[[pp. 61793-61842]] Amendments for Testing and Monitoring Provisions

Note: EPA no longer updates this information, but it may be useful as a reference or resource.

[Federal Register: October 17, 2000 (Volume 65, Number 201)]
[Rules and Regulations]
[Page 61793-61842]
From the Federal Register Online via GPO Access [wais.access.gpo.gov]
[DOCID:fr17oc00-11]

[[Continued from page 61792]]

[[Page 61793]]

opening alignment is no longer within the specifications of Figure 2-2
and Figure 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.
10.2 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 6.7 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).
10.3 Temperature Sensors.
10.3.1 After each field use, calibrate dial thermometers, liquid-
filled bulb thermometers, thermocouple-potentiometer systems, and other
sensors at a temperature within 10 percent of the average absolute
stack temperature. For temperatures up to 405 deg.C (761 deg.F), use
an ASTM mercury-in-glass reference thermometer, or equivalent, as a
reference. Alternatively, either a reference thermocouple and
potentiometer (calibrated against NIST standards) or thermometric fixed
points (e.g., ice bath and boiling water, corrected for barometric
pressure) may be used. For temperatures above 405 deg.C (761 deg.F),
use a reference thermocouple-potentiometer system calibrated against
NIST standards or an alternative reference, subject to the approval of
the Administrator.
10.3.2 The temperature data recorded in the field shall be
considered valid. If, during calibration, the absolute temperature
measured with the sensor being calibrated and the reference sensor
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.
10.4 Barometer. Calibrate the barometer used against a mercury
barometer.

11.0 Analytical Procedure

Sample collection and analysis are concurrent for this method (see
Section 8.0).

12.0 Data Analysis and Calculations

Carry out calculations, retaining at least one extra significant
figure beyond that of the acquired data. Round off figures after final
calculation.
12.1 Nomenclature.

A = Cross-sectional area of stack, m\2\ (ft\2\).
Bws = Water vapor in the gas stream (from Method 4
(reference method) or Method 5), proportion by volume.
Cp = Pitot tube coefficient, dimensionless.
Cp(s) = Type S pitot tube coefficient, dimensionless.
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 6.7.1 to 6.7.5 of this method.
De = Equivalent diameter.
K = 0.127 mm H2O (metric units). 0.005 in. H2O
(English units).
Kp = Velocity equation constant.
L = Length.
Md = Molecular weight of stack gas, dry basis (see Section
8.6), g/g-mole (lb/lb-mole).
Ms = Molecular weight of stack gas, wet basis, g/g-mole (lb/
lb-mole).
n = Total number of traverse points.
Pbar = Barometric pressure at measurement site, mm Hg (in.
Hg).
Pg = Stack static pressure, mm Hg (in. Hg).
Ps = Absolute stack pressure (Pbar +
Pg), mm Hg (in. Hg),
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).
T = Sensitivity factor for differential pressure gauges.
Ts = Stack temperature, deg.C ( deg.F).
Ts(abs) = Absolute stack temperature, deg.K ( deg.R).
= 273 + Ts for metric units,
= 460 + Ts for English units.
Tstd = Standard absolute temperature, 293 deg.K (528
deg.R).
Vs = Average stack gas velocity, m/sec (ft/sec).
W = Width.
p = Velocity head of stack gas, mm H2O (in.
H20).
pi = Individual velocity head reading at traverse
point ``i'', mm (in.) H2O.
pstd = Velocity head measured by the standard pitot
tube, cm (in.) H2O.
ps = Velocity head measured by the Type S pitot
tube, cm (in.) H2O.
3600 = Conversion Factor, sec/hr.
18.0 = Molecular weight of water, g/g-mole (lb/lb-mole).

12.2 Calculate T as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.045

12.3 Calculate De as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.046

12.4 Calibration of Type S Pitot Tube.
12.4.1 For each of the six pairs of p readings (i.e.,
three from side A and three from side B) obtained in Section 10.1.3,
calculate the value of the Type S pitot tube coefficient according to
Equation 2-3:
[GRAPHIC] [TIFF OMITTED] TR17OC00.047

12.4.2 Calculate Cp(A), the mean A-side coefficient,
and Cp(B), the mean B-side coefficient. Calculate the
difference between these two average values.
12.4.3 Calculate the deviation of each of the three A-side values
of Cp(s) from Cp(A), and the deviation of each of
the three B-side values of Cp(s) from Cp(B),
using Equation 2-4:
[GRAPHIC] [TIFF OMITTED] TR17OC00.048

12.4.4 Calculate the average deviation from the mean,
for both the A and B sides of the pitot tube. Use Equation 2-5:
[GRAPHIC] [TIFF OMITTED] TR17OC00.049

12.5 Molecular Weight of Stack Gas.
[GRAPHIC] [TIFF OMITTED] TR17OC00.050

12.6 Average Stack Gas Velocity.

[[Page 61794]]

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[GRAPHIC] [TIFF OMITTED] TR17OC00.052

[GRAPHIC] [TIFF OMITTED] TR17OC00.053

12.7 Average Stack Gas Dry Volumetric Flow Rate.
[GRAPHIC] [TIFF OMITTED] TR17OC00.054

13.0 Method Performance [Reserved]

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 References

1. Mark, L.S. Mechanical Engineers' Handbook. New York. McGraw-
Hill Book Co., Inc. 1951.
2. Perry, J.H., ed. 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, N.C. (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, N.Y. 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, N.C.
(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, N.C. 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 Baseline 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 Tube Coefficients.
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, CT. 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., et al. 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.

[[Page 61795]]

17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.055

[[Page 61796]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.056

[[Page 61797]]

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[[Page 61798]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.058

[[Page 61799]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.059

PLANT-----------------------------------------------------------------
DATE------------------------------------------------------------------
RUN NO.---------------------------------------------------------------
STACK DIA. OR DIMENSIONS, m (in.)-------------------------------------
BAROMETRIC PRESS., mm Hg (in. Hg)-------------------------------------
CROSS SECTIONAL AREA, m\2\ (ft\2\)------------------------------------
OPERATORS-------------------------------------------------------------
PITOT TUBE I.D. NO.---------------------------------------------------
AVG. COEFFICIENT, Cp =------------------------------------------------
LAST DATE CALIBRATED--------------------------------------------------

------------------------------------------------------------------------

-------------------------------------------------------------------------

------------------------------------------------------------------------

SCHEMATIC OF STACK CROSS SECTION

[[Page 61800]]

--------------------------------------------------------------------------------------------------------------------------------------------------------
Stack temperature
Traverse Pt. No. Vel. Hd., p ----------------------------------------------- Pg mm Hg (in. Hg) (p)\1/2\
mm (in.) H2O Ts, deg.C ( deg.F) Ts, deg.K ( deg.R)
--------------------------------------------------------------------------------------------------------------------------------------------------------

--------------------------------------------------------------------------------------------------------------------------------------------------------

--------------------------------------------------------------------------------------------------------------------------------------------------------
Average(1)
--------------------------------------------------------------------------------------------------------------------------------------------------------

Figure 2-6. Velocity Traverse Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.060

[[Page 61801]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.061

[[Page 61802]]

PITOT TUBE IDENTIFICATION NUMBER:-------------------------------------
DATE:-----------------------------------------------------------------
CALIBRATED BY:--------------------------------------------------------

``A'' Side Calibration
----------------------------------------------------------------------------------------------------------------
Pstd cm P(s) cm Deviation Cp(s)--
Run No. H2O (in H2O) H2O (in H2O) Cp(s) Cp(A)
----------------------------------------------------------------------------------------------------------------
1
----------------------------------------------------------------------------------------------------------------
2
----------------------------------------------------------------------------------------------------------------
3
----------------------------------------------------------------------------------------------------------------
Cp, avg
(SIDE A)
----------------------------------------------------------------------------------------------------------------

``B'' Side Calibration
----------------------------------------------------------------------------------------------------------------
Pstd cm P(s) cm Deviation Cp(s)--
Run No. H2O (in H2O) H2O (in H2O) Cp(s) Cp(B)
----------------------------------------------------------------------------------------------------------------
1
----------------------------------------------------------------------------------------------------------------
2
----------------------------------------------------------------------------------------------------------------
3
----------------------------------------------------------------------------------------------------------------
Cp, avg
(SIDE B)
----------------------------------------------------------------------------------------------------------------

[GRAPHIC] [TIFF OMITTED] TR17OC00.062

[Cp, avg (side A)--Cp, avg (side B)]*

*Must be less than or equal to 0.01
Figure 2-9. Pitot Tube Calibration Data

[[Page 61803]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.063

Method 2A--Direct Measurement of Gas Volume Through Pipes and Small
Ducts

Note: This method does not include all of the specifications
(e.g., equipment and supplies) and procedures (e.g., sampling)
essential to its performance. Some material is incorporated by
reference from other methods in this part. Therefore, to obtain
reliable results, persons using this method should have a thorough
knowledge of at least the following additional test methods: Method
1, Method 2.

1.0 Scope and Application

1.1 This method is applicable for the determination of gas flow
rates in pipes and small ducts, either in-line or at exhaust positions,
within the temperature range of 0 to 50 deg.C (32 to 122 deg.F).
1.2 Data Quality Objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.

2.0 Summary of Method

2.1 A gas volume meter is used to measure gas volume directly.
Temperature and pressure measurements are made to allow correction of
the volume to standard conditions.

3.0 Definitions [Reserved]

4.0 Interferences [Reserved]

5.0 Safety

5.1 Disclaimer. This method may involve hazardous materials,
operations, and equipment. This test method may

[[Page 61804]]

not address all of the safety problems associated with its use. It is
the responsibility of the user of this test method to establish
appropriate safety and health practices and determine the applicability
of regulatory limitations prior to performing this test method.

6.0 Equipment and Supplies

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.
6.1 Gas Volume Meter. A positive displacement meter, turbine
meter, or other direct measuring device capable of measuring volume to
within 2 percent. The meter shall be equipped with a temperature sensor
(accurate to within 2 percent of the minimum absolute
temperature) and a pressure gauge (accurate to within 2.5
mm Hg). The manufacturer's recommended capacity of the meter shall be
sufficient for the expected maximum and minimum flow rates for the
sampling conditions. Temperature, pressure, corrosive characteristics,
and pipe size are factors necessary to consider in selecting a suitable
gas meter.
6.2 Barometer. A mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg.

Note: 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 (0.1 in.) Hg per 30 m (100 ft) elevation increase or vice versa
for elevation decrease.

6.3 Stopwatch. Capable of measurement to within 1 second.

7.0 Reagents and Standards [Reserved]

8.0 Sample Collection and Analysis

8.1 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.
8.2 Leak Test.
8.2.1 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.
8.2.2 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 to assure
leak-tight seals.
8.3 Volume Measurement.
8.3.1 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 temperatures and pressures 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, and
pressure. Record the barometric pressure at the beginning and end of
the test run. Record the data on a table similar to that shown in
Figure 2A-1.
8.3.2 For sources with noncontinuous, non-steady emission flow
rates, use the procedure in Section 8.3.1 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.

9.0 Quality Control

------------------------------------------------------------------------
Quality control
Section measure Effect
------------------------------------------------------------------------
10.1-10.4..................... Sampling Ensure accurate
equipment measurement of stack
calibration. gas flow rate,
sample volume.
------------------------------------------------------------------------

10.0 Calibration and Standardization

10.1 Volume Meter.
10.1.1 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.
10.1.2 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.
10.1.3 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 sensor and pressure gauge 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.
10.1.4 The calibration shall be performed during at least three
different flow rates. The calibration flow rates shall be about 0.3,
0.6, and 0.9 times the rated maximum flow rate of the test meter.
10.1.5 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.
10.1.6 Calculate the test meter calibration coefficient as
indicated in Section 12.2.
10.1.7 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.
10.1.8 The procedure above shall be performed at least once for
each volume meter. Thereafter, an abbreviated calibration check shall
be completed

[[Page 61805]]

following each field test. The calibration of the volume meter shall be
checked with the meter pressure set at the average value encountered
during the field test. Three calibration checks (runs) shall be
performed using this average flow rate value. 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.

10.2 Temperature Sensor. After each test series, check the
temperature sensor at ambient temperature. Use an American Society for
Testing and Materials (ASTM) mercury-in-glass reference thermometer, or
equivalent, as a reference. If the sensor 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 results shall be
made, subject to the approval of the Administrator.
10.3 Barometer. Calibrate the barometer used against a mercury
barometer prior to the field test.

11.0 Analytical Procedure

Sample collection and analysis are concurrent for this method (see
Section 8.0).

12.0 Data Analysis and Calculations

Carry out calculations, retaining at least one extra decimal figure
beyond that of the acquired data. Round off figures after final
calculation.

12.1 Nomenclature.

f = Final reading.
i = Initial reading.
Pbar = Barometric pressure, mm Hg.
Pg = Average static pressure in volume meter, mm Hg.
Qs = Gas flow rate, m3/min, standard conditions.
s = Standard conditions, 20 deg.C and 760 mm Hg.
Tr = Reference meter average temperature, deg.K ( deg.R).
Tm = Test meter average temperature, deg.K ( deg.R).
Vr = Reference meter volume reading, m3.
Vm = Test meter volume reading, m3.
Ym = Test meter calibration coefficient, dimensionless.
= Elapsed test period time, min.

12.2 Test Meter Calibration Coefficient.
[GRAPHIC] [TIFF OMITTED] TR17OC00.064

12.3 Volume.
[GRAPHIC] [TIFF OMITTED] TR17OC00.065

12.4 Gas Flow Rate.
[GRAPHIC] [TIFF OMITTED] TR17OC00.066

13.0 Method Performance. [Reserved]

14.0 Pollution Prevention. [Reserved]

15.0 Waste Management. [Reserved]

16.0 References

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.

