[[pp. 61843-61892]] 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 61843-61892]
From the Federal Register Online via GPO Access [wais.access.gpo.gov]
[DOCID:fr17oc00-12]

[[Continued from page 61842]]

[[Page 61843]]

[(mm Hg)(min)] {[(ft \3\)( deg.R)\1/2\)] [(in. Hg)(min)].
Tamb = Absolute ambient temperature, deg.K ( deg.R).
Calculate the arithmetic mean of the K' values. The individual K'
values should not differ by more than 0.5 percent from the
mean value.
16.2.3 Using the Critical Orifices as Calibration Standards.
16.2.3.1 Record the barometric pressure.
16.2.3.2 Calibrate the metering system according to the procedure
outlined in Section 16.2.2. Record the information listed in Figure 5-
12.
16.2.3.3 Calculate the standard volumes of air passed through the
DGM and the critical orifices, and calculate the DGM calibration
factor, Y, using the equations below:
[GRAPHIC] [TIFF OMITTED] TR17OC00.122

[GRAPHIC] [TIFF OMITTED] TR17OC00.123

[GRAPHIC] [TIFF OMITTED] TR17OC00.124

Where:

Vcr(std) = Volume of gas sample passed through the critical
orifice, corrected to standard conditions, dscm (dscf).
K1 = 0.3858 K/mm Hg for metric units
= 17.64 deg.R/in. Hg for English units.

16.2.3.4 Average the DGM calibration values for each of the flow
rates. The calibration factor, Y, at each of the flow rates should not
differ by more than 2 percent from the average.
16.2.3.5 To determine the need for recalibrating the critical
orifices, compare the DGM Y factors obtained from two adjacent orifices
each time a DGM is calibrated; for example, when checking orifice 13/
2.5, use orifices 12/10.2 and 13/5.1. If any critical orifice yields a
DGM Y factor differing by more than 2 percent from the others,
recalibrate the critical orifice according to Section 16.2.2.

17.0 References.

1. Addendum to Specifications for Incinerator Testing at Federal
Facilities. PHS, NCAPC. December 6, 1967.
2. Martin, Robert M. Construction Details of Isokinetic Source-
Sampling Equipment. Environmental Protection Agency. Research
Triangle Park, NC. APTD-0581. April 1971.
3. Rom, Jerome J. Maintenance, Calibration, and Operation of
Isokinetic Source Sampling Equipment. Environmental Protection
Agency. Research Triangle Park, NC. APTD-0576. March 1972.
4. Smith, W.S., R.T. Shigehara, and W.F. Todd. A Method of
Interpreting Stack Sampling Data. Paper Presented at the 63rd Annual
Meeting of the Air Pollution Control Association, St. Louis, MO.
June 14-19, 1970.
5. Smith, W.S., et al. Stack Gas Sampling Improved and
Simplified With New Equipment. APCA Paper No. 67-119. 1967.
6. Specifications for Incinerator Testing at Federal Facilities.
PHS, NCAPC. 1967.
7. Shigehara, R.T. Adjustment in the EPA Nomograph for Different
Pitot Tube Coefficients and Dry Molecular Weights. Stack Sampling
News 2:4-11. October 1974.
8. Vollaro, R.F. A Survey of Commercially Available
Instrumentation for the Measurement of Low-Range Gas Velocities.
U.S. Environmental Protection Agency, Emission Measurement Branch.
Research Triangle Park, NC. November 1976 (unpublished paper).
9. Annual Book of ASTM Standards. Part 26. Gaseous Fuels; Coal
and Coke; Atmospheric Analysis. American Society for Testing and
Materials. Philadelphia, PA. 1974. pp. 617-622.
10. Felix, L.G., G.I. Clinard, G.E. Lacy, and J.D. McCain.
Inertial Cascade Impactor Substrate Media for Flue Gas Sampling.
U.S. Environmental Protection Agency. Research Triangle Park, NC
27711. Publication No. EPA-600/7-77-060. June 1977. 83 pp.
11. Westlin, P.R. and R.T. Shigehara. Procedure for Calibrating
and Using Dry Gas Volume Meters as Calibration Standards. Source
Evaluation Society Newsletter. 3(1):17-30. February 1978.
12. Lodge, J.P., Jr., J.B. Pate, B.E. Ammons, and G.A. Swanson.
The Use of Hypodermic Needles as Critical Orifices in Air Sampling.
J. Air Pollution Control Association. 16:197-200. 1966.

18.0 Tables, Diagrams, Flowcharts, and Validation Data

----------------------------------------------------------------------------------------------------------------
Flow rate Flow rate
Gauge/cm liters/min. Gauge/cm liters/min.
----------------------------------------------------------------------------------------------------------------
12/7.6.......................................................... 32.56 14/2.5 19.54
12/10.2......................................................... 30.02 14/5.1 17.27
13/2.5.......................................................... 25.77 14/7.6 16.14
13/5.1.......................................................... 23.50 15/3.2 14.16
13/7.6.......................................................... 22.37 15/7.6 11.61
13/10.2......................................................... 20.67 15/10.2 10.48
----------------------------------------------------------------------------------------------------------------

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[[Page 61849]]

Plant-----------------------------------------------------------------
Date------------------------------------------------------------------
Run No.---------------------------------------------------------------
Filter No.------------------------------------------------------------
Amount liquid lost during transport-----------------------------------
Acetone blank volume, m1----------------------------------------------
Acetone blank concentration, mg/mg (Equation 5-4)---------------------
Acetone wash blank, mg (Equation 5-5)---------------------------------

