyclic Organic Matter (49 FR 31680; Aug. 8, 1984)
Toluene (49 FR 22195; May 25, 1984)
Trichloroethylene (50 FR 52422; Dec. 23, 1985)
Vinylidene Chloride (50 FR 32632; Aug. 13, 1985)
Zinc and Zinc Oxide (52 FR 32597, Aug. 28, 1987)
(c) This part applies to the owner or operator of any stationary
source for which a standard is prescribed under this part.
(50 FR 46290, Nov. 7, 1985, as amended at 51 FR 7715 and 7719, Mar.
5, 1986; 51 FR 11022, Apr. 1, 1986; 52 FR 37617, Oct. 8, 1987)
40 CFR 61.02 Definitions.
The terms used in this part are defined in the Act or in this section
as follows:
Act means the Clean Air Act (42 U.S.C. 7401 et seq.).
Administrator means the Administrator of the Environmental Protection
Agency or his authorized representative.
Alternative method means any method of sampling and analyzing for an
air pollutant which is not a reference method but which has been
demonstrated to the Administrator's satisfaction to produce results
adequate for the Administrator's determination of compliance.
Capital expenditure means an expenditure for a physical or
operational change to a stationary source which exceeds the product of
the applicable ''annual asset guideline repair allowance percentage''
specified in the latest edition of Internal Revenue Service (IRS)
Publication 534 and the stationary source's basis, as defined by section
1012 of the Internal Revenue Code. However, the total expenditure for a
physical or operational change to a stationary source must not be
reduced by any ''excluded additions'' as defined for stationary sources
constructed after December 31, 1981, in IRS Publication 534, as would be
done for tax purposes. In addition, ''annual asset guideline repair
allowance'' may be used even though it is excluded for tax purposes in
IRS Publication 534.
Commenced means, with respect to the definition of ''new source'' in
section 111(a)(2) of the Act, that an owner or operator has undertaken a
continuous program of construction or modification or that an owner or
operator has entered into a contractual obligation to undertake and
complete, within a reasonable time, a continuous program of construction
or modification.
Compliance schedule means the date or dates by which a source or
category of sources is required to comply with the standards of this
part and with any steps toward such compliance which are set forth in a
waiver of compliance under 61.11.
Construction means fabrication, erection, or installation of an
affected facility.
Effective date is the date of promulgation in the Federal Register of
an applicable standard or other regulation under this part.
Existing source means any stationary source which is not a new
source.
Monitoring system means any system, required under the monitoring
sections in applicable subparts, used to sample and condition (if
applicable), to analyze, and to provide a record of emissions or process
parameters.
New source means any stationary source, the construction or
modification of which is commenced after the publication in the Federal
Register of proposed national emission standards for hazardous air
pollutants which will be applicable to such source.
Owner or operator means any person who owns, leases, operates,
controls, or supervises a stationary source.
Reference method means any method of sampling and analyzing for an
air pollutant, as described in Appendix B to this part.
Run means the net period of time during which an emission sample is
collected. Unless otherwise specified, a run may be either intermittent
or continuous within the limits of good engineering practice.
Standard means a national emission standard including a design,
equipment, work practice or operational standard for a hazardous air
pollutant proposed or promulgated under this part.
Startup means the setting in operation of a stationary source for any
purpose.
Stationary source means any building, structure, facility, or
installation which emits or may emit any air pollutant which has been
designated as hazardous by the Administrator.
(44 FR 55174, Sept. 25, 1979, as amended at 50 FR 46290, Nov. 7,
1985)
40 CFR 61.03 Units and abbreviations.
Used in this part are abbreviations and symbols of units of measure.
These are defined as follows:
(a) System International (SI) units of measure:
A=ampere
g=gram
Hz=hertz
J=joule
K=degree Kelvin
kg=kilogram
m=meter
m2=square meter
m3=cubic meter
mg=milligram=10^3 gram
mm=millimeter=10^3 meter
Mg=megagram=10^6 gram
mol=mole
N=newton
ng=nanogram=10^9 gram
nm=nanometer=10^9 meter
Pa=pascal
s=second
V=volt
W=watt
V=ohm
g=microgram=10^6 gram
(b) Other units of measure:
C=degree Celsius (centigrade)
cfm=cubic feet per minute
cc=cubic centimeter
Ci=curie
d=day
F=degree Fahrenheit
ft2=square feet
ft3=cubic feet
gal=gallon
in=inch
in Hg=inches of mercury
in H2O=inches of water
l=liter
lb=pound
lpm=liter per minute
min=minute
ml=milliliter=10^3 liter
mrem=millirem=10^3 rem
oz=ounces
pCi=picocurie=10^12 curie
psig=pounds per square inch gage
R=degree Rankine
l=microliter=10^6 liter
v/v=volume per volume
yd2=square yards
yr=year
(c) Chemical nomenclature:
Be=beryllium
Hg=mercury
H2O=water
(d) Miscellaneous:
act=actual
avg=average
I.D.=inside diameter
M=molar
N=normal
O.D.=outside diameter
%=percent
std=standard
(42 FR 51574, Sept. 29, 1977, as amended at 54 FR 51704, Dec. 15,
1989)
40 CFR 61.04 Address.
(a) All requests, reports, applications, submittals, and other
communications to the Administrator pursuant to this part shall be
submitted in duplicate to the appropriate Regional Office of the U.S.
Environmental Protection Agency to the attention of the Director of the
Division indicated in the following list of EPA Regional Offices.
Region I (Connecticut, Maine, Massachusetts,New Hampshire, Rhode
Island, Vermont), Director, Air Management Division, U.S. Environmental
Protection Agency, John F. Kennedy Federal Building, Boston, MA 02203.
Region II (New Jersey, New York, Puerto Rico, Virgin Islands),
Director, Air and Waste Management Division, U.S. Environmental
Protection Agency, Federal Office Building, 26 Federal Plaza (Foley
Square), New York, NY 10278.
Region III (Delaware, District of Columbia, Maryland, Pennsylvania,
Virginia, West Virginia), Director, Air and Waste Management Division,
U.S. Environmental Protection Agency,Curtis Building, Sixth and Walnut
Streets, Philadelphia, PA 19106.
Region IV (Alabama, Florida, Georgia, Kentucky, Mississippi, North
Carolina, South Carolina, Tennessee), Director, Air and Waste Management
Division, U.S. Environmental Protection Agency, 345 Courtland Street,
NE., Atlanta, GA 30365.
Region V (Illinois, Indiana, Michigan, Minnesota, Ohio, Wisconsin),
Director, Air Management Division, U.S. Environmental Protection Agency,
230 South Dearborn Street, Chicago, IL 60604.
Region VI (Arkansas, Louisiana, New Mexico, Oklahoma, Texas);
Director; Air, Pesticides, and Toxics Division; U.S. Environmental
Protection Agency, 1445 Ross Avenue, Dallas, Texas 75202.
Region VII (Iowa, Kansas, Missouri, Nebraska), Director, Air and
Toxics Division, U.S. Environmental Protection Agency, 726 Minnesota
Avenue, Kansas City, KS 66101.
Region VIII (Colorado, Montana, North Dakota, South Dakota, Utah,
Wyoming), Director, Air and Waste Management Division, U.S.
Environmental Protection Agency, 1860 Lincoln Street, Denver, CO 80295.
Region IX (American Samoa, Arizona, California, Guam, Hawaii,
Nevada), Director, Air and Waste Management Division, U.S.
Environmental Protection Agency, 215 Fremont Street, San Francisco, CA
94105.
Region X (Alaska, Oregon, Idaho, Washington), Director, Air and Waste
Management Division, U.S. Environmental Protection Agency, 1200 Sixth
Avenue, Seattle, WA 98101.
(b) Section 112(d) directs the Administrator to delegate to each
State, when appropriate, the authority to implement and enforce national
emission standards for hazardous air pollutants for stationary sources
located in such State. If the authority to implement and enforce a
standard under this part has been delegated to a State, all information
required to be submitted to EPA under paragraph (a) of this section
shall also be submitted to the appropriate State agency (provided, that
each specific delegation may exempt sources from a certain Federal or
State reporting requirement). The Administrator may permit all or some
of the information to be submitted to the appropriate State agency only,
instead of to EPA and the State agency. The appropriate mailing address
for those States whose delegation request has been approved is as
follows:
(A) (Reserved)
(B) State of Alabama, Air Pollution Control Division, Air Pollution
Control Commission, 645 S. McDonough Street, Montgomery, AL 36104.
(C) State of Alaska, Department of Environmental Conservation, 3220
Hospital Drive, Juneau, AK 99811.
(D) Arizona.
Arizona Department of Health Services, 1740 West Adams Street,
Phoenix, AZ 85007.
Maricopa County Department of Health Services, Bureau of Air
Pollution Control, 1825 East Roosevelt Street, Phoenix, AZ. 85006.
Pima County Health Department, Air Quality Control District, 151 West
Congress, Tucson, AZ. 85701.
(E) State of Arkansas: Chief, Division of Air Pollution Control,
Arkansas Department of Pollution Control and Ecology, 8001 National
Drive, P.O. Box 9583, Little Rock, Arkansas 72209.
(F) California.
Amador County Air Pollution Control District, P.O. Box 430, 810 Court
Street, Jackson, CA 95642.
Bay Area Air Pollution Control District, 939 Ellis Street, San
Francisco, CA. 94109.
Butte County Air Pollution Control District, P.O. Box 1229, 316
Nelson Avenue, Oroville, CA 95965.
Calaveras County Air Pollution Control District, Government Center,
El Dorado Road, San Andreas, CA 95249.
Colusa County Air Pollution Control District, 751 Fremont Street,
Colusa, CA 95952.
El Dorado Air Pollution Control District, 330 Fair Lane, Placerville,
CA 95667.
Fresno County Air Pollution Control District, 1221 Fulton Mall,
Fresno, CA 93721.
Glenn County Air Pollution Control District, P.O. Box 351, 720 North
Colusa Street, Willows, CA 95988.
Great Basin Unified Air Pollution Control District, 157 Short Street,
Suite 6, Bishop, CA 93514.
Imperial County Air Pollution Control District, County Services
Building, 939 West Main Street, El Centro, CA 92243.
Kern County Air Pollution Control District, 1601 H Street, Suite 250,
Bakersfield, CA 93301.
Kings County Air Pollution Control District, 330 Campus Drive,
Hanford, CA 93230.
Lake County Air Pollution Control District, 255 North Forbes Street,
Lakeport, CA 95453.
Lassen County Air Pollution Control District, 175 Russell Avenue,
Susanville, CA 96130.
Madera County Air Pollution Control District, 135 West Yosemite
Avenue, Madera, CA. 93637.
Mariposa County Air Pollution Control District, Box 5, Mariposa, CA
95338.
Mendocino County Air Pollution Control District, County Courthouse,
Ukiah, CA. 94582.
Merced County Air Pollution Control District, P.O. Box 471, 240 East
15th Street, Merced, CA 95340.
Modoc County Air Pollution Control District, 202 West 4th Street,
Alturas, CA 96101.
Monterey Bay Unified Air Pollution Control, 1164 Monroe Street, Suite
10, Salinas, CA 93906.
Nevada County Air Pollution Control District, H.E.W. Complex, Nevada
City, CA 95959.
North Coast Unified Air Quality Management District, 5630 South
Broadway, Eureka CA 95501.
Northern Sonoma County Air Pollution Control District, 134 ''A''
Avenue, Auburn, CA 95448.
Placer County Air Pollution Control District, 11491 ''B'' Avenue,
Auburn, CA 95603.
Plumas County Air Pollution Control District, P.O. Box 480, Quincy,
CA 95971.
Sacramento County Air Pollution Control District, 3701 Branch Center
Road, Sacramento, CA. 95827.
San Bernardino County Air Pollution Control District, 15579-8th,
Victorville, CA 92392.
San Diego County Air Pollution Control District, 9150 Chesapeake
Drive, San Diego, CA. 92123.
San Joaquin County Air Pollution Control District, 1601 East Hazelton
Street (P.O. Box 2009), Stockton, CA. 95201.
San Luis Obispo County Air Pollution Control District, P.O. Box 637,
San Luis Obispo, CA 93406.
Santa Barbara County Air Pollution Control District, 315 Camino del
Rimedio, Santa Barbara, CA 93110.
Shasta County Air Pollution Control District, 2650 Hospital Lane,
Redding, CA 96001.
Sierra County Air Pollution Control District, P.O. Box 286,
Downieville, CA 95936.
Siskiyou County Air Pollution Control District, 525 South Foothill
Drive, Yreka, CA 96097.
South Coast Air Quality Management District, 9150 Flair Drive, El
Monte, CA 91731.
Stanislaus County Air Pollution Control District, 1030 Scenic Drive,
Modesto, CA 95350.
Sutter County Air Pollution Control District, Sutter County Office
Building, 142 Garden Highway, Yuba City, CA 95991.
Tehama County Air Pollution Control District, P.O. Box 38, 1760
Walnut Street, Red Bluff, CA 96080.
Tulare County Air Pollution Control District, County Civic Center,
Visalia, CA 93277.
Tuolumne County Air Pollution Control District, 9 North Washington
Street, Sonora, CA 95370.
Ventura County Air Pollution Control District, 800 South Victoria
Avenue, Ventura, CA 93009.
Yolo-Solano Air Pollution Control District, P.O. Box 1006, 323 First
Street, #5, Woodland, CA 95695.
(G) State of Colorado, Department of Health, Air Pollution Control
Division, 4210 East 11th Avenue, Denver, CO 80220.
Editorial Note: For a table listing Region VIII's NESHAPs delegation
status, see paragraph (c) of this section.
(H) State of Connecticut, Bureau of Air Management, Department of
Environmental Protection, State Office Building, 165 Capitol Avenue,
Hartford, CT 06106.
(I) State of Delaware:
Delaware Department of Natural Resources and Environmental Control,
Tatnall Building, P.O. Box 1401, Dover, DE 19901.
(J) (Reserved)
(K) Bureau of Air Quality Management, Department of Environmental
Regulation, Twin Towers Office Building, 2600 Blair Stone Road,
Tallahassee, FL 32301.
(L) State of Georgia, Environmental Protection Division, Department
of Natural Resources, 270 Washington Street, SW., Atlanta, GA 30334.
(M) Hawaii Department of Health, 1250 Punchbowl Street, Honolulu, HI
96813.
Hawaii Department of Health (mailing address), Post Office Box 3378,
Honolulu, HI 96801.
(N)-(O) (Reserved)
(P) State of Indiana, Indiana Department of Environmental Management,
105 South Meridian Street, P.O. Box 6015, Indianapolis, Indiana 46206.
(Q) State of Iowa: Iowa Department of Natural Resources,
Environmental Protection Division, Henry A. Wallace Building, 900 East
Grand, Des Moines, IA 50319.
(R) State of Kansas: Kansas Department of Health and Environment,
Bureau of Air Quality and Radiation Control, Forbes Field, Topeka, KS
66620.
(S) Division of Air Pollution Control, Department for Natural
Resources and Environmental Protection, U.S. 127, Frankfort, KY 40601.
(T) State of Louisiana: Program Administrator, Air Quality Division,
Louisiana Department of Environmental Quality, P.O. Box 44096, Baton
Rouge, Louisiana 70804.
(U) State of Maine, Bureau of Air Quality Control, Department of
Environmental Protection, State House, Station No. 17, Augusta, ME
04333.
(V) State of Maryland, Bureau of Air Quality and Noise Control,
Maryland State Department of Health and Mental Hygiene, 201 West Preston
Street, Baltimore, MD 21201.
(W) Commonwealth of Massachusetts, Division of Air Quality Control,
Department of Environmental Protection, One Winter Street, 7th floor,
Boston, MA 02108.
(X) State of Michigan, Air Pollution Control Division, Michigan
Department of Natural Resources, Stevens T. Mason Building, 8th Floor,
Lansing, MI 48926.
(Y) Minnesota Pollution Control Agency, Division of Air Quality, 520
Lafayette Road, St. Paul, Minnesota 55155.
(Z) Bureau of Pollution Control, Department of Natural Resources,
P.O. Box 10385, Jackson, MS 39209.
(AA) State of Missouri: Missouri Department of Natural Resources,
Division of Environmental Quality, P.O. Box 176, Jefferson City, MO
65102.
(BB) State of Montana, Department of Health and Environmental
Services, Air Quality Bureau, Cogswell Building, Helena, MT 59601.
Editorial Note: For a table listing Region VIII's NESHAPs delegation
status, see paragraph (c) of this section.
(CC) State of Nebraska, Nebraska Department of Environmental Control,
P.O. Box 94877, State House Station, Lincoln, NB 68509.
Lincoln-Lancaster County Health Department, Division of Environmental
Health, 2200 St. Marys Avenue, Lincoln, NB 68502.
(DD) Nevada.
Clark County, County District Health Department, Air Pollution
Control Division, 625 Shadow Lane, Las Vegas, NV 89106.
Nevada Department of Conservation and Natural Resources, Division of
Environmental Protection, 201 South Fall Street, Carson City, NV 89710.
Washoe County District Health Department, Division of Environmental
Protection, 10 Kirman Avenue, Reno, NV 89502.
(EE) State of New Hampshire, Air Resources Division, Department of
Environmental Services, 64 North Main Street, Caller Box 2033, Concord,
NH 03302-2033.
(FF) State of New Jersey: New Jersey Department of Environmental
Protection, John Fitch Plaza, P.O. Box 2807, Trenton, NJ 08625.
(GG) State of New Mexico: Director, New Mexico Environmental
Improvement Division, Health and Environment Department, 1190 St.
Francis Drive, Santa Fe, New Mexico 87503.
(i) The City of Albuquerque and Bernalillo County: Director, The
Albuquerque Environmental Health Department, The City of Albuquerque,
P.O. Box 1293, Albuquerque, New Mexico 87103.
(HH) New York: New York State Department of Environmental
Conservation, 50 Wolf Road, Albany, NY 12233, attention: Division of
Air Resources.
(II) North Carolina Environmental Management Commission, Department
of Natural and Economic Resources, Division of Environmental Management,
P.O. Box 27687, Raleigh, NC 27611. Attention: Air Quality Section.
(JJ) State of North Dakota, State Department of Health and
Consolidated Laboratories, Division of Environmental Engineering, State
Capitol, Bismarck, ND 58505.
Editorial Note: For a table listing Region VIII's NESHAPs delegation
status, see paragraph (c) of this section.
(KK) State of Ohio --
(i) Medina, Summit and Portage Counties: Director, Akron Regional
Air Quality Management District, 177 South Broadway, Akron, OH 44308.
(ii) Stark County: Director, Air Pollution Control Division, Canton
City Health Department, City Hall Annex Second Floor, 218 Cleveland
Avenue S.W., Canton, OH 44702.
(iii) Butler, Clermont, Hamilton and Warren Counties: Director,
Southwestern Ohio Air Pollution Control Agency, 2400 Beekman Street,
Cincinnati, OH 45214.
(iv) Cuyahoga County: Commissioner, Division of Air Pollution
Control, Department of Public Health and Welfare, 2735 Broadway Avenue,
Cleveland, OH 44115.
(v) Belmont, Carroll, Columbiana, Harrison, Jefferson, and Monroe
Counties: Director, North Ohio Valley Air Authority (NOVAA), 814 Adams
Street, Steubenville, OH 43952.
(vi) Clark, Darke, Greene, Miami, Montgomery, and Preble Counties:
Supervisor, Regional Air Pollution Control Agency (RAPCA), Montgomery
County Health Department, 451 West Third Street, Dayton, OH 45402.
(vii) Lucas County and the City of Rossford (in Wood County):
Director, Toledo Environmental Services Agency, 26 Main Street, Toledo,
OH 43605.
(viii) Adams, Brown, Lawrence, and Scioto Counties:
Engineer-Director, Air Division, Portsmouth City Health Department, 740
Second Street, Portsmouth, OH 45662.
(ix) Allen, Ashland, Auglaize, Crawford, Defiance, Erie, Fulton,
Hancock, Hardin, Henry, Huron, Marion, Mercer, Ottawa, Paulding, Putnam,
Richland, Sandusky, Seneca, Van West, Williams, Wood (except City of
Rossford), and Wyandot Counties: Ohio Environmental Protection Agency,
Northwest District Office, Air Pollution Unit, 1035 Dezlaz Grove Drive,
Bowling Green, OH 43402.
(x) Ashtabula, Holmes, Lorain, and Wayne Counties: Ohio
Environmental Protection Agency, Northeast District Office, Air
Pollution Unit, 2110 East Aurora Road, Twinsburg, OH 44087.
(xi) Athens, Coshocton, Gallia, Guernsey, Hocking, Jackson, Meigs,
Morgan, Muskingum, Noble, Perry, Pike, Ross, Tuscarawas, Vinton, and
Washington Counties: Ohio Environmental Protection Agency, Southeast
District Office, Air Pollution Unit, 2195 Front Street, Logan, OH 43138.
(xii) Champaign, Clinton, Highland, Logan, and Shelby Counties: Ohio
Environmental Protection Agency, Southwest District Office, Air
Pollution Unit, East Fourth Street, Dayton, OH 45402.
(xiii) Delaware, Fairfield, Fayette, Franklin, Knox, Licking,
Madison, Morrow, Pickaway, and Union Counties; Ohio Environmental
Protection Agency, Central District Office, Air Pollution Unit, P.O.
Box 1049, Columbus, OH 43266-0149.
(xiv) Geauga and Lake Counties: Lake County General Health District,
Air Pollution Control, 105 Main Street, Painesville, OH 44077.
(xv) Mahoning and Trumbull Counties: Mahoning-Trumbull Air Pollution
Control Agency, 9 West Front Street, Youngstown, OH 44503.
(LL) State of Oklahoma, Oklahoma State Department of Health, Air
Quality Service, P.O. Box 53551, Oklahoma City, OK 73152.
(i) Oklahoma City and County: Director, Oklahoma City-County Health
Department, 921 Northeast 23rd Street, Oklahoma City, Oklahoma 73105.
(ii) Tulsa County: Tulsa City-County Health Department, 4616 East
Fifteenth Street, Tulsa, OK 74112.
(MM) State of Oregon, Department of Environmental Quality, Yeon
Building, 522 SW. Fifth, Portland, OR 97204.
(i)-(vii) (Reserved)
(viii) Lane Regional Air Pollution Authority, 225 North Fifth, Suite
501, Springfield, OR 97477.
(NN) Pennsylvania.
(i) City of Philadelphia: Philadelphia Department of Public Health,
Air Management Services, 500 S. Broad Street, Philadelphia, PA 19146.
(ii) Commonwealth of Pennsylvania: Department of Environmental
Resources, Post Office Box 2063, Harrisburg, PA 17120.
(iii) Allegheny County: Allegheny County Health Department, Bureau
of Air Pollution Control, 301 Thirty-ninth Street, Pittsburgh, PA,
15201.
(OO) State of Rhode Island, Division of Air and Hazardous Materials,
Department of Environmental Management, 291 Promenade Street,
Providence, RI 02908.
(PP) State of South Carolina, Office of Environmental Quality
Control, Department of Health and Environmental Control, 2600 Bull
Street, Columbia, SC 29201.
(QQ) State of South Dakota, Department of Water and Natural
Resources, Office of Air Quality and Solid Waste, Joe Foss Building, 523
East Capitol, Pierre, SD 57501-3181.
Editorial Note: For a table listing Region VIII's NESHAPs delegation
status, see paragraph (c) of this section.
(RR) Division of Air Pollution Control, Tennessee Department of
Public Health, 256 Capitol Hill Building, Nashville, TN 37219.
Knox County Department of Air Pollution, City/County Building, Room
L222, 400 Main Avenue, Knoxville, TN 37902.
Air Pollution Control Bureau, Metropolitan Health Department, 311
23rd Avenue North, Nashville, TN 37203.
(SS) State of Texas, Texas Air Control Board, 6330 Highway 290 East,
Austin, TX 78723.
(TT) State of Utah, Department of Health, Bureau of Air Quality, 288
North 1460 West, P.O. Box 16690, Salt Lake City, UT 84116-0690.
Editorial Note: For a table listing Region VIII's NESHAPs delegation
status, see paragraph (c) of this section.
(UU) State of Vermont, Air Pollution Control Division, Agency of
Natural Resources, Building 3 South, 103 South Main Street, Waterbury,
VT 05676.
(VV) Commonwealth of Virginia, Virginia State Air Pollution Control
Board, Room 1106, Ninth Street Office Building, Richmond, VA 23219.
(WW)(i) Washington; State of Washington, Department of Ecology,
Olympia, WA 98504.
(ii) Northwest Air Pollution Authority, 207 Pioneer Building, Second
and Pine Streets, Mount Vernon, WA 98273.
(iii) Puget Sound Air Pollution Control Agency, 200 West Mercer
Street, Room 205, Seattle, WA 98119-3958.
(iv) Spokane County Air Pollution Control Authority, North 811
Jefferson, Spokane, WA 99201.
(v) Yakima County Clean Air Authority, County Courthouse, Yakima, WA
98901.
(vi) Olympic Air Pollution Control Authority, 120 East State Avenue,
Olympia, WA 98501.
(vii) Southwest Air Pollution Control Authority, Suite 7601 H, NE
Hazel Dell Avenue, Vancouver, WA 98665.
(viii) Grant County Clean Air Authority, P.O. Box 37, Ephrata, WA
98823.
(XX) State of West Virginia: Air Pollution Control Commission, 1558
Washington Street, East, Charleston, WV 25311.
(YY) Wisconsin -- Wisconsin Department of Natural Resources, P.O.
Box 7921, Madison, WI 53707.
(ZZ)-(AAA) (Reserved)
(BBB) Commonwealth of Puerto Rico: Commonwealth of Puerto Rico
Environmental Quality Board, P.O. Box 11785, Santurce, PR 00910.
(CCC) U.S. Virgin Islands: U.S. Virgin Islands Department of
Conservation and Cultural Affairs, P.O. Box 578, Charlotte Amalie, St.
Thomas, U.S. Virgin Islands 00801.
(c) The following is a table indicating the delegation status of
National Emission Standards for Hazardous Air Pollutants in Region VIII.
40 CFR 61.04
(40 FR 18170, Apr. 25, 1975)
Editorial Note: For Federal Register citations to 61.04 see the
List of CFR Sections Affected appearing in the Finding Aids section of
this volume.
40 CFR 61.05 Prohibited activities.
(a) After the effective date of any standard, no owner or operator
shall construct or modify any stationary source subject to that standard
without first obtaining written approval from the Administrator in
accordance with this subpart, except under an exemption granted by the
President under section 112(c)(2) of the Act. Sources, the construction
or modification of which commenced after the publication date of the
standards proposed to be applicable to the sources, are subject to this
prohibition.
(b) After the effective date of any standard, no owner or operator
shall operate a new stationary source subject to that standard in
violation of the standard, except under an exemption granted by the
President under section 112(c)(2) of the Act.
(c) Ninety days after the effective date of any standard, no owner or
operator shall operate any existing source subject to that standard in
violation of the standard, except under a waiver granted by the
Administrator under this part or under an exemption granted by the
President under section 112(c)(2) of the Act.
(d) No owner or operator subject to the provisions of this part shall
fail to report, revise reports, or report source test results as
required under this part.
(38 FR 8826, Apr. 6, 1973, as amended at 50 FR 46291, Nov. 7, 1985)
40 CFR 61.06 Determination of construction or modification.
An owner or operator may submit to the Administrator a written
application for a determination of whether actions intended to be taken
by the owner or operator constitute construction or modification, or
commencement thereof, of a source subject to a standard. The
Administrator will notify the owner or operator of his determination
within 30 days after receiving sufficient information to evaluate the
application.
(50 FR 46291, Nov. 7, 1985)
40 CFR 61.07 Application for approval of construction or modification.
(a) The owner or operator shall submit to the Administrator an
application for approval of the construction of any new source or
modification of any existing source. The application shall be submitted
before the construction or modification is planned to commence, or
within 30 days after the effective date if the construction or
modification had commenced before the effective date and initial startup
has not occurred. A separate application shall be submitted for each
stationary source.
(b) Each application for approval of construction shall include --
(1) The name and address of the applicant;
(2) The location or proposed location of the source; and
(3) Technical information describing the proposed nature, size,
design, operating design capacity, and method of operation of the
source, including a description of any equipment to be used for control
of emissions. Such technical information shall include calculations of
emission estimates in sufficient detail to permit assessment of the
validity of the calculations.
(c) Each application for approval of modification shall include, in
addition to the information required in paragraph (b) of this section --
(1) The precise nature of the proposed changes;
(2) The productive capacity of the source before and after the
changes are completed; and
(3) Calculations of estimates of emissions before and after the
changes are completed, in sufficient detail to permit assessment of the
validity of the calculations.
(50 FR 46291, Nov. 7, 1985)
40 CFR 61.08 Approval of construction or modification.
(a) The Administrator will notify the owner or operator of approval
or intention to deny approval of construction or modification within 60
days after receipt of sufficient information to evaluate an application
under 61.07.
(b) If the Administrator determines that a stationary source for
which an application under 61.07 was submitted will not cause emissions
in violation of a standard if properly operated, the Administrator will
approve the construction or modification.
(c) Before denying any application for approval of construction or
modification, the Administrator will notify the applicant of the
Administrator's intention to issue the denial together with --
(1) Notice of the information and findings on which the intended
denial is based; and
(2) Notice of opportunity for the applicant to present, within such
time limit as the Administrator shall specify, additional information or
arguments to the Administrator before final action on the application.
(d) A final determination to deny any application for approval will
be in writing and will specify the grounds on which the denial is based.
The final determination will be made within 60 days of presentation of
additional information or arguments, or 60 days after the final date
specified for presentation if no presentation is made.
(e) Neither the submission of an application for approval nor the
Administrator's approval of construction or modification shall --
(1) Relieve an owner or operator of legal responsibility for
compliance with any applicable provisions of this part or of any other
applicable Federal, State, or local requirement; or
(2) Prevent the Administrator from implementing or enforcing this
part or taking any other action under the Act.
(50 FR 46291, Nov. 7, 1985)
40 CFR 61.09 Notification of startup.
(a) The owner or operator of each stationary source which has an
initial startup after the effective date of a standard shall furnish the
Administrator with written notification as follows:
(1) A notification of the anticipated date of initial startup of the
source not more than 60 days nor less than 30 days before that date.
(2) A notification of the actual date of initial startup of the
source within 15 days after that date.
(b) If any State or local agency requires a notice which contains all
the information required in the notification in paragraph (a) of this
section, sending the Administrator a copy of that notification will
satisfy paragraph (a) of this section.
(50 FR 46291, Nov. 7, 1985)
40 CFR 61.10 Source reporting and waiver request.
(a) The owner or operator of each existing source or each new source
which had an initial startup before the effective date shall provide the
following information in writing to the Administrator within 90 days
after the effective date:
(1) Name and address of the owner or operator.
(2) The location of the source.
(3) The type of hazardous pollutants emitted by the stationary
source.
(4) A brief description of the nature, size, design, and method of
operation of the stationary source including the operating design
capacity of the source. Identify each point of emission for each
hazardous pollutant.
(5) The average weight per month of the hazardous materials being
processed by the source, over the last 12 months preceding the date of
the report.
(6) A description of the existing control equipment for each emission
point including --
(i) Each control device for each hazardous pollutant; and
(ii) Estimated control efficiency (percent) for each control device.
(7) A statement by the owner or operator of the source as to whether
the source can comply with the standards within 90 days after the
effective date.
(b) The owner or operator of an existing source unable to comply with
an applicable standard may request a waiver of compliance with that
standard for a period not exceeding 2 years after the effective date.
Any request shall be in writing and shall include the following
information:
(1) A description of the controls to be installed to comply with the
standard.
(2) A compliance schedule, including the date each step toward
compliance will be reached. The list shall include as a minimum the
following dates:
(i) Date by which contracts for emission control systems or process
changes for emission control will be awarded, or date by which orders
will be issued for the purchase of component parts to accomplish
emission control or process changes;
(ii) Date of initiation of onsite construction or installation of
emission control equipment or process change;
(iii) Date by which onsite construction or installation of emission
control equipment or process change is to be completed; and
(iv) Date by which final compliance is to be achieved.
(3) A description of interim emission control steps which will be
taken during the waiver period.
(c) Any change in the information provided under paragraph (a) of
this section or 61.07(b) shall be provided to the Administrator within
30 days after the change. However, if any change will result from
modification of the source, 61.07(c) and 61.08 apply.
(d) A possible format for reporting under this section is included as
Appendix A of this part. Advice on reporting the status of compliance
may be obtained from the Administrator.
(38 FR 8826, Apr. 6, 1973, as amended at 50 FR 46292, Nov. 7, 1985)
40 CFR 61.11 Waiver of compliance.
(a) Based on the information provided in any request under 61.10, or
other information, the Administrator may grant a waiver of compliance
with a standard for a period not exceeding 2 years after the effective
date of the standard.
(b) The waiver will be in writing and will --
(1) Identify the stationary source covered;
(2) Specify the termination date of the waiver;
(3) Specify dates by which steps toward compliance are to be taken;
and
(4) Specify any additional conditions which the Administrator
determines necessary to assure installation of the necessary controls
within the waiver period and to assure protection of the health of
persons during the waiver period.
(c) The Administrator may terminate the waiver at an earlier date
than specified if any specification under paragraphs (b)(3) and (b)(4)
of this section are not met.
(d) Before denying any request for a waiver, the Administrator will
notify the owner or operator making the request of the Administrator's
intention to issue the denial, together with --
(1) Notice of the information and findings on which the intended
denial is based; and
(2) Notice of opportunity for the owner or operator to present,
within the time limit the Administrator specifies, additional
information or arguments to the Administrator before final action on the
request.
(e) A final determination to deny any request for a waiver will be in
writing and will set forth the specific grounds on which the denial is
based. The final determination will be made within 60 days after
presentation of additional information or argument; or within 60 days
after the final date specified for the presentation if no presentation
is made.
(f) The granting of a waiver under this section shall not abrogate
the Administrator's authority under section 114 of the Act.
(50 FR 46292, Nov. 7, 1985)
40 CFR 61.12 Compliance with standards and maintenance requirements.
(a) Compliance with numerical emission limits shall be determined by
emission tests established in 61.13 unless otherwise specified in an
individual subpart.
(b) Compliance with design, equipment, work practice or operational
standards shall be determined as specified in an individual subpart.
(c) The owner or operator of each stationary source shall maintain
and operate the source, including associated equipment for air pollution
control, in a manner consistent with good air pollution control practice
for minimizing emissions. Determination of whether acceptable operating
and maintenance procedures are being used will be based on information
available to the Administrator which may include, but is not limited to,
monitoring results, review of operating and maintenance procedures, and
inspection of the source.
(d)(1) If, in the Administrator's judgment, an alternative means of
emission limitation will achieve a reduction in emissions of a pollutant
from a source at least equivalent to the reduction in emissions of that
pollutant from that source achieved under any design, equipment, work
practice or operational standard, the Administrator will publish in the
Federal Register a notice permitting the use of the alternative means
for purposes of compliance with the standard. The notice will restrict
the permission to the source(s) or category(ies) of sources on which the
alternative means will achieve equivalent emission reductions. The
notice may condition permission on requirements related to the operation
and maintenance of the alternative means.
(2) Any notice under paragraph (d)(1) shall be published only after
notice and an opportunity for a hearing.
(3) Any person seeking permission under this subsection shall, unless
otherwise specified in the applicable subpart, submit a proposed test
plan or the results of testing and monitoring, a description of the
procedures followed in testing or monitoring, and a description of
pertinent conditions during testing or monitoring.
(50 FR 46292, Nov. 7, 1985)
40 CFR 61.13 Emission tests and waiver of emission tests.
(a) If required to do emission testing by an applicable subpart and
unless a waiver of emission testing is obtained under this section, the
owner or operator shall test emissions from the source --
(1) Within 90 days after the effective date, for an existing source
or a new source which has an initial startup date before the effective
date; or
(2) Within 90 days after initial startup, for a new source which has
an initial startup date after the effective date.
(b) The Administrator may require an owner or operator to test
emissions from the source at any other time when the action is
authorized by section 114 of the Act.
(c) The owner or operator shall notify the Administrator of the
emission test at least 30 days before the emission test to allow the
Administrator the opportunity to have an observer present during the
test.
(d) If required to do emission testing, the owner or operator of each
new source and, at the request of the Administrator, the owner or
operator of each existing source shall provide emission testing
facilities as follows:
(1) Sampling ports adequate for test methods applicable to each
source.
(2) Safe sampling platform(s).
(3) Safe access to sampling platform(s).
(4) Utilities for sampling and testing equipment.
(5) Any other facilities that the Administrator needs to safely and
properly test a source.
(e) Each emission test shall be conducted under such conditions as
the Administrator shall specify based on design and operational
characteristics of the source.
(f) Unless otherwise specified in an applicable subpart, samples
shall be analyzed and emissions determined within 30 days after each
emission test has been completed. The owner or operator shall report
the determinations of the emission test to the Administrator by a
registered letter sent before the close of business on the 31st day
following the completion of the emission test.
(g) The owner or operator shall retain at the source and make
available, upon request, for inspection by the Administrator, for a
minimum of 2 years, records of emission test results and other data
needed to determine emissions.
(h)(1) Emission tests shall be conducted as set forth in this
section, the applicable subpart and appendix B unless the Administrator
--
(i) Specifies or approves the use of a reference method with minor
changes in methodology; or
(ii) Approves the use of an alternative method; or
(iii) Waives the requirement for emission testing because the owner
or operator of a source has demonstrated by other means to the
Administrator's satisfaction that the source is in compliance with the
standard.
(2) If the Administrator finds reasonable grounds to dispute the
results obtained by an alternative method, he may require the use of a
reference method. If the results of the reference and alternative
methods do not agree, the results obtained by the reference method
prevail.
(3) The owner or operator may request approval for the use of an
alternative method at any time, except --
(i) For an existing source or a new source that had an initial
startup before the effective date, any request for use of an alternative
method during the initial emission test shall be submitted to the
Administrator within 30 days after the effective date, or with the
request for a waiver of compliance if one is submitted under 60.10(b);
or
(ii) For a new source that has an initial startup after the effective
date, any request for use of an alternative method during the initial
emission test shall be submitted to the Administrator no later than with
the notification of anticipated startup required under 60.09.
(i)(1) Emission tests may be waived upon written application to the
Administrator if, in the Administrator's judgment, the source is meeting
the standard, or the source is being operated under a waiver or
compliance, or the owner or operator has requested a waiver of
compliance and the Administrator is still considering that request.
(2) If application for waiver of the emission test is made, the
application shall accompany the information required by 61.10 or the
notification of startup required by 61.09, whichever is applicable. A
possible format is contained in appendix A to this part.
(3) Approval of any waiver granted under this section shall not
abrogate the Administrator's authority under the Act or in any way
prohibit the Administrator from later cancelling the waiver. The
cancellation will be made only after notice is given to the owner or
operator of the source.
(50 FR 46292, Nov. 7, 1985)
40 CFR 61.14 Monitoring requirements.
(a) Unless otherwise specified, this section applies to each
monitoring system required under each subpart which requires monitoring.
(b) Each owner or operator shall maintain and operate each monitoring
system as specified in the applicable subpart and in a manner consistent
with good air pollution control practice for minimizing emissions. Any
unavoidable breakdown or malfunction of the monitoring system should be
repaired or adjusted as soon as practicable after its occurrence. The
Administrator's determination of whether acceptable operating and
maintenance procedures are being used will be based on information which
may include, but not be limited to, review of operating and maintenance
procedures, manufacturer recommendations and specifications, and
inspection of the monitoring system.
(c) When required by the applicable subpart, and at any other time
the Administrator may require, the owner or operator of a source being
monitored shall conduct a performance evaluation of the monitoring
system and furnish the Administrator with a copy of a written report of
the results within 60 days of the evaluation. Such a performance
evaluation shall be conducted according to the applicable specifications
and procedures described in the applicable subpart. The owner or
operator of the source shall furnish the Administrator with written
notification of the date of the performance evaluation at least 30 days
before the evaluation is to begin.
(d) When the effluents from a single source, or from two or more
sources subject to the same emission standards, are combined before
being released to the atmosphere, the owner or operator shall install a
monitoring system on each effluent or on the combined effluent. If two
or more sources are not subject to the same emission standards, the
owner or operator shall install a separate monitoring system on each
effluent, unless otherwise specified. If the applicable standard is a
mass emission standard and the effluent from one source is released to
the atmosphere through more than one point, the owner or operator shall
install a monitoring system at each emission point unless the
installation of fewer systems is approved by the Administrator.
(e) The owner or operator of each monitoring system shall reduce the
monitoring data as specified in each applicable subpart. Monitoring
data recorded during periods of unavoidable monitoring system
breakdowns, repairs, calibration checks, and zero and span adjustments
shall not be included in any data average.
(f) The owner or operator shall maintain records of monitoring data,
monitoring system calibration checks, and the occurrence and duration of
any period during which the monitoring system is malfunctioning or
inoperative. These records shall be maintained at the source for a
minimum of 2 years and made available, upon request, for inspection by
the Administrator.
(g)(1) Monitoring shall be conducted as set forth in this section and
the applicable subpart unless the Administrator --
(i) Specifies or approves the use of the specified monitoring
requirements and procedures with minor changes in methodology; or
(ii) Approves the use of alternatives to any monitoring requirements
or procedures.
(2) If the Administrator finds reasonable grounds to dispute the
results obtained by an alternative monitoring method, the Administrator
may require the monitoring requirements and procedures specified in this
part.
(50 FR 46293, Nov. 7, 1985)
40 CFR 61.15 Modification.
(a) Except as provided under paragraph (d) of this section, any
physical or operational change to a stationary source which results in
an increase in the rate of emission to the atmosphere of a hazardous
pollutant to which a standard applies shall be considered a
modification.
(b) Upon modification, an existing source shall become a new source
for each hazardous pollutant for which the rate of emission to the
atmosphere increases and to which a standard applies.
(c) Emission rate shall be expressed as kg/hr of any hazardous
pollutant discharged into the atmosphere for which a standard is
applicable. The Administrator shall use the following to determine the
emission rate:
(1) Emission factors as specified in the background information
document (BID) for the applicable standard, or in the latest issue of
''Compilation of Air Pollutant Emission Factors,'' EPA Publication No.
AP-42, or other emission factors determined by the Administrator to be
superior to AP-42 emission factors, in cases where use of emission
factors demonstrates that the emission rate will clearly increase or
clearly not increase as a result of the physical or operational change.
(2) Material balances, monitoring data, or manual emission tests in
cases where use of emission factors, as referenced in paragraph (c)(1)
of this section, does not demonstrate to the Administrator's
satisfaction that the emission rate will clearly increase or clearly not
increase as a result of the physical or operational change, or where an
interested person demonstrates to the Administrator's satisfaction that
there are reasonable grounds to dispute the result obtained by the
Administrator using emission factors. When the emission rate is based
on results from manual emission tests or monitoring data, the procedures
specified in appendix C of 40 CFR part 60 shall be used to determine
whether an increase in emission rate has occurred. Tests shall be
conducted under such conditions as the Administrator shall specify to
the owner or operator. At least three test runs must be conducted
before and at least three after the physical or operational change. If
the Administrator approves, the results of the emission tests required
in 61.13(a) may be used for the test runs to be conducted before the
physical or operational change. All operating parameters which may
affect emissions must be held constant to the maximum degree feasible
for all test runs.
(d) The following shall not, by themselves, be considered
modifications under this part:
(1) Maintenance, repair, and replacement which the Administrator
determines to be routine for a source category.
(2) An increase in production rate of a stationary source, if that
increase can be accomplished without a capital expenditure on the
stationary source.
(3) An increase in the hours of operation.
(4) Any conversion to coal that meets the requirements specified in
section 111(a)(8) of the Act.
(5) The relocation or change in ownership of a stationary source.
However, such activities must be reported in accordance with 61.10(c).
(50 FR 46294, Nov. 7, 1985)
40 CFR 61.16 Availability of information.
The availability to the public of information provided to, or
otherwise obtained by, the Administrator under this part shall be
governed by Part 2 of this chapter.
(38 FR 8826, Apr. 6, 1973. Redesignated at 50 FR 46294, Nov. 7, 1985)
40 CFR 61.17 State authority.
(a) This part shall not be construed to preclude any State or
political subdivision thereof from --
(1) Adopting and enforcing any emission limiting regulation
applicable to a stationary source, provided that such emission limiting
regulation is not less stringent than the standards prescribed under
this part; or
(2) Requiring the owner or operator of a stationary source to obtain
permits, licenses, or approvals prior to initiating construction,
modification, or operation of the source.
(50 FR 46294, Nov. 7, 1985)
40 CFR 61.18 Incorporations by reference.
The materials listed below are incorporated by reference in the
corresponding sections noted. These incorporations by reference were
approved by the Director of the Federal Register on the date listed.
These materials are incorporated as they exist on the date of the
approval, and a notice of any change in these materials will be
published in the Federal Register. The materials are available for
purchase at the corresponding address noted below, and all are available
for inspection at the Office of the Federal Register, Room 8401, 1100 L
Street, NW., Washington, DC and the Library (MD-35), U.S. EPA, Research
Triangle Park, North Carolina.
(a) The following material is available for purchase from at least
one of the following addresses: American Society for Testing and
Materials (ASTM), 1916 Race Street, Philadelphia, Pennsylvania 19103;
or University Microfilms International, 300 North Zeeb Road, Ann Arbor,
Michigan 48106.
(1) ASTM D737-75, Standard Test Method for Air Permeability of
Textile Fabrics, incorporation by reference (IBR) approved January 27,
1983 for 61.23(a).
(2) ASTM D 1193-77, Standard Specification for Reagent Water, IBR
approved for Method 101, par. 6.1.1; Method 101A, par. 6.1.1; Method
104, par. 3.1.2.
(3) ASTM D 2986-71 (Reapproved 1978), Standard Method for Evaluation
of Air, Assay Media by the Monodisperse DOP (Dioctyl Phthalate) Smoke
Test, IBR approved for Method 103, par. 2.1.3; Method 104, par.
3.1.1.
(4) ASTM D2267-68 (reapproved 1978) Aromatics in Light Naphthas and
Aviation Gasoline by Gas Chromatography, IBR approved June 6, 1984, for
61.245(d)(1) and IBR approved September 30, 1986 for 61.67(h)(1).
(5) ASTM D 2382-76, Heat of Combustion of Hydrocarbon Fuels by Bomb
Calorimeter (High-Precision Method), IBR approved June 6, 1984, for
61.245(e)(3).
(6) ASTM D 2504-67 (Reapproved 1977), Noncondensable Gases in C3 and
Lighter Hydrocarbon Products by Gas Chromatography, IBR approved June 6,
1984, for 61.245(e)(3).
(7) ASTM D 836-84, Standard Specification for Industrial Grade
Benzene, IBR approved September 14, 1989 for 61.270(a).
(8) ASTM D 835-85, Standard Specification for Refined Benzene-485,
IBR approved September 14, 1989 for 61.270(a).
(9) ASTM D 2359-85a, Standard Specification for Refined Benzene-535,
IBR approved September 14, 1989 for 61.270(a).
(10) ASTM D 4734-87, Standard Specification for Refined Benzene-545,
IBR approved September 14, 1989 for 61.270(a).
(11) ASTM E 50-82 (reapproved 1986), Standard Practices for Apparatus
Reagents, and Safety Precautions for Chemical Analysis of Metals, IBR
approved for Method 108C, par. 2.1.4.
(b) The following material is available from the U.S. EPA
Environmental Monitoring and Support Laboratory, Cincinnati, Ohio 45268.
(1) Method 601, Test Method for Purgeable Halocarbons, July 1982, IBR
approved September 30, 1986 for 61.67(g)(2).
(c) The following material is available for purchase from the
American National Standards Institute, Inc., 1430 Broadway, New York, NY
10018.
(1) ANSI N13.1 -- 1969, ''Guide to Sampling Airborne Radioactive
Materials in Nuclear Facilities.'' IBR approved for 61.93(b)(2)(ii);
61.107(b)(2)(ii); and Method 114, par. 2.1 of Appendix B to part 61.
(d) The following material is available from the Superintendent of
Documents, U.S. Government Printing Office, Washington, DC 20402-9325,
telephone (202) 783-3238.
(1) Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods, EPA Publication SW-846, Third Edition, November 1986, as
amended by Revision I, December 1987, Order Number 955-001-00000-1:
(i) Method 8020, Aromatic Volatile Organics, IBR approved March 7,
1990, for 61.355(c)(2)(iv)(A).
(ii) Method 8021, Volatile Organic Compounds in Water by Purge and
Trap Capillary Column Gas Chromatography with Photoionization and
Electrolytic Conductivity Detectors in Series, IBR approved March 7,
1990, for 61.355(c)(2)(iv)(B).
(iii) Method 8240, Gas Chromatography/Mass Spectrometry for Volatile
Organics, IBR approved March 7, 1990, for 61.355(c)(2)(iv)(C).
(iv) Method 8260, Gas Chromatography/Mass Spectrometry for Volatile
Organics: Capillary Column Technique, IBR approved March 7, 1990, for
61.355(c)(2)(iv)(D).
(48 FR 3740, Jan. 27, 1983, as amended at 48 FR 55266, Dec. 9, 1983;
49 FR 23520, June 6, 1984; 51 FR 34914, Sept. 30, 1986; 54 FR 38073,
Sept. 14, 1989; 54 FR 51704, Dec. 15, 1989; 55 FR 8341, Mar. 7, 1990;
55 FR 18331, May 2, 1990; 55 FR 22027, May 31, 1990; 55 FR 32914,
Aug. 13, 1990)
40 CFR 61.19 Circumvention.
No owner or operator shall build, erect, install, or use any article
machine, equipment, process, or method, the use of which conceals an
emission which would otherwise constitute a violation of an applicable
standard. Such concealment includes, but is not limited to, the use of
gaseous dilutants to achieve compliance with a visible emissions
standard, and the piecemeal carrying out of an operation to avoid
coverage by a standard that applies only to operations larger than a
specified size.
(40 FR 48299, Oct. 14, 1975. Redesignated at 50 FR 46294, Nov. 7,
1985)
40 CFR 61.19 Subpart B -- National Emission Standards for Radon
Emissions From Underground Uranium Mines
Source: 54 FR 51694, Dec. 15, 1989, unless otherwise noted.
40 CFR 61.20 Designation of facilities.
The provisions of this subpart are applicable to the owner or
operator of an active underground uranium mine which:
(a) Has mined, will mine or is designed to mine over 100,000 tons of
ore during the life of the mine; or
(b) Has had or will have an annual ore production rate greater than
10,000 tons, unless it can be demonstrated to EPA that the mine will not
exceed total ore production of 100,000 tons during the life of the mine.
40 CFR 61.21 Definitions.
As used in this subpart, all terms not defined here have the meaning
given them in the Clean Air Act or subpart A of part 61. The following
terms shall have the following specific meanings:
(a) Active mine means an underground uranium mine which is being
ventilated to allow workers to enter the mine for any purpose.
(b) Effective dose equivalent means the sum of the products of
absorbed dose and appropriate factors to account for differences in
biological effectiveness due to the quality of radiation and its
distribution in the body of reference man. The unit of the effective
dose equivalent is the rem. The method for calculating effective dose
equivalent and the definition of reference man are outlined in the
International Commission on Radiological Protection's Publication No.
26.
(c) Underground uranium mine means a man-made underground excavation
made for the purpose of removing material containing uranium for the
principal purpose of recovering uranium.
40 CFR 61.22 Standard.
Emissions of radon-222 to the ambient air from an underground uranium
mine shall not exceed those amounts that would cause any member of the
public to receive in any year an effective dose equivalent of 10 mrem/y.
40 CFR 61.23 Determining compliance.
(a) Compliance with the emission standard in this subpart shall be
determined and the effective dose equivalent calculated by the EPA
computer code COMPLY-R. An underground uranium mine owner or operator
shall calculate the source terms to be used for input into COMPLY-R by
conducting testing in accordance with the procedures described in
Appendix B, Method 115, or
(b) Owners or operators may demonstrate compliance with the emission
standard in this subpart through the use of computer models that are
equivalent to COMPLY-R provided that the model has received prior
approval from EPA headquarters. EPA may approve a model in whole or in
part and may limit its use to specific circumstances.
40 CFR 61.24 Annual Reporting Requirements.
(a) The mine owner or operator shall annually calculate and report
the results of the compliance calculations in section 61.23 and the
input parameters used in making the calculation. Such report shall
cover the emissions of a calendar year and shall be sent to EPA by March
31 of the following year. Each report shall also include the following
information:
(1) The name and location of the mine.
(2) The name of the person responsible for the operation of the
facility and the name of the person preparing the report (if different).
(3) The results of the emissions testing conducted and the dose
calculated using the procedures in 61.23.
(4) A list of the stacks or vents or other points where radioactive
materials are released to the atmosphere, including their location,
diameter, flow rate, effluent temperature and release height.
(5) A description of the effluent controls that are used on each
stack, vent, or other release point and the effluent controls used
inside the mine, and an estimate of the efficiency of each control
method or device.
(6) Distances from the points of release to the nearest residence,
school, business or office and the nearest farms producing vegetables,
milk, and meat.
(7) The values used for all other user-supplied input parameters for
the computer models (e.g., meteorological data) and the source of these
data.
(8) Each report shall be signed and dated by a corporate officer in
charge of the facility and contain the following declaration immediately
above the signature line: ''I certify under penalty of law that I have
personally examined and am familiar with the information submitted
herein and based on my inquiry of those individuals immediately
responsible for obtaining the information, I believe that the submitted
information is true, accurate and complete. I am aware that there are
significant penalties for submitting false information including the
possibility of fine and imprisonment. See, 18 U.S.C. 1001.''
(b) lf the facility is not in compliance with the emission standard
of 61.22 in the calendar year covered by the report, the facility must
then commence reporting to the Administrator on a monthly basis the
information listed in paragraph (a) of this section for the preceding
month. These reports will start the month immediately following the
submittal of the annual report for the year in noncompliance and will be
due 30 days following the end of each month. This increased level of
reporting will continue until the Administrator has determined that the
monthly reports are no longer necessary. In addition to all the
information required in paragraph (a) of this section, monthly reports
shall also include the following information:
(1) All controls or other changes in operation of the facility that
will be or are being installed to bring the facility into compliance.
(2) If the facility is under a judicial or administrative enforcement
decree the report will describe the facilities performance under the
terms of the decree.
(c) The first report will cover the emissions of calendar year 1990.
(Approved by the Office of Management and Budget under control number
2060-0191)
40 CFR 61.25 Recordkeeping requirements.
The owner or operator of a mine must maintain records documenting the
source of input parameters including the results of all measurements
upon which they are based, the calculations and/or analytical methods
used to derive values for input parameters, and the procedure used to
determine compliance. In addition, the documentation should be
sufficient to allow an independent auditor to verify the accuracy of the
determination made concerning the facility's compliance with the
standard. These records must be kept at the mine or by the owner or
operator for at least five years and upon request be made available for
inspection by the Administrator, or his authorized representative.
40 CFR 61.26 Exemption from the reporting and testing requirements of
40 CFR 61.10.
All facilities designated under this subpart are exempt from the
reporting requirements of 40 CFR 61.10.
40 CFR 61.26 Subpart C -- National Emission Standard for Beryllium
40 CFR 61.30 Applicability.
The provisions of this subpart are applicable to the following
stationary sources:
(a) Extraction plans, ceramic plants, foundries, incinerators, and
propellant plants which process beryllium ore, beryllium, beryllium
oxide, beryllium alloys, or beryllium-containing waste.
(b) Machine shops which process beryllium, beryllium oxides, or any
alloy when such alloy contains more than 5 percent beryllium by weight.
40 CFR 61.31 Definitions.
Terms used in this subpart are defined in the act, in subpart A of
this part, or in this section as follows:
(a) Beryllium means the element beryllium. Where weights or
concentrations are specified, such weights or concentrations apply to
beryllium only, excluding the weight or concentration of any associated
elements.
(b) Extraction plant means a facility chemically processing beryllium
ore to beryllium metal, alloy, or oxide, or performing any of the
intermediate steps in these processes.
(c) Beryllium ore means any naturally occurring material mined or
gathered for its beryllium content.
(d) Machine shop means a facility performing cutting, grinding,
turning, honing, milling, deburring, lapping, electrochemical machining,
etching, or other similar operations.
(e) Ceramic plant means a manufacturing plant producing ceramic
items.
(f) Foundry means a facility engaged in the melting or casting of
beryllium metal or alloy.
(g) Beryllium-containing waste means material contaminated with
beryllium and/or beryllium compounds used or generated during any
process or operation performed by a source subject to this subpart.
(h) Incinerator means any furnace used in the process of burning
waste for the primary purpose of reducing the volume of the waste by
removing combustible matter.
(i) Propellant means a fuel and oxidizer physically or chemically
combined which undergoes combustion to provide rocket propulsion.
(j) Beryllium alloy means any metal to which beryllium has been added
in order to increase its beryllium content and which contains more than
0.1 percent beryllium by weight.
(k) Propellant plant means any facility engaged in the mixing,
casting, or machining of propellant.
40 CFR 61.32 Emission standard.
(a) Emissions to the atmosphere from stationary sources subject to
the provisions of this subpart shall not exceed 10 grams of beryllium
over a 24-hour period, except as provided in paragraph (b) of this
section.
(b) Rather than meet the requirement of paragraph (a) of this
section, an owner or operator may request approval from the
Administrator to meet an ambient concentration limit on beryllium in the
vicinity of the stationary source of 0.01 g/m3, averaged over a 30-day
period.
(1) Approval of such requests may be granted by the Administrator
provided that:
(i) At least 3 years of data is available which in the judgment of
the Administrator demonstrates that the future ambient concentrations of
beryllium in the vicinity of the stationary source will not exceed 0.01
g/m3, averaged over a 30-day period. Such 3-year period shall be the 3
years ending 30 days before the effective date of this standard.