17.0 Tables, Diagrams, Flowcharts, and Validation Data [Reserved]

Method 2B--Determination of Exhaust Gas Volume Flow Rate From
Gasoline Vapor Incinerators

Note: This method does not include all of the specifications
(e.g., equipment and supplies) and procedures (e.g., sampling and
analytical) essential to its performance. Some material is
incorporated by reference from other methods in this part.
Therefore, to obtain reliable results, persons using this method
should also have a thorough knowledge of at least the following
additional test methods: Method 1, Method 2, Method 2A, Method 10,
Method 25A, Method 25B.

1.0 Scope and Application

1.1 This method is applicable for the determination 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 Data Quality Objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.

2.0 Summary of Method

2.1 Organic carbon concentration and volume flow rate are measured
at the incinerator inlet using either Method 25A or Method 25B and
Method 2A, respectively. Organic carbon, carbon dioxide
(CO2), and carbon monoxide (CO) concentrations are measured
at the outlet using either Method 25A or Method 25B and Method 10,
respectively. The ratio of total carbon at the incinerator inlet and
outlet is multiplied by the inlet volume to determine the exhaust
volume flow rate.

3.0 Definitions

Same as Section 3.0 of Method 10 and Method 25A.

4.0 Interferences

Same as Section 4.0 of Method 10.

[[Page 61806]]

5.0 Safety

5.1 This method may involve hazardous materials, operations, and
equipment. This test method may not address all of the safety problems
associated with its use. It is the responsibility of the user of this
test method to establish appropriate safety and health practices and
determine the applicability of regulatory limitations prior to
performing this test method.

6.0 Equipment and Supplies

Same as Section 6.0 of Method 2A, Method 10, and Method 25A and/or
Method 25B as applicable, with the addition of the following:
6.1 This analyzer must meet the specifications set forth in
Section 6.1.2 of Method 10, except that the span shall be 15 percent
CO2 by volume.

7.0 Reagents and Standards

Same as Section 7.0 of Method 10 and Method 25A, with the following
addition and exceptions:
7.1 Carbon Dioxide Analyzer Calibration. CO2 gases
meeting the specifications set forth in Section 7 of Method 6C are
required.
7.2 Hydrocarbon Analyzer Calibration. Methane shall not be used as
a calibration gas when performing this method.
7.3 Fuel Gas. If Method 25B is used to measure the organic carbon
concentrations at both the inlet and exhaust, no fuel gas is required.

8.0 Sample Collection and Analysis

8.1 Pre-test Procedures. Perform all pre-test procedures (e.g.,
system performance checks, leak checks) necessary to determine gas
volume flow rate and organic carbon concentration in the vapor line to
the incinerator inlet and to determine organic carbon, carbon monoxide,
and carbon dioxide concentrations at the incinerator exhaust, as
outlined in Method 2A, Method 10, and Method 25A and/or Method 25B as
applicable.
8.2 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. Conduct sampling and analysis as
outlined in Method 2A, Method 10, and Method 25A and/or Method 25B as
applicable. 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.
8.3 Post-test Procedures. Perform all post-test procedures (e.g.,
drift tests, leak checks), as outlined in Method 2A, Method 10, and
Method 25A and/or Method 25B as applicable.

9.0 Quality Control

Same as Section 9.0 of Method 2A, Method 10, and Method 25A.

10.0 Calibration and Standardization

Same as Section 10.0 of Method 2A, Method 10, and Method 25A.

Note: If a manifold system is used for the exhaust analyzers,
all the analyzers and sample pumps must be operating when the
analyzer calibrations are performed.

10.1 If an analyzer output does not meet the specifications of the
method, invalidate the test data for the period. Alternatively,
calculate the exhaust 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.

11.0 Analytical Procedure

Sample collection and analysis are concurrent for this method (see
Section 8.0).

12.0 Data Analysis and 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.
12.1 Nomenclature.

Coe = Mean carbon monoxide concentration in system exhaust,
ppm.
(CO2)2 = Ambient carbon dioxide concentration,
ppm (if not measured during the test period, may be assumed to equal
300 ppm).
(CO2)e = 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.
Ke = Hydrocarbon calibration gas factor for the exhaust
hydrocarbon analyzer, unitless [equal to the number of carbon atoms per
molecule of the gas used to calibrate the analyzer (2 for ethane, 3 for
propane, etc.)].
Ki = Hydrocarbon calibration gas factor for the inlet
hydrocarbon analyzer, unitless.
Ves = Exhaust gas volume, m\3\.
Vis = Inlet gas volume, m\3\.
Qes = Exhaust gas volume flow rate, m\3\/min.
Qis = Inlet gas volume flow rate, m\3\/min.
= Sample run time, min.
s = Standard conditions: 20 deg.C, 760 mm Hg.

12.2 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.
12.3 Exhaust Gas Volume. Calculate the exhaust gas volume as
follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.067

[[Page 61807]]

12.4 Exhaust Gas Volume Flow Rate. Calculate the exhaust gas
volume flow rate as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.210

13.0 Method Performance [Reserved]

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 References

Same as Section 16.0 of Method 2A, Method 10, and Method 25A.

17.0 Tables, Diagrams, Flowcharts, and Validation Data [Reserved]

Method 2C--Determination of Gas Velocity and Volumetric Flow Rate
in Small Stacks or Ducts (Standard Pitot Tube)

Note: This method does not include all of the specifications
(e.g., equipment and supplies) and procedures (e.g., sampling)
essential to its performance. Some material is incorporated by
reference from other methods in this part. Therefore, to obtain
reliable results, persons using this method should also have a
thorough knowledge of at least the following additional test
methods: Method 1, Method 2.

1.0 Scope and Application

1.1 This method is applicable for the determination of average
velocity and volumetric flow rate of gas streams in small stacks or
ducts. Limits on the applicability of this method are identical to
those set forth in Method 2, Section 1.0, except that this method is
limited to stationary source 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 Data Quality Objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.

2.0 Summary of Method

2.1 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.

3.0 Definitions [Reserved]

4.0 Interferences [Reserved]

5.0 Safety

6.0 Equipment and Supplies

Same as Method 2, Section 6.0, with the exception of the following:
6.1 Standard Pitot Tube (instead of Type S). A standard pitot tube
which meets the specifications of Section 6.7 of Method 2. Use a
coefficient of 0.99 unless it is calibrated against another standard
pitot tube with a NIST-traceable coefficient (see Section 10.2 of
Method 2).
6.2 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. Use a coefficient of 0.99 unless it
is calibrated as mentioned in Section 6.1 above. This pitot tube is
useful in particulate liquid droplet-laden gas streams when a ``back
purge'' is ineffective.

7.0 Reagents and Standards [Reserved]

8.0 Sample Collection and Analysis

8.1 Follow the general procedures in Section 8.0 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 particulate-laden gas streams.
Therefore, adequate proof that the openings of the pitot tube have not
plugged during the traverse period must be furnished; this can be done
by taking the velocity head (p) heading 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 (within 5 percent) the traverse
is acceptable. Otherwise, reject the run. Note that if the 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 take comparative p readings, as above, for the
last two back purges at which suitably high p readings are
observed.

9.0 Quality Control

10.0 Calibration and Standardization

Same as Method 2, Sections 10.2 through 10.4.

11.0 Analytical Procedure

Sample collection and analysis are concurrent for this method (see
Section 8.0).

12.0 Calculations and Data Analysis

Same as Method 2, Section 12.0.

13.0 Method Performance [Reserved]

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 References

Same as Method 2, Section 16.0.

[[Page 61808]]

17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.068

Method 2D--Measurement of Gas Volume Flow Rates in Small Pipes and
Ducts

Note: This method does not include all of the specifications
(e.g., equipment and supplies) and procedures (e.g., sampling)
essential to its performance. Some material is incorporated by
reference from other methods in this part. Therefore, to obtain
reliable results, persons using this method should also have a
thorough knowledge of at least the following additional test
methods: Method 1, Method 2, and Method 2A.

1.0 Scope and Application

1.1 This method is applicable for the determination of the
volumetric flow rates of gas streams in small pipes and ducts. It can
be applied to intermittent or variable gas flows only with particular
caution.
1.2 Data Quality Objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.

2.0 Summary of Method

2.1 All the gas flow in the pipe or duct is directed through a
rotameter, orifice plate or similar device to measure flow rate or
pressure drop. The device has been previously calibrated in a manner
that insures its proper calibration for the gas being measured.
Absolute temperature and pressure measurements are made to allow
correction of volumetric flow rates to standard conditions.

3.0 Definitions. [Reserved]

4.0 Interferences. [Reserved]

5.0 Safety

6.0 Equipment and Supplies

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.
6.1 Gas Metering Rate or Flow Element Device. A rotameter, orifice
plate, or other volume rate or pressure drop measuring device capable
of measuring the stack flow rate to within 5 percent. The
metering 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 metering 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, dewpoint, and corrosive characteristics, and
pipe or duct size are factors to consider in choosing a suitable
metering device.
6.2 Barometer. Same as Method 2, Section 6.5.
6.3 Stopwatch. Capable of measurement to within 1 second.

7.0 Reagents and Standards. [Reserved]

8.0 Sample Collection and Analysis

8.1 Installation and Leak Check. Same as Method 2A, Sections 8.1
and 8.2, respectively.
8.2 Volume Rate Measurement.
8.2.1 Continuous, Steady Flow. At least once an hour, record the
metering device flow rate or pressure drop reading, and the metering
device temperature and pressure. Make a minimum of 12 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 that shown in Figure 2D-1.
8.2.2 Noncontinuous and Nonsteady Flow. Use volume rate devices
with particular caution. Calibration will be affected by variation in
stack gas temperature, pressure and molecular

[[Page 61809]]

weight. Use the procedure in Section 8.2.1 with the addition of the
following: Record all the metering device parameters on a time interval
frequency sufficient to adequately profile each process cyclical or
noncontinuous event. A multichannel continuous recorder may be used.

9.0 Quality Control

10.0 Calibration and Standardization

Same as Method 2A, Section 10.0, with the following exception:
10.1 Gas Metering Device. Same as Method 2A, Section 10.1, except
calibrate the metering device with the principle stack gas to be
measured (examples: air, nitrogen) against a standard reference meter.
A calibrated dry gas meter is an acceptable reference meter. Ideally,
calibrate the metering device in the field with the actual gas to be
metered. For metering devices that have a volume rate readout,
calculate the test metering device calibration coefficient,
Ym, for each run shown in Equation 2D-2 Section 12.3.
10.2 For metering devices that do not have a volume rate readout,
refer to the manufacturer's instructions to calculate the
Vm2 corresponding to each Vr.
10.3 Temperature Gauge. Use the procedure and specifications in
Method 2A, Section 10.2. Perform the calibration at a temperature that
approximates field test conditions.
10.4 Barometer. Calibrate the barometer to be used in the field
test with a mercury barometer prior to the field test.

11.0 Analytical Procedure.

Sample collection and analysis are concurrent for this method (see
Section 8.0).

12.0 Data Analysis and Calculations

12.1 Nomenclature.

Pbar = Barometric pressure, mm Hg (in. Hg).
Pm = Test meter average static pressure, mm Hg (in. Hg).
Qr = Reference meter volume flow rate reading, m\3\/min
(ft\3\/min).
Qm = Test meter volume flow rate reading, m\3\/min (ft\3\/
min).
Tr = Absolute reference meter average temperature, deg.K
( deg.R).
Tm = Absolute test meter average temperature, deg.K
( deg.R).
Kl = 0.3855 deg.K/mm Hg for metric units, = 17.65 deg.R/
in. Hg for English units.
12.2 Gas Flow Rate.

[GRAPHIC] [TIFF OMITTED] TR17OC00.069

12.3 Test Meter Device Calibration Coefficient. Calculation for
testing metering device calibration coefficient, Ym.
[GRAPHIC] [TIFF OMITTED] TR17OC00.070

13.0 Method Performance [Reserved]

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 References

1. Spink, L.K. Principles and Practice of Flowmeter Engineering.
The Foxboro Company. Foxboro, MA. 1967.
2. Benedict, R.P. Fundamentals of Temperature, Pressure, and
Flow Measurements. John Wiley & Sons, Inc. New York, NY. 1969.
3. Orifice Metering of Natural Gas. American Gas Association.
Arlington, VA. Report No. 3. March 1978. 88 pp.

17.0 Tables, Diagrams, Flowcharts, and Validation Data

Plant-----------------------------------------------------------------
Date------------------------------------------------------------------
Run No.---------------------------------------------------------------
Sample location-------------------------------------------------------
Barometric pressure (mm Hg):
Start-----------------------------------------------------------------
Finish----------------------------------------------------------------
Operators-------------------------------------------------------------
Metering device No.---------------------------------------------------
Calibration coefficient-----------------------------------------------
Calibration gas-------------------------------------------------------
Date to recalibrate---------------------------------------------------

----------------------------------------------------------------------------------------------------------------
Temperature
Time Flow rate reading Static Pressure ---------------------------------------
[mm Hg (in. Hg)] deg.C ( deg.F) deg.K ( deg.R)
----------------------------------------------------------------------------------------------------------------

----------------------------------------------------------------------------------------------------------------

----------------------------------------------------------------------------------------------------------------
Average
----------------------------------------------------------------------------------------------------------------

Figure 2D-1. Volume Flow Rate Measurement Data

[[Page 61810]]

Method 2E--Determination of Landfill Gas Production Flow Rate

1.0 Scope and Application

1.1 Applicability. This method applies to the measurement of
landfill gas (LFG) production flow rate from municipal solid waste
landfills and is used to calculate the flow rate of nonmethane organic
compounds (NMOC) from landfills.
1.2 Data Quality Objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.