----------------------------------------------------------------------------------------------------------------
Weight of particulate collected, mg
Container number --------------------------------------------------------------------------
Final weight Tare weight Weight gain
----------------------------------------------------------------------------------------------------------------
1.
----------------------------------------------------------------------------------------------------------------
2.
----------------------------------------------------------------------------------------------------------------
Total:
Less acetone blank...........
Weight of particulate matter.
----------------------------------------------------------------------------------------------------------------

------------------------------------------------------------------------
Volume of liquid water collected
---------------------------------------
Impinger volume, Silica gel weight,
ml g
------------------------------------------------------------------------
Final
Initial
Liquid collected
Total volume collected.... .................. g* ml
------------------------------------------------------------------------
* Convert weight of water to volume by dividing total weight increase by
density of water (1 g/ml).

Figure 5-6. Analytical Data Sheet
[GRAPHIC] [TIFF OMITTED] TR17OC00.147

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[[Page 61854]]

----------------------------------------------------------------------
Date------------------------------------------------------------------
Train ID--------------------------------------------------------------
DGM cal. factor-------------------------------------------------------
Critical orifice ID---------------------------------------------------

------------------------------------------------------------------------
Run No.
Dry gas meter -------------------------
1 2
------------------------------------------------------------------------
Final reading................ m3 (ft3)....... ........... ...........
Initial reading.............. m3 (ft3)....... ........... ...........
Difference, Vm............... m 3 (ft 3)..... ........... ...........
Inlet/Outlet................. ............... ........... ...........
Temperatures:............ deg.C ( deg.F) / /
Initial.................. deg.C ( deg.F) / /
Final.................... min/sec........ / /
Av. Temeperature, t m.... min............ ........... ...........
Time, ............. ............... ........... ...........
Orifice man. rdg., H mm (in.) H 2... ........... ...........
Bar. pressure, P bar......... mm (in.) Hg.... ........... ...........
Ambient temperature, tamb.... mm (in.) Hg.... ........... ...........
Pump vacuum.................. ............... ........... ...........
K' factor.................... ............... ........... ...........
Average.................. ............... ........... ...........
------------------------------------------------------------------------

Figure 5-11. Data sheet of determining K' factor.
Date------------------------------------------------------------------
Train ID--------------------------------------------------------------
Critical orifice ID---------------------------------------------------
Critical orifice K' factor--------------------------------------------

------------------------------------------------------------------------
Run No.
Dry gas meter -------------------------
1 2
------------------------------------------------------------------------
Final reading................ m\3\ (ft\3\)... ........... ...........
Initial reading.............. m\3\ (ft\3\)... ........... ...........
Difference, Vm............... m\3\ (ft\3\)... ........... ...........
Inlet/outlet temperatures.... deg.C ( deg.F) / /
Initial.................. deg.C ( deg.F) / /
Final.................... deg.C ( deg.F) ........... ...........
Avg. Temperature, tm..... min/sec........ / /
Time, ............. min............ ........... ...........
Orifice man. rdg., H min............ ........... ...........
Bar. pressure, Pbar.......... mm (in.) H2O... ........... ...........
Ambient temperature, tamb.... mm (in.) Hg.... ........... ...........
Pump vacuum.................. deg.C ( deg.F) ........... ...........
Vm(std)...................... mm (in.) Hg.... ........... ...........
Vcr(std)..................... m\3\ (ft\3\)... ........... ...........
DGM cal. factor, Y........... m\3\ (ft\3\)... ........... ...........
------------------------------------------------------------------------

Figure 5-12. Data Sheet for Determining DGM Y Factor

Method 5A--Determination of Particulate Matter Emissions From the
Asphalt Processing and Asphalt Roofing Industry

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, and Method 5.

1.0 Scope and Applications

1.1 Analyte. Particulate matter (PM). No CAS number assigned.
1.2 Applicability. This method is applicable for the determination
of PM emissions from asphalt roofing industry process saturators,
blowing stills, and other sources as specified in the regulations.
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 42
10 deg.C (108 18 deg.F). 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

[[Page 61855]]

method to establish appropriate safety and health practices and to
determine the applicability of regulatory limitations prior to
performing this test method.

6.0 Equipment and Supplies

6.1 Sample Collection. Same as Method 5, Section 6.1, with the
following exceptions and additions:
6.1.1 Probe Liner. Same as Method 5, Section 6.1.1.2, with the
note that at high stack gas temperatures greater than 250 deg.C (480
deg.F), water-cooled probes may be required to control the probe exit
temperature to 42 10 deg.C (108 18 deg.F).
6.1.2 Precollector Cyclone. Borosilicate glass following the
construction details shown in Air Pollution Technical Document (APTD)-
0581, ``Construction Details of Isokinetic Source-Sampling Equipment''
(Reference 2 in Method 5, Section 17.0).

Note: The cyclone shall be used when the stack gas moisture is
greater than 10 percent, and shall not be used otherwise.