(ii) The owner or operator requests such approval in writing within
30 days after the effective date of this standard.
(iii) The owner or operator submits a report to the Administrator
within 45 days after the effective date of this standard which report
includes the following information:
(a) Description of sampling method including the method and frequency
of calibration.
(b) Method of sample analysis.
(c) Averaging technique for determining 30-day average
concentrations.
(d) Number, identity, and location (address, coordinates, or distance
and heading from plant) of sampling sites.
(e) Ground elevations and height above ground of sampling inlets.
(f) Plant and sampling area plots showing emission points and
sampling sites. Topographic features significantly affecting dispersion
including plant building heights and locations shall be included.
(g) Information necessary for estimating dispersion including stack
height, inside diameter, exit gas temperature, exit velocity or flow
rate, and beryllium concentration.
(h) A description of data and procedures (methods or models) used to
design the air sampling network (i.e., number and location of sampling
sites).
(i) Air sampling data indicating beryllium concentrations in the
vicinity of the stationary source for the 3-year period specified in
paragraph (b)(1) of this section. This data shall be presented
chronologically and include the beryllium concentration and location of
each individual sample taken by the network and the corresponding 30-day
average beryllium concentrations.
(2) Within 60 days after receiving such report, the Administrator
will notify the owner or operator in writing whether approval is granted
or denied. Prior to denying approval to comply with the provisions of
paragraph (b) of this section, the Administrator will consult with
representatives of the statutory source for which the demonstration
report was submitted.
(c) The burning of beryllium and/or beryllium-containing waste,
except propellants, is prohibited except in incinerators, emissions from
which must comply with the standard.
40 CFR 61.33 Stack sampling.
(a) Unless a waiver of emission testing is obtained under 61.13,
each owner or operator required to comply with 61.32(a) shall test
emissions from the source according to Method 104 of appendix B to this
part. Method 103 of appendix B to this part is approved by the
Administrator as an alternative method for sources subject to 61.32(a).
The emission test shall be performed --
(1) Within 90 days of the effective date in the case of an existing
source or a new source which has an initial startup date preceding the
effective date; or
(2) Within 90 days of startup in the case of a new source which did
not have an initial startup date preceding the effective date.
(b) The Administrator shall be notified at least 30 days prior to an
emission test so that he may at his option observe the test.
(c) Samples shall be taken over such a period or periods as are
necessary to accurately determine the maximum emissions which will occur
in any 24-hour period. Where emissions depend upon the relative
frequency of operation of different types of processes, operating hours,
operating capacities, or other factors, the calculation of maximum
24-hour-period emissions will be based on that combination of factors
which is likely to occur during the subject period and which result in
the maximum emissions. No changes in the operation shall be made, which
would potentially increase emissions above that determined by the most
recent source test, until a new emission level has been estimated by
calculation and the results reported to the Administrator.
(d) All samples shall be analyzed and beryllium emissions shall be
determined within 30 days after the source test. All determinations
shall be reported to the Administrator by a registered letter dispatched
before the close of the next business day following such determination.
(e) Records of emission test results and other data needed to
determine total emissions shall be retained at the source and made
available, for inspection by the Administrator, for a minimum of 2
years.
(38 FR 8826, Apr. 6, 1973, as amended at 50 FR 46294, Nov. 7, 1985)
40 CFR 61.34 Air sampling.
(a) Stationary sources subject to 61.32(b) shall locate air sampling
sites in accordance with a plan approved by the Administrator. Such
sites shall be located in such a manner as is calculated to detect
maximum concentrations of beryllium in the ambient air.
(b) All monitoring sites shall be operated continuously except for a
reasonable time allowance for instrument maintenance and calibration,
for changing filters, or for replacement of equipment needing major
repair.
(c) Filters shall be analyzed and concentrations calculated within 30
days after filters are collected. Records of concentrations at all
sampling sites and other data needed to determine such concentrations
shall be retained at the source and made available, for inspection by
the Administrator, for a minimum of 2 years.
(d) Concentrations measured at all sampling sites shall be reported
to the Administrator every 30 days by a registered letter.
(e) The Administrator may at any time require changes in, or
expansion of, the sampling network.
40 CFR 61.34 Subpart D -- National Emission Standard for Beryllium Rocket Motor Firing
40 CFR 61.40 Applicability.
The provisions of this subpart are applicable to rocket motor test
sites.
40 CFR 61.41 Definitions.
Terms used in this subpart are defined in the Act, in subpart A of
this part, or in this section as follows:
(a) Rocket motor test site means any building, structure, facility,
or installation where the static test firing of a beryllium rocket motor
and/or the disposal of beryllium propellant is conducted.
(b) Beryllium propellant means any propellant incorporating
beryllium.
40 CFR 61.42 Emission standard.
(a) Emissions to the atmosphere from rocket-motor test sites shall
not cause time-weighted atmospheric concentrations of beryllium to
exceed 75 microgram minutes per cubic meter of air within the limits of
10 to 60 minutes, accumulated during any 2 consecutive weeks, in any
area in which an effect adverse to public health could occur.
(b) If combustion products from the firing of beryllium propellant
are collected in a closed tank, emissions from such tank shall not
exceed 2 grams per hour and a maximum of 10 grams per day.
40 CFR 61.43 Emission testing -- rocket firing or propellant disposal.
(a) Ambient air concentrations shall be measured during and after
firing of a rocket motor or propellant disposal and in such a manner
that the effect of these emissions can be compared with the standard.
Such sampling techniques shall be approved by the Administrator.
(b) All samples shall be analyzed and results shall be calculated
within 30 days after samples are taken and before any subsequent rocket
motor firing or propellant disposal at the given site. All results
shall be reported to the Administrator by a registered letter dispatched
before the close of the next business day following determination of
such results.
(c) Records of air sampling test results and other data needed to
determine integrated intermittent concentrations shall be retained at
the source and made available, for inspection by the Administrator, for
a minimum of 2 years.
(d) The Administrator shall be notified at least 30 days prior to an
air sampling test, so that he may at his option observe the test.
40 CFR 61.44 Stack sampling.
(a) Sources subject to 61.42(b) shall be continuously sampled,
during release of combustion products from the tank, according to Method
104 of appendix B to this part. Method 103 of appendix B to this part
is approved by the Administrator as an alternative method for sources
subject to 61.42(b).
(b) All samples shall be analyzed, and beryllium emissions shall be
determined within 30 days after samples are taken and before any
subsequent rocket motor firing or propellant disposal at the given site.
All determinations shall be reported to the Administrator by a
registered letter dispatched before the close of the next business day
following such determinations.
(c) Records of emission test results and other data needed to
determine total emissions shall be retained at the source and made
available, for inspection by the Administrator, for a minimum of 2
years.
(d) The Administrator shall be notified at least 30 days prior to an
emission test, so that he may at his option observe the test.
(38 FR 8826, Apr. 6, 1973, as amended at 50 FR 46294, Nov. 7, 1985)
40 CFR 61.44 Subpart E -- National Emission Standard for Mercury
40 CFR 61.50 Applicability.
The provisions of this subpart are applicable to those stationary
sources which process mercury ore to recover mercury, use mercury
chlor-alkali cells to produce chlorine gas and alkali metal hydroxide,
and incinerate or dry wastewater treatment plant sludge.
(40 FR 48302, Oct. 14, 1975)
40 CFR 61.51 Definitions.
Terms used in this subpart are defined in the act, in subpart A of
this part, or in this section as follows:
(a) Mercury means the element mercury, excluding any associated
elements, and includes mercury in particulates, vapors, aerosols, and
compounds.
(b) Mercury ore means a mineral mined specifically for its mercury
content.
(c) Mercury ore processing facility means a facility processing
mercury ore to obtain mercury.
(d) Condenser stack gases mean the gaseous effluent evolved from the
stack of processes utilizing heat to extract mercury metal from mercury
ore.
(e) Mercury chlor-alkali cell means a device which is basically
composed of an electrolyzer section and a denuder (decomposer) section
and utilizes mercury to produce chlorine gas, hydrogen gas, and alkali
metal hydroxide.
(f) Mercury chlor-alkali electrolyzer means an electrolytic device
which is part of a mercury chlor-alkali cell and utilizes a flowing
mercury cathode to produce chlorine gas and alkali metal amalgam.
(g) Denuder means a horizontal or vertical container which is part of
a mercury chlor-alkali cell and in which water and alkali metal amalgam
are converted to alkali metal hydroxide, mercury, and hydrogen gas in a
short-circuited, electrolytic reaction.
(h) Hydrogen gas stream means a hydrogen stream formed in the
chlor-alkali cell denuder.
(i) End box means a container(s) located on one or both ends of a
mercury chlor-alkali electrolyzer which serves as a connection between
the electrolyzer and denuder for rich and stripped amalgam.
(j) End box ventilation system means a ventilation system which
collects mercury emissions from the end-boxes, the mercury pump sumps,
and their water collection systems.
(k) Cell room means a structure(s) housing one or more mercury
electrolytic chlor-alkali cells.
(l) Sludge means sludge produced by a treatment plant that processes
municipal or industrial waste waters.
(m) Sludge dryer means a device used to reduce the moisture content
of sludge by heating to temperatures above 65 C (ca. 150 F) directly
with combustion gases.
(38 FR 8826, Apr. 6, 1973, as amended at 40 FR 48302, Oct. 14, 1975)
40 CFR 61.52 Emission standard.
(a) Emissions to the atmosphere from mercury ore processing
facilities and mercury cell chlor-alkali plants shall not exceed 2300
grams of mercury per 24-hour period.
(b) Emissions to the atmosphere from sludge incineration plants,
sludge drying plants, or a combination of these that process wastewater
treatment plant sludges shall not exceed 3200 grams of mercury per
24-hour period.
(40 FR 48302, Oct. 14, 1975)
40 CFR 61.53 Stack sampling.
(a) Mercury ore processing facility. (1) Unless a waiver of emission
testing is obtained under 61.13, each owner or operator processing
mercury ore shall test emissions from the source according to Method 101
of appendix B to this part. The emission test shall be performed --
(i) Within 90 days of the effective date in the case of an existing
source or a new source which has an initial start-up date preceding the
effective date; or
(ii) Within 90 days of startup in the case of a new source which did
not have an initial startup date preceding the effective date.
(2) The Administrator shall be notified at least 30 days prior to an
emission test, so that he may at his option observe the test.
(3) Samples shall be taken over such a period or periods as are
necessary to accurately determine the maximum emissions which will occur
in a 24-hour period. No changes in the operation shall be made, which
would potentially increase emissions above that determined by the most
recent source test, until the new emission level has been estimated by
calculation and the results reported to the Administrator.
(4) All samples shall be analyzed and mercury emissions shall be
determined within 30 days after the stack test. Each determination
shall be reported to the Administrator by a registered letter dispatched
within 15 calendar days following the date such determination is
completed.
(5) Records of emission test results and other data needed to
determine total emissions shall be retained at the source and made
available, for inspection by the Administrator, for a minimum of 2
years.
(b) Mercury chlor-alkali plant -- hydrogen and end-box ventilation
gas streams. (1) Unless a waiver of emission testing is obtained under
61.13, each owner or operator employing mercury chlor-alkali cell(s)
shall test emissions from hydrogen streams according to Method 102 and
from end-box ventilation gas streams according to Method 101 of appendix
B to this part. The emission test shall be performed --
(i) Within 90 days of the effective date in the case of an existing
source or a new source which has an initial startup date preceding the
effective date; or
(ii) Within 90 days of startup in the case of a new source which did
not have an initial startup date preceding the effective date.
(2) The Administrator shall be notified at least 30 days prior to an
emission test, so that he may at his option observe the test.
(3) Samples shall be taken over such a period or periods as are
necessary to accurately determine the maximum emissions which will occur
in a 24-hour period. No changes in the operation shall be made, which
would potentially increase emissions above that determined by the most
recent source test, until the new emission has been estimated by
calculation and the results reported to the Administrator.
(4) All samples shall be analyzed and mercury emissions shall be
determined within 30 days after the stack test. Each determination
shall be reported to the Administrator by a registered letter dispatched
within 15 calendar days following the date such determination is
completed.
(5) Records of emission test results and other data needed to
determine total emissions shall be retained at the source and made
available, for inspection by the Administrator, for a minimum of 2
years.
(c) Mercury chlor-alkali plants -- cell room ventilation system. (1)
Stationary sources using mercury chlor-alkali cells may test cell room
emissions in accordance with paragraph (c)(2) of this section or
demonstrate compliance with paragraph (c)(4) of this section and assume
ventilation emissions of 1,300 gms/day of mercury.
(2) Unless a waiver of emission testing is obtained under 61.13,
each owner or operator shall pass all cell room air in force gas streams
through stacks suitable for testing and shall test emissions from the
source according to Method 101 in appendix B to this part. The emission
test shall be performed --
(i) Within 90 days of the effective date in the case of an existing
source or a new source which has an initial startup date preceding the
effective date; or
(ii) Within 90 days of startup in the case of a new source which did
not have an initial startup date preceding the effective date.
(3) The Administrator shall be notified at least 30 days prior to an
emission test, so that he may at his option observe the test.
(4) An owner or operator may carry out approved design, maintenance,
and housekeeping practices. A list of approved practices is provided in
appendix A of ''Review of National Emission Standards for Mercury,''
EPA-450/3-84-014a, December 1984. Copies are available from EPA's
Central Docket Section, Docket item number A-84-41, III-B-1.
(d) Sludge incineration and drying plants. (1) Unless a waiver of
emission testing is obtained under 61.13, each owner or operator of a
source subject to the standard in 61.52(b) shall test emissions from
that source. Such tests shall be conducted in accordance with the
procedures set forth either in paragraph (d) of this section or in
61.54.
(2) Method 101A in appendix B to this part shall be used to test
emissions as follows:
(i) The test shall be performed within 90 days of the effective date
of these regulations in the case of an existing source or a new source
which has an initial startup date preceding the effective date.
(ii) The test shall be performed within 90 days of startup in the
case of a new source which did not have an initial startup date
preceding the effective date.
(3) The Administrator shall be notified at least 30 days prior to an
emission test, so that he may at his option observe the test.
(4) Samples shall be taken over such a period or periods as are
necessary to determine accurately the maximum emissions which will occur
in a 24-hour period. No changes shall be made in the operation which
would potentially increase emissions above the level determined by the
most recent stack test, until the new emission level has been estimated
by calculation and the results reported to the Administrator.
(5) All samples shall be analyzed and mercury emissions shall be
determined within 30 days after the stack test. Each determination
shall be reported to the Administrator by a registered letter dispatched
within 15 calendar days following the date such determination is
completed.
(6) Records of emission test results and other data needed to
determine total emissions shall be retained at the source and shall be
made available, for inspection by the Administrator, for a minimum of 2
years.
(38 FR 8826, Apr. 6, 1973, as amended at 40 FR 48302, Oct. 14, 1975;
47 FR 24704, June 8, 1982; 50 FR 46294, Nov. 7, 1985; 52 FR 8726, Mar.
19, 1987)
40 CFR 61.54 Sludge sampling.
(a) As an alternative means for demonstrating compliance with
61.52(b), an owner or operator may use Method 105 of appendix B and the
procedures specified in this section.
(1) A sludge test shall be conducted within 90 days of the effective
date of these regulations in the case of an existing source or a new
source which has an initial startup date preceding the effective date;
or
(2) A sludge test shall be conducted within 90 days of startup in the
case of a new source which did not have an initial startup date
preceding the effective date.
(b) The Administrator shall be notified at least 30 days prior to a
sludge sampling test, so that he may at his option observe the test.
(c) Sludge shall be sampled according to paragraph (c)(1) of this
section, sludge charging rate for the plant shall be determined
according to paragraph (c)(2) of this section, and the sludge analysis
shall be performed according to paragraph (c)(3) of this section.
(1) The sludge shall be sampled according to Method 105 --
Determination of Mercury in Wastewater Treatment Plant Sewage Sludges.
A total of three composite samples shall be obtained within an operating
period of 24 hours. When the 24-hour operating period is not
continuous, the total sampling period shall not exceed 72 hours after
the first grab sample is obtained. Samples shall not be exposed to any
condition that may result in mercury contamination or loss.
(2) The maximum 24-hour period sludge incineration or drying rate
shall be determined by use of a flow rate measurement device that can
measure the mass rate of sludge charged to the incinerator or dryer with
an accuracy of 5 percent over its operating range. Other methods of
measuring sludge mass charging rates may be used if they have received
prior approval by the Administrator.
(3) The sampling, handling, preparation, and analysis of sludge
samples shall be accomplished according to Method 105 in appendix B of
this part.
(d) The mercury emissions shall be determined by use of the following
equation.
where:
EHg=Mercury emissions, g/day.
M=Mercury concentration of sludge on a dry solids basis, g/g.
Q=Sludge changing rate, kg/day.
Fsm=Weight fraction of solids in the collected sludge after mixing.
1000=Conversion factor, kg g/g /2/ .
(e) No changes in the operation of a plant shall be made after a
sludge test has been conducted which would potentially increase
emissions above the level determined by the most recent sludge test,
until the new emission level has been estimated by calculation and the
results reported to the Administrator.
(f) All sludge samples shall be analyzed for mercury content within
30 days after the sludge sample is collected. Each determination shall
be reported to the Administrator by a registered letter dispatched
within 15 calendar days following the date such determination is
completed.
(g) Records of sludge sampling, charging rate determination and other
data needed to determine mercury content of wastewater treatment plant
sludges shall be retained at the source and made available, for
inspection by the Administrator, for a minimum of 2 years.
(40 FR 48303, Oct. 14, 1975, as amended at 49 FR 35770, Sept. 12,
1984; 52 FR 8727, Mar. 19, 1987; 53 FR 36972, Sept. 23, 1988)
40 CFR 61.55 Monitoring of emissions and operations.
(a) Wastewater treatment plant sludge incineration and drying plants.
All the sources for which mercury emissions exceed 1,600 g per 24-hour
period, demonstrated either by stack sampling according to 61.53 or
sludge sampling according to 61.54, shall monitor mercury emissions at
intervals of at least once per year by use of Method 105 of appendix B
or the procedures specified in 61.53 (d) (2) and (4). The results of
monitoring shall be reported and retained according to 61.53(d) (5) and
(6) or 61.54 (f) and (g).
(b) Mercury cell chlor-alkali plants -- hydrogen and end-box
ventilation gas streams.
(1) The owner or operator of each mercury cell chlor-alkali plant
shall, within 1 year of the date of publication of these amendments or
within 1 year of startup for a plant with initial startup after the date
of publication, perform a mercury emission test that demonstrates
compliance with the emission limits in 61.52, on the hydrogen stream by
Reference Method 102 and on the end-box stream by Reference Method 101
for the purpose of establishing limits for parameters to be monitored.
(2) During tests specified in paragraph (b)(1) of this section, the
following control device parameters shall be monitored, except as
provided in paragraph (c) of this section, and recorded manually or
automatically at least once every 15 minutes:
(i) The exit gas temperature from uncontrolled streams;
(ii) The outlet temperature of the gas stream for the final (i.e.,
the farthest downstream) cooling system when no control devices other
than coolers and demisters are used;
(iii) The outlet temperature of the gas stream from the final cooling
system when the cooling system is followed by a molecular sieve or
carbon adsorber;
(iv) Outlet concentration of available chlorine, pH, liquid flow
rate, and inlet gas temperature of chlorinated brine scrubbers and
hypochlorite scrubbers;
(v) The liquid flow rate and exit gas temperature for water
scrubbers;
(vi) The inlet gas temperature of carbon adsorption systems; and
(vii) The temperature during the heating phase of the regeneration
cycle for carbon adsorbers or molecular sieves.
(3) The recorded parameters in paragraphs (b)(2)(i) through
(b)(2)(vi) of this section shall be averaged over the test period (a
minimum of 6 hours) to provide an average number. The highest
temperature reading that is measured in paragraph (b)(2)(vii) of this
section is to be identified as the reference temperature for use in
paragraph (b)(6)(ii) of this section.
(4)(i) Immediately following completion of the emission tests
specified in paragraph (b)(1) of this section, the owner or operator of
a mercury cell chlor-alkali plant shall monitor and record manually or
automatically at least once per hour the same parameters specified in
paragraphs (b)(2)(i) through (b)(2)(vi) of this section.
(ii) Immediately following completion of the emission tests specified
in paragraph (b)(1) of this section, the owner or operator shall monitor
and record manually or automatically, during each heating phase of the
regeneration cycle, the temperature specified in paragraph (b)(2)(vii)
of this section.
(5) Monitoring devices used in accordance with paragraphs (b)(2) and
(b)(4) of this section shall be certified by their manufacturer to be
accurate to within 10 percent, and shall be operated, maintained, and
calibrated according to the manufacturer's instructions. Records of the
certifications and calibrations shall be retained at the chlor-alkali
plant and made available for inspection by the Administrator as follows:
Certification, for as long as the device is used for this purpose;
calibration for a minimum of 2 years.
(6)(i) When the hourly value of a parameter monitored in accordance
with paragraph (b)(4)(i) of this section exceeds, or in the case of
liquid flow rate and available chlorine falls below the value of that
same parameter determined in paragraph (b)(2) of this section for 24
consecutive hours, the Administrator is to be notified within the next
10 days.
(ii) When the maximum hourly value of the temperature measured in
accordance with paragraph (b)(4)(ii) of this section is below the
reference temperature recorded according to paragraph (b)(3) of this
section for three consecutive regeneration cycles, the Administrator is
to be notified within the next 10 days.
(7) Semiannual reports shall be submitted to the Administrator
indicating the time and date on which the hourly value of each parameter
monitored according to paragraphs (b)(4)(i) and (b)(4)(ii) of this
section fell outside the value of that same parameter determined under
paragraph (b)(3) of this section; and corrective action taken, and the
time and date of the corrective action. Parameter excursions will be
considered unacceptable operation and maintenance of the emission
control system. In addition, while compliance with the emission limits
is determined primarily by conducting a performance test according to
the procedures in 61.53(b), reports of parameter excursions may be used
as evidence in judging the duration of a violation that is determined by
a performance test.
(8) Semiannual reports required in paragraph (b)(7) of this section
shall be submitted to the Administrator on September 15 and March 15 of
each year. The first semiannual report is to be submitted following the
first full 6 month reporting period. The semiannual report due on
September 15 (March 15) shall include all excursions monitored through
August 31 (February 28) of the same calendar year.
(c) As an alternative to the monitoring, recordkeeping, and reporting
requirements in paragraphs (b)(2) through (8) of this section, an owner
or operator may develop and submit for the Administrator's review and
approval a plant-specific monitoring plan. To be approved, such a plan
must ensure not only compliance with the emission limits of 61.52(a)
but also proper operation and maintenance of emissions control systems.
Any site-specific monitoring plan submitted must, at a minimum, include
the following:
(1) Identification of the critical parameter or parameters for the
hydrogen stream and for the end-box ventilation stream that are to be
monitored and an explanation of why the critical parameter(s) selected
is the best indicator of proper control system performance and of
mercury emission rates.
(2) Identification of the maximum or minimum value of each parameter
(e.g., degrees temperature, concentration of mercury) that is not to be
exceeded. The level(s) is to be directly correlated to the results of a
performance test, conducted no more than 180 days prior to submittal of
the plan, when the facility was in compliance with the emission limits
of 61.52(a).
(3) Designation of the frequency for recording the parameter
measurements, with justification if the frequency is less than hourly.
A longer recording frequency must be justified on the basis of the
amount of time that could elapse during periods of process or control
system upsets before the emission limits would be exceeded, and
consideration is to be given to the time that would be necessary to
repair the failure.
(4) Designation of the immediate actions to be taken in the event of
an excursion beyond the value of the parameter established in 2.
(5) Provisions for reporting, semiannually, parameter excursions and
the corrective actions taken, and provisions for reporting within 10
days any significant excursion.
(6) Identification of the accuracy of the monitoring device(s) or of
the readings obtained.
(7) Recordkeeping requirements for certifications and calibrations.
(d) Mercury cell chlor-alkali plants -- cell room ventilation system.
(1) Stationary sources determining cell room emissions in accordance
with 61.53(c)(4) shall maintain daily records of all leaks or spills of
mercury. The records shall indicate the amount, location, time, and
date the leaks or spills occurred, identify the cause of the leak or
spill, state the immediate steps taken to minimize mercury emissions and
steps taken to prevent future occurrences, and provide the time and date
on which corrective steps were taken.
(2) The results of monitoring shall be recorded, retained at the
source, and made available for inspection by the Administrator for a
minimum of 2 years.
(Approved by the Office of Management and Budget under control number
2060-0097)
(52 FR 8727, Mar. 19, 1987)
40 CFR 61.56 Delegation of authority.
(a) In delegating implementation and enforcement authority to a State
under section 112(d) of the Act, the authorities contained in paragraph
(b) of this section shall be retained by the Administrator and not
transferred to a State.
(b) Authorities which will not be delegated to States: Sections
61.53(c)(4) and 61.55(d). The authorities not delegated to States listed
are in addition to the authorities in the General Provisions, subpart A
of 40 CFR part 61, that will not be delegated to States ( 61.04(b),
61.12(d)(1), and 61.13(h)(1)(ii)).
(52 FR 8728, Mar. 19, 1987)
40 CFR 61.56 Subpart F -- National Emission Standard for Vinyl Chloride
Source: 41 FR 46564, Oct. 21, 1976, unless otherwise noted.
40 CFR 61.60 Applicability.
(a) This subpart applies to plants which produce:
(1) Ethylene dichloride by reaction of oxygen and hydrogen chloride
with ethylene,
(2) Vinyl chloride by any process, and/or
(3) One or more polymers containing any fraction of polymerized vinyl
chloride.
(b) This subpart does not apply to equipment used in research and
development if the reactor used to polymerize the vinyl chloride
processed in the equipment has a capacity of no more than 0.19 m3 (50
gal).
(c) Sections of this subpart other than 61.61; 61.64 (a)(1), (b),
(c), and (d); 61.67; 61.68; 61.69; 61.70; and 61.71 do not apply to
equipment used in research and development if the reactor used to
polymerize the vinyl chloride processed in the equipment has a capacity
of greater than 0.19 m3 (50 gal) and no more than 4.07 m3 (1075 gal).
(41 FR 46564, Oct. 21, 1976, as amended at 42 FR 29006, June 7, 1977;
53 FR 36972, Sept. 23, 1988)
40 CFR 61.61 Definitions.
Terms used in this subpart are defined in the Act, in subpart A of
this part, or in this section as follows:
(a) Ethylene dichloride plant includes any plant which produces
ethylene dichloride by reaction of oxygen and hydrogen chloride with
ethylene.
(b) Vinyl chloride plant includes any plant which produces vinyl
chloride by any process.
(c) Polyvinyl chloride plant includes any plant where vinyl chloride
alone or in combination with other materials is polymerized.
(d) Slip gauge means a gauge which has a probe that moves through the
gas/liquid interface in a storage or transfer vessel and indicates the
level of vinyl chloride in the vessel by the physical state of the
material the gauge discharges.
(e) Type of resin means the broad classification of resin referring
to the basic manufacturing process for producing that resin, including,
but not limited to, the suspension, dispersion, latex, bulk, and
solution processes.
(f) Grade of resin means the subdivision of resin classification
which describes it as a unique resin, i.e., the most exact description
of a resin with no further subdivision.
(g) Dispersion resin means a resin manufactured in such a way as to
form fluid dispersions when dispersed in a plasticizer or
plasticizer/diluent mixtures.
(h) Latex resin means a resin which is produced by a polymerization
process which initiates from free radical catalyst sites and is sold
undried.
(i) Bulk resin means a resin which is produced by a polymerization
process in which no water is used.
(j) Inprocess wastewater means any water which, during manufacturing
or processing, comes into direct contact with vinyl chloride or
polyvinyl chloride or results from the production or use of any raw
material, intermediate product, finished product, by-product, or waste
product containing vinyl chloride or polyvinyl chloride but which has
not been discharged to a wastewater treatment process or discharged
untreated as wastewater. Gasholder seal water is not inprocess
wastewater until it is removed from the gasholder.
(k) Wastewater treatment process includes any process which modifies
characteristics such as BOD, COD, TSS, and pH, usually for the purpose
of meeting effluent guidelines and standards; it does not include any
process the purpose of which is to remove vinyl chloride from water to
meet requirements of this subpart.
(l) In vinyl chloride service means that a piece of equipment either
contains or contacts a liquid that is a least 10 percent vinyl chloride
by weight or a gas that is at least 10 percent by volume vinyl chloride
as determined according to the provisions of 61.67(h). The provisions
of 61.67(h) also specify how to determine that a piece of equipment is
not in vinyl chloride service. For the purposes of this subpart, this
definition must be used in place of the definition of ''in VHAP
service'' in subpart V of this part.
(m) Standard operating procedure means a formal written procedure
officially adopted by the plant owner or operator and available on a
routine basis to those persons responsible for carrying out the
procedure.
(n) Run means the net period of time during which an emission sample
is collected.
(o) Ethylene dichloride purification includes any part of the process
of ethylene dichloride purification following ethylene dichloride
formation, but excludes crude, intermediate, and final ethylene
dichloride storage tanks.
(p) Vinyl chloride purification incudes any part of the process of
vinyl chloride production which follows vinyl chloride formation.
(q) Reactor includes any vessel in which vinyl chloride is partially
or totally polymerized into polyvinyl chloride.
(r) Reactor opening loss means the emissions of vinyl chloride
occurring when a reactor is vented to the atmosphere for any purpose
other than an emergency relief discharge as defined in 61.65(a).
(s) Stripper includes any vessel in which residual vinyl chloride is
removed from polyvinyl chloride resin, except bulk resin, in the slurry
form by the use of heat and/or vacuum. In the case of bulk resin,
stripper includes any vessel which is used to remove residual vinyl
chloride from polyvinyl chloride resin immediately following the
polymerization step in the plant process flow.
(t) Standard temperature means a temperature of 20 C (69 F).
(u) Standard pressure means a pressure of 760 mm of Hg (29.92 in. of
Hg).
(v) Relief valve means each pressure relief device including pressure
relief valves, rupture disks and other pressure relief systems used to
protect process components from overpressure conditions. ''Relief
valve'' does not include polymerization shortstop systems, referigerated
water systems or control valves or other devices used to control flow to
an incinerator or other air pollution control device.
(w) Leak means any of several events that indicate interruption of
confinement of vinyl chloride within process equipment. Leaks include
events regulated under subpart V of this part such as:
(1) An instrument reading of 10,000 ppm or greater measured according
to Method 21 (see appendix A of 40 CFR part 60);
(2) A sensor detection of failure of a seal system, failure of a
barrier fluid system, or both;
(3) Detectable emissions as indicated by an instrument reading of
greater than 500 ppm above background for equipment designated for no
detectable emissions measured according to Test Method 21 (see appendix
A of 40 CFR part 60); and
(4) In the case of pump seals regulated under 61.242-2, indications
of liquid dripping constituting a leak under 61.242-2.
Leaks also include events regulated under 61.65(b)(8)(i) for
detection of ambient concentrations in excess of background
concentrations. A relief valve discharge is not a leak.
(x) Exhaust gas means any offgas (the constituents of which may
consist of any fluids, either as a liquid and/or gas) discharged
directly or ultimately to the atmosphere that was initially contained in
or was in direct contact with the equipment for which gas limits are
prescribed in 61.62(a) and (b); 61.63(a); 61.64 (a)(1), (b), (c),
and (d); 61.65 (b)(1)(ii), (b)(2), (b)(3), (b)(5), (b)(6)(ii), (b)(7),
and (b)(9)(ii); and 61.65(d). A leak as defined in paragraph (w) of
this section is not an exhaust gas. Equipment which contains exhaust
gas is subject to 61.65(b)(8), whether or not that equipment contains
10 percent by volume vinyl chloride.
(y) Relief valve discharge means any nonleak discharge through a
relief valve.
(z) 3-hour period means any three consecutive 1-hour periods (each
commencing on the hour), provided that the number of 3-hour periods
during which the vinyl chloride concentration exceeds 10 ppm does not
exceed the number of 1-hour periods during which the vinyl chloride
concentration exceeds 10 ppm.
(41 FR 46564, Oct. 21, 1976, as amended at 42 FR 29006, June 7, 1977;
51 FR 34908, Sept. 30, 1986; 55 FR 28348, July 10, 1990)
40 CFR 61.62 Emission standard for ethylene dichloride plants.
(a) Ethylene dichloride purification. The concentration of vinyl
chloride in each exhaust gas stream from any equipment used in ethylene
dichloride purification is not to exceed 10 ppm (average for 3-hour
period), except as provided in 61.65(a). This requirement does not
preclude combining of exhaust gas streams provided the combined steam is
ducted through a control system from which the concentration of vinyl
chloride in the exhaust gases does not exceed 10 ppm, or equivalent as
provided in 61.66. This requirement does not apply to equipment that
has been opened, is out of operation, and met the requirement in
61.65(b)(6)(i) before being opened.
(b) Oxychlorination reactor. Except as provided in 61.65(a),
emissions of vinyl chloride to the atmosphere from each oxychlorination
reactor are not to exceed 0.2 g/kg (0.0002 lb/lb) (average for 3-hour
period) of the 100 percent ethylene dichloride product from the
oxychlorination process.
(51 FR 34909, Sept. 30, 1986)
40 CFR 61.63 Emission standard for vinyl chloride plants.
An owner or operator of a vinyl chloride plant shall comply with the
requirements of this section and 61.65.
(a) Vinyl chloride formation and purification: The concentration of
vinyl chloride in each exhaust gas stream from any equipment used in
vinyl chloride formation and/or purification is not to exceed 10 ppm
(average for 3-hour period), except as provided in 61.65(a). This
requirement does not preclude combining of exhaust gas streams provided
the combined steam is ducted through a control system from which the
concentration of vinyl chloride in the exhaust gases does not exceed 10
ppm, or equivalent as provided in 61.66. This requirement does not
apply to equipment that has been opened, is out of operation, and met
the requirement in 61.65(b)(6)(i) before being opened.
(51 FR 34909, Sept. 30, 1986)
40 CFR 61.64 Emission standard for polyvinyl chloride plants.
An owner or operator of a polyvinyl chloride plant shall comply with
the requirements of this section and 61.65.
(a) Reactor. The following requirements apply to reactors:
(1) The concentration of vinyl chloride in each exhaust gas stream
from each reactor is not to exceed 10 ppm (average for 3-hour period),
except as provided in paragraph (a)(2) of this section and 61.65(a).
(2) The reactor opening loss from each reactor is not to exceed 0.02
g vinyl chloride/kg (0.00002 lb vinyl chloride/lb) of polyvinyl chloride
product, except as provided in paragraph (f)(1) of this section, with
the product determined on a dry solids basis. This requirement does not
apply to prepolymerization reactors in the bulk process. This
requirement does apply to postpolymerization reactors in the bulk
process, where the product means the gross product of prepolymerization
and postpolymerization.
(3) Manual vent valve discharge. Except for an emergency manual vent
valve discharge, there is to be no discharge to the atmosphere from any
manual vent valve on a polyvinyl chloride reactor in vinyl chloride
service. An emergency manual vent valve discharge means a discharge to
the atmosphere which could not have been avoided by taking measures to
prevent the discharge. Within 10 days of any discharge to the
atmosphere from any manual vent valve, the owner or operator of the
source from which the discharge occurs shall submit to the Administrator
a report in writing containing information on the source, nature and
cause of the discharge, the date and time of the discharge, the
approximate total vinyl chloride loss during the discharge, the method
used for determining the vinyl chloride loss (the calculation of the
vinyl chloride loss), the action that was taken to prevent the
discharge, and measures adopted to prevent future discharges.
(b) Stripper. The concentration of vinly chloride in each exhaust
gas stream from each stripper is not to exceed 10 ppm (average for
3-hour period), except as provided in 61.65(a). This requirement does
not apply to equipment that has been opened, is out of operation, and
met the requiremention 61.65(b)(6)(i) before being opened.
(c) Mixing, weighing, and holding containers. The concentration of
vinyl chloride in each exhaust gas stream from each mixing, weighing, or
holding container in vinyl chloride service which precedes the stripper
(or the reactor if the plant has no stripper) in the plant process flow
is not to exceed 10 ppm (average for 3-hour period), except as provided
in 61.65(a). This requirement does not apply to equipment that has been
opened, is out of operation, and met the requirement in 61.65(b)(6)(i)
before being opened.
(d) Monomer recovery system. The concentration of vinyl chloride in
each exhaust gas stream from each monomer recovery system is not to
exceed 10 ppm (average for 3-hour period), except as provided in
61.65(a). This requirement does not apply to equipment that has been
opened, is out of operation, and met the requirement in 61.65(b)(6)(i)
before being opened.
(e) Sources following the stripper(s). The following requirements
apply to emissions of vinyl chloride to the atmosphere from the
combination of all sources following the stripper(s) (or the reactor(s)
if the plant has no stripper(s)) in the plant process flow including but
not limited to, centrifuges, concentrators, blend tanks, filters,
dryers, conveyor air discharges, baggers, storage containers, and
inprocess wastewater, except as provided in paragraph (f) of this
section:
(1) In polyvinyl chloride plants using stripping technology to
control vinyl chloride emissions, the weighted average residual vinyl
chloride concentration in all grades of polyvinyl chloride resin
processed through the stripping operation on each calendar day, measured
immediately after the stripping operation is completed, may not exceed:
(i) 2000 ppm for polyvinyl chloride dispersion resins, excluding
latex resins;
(ii) 400 ppm for all other polyvinyl chloride resins, including latex
resins, averaged separately for each type of resin; or
(2) In polyvinyl chloride plants controlling vinyl chloride emissions
with technology other than stripping or in addition to stripping,
emissions of vinyl chloride to the atmosphere may not exceed:
(i) 2 g/kg (0.002 lb/lb) product from the stripper(s) (or reactor(s)
if the plant has no stripper(s)) for dispersion polyvinyl chloride
resins, excluding latex resins, with the product determined on a dry
solids basis;
(ii) 0.4 g/kg (0.0004 lb/lb) product from the strippers (or
reactor(s) if the plant has no stripper(s)) for all other polyvinyl
chloride resins, including latex resins, with the product determined on
a dry solids basis.
(3) The provisions of this paragraph apply at all times including
when off-specification or other types of resins are made.
(f) Reactor used as stripper. When a nonbulk resin reactor is used
as a stripper this paragraph may be applied in lieu of 61.64 (a)(2) and
(e)(1):
(1) The weighted average emissions of vinyl chloride from reactor
opening loss and all sources following the reactor used as a stripper
from all grades of polyvinyl chloride resin stripped in the reactor on
each calendar day may not exceed:
(i) 2.02 g/kg (0.00202 lb/lb) of polyvinyl chloride product for
dispersion polyvinyl chloride resins, excluding latex resins, with the
product determined on a dry solids basis.
(ii) 0.42 g/kg (0.00042 lb/lb) of polyvinyl chloride product for all
other polyvinyl chloride resins, including latex resins, with the
product determined on a dry solids basis.
(41 FR 46564, Oct. 21, 1976, as amended at 51 FR 34909, Sept. 30,
1986; 53 FR 36972, Sept. 23, 1988)
40 CFR 61.65 Emission standard for ethylene dichloride, vinyl chloride
and polyvinyl chloride plants.
An owner or operator of an ethylene dichloride, vinyl chloride,
and/or polyvinyl chloride plant shall comply with the requirements of
this section.
(a) Relief valve discharge. Except for an emergency relief
discharge, and except as provided in 61.65(d), there is to be no
discharge to the atmosphere from any relief valve on any equipment in
vinyl chloride service. An emergency relief discharge means a discharge
which could not have been avoided by taking measures to prevent the
discharge. Within 10 days of any relief valve discharge, except for
those subject to 61.65(d), the owner or operator of the source from
which the relief valve discharge occurs shall submit to the
Administrator a report in writing containing information on the source,
nature and cause of the discharge, the date and time of the discharge,
the approximate total vinyl chloride loss during the discharge, the
method used for determining the vinyl chloride loss (the calculation of
the vinyl chloride loss), the action that was taken to prevent the
discharge, and measures adopted to prevent future discharges.
(b) Fugitive emission sources -- (1) Loading and unloading lines.
Vinyl chloride emissions from loading and unloading lines in vinyl
chloride service which are opened to the atmosphere after each loading
or unloading operation are to be minimized as follows:
(i) After each loading or unloading operation and before opening a
loading or unloading line to the atmosphere, the quantity of vinyl
chloride in all parts of each loading or unloading line that are to be
opened to the atmosphere is to be reduced so that the parts combined
contain no greater than 0.0038 m3(0.13 ft3) of vinyl chloride, at
standard temperature and pressure; and
(ii) Any vinyl chloride removed from a loading or unloading line in
accordance with paragraph (b)(1)(i) of this section is to be ducted
through a control system from which the concentration of vinyl chloride
in the exhaust gases does not exceed 10 ppm (average for 3-hour period),
or equivalent as provided in 61.66.
(2) Slip gauges. During loading or unloading operations, the vinyl
chloride emissions from each slip gauge in vinyl chloride service are to
be minimized by ducting any vinyl chloride discharged from the slip
gauge through a control system from which the concentration of vinyl
chloride in the exhaust gases does not exceed 10 ppm (average for 3-hour
period), or equivalent as provided in 61.66.
(3) Leakage from pump, compressor, and agitator seals:
(i) Rotating pumps. Vinyl chloride emissions from seals on all
rotating pumps in vinyl chloride service are to be minimized by
installing sealless pumps, pumps with double mechanical seals or
equivalent as provided in 61.66. If double mechanical seals are used,
vinyl chloride emissions from the seals are to be minimized by
maintaining the pressure between the two seals so that any leak that
occurs is into the pump; by ducting any vinyl chloride between the two
seals through a control system from which the concentration of vinyl
chloride in the exhaust gases does not exceed 10 ppm; or equivalent as
provided in 61.66. Compliance with the provisions of 40 CFR part 61
subpart V demonstrates compliance with the provisions of this paragraph.
(ii) Reciprocating pumps. Vinyl chloride emissions from seals on all
reciprocating pumps in vinyl chloride service are to be minimized by
installing double outboard seals, or equivalent as provided in 61.66.
If double outboard seals are used, vinyl chloride emissions from the
seals are to be minimized by maintaining the pressure between the two
seals so that any leak that occurs is into the pump; by ducting any
vinyl chloride between the two seals through a control system from which
the concentration of vinyl chloride in the exhaust gases does not exceed
10 ppm; or equivalent as provided in 61.66. Compliance with the
provisions of 40 CFR part 61 subpart V demonstrates compliance with the
provisions of this paragraph.
(iii) Rotating compressor. Vinyl chloride emissions from seals on
all rotating compressors in vinyl chloride service are to be minimized
by installing compressors with double mechanical seals, or equivalent as
provided in 61.66. If double mechanical seals are used, vinyl chloride
emissions from the seals are to be minimized by maintaining the pressure
between the two seals so that any leak that occurs is into the
compressor; by ducting any vinyl chloride between the two seals through
a control system from which the concentration of vinyl chloride in the
exhaust gases does not exceed 10 ppm; or equivalent as provided in
61.66. Compliance with the provisions of 40 CFR part 61 subpart V
demonstrates compliance with the provisions of this paragraph.
(iv) Reciprocating compressors. Vinyl chloride emissions from seals
on all reciprocating compressors in vinyl chloride service are to be
minimized by installing double outboard seals, or equivalent as provided
in 61.66. If double outboard seals are used, vinyl chloride emissions
from the seals are to be minimized by maintaining the pressure between
the two seals so that any leak that occurs is into the compressor; by
ducting any vinyl chloride between the two seals through a control
system from which concentration of vinyl chloride in the exhaust gases
does not exceed 10 ppm; or equivalent as provided in 61.66. Compliance
with the provisions of 40 CFR part 61 subpart V demonstrates compliance
with the provisions of this paragraph.
(v) Agitator. Vinyl chloride emissions from seals on all agitators
in vinyl chloride service are to be minimized by installing agitators
with double mechanical seals, or equivalent as provided in 61.66. If
double mechanical seals are used, vinyl chloride emissions from the
seals are to be minimized by maintaining the pressure between the two
seals so that any leak that occurs is into the agitated vessel; by
ducting any vinyl chloride between the two seals through a control
system from which the concentration of vinyl chloride in the exhaust
gases does not exceed 10 ppm; or equivalent as provided in 61.66.
(4) Leaks from relief valves. Vinyl chloride emissions due to leaks
from each relief valve on equipment in vinyl chloride service shall
comply with 61.242-4 of subpart V of this part.
(5) Manual venting of gases. Except as provided in 61.64(a)(3), all
gases which are manually vented from equipment in vinly chloride service
are to be ducted through a control system from which the concentration
of vinyl chloride in the exhaust gases does not exceed 10 ppm (average
for 3-hour period); or equivalent as provided in 61.66.
(6) Opening of equipment. Vinyl chloride emissions from opening of
equipment (excluding crude, intermediate, and final EDC storage tanks,
but including prepolymerization reactors used in the manufacture of bulk
resins and loading or unloading lines that are not opened to the
atmosphere after each loading or unloading operation) are to be
minimized follows:
(i) Before opening any equipment for any reason, the quantity of
vinyl chloride which is contained therein is to be reduced to an amount
which occupies a volume of no more than 2.0 percent of the equipment's
containment volume or 0.0950 cubic meters (25 gallons), whichever is
larger, at standard temperature and pressure.
(ii) Any vinyl chloride removed from the equipment in accordance with
paragraph (b)(6)(i) of this section is to be ducted through a control
system from which the concentration of vinyl chloride in the exhaust
gases does not exceed 10 ppm (average for 3-hour period); or equivalent
as provided in 61.66.
(7) Samples. Unused portions of samples containing at least 10
percent by weight vinyl chloride are to be returned to the process or
destroyed in a control device from which concentration of vinyl chloride
in the exhaust gas does not exceed 10 ppm (average for 3-hour period) or
equivalent as provided in 61.66. Sampling techniques are to be such
that sample containers in vinyl chloride service are purged into a
closed process system. Compliance with the provisions of 40 CFR part 61
subpart V demonstrates compliance with the provisions of this paragraph.
(8) Leak detection and elimination. Vinyl chloride emissions due to
leaks from equipment in vinyl chloride service are to be minimized as
follows:
(i) A reliable and accurate vinyl chloride monitoring system shall be
operated for detection of major leaks and identification of the general
area of the plant where a leak is located. A vinyl chloride monitoring
system means a device which obtains air samples from one or more points
on a continuous sequential basis and analyzes the samples with gas
chromatography or, if the owner or operator assumes that all
hydrocarbons measured are vinyl chloride, with infrared
spectrophotometry, flame ion detection, or an equivalent or alternative
method. The vinyl chloride monitoring system shall be operated
according to a program developed by the plant owner or operator. The
owner or operator shall submit a description of the program to the
Administrator within 45 days of the effective date of these regulations,
unless a waiver of compliance is granted under 61.11, or the program
has been approved and the Administrator does not request a review of the
program. Approval of a program will be granted by the Administrator
provided he finds:
(A) The location and number of points to be monitored and the
frequency of monitoring provided for in the program are acceptable when
they are compared with the number of pieces of equipment in vinyl
chloride service and size and physical layout of the plant.
(B) It contains a definition of leak which is acceptable when
compared with the background concentrations of vinyl chloride in the
areas of the plant to be monitored by the vinyl chloride monitoring
system. Measurements of background concentrations of vinyl chloride in
the areas of the plant to be monitored by the vinyl chloride monitoring
system are to be included with the description of the program. The
definition of leak for a given plant may vary among the different areas
within the plant and is also to change over time as background
concentrations in the plant are reduced.
(C) It contains an acceptable plan of action to be taken when a leak
is detected.
(D) It provides for an acceptable calibration and maintenance
schedule for the vinyl chloride monitoring system and portable
hydrocarbon detector. For the vinyl chloride monitoring system, a daily
span check is to be conducted with a concentration of vinyl chloride
equal to the concentration defined as a leak according to paragraph
(b)(8)(i)(B) of this section. The calibration is to be done with
either:
(1) A calibration gas mixture prepared from the gases specified in
sections 5.2.1. and 5.2.2. of Test Method 106 and in accordance with
section 7.1 of Test Method 106, or
(2) A calibration gas cylinder standard containing the appropriate
concentration of vinyl chloride. The gas composition of the calibration
gas cylinder standard is to have been certified by the manufacturer.
The manufacturer must have recommended a maximum shelf life for each
cylinder so that the concentration does not change greater than 5
percent from the certified value. The date of gas cylinder preparation,
certified vinyl chloride concentration, and recommended maximum self
life must have been affixed to the cylinder before shipment from the
manufacturer to the buyer. If a gas chromatograph is used as the vinyl
chloride monitoring system, these gas mixtures may be directly used to
prepare a chromatograph calibration curve as described in section 7.3 of
Test Method 106. The requirements in section 5.2.3.1. and 5.2.3.2. of
Test Method 106 for certification of cylinder standards and for
establishment and verification of calibration standards are to be
followed.
(ii) For each process unit subject to this subpart, a formal leak
detection and repair program shall be implemented consistent with
subpart V of this part, except as provided in paragraph (b)(8)(iii) of
this section. This program is to be implemented within 90 days of the
effective date of these regulations, unless a waiver of compliance is
granted under 61.11. Except as provided in paragraph (b)(8)(ii)(E) of
this section, an owner or operator shall be exempt from 61.242-1(d),
61.242-7 (a), (b), and (c), 61.246, and 61.247 of subpart V of this
part for any process unit in which the percentage of leaking valves is
demonstrated to be less than 2.0 percent, as determined in accordance
with the following:
(A) A performance test as specified in paragraph (b)(8)(ii)(B) of
this section shall be conducted initially within 90 days of the
effective date of these regulations, annually, and at times requested by
the Administrator.
(B) For each performance test, a minimum of 200 or 90 percent,
whichever is less, of the total valves in VOC service (as defined in
60.481 of subpart VV of part 60) within the process unit shall be
randomly selected and monitored within 1 week by the methods specified
in 61.245(b) of this part. If an instrument reading of 10,000 ppm or
greater is measured, a leak is detected. The leak percentage shall be
determined by dividing the number of valves in VOC service for which
leaks are detected by the number of tested valves in VOC service.
(C) If a leak is detected, it shall be repaired in accordance with
61.242-7 (d) and (e) of subpart V of this part.
(D) The results of the performance test shall be submitted in writing
to the Administrator in the first quarterly report following the
performance test as part of the reporting requirements of 61.70.
(E) Any process unit in which the percentage of leaking valves is
found to be greater than 2.0 percent according to the performance test
prescribed in paragraph (b)(8)(ii)(B) of this section must comply with
all provisions of subpart V of this part within 90 days.
(iii) Open-ended valves or lines located on multiple service process
lines which operate in vinyl chloride service less than 10 percent of
the time are exempt from the requirements of 61.242-6 of subpart V,
provided the open-ended valves or lines are addressed in the monitoring
system required by paragraph (b)(8)(i) of this section. The
Administrator may apply this exemption to other existing open-ended
valves or lines that are demonstrated to require significant retrofit
cost to comply with the requirements of 61.242-6 of subpart V.
(9) Inprocess wastewater. Vinyl chloride emissions to the atmosphere
from inprocess wastewater are to be reduced as follows:
(i) The concentration of vinyl chloride in each inprocess wastewater
stream containing greater than 10 ppm vinyl chloride measured
immediately as it leaves a piece of equipment and before being mixed
with any other inprocess wastewater stream is to be reduced to no more
than 10 ppm by weight before being mixed with any other inprocess
wastewater stream which contains less than 10 ppm vinyl chloride;
before being exposed to the atmosphere; before being discharged to a
wastewater treatment process; or before being discharged untreated as a
wastewater. This paragraph does apply to water which is used to
displace vinyl chloride from equipment before it is opened to the
atmosphere in accordance with 61.64(a)(2) or paragraph (b)(6) of this
section, but does not apply to water which is used to wash out equipment
after the equipment has already been opened to the atmosphere in
accordance with 61.64(a)(2) or paragraph (b)(6) of this section.
(ii) Any vinyl chloride removed from the inprocess wastewater in
accordance with paragraph (b)(9)(i) of this section is to be ducted
through a control system from which the concentration of vinyl chloride
in the exhaust gases does not exceed 10 ppm (average for 3-hour period);
or equivalent as provided in 61.66.
(c) The requirements in paragraphs (b)(1), (b)(2), (b)(5), (b)(6),
(b)(7) and (b)(8) of this section are to be incorporated into a standard
operating procedure, and made available upon request for inspection by
the Administrator. The standard operating procedure is to include
provisions for measuring the vinyl chloride in equipment 4.75 m /3/
(1255 gal) in volume for which an emission limit is prescribed in
61.65(b)(6)(i) after opening the equipment and using Test Method 106, a
portable hydrocarbon detector, or an alternative method. The method of
measurement is to meet the requirements in 61.67(g)(5)(i)(A) or
(g)(5)(i)(B).
(d) A RVD that is ducted to a control device that is continually
operating while emissions from the release are present at the device is
subject to the following requirements:
(1) A discharge from a control device other than a flare shall not
exceed 10 ppm (average over a 3-hour period) as determined by the
continuous emission monitor system required under 61.68. Such a
discharge is subject to the requirements of 61.70.
(2) For a discharge routed to a flare, the flare shall comply with
the requirements of 60.18.
(i) Flare operations shall be monitored in accordance with the
requirements of 60.18(d) and 60.18(f)(2). For the purposes of
60.18(d), the volume and component concentration of each relief valve
discharge shall be estimated and calculation shall be made to verify
ongoing compliance with the design and operating requirements of 60.18
(c)(3) through (c)(6). If more than one relief valve is discharged
simultaneously to a single flare, these calculations shall account for
the cumulative effect of all such relief valve discharges. These
calculations shall be made and reported quarterly for all discharges
within the quarter. Failure to comply with any of the requirements of
this paragraph will be a violation of 61.65(d)(2). Monitoring for the
presence of a flare pilot flame shall be conducted in accordance with
60.18(f)(2). If the results of this monitoring or any other information
shows that the pilot flame is not present 100 percent of the time during
which a relief valve discharge is routed to the flare, the relief valve
discharge is subject to the provisions of 61.65(a).
(ii) A report describing the flare design shall be provided to the
Administrator not later than 90 days after the adoption of this
provision or within 30 days of the installation of a flare system for
control of relief valve discharge whichever is later. The flare design
report shall include calculations based upon expected relief valve
discharge component concentrations and net heating values (for PVC this
calculation shall be based on values expected if a release occurred at
the instant the polymerization starts); and estimated maximum exit
velocities based upon the design throat capacity of the gas in the
relief valve.
(41 FR 46564, Oct. 21, 1976; 41 FR 53017, Dec. 3, 1976, as amended
at 42 FR 29006, June 7, 1977; 51 FR 34910, Sept. 30, 1986; 53 FR
36972, Sept. 23, 1988; 55 FR 28348, July 10, 1990)
40 CFR 61.66 Equivalent equipment and procedures.
Upon written application from an owner or operator, the Administrator
may approve use of equipment or procedures which have been demonstrated
to his satisfaction to be equivalent in terms of reducing vinyl chloride
emissions to the atmosphere to those prescribed for compliance with a
specific paragraph of this subpart.
(51 FR 34912, Sept. 30, 1986)
40 CFR 61.67 Emission tests.
(a) Unless a waiver of emission testing is obtained under 61.13, the
owner or operator of a source to which this subpart applies shall test
emissions from the source,
(1) Within 90 days of the effective date in the case of an existing
source or a new source which has an initial startup date preceding the
effective date, or
(2) Within 90 days of startup in the case of a new source, initial
startup of which occurs after the effective date.
(b) The owner or operator shall provide the Administrator at least 30
days prior notice of an emission test to afford the Administrator the
opportunity to have an observer present during the test.
(c) Any emission test is to be conducted while the equipment being
tested is operating at the maximum production rate at which the
equipment will be operated and under other relevant conditions as may be
specified by the Administrator based on representative performance of
the source.
(d) (Reserved)
(e) When at all possible, each sample is to be analyzed within 24
hours, but in no case in excess of 72 hours of sample collection. Vinyl
chloride emissions are to be determined within 30 days after the
emission test. The owner or operator shall report the determinations to
the Administrator by a registered letter dispatched before the close of
the next business day following the determination.
(f) The owner or operator shall retain at the plant and make
available, upon request, for inspection by the Administrator, for a
minimum of 3 years, records of emission test results and other data
needed to determine emissions.
(g) Unless otherwise specified, the owner or operator shall use test
Test Methods in appendix B to this part for each test as required by
paragraphs (g)(1), (g)(2), (g)(3), (g)(4), and (g)(5) of this section,
unless an alternative method has been approved by the Administrator. If
the Administrator finds reasonable grounds to dispute the results
obtained by an alternative method, he may require the use of a reference
method. If the results of the reference and alternative methods do not
agree, the results obtained by the reference method prevail, and the
Administrator may notify the owner or operator that approval of the
method previously considered to be alternative is withdrawn. Whenever
Test Method 107 is specified, and the conditions in Section 1.1,
''Applicability'' of Method 107A are met, Method 107A may be used.
(1) Test Method 106 is to be used to determine the vinyl chloride
emissions from any source for which an emission limit is prescribed in
61.62 (a) or (b) 61.63(a), or 61.64(a)(1), (b), (c), or (d), or from
any control system to which reactor emissions are required to be ducted
in 61.64(a)(2) or to which fugitive emissions are required to be ducted
is 61.65(b)(1)(ii), (b)(2), (b)(5), (b)(6)(ii), or (b)(9)(ii).
(i) For each run, one sample is to be collected. The sampling site
is to be at least two stack or duct diameters downstream and one half
diameter upstream from any flow disturbance such as a bend, expansion,
contraction, or visible flame. For a rectangular cross section an
equivalent diameter is to be determined from the following equation:
equivalent diameter=2 (length) (width)/length+width
The sampling point in the duct is to be at the centroid of the cross
section. The sample is to be extracted at a rate proportional to the
gas velocity at the sampling point. The sample is to contain a minimum
volume of 50 liters corrected to standard conditions and is to be taken
over a period as close to 1 hour as practicable.