2.0 Summary of Method

2.1 Extraction wells are installed either in a cluster of three or
at five dispersed locations in the landfill. A blower is used to
extract LFG from the landfill. LFG composition, landfill pressures, and
orifice pressure differentials from the wells are measured and the
landfill gas production flow rate is calculated.

3.0 Definitions [Reserved]

4.0 Interferences [Reserved]

5.0 Safety

5.1 Since this method is complex, only experienced personnel
should perform the test. Landfill gas contains methane, therefore
explosive mixtures may exist at or near the landfill. It is advisable
to take appropriate safety precautions when testing landfills, such as
refraining from smoking and installing explosion-proof equipment.

6.0 Equipment and Supplies

6.1 Well Drilling Rig. Capable of boring a 0.61 m (24 in.)
diameter hole into the landfill to a minimum of 75 percent of the
landfill depth. The depth of the well shall not extend to the bottom of
the landfill or the liquid level.
6.2 Gravel. No fines. Gravel diameter should be appreciably larger
than perforations stated in Sections 6.10 and 8.2.
6.3 Bentonite.
6.4 Backfill Material. Clay, soil, and sandy loam have been found
to be acceptable.
6.5 Extraction Well Pipe. Minimum diameter of 3 in., constructed
of polyvinyl chloride (PVC), high density polyethylene (HDPE),
fiberglass, stainless steel, or other suitable nonporous material
capable of transporting landfill gas.
6.6 Above Ground Well Assembly. Valve capable of adjusting gas
flow, such as a gate, ball, or butterfly valve; sampling ports at the
well head and outlet; and a flow measuring device, such as an in-line
orifice meter or pitot tube. A schematic of the aboveground well head
assembly is shown in Figure 2E-1.
6.7 Cap. Constructed of PVC or HDPE.
6.8 Header Piping. Constructed of PVC or HDPE.
6.9 Auger. Capable of boring a 0.15-to 0.23-m (6-to 9-in.)
diameter hole to a depth equal to the top of the perforated section of
the extraction well, for pressure probe installation.
6.10 Pressure Probe. Constructed of PVC or stainless steel (316),
0.025-m (1-in.). Schedule 40 pipe. Perforate the bottom two-thirds. A
minimum requirement for perforations is slots or holes with an open
area equivalent to four 0.006-m (\1/4\-in.) diameter holes spaced
90 deg. apart every 0.15 m (6 in.).
6.11 Blower and Flare Assembly. Explosion-proof blower, capable of
extracting LFG at a flow rate of 8.5 m 3/min (300 ft
3/min), a water knockout, and flare or incinerator.
6.12 Standard Pitot Tube and Differential Pressure Gauge for Flow
Rate Calibration with Standard Pitot. Same as Method 2, Sections 6.7
and 6.8.
6.13 Orifice Meter. Orifice plate, pressure tabs, and pressure
measuring device to measure the LFG flow rate.
6.14 Barometer. Same as Method 4, Section 6.1.5.
6.15 Differential Pressure Gauge. Water-filled U-tube manometer or
equivalent, capable of measuring within 0.02 mm Hg (0.01 in.
H2O), for measuring the pressure of the pressure probes.

7.0 Reagents and Standards. Not Applicable

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Placement of Extraction Wells. The landfill owner or operator
may install a single cluster of three extraction wells in a test area
or space five equal-volume wells over the landfill. The cluster wells
are recommended but may be used only if the composition, age of the
refuse, and the landfill depth of the test area can be determined.
8.1.1 Cluster Wells. Consult landfill site records for the age of
the refuse, depth, and composition of various sections of the landfill.
Select an area near the perimeter of the landfill with a depth equal to
or greater than the average depth of the landfill and with the average
age of the refuse between 2 and 10 years old. Avoid areas known to
contain nondecomposable materials, such as concrete and asbestos.
Locate the cluster wells as shown in Figure 2E-2.
8.1.1.1 The age of the refuse in a test area will not be uniform,
so calculate a weighted average age of the refuse as shown in Section
12.2.
8.1.2 Equal Volume Wells. Divide the sections of the landfill that
are at least 2 years old into five areas representing equal volumes.
Locate an extraction well near the center of each area.
8.2 Installation of Extraction Wells. Use a well drilling rig to
dig a 0.6 m (24 in.) diameter hole in the landfill to a minimum of 75
percent of the landfill depth, not to extend to the bottom of the
landfill or the liquid level. Perforate the bottom two thirds of the
extraction well pipe. A minimum requirement for perforations is holes
or slots with an open area equivalent to 0.01-m (0.5-in.) diameter
holes spaced 90 deg. apart every 0.1 to 0.2 m (4 to 8 in.). Place the
extraction well in the center of the hole and backfill with gravel to a
level 0.30 m (1 ft) above the perforated section. Add a layer of
backfill material 1.2 m (4 ft) thick. Add a layer of bentonite 0.9 m (3
ft) thick, and backfill the remainder of the hole with cover material
or material equal in permeability to the existing cover material. The
specifications for extraction well installation are shown in Figure 2E-
3.
8.3 Pressure Probes. Shallow pressure probes are used in the check
for infiltration of air into the landfill, and deep pressure probes are
use to determine the radius of influence. Locate pressure probes along
three radial arms approximately 120 deg. apart at distances of 3, 15,
30, and 45 m (10, 50, 100, and 150 ft) from the extraction well. The
tester has the option of locating additional pressure probes at
distances every 15 m (50 feet) beyond 45 m (150 ft). Example placements
of probes are shown in Figure 2E-4. The 15-, 30-, and 45-m, (50-, 100-,
and 150-ft) probes from each well, and any additional probes located
along the three radial arms (deep probes), shall

[[Page 61811]]

extend to a depth equal to the top of the perforated section of the
extraction wells. All other probes (shallow probes) shall extend to a
depth equal to half the depth of the deep probes.
8.3.1 Use an auger to dig a hole, 0.15- to 0.23-m (6-to 9-in.) in
diameter, for each pressure probe. Perforate the bottom two thirds of
the pressure probe. A minimum requirement for perforations is holes or
slots with an open area equivalent to four 0.006-m (0.25-in.) diameter
holes spaced 90 deg. apart every 0.15 m (6 in.). Place the pressure
probe in the center of the hole and backfill with gravel to a level
0.30 m (1 ft) above the perforated section. Add a layer of backfill
material at least 1.2 m (4 ft) thick. Add a layer of bentonite at least
0.3 m (1 ft) thick, and backfill the remainder of the hole with cover
material or material equal in permeability to the existing cover
material. The specifications for pressure probe installation are shown
in Figure 2E-5.
8.4 LFG Flow Rate Measurement. Place the flow measurement device,
such as an orifice meter, as shown in Figure 2E-1. Attach the wells to
the blower and flare assembly. The individual wells may be ducted to a
common header so that a single blower, flare assembly, and flow meter
may be used. Use the procedures in Section 10.1 to calibrate the flow
meter.
8.5 Leak-Check. A leak-check of the above ground system is
required for accurate flow rate measurements and for safety. Sample LFG
at the well head sample port and at the outlet sample port. Use Method
3C to determine nitrogen (N2) concentrations. Determine the
difference between the well head and outlet N2
concentrations using the formula in Section 12.3. The system passes the
leak-check if the difference is less than 10,000 ppmv.
8.6 Static Testing. Close the control valves on the well heads
during static testing. Measure the gauge pressure (Pg) at
each deep pressure probe and the barometric pressure (Pbar)
every 8 hours (hr) for 3 days. Convert the gauge pressure of each deep
pressure probe to absolute pressure using the equation in Section 12.4.
Record as Pi (initial absolute pressure).
8.6.1 For each probe, average all of the 8-hr deep pressure probe
readings (Pi) and record as Pia (average absolute
pressure). Pia is used in Section 8.7.5 to determine the
maximum radius of influence.
8.6.2 Measure the static flow rate of each well once during static
testing.
8.7 Short-Term Testing. The purpose of short-term testing is to
determine the maximum vacuum that can be applied to the wells without
infiltration of ambient air into the landfill. The short-term testing
is performed on one well at a time. Burn all LFG with a flare or
incinerator.
8.7.1 Use the blower to extract LFG from a single well at a rate
at least twice the static flow rate of the respective well measured in
Section 8.6.2. If using a single blower and flare assembly and a common
header system, close the control valve on the wells not being measured.
Allow 24 hr for the system to stabilize at this flow rate.
8.7.2 Test for infiltration of air into the landfill by measuring
the gauge pressures of the shallow pressure probes and using Method 3C
to determine the LFG N2 concentration. If the LFG
N2 concentration is less than 5 percent and all of the
shallow probes have a positive gauge pressure, increase the blower
vacuum by 3.7 mm Hg (2 in. H2O), wait 24 hr, and repeat the
tests for infiltration. Continue the above steps of increasing blower
vacuum by 3.7 mm Hg (2 in. H2O), waiting 24 hr, and testing
for infiltration until the concentration of N2 exceeds 5
percent or any of the shallow probes have a negative gauge pressure.
When this occurs,reduce the blower vacuum to the maximum setting at
which the N2 concentration was less than 5 percent and the
gauge pressures of the shallow probes are positive.
8.7.3 At this blower vacuum, measure atmospheric pressure
(Pbar) every 8 hr for 24 hr, and record the LFG flow rate
(Qs) and the probe gauge pressures (Pf) for all
of the probes. Convert the gauge pressures of the deep probes to
absolute pressures for each 8-hr reading at Qs as shown in
Section 12.4.
8.7.4 For each probe, average the 8-hr deep pressure probe
absolute pressure readings and record as Pfa (the final
average absolute pressure).
8.7.5 For each probe, compare the initial average pressure
(Pia) from Section 8.6.1 to the final average pressure
(Pfa). Determine the furthermost point from the well head
along each radial arm where Pfa Pia.
This distance is the maximum radius of influence (Rm), which
is the distance from the well affected by the vacuum. Average these
values to determine the average maximum radius of influence
(Rma).
8.7.6 Calculate the depth (Dst) affected by the
extraction well during the short term test as shown in Section 12.6. If
the computed value of Dst exceeds the depth of the landfill,
set Dst equal to the landfill depth.
8.7.7 Calculate the void volume (V) for the extraction well as
shown in Section 12.7.
8.7.8 Repeat the procedures in Section 8.7 for each well.
8.8 Calculate the total void volume of the test wells
(Vv) by summing the void volumes (V) of each well.
8.9 Long-Term Testing. The purpose of long-term testing is to
extract two void volumes of LFG from the extraction wells. Use the
blower to extract LFG from the wells. If a single Blower and flare
assembly and common header system are used, open all control valves and
set the blower vacuum equal to the highest stabilized blower vacuum
demonstrated by any individual well in Section 8.7. Every 8 hr, sample
the LFG from the well head sample port, measure the gauge pressures of
the shallow pressure probes, the blower vacuum, the LFG flow rate, and
use the criteria for infiltration in Section 8.7.2 and Method 3C to
test for infiltration. If infiltration is detected, do not reduce the
blower vacuum, instead reduce the LFG flow rate from the well by
adjusting the control valve on the well head. Adjust each affected well
individually. Continue until the equivalent of two total void volumes
(Vv) have been extracted, or until Vt =
2Vv.
8.9.1 Calculate Vt, the total volume of LFG extracted
from the wells, as shown in Section 12.8.
8.9.2 Record the final stabilized flow rate as Qf and
the gauge pressure for each deep probe. If, during the long term
testing, the flow rate does not stabilize, calculate Qf by
averaging the last 10 recorded flow rates.
8.9.3 For each deep probe, convert each gauge pressure to absolute
pressure as in Section 12.4. Average these values and record as
Psa. For each probe, compare Pia to
Psa. Determine the furthermost point from the well head
along each radial arm where Psa Pia.
This distance is the stabilized radius of influence. Average these
values to determine the average stabilized radius of influence
(Rsa).
8.10 Determine the NMOC mass emission rate using the procedures in
Section 12.9 through 12.15.

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures.

[[Page 61812]]

10.0 Calibration and Standardization

10.1 LFG Flow Rate Meter (Orifice) Calibration Procedure. Locate a
standard pitot tube in line with an orifice meter. Use the procedures
in Section 8, 12.5, 12.6, and 12.7 of Method 2 to determine the average
dry gas volumetric flow rate for at least five flow rates that bracket
the expected LFG flow rates, except in Section 8.1, use a standard
pitot tube rather than a Type S pitot tube. Method 3C may be used to
determine the dry molecular weight. It may be necessary to calibrate
more than one orifice meter in order to bracket the LFG flow rates.
Construct a calibration curve by plotting the pressure drops across the
orifice meter for each flow rate versus the average dry gas volumetric
flow rate in m\3\/min of the gas.