6.1.3 Filter Heating System. Any heating (or cooling) system
capable of maintaining a sample gas temperature at the exit end of the
filter holder during sampling at 42 10 deg.C (108
18 deg.F).
6.2 Sample Recovery. The following items are required for sample
recovery:
6.2.1 Probe-Liner and Probe-Nozzle Brushes, Graduated Cylinder
and/or Balance, Plastic Storage Containers, and Funnel and Rubber
Policeman. Same as in Method 5, Sections 6.2.1, 6.2.5, 6.2.6, and
6.2.7, respectively.
6.2.2 Wash Bottles. Glass.
6.2.3 Sample Storage Containers. Chemically resistant 500-ml or
1,000-ml borosilicate glass bottles, with rubber-backed Teflon screw
cap liners or caps that are constructed so as to be leak-free, and
resistant to chemical attack by 1,1,1-trichloroethane (TCE). (Narrow-
mouth glass bottles have been found to be less prone to leakage.)
6.2.4 Petri Dishes. Glass, unless otherwise specified by the
Administrator.
6.2.5 Funnel. Glass.
6.3 Sample Analysis. Same as Method 5, Section 6.3, with the
following additions:
6.3.1 Beakers. Glass, 250-ml and 500-ml.
6.3.2 Separatory Funnel. 100-ml or greater.

7.0. Reagents and Standards

7.1 Sample Collection. The following reagents are required for
sample collection:
7.1.1 Filters, Silica Gel, Water, and Crushed Ice. Same as in
Method 5, Sections 7.1.1, 7.1.2, 7.1.3, and 7.1.4, respectively.
7.1.2 Stopcock Grease. TCE-insoluble, heat-stable grease (if
needed). This is not necessary if screw-on connectors with Teflon
sleeves, or similar, are used.
7.2 Sample Recovery. Reagent grade TCE, 0.001 percent
residue and stored in glass bottles. Run TCE blanks before field use,
and use only TCE with low blank values (0.001 percent). In
no case shall a blank value of greater than 0.001 percent of the weight
of TCE used be subtracted from the sample weight.
7.3 Analysis. Two reagents are required for the analysis:
7.3.1 TCE. Same as in Section 7.2.
7.3.2 Desiccant. Same as in Method 5, Section 7.3.2.

8.0. Sample Collection, Preservation, Storage, and Transport

8.1. Pretest Preparation. Unless otherwise specified, maintain and
calibrate all components according to the procedure described in APTD-
0576, ``Maintenance, Calibration, and Operation of Isokinetic Source-
Sampling Equipment'' (Reference 3 in Method 5, Section 17.0).
8.1.1 Prepare probe liners and sampling nozzles as needed for use.
Thoroughly clean each component with soap and water followed by a
minimum of three TCE rinses. Use the probe and nozzle brushes during at
least one of the TCE rinses (refer to Section 8.7 for rinsing
techniques). Cap or seal the open ends of the probe liners and nozzles
to prevent contamination during shipping.
8.1.2 Prepare silica gel portions and glass filters as specified
in Method 5, Section 8.1.
8.2 Preliminary Determinations. Select the sampling site, probe
nozzle, and probe length as specified in Method 5, Section 8.2. Select
a total sampling time greater than or equal to the minimum total
sampling time specified in the ``Test Methods and Procedures'' section
of the applicable subpart of the regulations. Follow the guidelines
outlined in Method 5, Section 8.2 for sampling time per point and total
sample volume collected.
8.3 Preparation of Sampling Train. Prepare the sampling train as
specified in Method 5, Section 8.3, with the addition of the
precollector cyclone, if used, between the probe and filter holder. The
temperature of the precollector cyclone, if used, should be maintained
in the same range as that of the filter, i.e., 42 10
deg.C (108 18 deg.F). Use no stopcock grease on ground
glass joints unless grease is insoluble in TCE.
8.4 Leak-Check Procedures. Same as Method 5, Section 8.4.
8.5 Sampling Train Operation. Operate the sampling train as
described in Method 5, Section 8.5, except maintain the temperature of
the gas exiting the filter holder at 42 10 deg.C (108
18 deg.F).
8.6 Calculation of Percent Isokinetic. Same as Method 5, Section
8.6.
8.7 Sample Recovery. Same as Method 5, Section 8.7.1 through
8.7.6.1, with the addition of the following:
8.7.1 Container No. 2 (Probe to Filter Holder).
8.7.1.1 Taking care to see that material 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, precollector cyclone and collector flask
(if used), and front half of the filter holder by washing these
components with TCE and placing the wash in a glass container.
Carefully measure the total amount of TCE used in the rinses. Perform
the TCE rinses as described in Method 5, Section 8.7.6.2, using TCE
instead of acetone.
8.7.1.2 Brush and rinse the inside of the cyclone, cyclone
collection flask, and the front half of the filter holder. Brush and
rinse each surface three times or more, if necessary, to remove visible
PM.
8.7.2 Container No. 3 (Silica Gel). Same as in Method 5, Section
8.7.6.3.
8.7.3 Impinger Water. Same as Method 5, Section 8.7.6.4.
8.8 Blank. Save a portion of the TCE used for cleanup as a blank.
Take 200 ml of this TCE directly from the wash bottle being used, and
place it in a glass sample container labeled ``TCE Blank.''

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures.

[[Page 61856]]

9.2 A quality control (QC) check of the volume metering system at
the field site is suggested before collecting the sample. Use the
procedure outlined in Method 5, Section 9.2.

10.0 Calibration and Standardization

Same as Method 5, Section 10.0.