(ii) Each emission test is to consist of three runs. For the purpose
of determining emissions, the average of results of all runs is to
apply. The average is to be computed on a time weighted basis.
(iii) For gas streams containing more than 10 percent oxygen the
concentration of vinyl chloride as determined by Test Method 106 is to
be corrected to 10 percent oxygen (dry basis) for determination of
emissions by using the following equation:
where:
Cb (corrected)=The concentration of vinyl chloride in the exhaust
gases, corrected to 10-percent oxygen.
Cb=The concentration of vinyl chloride as measured by Test Method
106.
20.9=Percent oxygen in the ambient air at standard conditions.
10.9=Percent oxygen in the ambient air at standard conditions, minus
the 10.0-percent oxygen to which the correction is being made.
Percent O2=Percent oxygen in the exhaust gas as measured by Reference
Method 3 in Appendix A of part 60 of this chapter.
(iv) For those emission sources where the emission limit is
prescribed in terms of mass rather than concentration, mass emissions in
kg/100 kg product are to be determined by using the following equation:
where:
CBX=kg vinyl chloride/100 kg product.
Cb=The concentration of vinyl chloride as measured by Test Method
106.
2.60=Density of vinyl chloride at one atmosphere and 20 C in kg/m3.
Q=Volumetric flow rate in m3/hr as determined by Reference Method 2
of Appendix A to part 60 of this chapter.
10^6=Conversion factor for ppm.
Z=Production rate (kg/hr).
(2) Test Method 107 or Method 601 (incorporated by reference as
specified in 61.18) is to be used to determine the concentration of
vinyl chloride in each inprocess wastewater stream for which an emission
limit is prescribed in 61.65(b)(9)(i).
(3) When a stripping operation is used to attain the emission limits
in 61.64 (e) and (f), emissions are to be determined using Test Method
107 as follows:
(i) The number of strippers (or reactors used as strippers) and
samples and the types and grades of resin to be sampled are to be
determined by the Administrator for each individual plant at the time of
the test based on the plant's operation.
(ii) Each sample is to be taken immediately following the stripping
operation.
(iii) The corresponding quantity of material processed by each
stripper (or reactor used as a stripper) is to be determined on a dry
solids basis and by a method submitted to and approved by the
Administrator.
(iv) At the prior request of the Administrator, the owner or operator
shall provide duplicates of the samples required in paragraph (g)(3)(i)
of this section.
(4) Where control technology other than or in addition to a stripping
operation is used to attain the emission limit in 61.64(e), emissions
are to be determined as follows:
(i) Test Method 106 is to be used to determine atmospheric emissions
from all of the process equipment simultaneously. The requirements of
paragraph (g)(1) of this section are to be met.
(ii) Test Method 107 is to be used to determine the concentration of
vinyl chloride in each inprocess wastewater stream subject to the
emission limit prescribed in 61.64(e). The mass of vinyl chloride in
kg/100 kg product in each inprocess wastewater stream is to be
determined by using the following equation:
where:
CBX=kg vinyl chloride/100 kg product.
Cd=the concentration of vinyl chloride as measured by Test Method
107.
R=water flow rate in 1/hr, determined in accordance with a method
which has been submitted to and approved by the Administrator.
10^6=Conversion factor for ppm.
Z=Production rate (kg/hr), determined in accordance with a method
which has been submitted and approved by the Administrator.
(5) The reactor opening loss for which an emission limit is
prescribed in 61.64(a)(2) is to be determined. The number of reactors
for which the determination is to be made is to be specified by the
Administrator for each individual plant at the time of the determination
based on the plant's operation.
(i) Except as provided in paragraph (g)(5)(ii) of this section, the
reactor opening loss is to be determined using the following equation:
where:
C=kg vinyl chloride emissions/kg product.
W=Capacity of the reactor in m3.
2.60=Density of vinyl chloride at one atmosphere and 20 C in kg/m3.
10^6=Conversion factor for ppm.
Cb=ppm by volume vinyl chloride as determined by Test Method 106 or a
portable hydrocarbon detector which measures hydrocarbons with a
sensitivity of at least 10 ppm.
Y=Number of batches since the reactor was last opened to the
atmosphere.
Z=Average kg of polyvinyl chloride produced per batch in the number
of batches since the reactor was last opened to the atmosphere.
(A) If Method 106 is used to determine the concentration of vinyl
chloride (Cb), the sample is to be withdrawn at a constant rate with a
probe of sufficient length to reach the vessel bottom from the manhole.
Samples are to be taken for 5 minutes within 6 inches of the vessel
bottom, 5 minutes near the vessel center, and 5 minutes near the vessel
top.
(B) If a portable hydrocarbon detector is used to determine the
concentration of vinyl chloride (Cb), a probe of sufficient length to
reach the vessel bottom from the manhole is to be used to make the
measurements. One measurement will be made within 6 inches of the
vessel bottom, one near the vessel center and one near the vessel top.
Measurements are to be made at each location until the reading is
stabilized. All hydrocarbons measured are to be assumed to be vinyl
chloride.
(C) The production rate of polyvinyl chloride (Z) is to be determined
by a method submitted to and approved by the Administrator.
(ii) A calculation based on the number of evacuations, the vacuum
involved, and the volume of gas in the reactor is hereby approved by the
Administrator as an alternative method for determining reactor opening
loss for postpolymerization reactors in the manufacture of bulk resins.
Calculation methods based on techniques other than repeated evacuation
of the reactor may be approved by the Administrator for determining
reactor opening loss for postpolymerization reactors in the manufacture
of bulk resins.
(6) For a reactor that is used as a stripper, the emissions of vinyl
chloride from reactor opening loss and all sources following the reactor
used as a stripper for which an emission limit is prescribed in
61.64(f) are to be determined. The number of reactors for which the
determination is to be made is to be specified by the Administrator for
each individual plant at the time of the determination based on the
plant's operation.
(i) For each batch stripped in the reactor, the following
measurements are to be made:
(A) The concentration (ppm) of vinyl chloride in resin after
stripping, measured according to paragraph (g)(3) of this section;
(B) The reactor vacuum (mm Hg) at end of strip from plant instrument;
and
(C) The reactor temperature ( C) at end of strip from plant
instrument.
(ii) For each batch stripped in the reactor, the following
information is to be determined:
(A) The vapor pressure (mm Hg) of water in the reactor at end of
strip from the following table:
(B) The partial pressure (mm Hg) of vinyl chloride in reactor at end
of strip from the following equation:
PPVC= 760^RV^VPW
where:
PPVC=partial pressure of vinyl chloride, in mm Hg
760=atmospheric pressure at 0 C, in mm Hg
RV=absolute value of reactor vacuum, in mm Hg
VPW=vapor pressure of water, in mm Hg
(C) The reactor vapor space volume (m3) at end of strip from the
following equation:
where:
RVSV=reactor vapor space volume, in m /3/
RC=reactor capacity, in m /3/
WV=volume of water in reactor from recipe, in m /3/
PVCW=dry weight of polyvinyl chloride in reactor from recipe, in kg
1,400=typical density of polyvinyl chloride, in kg/m /3/
(iii) For each batch stripped in the reactor, the combined reactor
opening loss and emissions from all sources following the reactor used
as a stripper is to be determined using the following equation:
where:
C=g vinyl chloride/kg polyvinyl chloride product
PPMVC=concentration of vinyl chloride in resin after stripping, in
ppm
10^3=conversion factor for ppm
PPVC=partial pressure of vinyl chloride determined according to
paragraph (g)(6)(ii)(B) of this section, in mm Hg
RVSV=reactor vapor space volume determined according to paragraph
(g)(6)(ii)(C) of this section, in m3
1,002=ideal gas constant in g^ K/mm Hg^m3 for vinyl chloride
PVCW=dry weight of polyvinyl chloride in reactor from recipe, in kg
273=conversion factor for C to K
RT=reactor temperature, in C
(h)(1) Each piece of equipment within a process unit that can
reasonably contain equipment in vinyl chloride service is presumed to be
in vinyl chloride service unless an owner or operator demonstrates that
the piece of equipment is not in vinyl chloride service. For a piece of
equipment to be considered not in vinyl chloride service, it must be
determined that the percent vinyl chloride content can be reasonably
expected not to exceed 10 percent by weight for liquid streams or
contained liquid volumes and 10 percent by volume for gas streams or
contained gas volumes, which also includes gas volumes above liquid
streams or contained liquid volumes. For purposes of determining the
percent vinyl chloride content of the process fluid that is contained in
or contacts equipment, procedures that conform to the methods described
in ASTM Method D-2267 (incorporated by reference as specified in 61.18)
shall be used.
(2)(i) An owner or operator may use engineering judgment rather than
the procedures in paragraph (h)(1) of this section to demonstrate that
the percent vinyl chloride content does not exceed 10 percent by weight
for liquid streams and 10 percent by volume for gas streams, provided
that the engineering judgment demonstrates that the vinyl chloride
content clearly does not exceed 10 percent. When an owner or operator
and the Administrator do not agree on whether a piece of equipment is
not in vinyl chloride service, however, the procedures in paragraph
(h)(1) of this section shall be used to resolve the disagreement.
(ii) If an owner or operator determines that a piece of equipment is
in vinyl chloride service, the determination can be revised only after
following the procedures in paragraph (h)(1) of this section.
(3) Samples used in determining the percent vinyl chloride content
shall be representative of the process fluid that is contained in or
contacts the equipment.
(41 FR 46564, Oct. 21, 1976, as amended at 42 FR 29007, June 7, 1977;
47 FR 39486, Sept. 8, 1982; 50 FR 46295, Nov. 7, 1985; 51 FR 34912,
Sept. 30, 1986)
40 CFR 61.68 Emission monitoring.
(a) A vinyl chloride monitoring system is to be used to monitor on a
continuous basis the emissions from the sources for which emission
limits are prescribed in 61.62 (a) and (b), 61.63(a), and 61.64
(a)(1), (b), (c), and (d), and for any control system to which reactor
emissions are required to be ducted in 61.64(a)(2) or to which fugitive
emissions are required to be ducted in 61.65 (b)(1)(ii), and (b)(2),
(b)(5), (b)(6) (ii), and (b)(9)(ii).
(b) The vinyl chloride monitoring system(s) used to meet the
requirement in paragraph (a) of this section is to be a device which
obtains representative samples from one or more applicable emission
points on a continuous sequential basis and analyzes the samples with
gas chromatography or, if the owner or operator assumes that all
hydrocarbons measured are vinyl chloride, with infrared
spectrophotometry, flame ion detection, or an alternative method. The
vinyl chloride monitoring system used to meet the requirements in
61.65(b)(8)(i) may be used to meet the requirements of this section.
(c) A daily span check is to be conducted for each vinyl chloride
monitoring system used. For all of the emission sources listed in
paragraph (a) of this section, except the one for which an emission
limit is prescribed in 61.62(b), the daily span check is to be
conducted with a concentration of vinyl chloride equal to 10 ppm. For
the emission source for which an emission limit is prescribed in
61.62(b), the daily span check is to be conducted with a concentration
of vinyl chloride which is determined to be equivalent to the emission
limit for that source based on the emission test required by 61.67. The
calibration is to be done with either:
(1) A calibration gas mixture prepared from the gases specified in
sections 5.2.1 and 5.2.2 of Test Method 106 and in accordance with
section 7.1 of Test Method 106, or
(2) A calibration gas cylinder standard containing the appropriate
concentration of vinyl chloride. The gas composition of the calibration
gas cylinder standard is to have been certified by the manufacturer.
The manufacturer must have recommended a maximum shelf life for each
cylinder so that the concentration does not change greater than 5
percent from the certified value. The date of gas cylinder preparation,
certified vinyl chloride concentration and recommended maximum shelf
life must have been affixed to the cylinder before shipment from the
manufacturer to the buyer. If a gas chromatograph is used as the vinyl
chloride monitoring system, these gas mixtures may be directly used to
prepare a chromatograph calibration curve as described in section 7.3 of
Test Method 106. The requirements in sections 5.2.3.1 and 5.2.3.2 of
Test Method 106 for certification of cylinder standards and for
establishment and verification of calibration standards are to be
followed.
(d) When exhaust gas(es), having emission limits that are subject to
the requirement of paragraph (a) of this section, are emitted to the
atmosphere without passing through the control system and required vinyl
chloride monitoring system, the vinyl chloride content of the emission
shall be calculated (in units of each applicable emission limit) by best
practical engineering judgment based on the discharge duration and known
VC concentrations in the affected equipment as determined in accordance
with 61.67(h) or other acceptable method.
(e) For each 3-hour period, the vinyl chloride content of emissions
subject to the requirements of paragraphs (a) and (d) of this section
shall be averaged (weighted according to the proportion of time that
emissions were continuously monitored and that emissions bypassed the
continuous monitor) for purposes of reporting excess emissions under
61.70(c)(1).
(f) For each vinyl chloride emission to the atmosphere determined in
accordance with paragraph (e) of this section to be in excess of the
applicable emission limits, the owner or operator shall record the
identity of the source(s), the date, time, and duration of the excess
emission, the cause of the excess emission, and the approximate total
vinyl chloride loss during the excess emission, and the method used for
determining the vinyl chloride loss. This information shall be retained
and made available for inspection by the Administrator as required by
61.71(a).
(41 FR 46564, Oct. 21, 1976; 41 FR 53017, Dec. 3, 1976, as amended
at 42 FR 29007, June 7, 1977; 50 FR 46295, Nov. 7, 1985; 51 FR 34913,
Sept. 30, 1986; 55 FR 28349, July 10, 1990)
40 CFR 61.69 Initial report.
(a) An owner or operator of any source to which this subpart applies
shall submit a statement in writing notifying the Administrator that the
equipment and procedural specifications in 61.65 (b)(1), (b)(2),
(b)(3), (b)(4), (b)(5), (b)(6), (b)(7), and (b)(8) are being
implemented.
(b)(1) In the case of an existing source or a new source which has an
initial startup date preceding the effective date, the statement is to
be submitted within 90 days of the effective date, unless a waiver of
compliance is granted under 61.11, along with the information required
under 61.10. If a waiver of compliance is granted, the statement is to
be submitted on a date scheduled by the Administrator.
(2) In the case of a new source which did not have an initial startup
date preceding the effective date, the statement is to be submitted
within 90 days of the initial startup date.
(c) The statement is to contain the following information:
(1) A list of the equipment installed for compliance,
(2) A description of the physical and functional characteristics of
each piece of equipment,
(3) A description of the methods which have been incorporated into
the standard operating procedures for measuring or calculating the
emissions for which emission limits are prescribed in 61.65 (b)(1)(i)
and (b)(6)(i),
(4) A statement that each piece of equipment is installed and that
each piece of equipment and each procedure is being used.
40 CFR 61.70 Reporting.
(a)(1) The owner or operator of any source to which this subpart
applies shall submit to the Administrator on March 15, June 15,
September 15, and December 15 of each year a report in writing
containing the information required by this section. The first report
is to be submitted following the first full 3-month reporting period
after the initial report is submitted.
(2) In the case of an existing source, the approved reporting
schedule shall be used. In addition, quarterly reports shall be
submitted exactly 3 months following the current reporting dates.
(b)(1) In the case of an existing source or a new source which has an
initial startup date preceding the effective date, the first report is
to be submitted within 180 days of the effective date, unless a waiver
of compliance is granted under 61.11. If a waiver of compliance is
granted, the first report is to be submitted on a date scheduled by the
Administrator.
(2) In the case of a new source which did not have an initial startup
date preceding the effective date, the first report is to be submitted
within 180 days of the initial startup date.
(c) Unless otherwise specified, the owner or operator shall use the
Test Methods in appendix B to this part to conduct emission tests as
required by paragraphs (c)(2) and (c)(3) of this section, unless an
alternative method has been approved by the Administrator. If the
Administrator finds reasonable grounds to dispute the results obtained
by an alternative method, he may require the use of a reference method.
If the results of the reference and alternative methods do not agree,
the results obtained by the reference method prevail, and the
Administrator may notify the owner or operator that approval of the
method previously considered to be alternative is withdrawn.
(1) The owner or operator shall include in the report a record of the
vinyl chloride content of emissions for each 3-hour period during which
average emissions are in excess of the emission limits in 61.62 (a) or
(b), 61.63 (a), or 61.64 (a)(1), (b), (c), or (d), or during which
average emissions are in excess of the emission limits specified for any
control system to which reactor emissions are required to be ducted in
61.64 (a)(2) or to which fugitive emissions are required to be ducted in
61.65 (b)(i)(ii), (b)(2), (b)(5), (b)(6)(ii), or (b)(9)(ii).The number
of 3-hour periods for which average emissions were determined during the
reporting period shall be reported. If emissions in excess of the
emission limits are not detected, the report shall contain a statement
that no excess emissions have been detected. The emissions are to be
determined in accordance with 61.68(e).
(2) In polyvinyl chloride plants for which a stripping operation is
used to attain the emission level prescribed in 61.64(e), the owner or
operator shall include in the report a record of the vinyl chloride
content in the polyvinyl chloride resin.
(i) If batch stripping is used, one representative sample of
polyvinyl chloride resin is to be taken from each batch of each grade of
resin immediately following the completion of the stripping operation,
and identified by resin type and grade and the date and time the batch
is completed. The corresponding quantity of material processed in each
stripper batch is to be recorded and identified by resin type and grade
and the date and time the batch is completed.
(ii) If continuous stripping is used, one representative sample of
polyvinyl chloride resin is to be taken for each grade of resin
processed or at intervals of 8 hours for each grade of resin which is
being processed, whichever is more frequent. The sample is to be taken
as the resin flows out of the stripper and identified by resin type and
grade and the date and time the sample was taken. The corresponding
quantity of material processed by each stripper over the time period
represented by the sample during the 8-hour period, is to be recorded
and identified by resin type and grade and the date and time it
represents.
(iii) The vinyl chloride content in each sample is to be determined
by Test Method 107 as prescribed in 61.67(g)(3).
(iv) (Reserved)
(v) The report to the Administrator by the owner or operator is to
include a record of any 24-hour average resin vinyl chloride
concentration, as determined in this paragraph, in excess of the limits
prescribed in 61.64(e). The vinyl chloride content found in each sample
required by paragraphs (c)(2)(i) and (c)(2)(ii) of this section shall be
averaged separately for each type of resin, over each calendar day and
weighted according to the quantity of each grade of resin processed by
the stripper(s) that calendar day, according to the following equation:
where:
AT =24-hour average concentration of type T resin in ppm (dry weight
basis)
QT =Total production of type T resin over the 24-hour period, in kg.
T=Type of resin.
MGi=Concentration of vinyl chloride in one sample of grade Gi resin
in ppm.
PGi=Production of grade Gi resin represented by the sample, in kg.
Gi=Grade of resin: e.g., G1, G2, G3.
n=Total number of grades of resin produced during the 24-hour period.
The number of 24-hour average concentrations for each resin type
determined during the reporting period shall be reported. If no 24-hour
average resin vinyl chloride concentrations in excess of the limits
prescribed in 61.64(e) are measured, the report shall state that no
excess resin vinyl chloride concentrations were measured.
(vi) The owner or operator shall retain at the source and make
available for inspection by the Administrator for a minimum of 3 years
records of all data needed to furnish the information required by
paragraph (c)(2)(v) of this section. The records are to contain the
following information:
(A) The vinyl chloride content found in all the samples required in
paragraphs (c)(2)(i) and (c)(2)(ii) of this section, identified by the
resin type and grade and the time and date of the sample, and
(B) The corresponding quantity of polyvinyl chloride resin processed
by the stripper(s), identified by the resin type and grade and the time
and date it represents.
(3) The owner or operator shall include in the report a record of any
emissions from each reactor opening in excess of the emission limits
prescribed in 61.64(a)(2). Emissions are to be determined in accordance
with 61.67(g)(5), except that emissions for each reactor are to be
determined. The number of reactor openings during the reporting period
shall be reported. If emissions in excess of the emission limits are
not detected, the report shall include a statement that excess emissions
have not been detected.
(4) In polyvinyl chloride plants for which stripping in the reactor
is used to attain the emission level prescribed in 61.64(f), the owner
or operator shall include in the report a record of the vinyl chloride
emissions from reactor opening loss and all sources following the
reactor used as a stripper.
(i) One representative sample of polyvinyl chloride resin is to be
taken from each batch of each grade of resin immediately following the
completion of the stripping operation, and identified by resin type and
grade and the date and time the batch is completed. The corresponding
quantity of material processed in each stripper batch is to be recorded
and identified by resin type and grade and the date and time the batch
is completed.
(ii) The vinyl chloride content in each sample is to be determined by
Test Method 107 as prescribed in 61.67(g)(3).
(iii) The combined emissions from reactor opening loss and all
sources following the reactor used as a stripper are to be determined
for each batch stripped in a reactor according to the procedure
prescribed in 61.67(g)(6).
(iv) The report to the Administrator by the owner or operator is to
include a record of any 24-hour average combined reactor opening loss
and emissions from all sources following the reactor used as a stripper
as determined in this paragraph, in excess of the limits prescribed in
61.64(f). The combined reactor opening loss and emissions from all
sources following the reactor used as a stripper associated with each
batch are to be averaged separately for each type of resin, over each
calendar day and weighted according to the quantity of each grade of
resin stripped in reactors that calendar day as follows:
For each type of resin (suspension, dispersion, latex, bulk, other),
the following calculation is to be performed:
where:
AT =24-hour average combined reactor opening loss and emissions from
all sources following the reactor used as a stripper, in g vinyl
chloride/kg product (dry weight basis).
QT=Total production of resin in batches for which stripping is
completed during the 24-hour period, in kg.
T=Type of resin.
CGi=Average combined reactor opening loss and emissions from all
sources following the reactor used as a stripper of all batches of grade
Gi resin for which stripping is completed during the 24-hour period, in
g vinyl chloride/kg product (dry weight basis) (determined according to
procedure prescribed in 61.67(g)(6)).
PGi=Production of grade Gi resin in the batches for which C is
determined, in kg.
Gi=Grade of resin e.g., G1, G2, and G3.
n=Total number of grades of resin in batches for which stripping is
completed during the 24-hour period.
The number of 24-hour average emissions determined during the
reporting period shall be reported. If no 24-hour average combined
reactor opening loss and emissions from all sources following the
reactor used a stripper in excess of the limits prescribed in 61.64(f)
are determined, the report shall state that no excess vinyl chloride
emissions were determined.
(41 FR 46564, Oct. 21, 1976 as amended at 42 FR 29007, June 7, 1977;
50 FR 46295, Nov. 7, 1985; 51 FR 34914, Sept. 30, 1986; 53 FR 36972,
Sept. 23, 1988; 53 FR 46976, Nov. 21, 1988)
40 CFR 61.71 Recordkeeping.
(a) The owner or operator of any source to which this subpart applies
shall retain the following information at the source and make it
available for inspection to the Administrator for a minimum of 3 years:
(1) A record of the leaks detected by the vinyl chloride monitoring
system, as required by 61.65(b)(8), including the concentrations of
vinyl chloride measured, analyzed, and recorded by the vinyl chloride
detector, the location of each measurement and the date and approximate
time of each measurement.
(2) A record of the leaks detected during routine monitoring with the
portable hydrocarbon detector and the action taken to repair the leaks,
as required by 61.65(b)(8), including a brief statement explaining the
location and cause of each leak detected with the portable hydrocarbon
detector, the date and time of the leak, and any action taken to
eliminate that leak.
(3) A record of emissions measured in accordance with 61.68.
(4) A daily operating record for each polyvinyl chloride reactor,
including pressures and temperatures.
(41 FR 46594, Oct. 21, 1976, as amended at 42 FR 29007, June 7, 1977;
51 FR 34914, Sept. 30, 1986)
40 CFR 61.71 Subpart G -- (Reserved)
40 CFR 61.71 Subpart H -- National Emission Standards for Emissions of
Radionuclides Other Than Radon From Department of Energy Facilities
Source: 54 FR 51695, Dec. 15, 1989, unless otherwise noted.
40 CFR 61.90 Designation of facilities.
The provisions of this subpart apply to operations at any facility
owned or operated by the Department of Energy that emits any
radionuclide other than radon-222 and radon-220 into the air, except
that this subpart does not apply to disposal at facilities subject to 40
CFR part 191, subpart B or 40 CFR part 192.
40 CFR 61.91 Definitions.
As used in this subpart, all terms not defined here have the meaning
given them in the Clean Air Act or 40 CFR part 61, subpart A. The
following terms shall have the following specific meanings:
(a) Effective dose equivalent means the sum of the products of
absorbed dose and appropriate factors to account for differences in
biological effectiveness due to the quality of radiation and its
distribution in the body of reference man. The unit of the effective
dose equivalent is the rem. For purposes of this subpart, doses caused
by radon-222 and its respective decay products formed after the radon is
released from the facility are not included. The method for calculating
effective dose equivalent and the definition of reference man are
outlined in the International Commission on Radiological Protection's
Publication No. 26.
(b) Facility means all buildings, structures and operations on one
contiguous site.
(c) Radionuclide means a type of atom which spontaneously undergoes
radioactive decay.
(d) Residence means any home, house, apartment building, or other
place of dwelling which is occupied during any portion of the relevant
year.
40 CFR 61.92 Standard.
Emissions of radionuclides to the ambient air from Department of
Energy facilities shall not exceed those amounts that would cause any
member of the public to receive in any year an effective dose equivalent
of 10 mrem/yr.
40 CFR 61.93 Emission monitoring and test procedures.
(a) To determine compliance with the standard, radionuclide emissions
shall be determined and effective dose equivalent values to members of
the public calculated using EPA approved sampling procedures, computer
models CAP-88 or AIRDOS-PC, or other procedures for which EPA has
granted prior approval. DOE facilities for which the maximally exposed
individual lives within 3 kilometers of all sources of emissions in the
facility, may use EPA's COMPLY model and associated procedures for
determining dose for purposes of compliance.
(b) Radionuclide emission rates from point sources (stacks or vents)
shall be measured in accordance with the following requirements or other
procedures for which EPA has granted prior approval:
(1) Effluent flow rate measurements shall be made using the following
methods:
(i) Reference Method 2 of appendix A to part 60 shall be used to
determine velocity and volumetric flow rates for stacks and large vents.
(ii) Reference Method 2A of appendix A to part 60 shall be used to
measure flow rates through pipes and small vents.
(iii) The frequency of the flow rate measurements shall depend upon
the variability of the effluent flow rate. For variable flow rates,
continuous or frequent flow rate measurements shall be made. For
relatively constant flow rates only periodic measurements are necessary.
(2) Radionuclides shall be directly monitored or extracted, collected
and measured using the following methods:
(i) Reference Method 1 of appendix A part 60 shall be used to select
monitoring or sampling sites.
(ii) The effluent stream shall be directly monitored continuously
with an in-line detector or representative samples of the effluent
stream shall be withdrawn continuously from the sampling site following
the guidance presented in ANSIN13.1-1969 ''Guide to Sampling Airborne
Radioactive Materials in Nuclear Facilities'' (including the guidance
presented in appendix A of ANSIN13.1) (incorporated by reference -- see
61.18). The requirements for continuous sampling are applicable to batch
processes when the unit is in operation. Periodic sampling (grab
samples) may be used only with EPA's prior approval. Such approval may
be granted in cases where continuous sampling is not practical and
radionuclide emission rates are relatively constant. In such cases,
grab samples shall be collected with sufficient frequency so as to
provide a representative sample of the emissions.
(iii) Radionuclides shall be collected and measured using procedures
based on the principles of measurement described in appendix B, Method
114. Use of methods based on principles of measurement different from
those described in appendix B, Method 114 must have prior approval from
the Administrator. EPA reserves the right to approve measurement
procedures.
(iv) A quality assurance program shall be conducted that meets the
performance requirements described in appendix B, Method 114.
(3) When it is impractical to measure the effluent flow rate at an
existing source in accordance with the requirements of paragraph (b)(1)
of this section or to monitor or sample an effluent stream at an
existing source in accordance with the site selection and sample
extraction requirements of paragraph (b)(2) of this section, the
facility owner or operator may use alternative effluent flow rate
measurement procedures or site selection and sample extraction
procedures provided that:
(i) It can be shown that the requirements of paragraph (b) (1) or (2)
of this section are impractical for the effluent stream.
(ii) The alternative procedure will not significantly underestimate
the emissions.
(iii) The alternative procedure is fully documented.
(iv) The owner or operator has received prior approval from EPA.
(4)(i) Radionuclide emission measurements in conformance with the
requirements of paragraph (b) of this section shall be made at all
release points which have a potential to discharge radionuclides into
the air in quantities which could cause an effective dose equivalent in
excess of 1% of the standard. All radionuclides which could contribute
greater than 10% of the potential effective dose equivalent for a
release point shall be measured. With prior EPA approval, DOE may
determine these emissions through alternative procedures. For other
release points which have a potential to release radionuclides into the
air, periodic confirmatory measurements shall be made to verify the low
emissions.
(ii) To determine whether a release point is subject to the emission
measurement requirements of paragraph (b) of this section, it is
necessary to evaluate the potential for radionuclide emissions for that
release point. In evaluating the potential of a release point to
discharge radionuclides into the air for the purposes of this section,
the estimated radionuclide release rates shall be based on the discharge
of the effluent stream that would result if all pollution control
equipment did not exist, but the facilities operations were otherwise
normal.
(5) Environmental measurements of radionuclide air concentrations at
critical receptor locations may be used as an alternative to air
dispersion calculations in demonstrating compliance with the standard if
the owner or operator meets the following criteria:
(i) The air at the point of measurement shall be continuously sampled
for collection of radionuclides.
(ii) Those radionuclides released from the facility, which are the
major contributors to the effective dose equivalent must be collected
and measured as part of the environmental measurement program.
(iii) Radionuclide concentrations which would cause an effective dose
equivalent of 10% of the standard shall be readily detectable and
distinguishable from background.
(iv) Net measured radionuclide concentrations shall be compared to
the concentration levels in Table 2 of appendix E to determine
compliance with the standard. In the case of multiple radionuclides
being released from a facility, compliance shall be demonstrated if the
value for all radionuclides is less than the concentration level in
Table 2, and the sum of the fractions that result when each measured
concentration value is divided by the value in Table 2 for each
radionuclide is less than 1.
(v) A quality assurance program shall be conducted that meets the
performance requirements described in appendix B, Method 114.
(vi) Use of environmental measurements to demonstrate compliance with
the standard is subject to prior approval of EPA. Applications for
approval shall include a detailed description of the sampling and
analytical methodology and show how the above criteria will be met.
40 CFR 61.94 Compliance and reporting.
(a) Compliance with this standard shall be determined by calculating
the highest effective dose equivalent to any member of the public at any
offsite point where there is a residence, school, business or office.
The owners or operators of each facility shall submit an annual report
to both EPA headquarters and the appropriate regional office by June 30
which includes the results of the monitoring as recorded in DOE's
Effluent Information System and the dose calculations required by
61.93(a) for the previous calendar year.
(b) In addition to the requirements of paragraph (a) of this section,
an annual report shall include the following information:
(1) The name and location of the facility.
(2) A list of the radioactive materials used at the facility.
(3) A description of the handling and processing that the radioactive
materials undergo at the facility.
(4) A list of the stacks or vents or other points where radioactive
materials are released to the atmosphere.
(5) A description of the effluent controls that are used on each
stack, vent, or other release point and an estimate of the efficiency of
each control device.
(6) Distances from the points of release to the nearest residence,
school, business or office and the nearest farms producing vegetables,
milk, and meat.
(7) The values used for all other user-supplied input parameters for
the computer models (e.g., meteorological data) and the source of these
data.
(8) A brief description of all construction and modifications which
were completed in the calendar year for which the report is prepared,
but for which the requirement to apply for approval to construct or
modify was waived under 61.96 and associated documentation developed by
DOE to support the waiver. EPA reserves the right to require that DOE
send to EPA all the information that normally would be required in an
application to construct or modify, following receipt of the description
and supporting documentation.
(9) Each report shall be signed and dated by a corporate officer or
public official in charge of the facility and contain the following
declaration immediately above the signature line: ''I certify under
penalty of law that I have personally examined and am familiar with the
information submitted herein and based on my inquiry of those
individuals immediately responsible for obtaining the information, I
believe that the submitted information is true, accurate and complete.
I am aware that there are significant penalties for submitting false
information including the possibility of fine and imprisonment. See, 18
U.S.C. 1001.''
(c) If the facility is not in compliance with the emission limits of
61.92 in the calendar year covered by the report, then the facility must
commence reporting to the Administrator on a monthly basis the
information listed in paragraph (b) of this section, for the preceding
month. These reports will start the month immediately following the
submittal of the annual report for the year in noncompliance and will be
due 30 days following the end of each month. This increased level of
reporting will continue until the Administrator has determined that the
monthly reports are no longer necessary. In addition to all the
information required in paragraph (b) of this section, monthly reports
shall also include the following information:
(1) All controls or other changes in operation of the facility that
will be or are being installed to bring the facility into compliance.
(2) If the facility is under a judicial or administrative enforcement
decree, the report will describe the facilities performance under the
terms of the decree.
(d) In those instances where the information requested is classified,
such information will be made available to EPA separate from the report
and will be handled and controlled according to applicable security and
classification regulations and requirements.
(Approved by the Office of Management and Budget under control number
2060-0191)
40 CFR 61.95 Recordkeeping requirements.
All facilities must maintain records documenting the source of input
parameters including the results of all measurements upon which they are
based, the calculations and/or analytical methods used to derive values
for input parameters, and the procedure used to determine effective dose
equivalent. This documentation should be sufficient to allow an
independent auditor to verify the accuracy of the determination made
concerning the facility's compliance with the standard. These records
must be kept at the site of the facility for at least five years and,
upon request, be made available for inspection by the Administrator, or
his authorized representative.
40 CFR 61.96 Applications to construct or modify.
(a) In addition to any activity that is defined as construction under
40 CFR part 61, subpart A, any fabrication, erection or installation of
a new building or structure within a facility that emits radionuclides
is also defined as new construction for purposes of 40 CFR part 61,
subpart A.
(b) An application for approval under 61.07 or notification of
startup under 61.09 does not need to be filed for any new construction
of or modification within an existing facility if the effective dose
equivalent, caused by all emissions from the new construction or
modification, is less than 1% of the standard prescribed in 61.92. For
purposes of this paragraph the effective dose equivalent shall be
calculated using the source term derived using appendix D as input to
the dispersion and other computer models described in 61.93. DOE may,
with prior approval from EPA, use another procedure for estimating the
source term for use in this paragraph. A facility is eligible for this
exemption only if, based on its last annual report, the facility is in
compliance with this subpart.
(c) Conditions to approvals granted under 61.08 will not contain
requirements for post approval reporting on operating conditions beyond
those specified in 61.94.
40 CFR 61.97 Exemption from the reporting and testing requirements of
40 CFR 61.10.
All facilities designated under this subpart are exempt from the
reporting requirements of 40 CFR 61.10.
40 CFR 61.97 Subpart I -- National Emission Standards for Radionuclide
Emissions From Facilities Licensed by the Nuclear Regulatory Commission
and Federal Facilities Not Covered by Subpart H
Source: 54 FR 51697, Dec. 15, 1989, unless otherwise noted.
Effective Date Note: At 55 FR 38057, Sept. 17, 1990, subpart I was
stayed until March 10, 1991. At 56 FR 10514, Mar. 13, 1991, the
effectiveness of subpart I for all NRC-licensed facilities other than
nuclear power reactors was stayed until April 15, 1991. At 56 FR 18738,
Apr. 24, 1991, the effectiveness for all facilities licensed by the NRC
or by an Agreement State, except for nuclear power reactors, was stayed
until November 15, 1992. For the convenience of the user the superseded
text appears after the new material below.
Editorial Note: The effectiveness of subpart I for nuclear power
reactors was temporarily stayed at 56 FR 10523, March 13, 1991.
40 CFR 61.100 Applicability.
The provisions of this subpart apply to Nuclear Regulatory
Commission-licensed facilities and to facilities owned or operated by
any Federal agency other than the Department of Energy, except that this
subpart does not apply to disposal at facilities regulated under 40 CFR
part 191, subpart B, or to any uranium mill tailings pile after it has
been disposed of under 40 CFR part 192, or to low energy accelerators,
or to any NRC-licensee that possesses and uses radionuclides only in the
form of sealed sources.
40 CFR 61.101 Definitions.
As used in this subpart, all terms not defined here have the meaning
given them in the Clean Air Act or subpart A of part 61. The following
terms shall have the following specific meanings:
(a) Agreement State means a State with which the Atomic Energy
Commission or the Nuclear Regulatory Commission has entered into an
effective agreement under subsection 274(b) of the Atomic Energy Act of
1954, as amended.
(b) Effective dose equivalent means the sum of the products of
absorbed dose and appropriate factors to account for differences in
biological effectiveness due to the quality of radiation and its
distribution in the body of reference man. The unit of the effective
dose equivalent is the rem. For purposes of this subpart doses caused
by radon-222 and its decay products formed after the radon is released
from the facility are not included. The method for calculating
effective dose equivalent and the definition of reference man are
outlined in the International Commission on Radiological Protection's
Publication No. 26.
(c) Facility means all buildings, structures and operations on one
contiguous site.
(d) Federal facility means any facility owned or operated by any
department, commission, agency, office, bureau or other unit of the
government of the United States of America except for facilities owned
or operated by the Department of Energy.
(e) NRC-licensed facility means any facility licensed by the Nuclear
Regulatory Commission or any Agreement State to receive title to,
receive, possess, use, transfer, or deliver any source, by-product, or
special nuclear material.
(f) Radionuclide means a type of atom which spontaneously undergoes
radioactive decay.
40 CFR 61.102 Standard.
(a) Emissions of radionuclides, including iodine, to the ambient air
from a facility regulated under this subpart shall not exceed those
amounts that would cause any member of the public to receive in any year
an effective dose equivalent of 10 mrem/yr.
(b) Emissions of iodine to the ambient air from a facility regulated
under this subpart shall not exceed those amounts that would cause any
member of the public to receive in any year an effective dose equivalent
of 3 mrem/yr.
40 CFR 61.103 Determining compliance.
(a) Compliance with the emission standard in this subpart shall be
determined through the use of either the EPA computer code COMPLY or the
alternative requirements of appendix E. Facilities emitting
radionuclides not listed in COMPLY or appendix E shall contact EPA to
receive the information needed to determine dose. The source terms to
be used for input into COMPLY shall be determined through the use of the
measurement procedures listed in 61.107 or the emission factors in
appendix D or through alternative procedures for which EPA has granted
prior approval; or,
(b) Facilities may demonstrate compliance with the emission standard
in this subpart through the use of computer models that are equivalent
to COMPLY, provided that the model has received prior approval from EPA
headquarters. Any facility using a model other than COMPLY must file an
annual report. EPA may approve an alternative model in whole or in part
and may limit its use to specific circumstances.
40 CFR 61.104 Reporting requirements.
(a) The owner or operator of a facility subject to this subpart must
submit an annual report to the EPA covering the emissions of a calendar
year by March 31 of the following year.
(1) The report or application for approval to construct or modify as
required by 40 CFR part 61, subpart A and 61.106, must provide the
following information:
(i) The name of the facility.
(ii) The name of the person responsible for the operation of the
facility and the name of the person preparing the report (if different).
(iii) The location of the facility, including suite and/or building
number, street, city, county, state, and zip code.
(iv) The mailing address of the facility, if different from item
(iii).
(v) A list of the radioactive materials used at the facility.
(vi) A description of the handling and processing that the
radioactive materials undergo at the facility.
(vii) A list of the stacks or vents or other points where radioactive
materials are released to the atmosphere.
(viii) A description of the effluent controls that are used on each
stack, vent, or other release point and an estimate of the efficiency of
each device.
(ix) Distances from the point of release to the nearest residence,
school, business or office and the nearest farms producing vegetables,
milk, and meat.
(x) The effective dose equivalent calculated using the compliance
procedures in 61.103.
(xi) The physical form and quantity of each radionuclide emitted from
each stack, vent or other release point, and the method(s) by which
these quantities were determined.
(xii) The volumetric flow, diameter, effluent temperature, and
release height for each stack, vent or other release point where
radioactive materials are emitted, the method(s) by which these were
determined.
(xiii) The height and width of each building from which radionuclides
are emitted.
(xiv) The values used for all other user-supplied input parameters
(e.g., meteorological data) and the source of these data.
(xv) A brief description of all construction and modifications which
were completed in the calendar year for which the report is prepared,
but for which the requirement to apply for approval to construct or
modify was waived under section 61.106, and associated documentation
developed by the licensee to support the waiver. EPA reserves the right
to require that the licensee send to EPA all the information that
normally would be required in an application to construct or modify,
following receipt of the description and supporting documentation.
(xvi) Each report shall be signed and dated by a corporate officer or
public official in charge of the facility and contain the following
declaration immediately above the signature line: ''I certify under
penalty of law that I have personally examined and am familiar with the
information submitted herein and based on my inquiry of those
individuals immediately responsible for obtaining the information, I
believe that the submitted information is true, accurate and complete.
I am aware that there are significant penalties for submitting false
information including the possibility of fine and imprisonment. See, 18
U.S.C. 1001.''
(b) Facilities emitting radionuclides in an amount that would cause
less than 10% of the dose standard in 61.102, as determined by the
compliance procedures from 61.103(a), are exempt from the reporting
requirements of 61.104(a). Facilities shall annually make a new
determination whether they are exempt from reporting.
(c) If the facility is not in compliance with the emission limits of
61.102 in the calendar year covered by the report, the facility must
report to the Administrator on a monthly basis the information listed in
paragraph (a) of this section, for the preceding month. These reports
will start the month immediately following the submittal of the annual
report for the year in noncompliance and will be due 30 days following
the end of each month. This increased level of reporting will continue
until the Administrator has determined that the monthly reports are no
longer necessary. In addition to all the information required in
paragraph (a) of this section, monthly reports shall also include the
following information:
(1) All controls or other changes in operation of the facility that
will be or are being installed to bring the facility into compliance.
(2) If the facility is under a judicial or administrative enforcement
decree the report will describe the facilities performance under the
terms of the decree.
(d) The first report will cover the emissions of calendar year 1990.
40 CFR 61.105 Recordkeeping requirements.
The owner or operator of any facility must maintain records
documenting the source of input parameters including the results of all
measurements upon which they are based, the calculations and/or
analytical methods used to derive values for input parameters, and the
procedure used to determine compliance. This documentation should be
sufficient to allow an independent auditor to verify the accuracy of the
determination made concerning the facility's compliance with the
standard, and, if claimed, qualification for exemption from reporting.
These records must be kept at the site of the facility for at least five
years and upon request be made available for inspection by the
Administrator, or his authorized representative.
40 CFR 61.106 Applications to construct or modify.
(a) In addition to any activity that is defined as construction under
40 CFR part 61, subpart A, any fabrication, erection or installation of
a new building or structure within a facility is also defined as new
construction for purposes of 40 CFR part 61, subpart A.
(b) An application under 61.07 does not need to be filed for any new
construction of or modification within an existing facility if one of
the following conditions is met:
(1) The effective dose equivalent calculated by using methods
described in 61.103, that is caused by all emissions from the facility
including those potentially emitted by the proposed new construction or
modification, is less than 10% of the standard prescribed in 61.102.
(2) The effective dose equivalent calculated by using methods
described in 61.103, that is caused by all emissions from the new
construction or modification, is less than 1% of the limit prescribed in
61.102. A facility is eligible for this exemption only if the facility,
based on its last annual report, is in compliance with this subpart.
40 CFR 61.107 Emission determination.
(a) Facility owners or operators may, in lieu of monitoring, estimate
radionuclide emissions in accordance with appendix D, or other procedure
for which EPA has granted prior approval.
(b) Radionuclide emission rates from point sources (e.g. stacks or
vents) shall be measured in accordance with the following requirements:
(1) Effluent flow rate measurements shall be made using the following
methods:
(i) Reference Method 2 of appendix A to part 60 shall be used to
determine velocity and volumetric flow rates for stacks and large vents.
(ii) Reference Method 2A of appendix A to part 60 shall be used to
measure flow rates through pipes and small vents.
(iii) The frequency of the flow rate measurements shall depend upon
the variability of the effluent flow rate. For variable flow rates,
continuous or frequent flow rate measurements shall be made. For
relatively constant flow rates only periodic measurements are necessary.
(2) Radionuclides shall be directly monitored or extracted,
collected, and measured using the following methods:
(i) Reference Method 1 of appendix A part 60 shall be used to select
monitoring or sampling sites.
(ii) The effluent stream shall be directly monitored continuously
using an in-line detector or representative samples of the effluent
stream shall be withdrawn continuously from the sampling site following
the guidance presented in ANSIN13.1-1969 ''Guide to Sampling Airborne
Radioactive Materials in Nuclear Facilities'' (including the guidance
presented in appendix A of ANSIN13.1) (incorporated by reference -- see
61.18). The requirements for continuous sampling are applicable to batch
processes when the unit is in operation. Periodic sampling (grab
samples) may be used only with EPA's prior approval. Such approval may
be granted in cases where continuous sampling is not practical and
radionuclide emission rates are relatively constant. In such cases,
grab samples shall be collected with sufficient frequency so as to
provide a representative sample of the emissions.
(iii) Radionuclides shall be collected and measured using procedures
based on the principles of measurement described in appendix B, Method
114. Use of methods based on principles of measurement different from
those described in appendix B, Method 114 must have prior approval from
the Administrator. EPA reserves the right to approve alternative
measurement procedures in whole or in part.
(iv) A quality assurance program shall be conducted that meets the
performance requirements described in appendix B, method 114.
(3) When it is impractical to measure the effluent flow rate at an
existing source in accordance with the requirements of paragraph (b)(1)
of this section or to monitor or sample an effluent stream at an
existing source in accordance with the site selection and sample
extraction requirements of paragraph (b)(2) of this section, the
facility owner or operator may use alternative effluent flow rate
measurement procedures or site selection and sample extraction
procedures provided that:
(i) It can be shown that the requirements of paragraphs (b) (1) and
(2) of this section are impractical for the effluent stream.
(ii) The alternative procedure will not significantly underestimate
the emissions.
(iii) The alternative procedure is fully documented.
(iv) The owner or operator has received prior approval from EPA.
(4)(i) Radionuclide emission measurements in conformance with the
requirements of paragraph (b) of this section shall be made at all
release points which have a potential to discharge radionuclides into
the air in quantities which could cause an effective dose equivalent in
excess of 1% of the standard. All radionuclides which could contribute
greater than 10% of the potential effective dose equivalent for a
release point shall be measured. For other release points which have a
potential to release radionuclides into the air, periodic confirmatory
measurements should be made to verify the low emissions.
(ii) To determine whether a release point is subject to the emission
measurement requirements of paragraph (b) of this section, it is
necessary to evaluate the potential for radionuclide emissions for that
release point. In evaluating the potential of a release point to
discharge radionuclides into the air, the estimated radionuclide release
rates shall be based on the discharge of the uncontrolled effluent
stream into the air.
(5) Environmental measurements of radionuclide air concentrations at
critical receptor locations may be used as an alternative to air
dispersion calculations in demonstrating compliance with the standards
if the owner or operator meets the following criteria:
(i) The air at the point of measurement shall be continuously sampled
for collection of radionuclides.
(ii) Those radionuclides released from the facility, which are the
major contributors to the effective dose equivalent must be collected
and measured as part of the environmental measurements program.
(iii) Radionuclide concentrations which would cause an effective dose
equivalent greater than or equal to 10% of the standard shall be readily
detectable and distinguishable from background.
(iv) Net measured radionuclide concentrations shall be compared to
the concentration levels in table 2 of appendix E to determine
compliance with the standard. In the case of multiple radionuclides
being released from a facility, compliance shall be demonstrated if the
value for all radionuclides is less than the concentration level in
table 2 and the sum of the fractions that result when each measured
concentration value is divided by the value in table 2 for each
radionuclide is less than 1.
(v) A quality assurance program shall be conducted that meets the
performance requirements described in appendix B, method 114.
(vi) Use of environmental measurements to demonstrate compliance with
the standard is subject to prior approval of EPA. Applications for
approval shall include a detailed description of the sampling and
analytical methodology and show how the above criteria will be met.
(c) The following facilities may use either the methodologies and
quality assurance programs described in paragraph (b) of this section or
may use the following:
(1) Nuclear power reactors may determine their radionuclide emissions
in conformance with the Effluent Technical Specifications contained in
their Operating License issued by the Nuclear Regulatory Commission. In
addition, they may conduct a quality assurance program as described in
the Nuclear Regulatory Commission's Regulatory Guide 4.15 dated February
1979.
(2) Fuel processing and fabrication plants and uranium hexafluoride
plants may determine their emissions in conformance with the Nuclear
Regulatory Commission's Regulatory Guide 4.16 dated December 1985. In
addition, they may conduct a quality assurance program as described in
the Nuclear Regulatory Commission's Regulatory Guide 4.15 dated February
1979.
(3) Uranium mills may determine their emissions in conformance with
the Nuclear Regulatory Commission's Regulatory Guide 4.14 dated April
1980. In addition, they may conduct a quality assurance program as
described in the Nuclear Regulatory Commission's Regulatory Guide 4.15
dated February 1979.
40 CFR 61.108 Exemption from the reporting and testing requirements of
40 CFR 61.10.
All facilities designated under this subpart are exempt from the
reporting requirements of 40 CFR 61.10.
40 CFR 61.109 Stay of effective date.
(a)The effective date for subpart I is stayed for each category of
facilities which are licensed by the Nuclear Regulatory Commission or by
an Agreement State, except for nuclear power reactors, until November
15, 1992, or until such earlier date that EPA is prepared to make an
initial determination under Clean Air Act section 112(d)(9) and conclude
its reconsideration under section 307(d)(7)(B). If EPA makes an initial
determination under Clean Air Act 112(d)(9) and concludes its
reconsideration under section 307(d)(7)(B) for any category of
NRC-licensed facilities other than nuclear power reactors prior to
November 15, 1992, it will publish its decision and any actions required
to effectuate that decision in the Federal Register.
(b) The effective date for subpart I is stayed for commercial nuclear
power reactors which are licensed by the Nuclear Regulatory Commission
until the date on which EPA takes final action concerning its proposal
to rescind subpart I for nuclear power reactors pursuant to section
112(d)(9) of the Clean Air Act, as published on August 5, 1991. EPA
will publish any such final action in the Federal Register.
(56 FR 18738, Apr. 24, 1991, as amended at 56 FR 37160, Aug. 5, 1991)
Effective Date Note: At 54 FR 51697, Dec. 15, 1989, 61.100
through 61.108, subpart I was revised and the effective date was stayed
until Mar. 15, 1990. At 55 FR 38057, Sept. 17, 1990, subpart I was
stayed until March 10, 1991. At 56 FR 10514, Mar. 13, 1991, the
effectiveness of subpart I for all NRC-licensed facilities other than
nuclear power reactors was stayed until April 15, 1991. At 56 FR 18738,
Apr. 24, 1991, the effectiveness for all facilities licensed by the NRC
or by an Agreement State, except for nuclear power reactors, was stayed
until November 15, 1992. For the convenience of the user the superseded
text appears below.
Subpart I -- National Emission Standard for Radionuclide Emissions
From Facilities Licensed by the Nuclear Regulatory Commission (NRC) and
Federal Facilities Not Covered by Subpart H
Source: 50 FR 5195, Feb. 5, 1985, unless otherwise noted.
Editorial Note: The information collection requirements in 61.107
and 61.108, added at 50 FR 5195, Feb. 5, 1985, have not been approved
by the Office of Management and Budget. Compliance with those
provisions is not required until approved by OMB. EPA will publish a
document in the Federal Register indicating the approval once it has
been obtained.
61.100 Designation of facilities.
The provisions of this subpart apply to NRC-licensed facilities and
to facilities owned or operated by any Federal agency other than the
Department of Energy that emit radionuclides to air. This subpart does
not apply to facilities regulated under 40 CFR parts 190, 191, or 192,
to any low energy accelerator, or to any user of the sealed radiation
sources.
61.101 Definitions.
(a) Agreement State means any State with which the Atomic Energy
Commission or the Nuclear Regulatory Commission has entered into an
effective agreement under subsection 274(b) of the Atomic Energy Act of
1954, as amended.
(b) Dose equivalent means the product of absorbed dose and
appropriate factors to account for differences in biological
effectiveness due to the quality of radiation and its distribution in
the body. The unit of dose equivalent is the rem.
(c) NRC-licensed facility means any facility licensed by the Nuclear
Regulatory Commission or any Agreement State to receive title to,
receive, possess, use, transfer, or deliver any source, byproduct, or
special nuclear material, except facilities regulated by 40 CFR parts
190, 191, or 192.
(d) Critical organ means the most exposed human organ or tissue
exclusive of the integumentary system (skin) and the cornea.
(e) Radionuclide means any nuclide that emits radiation. (A nuclide
is a species of atom characterized by the constitution of its nucleus
and hence by the number of protons, the number of neutrons, and the
energy content.)
(f) Whole body means all organs or tissues exclusive of the
integumentary system (skin) and the cornea.
(g) Effective dose equivalent means the sum of the products of the
dose equivalents to individual organs and tissues and appropriate
weighting factors representing the risk relative to that for an equal
dose to the whole body.
61.102 Emission standard.
Emissions of radionuclides to air from facilities subject to this
subpart shall not exceed those amounts that cause a dose equivalent of
25 mrem/y to the whole body or 75 mrem/y to the critical organ of any
member of the public. Doses due to radon-220, radon-222, and their
respective decay products are excluded from these limits.
61.103 Emission monitoring and compliance procedures.
To determine compliance with the standard, radionuclide emissions
shall be determined and dose equivalent to members of the public shall
be calculated using EPA-approved sampling procedures, EPA codes
AIRDOS-EPA and RADRISK, or other procedures, including those based on
environmental measurements, that EPA has determined to be suitable. In
most cases, compliance with this standard will be determined by
calculating the dose to members of the public at the point of maximum
annual air concentration in an unrestricted area where any member of the
public resides or abides.
List of approved procedures: (Reserved)
61.104 Reporting. (Reserved)
61.105 Recordkeeping. (Reserved)
61.106 Exemption from reporting and testing requirements of 40 CFR
61.10.
Facilities in possession of a radionuclide in annual quantities less
than the activity shown in Table 1 are exempt from the reporting
requirements of 40 CFR 61.10. If a facility possesses more than one
radionuclide, and the sum of the annual amount possessed divided by the
equivalent activity in Table 1 is summed for all radionuclides in
possession, and the sum is less than unity, then the facility is exempt
from the reporting requirements of 40 CFR 61.10. For radionuclides not
on this list, a facility may apply to the Administrator for an exemption
from the reporting requirements.
61.107 Waiver of compliance.
(a) To request a waiver, applicants shall follow the requirements of
61.10 (b)-(d).
(b) The following provisions also apply:
(1) the owner or operator of any existing source, or any new source
to which a standard prescribed under this part is applicable which had
an initial startup which preceded the effective date of a standard
prescribed under this part shall, within 90 days after the effective
date, provide the following information in writing to the Administrator:
(i) Name and address of the owner or operator.
(ii) The location of the source.
(iii) The types of radionuclides emitted by the stationary source and
the annual quantity (in Ci/y for the most recent calendar year) of each
radionuclide emitted.
(iv) A brief description of the nature, size, design, and method of
operation of the stationary source including the operating design
capacity of such source. Identify each point of emission for each
hazardous pollutant.
(v) Estimate of dose equivalent rate to the member of the public at
the point of maximum annual air concentration in an unrestricted area
where any member of the public resides or abides.
(vi) A description of the existing control equipment for each
emission point.
(A) Primary control device (s) for radionuclide emissions.
(B) Secondary control device(s) for radionuclide emissions.
(C) Estimated control efficiency (percent) for each control device.
(vii) A statement by the owner or operator of the source as to
whether he can comply with the standards prescribed in this part within
90 days of the effective date.
61.108 Alternative emission standard.
If a facility may exceed the emission standard established in
61.102, the operator may apply to EPA for an alternative emission
standard. The Administrator will review such applications and will
establish an appropriate alternative emission standard that will ensure
that no member of the public being exposed to emissions from the
facility receives a continuous exposure of more than 100 mrem/y
effective dose equivalent and a noncontinuous exposure of more than 500
mrem/y effective dose equivalent from all sources, excluding natural
background and medical procedures. The application shall include the
following:
(a) An assessment of the additional effective dose equivalents to the
member of the public receiving maximum exposure from the facility due to
all other sources. The natural radiation background shall be part of
this assessment.
(b) The information required in 61.107.
(c) The effective dose equivalent shall be calculated using the
following weighting factors:
Requests for alternative emission standards shall be sent to the
Assistant Administrator for Air and Radiation (ANR-443), U.S.
Environmental Protection Agency, 401 M Street SW., Washington, DC 20460.
This action shall be taken, for existing facilities by April 17, 1985.
40 CFR 61.109 Subpart J -- National Emission Standard for Equipment
Leaks (Fugitive Emission Sources) of Benzene
Source: 49 FR 23513, June 6, 1984, unless otherwise noted.
40 CFR 61.110 Applicability and designation of sources.
(a) The provisions of this subpart apply to each of the following
sources that are intended to operate in benzene service: pumps,
compressors, pressure relief devices, sampling connections, systems,
open-ended valves or lines, valves, flanges and other connectors,
product accumulator vessels, and control devices or systems required by
this subpart.
(b) The provisions of this subpart do not apply to sources located in
coke by-product plants.
(c)(1) If an owner or operator applies for one of the exemptions in
this paragraph, then the owner or operator shall maintain records as
required in 61.246(i).
(2) Any equipment in benzene service that is located at a plant site
designed to produce or use less than 1,000 megagrams of benzene per year
is exempt from the requirements of 61.112.