11.0 Procedures [Reserved]

12.0 Data Analysis and Calculations

12.1 Nomenclature.

A = Age of landfill, yr.
Aavg = Average age of the refuse tested, yr.
Ai = Age of refuse in the ith fraction, yr.
Ar = Acceptance rate, Mg/yr.
CNMOC = NMOC concentration, ppmv as hexane (CNMOC
= Ct/6).
Co = Concentration of N2 at the outlet, ppmv.
Ct = NMOC concentration, ppmv (carbon equivalent) from
Method 25C.
Cw = Concentration of N2 at the wellhead, ppmv.
D = Depth affected by the test wells, m.
Dst = Depth affected by the test wells in the short-term
test, m.
e = Base number for natural logarithms (2.718).
f = Fraction of decomposable refuse in the landfill.
fi = Fraction of the refuse in the ith section.
k = Landfill gas generation constant, yr-\1\.
Lo = Methane generation potential, m\3\/Mg.
Lo' = Revised methane generation potential to account for
the amount of nondecomposable material in the landfill, m\3\/Mg.
Mi = Mass of refuse in the ith section, Mg.
Mr = Mass of decomposable refuse affected by the test well,
Mg.
Pbar = Atmospheric pressure, mm Hg.
Pf = Final absolute pressure of the deep pressure probes
during short-term testing, mm Hg.
Pfa = Average final absolute pressure of the deep pressure
probes during short-term testing, mm Hg.
Pgf = final gauge pressure of the deep pressure probes, mm
Hg.
Pgi = Initial gauge pressure of the deep pressure probes, mm
Hg.
Pi = Initial absolute pressure of the deep pressure probes
during static testing, mm Hg.
Pia = Average initial absolute pressure of the deep pressure
probes during static testing, mm Hg.
Ps = Final absolute pressure of the deep pressure probes
during long-term testing, mm Hg.
Psa = Average final absolute pressure of the deep pressure
probes during long-term testing, mm Hg.
Qf = Final stabilized flow rate, m\3\/min.
Qi = LFG flow rate measured at orifice meter during the ith
interval, m\3\/min.
Qs = Maximum LFG flow rate at each well determined by short-
term test, m\3\/min.
Qt = NMOC mass emission rate, m\3\/min.
Rm = Maximum radius of influence, m.
Rma = Average maximum radius of influence, m.
Rs = Stabilized radius of influence for an individual well,
m.
Rsa = Average stabilized radius of influence, m.
ti = Age of section i, yr.
tt = Total time of long-term testing, yr.
tvi = Time of the ith interval (usually 8), hr.
V = Void volume of test well, m\3\.
Vr = Volume of refuse affected by the test well, m\3\.
Vt = Total volume of refuse affected by the long-term
testing, m\3\.
Vv = Total void volume affected by test wells, m\3\.
WD = Well depth, m.
= Refuse density, Mg/m\3\ (Assume 0.64 Mg/m\3\ if data are
unavailable).

12.2 Use the following equation to calculate a weighted average
age of landfill refuse.
[GRAPHIC] [TIFF OMITTED] TR17OC00.071

12.3 Use the following equation to determine the difference in
N2 concentrations (ppmv) at the well head and outlet
location.
[GRAPHIC] [TIFF OMITTED] TR17OC00.072

12.4 Use the following equation to convert the gauge pressure
(Pg) of each initial deep pressure probe to absolute
pressure (Pi).
[GRAPHIC] [TIFF OMITTED] TR17OC00.073

12.5 Use the following equation to convert the gauge pressures of
the deep probes to absolute pressures for each 8-hr reading at
Qs.
[GRAPHIC] [TIFF OMITTED] TR17OC00.074

12.6 Use the following equation to calculate the depth
(Dst) affected by the extraction well during the short-term
test.
[GRAPHIC] [TIFF OMITTED] TR17OC00.075

12.7 Use the following equation to calculate the void volume for
the extraction well (V).
[GRAPHIC] [TIFF OMITTED] TR17OC00.076

12.8 Use the following equation to calculate Vt, the
total volume of LFG extracted from the wells.
[GRAPHIC] [TIFF OMITTED] TR17OC00.077

12.9 Use the following equation to calculate the depth affected by
the test well. If using cluster wells, use the average depth of the
wells for WD. If the value of D is greater than the depth of the
landfill, set D equal to the landfill depth.
[GRAPHIC] [TIFF OMITTED] TR17OC00.078

12.10 Use the following equation to calculate the volume of refuse
affected by the test well.
[GRAPHIC] [TIFF OMITTED] TR17OC00.079

12.11 Use the following equation to calculate the mass affected by
the test well.
[GRAPHIC] [TIFF OMITTED] TR17OC00.080

12.12 Modify Lo to account for the nondecomposable
refuse in the landfill.
[GRAPHIC] [TIFF OMITTED] TR17OC00.081

12.13 In the following equation, solve for k (landfill gas
generation constant) by iteration. A suggested procedure is to select a
value for k, calculate the left side of the equation, and if not equal
to zero, select another value for k. Continue this process until the
left hand side of the equation equals zero, 0.001.

[[Page 61813]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.082

12.14 Use the following equation to determine landfill NMOC mass
emission rate if the yearly acceptance rate of refuse has been
consistent (10 percent) over the life of the landfill.
[GRAPHIC] [TIFF OMITTED] TR17OC00.083

12.15 Use the following equation to determine landfill NMOC mass
emission rate if the acceptance rate has not been consistent over the
life of the landfill.
[GRAPHIC] [TIFF OMITTED] TR17OC00.084

13.0 Method Performance. [Reserved]

14.0 Pollution Prevention. [Reserved]

15.0 Waste Management. [Reserved]

16.0 References

1. Same as Method 2, Appendix A, 40 CFR Part 60.
2. Emcon Associates, Methane Generation and Recovery from
Landfills. Ann Arbor Science, 1982.
3. The Johns Hopkins University, Brown Station Road Landfill Gas
Resource Assessment, Volume 1: Field Testing and Gas Recovery
Projections. Laurel, Maryland: October 1982.
4. Mandeville and Associates, Procedure Manual for Landfill
Gases Emission Testing.
5. Letter and attachments from Briggum, S., Waste Management of
North America, to Thorneloe, S., EPA. Response to July 28, 1988
request for additional information. August 18, 1988.
6. Letter and attachments from Briggum, S., Waste Management of
North America, to Wyatt, S., EPA. Response to December 7, 1988
request for additional information. January 16, 1989.
BILLING CODE 6560-50-C

[[Page 61814]]

17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.085

[[Page 61815]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.086

[[Page 61816]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.087

[[Page 61817]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.088

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[GRAPHIC] [TIFF OMITTED] TR17OC00.089

BILLING CODE 6560-50-C

[[Page 61819]]

* * * * *

Method 3--Gas Analysis for the Determination of Dry Molecular
Weight

1.0 Scope and Application

1.1 Analytes.

------------------------------------------------------------------------
Analytes CAS No. Sensitivity
------------------------------------------------------------------------
Oxygen (O2)....................... 7782-44-7 2,000 ppmv.
Nitrogen (N2)..................... 7727-37-9 N/A.
Carbon dioxide (CO2).............. 124-38-9 2,000 ppmv.
Carbon monoxide (CO).............. 630-08-0 N/A.
------------------------------------------------------------------------

1.2 Applicability. This method is applicable for the determination
of CO2 and O2 concentrations and dry molecular
weight of a sample from an effluent gas stream of a fossil-fuel
combustion process or other process.
1.3 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 grab sampling method using an Orsat analyzer to
analyze the individual grab sample obtained at each point; (2) a method
for measuring either CO2 or O2 and using
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. 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.
1.4 Data Quality Objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.

2.0 Summary of Method

2.1 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 and percent O2. For dry
molecular weight determination, either an Orsat or a Fyrite analyzer
may be used for the analysis.

3.0 Definitions [Reserved]

4.0 Interferences

4.1 Several compounds can interfere, to varying degrees, with the
results of Orsat or Fyrite analyses. Compounds that interfere with
CO2 concentration measurement include acid gases (e.g.,
sulfur dioxide, hydrogen chloride); compounds that interfere with
O2 concentration measurement include unsaturated
hydrocarbons (e.g., acetone, acetylene), nitrous oxide, and ammonia.
Ammonia reacts chemically with the O2 absorbing solution,
and when present in the effluent gas stream must be removed before
analysis.

5.0 Safety

5.1 Disclaimer. This method may involve hazardous materials,
operations, and equipment. This test method may not address all of the
safety problems associated with its use. It is the responsibility of
the user of this test method to establish appropriate safety and health
practices and determine the applicability of regulatory limitations
prior to performing this test method.
5.2 Corrosive Reagents.
5.2.1 A typical Orsat analyzer requires four reagents: a gas-
confining solution, CO2 absorbent, O2 absorbent,
and CO absorbent. These reagents may contain potassium hydroxide,
sodium hydroxide, cuprous chloride, cuprous sulfate, alkaline
pyrogallic acid, and/or chromous chloride. Follow manufacturer's
operating instructions and observe all warning labels for reagent use.
5.2.2 A typical Fyrite analyzer contains zinc chloride,
hydrochloric acid, and either potassium hydroxide or chromous chloride.
Follow manufacturer's operating instructions and observe all warning
labels for reagent use.

6.0 Equipment and Supplies

Note: 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.

6.1 Grab Sampling (See Figure 3-1).
6.1.1 Probe. Stainless steel or borosilicate glass tubing equipped
with an in-stack or out-of-stack filter to remove particulate matter (a
plug of glass wool is satisfactory for this purpose). Any other
materials, resistant to temperature at sampling conditions and inert to
all components of the gas stream, may be used for the probe. Examples
of such materials may include aluminum, copper, quartz glass, and
Teflon.
6.1.2 Pump. A one-way squeeze bulb, or equivalent, to transport
the gas sample to the analyzer.
6.2 Integrated Sampling (Figure 3-2).
6.2.1 Probe. Same as in Section 6.1.1.
6.2.2 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.
6.2.3 Valve. A needle valve, to adjust sample gas flow rate.
6.2.4 Pump. A leak-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 rate meter.
6.2.5 Rate Meter. A rotameter, or equivalent, capable of measuring
flow rate to 2 percent of the selected flow rate. A flow
rate range of 500 to 1000 ml/min is suggested.
6.2.6 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 duration of the test run. A capacity in the range of 55 to 90
liters (1.9 to 3.2 ft3) 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

[[Page 61820]]

5 to 10 cm (2 to 4 in.) H2O and allow to stand overnight. A
deflated bag indicates a leak.
6.2.7 Pressure Gauge. A water-filled U-tube manometer, or
equivalent, of about 30 cm (12 in.), for the flexible bag leak-check.
6.2.8 Vacuum Gauge. A mercury manometer, or equivalent, of at
least 760 mm (30 in.) Hg, for the sampling train leak-check.
6.3 Analysis. An Orsat or Fyrite type combustion gas analyzer.

7.0 Reagents and Standards

7.1 Reagents. As specified by the Orsat or Fyrite-type combustion
analyzer manufacturer.
7.2 Standards. Two standard gas mixtures, traceable to National
Institute of Standards and Technology (NIST) standards, to be used in
auditing the accuracy of the analyzer and the analyzer operator
technique:
7.2.1. Gas cylinder containing 2 to 4 percent O2 and 14
to 18 percent CO2.
7.2.2. Gas cylinder containing 2 to 4 percent CO2 and
about 15 percent O2.

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Single Point, Grab Sampling Procedure.
8.1.1 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
1.0 m (3.3 ft), unless otherwise specified by the Administrator.
8.1.2 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 11.5; however, the leak-check is optional.
8.1.3 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, and
immediately analyze it for percent CO2 and percent
O2 according to Section 11.2.
8.2 Single-Point, Integrated Sampling Procedure.
8.2.1 The sampling point in the duct shall be located as specified
in Section 8.1.1.
8.2.2 Leak-check (optional) the flexible bag as in Section 6.2.6.
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.
8.2.3 Sample Collection. Sample at a constant rate (10
percent). 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 28 liters (1.0 ft3) of
sample gas is recommended; however, smaller volumes may be collected,
if desired.
8.2.4 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
according to Section 11.3.

Note: When using an Orsat analyzer, periodic Fyrite readings may
be taken to verify/confirm the results obtained from the Orsat.

8.3 Multi-Point, Integrated Sampling Procedure.
8.3.1 Unless otherwise specified in an applicable regulation, or
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.
8.3.2 Follow the procedures outlined in Sections 8.2.2 through
8.2.4, 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.

9.0 Quality Control

------------------------------------------------------------------------
Quality control
Section measure Effect
------------------------------------------------------------------------
8.2........................... Use of Fyrite to Ensures the accurate
confirm Orsat measurement of CO2
results. and O2.
10.1.......................... Periodic audit of Ensures that the
analyzer and analyzer is
operator operating properly
technique. and that the
operator performs
the sampling
procedure correctly
and accurately.
11.3.......................... Replicable Minimizes
analyses of experimental error.
integrated
samples.
------------------------------------------------------------------------

10.0 Calibration and Standardization

10.1 Analyzer. The analyzer and analyzer operator's technique
should be audited periodically as follows: take a sample from a
manifold containing a known mixture of CO2 and
O2, and analyze according to the procedure in Section 11.3.
Repeat this procedure until the measured concentration of three
consecutive samples agrees with the stated value 0.5
percent. If necessary, take corrective action, as specified in the
analyzer users manual.
10.2 Rotameter. The rotameter need not be calibrated, but should
be cleaned and maintained according to the manufacturer's instruction.