11.0 Analytical Procedures

11.1 Analysis. Record the data required on a sheet such as the one
shown in Figure 5A-1. Handle each sample container as follows:
11.1.1 Container No. 1 (Filter). Transfer the filter from the
sample container to a tared glass weighing dish, and desiccate for 24
hours in a desiccator containing anhydrous calcium sulfate. Rinse
Container No. 1 with a measured amount of TCE, and analyze this rinse
with the contents of Container No. 2. Weigh the filter to a constant
weight. For the purpose of this analysis, the term ``constant weight''
means a difference of no more than 10 percent of the net filter weight
or 2 mg (whichever is greater) between two consecutive weighings made
24 hours apart. Report the ``final weight'' to the nearest 0.1 mg as
the average of these two values.
11.1.2 Container No. 2 (Probe to Filter Holder).
11.1.2.1 Before adding the rinse from Container No. 1 to Container
No. 2, note the level of liquid in Container No. 2, and confirm on the
analysis sheet whether leakage occurred during transport. If noticeable
leakage occurred, either void the sample or take steps, subject to the
approval of the Administrator, to correct the final results.
11.1.2.2 Add the rinse from Container No. 1 to Container No. 2 and
measure the liquid in this container either volumetrically to
1 ml or gravimetrically to 0.5 g. Check to see
whether there is any appreciable quantity of condensed water present in
the TCE rinse (look for a boundary layer or phase separation). If the
volume of condensed water appears larger than 5 ml, separate the oil-
TCE fraction from the water fraction using a separatory funnel. Measure
the volume of the water phase to the nearest ml; adjust the stack gas
moisture content, if necessary (see Sections 12.3 and 12.4). Next,
extract the water phase with several 25-ml portions of TCE until, by
visual observation, the TCE does not remove any additional organic
material. Transfer the remaining water fraction to a tared beaker and
evaporate to dryness at 93 deg.C (200 deg.F), desiccate for 24 hours,
and weigh to the nearest 0.1 mg.
11.1.2.3 Treat the total TCE fraction (including TCE from the
filter container rinse and water phase extractions) as follows:
Transfer the TCE and oil to a tared beaker, and evaporate at ambient
temperature and pressure. The evaporation of TCE from the solution may
take several days. Do not desiccate the sample until the solution
reaches an apparent constant volume or until the odor of TCE is not
detected. When it appears that the TCE has evaporated, desiccate the
sample, and weigh it at 24-hour intervals to obtain a ``constant
weight'' (as defined for Container No. 1 above). The ``total weight''
for Container No. 2 is the sum of the evaporated PM weight of the TCE-
oil and water phase fractions. Report the results to the nearest 0.1
mg.
11.1.3 Container No. 3 (Silica Gel). This step may be conducted in
the field. Weigh the spent silica gel (or silica gel plus impinger) to
the nearest 0.5 g using a balance.
11.1.4 ``TCE Blank'' Container. Measure TCE in this container
either volumetrically or gravimetrically. Transfer the TCE to a tared
250-ml beaker, and evaporate to dryness at ambient temperature and
pressure. Desiccate for 24 hours, and weigh to a constant weight.
Report the results to the nearest 0.1 mg.

Note: In order to facilitate the evaporation of TCE liquid
samples, these samples may be dried in a controlled temperature oven
at temperatures up to 38 deg.C (100 deg.F) until the liquid is
evaporated.

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 as long as
they give equivalent results.
12.1 Nomenclature. Same as Method 5, Section 12.1, with the
following additions:

Ct = TCE blank residue concentration, mg/g.
mt = Mass of residue of TCE blank after evaporation, mg.
Vpc = Volume of water collected in precollector, ml.
Vt = Volume of TCE blank, ml.
Vtw = Volume of TCE used in wash, ml.
Wt = Weight of residue in TCE wash, mg.
t = Density of TCE (see label on bottle), g/ml.

12.2 Dry Gas Meter Temperature, Orifice Pressure Drop, and Dry Gas
Volume. Same as Method 5, Sections 12.2 and 12.3, except use data
obtained in performing this test.
12.3 Volume of Water Vapor.
[GRAPHIC] [TIFF OMITTED] TR17OC00.134

Where:

K2 = 0.001333 m\3\/ml for metric units.
= 0.04706 ft\3\/ml for English units.

12.4 Moisture Content.
[GRAPHIC] [TIFF OMITTED] TR17OC00.135

Note: In saturated or water droplet-laden gas streams, two
calculations of the moisture content of the stack gas shall be made,
one from the impinger and precollector analysis (Equations 5A-1 and
5A-2) and a second from the assumption of saturated conditions. The
lower of the two values of moisture content shall be considered
correct. The procedure for determining the moisture content based
upon assumption of saturated conditions is given in Section 4.0 of
Method 4. For the purpose of this method, the average stack gas
temperature from Figure 5-3 of Method 5 may be used to make this
determination, provided that the accuracy of the in-stack
temperature sensor is within 1 deg.C (2 deg.F).

12.5 TCE Blank Concentration.
[GRAPHIC] [TIFF OMITTED] TR17OC00.136

Note: In no case shall a blank value of greater than 0.001
percent of the weight of TCE used be subtracted from the sample
weight.