(3) Any process unit (defined in 61.241) that has no equipment in
benzene service is exempt from the requirements of 61.112.
(d) While the provisions of this subpart are effective, a source to
which this subpart applies that is also subject to the provisions of 40
CFR part 60 only will be required to comply with the provisions of this
subpart.
40 CFR 61.111 Definitions.
As used in this subpart, all terms not defined herein shall have the
meaning given them in the Act, in subpart A of part 61, or in subpart V
of part 61, and the following terms shall have the specific meanings
given them:
In benzene service means that a piece of equipment either contains or
contacts a fluid (Liquid or gas) that is at least 10 percent benzene by
weight as determined according to the provisions of 61.245(d). The
provisions of 61.245(d) also specify how to determine that a piece of
equipment is not in benzene service.
Semiannual means a 6-month period; the first semiannual period
concludes on the last day of the last month during the 180 days
following initial startup for new sources; and the first semiannual
period concludes on the last day of the last full month during the 180
days after June 6, 1984 for existing sources.
40 CFR 61.112 Standards.
(a) Each owner or operator subject to the provisions of this subpart
shall comply with the requirements of subpart V of this part.
(b) An owner or operator may elect to comply with the requirements of
61.243-1 and 61.243-2.
(c) An owner or operator may apply to the Administrator for a
determination of an alternative means of emission limitation that
achieves a reduction in emissions of benzene at least equivalent to the
reduction in emissions of benzene achieved by the controls required in
this subpart. In doing so, the owner or operator shall comply with
requirements of 61.244.
40 CFR 61.112 Subpart K -- National Emission Standards for Radionuclide
Emissions From Elemental Phosphorus Plants
Source: 54 FR 51699, Dec. 15, 1989, unless otherwise noted.
40 CFR 61.120 Applicability.
The provisions of this subpart are applicable to owners or operators
of calciners and nodulizing kilns at elemental phosphorus plants.
40 CFR 61.121 Definitions.
(a) Elemental phosphorus plant or plant means any facility that
processes phosphate rock to produce elemental phosphorus. A plant
includes all buildings, structures, operations, calciners and nodulizing
kilns on one contiguous site.
(b) Calciner or Nodulizing kiln means a unit in which phosphate rock
is heated to high temperatures to remove organic material and/or to
convert it to a nodular form. For the purpose of this subpart,
calciners and nodulizing kilns are considered to be similar units.
40 CFR 61.122 Emission standard.
Emissions of polonium-210 to the ambient air from all calciners and
nodulizing kilns at an elemental phosphorus plant shall not exceed a
total of 2 curies a year; except that compliance with this standard may
be conclusively shown if the elemental phosphorus plant:
(a) Installs a Hydro-Sonic# Tandem Nozzle Fixed Throat Free-Jet
Scrubber System including four scrubber units,
(b) All four scrubber units are operated continuously with a minimum
average over any 6-hour period of 40 inches (water column) of pressure
drop across each scrubber during calcining of phosphate shale,
(c) The system is used to scrub emissions from all calciners and/or
nodulizing kilns at the plant, and
(d) Total emissions of polonium-210 from the plant do not exceed 4.5
curies per year.
Alternative operating conditions, which can be shown to achieve an
overall removal efficiency for emissions of polonium-210 which is equal
to or greater than the efficiency which would be achieved under the
operating conditions described in paragraphs (a), (b), and (c) of this
section, may be used with prior approval of the Administrator. A
facility shall apply for such approval in writing, and the Administrator
shall act upon the request within 30 days after receipt of a complete
and technically sufficient application.
(56 FR 65943, Dec. 19, 1991)
40 CFR 61.123 Emission testing.
(a) Each owner or operator of an elemental phosphorus plant shall
test emissions from the plant within 90 days of the effective date of
this standard and annually thereafter. The Administrator may
temporarily or permanently waive the annual testing requirement or
increase the frequency of testing, if the Administrator determines that
more testing is required.
(b) The Administrator shall be notified at least 30 days prior to an
emission test so that EPA may, at its option, observe the test.
(c) An emission test shall be conducted at each operational calciner
or nodulizing kiln. If emissions from a calciner or nodulizing kiln are
discharged through more than one stack, then an emission test shall be
conducted at each stack and the total emission rate from the calciner or
kiln shall be the sum of the emission rates from each of the stacks.
(d) Each emission test shall consist of three sampling runs that meet
the requirements of 61.125. The phosphate rock processing rate during
each run shall be recorded. An emission rate in curies per metric ton
of phosphate rock processed shall be calculated for each run. The
average of all three runs shall apply in computing the emission rate for
the test. The annual polonium-210 emission rate from a calciner or
nodulizing kiln shall be determined by multiplying the measured
polonium-210 emission rate in curies per metric ton of phosphate rock
processed by the annual phosphate rock processing rate in metric tons.
In determining the annual phosphate rock processing rate, the values
used for operating hours and operating capacity shall be values that
will maximize the expected processing rate. For determining compliance
with the emission standard of 61.122, the total annual emission rate is
the sum of the annual emission rates for all operating calciners and
nodulizing kilns.
(e) If the owner or operator changes his operation in such a way as
to increase his emissions of polonium-210, such as changing the type of
rock processed, the temperature of the calciners or kilns, or increasing
the annual phosphate rock processing rate, then a new emission test,
meeting the requirements of this section, shall be conducted within 45
days under these conditions.
(f) Each owner or operator of an elemental phosphorus plant shall
furnish the Administrator with a written report of the results of the
emission test within 60 days of conducting the test. The report must
provide the following information:
(1) The name and location of the facility.
(2) The name of the person responsible for the operation of the
facility and the name of the person preparing the report (if different).
(3) A description of the effluent controls that are used on each
stack, vent, or other release point and an estimate of the efficiency of
each device.
(4) The results of the testing, including the results of each
sampling run completed.
(5) The values used in calculating the emissions and the source of
these data.
(6) Each report shall be signed and dated by a corporate officer in
charge of the facility and contain the following declaration immediately
above the signature line: ''I certify under penalty of law that I have
personally examined and am familiar with the information submitted
herein and based on my inquiry of those individuals immediately
responsible for obtaining the information, I believe that the submitted
information is true, accurate and complete. I am aware that there are
significant penalties for submitting false information including the
possibility of fine and imprisonment. See, 18 U.S.C. 1001.''
(Approved by the Office of Management and Budget under control number
2060-0191)
40 CFR 61.124 Recordkeeping requirements.
The owner or operator of any plant must maintain records documenting
the source of input parameters including the results of all measurements
upon which they are based, the calculations and/or analytical methods
used to derive values for input parameters, and the procedure used in
emission testing. This documentation should be sufficient to allow an
independent auditor to verify the accuracy of the results of the
emission testing. These records must be kept at the site of the plant
for at least five years and, upon request, be made available for
inspection by the Administrator, or his authorized representative.
40 CFR 61.125 Test methods and procedures.
(a) Each owner or operator of a source required to test emissions
under 61.123, unless an equivalent or alternate method has been
approved by the Administrator, shall use the following test methods:
(1) Test Method 1 of Appendix A to 40 CFR part 60 shall be used to
determine sample and velocity traverses;
(2) Test Method 2 of Appendix A to 40 CFR part 60 shall be used to
determine velocity and volumetric flow rate;
(3) Test Method 3 of Appendix A to 40 CFR part 60 shall be used for
gas analysis;
(4) Test Method 5 of Appendix A to 40 CFR part 60 shall be used to
collect particulate matter containing the polonium-210; and
(5) Test Method 111 of Appendix B to 40 CFR part 61 shall be used to
determine the polonium-210 emissions.
40 CFR 61.126 Monitoring of operations.
(a) The owner or operator of any source subject to this subpart using
a wet-scrubbing emission control device shall install, calibrate,
maintain, and operate a monitoring device for the continuous measurement
and recording of the pressure drop of the gas stream across each
scrubber. The monitoring device must be certified by the manufacturer
to be accurate within 250 pascal ( 1 inch of water). The owner or
operator of any source subject to this subpart using a wet-scrubbing
emission control device shall also install, calibrate, maintain, and
operate a monitoring device for the continuous measurement and recording
of the scrubber fluid flow rate. These continuous measurement
recordings shall be maintained at the source and made available for
inspection by the Administrator, or his authorized representative, for a
minimum of 5 years.
(b) The owner or operator of any source subject to this subpart using
an electrostatic precipitator control device shall install, calibrate,
maintain, and operate a monitoring device for the continuous measurement
and recording of the primary and secondary current and the voltage in
each electric field. These continuous measurement recordings shall be
maintained at the source and made available for inspection by the
Administrator, or his authorized representative, for a minimum of 5
years.
(56 FR 65943, Dec. 19, 1991)
40 CFR 61.127 Exemption from the reporting and testing requirements of
40 CFR 61.10.
All facilities designated under this subpart are exempt from the
reporting requirements of 40 CFR 61.10.
40 CFR 61.127 Subpart L -- National Emission Standard for Benzene
Emissions from Coke By-Product Recovery Plants
Source: 54 FR 38073, Sept. 14, 1989, unless otherwise noted.
40 CFR 61.130 Applicability, designation of sources, and delegation of
authority.
(a) The provisions of this subpart apply to each of the following
sources at furnace and foundry coke by-product recovery plants: tar
decanters, tar storage tanks, tar-intercepting sumps, flushing-liquor
circulation tanks, light-oil sumps, light-oil condensers, light-oil
decanters, wash-oil decanters, wash-oil circulation tanks, naphthalene
processing, final coolers, final-cooler cooling towers, and the
following equipment that are intended to operate in benzene service:
pumps, valves, exhausters, pressure relief devices, sampling connection
systems, open-ended valves or lines, flanges or other connectors, and
control devices or systems required by 61.135.
(b) The provisions of this subpart also apply to benzene storage
tanks, BTX storage tanks, light-oil storage tanks, and excess
ammonia-liquor storage tanks at furnace coke by-product recovery plants.
(c) In delegating implementation and enforcement authority to a State
under section 112 of the Act, the authorities contained in paragraph (d)
of this section shall be retained by the Administrator and not
transferred to a State.
(d) Authorities that will not be delegated to States: 61.136(d).
(54 FR 51699, Dec. 15, 1989, as amended at 56 FR 47406, Sept. 19,
1991)
40 CFR 61.131 Definitions.
As used in this subpart, all terms not defined herein shall have the
meaning given them in the Act, in subpart A of part 61, and in subpart V
of part 61. The following terms shall have the specific meanings given
them:
Annual coke production means the coke produced in the batteries
connected to the coke by-product recovery plant over a 12-month period.
The first 12-month period concludes on the first December 31 that comes
at least 12 months after the effective date or after the date of initial
startup if initial startup is after the effective date.
Benzene storage tank means any tank, reservoir, or container used to
collect or store refined benzene.
BTX storage tank means any tank, reservoir, or container used to
collect or store benzene-toluene-xylene or other light-oil fractions.
Car seal means a seal that is placed on the device used to change the
position of a valve (e.g., from open to closed) such that the position
of the valve cannot be changed without breaking the seal and requiring
the replacement of the old seal, once broken, with a new seal.
Coke by-product recovery plant means any plant designed and operated
for the separation and recovery of coal tar derivatives (by-products)
evolved from coal during the coking process of a coke oven battery.
Equipment means each pump, valve, exhauster, pressure relief device,
sampling connection system, open-ended valve or line, and flange or
other connector in benzene service.
Excess ammonia-liquor storage tank means any tank, reservoir, or
container used to collect or store a flushing liquor solution prior to
ammonia or phenol recovery.
Exhauster means a fan located between the inlet gas flange and outlet
gas flange of the coke oven gas line that provides motive power for coke
oven gases.
Foundry coke means coke that is produced from raw materials with less
than 26 percent volatile material by weight and that is subject to a
coking period of 24 hours or more. Percent volatile material of the raw
materials (by weight) is the weighted average percent volatile material
of all raw materials (by weight) charged to the coke oven per coking
cycle.
Foundry coke by-product recovery plant means a coke by-product
recovery plant connected to coke batteries whose annual coke production
is at least 75 percent foundry coke.
Flushing-liquor circulation tank means any vessel that functions to
store or contain flushing liquor that is separated from the tar in the
tar decanter and is recirculated as the cooled liquor to the gas
collection system.
Furnace coke means coke produced in by-product ovens that is not
foundry coke.
Furnace coke by-product recovery plant means a coke by-product
recovery plant that is not a foundry coke by-product recovery plant.
In benzene service means a piece of equipment, other than an
exhauster, that either contains or contacts a fluid (liquid or gas) that
is at least 10 percent benzene by weight or any exhauster that either
contains or contacts a fluid (liquid or gas) at least 1 percent benzene
by weight as determined by the provisions of 61.137(b). The provisions
of 61.137(b) also specify how to determine that a piece of equipment is
not in benzene service.
Light-oil condenser means any unit in the light-oil recovery
operation that functions to condense benzene-containing vapors.
Light-oil decanter means any vessel, tank, or other type of device in
the light-oil recovery operation that functions to separate light oil
from water downstream of the light-oil condenser. A light-oil decanter
also may be known as a light-oil separator.
Light-oil storage tank means any tank, reservoir, or container used
to collect or store crude or refined light-oil.
Light-oil sump means any tank, pit, enclosure, or slop tank in
light-oil recovery operations that functions as a wastewater separation
device for hydrocarbon liquids on the surface of the water.
Naphthalene processing means any operations required to recover
naphthalene including the separation, refining, and drying of crude or
refined naphthalene.
Non-regenerative carbon adsorber means a series, over time, of
non-regenerative carbon beds applied to a single source or group of
sources, where non-regenerative carbon beds are carbon beds that are
either never regenerated or are moved from their location for
regeneration.
Process vessel means each tar decanter, flushing-liquor circulation
tank, light-oil condenser, light-oil decanter, wash-oil decanter, or
wash-oil circulation tank.
Regenerative carbon adsorber means a carbon adsorber applied to a
single source or group of sources, in which the carbon beds are
regenerated without being moved from their location.
Semiannual means a 6-month period; the first semiannual period
concludes on the last day of the last full month during the 180 days
following initial startup for new sources; the first semiannual period
concludes on the last day of the last full month during the 180 days
after the effective date of the regulation for existing sources.
Tar decanter means any vessel, tank, or container that functions to
separate heavy tar and sludge from flushing liquor by means of gravity,
heat, or chemical emulsion breakers. A tar decanter also may be known
as a flushing-liquor decanter.
Tar storage tank means any vessel, tank, reservoir, or other type of
container used to collect or store crude tar or tar-entrained
naphthalene, except for tar products obtained by distillation, such as
coal tar pitch, creosotes, or carbolic oil. This definition also
includes any vessel, tank, reservoir, or container used to reduce the
water content of the tar by means of heat, residence time, chemical
emulsion breakers, or centrifugal separation. A tar storage tank also
may be known as a tar-dewatering tank.
Tar-intercepting sump means any tank, pit, or enclosure that serves
to receive or separate tars and aqueous condensate discharged from the
primary cooler. A tar-intercepting sump also may be known as a
primary-cooler decanter.
Vapor incinerator means any enclosed combustion device that is used
for destroying organic compounds and does not necessarily extract energy
in the form of steam or process heat.
Wash-oil circulation tank means any vessel that functions to hold the
wash oil used in light-oil recovery operations or the wash oil used in
the wash-oil final cooler.
Wash-oil decanter means any vessel that functions to separate, by
gravity, the condensed water from the wash oil received from a wash-oil
final cooler or from a light-oil scrubber.
(54 FR 38073, Sept. 14, 1989, as amended at 56 FR 47406, Sept. 19,
1991)
40 CFR 61.132 Standard: Process vessels, storage tanks, and
tar-intercepting sumps.
(a)(1) Each owner or operator of a furnace or a foundry coke
byproduct recovery plant shall enclose and seal all openings on each
process vessel, tar storage tank, and tar-intercepting sump.
(2) The owner or operator shall duct gases from each process vessel,
tar storage tank, and tar-intercepting sump to the gas collection
system, gas distribution system, or other enclosed point in the
by-product recovery process where the benzene in the gas will be
recovered or destroyed. This control system shall be designed and
operated for no detectable emissions, as indicated by an instrument
reading of less than 500 ppm above background and visual inspections, as
determined by the methods specified in 61.245(c). This system can be
designed as a closed, positive pressure, gas blanketing system.
(i) Except, the owner or operator may elect to install, operate, and
maintain a pressure relief device, vacuum relief device, an access
hatch, and a sampling port on each process vessel, tar storage tank, and
tar-intercepting sump. Each access hatch and sampling port must be
equipped with a gasket and a cover, seal, or lid that must be kept in a
closed position at all times, unless in actual use.
(ii) The owner or operator may elect to leave open to the atmosphere
the portion of the liquid surface in each tar decanter necessary to
permit operation of a sludge conveyor. If the owner or operator elects
to maintain an opening on part of the liquid surface of the tar
decanter, the owner or operator shall install, operate, and maintain a
water leg seal on the tar decanter roof near the sludge discharge chute
to ensure enclosure of the major portion of liquid surface not necessary
for the operation of the sludge conveyor.
(b) Following the installation of any control equipment used to meet
the requirements of paragraph (a) of this section, the owner or operator
shall monitor the connections and seals on each control system to
determine if it is operating with no detectable emissions, using
Reference Method 21 (40 CFR part 60, appendix A) and procedures
specified in 61.245(c), and shall visually inspect each source
(including sealing materials) and the ductwork of the control system for
evidence of visible defects such as gaps or tears. This monitoring and
inspection shall be conducted on a semiannual basis and at any other
time after the control system is repressurized with blanketing gas
following removal of the cover or opening of the access hatch.
(1) If an instrument reading indicates an organic chemical
concentration more than 500 ppm above a background concentration, as
measured by Reference Method 21, a leak is detected.
(2) If visible defects such as gaps in sealing materials are observed
during a visual inspection, a leak is detected.
(3) When a leak is detected, it shall be repaired as soon as
practicable, but not later than 15 calendar days after it is detected.
(4) A first attempt at repair of any leak or visible defect shall be
made no later than 5 calendar days after each leak is detected.
(c) Following the installation of any control system used to meet the
requirements of paragraph (a) of this section, the owner or operator
shall conduct a maintenance inspection of the control system on an
annual basis for evidence of system abnormalities, such as blocked or
plugged lines, sticking valves, plugged condensate traps, and other
maintenance defects that could result in abnormal system operation. The
owner or operator shall make a first attempt at repair within 5 days,
with repair within 15 days of detection.
(d) Each owner or operator of a furnace coke by-product recovery
plant also shall comply with the requirements of paragraphs (a)-(c) of
this section for each benzene storage tank, BTX storage tank, light-oil
storage tank, and excess ammonia-liquor storage tank.
40 CFR 61.133 Standard: Light-oil sumps.
(a) Each owner or operator of a light-oil sump shall enclose and seal
the liquid surface in the sump to form a closed system to contain the
emissions.
(1) Except, the owner or operator may elect to install, operate, and
maintain a vent on the light-oil sump cover. Each vent pipe must be
equipped with a water leg seal, a pressure relief device, or vacuum
relief device.
(2) Except, the owner or operator may elect to install, operate, and
maintain an access hatch on each light-oil sump cover. Each access
hatch must be equipped with a gasket and a cover, seal, or lid that must
be kept in a closed position at all times, unless in actual use.
(3) The light-oil sump cover may be removed for periodic maintenance
but must be replaced (with seal) at completion of the maintenance
operation.
(b) The venting of steam or other gases from the by-product process
to the light-oil sump is not permitted.
(c) Following the installation of any control equipment used to meet
the requirements of paragraph (a) of this section, the owner or operator
shall monitor the connections and seals on each control system to
determine if it is operating with no detectable emissions, using
Reference Method 21 (40 CFR part 60, appendix A) and the procedures
specified in 61.245(c), and shall visually inspect each source
(including sealing materials) for evidence of visible defects such as
gaps or tears. This monitoring and inspection shall be conducted
semiannually and at any other time the cover is removed.
(1) If an instrument reading indicates an organic chemical
concentration more than 500 ppm above a background concentration, as
measured by Reference Method 21, a leak is detected.
(2) If visible defects such as gaps in sealing materials are observed
during a visual inspection, a leak is detected.
(3) When a leak is detected, it shall be repaired as soon as
practicable, but not later than 15 calendar days after it is detected.
(4) A first attempt at repair of any leak or visible defect shall be
made no later than 5 calendar days after each leak is detected.
40 CFR 61.134 Standard: Naphthalene processing, final coolers, and
final-cooler cooling towers.
(a) No (''zero'') emissions are allowed from naphthalene processing,
final coolers and final-cooler cooling towers at coke by-product
recovery plants.
40 CFR 61.135 Standard: Equipment leaks.
(a) Each owner or operator of equipment in benzene service shall
comply with the requirements of 40 CFR 61, subpart V, except as provided
in this section.
(b) The provisions of 61.242-3 and 61.242-9 of subpart V do not
apply to this subpart.
(c) Each piece of equipment in benzene service to which this subpart
applies shall be marked in such a manner that it can be distinguished
readily from other pieces of equipment in benzene service.
(d) Each exhauster shall be monitored quarterly to detect leaks by
the methods specified in 61.245(b) except as provided in 61.136(d) and
paragraphs (e)-(g) of this section.
(1) If an instrument reading of 10,000 ppm or greater is measured, a
leak is detected.
(2) When a leak is detected, it shall be repaired as soon as
practicable, but no later than 15 calendar days after it is detected,
except as provided in 61.242-10 (a) and (b). A first attempt at repair
shall be made no later than 5 calendar days after each leak is detected.
(e) Each exhauster equipped with a seal system that includes a
barrier fluid system and that prevents leakage of process fluids to the
atmosphere is exempt from the requirements of paragraph (d) of this
section provided the following requirements are met:
(1) Each exhauster seal system is:
(i) Operated with the barrier fluid at a pressure that is greater
than the exhauster stuffing box pressure; or
(ii) Equipped with a barrier fluid system that is connected by a
closed vent system to a control device that complies with the
requirements of 61.242-11; or
(iii) Equipped with a system that purges the barrier fluid into a
process stream with zero benzene emissions to the atmosphere.
(2) The barrier fluid is not in benzene service.
(3) Each barrier fluid system shall be equipped with a sensor that
will detect failure of the seal system, barrier fluid system, or both.
(4)(i) Each sensor as described in paragraph (e)(3) of this section
shall be checked daily or shall be equipped with an audible alarm.
(ii) The owner or operator shall determine, based on design
considerations and operating experience, a criterion that indicates
failure of the seal system, the barrier fluid system, or both.
(5) If the sensor indicates failure of the seal system, the barrier
system, or both (based on the criterion determined under paragraph
(e)(4)(ii) of this section), a leak is detected.
(6)(i) When a leak is detected, it shall be repaired as soon as
practicable, but not later than 15 calendar days after it is detected,
except as provided in 61.242-10.
(ii) A first attempt at repair shall be made no later than 5 calendar
days after each leak is detected.
(f) An exhauster is exempt from the requirements of paragraph (d) of
this section if it is equipped with a closed vent system capable of
capturing and transporting any leakage from the seal or seals to a
control device that complies with the requirements of 61.242-11 except
as provided in paragraph (g) of this section.
(g) Any exhauster that is designated, as described in 61.246(e) for
no detectable emissions, as indicated by an instrument reading of less
than 500 ppm above background, is exempt from the requirements of
paragraph (d) of this section if the exhauster:
(1) Is demonstrated to be operating with no detectable emissions, as
indicated by an instrument reading of less than 500 ppm above
background, as measured by the methods specified in 61.245(c); and
(2) Is tested for compliance with paragraph (g)(1) of this section
initially upon designation, annually, and at other times requested by
the Administrator.
(h) Any exhauster that is in vacuum service is excluded from the
requirements of this subpart if it is identified as required in
61.246(e)(5).
40 CFR 61.136 Compliance provisions and alternative means of emission
limitation.
(a) Each owner or operator subject to the provisions of this subpart
shall demonstrate compliance with the requirements of 61.132 through
61.135 for each new and existing source, except as provided under
61.243-1 and 61.243-2.
(b) Compliance with this subpart shall be determined by a review of
records, review of performance test results, inspections, or any
combination thereof, using the methods and procedures specified in
61.137.
(c) On the first January 1 after the first year that a plant's annual
coke production is less than 75 percent foundry coke, the coke
by-product recovery plant becomes a furnace coke by-product recovery
plant and shall comply with 61.132(d). Once a plant becomes a furnace
coke by-product recovery plant, it will continue to be considered a
furnace coke by-product recovery plant, regardless of the coke
production in subsequent years.
(d)(1) An owner or operator may request permission to use an
alternative means of emission limitation to meet the requirements in
61.132, 61.133, and 61.135 of this subpart and 61.242-2, -5, -6, -7,
-8, and -11 of subpart V. Permission to use an alternative means of
emission limitation shall be requested as specified in 61.12(d).
(2) When the Administrator evaluates requests for permission to use
alternative means of emission limitation for sources subject to 61.132
and 61.133 (except tar decanters) the Administrator shall compare test
data for the means of emission limitation to a benzene control
efficiency of 98 percent. For tar decanters, the Administrator shall
compare test data for the means of emission limitation to a benzene
control efficiency of 95 percent.
(3) For any requests for permission to use an alternative to the work
practices required under 61.135, the provisions of 61.244(c) shall
apply.
40 CFR 61.137 Test methods and procedures.
(a) Each owner or operator subject to the provisions of this subpart
shall comply with the requirements in 61.245 of 40 CFR part 61, subpart
V.
(b) To determine whether or not a piece of equipment is in benzene
service, the methods in 61.245(d) shall be used, except that, for
exhausters, the percent benzene shall be 1 percent by weight, rather
than the 10 percent by weight described in 61.245(d).
40 CFR 61.138 Recordkeeping and reporting requirements.
(a) The following information pertaining to the design of control
equipment installed to comply with 61.132 through 61.134 shall be
recorded and kept in a readily accessible location:
(1) Detailed schematics, design specifications, and piping and
instrumentation diagrams.
(2) The dates and descriptions of any changes in the design
specifications.
(b) The following information pertaining to sources subject to
61.132 and sources subject to 61.133 shall be recorded and maintained
for 2 years following each semiannual (and other) inspection and each
annual maintenance inspection:
(1) The date of the inspection and the name of the inspector.
(2) A brief description of each visible defect in the source or
control equipment and the method and date of repair of the defect.
(3) The presence of a leak, as measured using the method described in
61.245(c). The record shall include the date of attempted and actual
repair and method of repair of the leak.
(4) A brief description of any system abnormalities found during the
annual maintenance inspection, the repairs made, the date of attempted
repair, and the date of actual repair.
(c) Each owner or operator of a source subject to 61.135 shall
comply with 61.246.
(d) For foundry coke by-product recovery plants, the annual coke
production of both furnace and foundry coke shall be recorded and
maintained for 2 years following each determination.
(e)(1) An owner or operator of any source to which this subpart
applies shall submit a statement in writing notifying the Administrator
that the requirements of this subpart and 40 CFR 61, subpart V, have
been implemented.
(2) In the case of an existing source or a new source that has an
initial startup date preceding the effective date, the statement is to
be submitted within 90 days of the effective date, unless a waiver of
compliance is granted under 61.11, along with the information required
under 61.10. If a waiver of compliance is granted, the statement is to
be submitted on a date scheduled by the Administrator.
(3) In the case of a new source that did not have an initial startup
date preceding the effective date, the statement shall be submitted with
the application for approval of construction, as described under 61.07.
(4) The statement is to contain the following information for each
source:
(i) Type of source (e.g., a light-oil sump or pump).
(ii) For equipment in benzene service, equipment identification
number and process unit identification: percent by weight benzene in
the fluid at the equipment; and process fluid state in the equipment
(gas/vapor or liquid).
(iii) Method of compliance with the standard (e.g., ''gas
blanketing,'' ''monthly leak detection and repair,'' or ''equipped with
dual mechanical seals''). This includes whether the plant plans to be a
furnace or foundry coke by-product recovery plant for the purposes of
61.132(d).
(f) A report shall be submitted to the Administrator semiannually
starting 6 months after the initial reports required in 61.138(e) and
61.10, which includes the following information:
(1) For sources subject to 61.132 and sources subject to 61.133,
(i) A brief description of any visible defect in the source or
ductwork,
(ii) The number of leaks detected and repaired, and
(iii) A brief description of any system abnormalities found during
each annual maintenance inspection that occurred in the reporting period
and the repairs made.
(2) For equipment in benzene service subject to 61.135(a),
information required by 61.247(b).
(3) For each exhauster subject to 61.135 for each quarter during the
semiannual reporting period,
(i) The number of exhausters for which leaks were detected as
described in 61.135 (d) and (e)(5),
(ii) The number of exhausters for which leaks were repaired as
required in 61.135 (d) and (e)(6),
(iii) The results of performance tests to determine compliance with
61.135(g) conducted within the semiannual reporting period.
(4) A statement signed by the owner or operator stating whether all
provisions of 40 CFR part 61, subpart L, have been fulfilled during the
semiannual reporting period.
(5) For foundry coke by-product recovery plants, the annual coke
production of both furnace and foundry coke, if determined during the
reporting period.
(6) Revisions to items reported according to paragraph (e) of this
section if changes have occurred since the initial report or subsequent
revisions to the initial report.
Note: Compliance with the requirements of 61.10(c) is not required
for revisions documented under this paragraph.
(g) In the first report submitted as required in 61.138(e), the
report shall include a reporting schedule stating the months that
semiannual reports shall be submitted. Subsequent reports shall be
submitted according to that schedule unless a revised schedule has been
submitted in a previous semiannual report.
(h) An owner or operator electing to comply with the provisions of
61.243-1 and 61.243-2 shall notify the Administrator of the alternative
standard selected 90 days before implementing either of the provisions.
(i) An application for approval of construction or modification, as
required under 61.05(a) and 61.07, will not be required for sources
subject to 61.135 if:
(1) The new source complies with 61.135, and
(2) In the next semiannual report required by 61.138(f), the
information described in 61.138(e)(4) is reported.
(Approved by the Office of Management and Budget under control number
2060-0185)
(55 FR 38073, Sept. 14, 1990; 55 FR 14037, Apr. 13, 1990)
40 CFR 61.139 Provisions for alternative means for process vessels,
storage tanks, and tar-intercepting sumps.
(a) As an alternative means of emission limitation for a source
subject to 61.132(a)(2) or 61.132(d), the owner or operator may route
gases from the source through a closed vent system to a carbon adsorber
or vapor incinerator that is at least 98 percent efficient at removing
benzene from the gas stream.
(1) The provisions of 61.132(a)(1) and 61.132(a) (2)(i) and (ii)
shall apply to the source.
(2) The seals on the source and closed vent system shall be designed
and operated for no detectable emissions, as indicated by an instrument
reading of less than 500 ppm above background and visual inspections, as
determined by the methods specified in 61.245(c).
(3) The provisions of 61.132(b) shall apply to the seals and closed
vent system.
(b) For each carbon adsorber, the owner or operator shall adhere to
the following practices:
(1) Benzene captured by each carbon adsorber shall be recycled or
destroyed in a manner that prevents benzene from being emitted to the
atmosphere.
(2) Carbon removed from each carbon adsorber shall be regenerated or
destroyed in a manner that prevents benzene from being emitted to the
atmosphere.
(3) For each regenerative carbon adsorber, the owner or operator
shall initiate regeneration of the spent carbon bed and vent the
emissions from the source to a regenerated carbon bed no later than when
the benzene concentration or organic vapor concentration level in the
adsorber outlet vent reaches the maximum concentration point, as
determined in 61.139(h).
(4) For each non-regenerative carbon adsorber, the owner or operator
shall replace the carbon at the scheduled replacement time, or as soon
as practicable (but not later than 16 hours) after an exceedance of the
maximum concentration point is detected, whichever is sooner.
(i) For each non-regenerative carbon adsorber, the scheduled
replacement time means the day that is estimated to be 90 percent of the
demonstrated bed life, as defined in 61.139(h)(5).
(ii) For each non-regenerative carbon adsorber, an exceedance of the
maximum concentration point shall mean any concentration greater than or
equal to the maximum concentration point as determined in 61.139(h).
(c) Compliance with the provisions of this section shall be
determined as follows:
(1) For each carbon adsorber and vapor incinerator, the owner or
operator shall demonstrate compliance with the efficiency limit by a
compliance test as specified in 61.13 and 61.139(g). If a waiver of
compliance has been granted under 61.11, the deadline for conducting
the initial compliance test shall be incorporated into the terms of the
waiver. The benzene removal efficiency rate for each carbon adsorber
and vapor incinerator shall be calculated as in the following equation:
Where:
E=percent removal of benzene.
Caj=concentration of benzene in vents after the control device, parts
per million (ppm).
Cbi=concentration of benzene in vents before the control device, ppm.
Qaj=volumetric flow rate in vents after the control device, standard
cubic meters/minute (scm/min).
Qbi=volumetric flow rate in vents before the control device, scm/min.
m=number of vents after the control device.
n=number of vents after the control device.
(c) Compliance with all other provisions in this section shall be
determined by inspections or the review of records and reports.
(d) For each regenerative carbon adsorber, the owner or operator
shall install and operate a monitoring device that continuously
indicates and records either the concentration of benzene or the
concentration level of organic compounds in the outlet vent of the
carbon adsorber. The monitoring device shall be installed, calibrated,
maintained and operated in accordance with the manufacturer's
specifications.
(1) Measurement of benzene concentration shall be made according to
61.139(g)(2).
(2) All measurements of organic compound concentration levels shall
be reasonable indicators of benzene concentration.
(i) The monitoring device for measuring organic compound
concentration levels shall be based on one of the following detection
principles: Infrared absorption, flame ionization, catalytic oxidation,
photoionization, or thermal conductivity.
(ii) The monitoring device shall meet the requirements of part 60,
appendix A, method 21, sections 2, 3, 4.1, 4.2, and 4.4. For the purpose
of the application of method 21 to this section, the words ''leak
definition'' shall be the maximum concentration point, which would be
estimated until it is established under 61.139(h). The calibration gas
shall either be benzene or methane and shall be at a concentration
associated with 125 percent of the expected organic compound
concentration level for the carbon adsorber outlet vent.
(e) For each non-regenerative carbon adsorber, the owner or operator
shall monitor either the concentration of benzene or the concentration
level of organic compounds at the outlet vent of the adsorber. The
monitoring device shall be calibrated, operated and maintained in
accordance with the manufacturer's specifications.
(1) Measurements of benzene concentration shall be made according to
61.139(g)(2). The measurement shall be conducted over at least one
5-minute interval during which flow into the carbon adsorber is expected
to occur.
(2) All measurements of organic compound concentration levels shall
be reasonable indicators of benzene concentration.
(i) The monitoring device for measuring organic compound
concentration levels shall meet the requirements of paragraphs
61.139(d)(2) (i) and (ii).
(ii) The probe inlet of the monitoring device shall be placed at
approximately the center of the carbon adsorber outlet vent. The probe
shall be held there for at least 5 minutes during which flow into the
carbon adsorber is expected to occur. The maximum reading during that
period shall be used as the measurement.
(3) Monitoring shall be performed at least once within the first 7
days after replacement of the carbon bed occurs, and monthly thereafter
until 10 days before the scheduled replacement time, at which point
monitoring shall be done daily, except as specified in paragraphs (e)(4)
and (e)(5) of this section.
(4) If an owner or operator detects an exceedance of the maximum
concentration point during the monthly monitoring or on the first day of
daily monitoring as prescribed in paragraph (e)(3) of this section,
then, after replacing the bed, the owner or operator shall begin the
daily monitoring of the replacement carbon bed on the day after the last
scheduled monthly monitoring before the exceedance was detected, or 10
days before the exceedance was detected, whichever is longer.
(5) If an owner or operator detects an exceedance of the maximum
concentration point during the daily monitoring as prescribed in
paragraph (e)(3) of this section, except on the first day, then, after
replacing the bed, the owner or operator shall begin the daily
monitoring of the replacement carbon bed 10 days before the exceedance
was detected.
(6) If the owner or operator is monitoring on the schedule required
in paragraph (e)(4) or paragraph (e)(5) of this section, and the
scheduled replacement time is reached without exceeding the maximum
concentration point, the owner or operator may return to the monitoring
schedule in paragraph (e)(3) of this section for subsequent carbon beds.
Note: This note provides an example of the monitoring schedules in
paragraphs (e)(3), (e)(4) and (e)(5) of this section. Assume that the
scheduled replacement time for a non-regenerative carbon adsorber is the
105th day after installation. According to the monitoring schedule in
paragraph (e)(3) of this section, initial monitoring would be done
within 7 days after installation, monthly monitoring would be done on
the 30th, 60th and 90th days, and daily monitoring would begin on the
95th day after installation. Now assume that an exceedance of the
maximum concentration point is detected on the 90th day after
installation. On the replacement carbon bed, the owner or operator
would begin daily monitoring on the 61st day after installation (i.e.,
the day after the last scheduled monthly monitoring before the
exceedance was detected), according to the requirements in paragraph
(e)(4) of this section. If, instead, the exceedance were detected on
the first bed on the 95th day, the daily monitoring of the replacement
bed would begin on the 85th day after installation (i.e., 10 days before
the point in the cycle where the exceedance was detected); this is a
second example of the requirements in paragraph (e)(4) of this section.
Finally, assume that an exceedance of the maximum concentration point is
detected on the 100th day after the first carbon adsorber was installed.
According to paragraph (e)(5) of this section, daily monitoring of the
replacement bed would begin on the 90th day after installation (i.e., 10
days earlier than when the exceedance was detected on the previous bed).
In all of these examples, the initial monitoring of the replacement bed
within 7 days of installation and the monthly monitoring would proceed
as set out in paragraph (e)(3) of this section until daily monitoring
was required.
(f) For each vapor incinerator, the owner or operator shall comply
with the monitoring requirements specified below:
(1) Install, calibrate, maintain, and operate according to the
manufacturer's specifications a temperature monitoring device equipped
with a continuous recorder and having an accuracy of 1 percent of the
temperature being monitored expressed in degrees Celsius or 0.5 C,
whichever is greater.
(i) Where a vapor incinerator other than a catalytic incinerator is
used, the temperature monitoring device shall be installed in the
firebox.
(ii) Where a catalytic incinerator is used, temperature monitoring
devices shall be installed in the gas stream immediately before and
after the catalyst bed.
(2) Comply with paragraph (f)(2)(i), paragraph (f)(2)(ii), or
paragraph (f)(3)(iii) of this section.
(i) Install, calibrate, maintain and operate according to the
manufacturer's specifications a flow indicator that provides a record of
vent stream flow to the incinerator at least once every hour for each
source. The flow indicator shall be installed in the vent stream from
each source at a point closest to the inlet of each vapor incinerator
and before being joined with any other vent stream.
(ii) Install, calibrate, maintain and operate according to the
manufacturer's specifications a flow indicator that provides a record of
vent stream flow away from the vapor incinerator at least once every 15
minutes. The flow indicator shall be installed in each bypass line,
immediately downstream of the valve that, if opened, would divert the
vent stream away from the vapor incinerator.
(iii) Where a valve that opens a bypass line is secured in the closed
position with a car seal or a lock-and-key configuration, a flow
indicator is not required. The owner or operator shall perform a visual
inspection at least once every month to check the position of the valve
and the condition of the car seal or lock-and-key configuration. The
owner or operator shall also record the date and duration of each time
that the valve was opened and the vent stream diverted away from the
vapor incinerator.
(g) In conducting the compliance tests required in 61.139(c), and
measurements specified in 61.139(d)(1), (e)(1) and (h)(3)(ii), the
owner or operator shall use as reference methods the test methods and
procedures in appendix A to 40 CFR part 60, or other methods as
specified in this paragraph, except as specified in 61.13.
(1) For compliance tests, as described in 61.139(c)(1), the
following provisions apply.
(i) All tests shall be run under representative emission
concentration and vent flow rate conditions. For sources with
intermittent flow rates, representative conditions shall include typical
emission surges (for example, during the loading of a storage tank).
(ii) Each test shall consist of three separate runs. These runs will
be averaged to yield the volumetric flow rates and benzene
concentrations in the equation in 61.139(c)(1). Each run shall be a
minimum of 1 hour.
(A) For each regenerative carbon adsorber, each run shall take place
in one adsorption cycle, to include a minimum of 1 hour of sampling
immediately preceding the initiation of carbon bed regeneration.
(B) For each non-regenerative carbon adsorber, all runs can occur
during one adsorption cycle.
(iii) The measurements during the runs shall be paired so that the
inlet and outlet to the control device are measured simultaneously.
(iv) Method 1 or 1A shall be used as applicable for locating
measurement sites.
(v) Method 2, 2A, or 2D shall be used as applicable for measuring
vent flow rates.
(vi) Method 18 shall be used for determining the benzene
concentrations (Caj and Cbi). Either follow section 7.1, ''Integrated
Bag Sampling and Analysis,'' or section 7.2, ''Direct Interface Sampling
and Analysis Procedure.'' A separation column constructed of stainless
steel, 1.83 m by 3.2 mm, containing 10 percent 1,2,3-tris
(2-cyanoethoxy) propane (TECP) on 80/100 mesh Chromosorb P AW, with a
column temperature of 80 C, a detector temperature of 225 C, and a
flow rate of approximately 20 ml/min, may produce adequate separations.
The analyst can use other columns, provided that the precision and
accuracy of the analysis of benzene standards is not impaired. The
analyst shall have available for review information confirming that
there is adequate resolution of the benzene peak.
(A) If section 7.1 is used, the sample rate shall be adjusted to
maintain a constant proportion to vent flow rate.
(B) If section 7.2 is used, then each performance test run shall be
conducted in intervals of 5 minutes. For each interval ''t,'' readings
from each measurement shall be recorded, and the flow rate (Qaj or Qbi)
and the corresponding benzene concentration (Caj or Cbi) shall be
determined. The sampling system shall be constructed to include a
mixing chamber of a volume equal to 5 times the sampling flow rate per
minute. Each analysis performed by the chromatograph will then
represent an averaged emission value for a 5-minute time period. The
vent flow rate readings shall be timed to account for the total sample
system residence time. A dual column, dual detector chromatograph can
be used to achieve an analysis interval of 5 minutes. The individual
benzene concentrations shall be vent flow rate weighted to determine
sample run average concentrations. The individual vent flow rates shall
be time averaged to determine sample run average flow rates.
(2) For testing the benzene concentration at the outlet vent of the
carbon adsorber as specified under 61.139(d)(1), (e)(1) and
(h)(3)(ii), the following provisions apply.
(i) The measurement shall be conducted over one 5-minute period.
(ii) The requirements in 61.139(g)(1)(i) shall apply to the extent
practicable.
(iii) The requirements in 61.139(g)(1)(vi) shall apply. Section 7.2
of method 18 shall be used as described in 61.139(g)(1)(vi)(B) for
benzene concentration measurements.
(h) For each carbon adsorber, the maximum concentration point shall
be expressed either as a benzene concentration or organic compound
concentration level, whichever is to be indicated by the monitoring
device chosen under 61.139 (d) or (e).
(1) For each regenerative carbon adsorber, the owner or operator
shall determine the maximum concentration point at the following times:
(i) No later than the deadline for the initial compliance test as
specified in 61.139(c)(1);
(ii) At the request of the Administrator; and
(iii) At any time chosen by the owner or operator.
(2) For each non-regenerative carbon adsorber, the owner or operator
shall determine the maximum concentration point at the following times:
(i) On the first carbon bed to be installed in the adsorber;
(ii) At the request of the Administrator;
(iii) On the next carbon bed after the maximum concentration point
has been exceeded (before the scheduled replacement time) for each of
three previous carbon beds in the adsorber since the most recent
determination; and
(iv) At any other time chosen by the owner or operator.
(3) The maximum concentration point for each carbon adsorber shall be
determined through the simultaneous measurement of the outlet of the
carbon adsorber with the monitoring device and method 18, except as
allowed in paragraph (h)(4) of this section.
(i) Several data points shall be collected according to a schedule
determined by the owner or operator. The schedule shall be designed to
take frequent samples near the expected maximum concentration point.
(ii) Each data point shall consist of one 5-minute benzene
concentration measurement using method 18 as specified in 61.139(g)(2),
and of a simultaneous measurement by the monitoring device. The
monitoring device measurement shall be conducted according to 61.139
(d) or (e), whichever is applicable.
(iii) The maximum concentration point shall be the concentration
level, as indicated by the monitoring device, for the last data point at
which the benzene concentration is less than 2 percent of the average
value of the benzene concentration at the inlet to the carbon adsorber
during the most recent compliance test.
(4) If the maximum concentration point is expressed as a benzene
concentration, the owner or operator may determine it by calibrating the
monitoring device with benzene at a concentration that is 2 percent of
the average benzene concentration measured at the inlet to the carbon
adsorber during the most recent compliance test. The reading on the
monitoring device corresponding to the calibration concentration shall
be the maximum concentration point. This method of determination would
affect the owner or operator as follows:
(i) For a regenerative carbon adsorber, the owner or operator is
exempt from the provisions in paragraph (h)(3) of this section.
(ii) For a non-regenerative carbon adsorber, the owner or operator is
required to collect the data points in paragraph (h)(3) of this section
with only the monitoring device, and is exempt from the simultaneous
method 18 measurement.
(5) For each non-regenerative carbon adsorber, the demonstrated bed
life shall be the carbon bed life, measured in days from the time the
bed is installed until the maximum concentration point is reached, for
the carbon bed that is used to determine the maximum concentration
point.
(i) The following recordkeeping requirements are applicable to owners
and operators of control devices subject to 61.139. All records shall
be kept updated and in a readily accessible location.
(1) The following information shall be recorded for each control
device for the life of the control device:
(i) The design characteristics of the control device and a list of
the source or sources vented to it.
(ii) A plan for proper operation, maintenance, and corrective action
to achieve at least 98 percent control of benzene emissions.
(iii) The dates and descriptions of any changes in the design
specifications or plan.
(iv) For each carbon adsorber, the plan in paragraph (i)(1)(ii) of
this section shall include the method for handling captured benzene and
removed carbon to comply with 61.139(b) (1) and (2).
(v) For each carbon adsorber for which organic compounds are
monitored as provided under 61.139 (d) and (e), documentation to show
that the measurements of organic compound concentrations are reasonable
indicators of benzene concentrations.
(2) For each compliance test as specified in 61.139(c)(1), the date
of the test, the results of the test, and other data needed to determine
emissions shall be recorded as specified in 61.13(g) for at least 2
years or until the next compliance test on the control device, whichever
is longer.
(3) For each vapor incinerator, the average firebox temperature of
the incinerator (or the average temperature upstream and downstream of
the catalyst bed for a catalytic incinerator), measured and averaged
over the most recent compliance test shall be recorded for at least 2
years or until the next compliance test on the incinerator, whichever is
longer.
(4) For each carbon adsorber, for each determination of a maximum
concentration point as specified in 61.139(h), the date of the
determination, the maximum concentration point, and data needed to make
the determination shall be recorded for at least 2 years or until the
next maximum concentration point determination on the carbon adsorber,
whichever is longer.
(5) For each carbon absorber, the dates of and data from the
monitoring required in 61.139(d) and (e), the date and time of
replacement of each carbon bed, the date of each exceedance of the
maximum concentration point, and a brief description of the corrective
action taken shall be recorded for at least 2 years. Also, the
occurrences when the captured benzene or spent carbon are not handled as
required in 61.139(b)(1) and (2) shall be recorded for at least 2
years.
(6) For each vapor incinerator, the data from the monitoring required
in 61.139(f)(1), the dates of all periods of operation during which the
parameter boundaries established during the most recent compliance test
are exceeded, and a brief description of the corrective action taken
shall be recorded for at least 2 years. A period of operation during
which the parameter boundaries are exceeded is a 3-hour period of
operation during which:
(i) For each vapor incinerator other than a catalytic incinerator,
the average combustion temperature is more than 28 C (50 F) below the
average combustion temperature during the most recent performance test.
(ii) For each catalytic incinerator, the average temperature of the
vent stream immediately before the catalyst bed is more than 28 C (50 F)
below the average temperature of the vent stream during the most recent
performance test, or the average temperature difference across the
catalyst bed is less than 80 percent of the average temperature
difference across the catalyst bed during the most recent performance
test.
(7) For each vapor incinerator, the following shall be recorded for
at least 2 years:
(i) If subject to 61.139(f)(2)(i), records of the flow indication,
and of all periods when the vent stream is diverted from the vapor
incinerator or has no flow rate.
(ii) If subject to 61.139(f)(2)(ii), records of the flow indication,
and of all periods when the vent stream is diverted from the vapor
incinerator.
(iii) If subject to 61.139(f)(2)(iii), records of the conditions
found during each monthly inspection, and of each period when the car
seal is broken, when the valve position is changed, or when maintenance
on the bypass line valve is performed.
(j) The following reporting requirements are applicable to owners or
operators of control devices subject to 61.139:
(1) Compliance tests shall be reported as specified in 61.13(f).
(2) The following information shall be reported on a quarterly basis.
Two of the quarterly reports shall be submitted as part of the
semiannual reports required in 61.138(f).
(i) For each carbon adsorber:
(A) The date and time of detection of each exceedance of the maximum
concentration point and a brief description of the time and nature of
the corrective action taken.
(B) The date of each time that the captured benzene or removed carbon
was not handled as required in 61.139 (b)(1) and (2), and a brief
description of the corrective action taken.
(C) The date of each determination of the maximum concentration
point, as described in 61.139(h), and a brief reason for the
determination.
(ii) For each vapor incinerator, the date and duration of each
exceedance of the boundary parameters recorded under 61.139(i)(6) and a
brief description of the corrective action taken.
(iii) For each vapor incinerator, the date and duration of each
period specified as follows:
(A) Each period recorded under 61.139(i)(7)(i) when the vent stream
is diverted from the control device or has no flow rate;
(B) Each period recorded under 61.139(i)(7)(ii) when the vent stream
is diverted from the control device; and
(C) Each period recorded under 61.139(i)(7)(iii) when the vent
stream is diverted from the control device, when the car seal is broken,
when the valve is unlocked, or when the valve position has changed.
(iv) For each vapor incinerator, the owner or operator shall specify
the method of monitoring chosen under 61.139(f)(2) in the first
quarterly report. Any time the owner or operator changes that choice,
he shall specify the change in the first quarterly report following the
change.
(3) If, for a given quarter in which no semiannual report is due
under 61.138(f), there is no information to report under
61.139(j)(2)(i)(A), (j)(2)(i)(B), (j)(2)(ii)(A), and (j)(2)(ii)(B), then
the owner or operator may submit a statement to that effect along with
the information to be reported under 61.139(j)(2)(i)(C) in the next
semiannual report, rather than submitting a report at the end of the
quarter.
(Approved by the Office of Management and Budget under control number
2060-0185)
(56 FR 47407, Sept. 19, 1991)
40 CFR 61.139 Subpart M -- National Emission Standard for Asbestos
Authority: 42 U.S.C. 7401, 7412, 7414, 7416, 7601.
Source: 49 FR 13661, Apr. 5, 1984, unless otherwise noted.
40 CFR 61.140 Applicability.
The provisions of this subpart are applicable to those sources
specified in 61.142 through 61.151, 61.154, and 61.155.
(55 FR 48414, Nov. 20, 1990)
40 CFR 61.141 Definitions.
All terms that are used in this subpart and are not defined below are
given the same meaning as in the Act and in subpart A of this part.
Active waste disposal site means any disposal site other than an
inactive site.
Adequately wet means sufficiently mix or penetrate with liquid to
prevent the release of particulates. If visible emissions are observed
coming from asbestos-containing material, then that material has not
been adequately wetted. However, the absence of visible emissions is
not sufficient evidence of being adequately wet.
Asbestos means the asbestiform varieties of serpentinite
(chrysotile), riebeckite (crocidolite), cummingtonite-grunerite,
anthophyllite, and actinolite-tremolite.
Asbestos-containing waste materials means mill tailings or any waste
that contains commercial asbestos and is generated by a source subject
to the provisions of this subpart. This term includes filters from
control devices, friable asbestos waste material, and bags or other
similar packaging contaminated with commercial asbestos. As applied to
demolition and renovation operations, this term also includes regulated
asbestos-containing material waste and materials contaminated with
asbestos including disposable equipment and clothing.
Asbestos mill means any facility engaged in converting, or in any
intermediate step in converting, asbestos ore into commercial asbestos.
Outside storage of asbestos material is not considered a part of the
asbestos mill.
Asbestos tailings means any solid waste that contains asbestos and is
a product of asbestos mining or milling operations.
Asbestos waste from control devices means any waste material that
contains asbestos and is collected by a pollution control device.
Category I nonfriable asbestos-containing material (ACM) means
asbestos-containing packings, gaskets, resilient floor covering, and
asphalt roofing products containing more than 1 percent asbestos as
determined using the method specified in appendix A, subpart F, 40 CFR
part 763, section 1, Polarized Light Microscopy.
Category II nonfriable ACM means any material, excluding Category I
nonfriable ACM, containing more than 1 percent asbestos as determined
using the methods specified in appendix A, subpart F, 40 CFR part 763,
section 1, Polarized Light Microscopy that, when dry, cannot be
crumbled, pulverized, or reduced to powder by hand pressure.
Commercial asbestos means any material containing asbestos that is
extracted from ore and has value because of its asbestos content.
Cutting means to penetrate with a sharp-edged instrument and includes
sawing, but does not include shearing, slicing, or punching.
Demolition means the wrecking or taking out of any load-supporting
structural member of a facility together with any related handling
operations or the intentional burning of any facility.
Emergency renovation operation means a renovation operation that was
not planned but results from a sudden, unexpected event that, if not
immediately attended to, presents a safety or public health hazard, is
necessary to protect equipment from damage, or is necessary to avoid
imposing an unreasonable financial burden. This term includes
operations necessitated by nonroutine failures of equipment.
Fabricating means any processing (e.g., cutting, sawing, drilling) of
a manufactured product that contains commercial asbestos, with the
exception of processing at temporary sites (field fabricating) for the
construction or restoration of facilities. In the case of friction
products, fabricating includes bonding, debonding, grinding, sawing,
drilling, or other similar operations performed as part of fabricating.
Facility means any institutional, commercial, public, industrial, or
residential structure, installation, or building (including any
structure, installation, or building containing condominiums or
individual dwelling units operated as a residential cooperative, but
excluding residential buildings having four or fewer dwelling units);
any ship; and any active or inactive waste disposal site. For purposes
of this definition, any building, structure, or installation that
contains a loft used as a dwelling is not considered a residential
structure, installation, or building. Any structure, installation or
building that was previously subject to this subpart is not excluded,
regardless of its current use or function.
Facility component means any part of a facility including equipment.
Friable asbestos material means any material containing more than 1
percent asbestos as determined using the method specified in appendix A,
subpart F, 40 CFR part 763 section 1, Polarized Light Microscopy, that,
when dry, can be crumbled, pulverized, or reduced to powder by hand
pressure. If the asbestos content is less than 10 percent as determined
by a method other than point counting by polarized light microscopy
(PLM), verify the asbestos content by point counting using PLM.
Fugitive source means any source of emissions not controlled by an
air pollution control device.
Glove bag means a sealed compartment with attached inner gloves used
for the handling of asbestos-containing materials. Properly installed
and used, glove bags provide a small work area enclosure typically used
for small-scale asbestos stripping operations. Information on glove-bag
installation, equipment and supplies, and work practices is contained in
the Occupational Safety and Health Administration's (OSHA's) final rule
on occupational exposure to asbestos (appendix G to 29 CFR 1926.58).
Grinding means to reduce to powder or small fragments and includes
mechanical chipping or drilling.
In poor condition means the binding of the material is losing its
integrity as indicated by peeling, cracking, or crumbling of the
material.
Inactive waste disposal site means any disposal site or portion of it
where additional asbestos-containing waste material has not been
deposited within the past year.
Installation means any building or structure or any group of
buildings or structures at a single demolition or renovation site that
are under the control of the same owner or operator (or owner or
operator under common control).
Leak-tight means that solids or liquids cannot escape or spill out.
It also means dust-tight.
Malfunction means any sudden and unavoidable failure of air pollution
control equipment or process equipment or of a process to operate in a
normal or usual manner so that emissions of asbestos are increased.
Failures of equipment shall not be considered malfunctions if they are
caused in any way by poor maintenance, careless operation, or any other
preventable upset conditions, equipment breakdown, or process failure.
Manufacturing means the combining of commercial asbestos -- or, in
the case of woven friction products, the combining of textiles
containing commercial asbestos -- with any other material(s), including
commercial asbestos, and the processing of this combination into a
product. Chlorine production is considered a part of manufacturing.
Natural barrier means a natural object that effectively precludes or
deters access. Natural barriers include physical obstacles such as
cliffs, lakes or other large bodies of water, deep and wide ravines, and
mountains. Remoteness by itself is not a natural barrier.
Nonfriable asbestos-containing material means any material containing
more than 1 percent asbestos as determined using the method specified in
appendix A, subpart F, 40 CFR part 763, section 1, Polarized Light
Microscopy, that, when dry, cannot be crumbled, pulverized, or reduced
to powder by hand pressure.
Nonscheduled renovation operation means a renovation operation
necessitated by the routine failure of equipment, which is expected to
occur within a given period based on past operating experience, but for
which an exact date cannot be predicted.
Outside air means the air outside buildings and structures,
including, but not limited to, the air under a bridge or in an open air
ferry dock.
Owner or operator of a demolition or renovation activity means any
person who owns, leases, operates, controls, or supervises the facility
being demolished or renovated or any person who owns, leases, operates,
controls, or supervises the demolition or renovation operation, or both.
Particulate asbestos material means finely divided particles of
asbestos or material containing asbestos.
Planned renovation operations means a renovation operation, or a
number of such operations, in which some RACM will be removed or
stripped within a given period of time and that can be predicted.