11.0 Analytical Procedure

11.1 Maintenance. The Orsat or Fyrite-type analyzer should be
maintained and operated according to the manufacturers specifications.
11.2 Grab Sample Analysis. Use either an Orsat analyzer or a
Fyrite-type combustion gas analyzer to measure O2 and
CO2 concentration for dry molecular weight determination,
using procedures as specified in the analyzer user's manual. If an
Orsat analyzer is used, it is recommended that the Orsat leak-check,
described in Section 11.5, be performed before this determination;
however, the check is optional. Calculate the dry molecular weight as
indicated in Section 12.0. 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).
11.3 Integrated Sample Analysis. Use either an Orsat analyzer or a
Fyrite-type combustion gas analyzer to measure O2 and
CO2 concentration for dry molecular weight determination,
using procedures as specified in the analyzer user's manual. If an
Orsat analyzer is used, it is recommended that the Orsat leak-check,
described in Section 11.5, be performed before this determination;
however, the check is

[[Page 61821]]

optional. Calculate the dry molecular weight as indicated in Section
12.0. 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).
11.4 Standardization. A periodic check of the reagents and of
operator technique should be conducted at least once every three series
of test runs as outlined in Section 10.1.
11.5 Leak-Check Procedure for Orsat Analyzer. 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:
11.5.1 Bring the liquid level in each pipette up to the reference
mark on the capillary tubing, and then close the pipette stopcock.
11.5.2 Raise the leveling bulb sufficiently to bring the confining
liquid meniscus onto the graduated portion of the burette, and then
close the manifold stopcock.
11.5.3 Record the meniscus position.
11.5.4 Observe the meniscus in the burette and the liquid level in
the pipette for movement over the next 4 minutes.
11.5.5 For the Orsat analyzer to pass the leak-check, two
conditions must be met:
11.5.5.1 The liquid level in each pipette must not fall below the
bottom of the capillary tubing during this 4-minute interval.
11.5.5.2 The meniscus in the burette must not change by more than
0.2 ml during this 4-minute interval.
11.5.6 If the analyzer 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 any leaking
stopcocks. Replace leaking rubber connections. After the analyzer is
reassembled, repeat the leak-check procedure.

12.0 Calculations and Data Analysis

12.1 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.
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.
12.2 Nitrogen, Carbon Monoxide Concentration. Determine the
percentage of the gas that is N2 and CO by subtracting the
sum of the percent CO2 and percent O2 from 100
percent.
12.3 Dry Molecular Weight. Use Equation 3-1 to calculate the dry
molecular weight of the stack gas.
[GRAPHIC] [TIFF OMITTED] TR17OC00.090

Note: The above Equation 3-1 does not consider the effect on
calculated dry molecular weight of argon in the effluent gas. The
concentration of argon, with a molecular weight of 39.9, in ambient
air is about 0.9 percent. A negative error of approximately 0.4
percent is introduced. The tester may choose to include argon in the
analysis using procedures subject to approval of the Administrator.

13.0 Method Performance [Reserved]

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 References

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.
25:291-297. 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.

[[Page 61822]]

17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.091

[[Page 61823]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.092

----------------------------------------------------------------------------------------------------------------
Time Traverse point Q (liter/min) % Deviation a
----------------------------------------------------------------------------------------------------------------

----------------------------------------------------------------------------------------------------------------

Figure 3-3. Sampling Rate Data

[[Page 61824]]

* * * * *

Method 3B--Gas Analysis for the Determination of Emission Rate
Correction Factor or Excess Air

1.0 Scope and Application

1.1 Analytes.

------------------------------------------------------------------------
Analyte CAS No. Sensitivity
------------------------------------------------------------------------
Oxygen (O2)....................... 7782-44-7 2,000 ppmv.
Carbon Dioxide (CO2).............. 124-38-9 2,000 ppmv.
Carbon Monoxide (CO).............. 630-08-0 N/A.
------------------------------------------------------------------------

1.2 Applicability. This method is applicable for the determination
of O2, CO2, and CO concentrations in the effluent
from fossil-fuel combustion processes for use in excess air or emission
rate correction factor calculations. Where compounds other than
CO2, O2, CO, and nitrogen (N2) are
present in concentrations sufficient to affect the results, the
calculation procedures presented in this method must be modified,
subject to the approval of the Administrator.
1.3 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.
1.4 Data Quality Objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.

2.0 Summary of Method

2.1 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 using an Orsat combustion gas analyzer.

3.0 Definitions [Reserved]

4.0 Interferences

4.1 Several compounds can interfere, to varying degrees, with the
results of Orsat analyses. Compounds that interfere with CO2
concentration measurement include acid gases (e.g., sulfur dioxide,
hydrogen chloride); compounds that interfere with O2
concentration measurement include unsaturated hydrocarbons (e.g.,
acetone, acetylene), nitrous oxide, and ammonia. Ammonia reacts
chemically with the O2 absorbing solution, and when present
in the effluent gas stream must be removed before analysis.

5.0 Safety

5.1 Disclaimer. This method may involve hazardous materials,
operations, and equipment. This test method may not address all of the
safety problems associated with its use. It is the responsibility of
the user of this test method to establish appropriate safety and health
practices and determine the applicability of regulatory limitations
prior to performing this test method.
5.2 Corrosive Reagents. A typical Orsat analyzer requires four
reagents: a gas-confining solution, CO2 absorbent,
O2 absorbent, and CO absorbent. These reagents may contain
potassium hydroxide, sodium hydroxide, cuprous chloride, cuprous
sulfate, alkaline pyrogallic acid, and/or chromous chloride. Follow
manufacturer's operating instructions and observe all warning labels
for reagent use.

6.0 Equipment and Supplies

6.1 Grab Sampling and Integrated Sampling. Same as in Sections 6.1
and 6.2, respectively for Method 3.
6.2 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.

7.0 Reagents and Standards

7.1 Reagents. Same as in Method 3, Section 7.1.
7.2 Standards. Same as in Method 3, Section 7.2.

8.0 Sample Collection, Preservation, Storage, and Transport

Note: 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 Administrator. 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
also be used for calculating the dry molecular weight (see Method
3).

8.1 Single-Point, Grab Sampling and Analytical Procedure.

8.1.1 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
1.0 m (3.3 ft), unless otherwise specified by the Administrator.
8.1.2 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 11.5
of Method 3. This leak-check is mandatory.
8.1.3 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 for percent CO2 or

[[Page 61825]]

percent O2, as outlined in Section 11.2. For excess air
determination, immediately analyze the sample for percent
CO2, O2, and CO, as outlined in Section 11.2, and
calculate excess air as outlined in Section 12.2.
8.1.4 After the analysis is completed, leak-check (mandatory) the
Orsat analyzer once again, as described in Section 11.5 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.

8.2 Single-Point, Integrated Sampling and Analytical Procedure.

8.2.1 The sampling point in the duct shall be located as specified
in Section 8.1.1.
8.2.2 Leak-check (mandatory) the flexible bag as in Section 6.2.6
of Method 3. Set up the equipment as shown in Figure 3-2 of Method 3.
Just before sampling, leak-check (mandatory) the train 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.
8.2.3 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 28 liters (1.0 ft\3\) of sample gas.
Smaller volumes may be collected, subject to approval of the
Administrator.
8.2.4 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 Section
11.2).

8.3 Multi-Point, Integrated Sampling and Analytical Procedure.

8.3.1 Unless otherwise specified in an applicable regulation, or
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.
8.3.2 Follow the procedures outlined in Sections 8.2.2 through
8.2.4, 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.

9.0 Quality Control

9.1 Data Validation Using Fuel Factor. 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 data validation
procedure of Section 12.3 is suggested.

Note: Since this method for validating the 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 fuel factor check
minimally useful.

10.0 Calibration and Standardization

10.1 Analyzer. The analyzer and analyzer operator technique should
be audited periodically as follows: take a sample from a manifold
containing a known mixture of CO2 and O2, and
analyze according to the procedure in Section 11.3. Repeat this
procedure until the measured concentration of three consecutive samples
agrees with the stated value 0.5 percent. If necessary,
take corrective action, as specified in the analyzer users manual.
10.2 Rotameter. The rotameter need not be calibrated, but should
be cleaned and maintained according to the manufacturer's instruction.

11.0 Analytical Procedure

11.1 Maintenance. The Orsat analyzer should be maintained
according to the manufacturers specifications.
11.2 Grab Sample Analysis. 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.) Although in most
cases, only CO2 or O2 concentration is required,
it is recommended that both CO2 and O2 be
measured, and that the procedure in Section 12.3 be used to validate
the analytical data.

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.

11.3 Integrated Sample Analysis. The Orsat analyzer must be leak-
checked (see Section 11.5 of Method 3) before the analysis. If excess
air is desired, proceed as follows: (1) within 4 hours after the sample
is taken, analyze it (as in Sections 11.3.1 through 11.3.3) 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 12.2.
11.3.1 To ensure complete absorption of the CO2,
O2, or if applicable, CO, follow the procedure described in
Section 11.2.

Note: Although in most instances only CO2 or
O2 is required, it is recommended that both
CO2 and O2 be measured, and that the
procedures in Section 12.3 be used to validate the analytical data.

11.3.2 Repeat the analysis until the following criteria are met:
11.3.2.1 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.
11.3.2.2 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.
11.3.2.3 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

[[Page 61826]]

report the results to the nearest 0.1 percent.
11.3.3 After the analysis is completed, leak-check (mandatory) the
Orsat analyzer once again, as described in Section 11.5 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.
11.4 Standardization. A periodic check of the reagents and of
operator technique should be conducted at least once every three series
of test runs as indicated in Section 10.1.

12.0 Calculations and Data Analysis

12.1 Nomenclature. Same as Section 12.1 of Method 3 with the
addition of the following:
%EA = Percent excess air.
0.264 = Ratio of O2 to N2 in air, v/v.

12.2 Percent Excess Air. Determine the percentage of the gas that
is N2 by subtracting the sum of the percent CO2,
percent CO, and percent O2 from 100 percent. Calculate the
percent excess air (if applicable) by substituting the appropriate
values of percent O2, CO, and N2 into Equation
3B-1.
[GRAPHIC] [TIFF OMITTED] TR17OC00.093

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.

12.3 Data Validation When Both CO2 and O2
Are Measured.
12.3.1 Fuel Factor, Fo. Calculate the fuel factor (if
applicable) using Equation 3B-2:
[GRAPHIC] [TIFF OMITTED] TR17OC00.094

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 using Equations 3B-3 and
3B-4 before performing the calculation for Fo:
[GRAPHIC] [TIFF OMITTED] TR17OC00.095

[GRAPHIC] [TIFF OMITTED] TR17OC00.096

Where:
%CO = Percent CO by volume, dry basis.

12.3.2 Compare the calculated Fo factor with the
expected Fo values. Table 3B-1 in Section 17.0 may be used
in establishing acceptable ranges for the expected Fo 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, Section 12.2) according to the procedure in
Method 19, Sections 12.2 and 12.3. Then calculate the Fo
factor according to Equation 3B-5.
[GRAPHIC] [TIFF OMITTED] TR17OC00.097

12.3.3 Calculated Fo 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 Fo 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.

13.0 Method Performance. [Reserved]

14.0 Pollution Prevention. [Reserved]

15.0 Waste Management. [Reserved]

16.0 References

Same as Method 3, Section 16.0.

17.0 Tables, Diagrams, Flowcharts, and Validation Data

Table 3B-1.--Fo Factors for Selected Fuels
------------------------------------------------------------------------
Fuel type Fo range
------------------------------------------------------------------------
Coal:
Anthracite and lignite.............................. 1.016-1.130
Bituminous.......................................... 1.083-1.230
Oil:
Distillate.......................................... 1.260-1.413
Residual............................................ 1.210-1.370
Gas:
Natural............................................. 1.600-1.836
Propane............................................. 1.434-1.586
Butane.............................................. 1.405-1.553
Wood.................................................... 1.000-1.120
Wood bark............................................... 1.003-1.130
------------------------------------------------------------------------

* * * * *

Method 4--Determination of Moisture Content in Stack Gases

Note: This method does not include all the specifications (e.g.,
equipment and supplies) and procedures (e.g., sampling) essential to
its performance. Some material is incorporated by reference from
other methods in this part. Therefore, to obtain reliable results,
persons using this method should have a thorough knowledge of at
least the following additional test methods: Method 1, Method 5, and
Method 6.

1.0 Scope and Application

1.1 Analytes.

------------------------------------------------------------------------
Analyte CAS No. Sensitivity
------------------------------------------------------------------------
Water vapor (H2O)................. 7732-18-5 N/A
------------------------------------------------------------------------

1.2 Applicability. This method is applicable for the determination
of the moisture content of stack gas.
1.3 Data Quality Objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.

[[Page 61827]]

2.0 Summary of Method

2.1 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.
2.2 The method contains two possible procedures: a reference
method and an approximation method.
2.2.1 The reference method is used for accurate determinations of
moisture content (such as are needed to calculate emission data). The
approximation method, 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.
2.2.2 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, to be capable of yielding results within one
percent H2O of the reference method.

3.0 Definitions [Reserved]

4.0 Interferences

4.1 The moisture content of saturated gas streams or streams that
contain water droplets, as measured by the reference method, may be
positively biased. 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 deg.C (2 deg.F)] to the reference method
probe. Measure the stack gas temperature at each traverse point (see
Section 8.1.1.1) during the reference method traverse, and calculate
the average stack gas temperature. Next, determine the moisture
percentage, either by: (1) Using a psychrometric chart and making
appropriate corrections if the stack pressure is different from that of
the chart, or (2) using saturation vapor pressure tables. In cases
where the psychrometric 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.