12.6 TCE Wash Blank.
[GRAPHIC] [TIFF OMITTED] TR17OC00.137

12.7 Total PM Weight. Determine the total PM catch from the sum of
the weights obtained from Containers 1 and 2, less the TCE blank.
12.8 PM Concentration.
[GRAPHIC] [TIFF OMITTED] TR17OC00.138

Where:

K3 = 0.001 g/mg for metric units
= 0.0154 gr/mg for English units

12.9 Isokinetic Variation. Same as in Method 5, Section 12.11.

13.0 Method Performance [Reserved]

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 References

Same as Method 5, Section 17.0.

17.0 Tables, Diagrams, Flowcharts, and Validation Data

[[Page 61857]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.139

Method 5B--Determination of Nonsulfuric Acid Particulate Matter
Emissions From Stationary Sources

1.0 Scope and Application

1.1 Analyte. Nonsulfuric acid particulate matter. No CAS number
assigned.
1.2 Applicability. This method is determining applicable for the
determination of nonsulfuric acid particulate matter from stationary
sources, only where specified by an applicable subpart of the
regulations or where approved by the Administrator for a particular
application.
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 160
14 deg.C (320 25 deg.F). The collected
sample is then heated in an oven at 160 deg.C (320 deg.F) for 6 hours
to volatilize any condensed sulfuric acid that may have been collected,
and the nonsulfuric acid particulate mass is determined
gravimetrically.

3.0 Definitions [Reserved]

4.0 Interferences [Reserved]

5.0 Safety

6.0 Equipment and Supplies

Same as Method 5, Section 6.0, with the following addition and
exceptions:
6.1 Sample Collection. The probe liner heating system and filter
heating system must be capable of maintaining a sample gas temperature
of 160 14 deg.C (320 25 deg.F).
6.2 Sample Preparation. An oven is required for drying the sample.

7.0 Reagents and Standards

Same as Method 5, Section 7.0.

8.0 Sample Collection, Preservation, Storage, and Transport.

Same as Method 5, with the exception of the following:
8.1 Initial Filter Tare. Oven dry the filter at 160 5
deg.C (320 10 deg.F) for 2 to 3 hours, cool in a
desiccator for 2 hours, and weigh. Desiccate to constant weight to
obtain the initial tare weight. Use the applicable specifications and
techniques of Section 8.1.3 of Method 5 for this determination.
8.2 Probe and Filter Temperatures. Maintain the probe outlet and
filter temperatures at 160 14 deg.C (320 25
deg.F).

9.0 Quality Control

Same as Method 5, Section 9.0.

10.0 Calibration and Standardization

Same as Method 5, Section 10.0.

11.0 Analytical Procedure

Same as Method 5, Section 11.0, except replace Section
11.2.2 With the following:
11.1 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

[[Page 61858]]

contents to a tared 250 ml beaker, and evaporate to dryness at ambient
temperature and pressure. Then oven dry the probe and filter samples at
a temperature of 160 5 deg.C (320 10 deg.F)
for 6 hours. Cool in a desiccator for 2 hours, and weigh to constant
weight. Report the results to the nearest 0.1 mg.

12.0 Data Analysis and Calculations

Same as in Method 5, Section 12.0.

13.0 Method Performance [Reserved]

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 References

Same as Method 5, Section 17.0.

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

* * * * *

Method 5D--Determination of Particulate Matter Emissions from
Positive Pressure Fabric Filters

1.0 Scope and Application

1.1 Analyte. Particulate matter (PM). No CAS number assigned.
1.2 Applicability.
1.2.1 This method is applicable for the determination of PM
emissions from positive pressure fabric filters. Emissions are
determined in terms of concentration (mg/m3 or gr/
ft3) and emission rate (kg/hr or lb/hr).
1.2.2 The General Provisions of 40 CFR part 60, Sec. 60.8(e),
require that the owner or operator of an affected facility shall
provide performance testing facilities. Such performance testing
facilities include sampling ports, safe sampling platforms, safe access
to sampling sites, and utilities for testing. It is intended that
affected facilities also provide sampling locations that meet the
specification for adequate stack length and minimal flow disturbances
as described in Method 1. Provisions for testing are often overlooked
factors in designing fabric filters or are extremely costly. The
purpose of this procedure is to identify appropriate alternative
locations and procedures for sampling the emissions from positive
pressure fabric filters. The requirements that the affected facility
owner or operator provide adequate access to performance testing
facilities remain in effect.
1.3 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

2.1 Particulate matter is withdrawn isokinetically from the source
and collected on a glass fiber filter maintained at a temperature at or
above the exhaust gas temperature up to a nominal 120 deg.C (248
25 deg.F). The particulate 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

Same as Section 6.0 of either Method 5 or Method 17.

7.0 Reagents and Standards

Same as Section 7.0 of either Method 5 or Method 17.