Individual nonscheduled operations are included if a number of such
operations can be predicted to occur during a given period of time based
on operating experience.
Regulated asbestos-containing material (RACM) means (a) Friable
asbestos material, (b) Category I nonfriable ACM that has become
friable, (c) Category I nonfriable ACM that will be or has been
subjected to sanding, grinding, cutting, or abrading, or (d) Category II
nonfriable ACM that has a high probability of becoming or has become
crumbled, pulverized, or reduced to powder by the forces expected to act
on the material in the course of demolition or renovation operations
regulated by this subpart.
Remove means to take out RACM or facility components that contain or
are covered with RACM from any facility.
Renovation means altering a facility or one or more facility
components in any way, including the stripping or removal of RACM from a
facility component. Operations in which load-supporting structural
members are wrecked or taken out are demolitions.
Resilient floor covering means asbestos-containing floor tile,
including asphalt and vinyl floor tile, and sheet vinyl floor covering
containing more than 1 percent asbestos as determined using polarized
light microscopy according to the method specified in appendix A,
subpart F, 40 CFR part 763, Section 1, Polarized Light Microscopy.
Roadways means surfaces on which vehicles travel. This term includes
public and private highways, roads, streets, parking areas, and
driveways.
Strip means to take off RACM from any part of a facility or facility
components.
Structural member means any load-supporting member of a facility,
such as beams and load supporting walls; or any nonload-supporting
member, such as ceilings and nonload-supporting walls.
Visible emissions means any emissions, which are visually detectable
without the aid of instruments, coming from RACM or asbestos-containing
waste material, or from any asbestos milling, manufacturing, or
fabricating operation. This does not include condensed, uncombined
water vapor.
Waste generator means any owner or operator of a source covered by
this subpart whose act or process produces asbestos-containing waste
material.
Waste shipment record means the shipping document, required to be
originated and signed by the waste generator, used to track and
substantiate the disposition of asbestos-containing waste material.
Working day means Monday through Friday and includes holidays that
fall on any of the days Monday through Friday.
(49 FR 13661, Apr. 5, 1984; 49 FR 25453, June 21, 1984, as amended
by 55 FR 48414, Nov. 20, 1990; 56 FR 1669, Jan. 16, 1991)
40 CFR 61.142 Standard for asbestos mills.
(a) Each owner or operator of an asbestos mill shall either discharge
no visible emissions to the outside air from that asbestos mill,
including fugitive sources, or use the methods specified by 61.152 to
clean emissions containing particulate asbestos material before they
escape to, or are vented to, the outside air.
(b) Each owner or operator of an asbestos mill shall meet the
following requirements:
(1) Monitor each potential source of asbestos emissions from any part
of the mill facility, including air cleaning devices, process equipment,
and buildings that house equipment for material processing and handling,
at least once each day, during daylight hours, for visible emissions to
the outside air during periods of operation. The monitoring shall be by
visual observation of at least 15 seconds duration per source of
emissions.
(2) Inspect each air cleaning device at least once each week for
proper operation and for changes that signal the potential for
malfunction, including, to the maximum extent possible without
dismantling other than opening the device, the presence of tears, holes,
and abrasions in filter bags and for dust deposits on the clean side of
bags. For air cleaning devices that cannot be inspected on a weekly
basis according to this paragraph, submit to the Administrator, and
revise as necessary, a written maintenance plan to include, at a
minimum, the following:
(i) Maintenance schedule.
(ii) Recordkeeping plan.
(3) Maintain records of the results of visible emissions monitoring
and air cleaning device inspections using a format similar to that shown
in Figures 1 and 2 and include the following:
(i) Date and time of each inspection.
(ii) Presence or absence of visible emissions.
(iii) Condition of fabric filters, including presence of any tears,
holes, and abrasions.
(iv) Presence of dust deposits on clean side of fabric filters.
(v) Brief description of corrective actions taken, including date and
time.
(vi) Daily hours of operation for each air cleaning device.
(4) Furnish upon request, and make available at the affected facility
during normal business hours for inspection by the Administrator, all
records required under this section.
(5) Retain a copy of all monitoring and inspection records for at
least 2 years.
(6) Submit quarterly a copy of visible emission monitoring records to
the Administrator if visible emissions occurred during the report
period. Quarterly reports shall be postmarked by the 30th day following
the end of the calendar quarter.
Insert Illus. ??A
Insert Illus. ??B
(55 FR 48416, Nov. 20, 1990)
40 CFR 61.143 Standard for roadways.
No person may construct or maintain a roadway with asbestos tailings
or asbestos-containing waste material on that roadway, unless, for
asbestos tailings.
(a) It is a temporary roadway on an area of asbestos ore deposits
(asbestos mine): or
(b) It is a temporary roadway at an active asbestos mill site and is
encapsulated with a resinous or bituminous binder. The encapsulated
road surface must be maintained at a minimum frequency of once per year
to prevent dust emissions; or
(c) It is encapsulated in asphalt concrete meeting the specifications
contained in section 401 of Standard Specifications for Construction of
Roads and Bridges on Federal Highway Projects, FP-85, 1985, or their
equivalent.
(55 FR 48419, Nov. 20, 1990; 56 FR 1669, Jan. 16, 1991)
40 CFR 61.144 Standard for manufacturing.
(a) Applicability. This section applies to the following
manufacturing operations using commercial asbestos.
(1) The manufacture of cloth, cord, wicks, tubing, tape, twine, rope,
thread, yarn, roving, lap, or other textile materials.
(2) The manufacture of cement products.
(3) The manufacture of fireproofing and insulating materials.
(4) The manufacture of friction products.
(5) The manufacture of paper, millboard, and felt.
(6) The manufacture of floor tile.
(7) The manufacture of paints, coatings, caulks, adhesives, and
sealants.
(8) The manufacture of plastics and rubber materials.
(9) The manufacture of chlorine utilizing asbestos diaphragm
technology.
(10) The manufacture of shotgun shell wads.
(11) The manufacture of asphalt concrete.
(b) Standard. Each owner or operator of any of the manufacturing
operations to which this section applies shall either:
(1) Discharge no visible emissions to the outside air from these
operations or from any building or structure in which they are conducted
or from any other fugitive sources; or
(2) Use the methods specified by 61.152 to clean emissions from
these operations containing particulate asbestos material before they
escape to, or are vented to, the outside air.
(3) Monitor each potential source of asbestos emissions from any part
of the manufacturing facility, including air cleaning devices, process
equipment, and buildings housing material processing and handling
equipment, at least once each day during daylight hours for visible
emissions to the outside air during periods of operation. The
monitoring shall be by visual observation of at least 15 seconds
duration per source of emissions.
(4) Inspect each air cleaning device at least once each week for
proper operation and for changes that signal the potential for
malfunctions, including, to the maximum extent possible without
dismantling other than opening the device, the presence of tears, holes,
and abrasions in filter bags and for dust deposits on the clean side of
bags. For air cleaning devices that cannot be inspected on a weekly
basis according to this paragraph, submit to the Administrator, and
revise as necessary, a written maintenance plan to include, at a
minimum, the following:
(i) Maintenance schedule.
(ii) Recordkeeping plan.
(5) Maintain records of the results of visible emission monitoring
and air cleaning device inspections using a format similar to that shown
in Figures 1 and 2 and include the following.
(i) Date and time of each inspection.
(ii) Presence or absence of visible emissions.
(iii) Condition of fabric filters, including presence of any tears,
holes and abrasions.
(iv) Presence of dust deposits on clean side of fabric filters.
(v) Brief description of corrective actions taken, including date and
time.
(vi) Daily hours of operation for each air cleaning device.
(6) Furnish upon request, and make available at the affected facility
during normal business hours for inspection by the Administrator, all
records required under this section.
(7) Retain a copy of all monitoring and inspection records for at
least 2 years.
(8) Submit quarterly a copy of the visible emission monitoring
records to the Administrator if visible emissions occurred during the
report period. Quarterly reports shall be postmarked by the 30th day
following the end of the calendar quarter.
(49 FR 13661, Apr. 5, 1984, as amended at 55 FR 48419, Nov. 20, 1990;
56 FR 1669, Jan. 16, 1991)
40 CFR 61.145 Standard for demolition and renovation.
(a) Applicability. To determine which requirements of paragraphs
(a), (b), and (c) of this section apply to the owner or operator of a
demolition or renovation activity and prior to the commencement of the
demolition or renovation, thoroughly inspect the affected facility or
part of the facility where the demolition or renovation operation will
occur for the presence of asbestos, including Category I and Category II
nonfriable ACM. The requirements of paragraphs (b) and (c) of this
section apply to each owner or operator of a demolition or renovation
activity, including the removal of RACM as follows:
(1) In a facility being demolished, all the requirements of
paragraphs (b) and (c) of this section apply, except as provided in
paragraph (a)(3) of this section, if the combined amount of RACM is
(i) At least 80 linear meters (260 linear feet) on pipes or at least
15 square meters (160 square feet) on other facility components, or
(ii) At least 1 cubic meter (35 cubic feet) off facility components
where the length or area could not be measured previously.
(2) In a facility being demolished, only the notification
requirements of paragraphs (b)(1), (2), (3)(i) and (iv), and (4)(i)
through (vii) and (4)(ix) and (xvi) of this section apply, if the
combined amount of RACM is
(i) Less than 80 linear meters (260 linear feet) on pipes and less
than 15 square meters (160 square feet) on other facility components,
and
(ii) Less than one cubic meter (35 cubic feet) off facility
components where the length or area could not be measured previously or
there is no asbestos.
(3) If the facility is being demolished under an order of a State or
local government agency, issued because the facility is structurally
unsound and in danger of imminent collapse, only the requirements of
paragraphs (b)(1), (b)(2), (b)(3)(iii), (b)(4) (except (b)(4)(viii)),
(b)(5), and (c)(4) through (c)(9) of this section apply.
(4) In a facility being renovated, including any individual
nonscheduled renovation operation, all the requirements of paragraphs
(b) and (c) of this section apply if the combined amount of RACM to be
stripped, removed, dislodged, cut, drilled, or similarly disturbed is
(i) At least 80 linear meters (260 linear feet) on pipes or at least
15 square meters (160 square feet) on other facility components, or
(ii) At least 1 cubic meter (35 cubic feet) off facility components
where the length or area could not be measured previously.
(iii) To determine whether paragraph (a)(4) of this section applies
to planned renovation operations involving individual nonscheduled
operations, predict the combined additive amount of RACM to be removed
or stripped during a calendar year of January 1 through December 31.
(iv) To determine whether paragraph (a)(4) of this section applies to
emergency renovation operations, estimate the combined amount of RACM to
be removed or stripped as a result of the sudden, unexpected event that
necessitated the renovation.
(5) Owners or operators of demolition and renovation operations are
exempt from the requirements of 61.05(a), 61.07, and 61.09.
(b) Notification requirements. Each owner or operator of a
demolition or renovation activity to which this section applies shall:
(1) Provide the Administrator with written notice of intention to
demolish or renovate. Delivery of the notice by U.S. Postal Service,
commercial delivery service, or hand delivery is acceptable.
(2) Update notice, as necessary, including when the amount of
asbestos affected changes by at least 20 percent.
(3) Postmark or deliver the notice as follows:
(i) At least 10 working days before asbestos stripping or removal
work or any other activity begins (such as site preparation that would
break up, dislodge or similarly disturb asbestos material), if the
operation is described in paragraphs (a) (1) and (4) (except (a)(4)(iii)
and (a)(4)(iv)) of this section. If the operation is as described in
paragraph (a)(2) of this section, notification is required 10 working
days before demolition begins.
(ii) At least 10 working days before the end of the calendar year
preceding the year for which notice is being given for renovations
described in paragraph (a)(4)(iii) of this section.
(iii) As early as possible before, but not later than, the following
working day if the operation is a demolition ordered according to
paragraph (a)(3) of this section or, if the operation is a renovation
described in paragraph (a)(4)(iv) of this section.
(iv) For asbestos stripping or removal work in a demolition or
renovation operation, described in paragraphs (a) (1) and (4) (except
(a)(4)(iii) and (a)(4)(iv)) of this section, and for a demolition
described in paragraph (a)(2) of this section, that will begin on a date
other than the one contained in the original notice, notice of the new
start date must be provided to the Administrator as follows:
(A) When the asbestos stripping or removal operation or demolition
operation covered by this paragraph will begin after the date contained
in the notice,
(1) Notify the Administrator of the new start date by telephone as
soon as possible before the original start date, and
(2) Provide the Administrator with a written notice of the new start
date as soon as possible before, and no later than, the original start
date. Delivery of the updated notice by the U.S. Postal Service,
commercial delivery service, or hand delivery is acceptable.
(B) When the asbestos stripping or removal operation or demolition
operation covered by this paragraph will begin on a date earlier than
the original start date,
(1) Provide the Administrator with a written notice of the new start
date at least 10 working days before asbestos stripping or removal work
begins.
(2) For demolitions covered by paragraph (a)(2) of this section,
provide the Administrator written notice of a new start date at least 10
working days before commencement of demolition. Delivery of updated
notice by U.S. Postal Service, commercial delivery service, or hand
delivery is acceptable.
(C) In no event shall an operation covered by this paragraph begin on
a date other than the date contained in the written notice of the new
start date.
(4) Include the following in the notice:
(i) An indication of whether the notice is the original or a revised
notification.
(ii) Name, address, and telephone number of both the facility owner
and operator and the asbestos removal contractor owner or operator.
(iii) Type of operation: demolition or renovation.
(iv) Description of the facility or affected part of the facility
including the size (square meters (square feet) and number of floors),
age, and present and prior use of the facility.
(v) Procedure, including analytical methods, employed to detect the
presence of RACM and Category I and Category II nonfriable ACM.
(vi) Estimate of the approximate amount of RACM to be removed from
the facility in terms of length of pipe in linear meters (linear feet),
surface area in square meters (square feet) on other facility
components, or volume in cubic meters (cubic feet) if off the facility
components. Also, estimate the approximate amount of Category I and
Category II nonfriable ACM in the affected part of the facility that
will not be removed before demolition.
(vii) Location and street address (including building number or name
and floor or room number, if appropriate), city, county, and state, of
the facility being demolished or renovated.
(viii) Scheduled starting and completion dates of asbestos removal
work (or any other activity, such as site preparation that would break
up, dislodge, or similarly disturb asbestos material) in a demolition or
renovation; planned renovation operations involving individual
nonscheduled operations shall only include the beginning and ending
dates of the report period as described in paragraph (a)(4)(iii) of this
section.
(ix) Scheduled starting and completion dates of demolition or
renovation.
(x) Description of planned demolition or renovation work to be
performed and method(s) to be employed, including demolition or
renovation techniques to be used and description of affected facility
components.
(xi) Description of work practices and engineering controls to be
used to comply with the requirements of this subpart, including asbestos
removal and waste-handling emission control procedures.
(xii) Name and location of the waste disposal site where the
asbestos-containing waste material will be deposited.
(xiii) A certification that at least one person trained as required
by paragraph (c)(8) of this section will supervise the stripping and
removal described by this notification. This requirement shall become
effective 1 year after promulgation of this regulation.
(xiv) For facilities described in paragraph (a)(3) of this section,
the name, title, and authority of the State or local government
representative who has ordered the demolition, the date that the order
was issued, and the date on which the demolition was ordered to begin.
A copy of the order shall be attached to the notification.
(xv) For emergency renovations described in paragraph (a)(4)(iv) of
this section, the date and hour that the emergency occurred, a
description of the sudden, unexpected event, and an explanation of how
the event caused an unsafe condition, or would cause equipment damage or
an unreasonable financial burden.
(xvi) Description of procedures to be followed in the event that
unexpected RACM is found or Category II nonfriable ACM becomes crumbled,
pulverized, or reduced to powder.
(xvii) Name, address, and telephone number of the waste transporter.
(5) The information required in paragraph (b)(4) of this section must
be reported using a form similiar to that shown in Figure 3.
(c) Procedures for asbestos emission control. Each owner or operator
of a demolition or renovation activity to whom this paragraph applies,
according to paragraph (a) of this section, shall comply with the
following procedures:
(1) Remove all RACM from a facility being demolished or renovated
before any activity begins that would break up, dislodge, or similarly
disturb the material or preclude access to the material for subsequent
removal. RACM need not be removed before demolition if:
(i) It is Category I nonfriable ACM that is not in poor condition and
is not friable.
(ii) It is on a facility component that is encased in concrete or
other similarly hard material and is adequately wet whenever exposed
during demolition; or
(iii) It was not accessible for testing and was, therefore, not
discovered until after demolition began and, as a result of the
demolition, the material cannot be safely removed. If not removed for
safety reasons, the exposed RACM and any asbestos-contaminated debris
must be treated as asbestos-containing waste material and adequately wet
at all times until disposed of.
(iv) They are Category II nonfriable ACM and the probability is low
that the materials will become crumbled, pulverized, or reduced to
powder during demolition.
(2) When a facility component that contains, is covered with, or is
coated with RACM is being taken out of the facility as a unit or in
sections:
(i) Adequately wet all RACM exposed during cutting or disjoining
operations; and
(ii) Carefully lower each unit or section to the floor and to ground
level, not dropping, throwing, sliding, or otherwise damaging or
disturbing the RACM.
(3) When RACM is stripped from a facility component while it remains
in place in the facility, adequately wet the RACM during the stripping
operation.
(i) In renovation operations, wetting is not required if:
(A) The owner or operator has obtained prior written approval from
the Administrator based on a written application that wetting to comply
with this paragraph would unavoidably damage equipment or present a
safety hazard; and
(B) The owner or operator uses of the following emission control
methods:
(1) A local exhaust ventilation and collection system designed and
operated to capture the particulate asbestos material produced by the
stripping and removal of the asbestos materials. The system must
exhibit no visible emissions to the outside air or be designed and
operated in accordance with the requirements in 61.152.
(2) A glove-bag system designed and operated to contain the
particulate asbestos material produced by the stripping of the asbestos
materials.
(3) Leak-tight wrapping to contain all RACM prior to dismantlement.
(ii) In renovation operations where wetting would result in equipment
damage or a safety hazard, and the methods allowed in paragraph
(c)(3)(i) of this section cannot be used, another method may be used
after obtaining written approval from the Administrator based upon a
determination that it is equivalent to wetting in controlling emissions
or to the methods allowed in paragraph (c)(3)(i) of this section.
(iii) A copy of the Administrator's written approval shall be kept at
the worksite and made available for inspection.
(4) After a facility component covered with, coated with, or
containing RACM has been taken out of the facility as a unit or in
sections pursuant to paragraph (c)(2) of this section, it shall be
stripped or contained in leak-tight wrapping, except as described in
paragraph (c)(5) of this section. If stripped, either:
(i) Adequately wet the RACM during stripping; or
(ii) Use a local exhaust ventilation and collection system designed
and operated to capture the particulate asbestos material produced by
the stripping. The system must exhibit no visible emissions to the
outside air or be designed and operated in accordance with the
requirements in 61.152.
(5) For large facility components such as reactor vessels, large
tanks, and steam generators, but not beams (which must be handled in
accordance with paragraphs (c)(2), (3), and (4) of this section), the
RACM is not required to be stripped if the following requirements are
met:
(i) The component is removed, transported, stored, disposed of, or
reused without disturbing or damaging the RACM.
(ii) The component is encased in a leak-tight wrapping.
(iii) The leak-tight wrapping is labeled according to
61.149(d)(1)(i), (ii), and (iii) during all loading and unloading
operations and during storage.
(6) For all RACM, including material that has been removed or
stripped:
(i) Adequately wet the material and ensure that it remains wet until
collected and contained or treated in preparation for disposal in
accordance with 61.150; and
(ii) Carefully lower the material to the ground and floor, not
dropping, throwing, sliding, or otherwise damaging or disturbing the
material.
(iii) Transport the material to the ground via leak-tight chutes or
containers if it has been removed or stripped more than 50 feet above
ground level and was not removed as units or in sections.
(iv) RACM contained in leak-tight wrapping that has been removed in
accordance with paragraphs (c)(4) and (c)(3)(i)(B)(3) of this section
need not be wetted.
(7) When the temperature at the point of wetting is below 0 C (32
F):
(i) The owner or operator need not comply with paragraph (c)(2)(i)
and the wetting provisions of paragraph (c)(3) of this section.
(ii) The owner or operator shall remove facility components
containing, coated with, or covered with RACM as units or in sections to
the maximum extent possible.
(iii) During periods when wetting operations are suspended due to
freezing temperatures, the owner or operator must record the temperature
in the area containing the facility components at the beginning, middle,
and end of each workday and keep daily temperature records available for
inspection by the Administrator during normal business hours at the
demolition or renovation site. The owner or operator shall retain the
temperature records for at least 2 years.
(8) Effective 1 year after promulgation of this regulation, no RACM
shall be stripped, removed, or otherwise handled or disturbed at a
facility regulated by this section unless at least one on-site
representative, such as a foreman or management-level person or other
authorized representative, trained in the provisions of this regulation
and the means of complying with them, is present. Every 2 years, the
trained on-site individual shall receive refresher training in the
provisions of this regulation. The required training shall include as a
minimum: applicability; notifications; material identification;
control procedures for removals including, at least, wetting, local
exhaust ventilation, negative pressure enclosures, glove-bag procedures,
and High Efficiency Particulate Air (HEPA) filters; waste disposal work
practices; reporting and recordkeeping; and asbestos hazards and
worker protection. Evidence that the required training has been
completed shall be posted and made available for inspection by the
Administrator at the demolition or renovation site.
(9) For facilities described in paragraph (a)(3) of this section,
adequately wet the portion of the facility that contains RACM during the
wrecking operation.
(10) If a facility is demolished by intentional burning, all RACM
including Category I and Category II nonfriable ACM must be removed in
accordance with the NESHAP before burning.
Insert illustration 0 500
Insert illustration 0 501
(55 FR 48419, Nov. 20, 1990; 56 FR 1669, Jan. 16, 1991)
40 CFR 61.146 Standard for spraying.
The owner or operator of an operation in which asbestos-containing
materials are spray applied shall comply with the following
requirements:
(a) For spray-on application on buildings, structures, pipes, and
conduits, do not use material containing more than 1 percent asbestos as
determined using the method specified in appendix A, subpart F, 40 CFR
part 763, section 1, Polarized Light Microscopy, except as provided in
paragraph (c) of this section.
(b) For spray-on application of materials that contain more than 1
percent asbestos as determined using the method specified in appendix A,
subpart F, 40 CFR part 763, section 1, Polarized Light Microscopy, on
equipment and machinery, except as provided in paragraph (c) of this
section:
(1) Notify the Administrator at least 20 days before beginning the
spraying operation. Include the following information in the notice:
(i) Name and address of owner or operator.
(ii) Location of spraying operation.
(iii) Procedures to be followed to meet the requirements of this
paragraph.
(2) Discharge no visible emissions to the outside air from spray-on
application of the asbestos-containing material or use the methods
specified by 61.152 to clean emissions containing particulate asbestos
material before they escape to, or are vented to, the outside air.
(c) The requirements of paragraphs (a) and (b) of this section do not
apply to the spray-on application of materials where the asbestos fibers
in the materials are encapsulated with a bituminous or resinous binder
during spraying and the materials are not friable after drying.
(d) Owners or operators of sources subject to this paragraph are
exempt from the requirements of 61.05(a), 61.07 and 61.09.
(Approved by the Office of Management and Budget under control number
2000-0264)
(49 FR 13661, Apr. 5, 1984. Redesignated and amended at 55 FR 48424,
Nov. 20, 1990)
40 CFR 61.147 Standard for fabricating.
(a) Applicability. This section applies to the following fabricating
operations using commercial asbestos:
(1) The fabrication of cement building products.
(2) The fabrication of friction products, except those operations
that primarily install asbestos friction materials on motor vehicles.
(3) The fabrication of cement or silicate board for ventilation
hoods; ovens; electrical panels; laboratory furniture, bulkheads,
partitions, and ceilings for marine construction; and flow control
devices for the molten metal industry.
(b) Standard. Each owner or operator of any of the fabricating
operations to which this section applies shall either:
(1) Discharge no visible emissions to the outside air from any of the
operations or from any building or structure in which they are conducted
or from any other fugitive sources; or
(2) Use the methods specified by 61.152 to clean emissions
containing particulate asbestos material before they escape to, or are
vented to, the outside air.
(3) Monitor each potential source of asbestos emissions from any part
of the fabricating facility, including air cleaning devices, process
equipment, and buildings that house equipment for material processing
and handling, at least once each day, during daylight hours, for visible
emissions to the outside air during periods of operation. The
monitoring shall be by visual observation of at least 15 seconds
duration per source of emissions.
(4) Inspect each air cleaning device at least once each week for
proper operation and for changes that signal the potential for
malfunctions, including, to the maximum extent possible without
dismantling other than opening the device, the presence of tears, holes,
and abrasions in filter bags and for dust deposits on the clean side of
bags. For air cleaning devices that cannot be inspected on a weekly
basis according to this paragraph, submit to the Administrator, and
revise as necessary, a written maintenance plan to include, at a
minimum, the following:
(i) Maintenance schedule.
(ii) Recordkeeping plan.
(5) Maintain records of the results of visible emission monitoring
and air cleaning device inspections using a format similar to that shown
in Figures 1 and 2 and include the following:
(i) Date and time of each inspection.
(ii) Presence or absence of visible emissions.
(iii) Condition of fabric filters, including presence of any tears,
holes, and abrasions.
(iv) Presence of dust deposits on clean side of fabric filters.
(v) Brief description of corrective actions taken, including date and
time.
(vi) Daily hours of operation for each air cleaning device.
(6) Furnish upon request and make available at the affected facility
during normal business hours for inspection by the Administrator, all
records required under this section.
(7) Retain a copy of all monitoring and inspection records for at
least 2 years.
(8) Submit quarterly a copy of the visible emission monitoring
records to the Administrator if visible emissions occurred during the
report period. Quarterly reports shall be postmarked by the 30th day
following the end of the calendar quarter.
(49 FR 13661, Apr. 5, 1984. Redesignated and amended at 55 FR 48424,
Nov. 20, 1991)
40 CFR 61.148 Standard for insulating materials.
No owner or operator of a facility may install or reinstall on a
facility component any insulating materials that contain commercial
asbestos if the materials are either molded and friable or wet-applied
and friable after drying. The provisions of this section do not apply
to spray-applied insulating materials regulated under 61.146.
(55 FR 48424, Nov. 20, 1990)
40 CFR 61.149 Standard for waste disposal for asbestos mills.
Each owner or operator of any source covered under the provisions of
61.142 shall:
(a) Deposit all asbestos-containing waste material at a waste
disposal site operated in accordance with the provisions of 61.154;
and
(b) Discharge no visible emissions to the outside air from the
transfer of control device asbestos waste to the tailings conveyor, or
use the methods specified by 61.152 to clean emissions containing
particulate asbestos material before they escape to, or are vented to,
the outside air. Dispose of the asbestos waste from control devices in
accordance with 61.150(a) or paragraph (c) of this section; and
(c) Discharge no visible emissions to the outside air during the
collection, processing, packaging, or on-site transporting of any
asbestos-containing waste material, or use one of the disposal methods
specified in paragraphs (c) (1) or (2) of this section, as follows:
(1) Use a wetting agent as follows:
(i) Adequately mix all asbestos-containing waste material with a
wetting agent recommended by the manufacturer of the agent to
effectively wet dust and tailings, before depositing the material at a
waste disposal site. Use the agent as recommended for the particular
dust by the manufacturer of the agent.
(ii) Discharge no visible emissions to the outside air from the
wetting operation or use the methods specified by 61.152 to clean
emissions containing particulate asbestos material before they escape
to, or are vented to, the outside air.
(iii) Wetting may be suspended when the ambient temperature at the
waste disposal site is less than ^9.5 C (15 F), as determined by an
appropriate measurement method with an accuracy of 1 C ( 2 F).
During periods when wetting operations are suspended, the temperature
must be recorded at least at hourly intervals, and records must be
retained for at least 2 years in a form suitable for inspection.
(2) Use an alternative emission control and waste treatment method
that has received prior written approval by the Administrator. To
obtain approval for an alternative method, a written application must be
submitted to the Administrator demonstrating that the following criteria
are met:
(i) The alternative method will control asbestos emissions equivalent
to currently required methods.
(ii) The suitability of the alternative method for the intended
application.
(iii) The alternative method will not violate other regulations.
(iv) The alternative method will not result in increased water
pollution, land pollution, or occupational hazards.
(d) When waste is transported by vehicle to a disposal site:
(1) Mark vehicles used to transport asbestos-containing waste
material during the loading and unloading of the waste so that the signs
are visible. The markings must:
(i) Be displayed in such a manner and location that a person can
easily read the legend.
(ii) Conform to the requirements for 51 cm 36 cm (20 in 14 in)
upright format signs specified in 29 CFR 1910.145(d)(4) and this
paragraph; and
(iii) Display the following legend in the lower panel with letter
sizes and styles of a visibility at least equal to those specified in
this paragraph.
Spacing between any two lines must be a least equal to the height of
the upper of the two lines.
(2) For off-site disposal, provide a copy of the waste shipment
record, described in paragraph (e)(1) of this section, to the disposal
site owner or operator at the same time as the asbestos-containing waste
material is delivered to the disposal site.
(e) For all asbestos-containing waste material transported off the
facility site:
(1) Maintain asbestos waste shipment records, using a form similar to
that shown in Figure 4, and include the following information:
(i) The name, address, and telephone number of the waste generator.
(ii) The name and address of the local, State, or EPA Regional agency
responsible for administering the asbestos NESHAP program.
(iii) The quantity of the asbestos-containing waste material in cubic
meters (cubic yards).
(iv) The name and telephone number of the disposal site operator.
(v) The name and physical site location of the disposal site.
(vi) The date transported.
(vii) The name, address, and telephone number of the transporter(s).
(viii) A certification that the contents of this consignment are
fully and accurately described by proper shipping name and are
classified, packed, marked, and labeled, and are in all respects in
proper condition for transport by highway according to applicable
international and government regulations.
(2) For waste shipments where a copy of the waste shipment record,
signed by the owner or operator of the designated disposal site, is not
received by the waste generator within 35 days of the date the waste was
accepted by the initial transporter, contact the transporter and/or the
owner or operator of the designated disposal site to determine the
status of the waste shipment.
(3) Report in writing to the local, State, or EPA Regional office
responsible for administering the asbestos NESHAP program for the waste
generator if a copy of the waste shipment record, signed by the owner or
operator of the designated waste disposal site, is not received by the
waste generator within 45 days of the date the waste was accepted by the
initial transporter. Include in the report the following information:
(i) A copy of the waste shipment record for which a confirmation of
delivery was not received, and
(ii) A cover letter signed by the waste generator explaining the
efforts taken to locate the asbestos waste shipment and the results of
those efforts.
(4) Retain a copy of all waste shipment records, including a copy of
the waste shipment record signed by the owner or operator of the
designated waste disposal site, for at least 2 years.
(f) Furnish upon request, and make available for inspection by the
Administrator, all records required under this section.
Insert illustration 0 510
Insert illustration 0 511
Insert illustration 0 512
(49 FR 13661, Apr. 5,1984. Redesignated and amended at 55 FR 48424,
Nov. 20, 1990; 56 FR 1669, Jan. 16, 1991)
40 CFR 61.150 Standard for waste disposal for manufacturing,
fabricating, demolition, renovation, and spraying operations.
Each owner or operator of any source covered under the provisions of
61.144, 61.145, 61.146, and 61.147 shall comply with the following
provisions:
(a) Discharge no visible emissions to the outside air during the
collection, processing (including incineration), packaging, or
transporting of any asbestos-containing waste material generated by the
source, or use one of the emission control and waste treatment methods
specified in paragraphs (a) (1) through (4) of this section.
(1) Adequately wet asbestos-containing waste material as follows:
(i) Mix control device asbestos waste to form a slurry; adequately
wet other asbestos-containing waste material; and
(ii) Discharge no visible emissions to the outside air from
collection, mixing, wetting, and handling operations, or use the methods
specified by 61.152 to clean emissions containing particulate asbestos
material before they escape to, or are vented to, the outside air; and
(iii) After wetting, seal all asbestos-containing waste material in
leak-tight containers while wet; or, for materials that will not fit
into containers without additional breaking, put materials into
leak-tight wrapping; and
(iv) Label the containers or wrapped materials specified in paragraph
(a)(1)(iii) of this section using warning labels specified by
Occupational Safety and Health Standards of the Department of Labor,
Occupational Safety and Health Administration (OSHA) under 29 CFR
1910.1001(j)(2) or 1926.58(k)(2)(iii). The labels shall be printed in
letters of sufficient size and contrast so as to be readily visible and
legible.
(v) For asbestos-containing waste material to be transported off the
facility site, label containers or wrapped materials with the name of
the waste generator and the location at which the waste was generated.
(2) Process asbestos-containing waste material into nonfriable forms
as follows:
(i) Form all asbestos-containing waste material into nonfriable
pellets or other shapes;
(ii) Discharge no visible emissions to the outside air from
collection and processing operations, including incineration, or use the
method specified by 61.152 to clean emissions containing particulate
asbestos material before they escape to, or are vented to, the outside
air.
(3) For facilities demolished where the RACM is not removed prior to
demolition according to 61.145(c)(1) (i), (ii), (iii), and (iv) or for
facilities demolished according to 61.145(c)(9), adequately wet
asbestos-containing waste material at all times after demolition and
keep wet during handling and loading for transport to a disposal site.
Asbestos-containing waste materials covered by this paragraph do not
have to be sealed in leak-tight containers or wrapping but may be
transported and disposed of in bulk.
(4) Use an alternative emission control and waste treatment method
that has received prior approval by the Administrator according to the
procedure described in 61.149(c)(2).
(5) As applied to demolition and renovation, the requirements of
paragraph (a) of this section do not apply to Category I nonfriable ACM
waste and Category II nonfriable ACM waste that did not become crumbled,
pulverized, or reduced to powder.
(b) All asbestos-containing waste material shall be deposited as soon
as is practical by the waste generator at:
(1) A waste disposal site operated in accordance with the provisions
of 61.154, or
(2) An EPA-approved site that converts RACM and asbestos-containing
waste material into nonasbestos (asbestos-free) material according to
the provisions of 61.155.
(3) The requirements of paragraph (b) of this section do not apply to
Category I nonfriable ACM that is not RACM.
(c) Mark vehicles used to transport asbestos-containing waste
material during the loading and unloading of waste so that the signs are
visible. The markings must conform to the requirements of
61.149(d)(1) (i), (ii), and (iii).
(d) For all asbestos-containing waste material transported off the
facility site:
(1) Maintain waste shipment records, using a form similar to that
shown in Figure 4, and include the following information:
(i) The name, address, and telephone number of the waste generator.
(ii) The name and address of the local, State, or EPA Regional office
responsible for administering the asbestos NESHAP program.
(iii) The approximate quantity in cubic meters (cubic yards).
(iv) The name and telephone number of the disposal site operator.
(v) The name and physical site location of the disposal site.
(vi) The date transported.
(vii) The name, address, and telephone number of the transporter(s).
(viii) A certification that the contents of this consignment are
fully and accurately described by proper shipping name and are
classified, packed, marked, and labeled, and are in all respects in
proper condition for transport by highway according to applicable
international and government regulations.
(2) Provide a copy of the waste shipment record, described in
paragraph (d)(1) of this section, to the disposal site owners or
operators at the same time as the asbestos-containing waste material is
delivered to the disposal site.
(3) For waste shipments where a copy of the waste shipment record,
signed by the owner or operator of the designated disposal site, is not
received by the waste generator within 35 days of the date the waste was
accepted by the initial transporter, contact the transporter and/or the
owner or operator of the designated disposal site to determine the
status of the waste shipment.
(4) Report in writing to the local, State, or EPA Regional office
responsible for administering the asbestos NESHAP program for the waste
generator if a copy of the waste shipment record, signed by the owner or
operator of the designated waste disposal site, is not received by the
waste generator within 45 days of the date the waste was accepted by the
initial transporter. Include in the report the following information:
(i) A copy of the waste shipment record for which a confirmation of
delivery was not received, and
(ii) A cover letter signed by the waste generator explaining the
efforts taken to locate the asbestos waste shipment and the results of
those efforts.
(5) Retain a copy of all waste shipment records, including a copy of
the waste shipment record signed by the owner or operator of the
designated waste disposal site, for at least 2 years.
(e) Furnish upon request, and make available for inspection by the
Administrator, all records required under this section.
(55 FR 48429, Nov. 20, 1990; 56 FR 1669, Jan. 16, 1991)
40 CFR 61.151 Standard for inactive waste disposal sites for asbestos
mills and manufacturing and fabricating operations.
Each owner or operator of any inactive waste disposal site that was
operated by sources covered under 61.142, 61.144, or 61.147 and
received deposits of asbestos-containing waste material generated by the
sources, shall:
(a) Comply with one of the following:
(1) Either discharge no visible emissions to the outside air from an
inactive waste disposal site subject to this paragraph; or
(2) Cover the asbestos-containing waste material with at least 15
centimeters (6 inches) of compacted nonasbestos-containing material, and
grow and maintain a cover of vegetation on the area adequate to prevent
exposure of the asbestos-containing waste material. In desert areas
where vegetation would be difficult to maintain, at least 8 additional
centimeters (3 inches) of well-graded, nonasbestos crushed rock may be
placed on top of the final cover instead of vegetation and maintained to
prevent emissions; or
(3) Cover the asbestos-containing waste material with at least 60
centimeters (2 feet) of compacted nonasbestos-containing material, and
maintain it to prevent exposure of the asbestos-containing waste; or
(4) For inactive waste disposal sites for asbestos tailings, a
resinous or petroleum-based dust suppression agent that effectively
binds dust to control surface air emissions may be used instead of the
methods in paragraphs (a) (1), (2), and (3) of this section. Use the
agent in the manner and frequency recommended for the particular
asbestos tailings by the manufacturer of the dust suppression agent to
achieve and maintain dust control. Obtain prior written approval of the
Administrator to use other equally effective dust suppression agents.
For purposes of this paragraph, any used, spent, or other waste oil is
not considered a dust suppression agent.
(b) Unless a natural barrier adequately deters access by the general
public, install and maintain warning signs and fencing as follows, or
comply with paragraph (a)(2) or (a)(3) of this section.
(1) Display warning signs at all entrances and at intervals of 100 m
(328 ft) or less along the property line of the site or along the
perimeter of the sections of the site where asbestos-containing waste
material was deposited. The warning signs must:
(i) Be posted in such a manner and location that a person can easily
read the legend; and
(ii) Conform to the requirements for 51 cm 36 cm (20'' 14'') upright
format signs specified in 29 CFR 1910.145(d)(4) and this paragraph; and
(iii) Display the following legend in the lower panel with letter
sizes and styles of a visibility at least equal to those specified in
this paragraph.
Spacing between any two lines must be at least equal to the height of
the upper of the two lines.
(2) Fence the perimeter of the site in a manner adequate to deter
access by the general public.
(3) When requesting a determination on whether a natural barrier
adequately deters public access, supply information enabling the
Administrator to determine whether a fence or a natural barrier
adequately deters access by the general public.
(c) The owner or operator may use an alternative control method that
has received prior approval of the Administrator rather than comply with
the requirements of paragraph (a) or (b) of this section.
(d) Notify the Administrator in writing at least 45 days prior to
excavating or otherwise disturbing any asbestos-containing waste
material that has been deposited at a waste disposal site under this
section, and follow the procedures specified in the notification. If
the excavation will begin on a date other than the one contained in the
original notice, notice of the new start date must be provided to the
Administrator at least 10 working days before excavation begins and in
no event shall excavation begin earlier than the date specified in the
original notification. Include the following information in the notice:
(1) Scheduled starting and completion dates.
(2) Reason for disturbing the waste.
(3) Procedures to be used to control emissions during the excavation,
storage, transport, and ultimate disposal of the excavated
asbestos-containing waste material. If deemed necessary, the
Administrator may require changes in the emission control procedures to
be used.
(4) Location of any temporary storage site and the final disposal
site.
(e) Within 60 days of a site becoming inactive and after the
effective date of this subpart, record, in accordance with State law, a
notation on the deed to the facility property and on any other
instrument that would normally be examined during a title search; this
notation will in perpetuity notify any potential purchaser of the
property that:
(1) The land has been used for the disposal of asbestos-containing
waste material;
(2) The survey plot and record of the location and quantity of
asbestos-containing waste disposed of within the disposal site required
in 61.154(f) have been filed with the Administrator; and
(3) The site is subject to 40 CFR part 61, subpart M.
(49 FR 13661, Apr. 5, 1984, as amended at 53 FR 36972, Sept. 23,
1988. Redesignated and amended at 55 FR 48429, Nov. 20, 1990)
40 CFR 61.152 Air-cleaning.
(a) The owner or operator who uses air cleaning, as specified in
61.142(a), 61.144(b)(2), 61.145(c)(3)(i)(B)(1), 61.145(c)(4)(ii),
61.145(c)(11)(i), 61.146(b)(2), 61.147(b)(2), 61.149(b),
61.149(c)(1)(ii), 61.150(a)(1)(ii), 61.150(a)(2)(ii), and 61.155(e)
shall:
(1) Use fabric filter collection devices, except as noted in
paragraph (b) of this section, doing all of the following:
(i) Ensuring that the airflow permeability, as determined by ASTM
Method D737-75, does not exceed 9 m /3/ /min/m /2/ (30 ft /3/ /min/ft
/2/ ) for woven fabrics or 11 /3/ /min/m /2/ (35 ft /min5/m /2/ (40 ft
/3/ min/ft /2/ ) for woven and 14 m /3/ /min/m /2/ (45 ft /3/ min/ft /2/
) for felted fabrics is allowed for filtering air from asbestos ore
dryers; and
(ii) Ensuring that felted fabric weighs at least 475 grams per square
meter (14 ounces per square yard) and is at least 1.6 millimeters
(one-sixteenth inch) thick throughout; and
(iii) Avoiding the use of synthetic fabrics that contain fill yarn
other than that which is spun.
(2) Properly install, use, operate, and maintain all air-cleaning
equipment authorized by this section. Bypass devices may be used only
during upset or emergency conditions and then only for so long as it
takes to shut down the operation generating the particulate asbestos
material.
(3) For fabric filter collection devices installed after January 10,
1989, provide for easy inspection for faulty bags.
(b) There are the following exceptions to paragraph (a)(1):
(1) After January 10, 1989, if the use of fabric creates a fire or
explosion hazard, or the Administrator determines that a fabric filter
is not feasible, the Administrator may authorize as a substitute the use
of wet collectors designed to operate with a unit contacting energy of
at least 9.95 kilopascals (40 inches water gage pressure).
(2) Use a HEPA filter that is certified to be at least 99.97 percent
efficient for 0.3 micron particles.
(3) The Administrator may authorize the use of filtering equipment
other than described in paragraphs (a)(1) and (b)(1) and (2) of this
section if the owner or operator demonstrates to the Administrator's
satisfaction that it is equivalent to the described equipment in
filtering particulate asbestos material.
(49 FR 13661, Apr. 5, 1984; 49 FR 25453, June 21, 1984, as amended
at 51 FR 8199, Mar. 10, 1986. Redesignated and amended at 55 FR 48430,
Nov. 20, 1990)
40 CFR 61.153 Reporting.
(a) Any new source to which this subpart applies (with the exception
of sources subject to 61.143, 61.145, 61.146, and 61.148), which has
an initial startup date preceding the effective date of this revision,
shall provide the following information to the Administrator postmarked
or delivered within 90 days of the effective date. In the case of a new
source that does not have an initial startup date preceding the
effective date, the information shall be provided, postmarked or
delivered, within 90 days of the initial startup date. Any owner or
operator of an existing source shall provide the following information
to the Administrator within 90 days of the effective date of this
subpart unless the owner or operator of the existing source has
previously provided this information to the Administrator. Any changes
in the information provided by any existing source shall be provided to
the Administrator, postmarked or delivered, within 30 days after the
change.
(1) A description of the emission control equipment used for each
process; and
(i) If the fabric device uses a woven fabric, the airflow
permeability in m /3/ /min/m /2/ and; if the fabric is synthetic,
whether the fill yarn is spun or not spun; and
(ii) If the fabric filter device uses a felted fabric, the density in
g/m /2/ , the minimum thickness in inches, and the airflow permeability
in m /3/ /min/m /2/ .
(2) If a fabric filter device is used to control emissions,
(i) The airflow permeability in m /3/ /min/m /2/ (ft /3/ /min/ft /2/
) if the fabric filter device uses a woven fabric, and, if the fabric is
synthetic, whether the fill yarn is spun or not spun; and
(ii) If the fabric filter device uses a felted fabric, the density in
g/m /2/ (oz/yd /2/ ), the minimum thickness in millimeters (inches), and
the airflow permeability in m /3/ /min/m /2/ (ft /3/ /min/ft /2/ ).
(3) If a HEPA filter is used to control emissions, the certified
efficiency.
(4) For sources subject to 61.149 and 61.150:
(i) A brief description of each process that generates
asbestos-containing waste material; and
(ii) The average volume of asbestos-containing waste material
disposed of, measured in m /3/ /day (yd /3/ /day); and
(iii) The emission control methods used in all stages of waste
disposal; and
(iv) The type of disposal site or incineration site used for ultimate
disposal, the name of the site operator, and the name and location of
the disposal site.
(5) For sources subject to 61.151 and 61.154:
(i) A brief description of the site; and
(ii) The method or methods used to comply with the standard, or
alternative procedures to be used.
(b) The information required by paragraph (a) of this section must
accompany the information required by 61.10. Active waste disposal
sites subject to 61.154 shall also comply with this provision.
Roadways, demolition and renovation, spraying, and insulating materials
are exempted from the requirements of 61.10(a). The information
described in this section must be reported using the format of appendix
A of this part as a guide.
(Approved by the Office of Management and Budget under control number
2000-0264)
(Sec. 114. Clean Air Act as amended (42 U.S.C. 7414))
(49 FR 13661, Apr. 5, 1984. Redesignated and amended at 55 FR 48430,
Nov. 20, 1990; 56 FR 1669, Jan. 16, 1991)
40 CFR 61.154 Standard for active waste disposal sites.
Each owner or operator of an active waste disposal site that receives
asbestos-containing waste material from a source covered under 61.149,
61.150, or 61.155 shall meet the requirements of this section:
(a) Either there must be no visible emissions to the outside air from
any active waste disposal site where asbestos-containing waste material
has been deposited, or the requirements of paragraph (c) or (d) of this
section must be met.
(b) Unless a natural barrier adequately deters access by the general
public, either warning signs and fencing must be installed and
maintained as follows, or the requirements of paragraph (c)(1) of this
section must be met.
(1) Warning signs must be displayed at all entrances and at intervals
of 100 m (330 ft) or less along the property line of the site or along
the perimeter of the sections of the site where asbestos-containing
waste material is deposited. The warning signs must:
(i) Be posted in such a manner and location that a person can easily
read the legend; and
(ii) Conform to the requirements of 51 cm 36 cm (20'' 14'')
upright format signs specified in 29 CFR 1910.145(d)(4) and this
paragraph; and
(iii) Display the following legend in the lower panel with letter
sizes and styles of a visibility at least equal to those specified in
this paragraph.
Spacing between any two lines must be at least equal to the height of
the upper of the two lines.
(2) The perimeter of the disposal site must be fenced in a manner
adequate to deter access by the general public.
(3) Upon request and supply of appropriate information, the
Administrator will determine whether a fence or a natural barrier
adequately deters access by the general public.
(c) Rather than meet the no visible emission requirement of paragraph
(a) of this section, at the end of each operating day, or at least once
every 24-hour period while the site is in continuous operation, the
asbestos-containing waste material that has been deposited at the site
during the operating day or previous 24-hour period shall:
(1) Be covered with at least 15 centimeters (6 inches) of compacted
nonasbestos-containing material, or
(2) Be covered with a resinous or petroleum-based dust suppression
agent that effectively binds dust and controls wind erosion. Such an
agent shall be used in the manner and frequency recommended for the
particular dust by the dust suppression agent manufacturer to achieve
and maintain dust control. Other equally effective dust suppression
agents may be used upon prior approval by the Administrator. For
purposes of this paragraph, any used, spent, or other waste oil is not
considered a dust suppression agent.
(d) Rather than meet the no visible emission requirement of paragraph
(a) of this section, use an alternative emissions control method that
has received prior written approval by the Administrator according to
the procedures described in 61.149(c)(2).
(e) For all asbestos-containing waste material received, the owner or
operator of the active waste disposal site shall:
(1) Maintain waste shipment records, using a form similar to that
shown in Figure 4, and include the following information:
(i) The name, address, and telephone number of the waste generator.
(ii) The name, address, and telephone number of the transporter(s).
(iii) The quantity of the asbestos-containing waste material in cubic
meters (cubic yards).
(iv) The presence of improperly enclosed or uncovered waste, or any
asbestos-containing waste material not sealed in leak-tight containers.
Report in writing to the local, State, or EPA Regional office
responsible for administering the asbestos NESHAP program for the waste
generator (identified in the waste shipment record), and, if different,
the local, State, or EPA Regional office responsible for administering
the asbestos NESHAP program for the disposal site, by the following
working day, the presence of a significant amount of improperly enclosed
or uncovered waste. Submit a copy of the waste shipment record along
with the report.
(v) The date of the receipt.
(2) As soon as possible and no longer than 30 days after receipt of
the waste, send a copy of the signed waste shipment record to the waste
generator.
(3) Upon discovering a discrepancy between the quantity of waste
designated on the waste shipment records and the quantity actually
received, attempt to reconcile the discrepancy with the waste generator.
If the discrepancy is not resolved within 15 days after receiving the
waste, immediately report in writing to the local, State, or EPA
Regional office responsible for administering the asbestos NESHAP
program for the waste generator (identified in the waste shipment
record), and, if different, the local, State, or EPA Regional office
responsible for administering the asbestos NESHAP program for the
disposal site. Describe the discrepancy and attempts to reconcile it,
and submit a copy of the waste shipment record along with the report.
(4) Retain a copy of all records and reports required by this
paragraph for at least 2 years.
(f) Maintain, until closure, records of the location, depth and area,
and quantity in cubic meters (cubic yards) of asbestos-containing waste
material within the disposal site on a map or diagram of the disposal
area.
(g) Upon closure, comply with all the provisions of 61.151.
(h) Submit to the Administrator, upon closure of the facility, a copy
of records of asbestos waste disposal locations and quantities.
(i) Furnish upon request, and make available during normal business
hours for inspection by the Administrator, all records required under
this section.
(j) Notify the Administrator in writing at least 45 days prior to
excavating or otherwise disturbing any asbestos-containing waste
material that has been deposited at a waste disposal site and is
covered. If the excavation will begin on a date other than the one
contained in the original notice, notice of the new start date must be
provided to the Administrator at least 10 working days before excavation
begins and in no event shall excavation begin earlier than the date
specified in the original notification. Include the following
information in the notice:
(1) Scheduled starting and completion dates.
(2) Reason for disturbing the waste.
(3) Procedures to be used to control emissions during the excavation,
storage, transport, and ultimate disposal of the excavated
asbestos-containing waste material. If deemed necessary, the
Administrator may require changes in the emission control procedures to
be used.
(4) Location of any temporary storage site and the final disposal
site.
(Secs. 112 and 301(a) of the Clean Air Act as amended (42 U.S.C.
7412, 7601(a))
(49 FR 13661, Apr. 5, 1990. Redesignated and amended at 55 FR 48431,
Nov. 20, 1990; 56 FR 1669, Jan. 16, 1991)
40 CFR 61.155 Standard for operations that convert asbesto-containing
waste material into nonasbestos (asbestos-free) material.
Each owner or operator of an operation that converts RACM and
asbestos-containing waste material into nonasbestos (asbestos-free)
material shall:
(a) Obtain the prior written approval of the Administrator to
construct the facility. To obtain approval, the owner or operator shall
provide the Administrator with the following information:
(1) Application to construct pursuant to 61.07.
(2) In addition to the information requirements of 61.07(b)(3), a
(i) Description of waste feed handling and temporary storage.
(ii) Description of process operating conditions.
(iii) Description of the handling and temporary storage of the end
product.
(iv) Description of the protocol to be followed when analyzing output
materials by transmission electron microscopy.
(3) Performance test protocol, including provisions for obtaining
information required under paragraph (b) of this section.
(4) The Administrator may require that a demonstration of the process
be performed prior to approval of the application to construct.
(b) Conduct a start-up performance test. Test results shall include:
(1) A detailed description of the types and quantities of nonasbestos
material, RACM, and asbestos-containing waste material processed, e.g.,
asbestos cement products, friable asbestos insulation, plaster, wood,
plastic, wire, etc. Test feed is to include the full range of materials
that will be encountered in actual operation of the process.
(2) Results of analyses, using polarized light microscopy, that
document the asbestos content of the wastes processed.
(3) Results of analyses, using transmission electron microscopy, that
document that the output materials are free of asbestos. Samples for
analysis are to be collected as 8-hour composite samples (one 200-gram
(7-ounce) sample per hour), beginning with the initial introduction of
RACM or asbestos-containing waste material and continuing until the end
of the performance test.
(4) A description of operating parameters, such as temperature and
residence time, defining the full range over which the process is
expected to operate to produce nonasbestos (asbestos-free) materials.
Specify the limits for each operating parameter within which the process
will produce nonasbestos (asbestos-free) materials.
(5) The length of the test.
(c) During the initial 90 days of operation,
(1) Continuously monitor and log the operating parameters identified
during start-up performance tests that are intended to ensure the
production of nonasbestos (asbestos-free) output material.
(2) Monitor input materials to ensure that they are consistent with
the test feed materials described during start-up performance tests in
paragraph (b)(1) of this section.
(3) Collect and analyze samples, taken as 10-day composite samples
(one 200-gram (7-ounce) sample collected every 8 hours of operation) of
all output material for the presence of asbestos. Composite samples may
be for fewer than 10 days. Transmission electron microscopy (TEM) shall
be used to analyze the output material for the presence of asbestos.
During the initial 90-day period, all output materials must be stored
on-site until analysis shows the material to be asbestos-free or
disposed of as asbestos-containing waste material according to 61.150.
(d) After the initial 90 days of operation,
(1) Continuously monitor and record the operating parameters
identified during start-up performance testing and any subsequent
performance testing. Any output produced during a period of deviation
from the range of operating conditions established to ensure the
production of nonasbestos (asbestos-free) output materials shall be:
(i) Disposed of as asbestos-containing waste material according to
61.150, or
(ii) Recycled as waste feed during process operation within the
established range of operating conditions, or
(iii) Stored temporarily on-site in a leak-tight container until
analyzed for asbestos content. Any product material that is not
asbestos-free shall be either disposed of as asbestos-containing waste
material or recycled as waste feed to the process.
(2) Collect and analyze monthly composite samples (one 200-gram
(7-ounce) sample collected every 8 hours of operation) of the output
material. Transmission electron microscopy shall be used to analyze the
output material for the presence of asbestos.
(e) Discharge no visible emissions to the outside air from any part
of the operation, or use the methods specified by 61.152 to clean
emissions containing particulate asbestos material before they escape
to, or are vented to, the outside air.
(f) Maintain records on-site and include the following information:
(1) Results of start-up performance testing and all subsequent
performance testing, including operating parameters, feed
characteristic, and analyses of output materials.
(2) Results of the composite analyses required during the initial 90
days of operation under 61.155(c).
(3) Results of the monthly composite analyses required under
61.155(d).
(4) Results of continuous monitoring and logs of process operating
parameters required under 61.155 (c) and (d).
(5) The information on waste shipments received as required in
61.154(e).
(6) For output materials where no analyses were performed to
determine the presence of asbestos, record the name and location of the
purchaser or disposal site to which the output materials were sold or
deposited, and the date of sale or disposal.
(7) Retain records required by paragraph (f) of this section for at
least 2 years.
(g) Submit the following reports to the Administrator:
(1) A report for each analysis of product composite samples performed
during the initial 90 days of operation.
(2) A quarterly report, including the following information
concerning activities during each consecutive 3-month period:
(i) Results of analyses of monthly product composite samples.
(ii) A description of any deviation from the operating parameters
established during performance testing, the duration of the deviation,
and steps taken to correct the deviation.
(iii) Disposition of any product produced during a period of
deviation, including whether it was recycled, disposed of as
asbestos-containing waste material, or stored temporarily on-site until
analyzed for asbestos content.
(iv) The information on waste disposal activities as required in
61.154(f).
(h) Nonasbestos (asbestos-free) output material is not subject to any
of the provisions of this subpart. Output materials in which asbestos
is detected, or output materials produced when the operating parameters
deviated from those established during the start-up performance testing,
unless shown by TEM analysis to be asbestos-free, shall be considered to
be asbestos-containing waste and shall be handled and disposed of
according to 61.150 and 61.154 or reprocessed while all of the
established operating parameters are being met.
(55 FR 48431, Nov. 20, 1990)
40 CFR 61.156 Cross-reference to other asbestos regulations.
In addition to this subpart, the regulations referenced in Table 1
also apply to asbestos and may be applicable to those sources specified
in 61.142 through 61.151, 61.154, and 61.155 of this subpart. These
cross-references are presented for the reader's information and to
promote compliance with the cited regulations.
(55 FR 48432, Nov. 20, 1990)
40 CFR 61.157 Delegation of authority.
(a) In delegating implementation and enforcement authority to a State
under section 112(d) of the Act, the authorities contained in paragraph
(b) of this section shall be retained by the Administrator and not
transferred to a State.
(b) Authorities that will not be delegated to States:
(1) Section 61.149(c)(2)
(2) Section 61.150(a)(4)
(3) Section 61.151(c)
(4) Section 61.152(b)(3)
(5) Section 61.154(d)
(6) Section 61.155(a).
(55 FR 48433, Nov. 20, 1990)
40 CFR 61.157 Subpart N -- National Emission Standard for Inorganic
Arsenic Emissions from Glass Manufacturing Plants
Source: 51 FR 28025, Aug. 4, 1986, unless otherwise noted.