5.0 Safety

6.0 Equipment and Supplies

6.1 Reference Method. A schematic of the sampling train used in
this reference method is shown in Figure
4-1.
6.1.1 Probe. Stainless steel or glass tubing, sufficiently heated
to prevent water condensation, and equipped with a filter, either in-
stack (e.g., a plug of glass wool inserted into the end of the probe)
or heated out-of-stack (e.g., as described in Method 5), to remove
particulate matter. When stack conditions permit, other metals or
plastic tubing may be used for the probe, subject to the approval of
the Administrator.
6.1.2 Condenser. Same as Method 5, Section 6.1.1.8.
6.1.3 Cooling System. An ice bath container, crushed ice, and
water (or equivalent), to aid in condensing moisture.
6.1.4 Metering System. Same as in Method 5, Section 6.1.1.9,
except do not use sampling systems designed for flow rates higher than
0.0283 m\3\/min (1.0 cfm). Other metering systems, capable of
maintaining a constant sampling rate to within 10 percent and
determining sample gas volume to within 2 percent, may be used, subject
to the approval of the Administrator.
6.1.5 Barometer and Graduated Cylinder and/or Balance. Same as
Method 5, Sections 6.1.2 and 6.2.5, respectively.
6.2. Approximation Method. A schematic of the sampling train used
in this approximation method is shown in Figure 4-2.
6.2.1 Probe. Same as Section 6.1.1.
6.2.2 Condenser. Two midget impingers, each with 30-ml capacity,
or equivalent.
6.2.3 Cooling System. Ice bath container, crushed ice, and water,
to aid in condensing moisture in impingers.
6.2.4 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.
6.2.5 Valve. Needle valve, to regulate the sample gas flow rate.
6.2.6 Pump. Leak-free, diaphragm type, or equivalent, to pull the
gas sample through the train.
6.2.7 Volume Meter. Dry gas meter, sufficiently accurate to
measure the sample volume to within 2 percent, and calibrated over the
range of flow rates and conditions actually encountered during
sampling.
6.2.8 Rate Meter. Rotameter, or equivalent, to measure the flow
range from 0 to 3 liters/min (0 to 0.11 cfm).
6.2.9 Graduated Cylinder. 25-ml.
6.2.10 Barometer. Same as Method 5, Section 6.1.2.
6.2.11 Vacuum Gauge. At least 760-mm (30-in.) Hg gauge, to be used
for the sampling leak check.

7.0 Reagents and Standards [Reserved]

8.0 Sample Collection, Preservation, Transport, and Storage

8.1 Reference Method. The following procedure is intended for a
condenser system (such as the impinger system described in Section
6.1.1.8 of Method 5) incorporating volumetric analysis to measure the
condensed moisture, and silica gel and gravimetric analysis to measure
the moisture leaving the condenser.
8.1.1 Preliminary Determinations.
8.1.1.1 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.
8.1.1.2 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 m\3\/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.

[[Page 61828]]

8.1.2 Preparation of Sampling Train.
8.1.2.1 Place known volumes of water in the first two impingers;
alternatively, transfer water into the first two impingers and record
the weight of each impinger (plus water) to the nearest 0.5 g. 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.
8.1.2.2 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 approximately 120 deg.C (248 deg.F), to prevent water
condensation ahead of the condenser. Allow time for the temperatures to
stabilize. Place crushed ice and water in the ice bath container.
8.1.3 Leak Check Procedures. It is recommended, but not required,
that the volume metering system and sampling train be leak-checked as
follows:
8.1.3.1 Metering System. Same as Method 5, Section 8.4.1.
8.1.3.2 Sampling Train. 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 m\3\/min (0.020 cfm), whichever is less, is
unacceptable. Following the leak check, reconnect the probe to the
sampling train.
8.1.4 Sampling Train Operation. 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 a data
sheet similar to that shown in Figure 4-3. 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.

Note: When Method 4 is used concurrently with an isokinetic
method (e.g., Method 5) the sampling rate should be maintained at
isokinetic conditions rather than 10 percent of constant rate.

8.1.4.1 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 than 20 deg.C (68 deg.F) at the
silica gel outlet.
8.1.4.2 After collecting the sample, disconnect the probe from the
first impinger (or from the filter holder), and conduct a leak check
(mandatory) of the sampling train as described in Section 8.1.3.2.
Record the leak rate. If the leakage rate exceeds the allowable rate,
either reject the test results or correct the sample volume as in
Section 12.3 of Method 5.
8.2 Approximation Method.

Note: The approximation method described below is presented only
as a suggested method (see Section 2.0).

8.2.1 Place exactly 5 ml 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 (10 in.) Hg. Note the time rate of change of the dry gas
meter dial; alternatively, a rotameter (0 to 40 ml/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: Release the probe inlet plug slowly before turning off the
pump.

8.2.2 Connect the probe, insert it into the stack, and sample at a
constant rate of 2 liters/min (0.071 cfm). Continue sampling until the
dry gas meter registers about 30 liters (1.1 ft\3\) or until visible
liquid droplets are carried over from the first impinger to the second.
Record temperature, pressure, and dry gas meter readings as indicated
by Figure 4-4.

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures.

------------------------------------------------------------------------
Quality control
Section measure Effect
------------------------------------------------------------------------
Section 8.1.1.4............... Leak rate of the Ensures the accuracy
sampling system of the volume of gas
cannot exceed sampled. (Reference
four percent of Method)
the average
sampling rate or
0.00057 m\3\/min
(0.20 cfm).
Section 8.2.1................. Leak rate of the Ensures the accuracy
sampling system of the volume of gas
cannot exceed sampled.
two percent of (Approximation
the average Method)
sampling rate.
------------------------------------------------------------------------

9.2 Volume Metering System Checks. Same as Method 5, Section 9.2.

10.0 Calibration and Standardization

Note: Maintain a laboratory log of all calibrations.

10.1 Reference Method. Calibrate the metering system, temperature
sensors, and barometer according to Method 5, Sections 10.3, 10.5, and
10.6, respectively.
10.2 Approximation Method. Calibrate the metering system and the
barometer according to Method 6, Section 10.1 and Method 5, Section
10.6, respectively.

11.0 Analytical Procedure

11.1 Reference Method. Measure the volume of the moisture
condensed in each of the impingers to the nearest ml. Alternatively, if
the impingers were weighed prior to sampling, weigh the impingers after
sampling and record the difference in weight to the nearest 0.5 g.
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 4-5), and calculate the moisture content, as
described in Section 12.0.
11.2 Approximation Method. Combine the contents of the two
impingers, and measure the volume to the nearest 0.5 ml.

12.0 Data Analysis and Calculations

Carry out the following calculations, retaining at least one extra
significant figure beyond that of the acquired data. Round off figures
after final calculation.
12.1 Reference Method.
12.1.1 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)(m\3\)/(g-mole)( deg.K) for
metric units and 21.85 (in. Hg)(ft\3\)/(lb-mole)( deg.R) for English
units.
Tm = Absolute temperature at meter, deg.K ( deg.R).
Tstd = Standard absolute temperature, 293 deg.K (528
deg.R).

[[Page 61829]]

Vf = Final volume of condenser water, ml.
Vi = Initial volume, if any, of condenser water, ml.
Vm = Dry gas volume measured by dry gas meter, 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).
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.
Vm = Incremental dry gas volume measured by dry gas
meter at each traverse point, dcm (dcf).
w = Density of water, 0.9982 g/ml (0.002201 lb/ml).

12.1.2 Volume of Water Vapor Condensed.
[GRAPHIC] [TIFF OMITTED] TR17OC00.098

Where:

K1 = 0.001333 m\3\/ml for metric units,
= 0.04706 ft\3\/ml for English units.

12.1.3 Volume of Water Collected in Silica Gel.
[GRAPHIC] [TIFF OMITTED] TR17OC00.099

Where:

K2 = 1.0 g/g for metric units,
= 453.6 g/lb for English units.
K3 = 0.001335 m\3\/g for metric units,
= 0.04715 ft\3\/g for English units.

12.1.4 Sample Gas Volume.
[GRAPHIC] [TIFF OMITTED] TR17OC00.100

Where:

K4 = 0.3855 deg.K/mm Hg for metric units,
= 17.64 deg.R/in. Hg for English units.

Note: If the post-test leak rate (Section 8.1.4.2) exceeds the
allowable rate, correct the value of Vm in Equation 4-3, as
described in Section 12.3 of Method 5.

12.1.5 Moisture Content.
[GRAPHIC] [TIFF OMITTED] TR17OC00.101

12.1.6 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.
12.1.7 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
4.1), and another based upon the results of the impinger analysis. The
lower of these two values of Bws shall be considered
correct.
12.2 Approximation Method. The approximation 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.
12.2.1 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, mm Hg (in. Hg).
Pstd = Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
R = Ideal gas constant, 0.06236 [(mm Hg)(m\3\)]/[(g-mole)(K)] for
metric units and 21.85 [(in. Hg)(ft\3\)]/[(lb-mole)( deg.R)] for
English units.
Tm = Absolute temperature at meter, deg.K ( deg.R).
Tstd = Standard absolute temperature, 293 deg.K (528
deg.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).
Y = Dry gas meter calibration factor.
w = Density of water, 0.09982 g/ml (0.002201 lb/
ml).

12.2.2 Volume of Water Vapor Collected.
[GRAPHIC] [TIFF OMITTED] TR17OC00.102

Where:

K5 = 0.001333 m\3\/ml for metric units,
= 0.04706 ft\3\/ml for English units.

12.2.3 Sample Gas Volume.
[GRAPHIC] [TIFF OMITTED] TR17OC00.103

Where:

K6 = 0.3855 deg.K/mm Hg for metric units,
= 17.64 deg.R/in. Hg for English units.

12.2.4 Approximate Moisture Content.
[GRAPHIC] [TIFF OMITTED] TR17OC00.104

13.0 Method Performance [Reserved]

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 Alternative Procedures

The procedure described in Method 5 for determining moisture
content is acceptable as a reference method.

17.0 References

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.

[[Page 61830]]

18.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.105

[[Page 61831]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.106

[[Page 61832]]

Plant-----------------------------------------------------------------
Location--------------------------------------------------------------
Operator--------------------------------------------------------------
Date------------------------------------------------------------------
Run No.---------------------------------------------------------------
Ambient temperature---------------------------------------------------
Barometric pressure---------------------------------------------------
Probe Length----------------------------------------------------------

------------------------------------------------------------------------

-------------------------------------------------------------------------

------------------------------------------------------------------------

SCHEMATIC OF STACK CROSS SECTION

--------------------------------------------------------------------------------------------------------------------------------------------------------
Gas sample temperature Temperature
Pressure Meter at dry gas meter of gas
Sampling Stack differential reading gas -------------------------- leaving
time temperature across sample Vm condenser
Traverse Pt. No. (), deg.C ( orifice volume m\3\ Inlet Tmin Outlet or last
min deg.F) meter out impinger
D>H mm (ft\3\) deg.F) deg.C ( deg.C (
(in.) H2O deg.F) deg.F)
--------------------------------------------------------------------------------------------------------------------------------------------------------

--------------------------------------------------------------------------------------------------------------------------------------------------------

--------------------------------------------------------------------------------------------------------------------------------------------------------
Average
--------------------------------------------------------------------------------------------------------------------------------------------------------

Location--------------------------------------------------------------
Test------------------------------------------------------------------
Date------------------------------------------------------------------
Operator--------------------------------------------------------------
Barometric pressure---------------------------------------------------
Comments:-------------------------------------------------------------
----------------------------------------------------------------------
Figure 4-3. Moisture Determination--Reference Method

----------------------------------------------------------------------------------------------------------------
Gas Volume through Rate meter setting m3/ Meter temperature
Clock time meter, (Vm), m3 (ft3) min (ft3/min) deg.C ( deg.F)
----------------------------------------------------------------------------------------------------------------

----------------------------------------------------------------------------------------------------------------

Figure 4-4. Example Moisture Determination Field Data Sheet--
Approximation Method

------------------------------------------------------------------------
Impinger volume, Silica gel weight,
ml g
------------------------------------------------------------------------
Final
Initial
Difference
------------------------------------------------------------------------

Figure 4-5. Analytical Data--Reference Method

Method 5--Determination of Particulate Matter Emissions From
Stationary Sources

Note: This method does not include all of the specifications
(e.g., equipment and supplies) and procedures (e.g., sampling and
analytical) essential to its performance. Some material is
incorporated by reference from other methods in this part.
Therefore, to obtain reliable results, persons using this method
should have a thorough knowledge of at least the following
additional test methods: Method 1, Method 2, Method 3.

[[Page 61833]]

1.0 Scope and Application

1.1 Analyte. Particulate matter (PM). No CAS number assigned.
1.2 Applicability. This method is applicable for the determination
of PM emissions from stationary sources.
1.3 Data Quality Objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.

2.0 Summary of Method

Particulate matter is withdrawn isokinetically from the source and
collected on a glass fiber filter maintained at a temperature of 120
14 deg.C (248 25 deg.F) or such other
temperature as specified by an applicable subpart of the standards or
approved by the Administrator for a particular application. The PM
mass, which includes any material that condenses at or above the
filtration temperature, is determined gravimetrically after the removal
of uncombined water.

3.0 Definitions [Reserved]

4.0 Interferences [Reserved]

5.0 Safety

6.0 Equipment and Supplies

6.1 Sample Collection. The following items are required for sample
collection:
6.1.1 Sampling Train. A schematic of the sampling train used in
this method is shown in Figure 5-1 in Section 18.0. Complete
construction details are given in APTD-0581 (Reference 2 in Section
17.0); 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.

Note: The operating and maintenance procedures for the sampling
train are described in APTD-0576 (Reference 3 in Section 17.0).
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.