8.0 Sample Collection, Preservation, Storage, and Transport

Same Section 8.0 of either Method 5 or Method 17, except replace
Section 8.2.1 of Method 5 with the following:
8.1 Determination of Measurement Site. The configuration of
positive pressure fabric filter structures frequently are not amenable
to emission testing according to the requirements of Method 1.
Following are several alternatives for determining measurement sites
for positive pressure fabric filters.
8.1.1 Stacks Meeting Method 1 Criteria. Use a measurement site as
specified in Method 1, Section 11.1.
8.1.2 Short Stacks Not Meeting Method 1 Criteria. Use stack
extensions and the procedures in Method 1. Alternatively, use flow
straightening vanes of the ``egg-crate'' type (see Figure 5D-1). Locate
the measurement site downstream of the straightening vanes at a
distance equal to or greater than two times the average equivalent
diameter of the vane openings and at least one-half of the overall
stack diameter upstream of the stack outlet.
8.1.3 Roof Monitor or Monovent. (See Figure 5D-2). For a positive
pressure fabric filter equipped with a peaked roof monitor, ridge vent,
or other type of monovent, use a measurement site at the base of the
monovent. Examples of such locations are shown in Figure 5D-2. The
measurement site must be upstream of any exhaust point (e.g., louvered
vent).
8.1.4 Compartment Housing. Sample immediately downstream of the
filter bags directly above the tops of the bags as shown in the
examples in Figure 5D-2. Depending on the housing design, use sampling
ports in the housing walls or locate the sampling equipment within the
compartment housing.
8.2 Determination of Number and Location of Traverse Points.
Locate the traverse points according to Method 1, Section 11.3. Because
a performance test consists of at least three test runs and because of
the varied configurations of positive pressure fabric filters, there
are several schemes by which the number of traverse points can be
determined and the three test runs can be conducted.
8.2.1 Single Stacks Meeting Method 1 Criteria. Select the number
of traverse points according to Method 1. Sample all traverse points
for each test run.
8.2.2 Other Single Measurement Sites. For a roof monitor or
monovent, single compartment housing, or other stack not meeting Method
1 criteria, use at least 24 traverse points. For example, for a
rectangular measurement site, such as a monovent, use a balanced 5 x 5
traverse point matrix. Sample all traverse points for each test run.
8.2.3 Multiple Measurement Sites. Sampling from two or more stacks
or measurement sites may be combined for a test run, provided the
following guidelines are met:
8.2.3.1 All measurement sites up to 12 must be sampled. For more
than 12 measurement sites, conduct sampling on at least 12 sites or 50
percent of the sites, whichever is greater. The measurement sites
sampled should be evenly, or nearly evenly, distributed among the
available sites; if not, all sites are to be sampled.
8.2.3.2 The same number of measurement sites must be sampled for
each test run.
8.2.3.3 The minimum number of traverse points per test run is 24.
An exception to the 24-point minimum would be a test combining the
sampling from two stacks meeting Method 1 criteria for acceptable stack
length, and

[[Page 61859]]

Method 1 specifies fewer than 12 points per site.
8.2.3.4 As long as the 24 traverse points per test run criterion
is met, the number of traverse points per measurement site may be
reduced to eight.
8.2.3.5 Alternatively, conduct a test run for each measurement
site individually using the criteria in Section 8.2.1 or 8.2.2 to
determine the number of traverse points. Each test run shall count
toward the total of three required for a performance test. If more than
three measurement sites are sampled, the number of traverse points per
measurement site may be reduced to eight as long as at least 72
traverse points are sampled for all the tests.
8.2.3.6 The following examples demonstrate the procedures for
sampling multiple measurement sites.
8.2.3.6.1 Example 1: A source with nine circular measurement sites
of equal areas may be tested as follows: For each test run, traverse
three measurement sites using four points per diameter (eight points
per measurement site). In this manner, test run number 1 will include
sampling from sites 1,2, and 3; run 2 will include samples from sites
4, 5, and 6; and run 3 will include sites 7, 8, and 9. Each test area
may consist of a separate test of each measurement site using eight
points. Use the results from all nine tests in determining the emission
average.
8.2.3.6.2 Example 2: A source with 30 rectangular measurement
sites of equal areas may be tested as follows: For each of the three
test runs, traverse five measurement sites using a 3 x 3 matrix of
traverse points for each site. In order to distribute the sampling
evenly over all the available measurement sites while sampling only 50
percent of the sites, number the sites consecutively from 1 to 30 and
sample all the even numbered (or odd numbered) sites. Alternatively,
conduct a separate test of each of 15 measurement sites using Section
8.2.1 or 8.2.2 to determine the number and location of traverse points,
as appropriate.
8.2.3.6.3 Example 3: A source with two measurement sites of equal
areas may be tested as follows: For each test of three test runs,
traverse both measurement sites, using Section 8.2.3 in determining the
number of traverse points. Alternatively, conduct two full emission
test runs for each measurement site using the criteria in Section 8.2.1
or 8.2.2 to determine the number of traverse points.
8.2.3.7 Other test schemes, such as random determination of
traverse points for a large number of measurement sites, may be used
with prior approval from the Administrator.
8.3 Velocity Determination.
8.3.1 The velocities of exhaust gases from positive pressure
baghouses are often too low to measure accurately with the type S pitot
tube specified in Method 2 (i.e., velocity head 1.3 mm H2O
(0.05 in. H2O)). For these conditions, measure the gas flow
rate at the fabric filter inlet following the procedures outlined in
Method 2. Calculate the average gas velocity at the measurement site as
shown in Section 12.2 and use this average velocity in determining and
maintaining isokinetic sampling rates.
8.3.2 Velocity determinations to determine and maintain isokinetic
rates at measurement sites with gas velocities within the range
measurable with the type S pitot tube (i.e., velocity head greater than
1.3 mm H2O (0.05 in. H2O)) shall be conducted
according to the procedures outlined in Method 2.
8.4 Sampling. Follow the procedures specified in Sections 8.1
through 8.6 of Method 5 or Sections 8.1 through 8.25 in Method 17 with
the exceptions as noted above.
8.5 Sample Recovery. Follow the procedures specified in Section
8.7 of Method 5 or Section 8.2 of Method 17.