40 CFR 61.160 Applicability and designation of source.
(a) The source to which this subpart applies is each glass melting
furnace that uses commercial arsenic as a raw material. This subpart
does not apply to pot furnaces.
(b) Rebricking is not considered construction or modification for the
purposes of 61.05(a).
40 CFR 61.161 Definitions.
The terms used in this subpart are defined in the Clean Air Act, in
61.02, or in this section as follows:
Arsenic-containing glass type means any glass that is distinguished
from other glass solely by the weight percent of arsenic added as a raw
material and by the weight percent of arsenic in the glass produced.
Any two or more glasses that have the same weight percent of arsenic in
the raw materials as well as in the glass produced shall be considered
to belong to one arsenic-containing glass type, without regard to the
recipe used or any other characteristics of the glass or the method of
production.
By-pass the control device means to operate the glass melting furnace
without operating the control device to which that furnace's emissions
are directed routinely.
Commercial arsenic means any form of arsenic that is produced by
extraction from any arsenic-containing substance and is intended for
sale or for intentional use in a manufacturing process. Arsenic that is
a naturally occurring trace constituent of another substance is not
considered ''commercial arsenic.''
Cullet means waste glass recycled to a glass melting furnace.
Glass melting furnace means a unit comprising a refractory vessel in
which raw materials are charged, melted at high temperature, refined,
and conditioned to produce molten glass. The unit includes foundations,
superstructure and retaining walls, raw material charger systems, heat
exchangers, melter cooling system, exhaust system, refractory brick
work, fuel supply and electrical boosting equipment, integral control
systems and instrumentation, and appendages for conditioning and
distributing molten glass to forming apparatuses. The forming
apparatuses, including the float bath used in flat glass manufacturing,
are not considered part of the glass melting furnace.
Glass produced means the glass pulled from the glass melting furnace.
Inorganic arsenic means the oxides and other noncarbon compounds of
the element arsenic included in particulate matter, vapors, and
aerosols.
Malfunction means any sudden failure of air pollution control
equipment or process equipment or of a process to operate in a normal or
usual manner so that emissions of arsenic are increased.
Pot furnace means a glass melting furnace that contains one or more
refractory vessels in which glass is melted by indirect heating. The
openings of the vessels are in the outside wall of the furnace and are
covered with refractory stoppers during melting.
Rebricking means cold replacement of damaged or worn refractory parts
of the glass melting furnace. Rebricking includes replacement of the
refractories comprising the bottom, sidewalls, or roof of the melting
vessel; replacement of refractory work in the heat exchanger; and
replacement of refractory portions of the glass conditioning and
distribution system.
Shutdown means the cessation of operation of an affected source for
any purpose.
Theoretical arsenic emissions factor means the amount of inorganic
arsenic, expressed in grams per kilogram of glass produced, as
determined based on a material balance.
Uncontrolled total arsenic emissions means the total inorganic
arsenic in the glass melting furnace exhaust gas preceding any add-on
emission control device.
(51 FR 28025, Aug. 4, 1986; 51 FR 35355, Oct. 3, 1986)
40 CFR 61.162 Emission limits.
(a) The owner or operator of an existing glass melting furnace
subject to the provisions of this subpart shall comply with either
paragraph (a)(1) or (a)(2) of this section; except as provided in
paragraph (c) of this section.
(1) Uncontrolled total arsenic emissions from the glass melting
furnace shall be less than 2.5 Mg per year, or
(2) Total arsenic emissions from the glass melting furnace shall be
conveyed to a control device and reduced by at least 85 percent.
(b) The owner or operator of a new or modified glass melting furnace
subject to the provisions of this subpart shall comply with either
paragraph (b)(1) or (b)(2) of this section, except as provided in
paragraph (c) of this section.
(1) Uncontrolled total arsenic emissions from the glass melting
furnace shall be less than 0.4 Mg per year, or
(2) Total arsenic emissions from the glass melting furnace shall be
conveyed to a control device and reduced by at least 85 percent.
(c) An owner or operator of a source subject to the requirements of
this section may, after approval by the Administrator, bypass the
control device to which arsenic emissions from the furnace are directed
for a limited period of time for designated purposes such as maintenance
of the control device, as specified in 61.165(e).
(d) At all times, including periods of startup, shutdown, and
malfunction, the owner or operator of a glass melting furnace subject to
the provisions of this subpart shall operate and maintain the furnace
and associated air pollution control equipment in a manner consistent
with good air pollution control practice for minimizing emissions of
inorganic arsenic to the atmosphere to the maximum extent practicable.
Determination of whether acceptable operating and maintenance procedures
are being used will be based on information available to the
Administrator, which may include, but is not limited to, monitoring
results, review of operating and maintenance procedures, inspection of
the source, and review of other records.
40 CFR 61.163 Emission monitoring.
(a) An owner or operator of a glass melting furnace subject to the
emission limit in 61.162(a)(2) or 61.162(b)(2) shall:
(1) Install, calibrate, maintain, and operate a continuous monitoring
system for the measurement of the opacity of emissions discharged into
the atmosphere from the control device; and
(2) Install, calibrate, maintain, and operate a monitoring device for
the continuous measurement of the temperature of the gas entering the
control device.
(b) All continuous monitoring systems and monitoring devices shall be
installed and operational prior to performance of an emission test
required by 61.164(a). Verification of operational status shall, at a
minimum, consist of an evaluation of the monitoring system in accordance
with the requirements and procedures contained in Performance
Specification 1 of appendix B of 40 CFR part 60.
(c) During the emission test required in 61.164(a) each owner or
operator subject to paragraph (a) of this section shall:
(1) Conduct continuous opacity monitoring from the beginning of the
first test run until the completion of the third test run. Process and
control equipment shall be operated in a manner that will minimize
opacity of emissions, subject to the Administrator's approval.
(2) Calculate 6-minute opacity averages from 24 or more data points
equally spaced over each 6-minute period during the test runs.
(3) Determine, based on the 6-minute opacity averages, the opacity
value corresponding to the 97.5 percent upper confidence level of a
normal or lognormal (whichever the owner or operator determines is more
representative) distribution of the average opacity values.
(4) Conduct continuous monitoring of the temperature of the gas
entering the control device from the beginning of the first test run
until completion of the third test run.
(5) Calculate 15-minute averages of the temperature of the gas
entering the control device during each test run.
(d) An owner or operator may redetermine the values described in
paragraph (c) of this section during any emission test that demonstrates
compliance with the emission limits in 61.162(a)(2) or 61.162(b)(2).
(e) The requirements of 60.13(d) and 60.13(f) shall apply to an
owner or operator subject to paragraph (a) of this section.
(f) Except for system breakdowns, repairs, calibration checks, and
zero and span adjustments required under 60.13(d), all continuous
monitoring systems shall be in continuous operation and shall meet
minimum frequency of operation requirements by completing a minimum of
one cycle of sampling and analyzing for each successive 10-second period
and one cycle of data recording for each successive 6-minute period.
(g) An owner or operator subject to paragraph (a) of this section
shall:
(1) Reduce all opacity data to 6-minute averages. Six-minute
averages shall be calculated from 24 or more data points equally spaced
over each 6-minute period. Data recorded during periods of monitoring
system breakdowns, repairs, calibration checks, and zero and span
adjustments shall not be included in the data averages calculated under
this paragraph, and
(2) Calculate 15-minute averages of the temperature of the gas
entering the control device for each 15-minute operating period.
(h) After receipt and consideration of written application, the
Administrator may approve alternative monitoring systems for the
measurement of one or more process or operating parameters that is or
are demonstrated to enable accurate and representative monitoring of a
properly operating control device. Upon approval of an alternative
monitoring system for an affected source, the Administrator will specify
requirements to replace the requirements of paragraphs (a) -- (g) of
this section for that system.
40 CFR 61.164 Test methods and procedures.
(a) To demonstrate compliance with 61.162, the owner or operator
shall conduct emission tests, reduce test data, and follow the
procedures specified in this section unless the Administrator:
(1) Specifies or approves, in specific cases, the use of a reference
method with minor changes in methodology;
(2) Approves the use of an equivalent method;
(3) Approves the use of an alternative method the results of which he
has determined to be adequate for indicating whether a specific source
is in compliance; or
(4) Waives the requirement for emission tests as provided under
61.13.
(b) Unless a waiver of emission testing is obtained, the owner or
operator shall conduct emission tests required by this section:
(1) No later than 90 days after the effective date of this subpart
for a source that has an initial startup date preceding the effective
date; or
(2) No later than 90 days after startup for a source that has an
initial startup date after the effective date.
(3) At such other times as may be required by the Administrator under
section 114 of the Act.
(4) While the source is operating under such conditions as the
Administrator may specify, based on representative performance of the
source.
(c) To demonstrate compliance with 61.162(a)(1) when less than 8.0
Mg per year of elemental arsenic is added to any existing glass melting
furnace, or to demonstrate compliance with 61.162(b)(1) when less than
1.0 Mg per year of elemental arsenic is added to any new or modified
glass melting furnace, an owner or operator shall:
(1) Derive a theoretical uncontrolled arsenic emission factor (T), in
grams of elemental arsenic per kilogram of glass produced, based on
material balance calculations for each arsenic-containing glass type (i)
produced during the 12-month period, as follows:
Ti = (Abi Wbi) + (Aci Wci) ^ Agi
Where:
Ti = the theoretical uncontrolled arsenic emission factor (g/kg) for
each glass type (i).
Abi = fraction by weight of elemental arsenic in the fresh batch for
each glass type (i).
Wbi = weight (g) of fresh batch melted per kg of glass produced for
each glass type (i).
Aci = fraction by weight of elemental arsenic in cullet for each
glass type (i).
Wci = weight (g) of cullet melted per kg of glass produced for each
glass type (i).
Agi = weight (g) of elemental arsenic per kg glass produced for each
glass type (i).
(2) Estimate theoretical uncontrolled arsenic emissions for the
12-month period for each arsenic-containing glass type as follows:
Where:
Yi = the theoretical uncontrolled arsenic emission estimate for the
12-month period for each glass type (Mg/year).
Ti = the theoretical uncontrolled arsenic emission factor for each
type of glass (i) produced during the 12-month period as calculated in
paragraph (c)(1) of this section (g/kg).
Gi = the quantity (kg) of each arsenic-containing glass type (i)
produced during the 12-month period.
(3) Estimate the total theoretical uncontrolled arsenic emissions for
the 12-month period by finding the sum of the values calculated for Yi
in paragraph (c)(2) of this section.
(4) If the value determined in paragraph (c)(3) of this section is
equal to or greater than the applicable limit in 61.162(a)(1) or
(b)(1), conduct the emission testing and calculations described in
paragraphs (d)(1) through (d)(5) of this section. If the value is less
than the applicable limit, the source is in compliance and no emission
testing or additional calculations are required.
(d) To demonstrate compliance with 61.162(a)(1) when 8.0 Mg per year
or more of elemental arsenic are added to any existing glass melting
furnace, or to demonstrate compliance with 61.162(b)(1) when 1.0 Mg per
year or more of elemental arsenic is added to any new or modified glass
melting furnace, an owner or operator shall:
(1) Estimate the theoretical uncontrolled arsenic emissions for each
glass type for the 12-month period by performing the calculations
described in paragraphs (c)(1) and (c)(2) of this section.
(2) Conduct emission testing to determine the actual uncontrolled
arsenic emission rate during production of the arsenic-containing glass
type with the highest theoretical uncontrolled arsenic emissions as
calculated under paragraph (d)(1) of this section. The owner or
operator shall use the following test methods and procedures:
(i) Use Method 108 in appendix B to this part for determinig the
arsenic emission rate (g/h). The emission rate shall equal the
arithmetic mean of the results of three 60-minute test runs.
(ii) Use the following methods in appendix A to 40 CFR part 60:
(A) Method 1 for sample and velocity traverse.
(B) Method 2 for velocity and volumetric flowrate.
(C) Method 3 for gas analysis.
(D) For sources equipped with positive pressure fabric filters, use
Section 4 of Method 5D to determine a suitable sampling location and
procedure.
(3) Determine the actual uncontrolled arsenic emission factor (Ra) in
grams of elemental arsenic per kilogram of glass produced, as follows:
Ra=Ea'P
Where:
Ra=the actual uncontrolled arsenic emission factor (g/kg).
Ea=the actual uncontrolled arsenic emission rate (g/h) from paragraph
(d)(2) of this section.
P=the rate of glass production (kg/h), determined by dividing the
weight (kg) of glass pulled from the furnace during the emission test by
the number of hours (h) taken to perform the test under paragraph (d)(2)
of this section.
(4) Calculate a correction factor to relate the theoretical and the
actual uncontrolled arsenic emission factors as follows:
F=Ra'Ti
Where:
F=the correction factor.
Ra=the actual uncontrolled arsenic emission factor (g/kg) determined
in paragraph (d)(3) of this section.
Ti=the theoretical uncontrolled arsenic emission factor (g/kg)
determined in paragraph (c)(1) of this section for the same glass type
for which Ra was determined.
(5) Determine the uncontrolled arsenic emission rate for the 12-month
period, as follows:
Where:
U=the uncontrolled arsenic emission rate for the 12-month period
(Mg/year).
Ti=the theoretical uncontrolled arsenic emission factor for each
arsenic-containing glass type (i) produced during the 12-month period,
as calculated in paragraph (c)(1) of this section (g/kg).
F=the correction factor calculated in paragraph (d)(4) of this
section.
Gi=the quantity (kg) of each arsenic-containing glass type (i)
produced during the 12-month period.
n=the number of arsenic-containing glass types produced during the
12-month period.
(6) If the value determined in paragraph (d)(5) of this section is
less than the applicable limit in 61.162(a)(1) or (b)(1), the source is
in compliance.
(e) To demonstrate compliance with 61.162(a)(2) or (b)(2), an owner
or operator shall:
(1) Conduct emission testing to determine the percent reduction of
inorganic arsenic emissions being achieved by the control device, using
the following test methods and procedures:
(i) Use Method 108 in appendix B to this part to determine the
concentration of arsenic in the gas streams entering and exiting the
control device. Conduct three 60-minute test runs, each consisting of
simultaneous testing of the inlet and outlet gas streams. The gas
streams shall contain all the gas exhausted from the glass melting
furnace.
(ii) Use the following methods in appendix A to 40 CFR part 60:
(A) Method 1 for sample and velocity traverses.
(B) Method 2 for velocity and volumetric flowrate.
(C) Method 3 for gas analysis.
(D) For sources equipped with positive pressure fabric filters, use
Section 4 of Method 5D to determine a suitable sampling location and
procedure.
(2) Calculate the percent emission reduction for each run as follows:
Where:
D= the percent emission reduction.
Cb= the arsenic concentration of the stack gas entering the control
device, as measured by Method 108.
Ca= the arsenic concentration of the stack gas exiting the control
device, as measured by Method 108.
(3) Determine the average percent reduction of arsenic by calculating
the arithmetic mean of the results for the three runs. If it is at
least 85 percent, the source is in compliance.
(51 FR 28025, Aug. 4, 1986; 51 FR 35355, Oct. 3, 1986, as amended at
55 FR 22027, May 31, 1990)
40 CFR 61.165 Reporting and recordkeeping requirements.
(a) Each owner or operator of a source subject to the requirements of
61.162 shall maintain at the source for a period of at least 2 years
and make available to the Administrator upon request a file of the
following records:
(1) All measurements, including continuous monitoring for measurement
of opacity, and temperature of gas entering a control device;
(2) Records of emission test data and all calculations used to
produce the required reports of emission estimates to demonstrate
compliance with 61.162;
(3) All continous monitoring system performance evaluations,
including calibration checks and adjustments;
(4) The occurrence and duration of all startups, shutdowns, and
malfunctions of the furnace;
(5) All malfunctions of the air pollution control system;
(6) All periods during which any continuous monitoring system or
monitoring device is inoperative;
(7) all records of maintenance and repairs for each air pollution
control system, continuous monitoring system, or monitoring device;
(b) Each owner or operator who is given approval by the Administrator
to bypass a control device under paragraph (e) of this section shall
maintain at the source for a period of at least 2 years and make
available to the Administrator upon request a file of the following
records:
(1) The dates the control device is bypassed; and
(2) Steps taken to minimize arsenic emissions during the period the
control device was bypassed.
(c) Each owner or operator of a source subject to the emission limit
in 61.162(a)(1) or (b)(1) shall determine and record at the end of
every 6 months the uncontrolled arsenic emission rate for the preceding
and forthcoming 12-month periods. The determinations shall:
(1) Be made by following the procedures in 61.164(c)(1), (c)(2), and
(c)(3); or in 61.164(d)(5), whichever is applicable; and
(2) Take into account changes in production rates, types of glass
produced, and other factors that would affect the uncontrolled arsenic
emission rate.
(d) Each owner or operator of a source subject to the provisions of
this subpart shall:
(1) Provide the Administrator 30 days prior notice of any emission
test required in 61.164 to afford the Administrator the opportunity to
have an observer present; and
(2) Submit to the Administrator a written report of the results of
the emission test and associated calculations required in 61.164(d) or
(e), as applicable, within 60 days after conducting the test.
(3) Submit to the Administrator a written report of the arsenic
emission estimates calculated under 61.164(c):
(i) Within 45 days after the effective date of this subpart for a
source that has an initial startup date preceding the effective date;
or
(ii) Within 45 days after startup for a source that has an initial
startup date after the effective date.
(4) Submit to the Adminstrator a written report of the uncontrolled
arsenic emission rates determined in accordance with paragraph (c) of
this section, if:
(i) The emission rate for the preceding 12-month period (or preceding
6-month period for the first 6-month determination) exceeded the
applicable limit in 61.162(a)(1) or (b)(1).
(ii) The emission rate for the forthcoming 12-month period will
exceed the applicable limit in 61.162(a)(1) or (b)(1). In this case,
the owner or operator shall also notify the Administrator of the
anticipated date of the emission test to demonstrate compliance with the
applicable limit in 61.162(a)(2) or (b)(2).
(5) Ensure that the reports required in paragraph (d)(4) of this
section are postmarked by the tenth day following the end of the 6-month
reporting period.
(e) To obtain approval to bypass a control device, as provided in
61.162(c), an owner or operator of a source subject to this subpart may
make written application to the Administrator. Each application for
such a waiver shall be submitted to the Administrator no later than 60
days before the bypass period would begin and shall include:
(1) Name and address of the owner or operator;
(2) Location of the source;
(3) A brief description of the nature, size, design, and method of
operation of the source;
(4) The reason it is necessary to by-pass the control device;
(5) The length of time it will be necessary to by-pass the control
device;
(6) Steps that will be taken to minimize arsenic emissions during the
period the control device will be by-passed.
(7) The quantity of emissions that would be released while the
control device is by-passed if no steps were taken to minimize
emissions;
(8) The expected reduction in emissions during the by-pass period due
to the steps taken to minimize emissions during this period; and
(9) The type of glass to be produced during the bypass period, and,
if applicable, an explanation of why non-arsenic or
lower-arsenic-containing glass cannot be melted in the furnace during
the bypass period.
(f) Each owner or operator required to install and operate a
continuous opacity monitoring system under 61.163 shall:
(1) Submit a written report to the Administrator of the results of
the continuous monitoring system evaluation required under 61.163(b)
within 60 days after conducting the evaluation.
(2) Submit a written report to the Administrator every 6 months if
excess opacity occurred during the preceding 6-month period. For
purposes of this paragraph, an occurrence of excess opacity is any
6-minute period during which the average opacity, as measured by the
continuous monitoring system, exceeds the opacity level determined under
61.163(c)(3) or the opacity level redetermined under 61.163(d).
(3) Ensure that any semiannual report of excess opacity required by
paragraph (f)(2) of this section is postmarked by the thirtieth day
following the end of the 6-month period and includes the following
information:
(i) The magnitude of excess opacity, any conversion factor(s) used,
and the date and time of commencement and completion of each occurrence
of excess opacity.
(ii) Specific identification of each occurrence of excess opacity
that occurs during startups, shutdowns, and malfunctions of the source.
(iii) The date and time identifying each period during which the
continuous monitoring system was inoperative, except for zero and span
checks, and the nature of the system repairs or adjustments.
(Approved by the Office of Management and Budget under control number
2060-0043)
40 CFR 61.165 Subpart O -- National Emission Standard for Inorganic
Arsenic Emissions from Primary Copper Smelters
Source: 51 FR 28029, Aug. 4, 1986, unless otherwise noted.
40 CFR 61.170 Applicability and designation of source.
The provisions of this subpart are applicable to each copper
converter at any new or existing primary copper smelter, except as noted
in 61.172(a).
40 CFR 61.171 Definitions.
All terms used in this subpart shall have the meanings given to them
in the Act, in subpart A of part 61, and in this section as follows:
Blowing means the injection of air or oxygen-enriched air into a
molten converter bath.
Charging means the addition of a molten or solid material to a copper
converter.
Control device means the air pollution control equipment used to
collect particulate matter emissions.
Converter arsenic charging rate means the hourly rate at which
arsenic is charged to the copper converters in the copper converter
department based on the arsenic content of the copper matte and of any
lead matte that is charged to the copper converters.
Copper converter means any vessel in which copper matte is charged
and is oxidized to copper.
Copper converter department means all copper converters at a primary
copper smelter.
Copper matte means any molten solution of copper and iron sulfides
produced by smelting copper sulfide ore concentrates or calcines.
Holding of a copper converter means suspending blowing operations
while maintaining in a heated state the molten bath in the copper
converter.
Inorganic arsenic means the oxides and other noncarbon compounds of
the element arsenic included in particulate matter, vapors, and
aerosols.
Lead matte means any molten solution of copper and other metal
sulfides produced by reduction of sinter product from the oxidation of
lead sulfide ore concentrates.
Malfunction means any sudden failure of air pollution control
equipment or process equipment or of a process to operate in a normal or
usual manner so that emissions of inorganic arsenic are increased.
Opacity means the degree to which emissions reduce the transmission
of light.
Particulate matter means any finely divided solid or liquid material,
other than uncombined water, as measured by the specified reference
method.
Pouring means the removal of blister copper from the copper converter
bath.
Primary copper smelter means any installation or intermediate process
engaged in the production of copper from copper-bearing materials
through the use of pyrometallurgical techniques.
Primary emission control system means the hoods, ducts, and control
devices used to capture, convey, and collect process emissions.
Process emissions means inorganic arsenic emissions from copper
converters that are captured directly at the source of generation.
Secondary emissions means inorganic arsenic emissions that escape
capture by a primary emission control system.
Secondary hood system means the equipment (including hoods, ducts,
fans, and dampers) used to capture and transport secondary inorganic
arsenic emissions.
Shutdown means the cessation of operation of a stationary source for
any reason.
Skimming means the removal of slag from the molten converter bath.
40 CFR 61.172 Standard for new and existing sources.
(a) The provisions of paragraphs (b)-(f) of this section do not apply
to any copper converter at a facility where the total arsenic charging
rate for the copper converter department averaged over a 1-year period
is less than 75 kg/h, as determined under 61.174(f).
(b) The owner or operator of each copper converter subject to the
provisions of this subpart shall reduce inorganic arsenic emissions to
the atmosphere by meeting the following design, equipment, work
practice, and operational requirements:
(1) Install, operate, and maintain a secondary hood system on each
copper converter. Each secondary hood system shall consist of a hood
enclosure, air curtain fan(s), exhaust system fan(s), and ductwork that
conveys the captured emissions to a control device, and shall meet the
following specifications:
(i) The configuration and dimensions of the hood enclosure shall be
such that the copper converter mouth, charging ladles, skimming ladles,
and any other material transfer vessels used will be housed within the
confines or influence of the hood enclosure during each mode of copper
converter operation.
(ii) The back of the hood enclosure shall be fully enclosed and
sealed against the primary hood. Portions of the side-walls in contact
with the copper converter shall be sealed against the converter.
(iii) Openings in the top and front of the hood enclosure to allow
for the entry and egress of ladles and crane appartus shall be minimized
to the fullest extent practicable.
(iv) The hood enclosure shall be fabricated in such a manner and of
materials of sufficient strength to withstand incidental contact with
ladles and crane apparatus with no significant damage.
(v) One side-wall of the hood enclosure shall be equipped with a
horizontal-slotted plenum along the top, and the opposite side-wall
shall be equipped with an exhaust hood. The horizontal-slotted plenum
shall be designed to allow the distance from the base to the top of the
horizontal slot to be adjustable up to a dimension of 76 mm.
(vi) The horizontal-slotted plenum shall be connected to a fan. When
activated, the fan shall push air through the horizontal slot, producing
a horizontal air curtain above the copper converter that is directed to
the exhaust hood. The fan power output installed shall be sufficient to
overcome static pressure losses through the ductwork upstream of the
horizontal-slotted plenum and across the plenum, and to deliver at least
22,370 watts (30 air horsepower) at the horizontal-slotted plenum
discharge.
(vii) The exhaust hood shall be sized to completely intercept the
airstream from the horizontal-slotted plenum combined with the
additional airflow resulting from entrainment of the surrounding air.
The exhaust hood shall be connected to a fan. When activated, the fan
shall pull the combined airstream into the exhaust hood.
(viii) The entire secondary hood system shall be equipped with
dampers and instrumentation, as appropriate, so that the desired air
curtain and exhaust flow are maintained during each mode of copper
converter operation.
(2) Optimize the capture of secondary inorganic arsenic emissions by
operating the copper converter and secondary hood system at all times as
follows:
(i) Copper converter. (A) Increase the air curtain and exhaust flow
rates to their optimum conditions prior to raising the primary hood and
rolling the copper converter out for charging, skimming, or pouring.
(B) Once rolled out, prior to the commencement of skimming or
pouring, hold the copper converter in an idle position until fuming from
the molten bath has been minimized.
(C) During skimming, raise the receiving ladle off the ground and
position the ladle as close to the copper converter mouth as possible to
minimize the drop distance between the converter mouth and the receiving
ladle.
(D) Control the rate of flow into the receiving ladle to the extent
practicable to minimize fuming.
(E) Upon the completion of each charge, withdraw the charging ladle
or vessel used from the confines of the secondary hood in a slow,
deliberate manner.
(F) During charging, skimming, or pouring, ensure that the crane
block does not disturb the air flow between the horizontal-slotted
plenum and the exhaust hood.
(ii) Secondary hood system. (A) Operate the secondary hood system
under conditions that will result in the maximum capture of inorganic
arsenic emissions.
(B) Within 30 days after the effective date of this subpart, or
within 30 days after the initial operation of each secondary hood
system, whichever comes later, provide to the Administrator a list of
operating conditions for the secondary hood system that will result in
the maximum capture of inorganic arsenic emissions. This list shall
specify the operating parameters for the following:
(1) The dimensions of the horizontal slot.
(2) The velocity of air through the horizontal slot during each mode
of converter operation.
(3) The distance from the horizontal slot to the exhaust hood.
(4) The face velocity at the opening of the exhaust hood during each
mode of converter operation.
(C) Operate the secondary hood system under the conditions listed in
paragraph (b)(2)(ii)(B) of this section, unless otherwise specified by
the Administrator.
(D) Notify the Administrator in writing within 30 days if there is
any change in the operating conditions submitted pursuant to the
requirements of paragraph (b)(2)(ii)(B) that will result in any
reduction in the maximum capture of inorganic arsenic emissions.
(3) Comply with the following inspection and maintenance requirements
after installing the secondary hood system required in paragraph (b)(1)
of this section:
(i) At least once every month, visually inspect the components of the
secondary hood system that are exposed to potential damage from crane
and ladle operation, including the hood enclosure, side- and back-wall
hood seals, and the horizontal slot.
(ii) Replace or repair any defective or damaged components of the
secondary hood system within 30 days after discovering the defective or
damaged components.
(c) No owner or operator of a copper converter subject to the
provisions of this subpart shall cause or allow to be discharged into
the atmosphere any copper converter secondary emissions that exit from a
control device and contain particulate matter in excess of 11.6
milligrams per dry standard cubic meter.
(d) The owner or operator of a copper converter subject to the
provisions of this subpart shall submit a description of a plan for
control of inorganic arsenic emissions from the copper converter and
associated air pollution control equipment. This plan shall be
submitted within 90 days after the effective date of this subpart,
unless a waiver of compliance is granted under 61.11. If a waiver of
compliance is granted, the plan shall be submitted on a date set by the
Administrator. Approval of the plan will be granted by the
Administrator provided he finds that:
(1) It includes a systematic procedure for identifying malfunctions
and for reporting them immediately to smelter supervisory personnel.
(2) It specifies the procedures that will be followed to ensure that
equipment or process breakdowns due entirely or in part to poor
maintenance or other preventable conditions do not occur.
(3) It specifies the measures that will be taken to ensure compliance
with paragraph (b)(2) of this section.
(e) The owner or operator shall implement the plan required under
paragraph (d) of this section unless otherwise specified by the
Administrator.
(f) At all times, including periods of startup, shutdown, and
malfunction, the owner or operator of a copper converter subject to the
provisions of this subpart shall operate and maintain the converter and
associated air pollution control equipment in a manner consistent with
good air pollution control practice for minimizing emissions of
inorganic arsenic to the atmosphere to the maximum extent practicable.
Determination of whether acceptable operating and maintenance procedures
are being used will be based on information available to the
Administrator, which may include, but is not limited to, monitoring
results, review of operating and maintenance procedures, inspection of
the source, and review of other records.
40 CFR 61.173 Compliance provisions.
(a) The owner or operator of each copper converter to which
61.172(b) -- (f) applies shall demonstrate compliance with the
requirements of 61.172(b)(1) as follows:
(1) The owner or operator of each existing copper converter shall
install a secondary hood system to meet the requirements of
61.172(b)(1) no later than 90 days after the effective date, unless a
waiver of compliance has been approved by the Administrator in
accordance with 61.11.
(2) The owner or operator of each new copper converter shall install
a secondary hood system to meet the requirements of 61.172(b)(1) prior
to the initial startup of the converter, except that if startup occurs
prior to the effective date, the owner or operator shall meet the
requirements of 61.172(b)(1) on the effective date.
40 CFR 61.174 Test methods and procedures.
(a) To determine compliance with 61.172(c), the owner or operator
shall conduct emission tests and reduce the test data in accordance with
the test methods and procedures contained in this section unless the
Administrator:
(1) Specifies or approves, in specific cases, the use of a reference
method with minor changes in methodology,
(2) Approves the use of an equivalent method,
(3) Approves the use of an alternative method, the results of which
he has determined to be adequate for indicating whether a specific
source is in compliance, or
(4) Waives the requirement for emission tests as provided in 61.13.
(b) The owner or operator shall conduct the emission tests required
in paragraph (a) of this section:
(1) After achieving the optimum operating conditions submitted under
60.172(b)(2)(ii)(B) for the equipment required in 61.172(b)(1), but no
later than 90 days after the effective date of this subpart in the case
of an existing copper converter or a copper converter that has an
initial startup date preceding the effective date, or
(2) After achieving the optimum operating conditions submitted under
60.172(b)(2)(ii)(B) for the equipment required in 61.172(b)(1), but no
later than 90 days after startup in the case of a new copper converter,
initial startup of which occurs after the effective date, or
(3) At such other times as may be required by the Administrator under
section 114 of the Act.
(c) The owner or operator shall conduct each emission test under
representative operating conditions and at sample locations subject to
the Administrator's approval, and shall make available to the
Administrator such records as may be necessary to determine the
conditions of the emission test.
(d) For the purpose of determining compliance with 61.172(c), the
owner or operator shall use reference methods in 40 CFR part 60,
appendix A, as follows:
(1) Method 5 for the measurement of particulate matter,
(2) Method 1 for sample and velocity traverses,
(3) Method 2 for velocity and volumetric flow rate,
(4) Method 3 for gas analysis, and
(5) Method 4 for stack gas moisture.
(e) For Method 5, the sampling time for each run shall be at least 60
minutes and the minimum sampling volume shall be 0.85 dscm (30 dscf)
except that smaller times or volumes when necessitated by process
variables or other factors may be approved by the Administrator.
(f) For the purpose of determining applicability under 61.172(a),
the owner or operator shall determine the converter arsenic charging
rate as follows:
(1) Collect daily grab samples of copper matte and any lead matte
charged to the copper converters.
(2) Each calendar month, from the daily grab samples collected under
paragraph (f)(1) of this section, put together a composite copper matte
sample and a composite lead matte sample. Analyze the composite samples
individually using Method 108A, 108B, or 108C to determine the weight
percent of inorganic arsenic contained in each sample.
(3) Calculate the converter arsenic charging rate once per month
using the following equation:
Where:
Rc is the converter arsenic charging rate (kg/h).
Ac is the monthly average weight percent of arsenic in the copper
matte charged during the month (%) as determined under paragraph (f)(2)
of this section.
Al is the monthly average weight percent of arsenic in the lead matte
charged during the month (%) as determined under paragraph (f)(2) of
this section.
Wci is the total weight of copper matte charged to a copper converter
during the month (kg).
Wli is the total weight of lead matte charged to a copper converter
during the month (kg).
Hc is the total number of hours the copper converter department was
in operation during the month (h).
n is the number of copper converters in operation during the month.
(4) Determine an annual arsenic charging rate for the copper
converter department once per month by computing the arithmetic average
of the 12 monthly converter arsenic charging rate values (Rc) for the
preceding 12-month period.
(g) An owner or operator may petition the Administrator for a
modified sampling and analysis schedule if analyses performed for the
first 12-month period after the effective date show the source to be
considerably below the applicability limit prescribed in 61.172(a).
(51 FR 28029, Aug. 4, 1986, as amended at 55 FR 22027, May 31, 1990)
40 CFR 61.175 Monitoring requirements.
(a) Each owner or operator of a source that is subject to the
emission limit specified in 61.172(c) shall install, calibrate,
maintain, and operate a continuous monitoring system for the measurement
of the opacity of emissions discharged from the control device according
to the following procedures:
(1) Ensure that each system is installed and operational no later
than 90 days after the effective date of this subpart for a source that
has an initial startup date preceding the effective date; and no later
than 90 days after startup for other sources. Verification of the
operational status shall, as a minimum, consist of an evaluation of the
monitoring system in accordance with the requirements and procedures
contained in Performance Specification 1 of appendix B of 40 CFR part
60.
(2) Comply with the provisions of 60.13(d) of 40 CFR part 60.
(3) Except for system breakdowns, repairs, calibration checks, and
zero span adjustments, ensure that each continuous monitoring system is
in continuous operation and meets frequency of operation requirements by
completing a minimum of one cycle of sampling and analysis for each
successive 10-second period and one cycle of data recording for each
successive 6-minute period. Each data point shall represent the opacity
measured for one cycle of sampling and analysis and shall be expressed
as percent opacity.
(b) Except as required in paragraph (c) of this section, calculate
1-hour opacity averages from 360 or more consecutive data points equally
spaced over each 1-hour period. Data recorded during periods of
monitoring system breakdowns, repairs, calibration checks, and zero and
span adjustments shall not be included in the data averages computed
under this paragraph.
(c) No later than 60 days after each continuous opacity monitoring
system required in paragraph (a) of this section becomes operational,
the owner or operator shall establish a reference opacity level for each
monitored emission stream according to the following procedures:
(1) Conduct continuous opacity monitoring over a preplanned period of
not less than 36 hours during which the processes and emission control
equipment upstream of the monitoring system are operating under
representative operating conditions subject to the Administrator's
approval. This period shall include the time during which the emission
test required by 61.13 is conducted.
(2) Calculate 6-minute averages of the opacity readings using 36 or
more consecutive data points equally spaced over each 6-minute period.
(3) Calculate 1-hour average opacity values using 10 successive
6-minute average opacity values (i.e., calculate a new 1-hour average
opacity value every 6 minutes). Determine the highest 1-hour average
opacity value observed during the 36-hour preplanned test period.
(4) Calculate the reference opacity level by adding 5 percent opacity
to the highest 1-hour average opacity calculated in paragraph (c)(3) of
this section.
(d) The owner or operator may redetermine the reference opacity level
for the copper converter secondary emission stream at the time of each
emission test that demonstrates compliance with the emission limit
required in 61.172(c) according to the provisions of paragraphs (c)(1)
through (c)(4) of this section.
(e) With a minimum of 30 days prior notice, the Administrator may
require the owner or operator to redetermine the reference opacity level
for any monitored emission stream.
(f) Each owner or operator who is required to install the equipment
specified in 61.172(b)(1) for the capture of secondary copper converter
emissions shall install, calibrate, maintain, and operate a continuous
monitoring device on each secondary hood system for the measurement of
the air flow through the horizontal-slotted plenum and through the
exhaust hood. Each device shall be installed and operational no later
than 90 days after the effective date of this subpart for a source that
has an initial startup preceding the effective date; and no later than
90 days after startup for other sources.
(g) Each owner or operator subject to the requirements in paragraph
(f) of this section shall establish for each secondary hood system
reference air flow rates for the horizontal-slotted plenum and exhaust
hood for each mode of converter operation. The reference flow rates
shall be established when the equipment is operating under the optimum
operating conditions required in 61.172(b)(2)(ii).
(h) Each owner or operator shall install the continuous monitoring
systems and monitoring devices required in paragraphs (a) and (f) of
this section in such a manner that representative measurements of
emissions and process parameters are obtained.
40 CFR 61.176 Recordkeeping requirements.
(a) Each owner or operator subject to the requirements of
61.172(b)(1) shall maintain at the source for a period of at least 2
years records of the visual inspections, maintenance, and repairs
performed on each secondary hood system as required in 61.172(b)(3).
(b) Each owner or operator subject to the provisions of 61.172(c)
shall maintain at the source for a period of at least 2 years and make
available to the Administrator upon request a file of the following
records:
(1) All measurements, including continuous monitoring for measurement
of opacity;
(2) Records of emission test data and all calculations used to
produce the required reports of emission estimates to demonstrate
complaince with 61.172(c);
(3) All continuous monitoring system performance evaluations,
including calibration checks and adjustments;
(4) The occurrence and duration of all startups, shutdowns, and
malfunctions of the copper converters;
(5) All malfunctions of the air pollution control system;
(6) All periods during which any continuous monitoring system or
device is inoperative;
(7) All maintenance and repairs performed on each air pollution
control system, continuous monitoring system, or monitoring device;
(8) All records of 1-hour average opacity levels for each separate
control device; and
(9) For each secondary hood system:
(i) The reference flow rates for the horizontal-slotted plenum and
exhaust hood for each converter operating mode estabilshed under
61.175(g);
(ii) The actual flow rates; and
(iii) A daily log of the start time and duration of each converter
operating mode.
(c) Each owner or operator subject to the provisions of this subpart
shall maintain at the source for a period of at least 2 years and make
available to the Administrator upon request the following records:
(1) For each copper converter, a daily record of the amount of copper
matte and lead matte charged to the copper converter and the total hours
of operation.
(2) For each copper converter department, a monthly record of the
weight percent of arsenic contained in the copper matte and lead matte
as determined under 61.174(f).
(3) For each copper converter department, the monthly calculations of
the average annual arsenic charging rate for the preceding 12-month
period as determined under 61.174(f).
(Approved by the Office of Management and Budget under control number
2060-0044)
40 CFR 61.177 Reporting requirements.
(a) Each owner or operator subject to the provisions of 61.172(c)
shall:
(1) Provide the Administrator 30 days prior notice of the emission
test required in 61.174(a) to afford the Administrator the opportunity
to have an observer present; and
(2) Submit to the Administrator a written report of the results of
the emission test required in 61.174(a) within 60 days after conducting
the test.
(b) Each owner or operator subject to the provisions of 61.175(a)
shall provide the Administrator at least 30 days prior notice of each
reference opacity level determination required in 61.175(c) to afford
the Administrator the opportunity to have an observer present.
(c) Each owner or opertor subject to the provisions of 61.175(a)
shall submit to the Administrator:
(1) Within 60 days after conducting the evaluation required in
61.175(a)(1), a written report of the continuous monitoring system
evaluation;
(2) Within 30 days after establishing the reference opacity level
required in 61.175(c), a written report of the reference opacity level.
The report shall also include the opacity data used and the
calculations performed to determine the reference opacity level, and
sufficient documentation to show that process and emission control
equipment were operating normally during the reference opacity level
determination; and
(3) A written report each quarter of each occurrence of excess
opacity during the quarter. For purposes of this paragraph, an
occurrence of excess opacity is any 1-hour period during which the
average opacity, as measured by the continuous monitoring system,
exceeds the reference opacity level established under 61.175(c).
(d) The owner or operator subject to the provisions of 61.175(g)
shall submit to the Administrator:
(1) A written report of the reference air flow rate within 30 days
after establishing the reference air flow rates required in 61.175(g);
(2) A written report each quarter of all air flow rates monitored
during the preceding 3-month period that are less than 80 percent of the
corresponding reference flow rate established for each converter
operating mode; and
(3) A written report each quarter of any changes in the operating
conditions of the emission capture system, emission control device, or
the building housing the converters that might increase fugitive
emissions.
(e) All quarterly reports shall be postmarked by the 30th day
following the end of each 3-month period and shall include the following
information:
(1) The magnitude of each occurrence of excess opacity, any
conversion factor(s) used, and the dates and times of commencement and
completion of each occurrence of excess opacity, the cause of each
exceedance of the reference opacity level, and the measures taken to
minimize emissions.
(2) The magnitude of each occurrence of reduced flow rate and the
date and time of commencement and completion of each occurrence of
reduced flow rate, the cause of the reduced flow rate, and the
associated converter operating mode.
(3) Specific identification of each occurrence of excess opacity or
reduced flow rate that occurs during startups, shutdowns, and
malfunctions of the source.
(4) The date and time identifying each period during which the
continuous monitoring system or monitoring device was inoperative,
except for zero and span checks, and the nature of the system repairs or
adjustments.
(5) Specific identification of each change in operating conditions of
the emission capture system or control device, or in the condition of
the building housing the converters.
(f) Each owner or operator of a source subject to the provisions of
this subpart shall submit annually a written report to the Administrator
that includes the monthly computations of the average annual converter
arsenic charging rate as calculated under 61.174(f)(4). The annual
report shall be postmarked by the 30th day following the end of each
calendar year.
(Approved by the Office of Management and Budget under control number
2060-0044)
40 CFR 61.177 Subpart P -- National Emission Standard for Inorganic
Arsenic Emissions From Arsenic Trioxide and Metallic Arsenic Production
Facilities
Source: 51 FR 28033, Aug. 4, 1986, unless otherwise noted.
40 CFR 61.180 Applicability and designation of sources.
The provisions of this subpart are applicable to each metallic
arsenic production plant and to each arsenic trioxide plant that
processes low-grade arsenic bearing materials by a roasting condensation
process.
40 CFR 61.181 Definitions.
All terms used in this subpart shall have the meanings given them in
the Act, in subpart A of part 61, and in this section as follows:
Arsenic kitchen means a baffled brick chamber where inorganic arsenic
vapors are cooled, condensed, and removed in a solid form.
Control device means the air pollution control equipment used to
collect particulate matter emissions.
Curtail means to cease operations to the extent technically feasible
to reduce emissions.
Inorganic arsenic means the oxides and other noncarbon compounds of
the element arsenic included in particulate matter, vapors, and
aerosols.
Malfunction means any sudden failure of air pollution control
equipment or process equipment or of a process to operate in a normal or
usual manner so that emissions of inorganic arsenic are increased.
Opacity means the degree to which emissions reduce the transmission
of light.
Primary emission control system means the hoods, enclosures, ducts,
and control devices used to capture, convey, and remove particulate
matter from exhaust gases which are captured directly at the source of
generation.
Process emissions means inorganic arsenic emissions that are captured
and collected in a primary emission control system.
Roasting means the use of a furnace to heat arsenic plant feed
material for the purpose of eliminating a significant portion of the
volatile materials contained in the feed.
Secondary emissions means inorganic arsenic emissions that escape
capture by a primary emission control system.
Shutdown means the cessation of operation of a stationary source for
any purpose.
(51 FR 28033, Aug. 4, 1986; 51 FR 35355, Oct. 3, 1986)
40 CFR 61.182 Standard for new and existing sources.
(a) Within 30 days after the effective date of this subpart, the
owner or operator of each source to which this subpart applies shall
identify and submit to the Administrator a list of potential sources
(equipment and operations) of inorganic arsenic emissions.
(b) The owner or operator shall submit a description of an
inspection, maintenance, and housekeeping plan for control of inorganic
arsenic emissions from the potential sources identified under paragraph
(a) of this section. This plan shall be submitted within 90 days after
the effective date of this subpart, unless a waiver of compliance is
granted under 61.11. If a waiver of compliance is granted, the plan
shall be submitted on a date set by the Administrator. Approval of the
plan will be granted by the Administrator provided he finds that:
(1) It achieves the following objectives in a manner that does not
cause adverse impacts in other environmental media:
(i) Clean-up and proper disposal, wet-down, or chemical stabilization
to the extent practicable (considering access and safety) of any dry,
dusty material having an inorganic arsenic content greater than 2
percent that accumulates on any surface within the plant boundaries
outside of a dust-tight enclosure.
(ii) Immediate clean-up and proper disposal, wet-down, or chemical
stabilization of spills of all dry, dusty material having an inorganic
arsenic content greater than 2 percent.
(iii) Minimization of emissions of inorganic arsenic to the
atmosphere during removal of inorganic arsenic from the arsenic kitchen
and from flue pulling operations by properly handling, wetting down, or
chemically stabilizing all dusts and materials handled in these
operations.
(2) It includes an inspection program that requires all process,
conveying, and air pollution control equipment to be inspected at least
once per shift to ensure that the equipment is being properly operated
and maintained. The program will specify the evaluation criteria and
will use a standardized checklist, which will be included as part of the
plan required in paragraph (b) of this section, to document the
inspection, maintenance, and housekeeping status of the equipment and
that the objectives of paragraph (b)(1) of this section are being
achieved.
(3) It includes a systematic procedure for identifying malfunctions
and for reporting them immediately to supervisory personnel.
(4) It specifies the procedures that will be followed to ensure that
equipment or process malfunctions due entirely or in part to poor
maintenance or other preventable conditions do not occur.
(5) It includes a program for curtailing all operations necessary to
minimize any increase in emissions of inorganic arsenic to the
atmosphere resulting from a malfunction. The program will describe:
(i) The specific steps that will be taken to curtail each operation
as soon as technically feasible after the malfunction is discovered.
(ii) The minimum time required to curtail each operation.
(iii) The procedures that will be used to ensure that the curtailment
continues until after the malfunction is corrected.
(c) The owner or operator shall implement the plan required in
paragraph (b) of this section until otherwise specified by the
Administrator.
(d) At all times, including periods of startup, shutdown, and
malfunction, the owner or operator of each source to which this subpart
applies shall operate and maintain the source including associated air
pollution control equipment in a manner consistent with good air
pollution control practice for minimizing emissions of inorganic arsenic
to the atmosphere to the maximum extent practicable. Determination of
whether acceptable operating and maintenance procedures are being used
will be based on information available to the Administrator, which may
include, but is not limited to, monitoring results, review of operating
and maintenance procedures, inspection of the source, and review of
other records.
40 CFR 61.183 Emission monitoring.
(a) The owner or operator of each source subject to the provisions of
this subpart shall install, calibrate, maintain, and operate a
continuous monitoring system for the measurement of the opacity of each
arsenic trioxide and metallic arsenic process emission stream that exits
from a control device.
(b) The owner or operator shall install, operate, and maintain each
continuous monitoring system for the measurement of opacity required in
paragraph (a) of this section according to the following procedures:
(1) Ensure that each system is installed and operational no later
than 90 days after the effective date of this subpart for an existing
source or a new source that has an initial startup date preceding the
effective date. For a new source whose initial startup occurs after the
effective date of this subpart, ensure that the system is installed and
operational no later than 90 days after startup. Verification of the
operational status shall, as a minimum, consist of an evaluation of the
monitoring system in accordance with the requirements and procedures
contained in Performance Specification 1 of appendix B of 40 CFR part
60.
(2) Comply with the provisions of 60.13(d) of 40 CFR part 60.
(3) Except for system breakdowns, repairs, calibration checks, and
zero and span adjustments required under 60.13(d), ensure that each
continuous monitoring system is in continuous operation and meets
frequency of operation requirements by completing a minimum of one cycle
of sampling and analysis for each successive 10-second period and one
cycle of data recording for each successive 6-minute period. Each data
point shall represent the opacity measured for one cycle of sampling and
analysis and shall be expressed as percent opacity.
(c) The owner or operator shall calculate 6-minute opacity averages
from 36 or more consecutive data points equally spaced over each
6-minute period. Data recorded during periods of monitoring system
breakdowns, repairs, calibration checks, and zero and span adjustments
shall not be included in the data averages computed under this
paragraph.
(d) No later than 60 days after each continuous opacity monitoring
system required in paragraph (a) of this section becomes operational,
the owner or operator shall establish a reference opacity level for each
monitored emission stream according to the following procedures:
(1) Conduct continuous opacity monitoring over a preplanned period of
not less than 36 hours during which the processes and emission control
equipment upstream of the monitoring system are operating in a manner
that will minimize opacity under representative operating conditions
subject to the Administrator's approval.
(2) Calculate 6-minute averages of the opacity readings using 36 or
more consecutive data points equally spaced over each 6-minute period.
(3) Establish the reference opacity level by determining the highest
6-minute average opacity calculated under paragraph (d)(2) of this
section.
(e) With a minimum of 30 days prior notice, the Administrator may
require an owner or operator to redetermine the reference opacity level
for any monitored emission stream.
(f) Each owner or operator shall install all continuous monitoring
systems or monitoring devices required in paragraph (a) of this section
in such a manner that representative measurements of emissions or
process parameters are obtained.
40 CFR 61.184 Ambient air monitoring for inorganic arsenic.
(a) The owner or operator of each source to which this subpart
applies shall operate a continuous monitoring system for the measurement
of inorganic arsenic concentrations in the ambient air.
(b) The ambient air monitors shall be located at sites to detect
maximum concentrations of inorganic arsenic in the ambient air in
accordance with a plan approved by the Administrator that shall include
the sampling and analytical method used.
(c) The owner or operator shall submit a written plan describing, and
explaining the basis for, the design and adequacy of the monitoring
network, sampling and analytical procedures, and quality assurance
within 45 days after the effective date of this subpart.
(d) Each monitor shall be operated continuously except for a
reasonable time allowance for instrument maintenance and calibration,
for changing filters, or for replacement of equipment needing major
repair.
(e) Filters shall be changed daily and shall be analyzed and
concentrations calculated within 30 days after filters are collected.
(f) The Administrator at any time may require changes in, or
expansion of, the sampling program, including sampling and analytical
protocols and network design.
40 CFR 61.185 Recordkeeping requirements.
(a) Each owner or operator of a source subject to the provisions of
this subpart shall maintain at the source for a period of at least 2
years the following records: All measurements, including continuous
monitoring for measurement of opacity; all continuous monitoring system
performance evaluations, including calibration checks and adjustments;
all periods during which the continuous monitoring system or monitoring
device is inoperative; and all maintenance and repairs made to the
continuous monitoring system or monitoring device.
(b) Each owner or operator shall maintain at the source for a period
of at least 2 years a log for each plant department in which the
operating status of process, conveying, and emission control equipment
is described for each shift. For malfunctions and upsets, the following
information shall be recorded in the log:
(1) The time of discovery.
(2) A description of the malfunction or upset.
(3) The time corrective action was initiated.
(4) A description of corrective action taken.
(5) The time corrective action was completed.
(6) A description of steps taken to reduce emissions of inorganic
arsenic to the atmosphere between the time of discovery and the time
corrective action was taken.
(c) Each owner or operator subject to the provisions of this subpart
shall maintain for a period of a least 2 years records of 6-minute
average opacity levels for each separate control device.
(d) Each owner or operator subject to the provisions of 61.186 shall
maintain for a period of at least 2 years records of ambient inorganic
arsenic concentrations at all sampling sites and other data needed to
determine such concentrations.
(Approved by the Office of Management and Budget under control number
2060-0042)
40 CFR 61.186 Reporting requirements.
(a) Each owner or operator subject to the provisions of 61.183(a)
shall provide the Administrator at least 30 days prior notice of each
reference opacity level determination required in 61.183(a) to afford
the Administrator the opportunity to have an observer present.
(b) Each owner or operator subject to the provisions of 61.183(a)
shall submit to the Administrator:
(1) Within 60 days of conducting the evaluation required in
61.183(b)(1), a written report of the continuous monitoring system
evaluation;
(2) Within 30 days of establishing the reference opacity level
required in 61.183(d), a written report of the reference opacity level.
The report shall also include the opacity data used and the
calculations performed to determine the reference opacity level, and
sufficient documentation to show that process and emission control
equipment were operating normally during the reference opacity level
determination; and
(3) A written report each quarter of each occurrence of excess
opacity during the quarter. For the purposes of this paragraph, an
occurrence of excess opacity is any 6-minute period during which the
average opacity, as measured by the continuous monitoring system,
exceeds the reference opacity level established under 61.183(d).
(c) All quarterly reports of excess opacity shall be postmarked by
the 30th day following the end of each quarter and shall include the
following information:
(1) The magnitude of excess opacity, any conversion factor(s) used,
and the dates and times of commencement and completion of each
occurrence of excess opacity, the cause of each exceedance of the
reference opacity level, and the measures taken to minimize emissions.
(2) Specific identification of each period of excess opacity that
occurred during startups, shutdowns, and malfunctions of the source.
(3) The date and time identifying each period during which the
continuous monitoring system or monitoring device was inoperative,
except for zero and span checks, and the nature of the system repairs or
adjustments.
(d) Each owner or operator subject to this subpart shall submit a
written report semiannually to the Administrator that describes the
status and results, for the reporting period, of any pilot plant studies
on alternative arsenic trioxide production processes. Conclusions and
recommendations of the studies shall also be reported.
(e) All semiannual progress reports required in paragraph (d) of this
section shall be postmarked by the 30th day following the end of each
6-month period.
(f) Each owner or operator of a source to which this subpart applies
shall submit a written report each quarter to the Administrator that
includes the following information:
(1) All ambient inorganic arsenic concentrations measured at all
monitoring sites in accordance with 61.184.
(2) A description of any modifications to the sampling network,
during the reporting period, including any major maintenance, site
changes, calibrations, and quality assurance information including
sampling and analytical precision and accuracy estimates.
(g) All quarterly reports required in paragraph (f) of this section
shall be postmarked by the 30th day following the end of each quarter.
(Approved by the Office of Management and Budget under control number
2060-0042)
40 CFR 61.186 Subpart Q -- National Emission Standards for Radon
Emissions From Department of Energy Facilities
Source: 54 FR 51701, Dec. 15, 1989, unless otherwise noted.
40 CFR 61.190 Designation of facilities.
The provisions of this subpart apply to the design and operation of
all storage and disposal facilities for radium-containing material
(i.e., byproduct material as defined under section 11.e(2) of the Atomic
Energy Act of 1954 (as amended)) that are owned or operated by the
Department of Energy that emit radon-222 into air, including these
facilities: The Feed Materials Production Center, Fernald, Ohio; the
Niagara Falls Storage Site, Lewiston, New York; the Weldon Spring Site,
Weldon Spring, Missouri; the Middlesex Sampling Plant, Middlesex, New
Jersey; the Monticello Uranium Mill Tailings Pile, Monticello, Utah.
This subpart does not apply to facilities listed in, or designated by
the Secretary of Energy under title I of the Uranium Mill Tailings
Control Act of 1978.
40 CFR 61.191 Definitions.
As used in this subpart, all terms not defined here have the meaning
given them in the Clean Air Act or subpart A of part 61. The following
terms shall have the following specific meanings:
(a) Facility means all buildings, structures and operations on one
contiguous site.
(b) Source means any building, structure, pile, impoundment or area
used for interim storage or disposal that is or contains waste material
containing radium in sufficient concentration to emit radon-222 in
excess of this standard prior to remedial action.
40 CFR 61.192 Standard.
No source at a Department of Energy facility shall emit more than 20
pCi/- m /2/ -s of radon-222 as an average for the entire source, into
the air. This requirement will be part of any Federal Facilities
Agreement reached between Environmental Protection Agency and Department
of Energy.
40 CFR 61.193 Exemption from the reporting and testing requirements of
40 CFR 61.10.
All facilities designated under this subpart are exempt from the
reporting requirements of 40 CFR 61.10.
40 CFR 61.193 Subpart R -- National Emission Standards for Radon
Emissions From Phosphogypsum Stacks
Source: 57 FR 23317, June 3, 1992, unless otherwise noted.
40 CFR 61.200 Designation of facilities.
The provisions of this subpart apply to each owner or operator of a
phosphogypsum stack, and to each person who owns, sells, distributes, or
otherwise uses any quantity of phosphogypsum which is produced as a
result of wet acid phosphorus production or is removed from any existing
phosphogypsum stack.
40 CFR 61.201 Definitions.
As used in this subpart, all terms not defined here have the meaning
given them in the Clean Air Act or subpart A of part 61. The following
terms shall have the following specific meanings:
(a) Inactive stack means a stack to which no further routine
additions of phosphogypsum will be made and which is no longer used for
water management associated with the production of phosphogypsum. If a
stack has not been used for either purpose for two years, it is presumed
to be inactive.
(b) Phosphogypsum is the solid waste byproduct which results from the
process of wet acid phosphorus production.
(c) Phosphogypsum stacks or stacks are piles of waste resulting from
wet acid phosphorus production, including phosphate mines or other sites
that are used for the disposal of phosphogypsum.
40 CFR 61.202 Standard.
Each person who generates phosphogypsum shall place all phosphogypsum
in stacks. Phosphogypsum may be removed from a phosphogypsum stack only
as expressly provided by this subpart. After a phosphogypsum stack has
become an inactive stack, the owner or operator shall assure that the
stack does not emit more than 20 pCi/m2^s of radon-222 into the air.