6.1.1.1 Probe Nozzle. Stainless steel (316) or glass with a sharp,
tapered leading edge. The angle of taper shall be 30 deg.,
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. Typical nozzle sizes range from 0.32 to 1.27 cm
(\1/8\ to \1/2\ in) inside diameter (ID) in increments of 0.16 cm (\1/
16\ in). Larger nozzles sizes are also available if higher volume
sampling trains are used. Each nozzle shall be calibrated, according to
the procedures outlined in Section 10.1.
6.1.1.2 Probe Liner. Borosilicate or quartz glass tubing with a
heating system capable of maintaining a probe gas temperature during
sampling of 120 14 deg.C (248 25 deg.F), or
such other temperature as specified by an applicable subpart of the
standards or as approved by the Administrator for a particular
application. 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 deg.C (900 deg.F);
quartz glass liners shall be used for temperatures between 480 and 900
deg.C (900 and 1,650 deg.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 glass is 820 deg.C (1500 deg.F), and for quartz glass it
is 1500 deg.C (2700 deg.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 or
other corrosion resistant metals) made of seamless tubing may be used,
subject to the approval of the Administrator.
6.1.1.3 Pitot Tube. Type S, as described in Section 6.1 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 2-7) during sampling. The Type S
pitot tube assembly shall have a known coefficient, determined as
outlined in Section 10.0 of Method 2.
6.1.1.4 Differential Pressure Gauge. Inclined manometer or
equivalent device (two), as described in Section 6.2 of Method 2. One
manometer shall be used for velocity head (p) readings, and
the other, for orifice differential pressure readings.
6.1.1.5 Filter Holder. Borosilicate glass, with a glass frit
filter support and a silicone rubber gasket. Other materials of
construction (e.g., stainless steel, Teflon, 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 holder shall be attached immediately at the outlet of the
probe (or cyclone, if used).
6.1.1.6 Filter Heating System. Any heating system capable of
maintaining a temperature around the filter holder of 120
14 deg.C (248 25 deg.F) during sampling, or
such other temperature as specified by an applicable subpart of the
standards or approved by the Administrator for a particular
application.
6.1.1.7 Temperature Sensor. A temperature sensor capable of
measuring temperature to within 3 deg.C (5.4 deg.F) shall
be installed so that the sensing tip of the temperature sensor is in
direct contact with the sample gas, and the temperature around the
filter holder can be regulated and monitored during sampling.
6.1.1.8 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
noncontaminating fittings. The first, third, and fourth impingers shall
be of 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. 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 8.3.1), the third shall be empty, and the
fourth shall contain a known weight of silica gel, or equivalent
desiccant. A temperature sensor, capable of measuring temperature to
within 1 deg.C (2 deg.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

[[Page 61834]]

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. An acceptable technique involves the measurement of
condensed water either gravimetrically or volumetrically and the
determination of 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 deg.C (68 deg.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 PM 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.

6.1.1.9 Metering System. Vacuum gauge, leak-free pump, temperature
sensors capable of measuring temperature to within 3 deg.C (5.4
deg.F), dry gas meter (DGM) 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 allow
periodic checks of isokinetic rates.
6.1.1.10 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.
6.1.2 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in.).

Note: The barometric pressure reading may be obtained from a
nearby National Weather Service station. In this 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 made at a rate of minus 2.5 mm
Hg (0.1 in.) per 30 m (100 ft) elevation increase or plus 2.5 mm Hg
(0.1 in) per 30 m (100 ft) elevation decrease.

6.1.3 Gas Density Determination Equipment. Temperature sensor and
pressure gauge, as described in Sections 6.3 and 6.4 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 2-4). As a second alternative, if a difference of not
more than 1 percent in the average velocity measurement is to be
introduced, the temperature sensor need not be attached to the probe or
pitot tube. (This alternative is subject to the approval of the
Administrator.)
6.2 Sample Recovery. The following items are required for sample
recovery:
6.2.1 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) constructed 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.
6.2.2 Wash Bottles. Two Glass wash bottles are recommended.
Alternatively, polyethylene wash bottles may be used. It is recommended
that acetone not be stored in polyethylene bottles for longer than a
month.
6.2.3 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.
6.2.4 Petri Dishes. For filter samples; glass or polyethylene,
unless otherwise specified by the Administrator.
6.2.5 Graduated Cylinder and/or Balance. To measure condensed
water to within 1 ml or 0.5 g. Graduated cylinders shall have
subdivisions no greater than 2 ml.
6.2.6 Plastic Storage Containers. Air-tight containers to store
silica gel.
6.2.7 Funnel and Rubber Policeman. To aid in transfer of silica
gel to container; not necessary if silica gel is weighed in the field.
6.2.8 Funnel. Glass or polyethylene, to aid in sample recovery.
6.3 Sample Analysis. The following equipment is required for
sample analysis:
6.3.1 Glass Weighing Dishes.
6.3.2 Desiccator.
6.3.3 Analytical Balance. To measure to within 0.1 mg.
6.3.4 Balance. To measure to within 0.5 g.
6.3.5 Beakers. 250 ml.
6.3.6 Hygrometer. To measure the relative humidity of the
laboratory environment.
6.3.7 Temperature Sensor. To measure the temperature of the
laboratory environment.

7.0 Reagents and Standards

7.1 Sample Collection. The following reagents are required for
sample collection:
7.1.1 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 Method D 2986-71, 78,
or 95a (incorporated by reference--see Sec. 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. Reference 10 in Section 17.0 may be used to select the
appropriate filter.
7.1.2 Silica Gel. Indicating type, 6 to 16 mesh. If previously
used, dry at 175 deg.C (350 deg.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.
7.1.3 Water. When analysis of the material caught in the impingers
is required, deionized distilled water (to conform to ASTM D 1193-77 or
91 Type 3 (incorporated by reference--see Sec. 60.17)) shall be used.
Run blanks prior to field use to eliminate a high blank on test
samples.
7.1.4 Crushed Ice.
7.1.5 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.
7.2 Sample Recovery. Acetone, reagent grade, 0.001
percent residue, in glass bottles, is required. Acetone from metal
containers generally has a high

[[Page 61835]]

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.
7.3 Sample Analysis. The following reagents are required for
sample analysis:
7.3.1 Acetone. Same as in Section 7.2.
7.3.2 Desiccant. Anhydrous calcium sulfate, indicating type.
Alternatively, other types of desiccants may be used, subject to the
approval of the Administrator.

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Pretest Preparation. It is suggested that sampling equipment
be maintained according to the procedures described in APTD-0576.
8.1.1 Place 200 to 300 g of silica gel in each of several air-
tight containers. Weigh each container, including silica gel, to the
nearest 0.5 g, and record this weight. 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.
8.1.2 Check filters visually against light for irregularities,
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 polyethylene petri dishes), and
keep each filter in its identified container at all times except during
sampling.
8.1.3 Desiccate the filters at 20 5.6 deg.C (68
10 deg.F) and ambient pressure for at least 24 hours.
Weigh each filter (or filter and shipping container) 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 period for which the filter is exposed to the laboratory
atmosphere shall be less than 2 minutes. Alternatively (unless
otherwise specified by the Administrator), the filters may be oven
dried at 105 deg.C (220 deg.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.
8.2 Preliminary Determinations.
8.2.1 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 8.1) 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 8.6;
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.
8.2.2 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 8.3 of
Method 2).
8.2.3 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 required probe length.
8.2.4 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 (l) the sampling time per point is not less
than 2 minutes (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.
8.2.5 The sampling time at each point shall be the same. 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.
8.2.6 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.
8.3 Preparation of Sampling Train.
8.3.1 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.
8.3.2 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.
8.3.3 When glass probe liners are used, install the selected
nozzle using a Viton A O-ring when stack temperatures are less than 260
deg.C (500 deg.F) or a heat-resistant 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 discussed 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.
8.3.4 Set up the train as shown 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 the
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.
8.3.5 Place crushed ice around the impingers.
8.4 Leak-Check Procedures.
8.4.1 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-
2): 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

[[Page 61836]]

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.
8.4.2 Pretest Leak Check. A pretest leak check of the sampling
train is recommended, but not required. If the pretest leak check is
conducted, the following procedure should be used.
8.4.2.1 After the sampling train has been assembled, turn on and
set the filter and probe heating systems to 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 (15 in.) Hg vacuum.

Note: A lower vacuum may be used, provided that it is not
exceeded during the test.

8.4.2.2 If a heat-resistant 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 (15 in.) Hg vacuum (see Note in
Section 8.4.2.1). Then connect the probe to the train, and leak-check
at approximately 25 mm (1 in.) Hg vacuum; alternatively, the probe may
be leak-checked with the rest of the sampling train, in one step, at
380 mm (15 in.) Hg vacuum. Leakage rates in excess of 4 percent of the
average sampling rate or 0.00057 m\3\/min (0.020 cfm), whichever is
less, are unacceptable.
8.4.2.3 The following leak-check instructions for the sampling
train described in APTD-0576 and APTD-0581 may be helpful. Start the
pump with the bypass valve fully open and the 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 the direction of the bypass valve, as 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 and
start over.
8.4.2.4 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 the silica gel from being entrained backward into the third
impinger.
8.4.3 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 8.4.2 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 (0.020 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, either record
the leakage rate and plan to correct the sample volume as shown in
Section 12.3 of this method, or void the sample run.

Note: Immediately after component changes, leak checks are
optional. If such leak checks are done, the procedure outlined in
Section 8.4.2 above should be used.

8.4.4 Post-Test Leak Check. A leak check of the sampling train is
mandatory at the conclusion of each sampling run. The leak check shall
be performed in accordance with the procedures outlined in Section
8.4.2, 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
(0.020 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, either record the leakage rate and correct the sample
volume as shown in Section 12.3 of this method, or void the sampling
run.
8.5 Sampling 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 deg.C (248 25 deg.F), or
such other temperature as specified by an applicable subpart of the
standards or approved by the Administrator.
8.5.1 For each run, record the data required on a data sheet such
as the one shown in Figure 5-3. Be sure to record the initial DGM
reading. Record the DGM 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 indicated by Figure 5-3 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.
8.5.2 Clean the portholes prior to the test run to minimize the
chance of collecting deposited material. To begin sampling, verify that
the filter and probe heating systems are up to temperature, remove the
nozzle cap, verify 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 (Cp) is 0.85
0.02, and the stack gas equivalent density [dry molecular
weight (Md)] 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 Reference 7 in Section 17.0)
are taken to compensate for the deviations.
8.5.3 When the stack is under significant negative pressure (i.e.,
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.
8.5.4 When the probe is in position, block off the openings around
the probe and porthole to prevent unrepresentative dilution of the gas
stream.
8.5.5 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.
8.5.6 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
deg.C (68 deg.F) at the condenser/silica gel outlet. Also,

[[Page 61837]]

periodically check the level and zero of the manometer.
8.5.7 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 the 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 8.4.3). The total PM weight shall include the
summation of the filter assembly catches.
8.5.8 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: 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.

8.5.9 At the end of the sample run, close the coarse adjust valve,
remove the probe and nozzle from the stack, turn off the pump, record
the final DGM meter reading, and conduct a post-test leak check, as
outlined in Section 8.4.4. Also, leak-check the pitot lines as
described in Method 2, Section 8.1. The lines must pass this leak
check, in order to validate the velocity head data.
8.6 Calculation of Percent Isokinetic. Calculate percent
isokinetic (see Calculations, Section 12.11) to determine whether the
run was valid or another test run should be made. If there was
difficulty in maintaining isokinetic rates because of source
conditions, consult with the Administrator for possible variance on the
isokinetic rates.
8.7 Sample Recovery.
8.7.1 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.
8.7.2 When the probe can be safely handled, wipe off all external
PM near the tip of the probe nozzle, and place a cap over it to prevent
losing or gaining PM. Do not cap off the probe tip tightly while the
sampling train is cooling down. This would create a vacuum in the
filter holder, thereby drawing water from the impingers into the filter
holder.
8.7.3 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.
8.7.4 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.
8.7.5 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.''
8.7.6 Inspect the train prior to and during disassembly, and note
any abnormal conditions. Treat the samples as follows:
8.7.6.1 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
PM cake is inside the fold. Using a dry Nylon bristle brush and/or a
sharp-edged blade, carefully transfer to the petri dish any PM and/or
filter fibers that adhere to the filter holder gasket. Seal the
container.
8.7.6.2 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 PM 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. Deionized 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
rinse as follows:
8.7.6.2.1 Carefully remove the probe nozzle. 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.
8.7.6.2.2 Brush and rinse the inside parts of the fitting with
acetone in a similar way until no visible particles remain.
8.7.6.2.3 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 in 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 that is brushed from the probe. Run the
brush through the probe three times or more until no visible PM 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.
8.7.6.2.4 It is recommended that two people clean the probe to
minimize sample losses. Between sampling runs, keep brushes clean and
protected from contamination.
8.7.6.2.5 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 allow determination of whether
leakage

[[Page 61838]]

occurred during transport. Label the container to identify clearly its
contents.
8.7.6.3 Container No. 3. 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. 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
11.2.3.
8.7.6.4 Impinger Water. Treat the impingers as follows: Make a
notation of any color or film in the liquid catch. Measure the liquid
that 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. 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 6.1.1.8). If a different type of condenser is used,
measure the amount of moisture condensed either volumetrically or
gravimetrically.
8.8 Sample Transport. Whenever possible, containers should be
shipped in such a way that they remain upright at all times.

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures.