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures.

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

10.0 Calibration and Standardization

Same as Section 10.0 of either Method 5 or Method 17.

11.0 Analytical Procedure

Same as Section 11.0 of either Method 5 or Method 17.

12.0 Data Analysis and Calculations

Same as Section 12.0 of either Method 5 or Method 17 with the
following exceptions:
12.1 Nomenclature.
Ao = Measurement site(s) total cross-sectional area, m\2\
(ft\2\).
C or Cavg = Average concentration of PM for all n runs, mg/
scm (gr/scf).
Qi = Inlet gas volume flow rate, m\3\/sec (ft\3\/sec).
mi = Mass collected for run i of n, mg (gr).
To = Average temperature of gas at measurement site, deg.K
( deg.R).
Ti = Average temperature of gas at inlet, deg.K ( deg.R).
Voli = Sample volume collected for run i of n, scm (scf).
v = Average gas velocity at the measurement site(s), m/s (ft/s)
Qo = Total baghouse exhaust volumetric flow rate, m\3\/sec
(ft\3\/sec).
Qd = Dilution air flow rate, m\3\/sec (ft\3\/sec).
Tamb = Ambient Temperature, ( deg.K).

12.2 Average Gas Velocity. When following Section 8.3.1, calculate
the average gas velocity at the measurement site as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.140

12.3 Volumetric Flow Rate. Total volumetric flow rate may be
determined as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.141

12.4 Dilution Air Flow Rate.
[GRAPHIC] [TIFF OMITTED] TR17OC00.142

12.5 Average PM Concentration. For multiple measurement sites,
calculate the average PM concentration as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.143

13.0 Method Performance. [Reserved]

14.0 Pollution Prevention. [Reserved]

15.0 Waste Management. [Reserved]

16.0 References

Same as Method 5, Section 17.0.

[[Page 61860]]

17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.144

[[Page 61861]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.145

[[Page 61862]]

Method 5E--Determination of Particulate Matter Emissions From the
Wool Fiberglass Insulation Manufacturing Industry

1.0 Scope and Applications

1.1 Analyte. Particulate matter (PM). No CAS number assigned.
1.2 Applicability. This method is applicable for the determination
of PM emissions from wool fiberglass insulation manufacturing sources.

2.0 Summary of Method

Particulate matter is withdrawn isokinetically from the source and
is collected either on a glass fiber filter maintained at a temperature
in the range of 120 14 deg.C (248 25 deg.F)
and in impingers in solutions of 0.1 N sodium hydroxide (NaOH). The
filtered particulate mass, which includes any material that condenses
at or above the filtration temperature, is determined gravimetrically
after the removal of uncombined water. The condensed PM collected in
the impinger solutions is determined as total organic carbon (TOC)
using a nondispersive infrared type of analyzer. The sum of the
filtered PM mass and the condensed PM is reported as the total PM mass.

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 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 to determine the applicability of regulatory limitations
prior to performing this test method.
5.2 Corrosive Reagents. The following reagents are hazardous.
Personal protective equipment and safe procedures are useful in
preventing chemical splashes. If contact occurs, immediately flush with
copious amounts of water at least 15 minutes. Remove clothing under
shower and decontaminate. Treat residual chemical burn as thermal burn.
5.2.1 Hydrochloric Acid (HCl). Highly toxic. Vapors are highly
irritating to eyes, skin, nose, and lungs, causing severe damage. May
cause bronchitis, pneumonia, or edema of lungs. Exposure to
concentrations of 0.13 to 0.2 percent in air can be lethal in minutes.
Will react with metals, producing hydrogen.
5.2.2 Sodium Hydroxide (NaOH). Causes severe damage to eye tissues
and to skin. Inhalation causes irritation to nose, throat, and lungs.
Reacts exothermically with limited amounts of water.

6.0 Equipment and Supplies

6.1 Sample Collection. Same as Method 5, Section 6.1, with the
exception of the following:
6.1.1 Probe Liner. Same as described in Section 6.1.1.2 of Method
5 except use only borosilicate or quartz glass liners.
6.1.2 Filter Holder. Same as described in Section 6.1.1.5 of
Method 5 with the addition of a leak-tight connection in the rear half
of the filter holder designed for insertion of a temperature sensor
used for measuring the sample gas exit temperature.
6.2 Sample Recovery. Same as Method 5, Section 6.2, except three
wash bottles are needed instead of two and only glass storage bottles
and funnels may be used.
6.3 Sample Analysis. Same as Method 5, Section 6.3, with the
additional equipment for TOC analysis as described below:
6.3.1 Sample Blender or Homogenizer. Waring type or ultrasonic.
6.3.2 Magnetic Stirrer.
6.3.3 Hypodermic Syringe. 0- to 100-l capacity.
6.3.4 Total Organic Carbon Analyzer. Rosemount Model 2100A
analyzer or equivalent and a recorder.
6.3.5 Beaker. 30-ml.
6.3.6 Water Bath. Temperature controlled.
6.3.7 Volumetric Flasks. 1000-ml and 500-ml.