40 CFR 61.203 Radon monitoring and compliance procedures.
(a) Within sixty days following the date on which a stack becomes an
inactive stack, or within ninety days after the date on which this
subpart first took effect if a stack was already inactive on that date,
each owner or operator of an inactive phosphogypsum stack shall test the
stack for radon-222 flux in accordance with the procedures described in
40 CFR part 61, appendix B, Method 115. EPA shall be notified at least
30 days prior to each such emissions test so that EPA may, at its
option, observe the test. If meteorological conditions are such that a
test cannot be properly conducted, then the owner or operator shall
notify EPA and test as soon as conditions permit.
(b)(1) Within ninety days after the testing is required, the owner or
operator shall provide EPA with a report detailing the actions taken and
the results of the radon-222 flux testing. Each report shall also
include the following information:
(i) The name and location of the facility;
(ii) A list of the stacks at the facility including the size and
dimensions of each stack;
(iii) The name of the person responsible for the operation of the
facility and the name of the person preparing the report (if different);
(iv) A description of the control measures taken to decrease the
radon flux from the source and any actions taken to insure the long term
effectiveness of the control measures; and
(v) The results of the testing conducted, including the results of
each measurement.
(2) Each report shall be signed and dated by a corporate officer in
charge of the facility and contain the following declaration immediately
above the signature line: ''I certify under penalty of law that I have
personally examined and am familiar with the information submitted
herein and based on may inquiry of those individuals immediately
responsible for obtaining the information, I believe that the submitted
information is true, accurate and complete. I am aware that there are
significant penalties for submitting false information including the
possibility of fine and imprisonment. See, 18 U.S.C. 1001.''
(c) If the owner or operator of an inactive stack chooses to conduct
measurements over a one year period as permitted by Method 115 in
appendix B to part 61, within ninety days after the testing commences
the owner or operator shall provide EPA with an initial report,
including the results of the first measurement period and a schedule for
all subsequent measurements. An additional report containing all the
information in 61.203(b) shall be submitted within ninety days after
completion of the final measurements.
(d) If at any point an owner or operator of a stack once again uses
an inactive stack for the disposal of phosphogypsum or for water
management, the stack ceases to be in inactive status and the owner or
operator must notify EPA in writing within 45 days. When the owner or
operator ceases to use the stack for disposal of phosphogypsum or water
management, the stack will once again become inactive and the owner or
operator must satisfy again all testing and reporting requirements for
inactive stacks.
(e) If an owner or operator removes phosphogypsum from an inactive
stack, the owner shall test the stack in accordance with the procedures
described in 40 CFR part 61, appendix B, Method 115. The stack shall be
tested within ninety days of the date that the owner or operator first
removes phosphogypsum from the stack, and the test shall be repeated at
least once during each calendar year that the owner or operator removes
additional phosphogypsum from the stack. EPA shall be notified at least
30 days prior to an emissions test so that EPA may, at its option,
observe the test. If meteorological conditions are such that a test
cannot be properly conducted, then the owner shall notify EPA and test
as soon as conditions permit. Within ninety days after completion of a
test, the owner or operator shall provide EPA with a report detailing
the actions taken and the results of the radon-222 flux testing. Each
such report shall include all of the information specified by
61.203(b).
40 CFR 61.204 Distribution and use of phosphogypsum for agricultural
purposes.
Phosphogypsum may be lawfully removed from a stack and distributed in
commerce for use in agriculture if each of the following requirements is
satisfied:
(a) The owner or operator of the stack from which the phosphogypsum
is removed shall determine annually the average radium-226 concentration
at the location in the stack from which the phosphogypsum will be
removed, as provided by 61.207.
(b) The average radium-226 concentration at the location in the stack
from which the phosphogypsum will be removed, as determined pursuant to
61.207, shall not exceed 10 picocuries per gram (pCi/g).
(c) All phosphogypsum distributed in commerce for use in agriculture
by the owner or operator of a phosphogypsum stack shall be accompanied
by a certification document which conforms to the requirements of
61.208(a).
(d) Each distributor, retailer, or reseller who distributes
phosphogypsum for use in agriculture shall prepare certification
documents which conform to the requirements of 61.208(b).
40 CFR 61.205 Distribution and use of phosphogypsum for research and
development.
(a) Phosphogypsum may be lawfully removed from a stack and
distributed in commerce for use in research and development activities
if each of the following requirements is satisfied:
(1) The owner or operator of the stack from which the phosphogypsum
is removed shall determine annually the average radium-226 concentration
at the location in the stack from which the phosphogypsum will be
removed, as provided by 61.207.
(2) All phosphogypsum distributed in commerce for use in research or
development by the owner or operator of a phosphogypsum stack or by a
distributor, retailer, or reseller shall be accompanied at all times by
certification documents which conform to the requirements of 61.208.
(b) Phosphogypsum may be purchased and used for research and
development purposes if the following requirements are satisfied:
(1) Each quantity of phosphogypsum purchased by a facility for a
particular research and development activity shall be accompanied by
certification documents which conform to the requirements of 61.208.
(2) No facility shall purchase or possess more than 700 pounds of
phosphogypsum for a particular research and development activity.
(3) Containers of phosphogypsum used in research and development
activities shall be labeled with the following warning:
40 CFR 61.205 Caution: Phosphogypsum Contains Elevated Levels of
Naturally Occuring Radioactivity
(4) For each research and development activity in which phosphogypsum
is used, the facility shall maintain records which conform to the
requirements of 61.209(c).
(c) Phosphogypsum not intended for distribution in commerce may be
lawfully removed from a stack by an owner or operator to perform
laboratory analyses required by this subpart or any other quality
control or quality assurance analyses associated with wet acid
phosphorus production.
40 CFR 61.206 Distribution and use of phosphogypsum for other purposes.
(a) Phosphogypsum may not be lawfully removed from a stack and
distributed or used for any purpose not expressly specified in 61.204
or 61.205 without prior EPA approval.
(b) A request that EPA approve distribution and/or use of
phosphogypsum for any other purpose must be submitted in writing and
must contain the following information:
(1) The name and address of the person(s) making the request.
(2) A description of the proposed use, including any handling and
processing that the phosphogypsum will undergo.
(3) The location of each facility, including suite and/or building
number, street, city, county, state, and zip code, where any use,
handling, or processing of the phosphogypsum will take place.
(4) The mailing address of each facility where any use, handling, or
processing of the phosphogypsum will take place, if different from
paragraph (b)(3) of this section.
(5) The quantity of phosphogypsum to be used by each facility.
(6) The average concentration of radium-226 in the phosphogypsum to
be used.
(7) A description of any measures which will be taken to prevent the
uncontrolled release of phosphogypsum into the environment.
(8) An estimate of the maximum individual risk, risk distribution,
and incidence associated with the proposed use, including the ultimate
disposition of the phosphogypsum or any product in which the
phosphogypsum is incorporated.
(9) A description of the intended disposition of any unused
phosphogypsum.
(10) Each request shall be signed and dated by a corporate officer or
public official in charge of the facility.
(c) The Assistant Administrator for Air and Radiation may decide to
grant a request that EPA approve distribution and/or use of
phosphogypsum if he determines that the proposed distribution and/or use
is at lease as protective of public health, in both the short term and
the long term, as disposal of phosphogypsum in a stack or a mine.
(d) If the Assistant Administrator for Air and Radiation decides to
grant a request that EPA approve distribution and/or use of
phosphogypsum for a specified purpose, each of the following
requirements shall be satisfied:
(1) The owner or operator of the stack from which the phosphogypsum
is removed shall determine annually the average radium-226 concentration
at the location in the stack from which the phosphogypsum will be
removed, as provided by 61.207.
(2) All phosphogypsum distributed in commerce by the owner or
operator of a phosphogypsum stack, or by a distributor, retailer, or
reseller, or purchased by the end-user, shall be accompanied at all
times by certification documents which conform to the requirements
61.208.
(3) The end-user of the phosphogypsum shall maintain records which
conform to the requirements of 61.209(c).
(e) If the Assistant Administrator for Air and Radiation decides to
grant a request that EPA approve distribution and/or use of
phosphogypsum for a specified purpose, the Assistant Administrator may
decide to impose additional terms or conditions governing such
distribution or use. In appropriate circumstances, the Assistant
Administrator may also decide to waive or modify the recordkeeping
requirements established by 61.209(c).
40 CFR 61.207 Radium-226 sampling and measurement procedures.
(a) Before removing phosphogypsum from a stack for distribution to
commerce pursuant to 61.204, 61.205, or 61.206, the owner or operator
of a phosphogypsum stack shall measure the average radium-226
concentration at the location in the stack from which phosphogypsum will
be removed. Measurements shall be performed for each such location
prior to the intitial distribution in commerce of phosphogypsum removed
from that location and at least once during each calendar year while
distribution of phosphogypsum removed from the location continues.
(b) The radium-226 concentration shall be determined in accordance
with the analytical procedures described in 40 CFR part 61, appendix B,
Method 114.
(c) Phosphogysum samples shall be taken at regularly spaced intervals
across the surface of the location in the phosphogypsum stack from which
phosphogypsum will be removed.
(d) The minimum number of samples considered necessary to determine a
representative average radium-226 concentration for the location on the
stack to be analyzed shall be calculated as follows:
(1) Obtain the measured mean and standard deviation of 30 regularly
spaced phosphogypsum samples.
(2) Solve the following equation for the number of samples required
to achieve a 95% confidence interval:
where:
t is the students^t distribution,
s = measured standard deviation of the radium-226 concentration,
x = measured mean of the radium-226 concentration,
e = allowable error (expressed as a fraction), and
n = number of samples.
See Reference 1 of Method 115 in appendix B to part 61 for a detailed
discussion of this statistical technique.
(3) If the number of samples required is greater than 30, then obtain
and analyze the necessary number of additional samples and recalculate
the average radium-226 concentration using the combination of the
results of the original 30 samples and additional samples. The
additional samples shall also be regularly spaced across the surface of
the location in the phosphogypsum stack from which phosphogypsum will be
removed.
40 CFR 61.208 Certification requirements.
(a)(1) The owner or operator of a stack from which phosphogypsum will
be removed and distributed in commerce pursuant to 61.204, 61.205, or
61.206 shall prepare a certification document for each quantity of
phosphogypsum which is distributed in commerce which includes:
(i) The name and address of the owner or operator;
(ii) The name and address of the purchaser or recipient of the
phosphogypsum;
(iii) The quantity (in pounds) of phosphogypsum sold or transferred;
(iv) The date of sale or transfer;
(v) A description of the intended end-use for the phosphogypsum;
(vi) The average radium-226 concentration, in pCi/g, of the
phosphogypsum, as determined pursuant to 61.207; and
(vii) The signature of the person who prepared the certification.
(2) The owner or operator shall retain the certification document for
five years from the date of sale or transfer, and shall produce the
document for inspection upon request by the Administrator, or his
authorized representative. The owner or operator shall also provide a
copy of the certification document to the purchaser or recipient.
(b)(1) Each distributor, retailer, or reseller who purchases or
receives phosphogypsum for subsequent resale or transfer shall prepare a
certification document for each quantity of phosphogypsum which is
resold or transferred which includes:
(i) The name and address of the distributor, retailer, or reseller;
(ii) The name and address of the purchaser or recipient of the
phosphogypsum;
(iii) The quantity (in pounds) of phosphogypsum resold or
transferred;
(iv) The date of resale or transfer;
(v) A description of the intended end-use for the phosphogypsum;
(vi) A copy of each certification document which accompanied the
phosphogypsum at the time it was purchased or received by the
distributor, retailer, or reseller; and
(vii) The signature of the person who prepared the certification.
(2) The distributor, retailer, or reseller shall retain the
certification document for five years from the date of resale or
transfer, and shall produce the document for inspection upon request by
the Administrator, or his authorized representative. For every resale
or transfer of phosphogypsum to a person other than an agricultural
end-user, the distributor, retailer, or reseller shall also provide a
copy of the certification document to the purchaser or transferee.
40 CFR 61.209 Required records.
(a) Each owner or operator of a phosphogypsum stack must maintain
records for each stack documenting the procedure used to verify
compliance with the flux standard in 61.202, including all
measurements, calculations, and analytical methods on which input
parameters were based. The required documentation shall be sufficient
to allow an independent auditor to verify the correctness of the
determination made concerning compliance of the stack with flux
standard.
(b) Each owner or operator of a phosphogypsum stack must maintain
records documenting the procedure used to determine average radium-226
concentration pursuant to 61.207, including all measurements,
calculations, and analytical methods on which input parameters were
based. The required documentation shall be sufficient to allow an
independent auditor to verify the accuracy of the radium-226
concentration.
(c) Each facility which uses phosphogypsum pursuant to 61.205 or
61.206 shall prepare records which include the following information:
(1) The name and address of the person in charge of the activity
involving use of phosphogypsum.
(2) A description of each use of phosphogypsum, including the
handling and processing that the phosphogypsum underwent.
(3) The location of each site where each use of phosphogypsum
occurred, including the suite and/or building number, street, city,
county, state, and zip code.
(4) The mailing address of each facility using phosphogypsum, if
different from paragraph (c)(3) of this section.
(5) The date of each use of phosphogypsum.
(6) The quantity of phosphogypsum used.
(7) The certified average concentration of radium-226 for the
phosphogypsum which was used.
(8) A description of all measures taken to prevent the uncontrolled
release of phosphogypsum into the environment.
(9) A description of the disposition of any unused phosphogypsum.
(d) These records shall be retained by the facility for at least five
years from the date of use of the phosphogypsum and shall be produced
for inspection upon request by the Administrator, or his authorized
representative.
40 CFR 61.210 Exemption from the reporting and testing requirements of
40 CFR 61.10.
All facilities designated under this subpart are exempt from the
reporting requirements of 40 CFR 61.10.
40 CFR 61.210 Subpart S -- (Reserved)
40 CFR 61.210 Subpart T -- National Emission Standards for Radon
Emissions From the Disposal of Uranium Mill Tailings
Source: 54 FR 51702, Dec. 15, 1989, unless otherwise noted.
40 CFR 61.220 Designation of facilities.
(a) The provisions of this subpart apply to the owners and operators
of all sites that are used for the disposal of tailings, and that
managed residual radioactive material or uranium byproduct materials
during and following the processing of uranium ores, commonly referred
to as uranium mills and their associated tailings, that are listed in,
or designated by the Secretary of Energy under title I of the Uranium
Mill Tailings Control Act of 1978 or regulated under title II of the
Uranium Mill Tailings Control Act of 1978.
(b) The effective date for subpart T is stayed for owners and
operators of all sites that are used for the disposal of tailings,
commonly referred to as uranium mills and their associated tailings,
that are regulated under Title II of the Uranium Mill Tailings Control
Act of 1978, until the date on which EPA takes final action concerning
its proposal to rescind subpart T for owners and operators of all sites
that are used for the disposal of tailings that are regulated under
title II of the Uranium Mill Tailings Control Act of 1978, pursuant to
section 112(d)(9) of the Clean Air Act, as amended, as published on
(date of this publication), or June 30, 1994, whichever first occurs.
EPA will publish any such final action in the Federal Register.
(54 FR 51702, Dec. 15, 1989, as amended at 56 FR 67542, Dec. 31,
1991)
40 CFR 61.221 Definitions.
As used in this subpart, all terms not defined here have the meaning
given them in the Clean Air Act or subpart A of part 61. The following
terms shall have the following specific meanings:
(a) Long term stabilization means the addition of material on a
uranium mill tailings pile for purpose of ensuring compliance with the
requirements of 40 CFR 192.02(a) or 192.32(b)(i). These actions shall be
considered complete when the Nuclear Regulatory Commission determines
that the requirements of 40 CFR 192.02(a) or 192.32(b)(i) have been met.
(b) Operational means a uranium mill tailings pile that is licensed
to accept additional tailings, and those tailings can be added without
violating subpart W or any other Federal, state or local rule or law. A
pile cannot be considered operational if it is filled to capacity or the
mill it accepts tailings from has been dismantled or otherwise
decommissioned.
(c) Uranium byproduct material or tailings means the waste produced
by the extraction or concentration of uranium from any ore processed
primarily for its source material content. Ore bodies depleted by
uranium solution extraction and which remain underground do not
constitute byproduct material for the purposes of this subpart.
40 CFR 61.222 Standard.
(a) Radon-222 emissions to the ambient air from uranium mill tailings
pile that are no longer operational shall not exceed 20 pCi/m /2/ -s of
radon-222.
(b) Once a uranium mill tailings pile or impoundment ceases to be
operational it must be disposed of and brought into compliance with this
standard within two years of the effective date or within two years of
the day it ceases to be operational whichever is later. If it is not
physically possible for a mill owner or operator to complete disposal
within that time, EPA shall, after consultation with the mill owner or
operator, establish a compliance agreement which will assure that
disposal will be completed as quickly as possible.
40 CFR 61.223 Compliance procedures.
(a) Sixty days following the completion of covering the pile to limit
radon emissions but prior to the long term stabilization of the pile,
the owners or operators of uranium mill tailings shall conduct testing
for all piles within the facility in accordance with the procedures
described in 40 CFR part 61, appendix B, Method 115, or other procedures
for which EPA has granted prior approval.
(b) Ninety days after the testing is required, each facility shall
provide EPA with a report detailing the actions taken and the results of
the radon-222 flux testing. EPA shall be notified at least 30 days
prior to an emission test so that EPA may, at its option, observe the
test. If meteorological conditions are such that a test cannot be
properly conducted, then the owner or operator shall notify EPA and test
as soon as conditions permit. Each report shall also include the
following information:
(1) The name and location of the facility.
(2) A list of the piles at the facility.
(3) A description of the control measures taken to decrease the radon
flux from the source and any actions taken to insure the long term
effectiveness of the control measures.
(4) The results of the testing conducted, including the results of
each measurement.
(5) Each report shall be signed and dated by a corporate officer or
public official in charge of the facility and contain the following
declaration immediately above the signature line: ''I certify under
penalty of law that I have personally examined and am familiar with the
information submitted herein and based on my inquiry of those
individuals immediately responsible for obtaining the information, I
believe that the submitted information is true, accurate and complete.
I am aware that there are significant penalties for submitting false
information including the possibility of fine and imprisonment. See, 18
U.S.C. 1001.''
(c) If year long measurements are made in accordance with Method 115
of appendix B of part 61, this report shall include the results of the
first measurement period and provide a schedule for the measurement
frequency to be used. An additional report shall be submitted ninety
days after completion of the final measurements.
(d) If long term stabilization has begun before the effective date of
the rule then testing may be conducted at any time, up to 60 days after
the long term stabilization is completed.
(e) If the testing demonstrates that the pile meets the requirement
of 61.222(a) and long term stabilization has been completed then the
pile is considered disposed for purposes of this rule.
(Approved by the Office of Management and Budget under control number
2060-0191)
40 CFR 61.224 Recordkeeping requirements.
The owner or operator must maintain records documenting the source of
input parameters including the results of all measurements upon which
they are based, the calculations and/or analytical methods used to
derive values for input parameters, and the procedure used to determine
compliance. This documentation should be sufficient to allow an
independent auditor to verify the accuracy of the determination made
concerning the facility's compliance with the standard. The
Administrator shall be kept apprised of the location of these records
and the records must be kept for at least five years and upon request be
made available for inspection by the Administrator, or his authorized
representative.
40 CFR 61.225 Exemption from the reporting and testing requirements of
40 CFR 61.10.
All facilities designated under this subpart are exempt from the
reporting requirements of 40 CFR 61.10.
40 CFR 61.225 Subpart U -- (Reserved)
40 CFR 61.225 Subpart V -- National Emission Standard for Equipment
Leaks (Fugitive Emission Sources)
Source: 49 FR 23513, June 6, 1984, unless otherwise noted.
40 CFR 61.240 Applicability and designation of sources.
(a) The provisions of this subpart apply to each of the following
sources that are intended to operate in volatile hazardous air pollutant
(VHAP) service: pumps, compressors, pressure relief devices, sampling
connection systems, open-ended valves or lines, valves, flanges and
other connectors, product accumulator vessels, and control devices or
systems required by this subpart.
(b) The provisions of this subpart apply to the sources listed in
paragraph (a) after the date of promulgation of a specific subpart in
part 61.
(c) While the provisions of this subpart are effective, a source to
which this subpart applies that is also subject to the provisions of 40
CFR part 60 only will be required to comply with the provisions of this
subpart.
40 CFR 61.241 Definitions.
As used in this subpart, all terms not defined herein shall have the
meaning given them in the Act, in subpart A of part 61, or in specific
subparts of part 61; and the following terms shall have specific
meaning given them:
Closed-vent system means a system that is not open to atmosphere and
that is composed of piping, connections, and, if necessary,
flow-inducing devices that transport gas or vapor from a piece or pieces
of equipment to a control device.
Connector means flanged, screwed, welded, or other joined fittings
used to connect two pipe lines or a pipe line and a piece of equipment.
For the purpose of reporting and recordkeeping, connector means flanged
fittings that are not covered by insulation or other materials that
prevent location of the fittings.
Control device means an enclosed combustion device, vapor recovery
system, or flare.
Double block and bleed system means two block valves connected in
series with a bleed valve or line that can vent the line between the two
block valves.
Equipment means each pump, compressor, pressure relief device,
sampling connection system, open-ended valve or line, valve, flange or
other connector, product accumulator vessel in VHAP service, and any
control devices or systems required by this subpart.
First attempt at repair means to take rapid action for the purpose of
stopping or reducing leakage of organic material to atmosphere using
best practices.
In gas/vapor service means that a piece of equipment contains process
fluid that is in the gaseous state at operating conditions.
In liquid service means that a piece of equipment is not in gas/vapor
service.
In-situ sampling systems means nonextractive samplers or in-line
samplers.
In vacuum service means that equipment is operating at an internal
pressure which is at least 5 kilopascals (kPa) below ambient pressure.
In VHAP service means that a piece of equipment either contains or
contacts a fluid (liquid or gas) that is at least 10 percent by weight a
volatile hazardous air pollutant (VHAP) as determined according to the
provisions of 61.245(d). The provisions of 61.245(d) also specify how
to determine that a piece of equipment is not in VHAP service.
In VOC service means, for the purposes of this subpart, that (a) the
piece of equipment contains or contacts a process fluid that is at least
10 percent VOC by weight (see 40 CFR 60.2 for the definition of volatile
organic compound or VOC and 40 CFR 60.485(d) to determine whether a
piece of equipment is not in VOC service) and (b) the piece of equipment
is not in heavy liquid service as defined in 40 CFR 60.481.
Open-ended valve or line means any valve, except pressure relief
valves, having one side of the valve seat in contact with process fluid
and one side open to atmosphere, either directly or through open piping.
Pressure release means the emission of materials resulting from the
system pressure being greater than the set pressure of the pressure
relief device.
Process unit means equipment assembled to produce a VHAP or its
derivatives as intermediates or final products, or equipment assembled
to use a VHAP in the production of a product. A process unit can
operate independently if supplied with sufficient feed or raw materials
and sufficient product storage facilities.
Process unit shutdown means a work practice or operational procedure
that stops production from a process unit or part of a process unit. An
unscheduled work practice or operational procedure that stops production
from a process unit or part of a process unit for less than 24 hours is
not a process unit shutdown. The use of spare equipment and technically
feasible bypassing of equipment without stopping production are not
process unit shutdowns.
Product accumulator vessel means any distillate receiver, bottoms
receiver, surge control vessel, or product separator in VHAP service
that is vented to atmosphere either directly or through a
vacuum-producing system. A product accumulator vessel is in VHAP
service if the liquid or the vapor in the vessel is at least 10 percent
by weight VHAP.
Repaired means that equipment is adjusted, or otherwise altered, to
eliminate a leak.
Semiannual means a 6-month period; the first semiannual period
concludes on the last day of the last month during the 180 days
following initial startup for new sources; and the first semiannual
period concludes on the last day of the last full month during the 180
days after the effective date of a specific subpart that references this
subpart for existing sources.
Sensor means a device that measures a physical quantity or the change
in a physical quantity, such as temperature, pressure, flow rate, pH, or
liquid level.
Stuffing box pressure means the fluid (liquid or gas) pressure inside
the casing or housing of a piece of equipment, on the process side of
the inboard seal.
Volatile hazardous air pollutant or VHAP means a substance regulated
under this part for which a standard for equipment leaks of the
substance has been proposed and promulgated. Benzene is a VHAP. Vinyl
chloride is a VHAP.
(49 FR 23513, June 6, 1984; 49 FR 38946, Oct. 2, 1984, as amended at
51 FR 34915, Sept. 30, 1986; 54 FR 38076, Sept. 14, 1989)
40 CFR 61.242-1 Standards: General.
(a) Each owner or operator subject to the provisions of this subpart
shall demonstrate compliance with the requirements of 61.242-1 to
61.242-11 for each new and existing source as required in 40 CFR 61.05,
except as provided in 61.243 and 61.244.
(b) Compliance with this subpart will be detemined by review of
records, review of performance test results, and inspection using the
methods and procedures specified in 61.245.
(c)(1) An owner or operator may request a determination of
alternative means of emission limitation to the requirements of
61.242-2, 61.242-3, 61.242-5, 61.242-6, 61.242-7, 61.242-8, 61.242-9 and
61.242-11 as provided in 61.244.
(2) If the Administrator makes a determination that a means of
emission limitation is at least a permissible alternative to the
requirements of 61.242-2, 61.242-3, 61.242-5, 61.242-6, 61.242-7,
61.242-8, 61.242-9 or 61.242-11, an owner or operator shall comply with
the requirements of that determination.
(d) Each piece of equipment to which this subpart applies shall be
marked in such a manner that it can be distinquished readily from other
pieces of equipment.
(e) Equipment that is in vacuum service is excluded from the
requirements of 61.242-2, to 61.242-11 if it is identified as required
in 61.246(e)(5).
(49 FR 23513, June 6, 1984; 49 FR 38946, Oct. 2, 1984)
40 CFR 61.242-2 Standards: Pumps.
(a)(1) Each pump shall be monitored monthly to detect leaks by the
methods specified in 61.245(b), except as provided in 61.242-1(c) and
paragraphs (d), (e), and (f) of this section.
(2) Each pump shall be checked by visual inspection each calendar
week for indications of liquids dripping from the pump seal.
(b)(1) if an instrument reading of 10,000 ppm or greater is measured,
a leak is detected.
(2) If there are indications of liquids dripping from the pump seal,
a leak is detected.
(c)(1) When a leak is detected, it shall be repaired as soon as
practicable, but not later than 15 calendar days after it is detected,
except as provided in 61.242-10.
(2) A first attempt at repair shall be made no later than 5 calendar
days after each leak is detected.
(d) Each pump equipped with a dual mechanical seal system that
includes a barrier fluid system is exempt from the requirements of
paragraphs (a) and (b) of this section, provided the following
requirements are met:
(1) Each dual mechanical seal system is:
(i) Operated with the barrier fluid at a pressure that is at all
times greater than the pump stuffing box pressure; or
(ii) Equipped with a barrier fluid degassing reservior that is
connected by a closed-vent system to a control device that complies with
the requirements of 61.242-11; or
(iii) Equipped with a system that purges the barrier fluid into a
process stream with zero VHAP emissions to atmosphere.
(2) The barrier fluid is not in VHAP service and, if the pump is
covered by standards under 40 CFR part 60, is not in VOC service.
(3) Each barrier fluid system is equipped with a sensor that will
detect failure of the seal system, the barrier fluid system, or both.
(4) Each pump is checked by visual inspection each calendar week for
indications of liquids dripping from the pump seal.
(i) If there are indications of liquid dripping from the pump seal at
the time of the weekly inspection, the pump shall be monitored as
specified in 61.245 to determine the presence of VOC and VHAP in the
barrier fluid.
(ii) If the monitor reading (taking into account any background
readings) indicates the presence of VHAP, a leak is detected. For the
purpose of this paragraph, the monitor may be calibrated with VHAP, or
may employ a gas chromatography column to limit the response of the
monitor to VHAP, at the option of the owner or operator.
(iii) If an instrument reading of 10,000 ppm or greater (total VOC)
is measured, a leak is detected.
(5) Each sensor as described in paragraph (d)(3) of this section is
checked daily or is equipped with an audible alarm.
(6)(i) The owner or operator determines, based on design
considerations and operating experience, criteria applicable to the
presence and frequency of drips and to the sensor that indicates failure
of the seal system, the barrier fluid system, or both.
(ii) If indications of liquids dripping from the pump seal exceed the
criteria established in paragraph (d)(6)(i) of this section, or if,
based on the criteria established in paragraph (d)(6)(i) of this
section, the sensor indicates failure of the seal system, the barrier
fluid system, or both, a leak is detected.
(iii) When a leak is detected, it shall be repaired as soon as
practicable, but no later than 15 calendar days after it is detected,
except as provided in 61.242-10.
(iv) A first attempt at repair shall be made no later than five
calendar days after each leak is detected.
(e) Any pump that is designated, as described in 61.246(e)(2), for
no detectable emissions, as indicated by an instrument reading of less
than 500 ppm above background, is exempt from the requirements of
paragraphs (a), (c), and (d) if the pump:
(1) Has no externally actuated shaft penetrating the pump housing,
(2) Is demonstrated to be operating with no detectable emissions, as
indicated by an instrument reading of less than 500 ppm above
background, as measured by the method specified in 61.245(c), and
(3) Is tested for compliance with paragraph (e)(2) initially upon
designation, annually, and at other times requested by the
Administrator.
(f) If any pump is equipped with a closed-vent system capable of
capturing and transporting any leakage from the seal or seals to a
control device that complies with the requirements of 61.242-11, it is
exempt from the requirements of paragraphs (a)-(e).
(g) Any pump that is located within the boundary of an unmanned plant
site is exempt from the weekly visual inspection requirement of
paragraphs (a)(2) and (d)(4) of this section, and the daily requirements
of paragraph (d)(5)(i) of this section, provided that each pump is
visually inspected as often as practicable and at least monthly.
(49 FR 23513, June 6, 1984, as amended at 49 FR 38946, Oct. 2, 1984;
55 FR 28349, July 10, 1990)
40 CFR 61.242-3 Standards: Compressors.
(a) Each compressor shall be equipped with a seal system that
includes a barrier fluid system and that prevents leakage of process
fluid to atmosphere, except as provided in 61.242-1(c) and paragraphs
(h) and (i) of this section.
(b) Each compressor seal system as required in paragraph (a) shall
be:
(1) Operated with the barrier fluid at a pressure that is greater
than the compressor stuffing box pressure; or
(2) Equipped with a barrier fluid system that is connected by a
closed-vent system to a control device that complies with the
requirements of 61.242-11; or
(3) Equipped with a system that purges the barrier fluid into a
process stream with zero VHAP emissions to atmosphere.
(c) The barrier fluid shall not be in VHAP service and, if the
compressor is covered by standards under 40 CFR part 60, shall not be in
VOC service.
(d) Each barrier fluid system as described in paragraphs (a)-(c) of
this section shall be equipped with a sensor that will detect failure of
the seal system, barrier fluid system, or both.
(e)(1) Each sensor as required in paragraph (d) of this section shall
be checked daily or shall be equipped with an audible alarm unless the
compressor is located within the boundary of an unmanned plant site.
(2) The owner or operator shall determine, based on design
considerations and operating experience, a criterion that indicates
failure of the seal system, the barrier fluid system, or both.
(f) If the sensor indicates failure of the seal system, the barrier
fluid system, or both based on the criterion determined under paragraph
(e)(2) of this section, a leak is detected.
(g)(1) When a leak is detected, it shall be repaired as soon as
practicable, but not later than 15 calendar days after it is detected,
except as provided in 61.242-10.
(2) A first attempt at repair shall be made no later than 5 calendar
days after eack leak is detected.
(h) A compressor is exempt from the requirements of paragraphs (a)
and (b) if it is equipped with a closed-vent system capable of capturing
and transporting any leakage from the seal to a control device that
complies with the requirements of 61.242-11, except as provided in
paragraph (i).
(i) Any Compressor that is designated, as described in 61.246(e)(2),
for no detectable emission as indicated by an instrument reading of less
than 500 ppm above background is exempt from the requirements of
paragraphs (a)-(h) if the compressor:
(1) Is demonstrated to be operating with no detectable emissions, as
indicated by an instrument reading of less than 500 ppm above
background, as measured by the method specified in 61.245(c); and
(2) Is tested for compliance with paragraph (i)(1) initially upon
designation, annually, and at other times requested by the
Administrator.
(49 FR 23513, June 6, 1984; 49 FR 38946, Oct. 2, 1984)
40 CFR 61.242-4 Standards: Pressure relief devices in gas/vapor
service.
(a) Except during pressure releases, each pressure relief device in
gas/vapor service shall be operated with no detectable emissions, as
indicated by an instrument reading of less than 500 ppm above
background, as measured by the method specified in 61.245(c).
(b)(1) After each pressure release, the pressure relief device shall
be returned to a condition of no detectable emissions, as indicated by
an instrument reading of less than 500 ppm above background, as soon as
practicable, but no later than 5 calendar days after each pressure
release, except as provided in 61.242-10.
(2) No later than 5 calendar days after the pressure release, the
pressure relief device shall be monitored to confirm the condition of no
detectable emissions, as indicated by an instrument reading of less than
500 ppm above background, as measured by the method specified in
61.245(c).
(c) Any pressure relief device that is equipped with a closed-vent
system capable of capturing and transporting leakage from the pressure
relief device to a control device as described in 61.242-11 is exempt
from the requirements of paragraphs (a) and (b).
(49 FR 23513, June 6, 1984; 49 FR 38946, Oct. 2, 1984)
40 CFR 61.242-5 Standards: Sampling connecting systems.
(a) Each sampling connection system shall be equipped with a
closed-purge system or closed vent system, except as provided in
61.242-1(c).
(b) Each closed-purge system or closed-vent system as required in
paragraph (a) shall:
(1) Return the purged process fluid directly to the process line with
zero VHAP emissions to atmosphere; or
(2) Collect and recycle the purged process fluid with zero VHAP
emissions to atmosphere; or
(3) Be designed and operated to capture and transport all the purged
process fluid to a control device that complies with the requirements of
61.242-11.
(c) In-situ sampling systems are exempt from the requirements of
paragraphs (a) and (b).
40 CFR 61.242-6 Standards: Open-ended valves or lines.
(a)(1) Each open-ended valve or line shall be equipped with a cap,
blind flange, plug, or a second valve, except as provided in
61.242-1(c).
(2) The cap, blind flange, plug, or second valve shall seal the open
end at all times except during operations requiring process fluid flow
through the open-ended valve or line.
(b) Each open-ended valve or line equipped with a second valve shall
be operated in a manner such that the valve on the process fluid end is
closed before the second valve is closed.
(c) When a double block and bleed system is being used, the bleed
valve or line may remain open during operations that require venting the
line between the block valves but shall comply with paragraph (a) at all
other times.
40 CFR 61.242-7 Standards: Valves.
(a) Each valve shall be monitored monthly to detect leaks by the
method specified in 61.245(b) and shall comply with paragraphs (b)-(e),
except as provided in paragraphs (f), (g), and (h) of this section,
61.243-1 or 61.243-2, and 61.242-1(c).
(b) If an instrument reading of 10,000 ppm or greater is measured, a
leak is detected.
(c)(1) Any valve for which a leak is not detected for 2 successive
months may be monitored the first month of every quarter, beginning with
the next quarter, until a leak is detected.
(2) If a leak is detected, the valve shall be monitored monthly until
a leak is not detected for 2 successive months.
(d)(1) When a leak is detected, it shall be repaired as soon as
practicable, but no later than 15 calendar days after the leak is
detected, except as provided in 61.242-10.
(2) A first attempt at repair shall be made no later than 5 calendar
days after each leak is detected.
(e) First attempts at repair include, but are not limited to, the
following best practices where practicable:
(1) Tightening of bonnet bolts;
(2) Replacement of bonnet bolts;
(3) Tightening of packing gland nuts; and
(4) Injection of lubricant into lubricated packing.
(f) Any valve that is designated, as described in 61.246(e)(2), for
no detectable emissions, as indicated by an instrument reading of less
than 500 ppm above background, is exempt from the requirements of
paragraph (a) if the valve:
(1) Has no external actuating mechanism in contact with the process
fluid;
(2) Is operated with emissions less than 500 ppm above background, as
measured by the method specified in 61.245(c); and
(3) Is tested for compliance with paragraph (f)(2) initially upon
designation, annually, and at other times requested by the
Administrator.
(g) Any valve that is designated, as described in 61.246(f)(1), as
an unsafe-to-monitor valve is exempt from the requirements of paragraph
(a) if:
(1) The owner or operator of the valve demonstrates that the valve is
unsafe to monitor because monitoring personnel would be exposed to an
immediate danger as a consequence of complying with paragraph (a); and
(2) The owner or operator of the valve has a written plan that
requires monitoring of the valve as frequent as practicable during
safe-to-monitor times.
(h) Any valve that is designated, as described in 61.246(f)(2), as a
difficult-to-monitor valve is exempt from the requirements of paragraph
(a) if:
(1) The owner or operator of the valve demonstrates that the valve
cannot be monitored without elevating the monitoring personnel more than
2 meters above a support surface;
(2) The process unit within which the valve is located is an existing
process unit; and
(3) The owner or operator of the valve follows a written plan that
requires monitoring of the valve at least once per calendar year.
40 CFR 61.242-8 Standards: Pressure relief devices in liquid service
and flanges and other connectors.
(a) Pressure relief devices in liquid service and flanges and other
connectors shall be monitored within 5 days by the method specified in
61.245(b) if evidence of a potential leak is found by visual, audible,
olfactory, or any other detection method, except at provided in
61.242-1(c).
(b) If an instrument reading of 10,000 ppm or greater is measured, a
leak is detected.
(c)(1) When a leak is detected, it shall be repaired as soon as
practicable, but not later than 15 calendar days after it is detected,
except as provided in 61.242-10.
(2) The first attempt at repair shall be made no later than 5
calendar days after each leak is detected.
(d) First attempts at repair include, but are not limited to, the
best practices described under 61.242-7(e).
(49 FR 23513, June 6, 1984; 49 FR 38946, Oct. 2, 1984)
40 CFR 61.242-9 Standards: Product accumulator vessels.
Each product accumulator vessel shall be equipped with a closed-vent
system capable of capturing and transporting any leakage from the vessel
to a control device as described in 61.242-11, except as provided in
61.242-1(c).
(49 FR 23513, June 6, 1984; 49 FR 38946, Oct. 2, 1984)
40 CFR 61.242-10 Standards: Delay of repair.
(a) Delay of repair of equipment for which leaks have been detected
will be allowed if the repair is technically infeasible without a
process unit shutdown. Repair of this equipment shall occur before the
end of the next process unit shutdown.
(b) Delay of repair of equipment for which leaks have been detected
will be allowed for equipment that is isolated from the process and that
does not remain in VHAP service.
(c) Delay of repair for valves will be allowed if:
(1) The owner or operator demonstrates that emissions of purged
material resulting from immediate repair are greater than the fugitive
emissions likely to result from delay of repair, and
(2) When repair procedures are effected, the purged material is
collected and destroyed or recovered in a control device complying with
61.242-11.
(d) Delay of repair for pumps will be allowed if:
(1) Repair requires the use of a dual mechanical seal system that
includes a barrier fluid system, and
(2) Repair is completed as soon as practicable, but not later than 6
months after the leak was detected.
(e) Delay of repair beyond a process unit shutdown will be allowed
for a valve if valve assembly replacement is necessary during the
process unit shutdown, valve assembly supplies have been depleted, and
valve assembly supplies had been sufficiently stocked before the
supplies were depleted. Delay of repair beyond the next process unit
shutdown will not be allowed unless the next process unit shutdown
occurs sooner than 6 months after the first process unit shutdown.
40 CFR 61.242-11 Standards: Closed-vent systems and control devices.
(a) Owners or operators of closed-vent systems and control devices
used to comply with provisions of this subpart shall comply with the
provisions of this section, except as provided in 61.242-1(c).
(b) Vapor recovery systems (for example, condensers and adsorbers)
shall be designed and operated to recover the organic vapors vented to
them with an efficiency of 95 percent or greater.
(c) Enclosed combustion devices shall be designed and operated to
reduce the VHAP emissions vented to them with an efficiency of 95
percent or greater or to provide a minimum residence time of 0.50
seconds at a minimum temperature of 760 C.
(d) Flares shall used to comply with this subpart shall comply with
the requirements of 60.18.
(e) Owners or operators of control devices that are used to comply
with the provisions of this supbart shall monitor these control devices
to ensure that they are operated and maintained in conformance with
their design.
(f)(1) Closed-vent systems shall be designed for and operated with no
detectable emissions, as indicated by an instrument reading of less than
500 ppm above background and by visual inspections, as determined by the
methods specified as 61.245(c).
(2) Closed-event systems shall be monitored to determine compliance
with this section initially in accordance with 61.05, annually, and at
other times requested by the administrator.
(3) Leaks, as indicated by an instrument reading greater than 500 ppm
and visual inspections, shall be repaired as soon as practicable, but
not later than 15 calendar days after the leak is detected.
(4) A first attempt at repair shall be made no later than 5 calendar
days after the leak is detected.
(g) Closed-vent systems and control devices use to comply with
provisions of this subpart shall be operated at all times when emissions
may be vented to them.
(49 FR 23513, June 6, 1984; 49 FR 38946, Oct. 2, 1984, as amended at
51 FR 2702, Jan. 21, 1986)
40 CFR 61.243-1 Alternative standards for valves in VHAP service --
allowable percentage of valves leaking.
(a) An owner or operator may elect to have all valves within a
process unit to comply with an allowable percentage of valves leaking of
equal to or less than 2.0 percent.
(b) The following requirements shall be met if an owner or operator
decides to comply with an allowable percentage of valves leaking:
(1) An owner or operator must notify the Administrator that the owner
or operator has elected to have all valves within a process unit to
comply with the allowable percentage of valves leaking before
implementing this alternative standard, as specified in 61.247(d).
(2) A performance test as specified in paragraph (c) of this section
shall be conducted initially upon designation, annually, and at other
times requested by the Administrator.
(3) If a valve leak is detected, it shall be repaired in accordance
with 61.242-7(d) and (e).
(c) Performance tests shall be conducted in the following manner:
(1) All valves in VHAP service within the process unit shall be
monitored within 1 week by the methods specified in 61.245(b).
(2) If an instrument reading of 10,000 ppm or greater is measured, a
leak is detected.
(3) The leak percentage shall be determined by dividing the number of
valves in VHAP service for which leaks are detected by the number of
valves in VHAP service within the process unit.
(d) Owner or operators who elect to have all valves comply with this
alternative standard shall not have a process unit with a leak
percentage greater than 2.0 percent.
(e) If an owner or operator decides no longer to comply with
61.243-1, the owner or operator must notify the Administrator in writing
that the work practice standard described in 61.242-7(a)-(e) will be
followed.
40 CFR 61.243-2 Alternative standards for valves in VHAP service --
skip period leak detection and repair.
(a)(1) An owner or operator may elect for all valves within a process
unit to comply with one of the alternative work practices specified in
paragraphs (b)(2) and (3) of this section.
(2) An owner or operator must notify the Administrator before
implementing one of the alternative work practices, as specified in
61.247(d).
(b)(1) An owner or operator shall comply initially with the
requirements for valves, as described in 61.242-7.
(2) After 2 consecutive quarterly leak detection periods with the
percentage of valves leaking equal to or less than 2.0, an owner or
operator may begin to skip 1 of the quarterly leak detection periods for
the valves in VHAP service.
(3) After 5 consecutive quarterly leak detection periods with the
percentage of valves leaking equal to or less than 2.0, an owner or
operator may begin to skip 3 of the quartely leak detection periods for
the valves in VHAP service.
(4) If the percentage of valves leaking is greater than 2.0, the
owner or operator shall comply with the requirements as described in
61.242-7 but may again elect to use this section.
40 CFR 61.244 Alternative means of emission limitation.
(a) Permission to use an alternative means of emission limitation
under section 112(e)(3) of the Clean Air Act shall be governed by the
following procedures:
(b) Where the standard is an equipment, design, or operational
requirement:
(1) Each owner or operator applying for permission shall be
responsible for collecting and verifying test data for an alternative
means of emission limitation.limitation to test data for the equipment,
design, and operational requirements.
(3) The Administrator may condition the permission on requirements
that may be necessary to assure operation and maintenance to achieve the
same emission reduction as the equipment, design, and operational
requirements.
(c) Where the standard is a work practice:
(1) Each owner or operator applying for permission shall be
responsible for collecting and verifying test data for an alternative
means of emission limitation.
(2) For each source for which permission is requested, the emission
reduction achieved by the required work practices shall be demonstrated
for a minimum period of 12 months.
(3) For each source for which permission is requested, the emission
reduction achieved by the alternative means of emission limitation shall
be demonstrated.
(4) Each owner or operator applying for permission shall commit in
writing each source to work practices that provide for emission
reductions equal to or greater than the emission reductions achieved by
the required work practices.
(5) The Administrator will compare the demonstrated emission
reduction for the alternative means of emission limitation to the
demonstrated emission reduction for the required work practices and will
consider the commitment in paragraph (c)(4).
(6) The Administrator may condition the permission on requirements
that may be necessary to assure operation and maintenance to achieve the
same emission reduction as the required work practices of this subpart.
(d) An owner or operator may offer a unique approach to demonstrate
the alternative means of emission limitation.
(e)(1) Manufacturers of equipment used to control equipment leaks of
a VHAP may apply to the Administrator for permission for an alternative
means of emission limitation that achieves a reduction in emissions of
the VHAP achieved by the equipment, design, and operational requirements
of this subpart.
(2) The Administrator will grant permission according to the
provisions of paragraphs (b), (c), and (d).
40 CFR 61.245 Test methods and procedures.
(a) Each owner or operator subject to the provisions of this subpart
shall comply with the test methods and procedures requirements provided
in this section.
(b) Monitoring, as required in 61.242, 61.243, 61.244, and 61.135,
shall comply with the following requirements:
(1) Monitoring shall comply with Method 21 of appendix A of 40 CFR
part 60.
(2) The detection instrument shall meet the performance criteria of
Reference Method 21.
(3) The instrument shall be calibrated before use on each day of its
use by the procedures specified in Reference Method 21.
(4) Calibration gases shall be:
(i) Zero air (less than 10 ppm of hydrocarbon in air); and
(ii) A mixture of methane or n-hexane and air at a concentration of
approximately, but less than, 10,000 ppm methane or n-hexane.
(5) The instrument probe shall be traversed around all potential leak
interfaces as close to the interface as possible as described in
Reference Method 21.
(c) When equipment is tested for compliance with or monitored for no
detectable emissions, the owner or operator shall comply with the
following requirements:
(1) The requirements of paragraphs (b) (1) through (4) shall apply.
(2) The background level shall be determined, as set forth in
Reference Method 21.
(3) The instrument probe shall be traversed around all potential leak
interfaces as close to the interface as possible as described in
Reference Method 21.
(4) The arithmetic difference between the maximum concentration
indicated by the instrument and the background level is compared with
500 ppm for determining compliance.
(d)(1) Each piece of equipment within a process unit that can
conceivably contain equipment in VHAP service is presumed to be in VHAP
service unless an owner or operator demonstrates that the piece of
equipment is not in VHAP service. For a piece of equipment to be
considered not in VHAP service, it must be determined that the percent
VHAP content can be reasonably expected never to exceed 10 percent by
weight. For purposes of determining the percent VHAP content of the
process fluid that is contained in or contacts equipment, procedures
that conform to the methods described in ASTM Method D-2267
(incorporated by the reference as specified in 61.18) shall be used.
(2)(i) An owner or operator may use engineering judgment rather than
the procedures in paragraph (d)(1) of this section to demonstrate that
the percent VHAP content does not exceed 10 percent by weight, provided
that the engineering judgment demonstrates that the VHAP content clearly
does not exceed 10 percent by weight. When an owner or operator and the
Administrator do not agree on whether a piece of equipment is not in
VHAP service, however, the procedures in paragraph (d)(1) of this
section shall be used to resolve the disagreement.
(ii) If an owner or operator determines that a piece of equipment is
in VHAP service, the determination can be revised only after following
the procedures in paragraph (d)(1) of this section.
(3) Samples used in determining the percent VHAP content shall be
representative of the process fluid that is contained in or contacts the
equipment or the gas being combusted in the flare.
(e)(1) Method 22 of appendix A of 40 CFR part 60 shall be used to
determine compliance of flares with the visible emission provisions of
this subpart.
(2) The presence of a flare pilot flame shall be monitored using a
thermocouple or any other equivalent device to detect the presence of a
flame.
(3) The net heating value of the gas being combusted in a flare shall
be calculated using the following equation:
Where:
HT=Net heating value of the sample, MJ/scm; where the net enthalpy
per mole of offgas is based on combustion at 25 C and 760 mm Hg, but the
standard temperature for determining the volume corresponding to one
mole is 20 C.
K=Constant, 1.74 10-^7 (1/ppm) (g mole/scm) (MJ/kcal) where standard
temperature for (g mole/scm) is 20 C
Ci=Concentration of sample component i in ppm, as measured by
Reference Method 18 of Appendix A of 40 FR part 60 and ASTM D2504-67
(reapproved 1977) (incorporated by reference as specified in 61.18).
Hi=Net heat of combustion of sample component i, kcal/g mole. The
heats of combustion may be determined using ASTM D2382-76 (incorporated
by reference as specified in 61.18) if published values are not
available or cannot be calculated.
(4) The actual exit velocity of a flare shall be determined by
dividing the volumetric flowrate (in units of standard temperature and
pressure), as determined by Reference Method 2, 2A, 2C, or 2D, as
appropriate, by the unobstructed (free) cross section area of the flare
tip.
(5) The maximum permitted velocity, Vmax, for air-assisted flares
shall be determined by the following equation:
Where:
VMax=Maximum permitted velocity, m/sec
8.706=Constant.
0.7084=Constant.
HT=The net heating value as determined in paragraph (e)(3) of this
section.
(49 FR 23513, June 6, 1984, as amended at 49 FR 38946, Oct. 2, 1984;
49 FR 43647, Oct. 31, 1984; 53 FR 36972, Sept. 23, 1988; 54 FR 38077,
Sept. 14, 1989)
40 CFR 61.246 Recordkeeping requirements.
(a)(1) Each owner or operator subject to the provisions of this
subpart shall comply with the recordkeeping requirements of this
section.
(2) An owner or operator of more than one process unit subject to the
provisions of this subpart may comply with the recordkeeping
requirements for these process units in one recordkeeping system if the
system identifies each record by each process unit.
(b) When each leak is detected as specified in 61.242-2, 61.242-3,
61.242-7, 61.242-8, and 61.135, the following requirements apply:
(1) A weatherproof and readily visible identification, marked with
the equipment identification number, shall be attached to the leaking
equipment.
(2) The identification on a valve may be removed after it has been
monitored for 2 successive months as specified in 61.242-7(c) and no
leak has been detected during those 2 months.
(3) The identification on equipment, except on a valve, may be
removed after it has been repaired.
(c) When each leak is detected as specified in 61.242-2, 61.242-3.
61.242-7, 61.242-8, and 61.135, the following information shall be
recorded in a log and shall be kept for 2 years in a readily accessible
location:
(1) The instrument and operator identification numbers and the
equipment identification number.
(2) The date the leak was detected and the dates of each attempt to
repair the leak.
(3) Repair methods applied in each attempt to repair the leak.
(4) ''Above 10,000'' if the maximum instrument reading measured by
the methods specified in 61.245(a) after each repair attempt is equal
to or greater than 10,000 ppm.
(5) ''Repair delayed'' and the reason for the delay if a leak is not
repaired within 15 calendar days after discovery of the leak.
(6) The signature of the owner or operator (or designate) whose
decision it was that repair could not be effected without a process
shutdown.
(7) The expected date of successful repair of the leak if a leak is
not repaired within 15 calendar days.unrepaired.
(9) The date of successful repair of the leak.
(d) The following information pertaining to the design requirements
for closed-vent systems and control devices described in 61.242-11
shall be recorded and kept in a readily accessible location:
(1) Detailed schematics, design specifications, and piping and
instrumentation diagrams.
(2) The dates and descriptions of any changes in the design
specifications.
(3) A description of the parameter or parameters monitored, as
required in 61.242-11(e), to ensure that control devices are operated
and maintained in conformance with their design and an explanation of
why that parameter (or parameters) was selected for the monitoring.
(4) Periods when the closed-vent systems and control devices required
in 61.242-2, 61.242-3, 61.242-4, 61.242-5 and 61.242-9 are not
operated as designed, including periods when a flare pilot light does
not have a flame.
(5) Dates of startups and shutdowns of the closed-vent systems and
control devices required in 61.242-2, 61.242-3, 61.242-4, 61.242-5 and
61.242-9.
(e) The following information pertaining to all equipment to which a
standard applies shall be recorded in a log that is kept in a readily
accessible location:
(1) A list of identification numbers for equipment (except welded
fittings) subject to the requirements of this subpart.
(2)(i) A list of identification numbers for equipment that the owner
or operator elects to designate for no detectable emissions as indicated
by an instrument reading of less than 500 ppm above background.
(ii) The designation of this equipment for no detectable emissions
shall be signed by the owner or operator.
(3) A list of equipment identification numbers for pressure relief
devices required to comply with 61.242-4(a).
(4)(i) The dates of each compliance test required in 61.242-2(e),
61.242-3(i), 61.242-4, 61.242-7(f), and 61.135(g).
(ii) The background level measured during each compliance test.
(iii) The maximum instrument reading measured at the equipment during
each compliance test.
(5) A list of identification numbers for equipment in vacuum service.
(f) The following information pertaining to all valves subject to the
requirements of 61.242-7(g) and (h) shall be recorded in a log that is
kept in a readily accessible location:
(1) A list of identification numbers for valves that are designated
as unsafe to monitor, an explanation for each valve stating why the
valve is unsafe to monitor, and the plan for monitoring each valve.
(2) A list of identification numbers for valves that are designated
as difficult to monitor, an explanation for each valve stating why the
valve is difficult to monitor, and the planned schedule for monitoring
each valve.
(g) The following information shall be recorded for valves complying
with 61.243-2:
(1) A schedule of monitoring.
(2) The percent of valves found leaking during each monitoring
period.
(h) The following information shall be recorded in a log that is kept
in a readily accessible location:
(1) Design criterion required in 61.242-2(d)(5), 61.242-3(e)(2),
and 61.135(e)(4) and an explanation of the design criterion; and
(2) Any changes to this criterion and the reasons for the changes.
(i) The following information shall be recorded in a log that is kept
in a readily accessible location for use in determining exemptions as
provided in the applicability section of this subpart and other specific
subparts:
(1) An analysis demonstrating the design capacity of the process
unit, and
(2) An analysis demonstrating that equipment is not in VHAP service.
(j) Information and data used to demonstrate that a piece of
equipment is not in VHAP service shall be recorded in a log that is kept
in a readily accessible location.
(Approved by the Office of Management and Budget under control number
2060-0068)
(49 FR 23513, June 6, 1984, as amended at 49 FR 38946, Oct. 2, 1984;
54 FR 38077, Sept. 14, 1989)
40 CFR 61.247 Reporting requirements.
(a)(1) An owner or operator of any piece of equipment to which this
subpart applies shall submit a statement in writing notifying the
Administrator that the requirements of 61.242, 61.245, 61.246, and
61.247 are being implemented.
(2) In the case of an existing source or a new source which has an
initial startup date preceding the effective date, the statement is to
be submitted within 90 days of the effective date, unless a waiver of
compliance is granted under 61.11, along with the information required
under 61.10. If a waiver of compliance is granted, the statement is to
be submitted on a date scheduled by the Administrator.
(3) In the case of new sources which did not have an initial startup
date preceding the effective date, the statement shall be submitted with
the application for approval of construction, as described in 61.07.
(4) The statement is to contain the following information for each
source:
(i) Equipment identification number and process unit identification.
(ii) Type of equipment (for example, a pump or pipeline valve).
(iii) Percent by weight VHAP in the fluid at the equipment.
(iv) Process fluid state at the equipment (gas/vapor or liquid).
(v) Method of compliance with the standard (for example, ''monthly
leak detection and repair'' or ''equipped with dual mechanical seals'').
(b) A report shall be submitted to the Administrator semiannually
starting 6 months after the initial report required in paragraph (a) of
this section, that includes the following information:
(1) Process unit identification.
(2) For each month during the semiannual reporting period,
(i) Number of valves for which leaks were detected as described in
61.242-7(b) of 61.243-2.
(ii) Number of valves for which leaks were not repaired as required
in 61.242-7(d).
(iii) Number of pumps for which leaks were detected as described in
61.242-2 (b) and (d)(6).
(iv) Number of pumps for which leaks were not repaired as required in
61.242-2 (c) and (d)(6).
(v) Number of compressors for which leaks were detected as described
in 61.242-3(f).
(vi) Number of compressors for which leaks were not repaired as
required in 61.242-3(g).
(vii) The facts that explain any delay of repairs and, where
appropriate, why a process unit shutdown was technically infeasible.
(3) Dates of process unit shutdowns which occurred within the
semiannual reporting period.
(4) Revisions to items reported according to paragraph (a) if changes
have occurred since the initial report or subsequent revisions to the
initial report.
Note: Compliance with the requirements of 61.10(c) is not required
for revisions documented under this paragraph.
(5) The results of all performance tests and monitoring to determine
compliance with no detectable emissions and with 61.243 -- 1 and
61.243 -- 2 conducted within the semiannual reporting period.
(c) In the first report submitted as required in paragraph (a) of
this section, the report shall include a reporting schedule stating the
months that semiannual reports shall be submitted. Subsequent reports
shall be submitted according to that schedule, unless a revised schedule
has been submitted in a previous semiannual report.
(d) An owner or operator electing to comply with the provisions of
61.243-1 and 61.243-2 shall notify the Administrator of the alternative
standard selected 90 days before implementing either of the provisions.