------------------------------------------------------------------------
Quality control
Section measure Effect
------------------------------------------------------------------------
8.4, 10.1-10.6................ Sampling Ensures accurate
equipment leak measurement of stack
check and gas flow rate,
calibration. sample volume.
------------------------------------------------------------------------

9.2 Volume Metering System Checks. The following procedures are
suggested to check the volume metering system calibration values at the
field test site prior to sample collection. These procedures are
optional.
9.2.1 Meter Orifice Check. Using the calibration data obtained
during the calibration procedure described in Section 10.3, determine
the H@ for the metering system orifice. The H@ is the
orifice pressure differential in units of in. H2O that
correlates to 0.75 cfm of air at 528 deg.R and 29.92 in. Hg. The
H@ is calculated as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.107

Where:

H = Average pressure differential across the orifice meter,
in. H2O.
Tm = Absolute average DGM temperature, deg.R.
Pbar = Barometric pressure, in. Hg.
= Total sampling time, min.
Y = DGM calibration factor, dimensionless.
Vm = Volume of gas sample as measured by DGM, dcf.
0.0319 = (0.0567 in. Hg/ deg.R) (0.75 cfm)\2\

9.2.1.1 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 H@ pressure
differential for 10 minutes. Record the volume collected, the DGM
temperature, and the barometric pressure. Calculate a DGM calibration
check value, Yc, as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.108

where:

Yc = DGM calibration check value, dimensionless.
10 = Run time, min.
9.2.1.2 Compare the Yc value with the dry gas meter
calibration factor Y to determine that: 0.97Y Yc 1.03Y. If
the Yc value is not within this range, the volume metering
system should be investigated before beginning the test.
9.2.2 Calibrated Critical Orifice. A 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 check by
following the procedure of Section 16.2.

10.0 Calibration and Standardization

Note: Maintain a laboratory log of all calibrations.

10.1 Probe Nozzle. Probe nozzles shall be calibrated before their
initial use in the field. Using a micrometer, measure the ID 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.
10.2 Pitot Tube Assembly. The Type S pitot tube assembly shall be
calibrated according to the procedure outlined in Section 10.1 of
Method 2.
10.3 Metering System.
10.3.1 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 5-4. The wet test meter
should have a capacity of 30 liters/rev (1 ft3/rev). A
spirometer of 400 liters (14 ft3) 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 DGM. Also note the barometric pressure and the
temperatures of the wet test meter, the inlet of the DGM, and the
outlet of the DGM. Select the highest and lowest orifice settings to
bracket the expected field operating range of the orifice. Use a
minimum volume of 0.14 m3 (5 ft3) at all orifice
settings. Record all the data on a form similar to Figure 5-5 and
calculate Y, the DGM calibration factor, and H@,
the orifice calibration factor, at each orifice setting as shown on
Figure 5-5. Allowable tolerances for

[[Page 61839]]

individual Y and H@ values are given in Figure 5-5.
Use the average of the Y values in the calculations in Section 12.0.
10.3.1.1 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 (0.020 cfm). At the end of the run, take the difference of the
measured wet test meter and DGM volumes. Divide the difference by 10 to
get the leak rate. The leak rate should not exceed 0.00057
m3/min (0.020 cfm).
10.3.2 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 DGM calibration factor. If the value
has changed by more than 5 percent, recalibrate the meter over the full
range of orifice settings, as detailed in Section 10.3.1.

Note: Alternative procedures (e.g., rechecking the orifice meter
coefficient) may be used, subject to the approval of the
Administrator.

10.3.3 Acceptable Variation in Calibration. If the DGM 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.
10.4 Probe Heater Calibration. 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 sample 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.

Note: The probe heating system shall be calibrated before its
initial use in the field.

10.5 Temperature Sensors. Use the procedure in Section 10.3 of
Method 2 to calibrate in-stack temperature sensors. Dial thermometers,
such as are used for the DGM and condenser outlet, shall be calibrated
against mercury-in-glass thermometers.
10.6 Barometer. Calibrate against a mercury barometer.

11.0 Analytical Procedure

11.1 Record the data required on a sheet such as the one shown in
Figure 5-6.
11.2 Handle each sample container as follows:
11.2.1 Container No. 1. Leave the contents in the shipping
container or transfer the filter and any loose PM 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 the purposes
of this section, 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 104 deg.C (220 deg.F) for 2 to 3 hours,
cooled in the desiccator, and weighed to a constant weight, unless
otherwise specified by the Administrator. The sample may be oven dried
at 104 deg.C (220 deg.F) for 2 to 3 hours. Once the sample has
cooled, weigh the sample, and use this weight as a final weight.
11.2.2 Container No. 2. 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. 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.
11.2.3 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.
11.2.4 Acetone Blank Container. Measure the 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: 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.

12.0 Data Analysis and Calculations

Carry out calculations, retaining at least one extra significant
figure beyond that of the acquired data. Round off figures after the
final calculation. Other forms of the equations may be used, provided
that they give equivalent results.
12.1 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 (gr/dscf).
I = Percent of isokinetic sampling.
L1 = Individual leakage rate observed during the leak-check
conducted prior to the first component change, m3/min
(ft3/min)
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 (0.020 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 ``i\th\'' 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)(m \3\))/((K)(g-mole)) {21.85
((in. Hg) (ft \3\))/(( deg.R) (lb-mole))}.

[[Page 61840]]

Tm = Absolute average DGM temperature (see Figure 5-3), K
( deg.R).
Ts = Absolute average stack gas temperature (see Figure 5-
3), K ( deg.R).
Tstd = Standard absolute temperature, 293 K (528 deg.R).
Va = Volume of acetone blank, ml.
Vaw = Volume of acetone used in wash, ml.
V1c = Total volume of liquid collected in impingers and
silica gel (see Figure 5-6), 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-
7, 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 5-4), 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 (n
\th\) component change until the end of the sampling run, min.
13.6 = Specific gravity of mercury.
60 = Sec/min.
100 = Conversion to percent.

12.2 Average Dry Gas Meter Temperature and Average Orifice
Pressure Drop. See data sheet (Figure 5-3).
12.3 Dry Gas Volume. Correct the sample volume measured by the dry
gas meter to standard conditions (20 deg.C, 760 mm Hg or 68 deg.F,
29.92 in. Hg) by using Equation 5-1.
[GRAPHIC] [TIFF OMITTED] TR17OC00.109

Where:

K1 = 0.3858 deg.K/mm Hg for metric units, = 17.64 deg.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 Li
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:
[GRAPHIC] [TIFF OMITTED] TR17OC00.110

(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:
[GRAPHIC] [TIFF OMITTED] TR17OC00.111

and substitute only for those leakage rates (Li or
Lp) which exceed La.
12.4 Volume of Water Vapor Condensed.
[GRAPHIC] [TIFF OMITTED] TR17OC00.112

Where:

K2 = 0.001333 m \3\/ml for metric units, = 0.04706 ft \3\/ml
for English units.
12.5 Moisture Content.
[GRAPHIC] [TIFF OMITTED] TR17OC00.113

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 the assumption of
saturated conditions is given in Section 4.0 of Method 4. For the
purposes of this method, the average stack gas temperature from
Figure 5-3 may be used to make this determination, provided that the
accuracy of the in-stack temperature sensor is 1 deg.C
(2 deg.F).

12.6 Acetone Blank Concentration.
[GRAPHIC] [TIFF OMITTED] TR17OC00.114

12.7 Acetone Wash Blank.
[GRAPHIC] [TIFF OMITTED] TR17OC00.115

12.8 Total Particulate Weight. Determine the total particulate
matter

[[Page 61841]]

catch from the sum of the weights obtained from Containers 1 and 2 less
the acetone blank (see Figure 5-6).

Note: 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. Refer to Section 8.5.8 to assist in calculation of results
involving two or more filter assemblies or two or more sampling
trains.

12.9 Particulate Concentration.
[GRAPHIC] [TIFF OMITTED] TR17OC00.116

Where:

K3 = 0.001 g/mg for metric units.
= 0.0154 gr/mg for English units.
12.10 Conversion Factors:

------------------------------------------------------------------------
From To Multiply by
------------------------------------------------------------------------
ft\3\............................... m\3\ 0.02832
gr.................................. mg 64.80004
gr/ft\3\............................ mg/m\3\ 2288.4
mg.................................. g 0.001
gr.................................. lb 1.429 x 10-\4\
------------------------------------------------------------------------

12.11 Isokinetic Variation.
12.11.1 Calculation from Raw Data.
[GRAPHIC] [TIFF OMITTED] TR17OC00.117

Where:
K4 = 0.003454 ((mm Hg)(m\3\))/((ml)( deg.K)) for metric
units,
= 0.002669 ((in. Hg)(ft\3\))/((ml)( deg.R)) for English units.

12.11.2 Calculation from Intermediate Values.
[GRAPHIC] [TIFF OMITTED] TR17OC00.118

Where:

K5 = 4.320 for metric units,
= 0.09450 for English units.

12.11.3 Acceptable Results. If 90 percent I
110 percent, the results are acceptable. If the PM results
are low in comparison to the standard, and ``I'' is over 110 percent or
less than 90 percent, the Administrator may opt to accept the results.
Reference 4 in Section 17.0 may be used to make acceptability
judgments. If ``I'' is judged to be unacceptable, reject the results,
and repeat the sampling run.
12.12 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 12.3 and
12.4 of Method 2.
13.0 Method Performance. [Reserved]
14.0 Pollution Prevention. [Reserved]
15.0 Waste Management. [Reserved]

16.0 Alternative Procedures

16.1 Dry Gas Meter as a Calibration Standard. A DGM may be used as
a calibration standard for volume measurements in place of the wet test
meter specified in Section 10.3, provided that it is calibrated
initially and recalibrated periodically as follows:
16.1.1 Standard Dry Gas Meter Calibration.
16.1.1.1. The DGM 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 (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 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.
16.1.1.2 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 DGM 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.
16.1.1.3 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.
16.1.1.4 Calculate flow rate, Q, for each run using the wet test
meter volume, VW, and the run time, . Calculate
the DGM coefficient, Yds, for each run. These calculations
are as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.119

[GRAPHIC] [TIFF OMITTED] TR17OC00.120

Where:

K1 = 0.3858 deg.C/mm Hg for metric units=17.64 deg.F/in.
Hg for English units.
VW = Wet test meter volume, liter (ft\3\).
Vds = Dry gas meter volume, liter (ft\3\).
Tds = Average dry gas meter temperature, deg.C ( deg.F).
Tadj = 273 deg.C for metric units = 460 deg.F for English
units.
TW = Average wet test meter temperature, deg.C ( deg.F)

[[Page 61842]]

Pbar = Barometric pressure, mm Hg (in. Hg).
p = Dry gas meter inlet differential pressure, mm
H2O (in. H2O).
= Run time, min.

16.1.1.5 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 no less than five average meter coefficients,
Yds.
16.1.1.6 Prepare a curve of meter coefficient, Yds,
versus flow rate, Q, for the DGM. This curve shall be used as a
reference when the meter is used to calibrate other DGMs and to
determine whether recalibration is required.
16.1.2 Standard Dry Gas Meter Recalibration.
16.1.2.1 Recalibrate the standard DGM 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 DGM 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.
16.1.2.2 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 30 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.
16.2 Critical Orifices As Calibration Standards. Critical orifices
may be used as calibration standards in place of the wet test meter
specified in Section 16.1, provided that they are selected, calibrated,
and used as follows:
16.2.1 Selection of Critical Orifices.
16.2.1.1 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 16.2.2.2.3). Select five critical orifices that
are appropriately sized to cover the range of flow rates between 10 and
34 liters/min (0.35 and 1.2 cfm) 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 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 in Table 5-1 in Section 18.0 give
the approximate flow rates.
16.2.1.2 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 (or equivalent) quick connect. Insert
the needle into the stopper as shown in Figure 5-9.
16.2.2 Critical Orifice Calibration. The procedure described in
this section uses the Method 5 meter box configuration with a DGM as
described in Section 6.1.1.9 to calibrate the critical orifices. Other
schemes may be used, subject to the approval of the Administrator.
16.2.2.1 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).
16.2.2.1.1 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 turn 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).
16.2.2.1.2 Check also for leakages in that portion of the sampling
train between the pump and the orifice meter. See Section 8.4.1 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.
16.2.2.1.3 After determining that the meter box is leakless,
calibrate the meter box according to the procedure given in Section
10.3. Make sure that the wet test meter meets the requirements stated
in Section 16.1.1.1. Check the water level in the wet test meter.
Record the DGM calibration factor, Y.
16.2.2.2 Calibration of Critical Orifices. Set up the apparatus as
shown in Figure 5-10.
16.2.2.2.1 Allow a warm-up time of 15 minutes. This step is
important to equilibrate the temperature conditions through the DGM.
16.2.2.2.2 Leak check the system as in Section 16.2.2.1.1. The
leakage rate shall be zero.
16.2.2.2.3 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.
16.2.2.2.4 Obtain the barometric pressure using a barometer as
described in Section 6.1.2. Record the barometric pressure,
Pbar, in mm Hg (in. Hg).
16.2.2.2.5 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
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' (see
Eq. 5-11). Record the information listed in Figure 5-11.
16.2.2.2.6 Calculate K' using Equation 5-11.
[GRAPHIC] [TIFF OMITTED] TR17OC00.121

Where:

K' = Critical orifice coefficient,
[m \3\)( deg.K)\1/2\]/

[[Continued on page 61843]]

Notices For
2009
2008
2007
2006
2005
2004
2003
2002
2001
2000
1999
1998
1997
1996
1995
1994

[[pp. 61793-61842]] Amendments for Testing and Monitoring Provisions

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