(e) An application for approval of construction or modification,
61.05(a) and 61.07, will not be required if --
(1) The new source complies with the standard, 61.242;
(2) The new source is not part of the construction of a process unit;
and
(3) In the next semiannual report required by paragraph (b) of this
section, the information in paragraph (a)(4) of this section is
reported.
(Approved by the Office of Management and Budget under control number
ICR-1153)
(49 FR 23513, June 6, 1984, as amended at 49 FR 38947, Oct. 2, 1984;
54 FR 38077, Sept. 14, 1989)
40 CFR 61.247 Subpart W -- National Emission Standards for Radon
Emissions From Operating Mill Tailings
Source: 54 FR 51703, Dec. 15, 1989, unless otherwise noted.
40 CFR 61.250 Designation of facilities.
The provisions of this subpart apply to owners or operators of
facilities licensed to manage uranium byproduct materials during and
following the processing of uranium ores, commonly referred to as
uranium mills and their associated tailings. This subpart does not
apply to the disposal of tailings.
40 CFR 61.251 Definitions.
As used in this subpart, all terms not defined here have the meaning
given them in the Clean Air Act or 40 CFR part 61, subpart A. The
following terms shall have the following specific meanings:
(a) Area means the vertical projection of the pile upon the earth's
surface.
(b) Continuous disposal means a method of tailings management and
disposal in which tailings are dewatered by mechanical methods
immediately after generation. The dried tailings are then placed in
trenches or other disposal areas and immediately covered to limit
emissions consistent with applicable Federal standards.
(c) Dewatered means to remove the water from recently produced
tailings by mechanical or evaporative methods such that the water
content of the tailings does not exceed 30 percent by weight.
(d) Existing impoundment means any uranium mill tailings impoundment
which is licensed to accept additional tailings and is in existence as
of December 15, 1989.
(e) Operation means that an impoundment is being used for the
continued placement of new tailings or is in standby status for such
placement. An impoundment is in operation from the day that tailings
are first placed in the impoundment until the day that final closure
begins.
(f) Phased disposal means a method of tailings management and
disposal which uses lined impoundments which are filled and then
immediately dried and covered to meet all applicable Federal standards.
(g) Uranium byproduct material or tailings means the waste produced
by the extraction or concentration of uranium from any ore processed
primarily for its source material content. Ore bodies depleted by
uranium solution extraction and which remain underground do not
constitute byproduct material for the purposes of this subpart.
40 CFR 61.252 Standard.
(a) Radon-222 emissions to the ambient air from an existing uranium
mill tailings pile shall not exceed 20 pCi/m2-s of radon-222.
(b) After December 15, 1989, no new tailings impoundment can be built
unless it is designed, constructed and operated to meet one of the two
following work practices:
(1) Phased disposal in lined tailings impoundments that are no more
than 40 acres in area and meet the requirements of 40 CFR 192.32(a) as
determined by the Nuclear Regulatory Commission. The owner or operator
shall have no more than two impoundments, including existing
impoundments, in operation at any one time.
(2) Continuous disposal of tailings such that tailings are dewatered
and immediately disposed with no more than 10 acres uncovered at any
time and operated in accordance with 192.32(a) as determined by the
Nuclear Regulatory Commission.
(c) All mill owners or operators shall comply with the provisions of
40 CFR 192.32(a) in the operation of tailings piles, the exemption for
existing piles in 40 CFR 192.32(a) notwithstanding.
40 CFR 61.253 Determining compliance.
Compliance with the emission standard in this subpart shall be
determined annually through the use of Method 115 of appendix B. When
measurements are to be made over a one year period, EPA shall be
provided with a schedule of the measurement frequency to be used. The
schedule may be submitted to EPA prior to or after the first measurement
period. EPA shall be notified 30 days prior to any emissions test so
that EPA may, at its option, observe the test.
40 CFR 61.254 Annual reporting requirements.
(a) The owners or operators of operating existing mill impoundments
shall report the results of the compliance calculations required in
61.253 and the input parameters used in making the calculation for each
calendar year shall be sent to EPA by March 31 of the following year.
Each report shall also include the following information:
(1) The name and location of the mill.
(2) The name of the person responsible for the operation of the
facility and the name of the person preparing the report (if different).
(3) The results of the testing conducted, including the results of
each measurement.
(4) Each report shall be signed and dated by a corporate officer in
charge of the facility and contain the following declaration immediately
above the signature line: ''I certify under penalty of law that I have
personally examined and am familiar with the information submitted
herein and based on my inquiry of those individuals immediately
responsible for obtaining the information, I believe that the submitted
information is true, accurate and complete. I am aware that there are
significant penalties for submitting false information including the
possibility of fine and imprisonment. See, 18 U.S.C. 1001.''
(b) If the facility is not in compliance with the emission limits of
61.252 in the calendar year covered by the report, then the facility
must commence reporting to the Administrator on a monthly basis the
information listed in paragraph (a) of this section, for the preceding
month. These reports will start the month immediately following the
submittal of the annual report for the year in noncompliance and will be
due 30 days following the end of each month. This increased level of
reporting will continue until the Administrator has determined that the
monthly reports are no longer necessary. In addition to all the
information required in paragraph (a) of this section, monthly reports
shall also include the following information:
(1) All controls or other changes in operation of the facility that
will be or are being installed to bring the facility into compliance.
(2) If the facility is under a judicial or administrative enforcement
decree, the report will describe the facilities performance under the
terms of the decree.
(c) The first report will cover the emissions of calendar year 1990.
(Approved by the Office of Management and Budget under control number
2060-0191)
40 CFR 61.255 Recordkeeping requirements.
The owner or operator of the mill must maintain records documenting
the source of input parameters including the results of all measurements
upon which they are based, the calculations and/or analytical methods
used to derive values for input parameters, and the procedure used to
determine compliance. In addition, the documentation should be
sufficient to allow an independent auditor to verify the accuracy of the
determination made concerning the facility's compliance with the
standard. These records must be kept at the mill for at least five
years and upon request be made available for inspection by the
Administrator, or his authorized representative.
40 CFR 61.256 Exemption from the reporting and testing requirements of
40 CFR 61.10.
All facilities designated under this subpart are exempt from the
reporting requirements of 40 CFR 61.10.
40 CFR 61.256 Subpart X -- (Reserved)
40 CFR 61.256 Subpart Y -- National Emission Standard for Benzene
Emissions from Benzene Storage Vessels
Source: 54 FR 38077, Sept. 14, 1989, unless otherwise noted.
40 CFR 61.270 Applicability and designation of sources.
(a) The source to which this subpart applies is each storage vessel
that is storing benzene having a specific gravity within the range of
specific gravities specified in ASTM D 836-84 for Industrial Grade
Benzene, ASTM D 835-85 for Refined Benzene-485, ASTM D 2359-85a for
Refined Benzene-535, and ASTM D 4734-87 for Refined Benzene-545. These
specifications are incorporated by reference as specified in 61.18.
(b) Except for paragraph (b) in 61.276, storage vessels with a
design storage capacity less than 38 cubic meters (10,000 gallons) are
exempt from the provisions of this subpart.
(c) This subpart does not apply to storage vessels used for storing
benzene at coke by-product facilities.
(d) This subpart does not apply to vessels permanently attached to
motor vehicles such as trucks, rail cars, barges, or ships.
(e) This subpart does not apply to pressure vessels designed to
operate in excess of 204.9 kPa and without emissions to the atmosphere.
(f) A designated source subject to the provisions of this subpart
that is also subject to applicable provisions of 40 CFR part 60 subparts
K, Ka, and Kb shall be required to comply only with the subpart that
contains the most stringent requirements for that source.
40 CFR 61.271 Emission standard.
The owner or operator of each storage vessel with a design storage
capacity greater than or equal to 38 cubic meters (10,000 gallons) to
which this subpart applies shall comply with the requirements in
paragraph (d) of this section and with the requirements either in
paragraph (a), (b), or (c) of this section, or equivalent as provided in
61.273.
(a) The storage vessel shall be equipped with a fixed roof and an
internal floating roof.
(1) An internal floating roof means a cover that rests on the liquid
surface (but not necessarily in complete contact with it) inside a
storage vessel that has a permanently affixed roof. The internal
floating roof shall be floating on the liquid surface at all times,
except during initial fill and during those intervals when the storage
vessel is completely emptied or subsequently emptied and refilled. When
the roof is resting on the leg supports, the process of filling,
emptying, or refilling shall be continuous and shall be accomplished as
rapidly as possible.
(2) Each internal floating roof shall be equipped with one of the
closure devices listed in paragraphs (a)(2) (i), (ii), or (iii) of this
section between the wall of the storage vessel and the edge of the
internal floating roof. This requirement does not apply to each
existing storage vessel for which construction of an internal floating
roof equipped with a continuous seal commenced on or before July 28,
1988. A continuous seal means a seal that forms a continuous closure
that completely covers the space between the wall of the storage vessel
and the edge of the internal floating roof.
(i) A foam- or liquid-filled seal mounted in contact with the liquid
(liquid-mounted seal). A liquid-mounted seal means a foam- or
liquid-filled seal mounted in contact with the liquid between the wall
of the storage vessel and the floating roof continuously around the
circumference of the vessel.
(ii) Two seals mounted one above the other so that each forms a
continuous closure that completely covers the space between the wall of
the storage vessel and the edge of the internal floating roof. The
lower seal may be vapor-mounted, but both must be continuous.
(iii) A metallic shoe seal. A metallic shoe seal (also referred to
as a mechanical shoe seal) is, but is not limited to, a metal sheet held
vertically against the wall of the storage vessel by springs or weighted
levers and is connected by braces to the floating roof. A flexible
coated fabric (envelope) spans the annular space between the metal sheet
and the floating roof.
(3) Automatic bleeder vents are to be closed at all times when the
roof is floating, except when the roof is being floated off or is being
landed on the roof leg supports.
(4) Each opening in a noncontact internal floating roof except for
automatic bleeder vents (vacuum breaker vents) and the rim space vents
is to provide a projection below the liquid surface.
(5) Each internal floating roof shall meet the specifications listed
below. If an existing storage vessel had an internal floating roof with
a continuous seal as of July 28, 1988, the requirements listed below do
not have to be met until the first time after September 14, 1989, the
vessel is emptied and degassed or September 14, 1999, whichever occurs
first,
(i) Each opening in the internal floating roof except for leg
sleeves, automatic bleeder vents, rim space vents, column wells, ladder
wells, sample wells, and stub drains is to be equipped with a cover or
lid. The cover or lid shall be equipped with a gasket. Covers on each
access hatch and automatic gauge float well shall be bolted.
(ii) Each penetration of the internal floating roof for the purposes
of sampling shall be a sample well. Each sample well shall have a slit
fabric cover that covers at least 90 percent of the opening.
(iii) Each automatic bleeder vent shall be gasketed.
(iv) Rim space vents shall be equipped with a gasket.
(v) Each penetration of the internal floating roof that allows for
passage of a ladder shall have a gasketed sliding cover.
(vi) Each penetration of the internal floating roof that allows for
passage of a column supporting the fixed roof shall have a flexible
fabric sleeve seal or a gasketed sliding cover.
(6) Each cover or lid on any opening in the internal floating roof
shall be closed (i.e., no visible gaps), except when a device is in
actual use Covers on each access hatch and each automatic gauge float
well which are equipped with bolts shall be bolted when they are not in
use. Rim space vents are to be set to open only when the internal
floating roof is not floating or at the manufacturer's recommended
setting.
(b) The storage vessel shall have an external floating roof.
(1) An external floating roof means a pontoon-type or
double-deck-type cover that rests on the liquid surface in a vessel with
no fixed roof.
(2) Each external floating roof shall be equipped with a closure
device between the wall of the storage vessel and the roof edge. Except
as provided in paragraph (b)(5) of this section, the closure device is
to consist of two seals, one above the other. The lower seal is
referred to as the primary seal and the upper seal is referred to as the
secondary seal.
(i) The primary seal shall be either a metallic shoe seal or a
liquid-mounted seal. A liquid-mounted seal means a foam- or
liquid-filled seal mounted in contact with the liquid between the wall
of the storage vessel and the floating roof continuously around the
circumference of the vessel. A metallic shoe seal (which can also be
referred to as a mechanical shoe seal) is, but is not limited to, a
metal sheet held vertically against the wall of the storage vessel by
springs or weighted levers and is connected by braces to the floating
roof. A flexible coated fabric (envelope) spans the annular space
between the metal sheet and the floating roof. Except as provided in
61.272(b)(4), the primary seal shall completely cover the annular space
between the edge of the floating roof and the vessel wall.
(ii) The secondary seal shall completely cover the annular space
between the external floating roof and the wall of the storage vessel in
a continuous fashion except as allowed in 61.272(b)(4).
(3) Except for automatic bleeder vents and rim space vents, each
opening in the noncontact external floating roof shall provide a
projection below the liquid surface. Except for automatic bleeder
vents, rim space vents, roof drains, and leg sleeves, each opening in
the roof is to be equipped with a gasketed cover, seal or lid which is
to be maintained in a closed position at all times (i.e., no visible
gap) except when the device is in actual use. Automatic bleeder vents
are to be closed at all times when the roof is floating, except when the
roof is being floated off or is being landed on the roof leg supports.
Rim vents are to be set to open when the roof is being floated off the
roof leg supports or at the manufacturer's recommended setting.
Automatic bleeder vents and rim space vents are to be gasketed. Each
emergency roof drain is to be provided with a slotted membrane fabric
cover that covers at least 90 percent of the area of the opening.
(4) The roof shall be floating on the liquid at all times (i.e., off
the roof leg supports) except during initial fill until the roof is
lifted off leg supports and when the vessel is completely emptied and
subsequently refilled. The process of emptying and refilling when the
roof is resting on the leg supports shall be continuous and shall be
accomplished as rapidly as possible.
(5) The requirement for a secondary seal does not apply to each
existing storage vessel that was equipped with a liquid-mounted primary
seal as of July 28, 1988, until after the first time after September 14,
1989, when the vessel is emptied and degassed or 10 years from September
14, 1989, whichever occurs first.
(c) The storage vessel shall be equipped with a closed vent system
and a control device.
(1) The closed vent system shall be designed to collect all benzene
vapors and gases discharged from the storage vessel and operated with no
detectable emissions, as indicated by an instrument reading of less than
500 ppm above background and visual inspections, as determined in
61.242-11 (subpart V).
(2) The control device shall be designed and operated to reduce inlet
benzene emissions by 95 percent or greater. If a flare is used as the
control device, it shall meet the specifications described in the
general control device requirements of 40 CFR 60.18.
(3) The specifications and requirements listed in paragraphs (c)(1)
and (c)(2) of this section for closed vent systems and control devices
do not apply during periods of routine maintenance. During periods of
routine maintenance, the benzene level in the storage vessel(s) serviced
by the control device subject to the provisions of 61.271(c) may be
lowered but not raised. Periods of routine maintenance shall not exceed
72 hours as outlined in the maintenance plan required by
61.272(c)(1)(iii).
(4) The specifications and requirements listed in paragraphs (c)(1)
and (c)(2) of this section for closed vents and control devices do not
apply during a control system malfunction. A control system malfunction
means any sudden and unavoidable failure of air pollution control
equipment. A failure caused entirely or in part by design deficiencies,
poor maintenance, careless operation, or other preventable upset
condition or equipment breakdown is not considered a malfunction.
(d) The owner or operator of each affected storage vessel shall meet
the requirements of paragraph (a), (b), or (c) of this section as
follows:
(1) The owner or operator of each existing benzene storage vessel
shall meet the requirements of paragraph (a), (b), or (c) of this
section no later than 90 days after September 14, 1989, with the
exceptions noted in paragraphs (a)(5) and (b)(5), unless a waiver of
compliance has been approved by the Administrator in accordance with
61.11.
(2) The owner or operator of each benzene storage vessel upon which
construction commenced after September 14, 1989, shall meet the
requirements of paragraph (a), (b), or (c) of this section prior to
filling (i.e., roof is lifted off leg supports) the storage vessel with
benzene.
(3) The owner or operator of each benzene storage vessel upon which
construction commenced on or after July 28, 1988, and before September
14, 1989, shall meet the requirements of paragraph (a), (b), or (c) of
this section on September 14, 1989.
(54 FR 38077, Sept. 14, 1989; 54 FR 50887, Dec. 11, 1989)
40 CFR 61.272 Compliance provisions.
(a) For each vessel complying with 61.271(a) (fixed roof and
internal floating roof) each owner or operator shall:
(1) After installing the control equipment required to comply with
61.271(a), visually inspect the internal floating roof, the primary
seal, and the secondary seal (if one is in service), prior to filling
the storage vessel with benzene. If there are holes, tears or other
openings in the primary seal, the secondary seal, or the seal fabric, or
defects in the internal floating roof, the owner or operator shall
repair the items before filling the storage vessel.
(2) Visually inspect the internal floating roof and the primary seal
or the secondary seal (if one is in service) through manholes and roof
hatches on the fixed roof at least once every 12 months after initial
fill, or at least once every 12 months after September 14, 1989, except
as provided in paragraph (a)(4)(i) of this section. If the internal
floating roof is not resting on the surface of the benzene liquid inside
the storage vessel, or there is liquid on the roof, or the seal is
detached, or there are holes or tears in the seal fabric, the owner or
operator shall repair the items or empty and remove the storage vessel
from service within 45 days. If a failure that is detected during
inspections required in this paragraph cannot be repaired within 45 days
and if the vessel cannot be emptied within 45 days, an extension of up
to 30 additional days may be requested from the Administrator in the
inspection report required in 61.275(a). Such a request for an
extension must document that alternate storage capacity is unavailable
and specify a schedule of actions the company will take that will ensure
that the control equipment will be repaired or the vessel will be
emptied as soon as possible.
(3) Visually inspect the internal floating roof, the primary seal,
the secondary seal (if one is in service), gaskets, slotted membranes
and sleeve seals (if any) each time the storage vessel is emptied and
degassed. In no event shall inspections conducted in accordance with
this provision occur at intervals greater than 10 years in the case of
vessels conducting the annual visual inspections as specified in
paragraph (a)(2) of this section and at intervals greater than 5 years
in the case of vessels specified in paragraph (a)(4)(i) of this section.
(i) For all the inspections required by paragraphs (a)(1) and (a)(3)
of this section, the owner or operator shall notify the Administrator in
writing at least 30 days prior to the refilling of each storage vessel
to afford the Administrator the opportunity to have an observer present.
If the inspection required by paragraph (a)(3) of this section is not
planned and the owner or operator could not have known about the
inspection 30 days in advance of refilling the vessel, the owner or
operator shall notify the Administrator at least 7 days prior to the
refilling of the storage vessel. Notification shall be made by
telephone immediately followed by written documentation demonstrating
why the inspection was unplanned. Alternatively, the notification
including the written documentation may be made in writing and sent by
express mail so that it is received by the Administrator at least 7 days
prior to refilling.
(ii) If the internal floating roof has defects, the primary seal has
holes, tears, or other openings in the seal or the seal fabric, or the
secondary seal has holes, tears, or other openings in the seal or the
seal fabric, or the gaskets no longer close off the liquid surfaces from
the atmosphere, or the slotted membrane has more than 10 percent open
area, the owner or operator shall repair the items as necessary so that
none of the conditions specified in this paragraph exist before
refilling the storage vessel with benzene.
(4) For vessels equipped with a double-seal system as specified in
61.271(a)(2)(ii):
(i) Visually inspect the vessel as specified in paragraph (a)(3) of
this section at least every 5 years; or
(ii) Visually inspect the vessel annually as specified in paragraph
(a)(2) of this section, and at least every 10 years as specified in
paragraph (a)(3) of this section.
(b) For each vessel complying with 61.271(b) (external floating
roof) the owner or operator shall:
(1) Determine the gap areas and maximum gap widths between the
primary seal and the wall of the storage vessel, and the secondary seal
and the wall of the storage vessel according to the following frequency.
(i) For an external floating roof vessel equipped with primary and
secondary seals, measurements of gaps between the vessel wall and the
primary seal (seal gaps) shall be performed during the hydrostatic
testing of the vessel or within 90 days of the initial fill with benzene
or within 90 days of September 14, 1989, whichever occurs last, and at
least once every 5 years thereafter, except as provided in paragraph
(b)(1)(ii) of this section.
(ii) For an external floating roof vessel equipped with a
liquid-mounted primary seal and without a secondary seal as provided for
in 61.271(b)(5), measurement of gaps between the vessel wall and the
primary seal (seal gaps) shall be performed within 90 days of September
14, 1989, and at least once per year thereafter. When a secondary seal
is installed over the primary seal, measurement of primary seal gaps
shall be performed within 90 days of installation and at least once
every 5 years thereafter.
(iii) For an external floating roof vessel equipped with primary and
secondary seals, measurements of gaps between the vessel wall and the
secondary seal shall be performed within 90 days of the initial fill
with benzene, within 90 days of installation of the secondary seal, or
within 90 days after September 14, 1989, whichever occurs last, and at
least once per year thereafter.
(iv) If any source ceases to store benzene for a period of 1 year or
more, subsequent introduction of benzene into the vessel shall be
considered an initial fill for the purposes of paragraphs (b)(1)(i),
(b)(1)(ii), and (b)(1)(iii) of this section.
(2) Determine gap widths and areas in the primary and secondary seals
individually by the following procedures:
(i) Measure seal gaps, if any, at one or more floating roof levels
when the roof is floating off the roof leg supports.
(ii) Measure seal gaps around the entire circumference of the vessel
in each place where a 0.32 centimeter (cm) (1/8 in) diameter uniform
probe passes freely (without forcing or binding against the seal)
between the seal and the wall of the storage vessel and measure the
circumferential distance of each such location.
(iii) The total surface area of each gap described in paragraph
(b)(2)(ii) of this section shall be determined by using probes of
various widths to measure accurately the actual distance from the vessel
wall to the seal and multiplying each such width by its respective
circumferential distance.
(3) Add the gap surface area of each gap location for the primary
seal and the secondary seal individually. Divide the sum for each seal
by the nominal diameter of the vessel and compare each ratio to the
respective standards in 61.272(b)(4) and 61.272(b)(5).
(4) Repair conditions that do not meet requirements listed in
paragraph (b)(4) (i) and (ii) within 45 days of identification in any
inspection or empty and remove the storage vessel from service within 45
days.
(i) The accumulated area of gaps between the vessel wall and the
metallic shoe seal or the liquid-mounted primary seal shall not exceed
212 cm /2/ per meter of vessel diameter (10.0 in /2/ per foot of vessel
diameter) and the width of any portion of any gap shall not exceed 3.81
cm (1 1/2 in).
(A) One end of the metallic shoe is to extend into the stored liquid
and the other end is to extend a minimum vertical distance of 61 cm (24
in) above the stored liquid surface.
(B) There are to be no holes, tears, or other openings in the shoe,
seal fabric, or seal envelope.
(ii) The secondary seal is to meet the following requirements:
(A) The secondary seal is to be installed above the primary seal so
that it completely covers the space between the roof edge and the vessel
wall except as provided in paragraph (b)(4)(ii)(B) of this section.
(B) The accumulated area of gaps between the vessel wall and the
secondary seal shall not exceed 21.2 cm /2/ per meter of vessel diameter
(1.0 in /2/ per foot of vessel diameter) or the width of any portion of
any gap shall not exceed 1.27 cm ( 1/2 in). These seal gap requirements
may be exceeded during the measurement of primary seal gaps as required
by paragraph (b)(1)(i) or (b)(1)(ii) of this section.
(C) There are to be no holes, tears, or other openings in the seal or
seal fabric.
(iii) If a failure that is detected during inspections required in
this paragraph cannot be repaired within 45 days and if the vessel
cannot be emptied within 45 days, an extension of up to 30 additional
days may be requested from the Administrator in the inspection report
required in 61.275(d). Such extension request must include a
demonstration of unavailability of alternate storage capacity and a
specification of a schedule that will assure that the control equipment
will be repaired or the vessel will be emptied as soon as possible.
(5) The owner or operator shall notify the Administrator 30 days in
advance of any gap measurements required by paragraph (b)(1) of this
section to afford the Administrator the opportunity to have an observer
present.
(6) Visually inspect the external floating roof, the primary seal,
secondary seal, and fittings each time the vessel is emptied and
degassed.
(i) If the external floating roof has defects, the primary seal has
holes, tears, or other openings in the seal or the seal fabric, or the
secondary seal has holes, tears, or other openings in the seal or the
seal fabric, the owner or operator shall repair the items as necessary
so that none of the conditions specified in this paragraph exist before
filling or refilling the storage vessel with benzene.
(ii) For all the inspections required by paragraph (b)(6) of this
section, the owner or operator shall notify the Administrator in writing
at least 30 days prior to filling or refilling of each storage vessel to
afford the Administrator the opportunity to inspect the storage vessel
prior to refilling. If the inspection required by paragraph (b)(6) of
this section is not planned and the owner or operator could not have
known about the inspection 30 days in advance of refilling the vessel,
the owner or operator shall notify the Administrator at least 7 days
prior to refilling of the storage vessel. Notification shall be made by
telephone immediately followed by written documentation demonstrating
why the inspection was unplanned. Alternatively, this notification
including the written documentation may be made in writing and sent by
express mail so that it is received by the Administrator at least 7 days
prior to the refilling.
(c) The owner or operator of each source that is equipped with a
closed vent system and control device as required in 60.271(c), other
than a flare, shall meet the following requirements.
(1) Within 90 days after initial fill or after September 14, 1989,
whichever comes last, submit for approval by the Administrator, an
operating plan containing the information listed below.
(i) Documentation demonstrating that the control device being used
achieves the required control efficiency during reasonably expected
maximum loading conditions. This documentation is to include a
description of the gas stream which enters the control device, including
flow and benzene content under varying liquid level conditions (dynamic
and static) and manufacturer's design specifications for the control
device. If the control device or the closed vent capture system
receives vapors, gases or liquids, other than fuels, from sources that
are not designated sources under this subpart, the efficiency
demonstration is to include consideration of all vapors, gases and
liquids received by the closed vent capture system and control device.
If an enclosed combustion device with a minimum residence time of 0.75
seconds and a minimum temperature of 816 C is used to meet the 95
percent requirement, documentation that those conditions exist is
sufficient to meet the requirements of this paragraph.
(ii) A description of the parameter or parameters to be monitored to
ensure that the control device is operated and maintained in conformance
with its design and an explanation of the criteria used for selection of
that parameter (or parameters).
(iii) A maintenance plan for the system including the type of
maintenance necessary, planned frequency of maintenance, and lengths of
maintenance periods for those operations that would require the closed
vent system or the control device to be out of compliance with
61.271(c). The maintenance plan shall require that the system be out of
compliance with 61.271(c) for no more than 72 hours per year.
(2) Operate, monitor the parameters, and maintain the closed vent
system and control device in accordance with the operating plan
submitted to the Administrator in accordance with paragraph (c)(1) of
this section, unless the plan was modified by the Administrator during
the approval process. In this case, the modified plan applies.
(d) The owner or operator of each source that is equipped with a
closed vent system and a flare to meet the requirements in 61.271(c)
shall meet the requirements as specified in the general control device
requirements in 40 CFR 6O.18 (e) and (f).
40 CFR 61.273 Alternative means of emission limitation.
(a) Upon written application from any person, the Administrator may
approve the use of alternative means of emission limitation which have
been demonstrated to his satisfaction to achieve a reduction in benzene
emissions at least equivalent to the reduction in emissions achieved by
any requirement in 61.271 (a), (b), or (c) of this subpart.
(b) Determination of equivalence to the reduction in emissions
achieved by the requirements of 61.271 (a), (b), or (c) will be
evaluated using the following information to be included in the written
application to the Administrator:
(1) Actual emissions tests that use full-size or scale-model storage
vessels that accurately collect and measure all benzene emissions from a
given control device, and that accurately simulate wind and account for
other emission variables such as temperature and barometric pressure.
(2) An engineering evaluation that the Administrator determines is an
accurate method of determining equivalence.
(c) The Administrator may condition approval of equivalency on
requirements that may be necessary to ensure operation and maintenance
to achieve the same emission reduction as the requirements of 61.271
(a), (b), or (c).
(d) If, in the Administrator's judgment, an application for
equivalence may be approvable, the Administrator will publish a notice
of preliminary determination in the Federal Register and provide the
opportunity for public hearing. After notice and opportunity for public
hearing, the Administrator will determine the equivalence of the
alternative means of emission limitation and will publish the final
determination in the Federal Register.
40 CFR 61.274 Initial report.
(a) The owner or operator of each storage vessel to which this
subpart applies and which has a design capacity greater than or equal to
38 cubic meters (10,000 gallons) shall submit an initial report
describing the controls which will be applied to meet the equipment
requirements in 61.271. For an existing storage vessel or a new storage
vessel for which construction and operation commenced prior to September
14, 1989, this report shall be submitted within 90 days of September 14,
1989, and can be combined with the report required by 61.10. For a new
storage vessel for which construction or operation commenced on or after
September 14, 1989, the report shall be combined with the report
required by 61.07. In the case where the owner or operator seeks to
comply with 61.271(c) with a control device other than a flare, this
information may consist of the information required by 61.272(c)(1).
(b) The owner or operator of each storage vessel seeking to comply
with 61.271(c) with a flare, shall submit a report containing the
measurements required by 40 CFR 60.18(f) (1), (2), (3), (4), (5), and
(6). For the owner or operator of an existing storage vessel not
seeking to obtain a waiver or a new storage vessel for which
construction and operation commenced prior to September 14, 1989, this
report shall be combined with the report required by paragraph (a) of
this section. For the owner or operator of an existing storage vessel
seeking to obtain a waiver, the reporting date will be established in
the response to the waiver request. For the owner or operator of a new
storage vessel for which construction or operation commenced after
September 14, 1989, the report shall be submitted within 9O days of the
date the vessel is initially filled (or partially filled) with benzene.
(Approved by the Office of Management and Budget under control number
2060-0185)
40 CFR 61.275 Periodic report.
(a) The owner or operator of each storage vessel to which this
subpart applies after installing control equipment in accordance with
61.271(a) (fixed roof and internal floating roof) shall submit a report
describing the results of each inspection conducted in accordance with
61.272(a). For vessels for which annual inspections are required under
61.272(a)(2), the first report is to be submitted no more than 12 months
after the initial report submitted in accordance with 61.274, and each
report is to be submitted within 60 days of each annual inspection.
(1) Each report shall include the date of the inspection of each
storage vessel and identify each storage vessel in which:
(i) The internal floating roof is not resting on the surface of the
benzene liquid inside the storage vessel, or there is liquid on the
roof, or the seal is detached from the internal floating roof, or there
are holes, tears or other openings in the seal or seal fabric; or
(ii) There are visible gaps between the seal and the wall of the
storage vessel.
(2) Where an annual report identifies any condition in paragraph
(a)(1) of this section the annual report shall describe the nature of
the defect, the date the storage vessel was emptied, and the nature of
an date the repair was made, except as provided in paragraph (a)(3) of
this section.
(3) If an extension is requested in an annual periodic report in
accordance with 61.272(a)(2), a supplemental periodic report shall be
submitted within 15 days of repair. The supplemental periodic report
shall identify the vessel and describe the date the storage vessel was
emptied and the nature of and date the repair was made.
(b) The owner or operator of each storage vessel to which this
subpart applies after installing control equipment in accordance with
61.271(a) (fixed roof and internal floating roof) shall submit a report
describing the results of each inspection conducted in accordance with
61.272(a) (3) or (4).
(1) The report is to be submitted within 60 days of conducting each
inspection required by 61.272(a) (3) or (4).
(2) Each report shall identify each storage vessel in which the owner
or operator finds that the internal floating roof has defects, the
primary seal has holes, tears, or other openings in the seal or the seal
fabric, or the secondary seal (if one has been installed) has holes,
tears, or other openings in the seal or the seal fabric, or the gaskets
no longer close off the liquid surfaces from the atmosphere, or the
slotted membrane has more than 10 percent open area. The report shall
also describe the nature of the defect, the date the storage vessel was
emptied, and the nature of and date the repair was made.
(c) Any owner or operator of an existing storage vessel which had an
internal floating roof with a continuous seal as of July 28, 1988, and
which seeks to comply with the requirements of 61.271(a)(5) during the
first time after September 14, 1989, when the vessel is emptied and
degassed but no later than 10 years from September 14, 1989, shall
notify the Administrator 30 days prior to the completion of the
installation of such controls and the date of refilling of the vessel so
the Administrator has an opportunity to have an observer present to
inspect the storage vessel before it is refilled. This report can be
combined with the one required by 61.275(b).
(d) The owner or operator of each storage vessel to which this
subpart applies after installing control equipment in accordance with
61.271(b) (external floating roof) shall submit a report describing the
results of each seal gap measurement made in accordance with 61.272(b).
The first report is to be submitted no more than 12 months after the
initial report submitted in accordance with 61.274(a), and each annual
periodic report is to be submitted within 60 days of each annual
inspection.
(1) Each report shall include the date of the measurement, the raw
data obtained in the measurement, and the calculations described in
61.272(b) (2) and (3), and shall identify each storage vessel which does
not meet the gap specifications of 61.272(b). Where an annual report
identifies any vessel not meeting the seal gap specifications of
61.272(b) the report shall describe the date the storage vessel was
emptied, the measures used to correct the condition and the date the
storage vessel was brought into compliance.
(2) If an extension is requested in an annual periodic report in
accordance with 61.272(b)(4)(iii), a supplemental periodic report shall
be submitted within 15 days of repair. The supplemental periodic report
shall identify the vessel and describe the date the vessel was emptied
and the nature of and date the repair was made.
(e) Excess emission report.
(1) The owner or operator of each source seeking to comply with
61.271(c) (vessels equipped with closed vent systems with control
devices) shall submit a quarterly report informing the Administrator of
each occurrence that results in excess emissions. Excess emissions are
emissions that occur at any time when compliance with the specifications
and requirements of 61.271(c) are not achieved, as evidenced by the
parameters being measured in accordance with 61.272(c)(1)(ii) if a
control device other than a flare is used, or by the measurements
required in 61.272(d) and the general control device requirements in 40
CFR 60.18(f) (1) and (2) if a flare is used.
(2) The owner or operator shall submit the following information as a
minimum in the report required by (e)(1) of this section:
(i) Identify the stack and other emission points where the excess
emissions occurred;
(ii) A statement of whether or not the owner or operator believes a
control system malfunction has occurred.
(3) If the owner or operator states that a control system malfunction
has occurred, the following information as a minimum is also to be
included in the report required under paragraph (e)(1) of this section:
(i) Time and duration of the control system malfunction as determined
by continuous monitoring data (if any), or the inspections or monitoring
done in accordance with the operating plan required by 61.272(c).
(ii) Cause of excess emissions.
(Approved by the Office of Management and Budget under control number
2060-0185)
40 CFR 61.276 Recordkeeping.
(a) Each owner or operator with a storage vessel subject to this
subpart shall keep copies of all the reports and records required by
this subpart for at least 2 years, except as specified in paragraphs (b)
and (c)(1) of this section.
(b) Each owner or operator with a storage vessel, including any
vessel which has a design storage capacity less than 38 cubic meters
(10,000 gallons), shall keep readily accessible records showing the
dimensions of the storage vessel and an analysis showing the capacity of
the storage vessel. This record shall be kept as long as the storage
vessel is in operation. Each storage vessel with a design capacity of
less than 38 cubic meters (10,000 gallons) is subject to no provisions
of this subpart other than those required by this paragraph.
(c) The following information pertaining to closed vent system and
control devices shall be kept in a readily accessible location.
(1) A copy of the operating plan. This record shall be kept as long
as the closed vent system and control device is in use.
(2) A record of the measured values of the parameters monitored in
accordance with 61.272(c)(1)(ii) and 61.272(c)(2).
(3) A record of the maintenance performed in accordance with
61.272(c)(1)(iii) of the operating plan, including the following:
(i) The duration of each time the closed vent system and control
device does not meet the specifications of 61.271(c) due to
maintenance, including the following:
(A) The first time of day and date the requirements of 61.271(c) were
not met at the beginning of maintenance.
(B) The first time of day and date the requirements of 61.271(c)
were met at the conclusion of maintenance.
(C) A continuous record of the liquid level in each storage vessel
that the closed vent system and control device receive vapors from
during the interval between the times specified by (c)(3)(i)(A) and
(c)(3)(i)(B). Pumping records (simultaneous input and output) may be
substituted for records of the liquid level.
(Approved by the Office of Management and Budget under control number
2060-0185)
40 CFR 61.277 Delegation of authority.
(a) In delegating implementation and enforcement authority to a State
under section 112(d) of the Act, the authorities contained in paragraph
(b) of this section shall be retained by the Administrator and not
transferred to a State.
(b) Authorities which will not be delegated to States: 61.273.
40 CFR 61.277 Subparts Z-AA -- (Reserved)
40 CFR 61.277 Subpart BB -- National Emission Standard for Benzene
Emissions from Benzene Transfer Operations
Source: At 55 FR 8341, Mar. 7, 1990, unless otherwise noted.
40 CFR 61.300 Applicability.
(a) The affected facility to which this subpart applies is the total
of all loading racks at which benzene is loaded into tank trucks,
railcars, or marine vessels at each benzene production facility and each
bulk terminal. However, specifically exempted from this regulation are
loading racks at which only the following are loaded: Benzene-laden
waste (covered under subpart FF of this part), gasoline, crude oil,
natural gas liquids, petroleum distillates (e.g., fuel oil, diesel, or
kerosene), or benzene-laden liquid from coke by-product recovery plants.
(b) Any affected facility under paragraph (a) of this section which
loads only liquid containing less than 70 weight-percent benzene is
exempt from the requirements of this subpart, except for the
recordkeeping and reporting requirements in 61.305(i).
(c) Any affected facility under paragraph (a) of this section shall
comply with the standards in 61.302 at each loading rack that is
handling a liquid containing 70 weight-percent or more benzene.
(d) Any affected facility under paragraph (a) of this section whose
annual benzene loading is less than 1.3 million liters of 70
weight-percent or more benzene is exempt from the requirements of this
subpart, except for the recordkeeping and reporting requirements in
61.305(i).
(e) The owner or operator of an affected facility, as defined in
61.300(a) that loads a marine vessel shall be in compliance with the
provisions of this subpart on and after July 23, 1991. If an affected
facility that loads a marine vessel also loads a tank truck or railcar,
the marine vessel loading racks shall be in compliance with the
provisions of this subpart on and after July 23, 1991, while the tank
truck loading racks and the railcar loading racks shall be in compliance
as required by 61.12.
(55 FR 8341, Mar. 7, 1990, as amended at 55 FR 45804, Oct. 31, 1990)
40 CFR 61.301 Definitions.
As used in this subpart, all terms not defined herein shall have the
meaning given them in the Act, or in subpart A or subpart V of part 61.
Bulk terminal means any facility which receives liquid product
containing benzene by pipelines, marine vessels, tank trucks, or
railcars, and loads the product for further distribution into tank
trucks, railcars, or marine vessels.
Car-sealed means having a seal that is placed on the device used to
change the position of a valve (e.g., from open to closed) such that the
position of the valve cannot be changed without breaking the seal and
requiring the replacement of the old seal, once broken, with a new seal.
Control device means all equipment used for recovering or oxidizing
benzene vapors displaced from the affected facility.
Incinerator means any enclosed combustion device that is used for
destroying organic compounds and that does not extract energy in the
form of steam or process heat. These devices do not rely on the heating
value of the waste gas to sustain efficient combustion. Auxiliary fuel
is burned in the device and the heat from the fuel flame heats the waste
gas to combustion temperature. Temperature is controlled by controlling
combustion air or fuel.
Leak means any instrument reading of 10,000 ppmv or greater using
method 21 of 40 CFR part 60, appendix A.
Loading cycle means the time period from the beginning of filling a
tank truck, railcar, or marine vessel until flow to the control device
ceases, as measured by the flow indicator.
Loading rack means the loading arms, pumps, meters, shutoff valves,
relief valves, and other piping and valves necessary to fill tank
trucks, railcars, or marine vessels.
Marine vessel means any tank ship or tank barge which transports
liquid product such as benzene.
Nonvapor tight means any tank truck, railcar, or marine vessel that
does not pass the required vapor-tightness test.
Process heater means a device that transfers heat liberated by
burning fuel to fluids contained in tubes, except water that is heated
to produce steam.
Steam generating unit means any enclosed combustion device that uses
fuel energy in the form of steam.
Vapor collection system means any equipment located at the affected
facility used for containing benzene vapors displaced during the loading
of tank trucks, railcars, or marine vessels. This does not include the
vapor collection system that is part of any tank truck, railcar, or
marine vessel vapor collection manifold system.
Vapor-tight marine vessel means a marine vessel with a benzene
product tank that has been demonstrated within the preceding 12 months
to have no leaks. This demonstration shall be made using method 21 of
part 60, appendix A, during the last 20 percent of loading and during a
period when the vessel is being loaded at its maximum loading rate. A
reading of greater than 10,000 ppm as methane shall constitute a leak.
As an alternative, a marine vessel owner or operator may use the
vapor-tightness test described in 61.304(f) to demonstrate vapor
tightness. A marine vessel operated at negative pressure is assumed to
be vapor-tight for the purpose of this standard.
Vapor-tight tank truck or vapor-tight railcar means a tank truck or
railcar for which it has been demonstrated within the preceding 12
months that its product tank will sustain a pressure change of not more
than 750 pascals within 5 minutes after it is pressurized to a minimum
of 4,500 pascals. This capability is to be demonstrated using the
pressure test procedure specified in method 27 of part 60, appendix A,
and a pressure measurement device which has a precision of 2.5 mm water
and which is capable of measuring above the pressure at which the tank
truck or railcar is to be tested for vapor tightness.
40 CFR 61.302 Standards.
(a) The owner or operator of an affected facility shall equip each
loading rack with a vapor collection system that is:
(1) Designed to collect all benzene vapors displaced from tank
trucks, railcars, or marine vessels during loading, and
(2) Designed to prevent any benzene vapors collected at one loading
rack from passing through another loading rack to the atmosphere.
(b) The owner or operator of an affected facility shall install a
control device and reduce benzene emissions routed to the atmosphere
through the control device by 98 weight percent. If a boiler or process
heater is used to comply with the percent reduction requirement, then
the vent stream shall be introduced into the flame zone of such a
device.
(c) The owner or operator of an affected facility shall operate any
flare used to comply with paragraph (b) of this section in accordance
with the requirements of 60.18 (b) through (f).
(d) The owner or operator of an affected facility shall limit loading
of benzene into vapor-tight tank trucks and vapor-tight railcars using
the following procedures:
(1) The owner or operator shall obtain the vapor-tightness
documentation described in 61.305(h) for each tank truck or railcar
loaded at the affected facility. The test date in the documentation
must be within the preceding 12 months. The vapor-tightness test to be
used for tank trucks and railcars is method 27 of part 60, appendix A.
(2) The owner or operator shall cross-check the identification number
for each tank truck or railcar to be loaded with the file of
vapor-tightness documentation before the corresponding tank truck or
railcar is loaded. If no documentation is on file, the owner or
operator shall obtain a copy of the information from the tank truck or
railcar operator before the tank truck or railcar is loaded.
(3) Alternate procedures to those described in paragraphs (d)(1) and
(d)(2) of this section may be used upon application to, and approval by,
the Administrator.
(e) The owner or operator of an affected facility shall limit the
loading of marine vessels to those vessels that are vapor tight as
determined by either paragraph (e)(1), (e)(2), (e)(3), or (e)(4) of this
section.
(1) The owner or operator of an affected facility shall ensure that
each marine vessel is loaded with the benzene product tank below
atmospheric pressure (i.e., at negative pressure). If the pressure is
measured at the interface between the shoreside vapor collection pipe
and the marine vessel vapor line, the pressure measured according to the
procedures in 61.303(f) must be below atmospheric pressure.
(2) The owner or operator of an affected facility shall use the
following procedure to obtain the vapor-tightness documentation
described in 61.305(h). The vapor-tightness test for marine vessels is
method 21 of part 60, appendix A, and shall be applied to any potential
sources of vapor leaks. A reading of 10,000 ppmv or greater as methane
shall constitute a leak.
(i) The owner or operator of an affected facility shall obtain the
leak test documentation described in 61.305(h) for each marine vessel
prior to loading, if available. The date of the test listed in the
documentation must be within the 12 preceding months.
(ii) If there is no documentation of a successful leak test conducted
on the marine vessel in the preceding 12 months, the owner or operator
of an affected facility shall require that a leak test of the marine
vessel be conducted during the final 20 percent of loading of the marine
vessel or shall not load the vessel. The test shall be conducted when
the marine vessel is being loaded at the maximum allowable loading rate.
(A) If no leak is detected, the owner or operator of an affected
facility shall require that the documentation described in 61.305(h) is
completed prior to departure of the vessel. The owner or operator of
the affected facility shall retain a copy of the vapor-tightness
documentation on file.
(B) If any leak is detected, the owner or operator of an affected
facility shall require that the vapor-tightness failure be documented
for the marine vessel owner or operator prior to departure of the
vessel. The owner or operator of the affected facility shall retain a
copy of the vapor-tightness documentation on file. Delay of repair of
equipment for which leaks have been detected will be allowed if the
repair is technically infeasible without dry-docking the vessel. This
equipment will be excluded from future method 21 tests until repairs are
effected. Repair of this equipment shall occur the next time the vessel
is dry-docked.
(iii) If the marine vessel has failed its most recent vapor-tightness
test as described in 61.302(e)(2)(ii), the owner or operator of the
affected facility shall require that the owner or operator of the
nonvapor-tight marine vessel provide documentation that the leaks
detected during the previous vapor-tightness test have been repaired, or
proof that repair is technically infeasible without dry-docking the
vessel. Once the repair documentation has been provided, the owner or
operator may load the marine vessel. The owner or operator shall
require that the vapor-tightness test described in 61.302(e)(2)(ii) be
conducted during loading, and shall retain a copy of the vapor-tightness
documentation on file.
(3) The owner or operator of an affected facility shall obtain a copy
of the marine vessel's vapor-tightness documentation described in
61.305(h) for a test conducted within the preceding 12 months in
accordance with 61.304(f).
(4) Alternate procedures to those described in paragraphs (e)(1),
(e)(2) and (e)(3) of this section may be used upon application to, and
approval by, the Administrator.
(f) The owner or operator of an affected facility shall limit loading
of benzene to tank trucks, railcars, and marine vessels equipped with
vapor collection equipment that is compatible with the affected
facility's vapor collection system.
(g) The owner or operator of an affected facility shall limit loading
of tank trucks, railcars, and marine vessels to tank trucks, railcars,
and marine vessels whose collection systems are connected to the
affected facility's vapor collection systems.
(h) The owner or operator of an affected facility shall ensure that
the vapor collection and benzene loading equipment of tank trucks and
railcars shall be designed and operated to prevent gauge pressure in the
tank truck or railcar tank from exceeding, during loading, the initial
pressure the tank was pressured up to and shown to be vapor tight at
during the most recent vapor-tightness test using method 27 of part 60,
appendix A. This vapor-tightness test pressure is not to be exceeded
when measured by the procedures specified in 61.304(c).
(i) The owner or operator of an affected facility shall ensure that
no pressure-vacuum vent in the affected facility's vapor collection
system for tank trucks and railcars shall begin to open at a system
pressure less than the maximum pressure at which the tank truck or
railcar is operated.
(j) The owner or operator of an affected facility shall ensure that
the maximum normal operating pressure of the marine vessel's vapor
collection equipment shall not exceed 0.8 times the relief set pressure
of the pressure-vacuum vents. This level is not to be exceeded when
measured by the procedures specified in 61.304(d).
(k) The owner or operator of an affected facility shall inspect the
vapor collection system and the control device for detectable emissions,
and shall repair any leaks detected, in accordance with 61.242-11 (e)
and (f). This inspection of the vapor collection system and control
device shall be done during the loading of tank trucks, railcars, or
marine vessels.
(l) Vent systems that contain valves that could divert a vent stream
from a control device shall have car-sealed opened all valves in the
vent system from the emission source to the control device, and
car-sealed closed all valves in the vent system that would lead the vent
stream to the atmosphere, either directly or indirectly, bypassing the
control device.
40 CFR 61.303 Monitoring requirements.
(a) Each owner or operator of an affected facility that uses an
incinerator to comply with the percent reduction requirement specified
under 61.302(b) shall install, calibrate, maintain, and operate
according to manufacturer's specifications a temperature monitoring
device equipped with a continuous recorder and having an accuracy of 1
percent of the combustion temperature being measured expressed in
degrees Celsius or 0.5 C, whichever is greater.
(1) Where an incinerator other than a catalytic incinerator is used,
the owner or operator of the affected facility shall install a
temperature monitoring device in the firebox.
(2) Where a catalytic incinerator is used, the owner or operator
shall install temperature monitoring devices in the gas stream
immediately before and after the catalyst bed.
(b) Each owner or operator of an affected facility that uses a flare
to comply with 61.302(b) shall install, calibrate, maintain, and
operate according to manufacturer's specifications a heat sensing
device, such as an ultraviolet beam sensor or thermocouple, at the pilot
light to indicate the presence of a flame during the entire loading
cycle.
(c) Each owner or operator of an affected facility that uses a steam
generating unit or process heater to comply with 61.302(b) shall comply
with the following requirements. Where a steam generating unit with a
design heat input capacity of less than 44 MW is used to comply with
61.302(b), the owner or operator of an affected facility shall comply
with paragraph (c)(1) of this section. Where a steam generating unit or
process heater with a design heat input capacity of 44 MW or greater is
used to comply with 61.302(b), the owner or operator of an affected
facility shall comply with paragraph (c)(2) of this section.
(1) Install in the firebox, calibrate, maintain, and operate
according to manufacturer's specifications a temperature monitoring
device equipped with a continuous recorder and having an accuracy of 1
percent of the temperature being measured expressed in degrees Celsius
or 0.5 C, whichever is greater, for steam generating units or process
heaters of less than 44 MW design heat input capacity.
(2) Monitor and record the periods of operation of the steam
generating units or process heater if the design heat input capacity of
the steam generating unit or process heater is 44 MW or greater. The
records must be readily available for inspection.
(d) Each owner or operator of an affected facility that uses a carbon
adsorption system to comply with the percent reduction requirement
specified under 61.302(b) shall install, calibrate, maintain, and
operate according to manufacturer's specifications a device that
continuously indicates and records the concentration or reading of
organic compounds in the outlet gas stream of each carbon adsorber bed.
(e) The owner or operator of an affected facility who wishes to
demonstrate compliance with the standards specified under 61.302(b)
using control devices other than an incinerator, steam generating unit,
process heater, carbon adsorber, or flare shall provide the
Administrator with information describing the operation of the control
device and the process parameter(s) that would indicate proper operation
and maintenance of the device. The Administrator may request further
information and will specify appropriate monitoring procedures or
requirements.
(f) Each owner or operator of an affected facility complying with
61.302(e)(1) shall install, calibrate, maintain, and operate a recording
pressure measurement device (magnehelic gauge or equivalent device) and
an audible and visible alarm system that is activated when the pressure
vacuum specified in 61.302(e)(1) is not attained. The owner or
operator shall place the alarm system so that it can be seen and heard
where cargo transfer is controlled and on the open deck.
(g) Owners or operators using a vent system that contains valves that
could divert a vent stream from a control device used to comply with the
provisions of this subpart shall do one or a combination of the
following:
(1) Install a flow indicator immediately downstream of each valve
that if opened would allow a vent stream to bypass the control device
and be emitted, either directly or indirectly, to the atmosphere. The
flow indicator shall be capable of recording flow at least once every 15
minutes.
(2) Monitor the valves once a month, checking the position of the
valves and the condition of the car seal, and identify all times when
the car seals have been broken and the valve position has been changed
(i.e., from opened to closed for valves in the vent piping to the
control device and from closed to open for valves that allow the stream
to be vented directly or indirectly to the atmosphere).
(Approved by the Office of Management and Budget under control number
2060-0182)
40 CFR 61.304 Test methods and procedures.
(a) The procedures for determining compliance with 61.302(b) for all
control devices other than flares is as follows:
(1) All testing equipment shall be prepared and installed as
specified in the appropriate test methods.
(2) The time period for a performance test shall be not less than 6
hours, during which at least 300,000 liters of benzene are loaded. If
the throughput criterion is not met during the initial 6 hours, the test
may be either continued until the throughput criterion is met, or
resumed the next day with at least another 6 complete hours of testing.
(3) For intermittent control devices:
(i) The vapor holder level of the intermittent control device shall
be recorded at the start of the performance test. The end of the
performance test shall coincide with the time when the vapor holder is
at its original level.
(ii) At least two startups and shutdowns of the control device shall
occur during the performance test. If this does not occur under an
automatically controlled operation, the system shall be manually
controlled.
(4) An emission testing interval shall consist of each 5-minute
period during the performance test. For each interval:
(i) The reading from each measurement instrument shall be recorded.
(ii) Method 1 or 1A of part 60, appendix A, as appropriate, shall be
used for selection of the sampling site,
(iii) The volume exhausted shall be determined using method 2, 2A,
2C, or 2D of part 60, appendix A, as appropriate.
(iv) The average benzene concentration upstream and downstream of the
control device in the vent shall be determined using method 25A or
method 25B of appendix A of this part, using benzene as the calibration
gas. The average benzene concentration shall correspond to the volume
measurement by taking into account the sampling system response time.
(5) The mass emitted during each testing interval shall be calculated
as follows:
Mi=FKVSC
where:
Mi=Mass of benzene emitted during testing interval i, kg.
Vs=Volume of air-vapor mixture exhausted, m /3/ at standard
conditions.
C=Benzene concentration (as measured) at the exhaust vent, ppmv.
K=Density, (kg/m /3/ benzene), standard conditions.
K=3.25 for benzene.
F=Conversion factor, (m /3/ benzene/m /3/ air)(1/ppmv).
F=10/^6/.
s=Standard conditions, 20 C and 760 mm Hg.
(6) The benzene mass emission rates before and after the control
device shall be calculated as follows:
where:
E=Mass flow rate of benzene emitted, kg/hr.
Mi=Mass of benzene emitted during testing interval i, kg.
T=Total time of all testing intervals, hr.
n=Number of testing intervals.
(7) The percent reduction across the control device shall be
calculated as follows:
where:
R=Control efficiency of control device, %.
Eb=Mass flow rate of benzene prior to control device, kg/hr.
Ea=Mass flow rate of benzene after control device, kg/hr.
(b) When a flare is used to comply with 61.302(b), a performance
test according to method 22 of appendix A of this part, shall be
performed to determine visible emissions. The observation period shall
be at least 2 hours and shall be conducted according to method 22.
Performance testing shall be conducted during at least three complete
loading cycles with a separate test run for each loading cycle. The
observation period for detecting visible emissions shall encompass each
loading cycle. Integrated sampling to measure process vent stream flow
rate shall be performed continuously during each loading cycle.
(c) For the purpose of determining compliance with 61.302(h), the
following procedures shall be used:
(1) Calibrate and install a pressure measurement device (liquid
manometer, magnehelic gauge, or equivalent instrument), which has a
precision of 2.5 mm H20 in the range that the tank truck or railcar was
initially pressured to during the most recent vapor-tightness test.
(2) Connect the pressure measurement device to a pressure tap in the
affected facility's vapor collection system, located as close as
possible to the connection with the tank truck or railcar.
(3) During the performance test, record the pressure every 5 minutes
while a tank truck or railcar is being loaded, and record the highest
instantaneous pressure that occurs during each loading cycle. Every
loading rack shall be tested at least once during the performance test.
(4) If more than one loading rack is used simultaneously, then the
performance test shall be conducted simultaneously to represent the
maximum capacity.
(d) For the purpose of determining compliance with 61.302(j), the
following procedures shall be used:
(1) Calibrate and install a pressure measurement device (liquid
manometer, magnehelic gauge, or equivalent instrument), capable of
measuring up to the relief set pressure of the pressure-vacuum vents.
(2) Connect the pressure measurement device to a pressure tap in the
affected facility's vapor collection system, located as close as
possible to the connection with the marine vessel.
(3) During the performance test, record the pressure every 5 minutes
while a marine vessel is being loaded, and record the highest
instantaneous pressure that occurs during each loading cycle.
(e) Immediately prior to a performance test required for
determination of compliance with 61.302(b), all potential sources of
vapor leakage in the affected facility's vapor collection system
equipment shall be inspected for detectable emissions as required in
61.302(k). The monitoring shall be conducted only while a vapor-tight
tank truck, railcar, or marine vessel is being loaded. All identified
leaks in the terminal's vapor collection system shall be repaired prior
to conducting the performance test.
(f) The following test method shall be used to comply with the marine
vessel vapor-tightness requirements of 61.302(e)(3):
(1) Each benzene product tank shall be pressurized with dry air or
inert gas to not less than 1.0 psig and not more than the pressure of
the lowest relief valve setting.
(2) Once the pressure is obtained, the dry air or inert gas source
shall be shut off.
(3) At the end of one-half hour, the pressure in the benzene product
tank and piping shall be measured. The change in pressure shall be
calculated using the following formula:
DP=Pi^Pf
where:
DP=Change in pressure, inches of water.
Pi=Pressure in tank when air/gas source is shut off, inches of water.
Pf=Pressure in tank at the end of one-half hour after air/gas source
is shut off, inches of water.
(4) The change in pressure, DP, shall be compared to the pressure
drop calculated using the following formula:
DPM=0.861 Pia L/V
where:
DPM=Maximum allowable pressure change, inches of water.
Pia=Pressure in tank when air/gas source is shut off, pounds per
square inch, absolute (psia).
L=Maximum permitted loading rate of vessel, barrels per hour.
V=Total volume of product tank, barrels.
(5) If DP>DPM, the vessel is vapor tight.
(6) If DP DPM, the vessel is not vapor tight and the source of the
leak must be identified and repaired prior to retesting.
(55 FR 8341, Mar. 7, 1990; 55 FR 12444, Apr. 3, 1990