7.0 Reagents and Standards

Unless otherwise indicated, it is intended that all reagents
conform to the specifications established by the Committee on
Analytical Reagents of the American Chemical Society, where such
specifications are available; otherwise, use the best available grade.
7.1 Sample Collection. Same as Method 5, Section 7.1, with the
addition of 0.1 N NaOH (Dissolve 4 g of NaOH in water and dilute to 1
liter).
7.2 Sample Recovery. Same as Method 5, Section 7.2, with the
addition of the following:
7.2.1 Water. Deionized distilled to conform to ASTM Specification
D 1193-77 or 91 Type 3 (incorporated by reference--see Sec. 60.17). The
potassium permanganate (KMnO4) test for oxidizable organic
matter may be omitted when high concentrations of organic matter are
not expected to be present.
7.2.2 Sodium Hydroxide. Same as described in Section 7.1.
7.3 Sample Analysis. Same as Method 5, Section 7.3, with the
addition of the following:
7.3.1 Carbon Dioxide-Free Water. Distilled or deionized water that
has been freshly boiled for 15 minutes and cooled to room temperature
while preventing exposure to ambient air by using a cover vented with
an Ascarite tube.
7.3.2 Hydrochloric Acid. HCl, concentrated, with a dropper.
7.3.3 Organic Carbon Stock Solution. Dissolve 2.1254 g of dried
potassium biphthalate (HOOCC6H4COOK) in
CO2-free water, and dilute to 1 liter in a volumetric flask.
This solution contains 1000 mg/L organic carbon.
7.3.4 Inorganic Carbon Stock Solution. Dissolve 4.404 g anhydrous
sodium carbonate (Na2CO3.) in about 500 ml of
CO2-free water in a 1-liter volumetric flask. Add 3.497 g
anhydrous sodium bicarbonate (NaHCO3) to the flask, and
dilute to 1 liter with CO2 -free water. This solution
contains 1000 mg/L inorganic carbon.
7.3.5 Oxygen Gas. CO2 -free.

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Pretest Preparation and Preliminary Determinations. Same as
Method 5, Sections 8.1 and 8.2, respectively.
8.2 Preparation of Sampling Train. Same as Method 5, Section 8.3,
except that 0.1 N NaOH is used in place of water in the impingers. The
volumes of the solutions are the same as in Method 5.
8.3 Leak-Check Procedures, Sampling Train Operation, Calculation
of Percent Isokinetic. Same as Method 5, Sections 8.4 through 8.6,
respectively.
8.4 Sample Recovery. Same as Method 5, Sections 8.7.1 through
8.7.4, with the addition of the following:
8.4.1 Save portions of the water, acetone, and 0.1 N NaOH used for
cleanup as blanks. Take 200 ml of each liquid directly from the wash
bottles being used, and place in glass sample containers labeled
``water blank,'' ``acetone blank,'' and ``NaOH blank,'' respectively.

[[Page 61863]]

8.4.2 Inspect the train prior to and during disassembly, and note
any abnormal conditions. Treat the samples as follows:
8.4.2.1 Container No. 1. Same as Method 5, Section 8.7.6.1.
8.4.2.2 Container No. 2. Use water to rinse the sample nozzle,
probe, and front half of the filter holder three times in the manner
described in Section 8.7.6.2 of Method 5 except that no brushing is
done. Put all the water wash in one container, seal, and label.
8.4.2.3 Container No. 3. Rinse and brush the sample nozzle, probe,
and front half of the filter holder with acetone as described for
Container No. 2 in Section 8.7.6.2 of Method 5.
8.4.2.4 Container No. 4. Place the contents of the silica gel
impinger in its original container as described for Container No. 3 in
Section 8.7.6.3 of Method 5.
8.4.2.5 Container No. 5. Measure the liquid in the first three
impingers and record the volume or weight as described for the Impinger
Water in Section 8.7.6.4 of Method 5. Do not discard this liquid, but
place it in a sample container using a glass funnel to aid in the
transfer from the impingers or graduated cylinder (if used) to the
sample container. Rinse each impinger thoroughly with 0.1 N NaOH three
times, as well as the graduated cylinder (if used) and the funnel, and
put these rinsings in the same sample container. Seal the container and
label to clearly identify its contents.
8.5 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.

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

10.0 Calibration and Standardization

Same as Method 5, Section 10.0, with the addition of the following
procedures for calibrating the total organic carbon analyzer:
10.1 Preparation of Organic Carbon Standard Curve.
10.1.1 Add 10 ml, 20 ml, 30 ml, 40 ml, and 50 ml of the organic
carbon stock solution to a series of five 1000-ml volumetric flasks.
Add 30 ml, 40 ml, and 50 ml of the same solution to a series of three
500-ml volumetric flasks. Dilute the contents of each flask to the mark
using CO2-free water. These flasks contain 10, 20, 30, 40,
50, 60, 80, and 100 mg/L organic carbon, respectively.
10.1.2 Use a hypodermic syringe to withdraw a 20- to 50-l
aliquot from the 10 mg/L standard solution and inject it into the total
carbon port of the analyzer. Measure the peak height. Repeat the
injections until three consecutive peaks are obtained within 10 percent
of their arithmetic mean. Repeat this procedure for the remaining
organic carbon standard solutions.
10.1.3 Calculate the corrected peak height for each standard by
deducting the blank correction (see Section 11.2.5.3) as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.146

Where:

A = Peak height of standard or sample, mm or other appropriate unit.
B = Peak height of blank, mm or other appropriate unit.

10.1.4 Prepare a linear regression plot of the arithmetic mean of
the three consecutive peak heights obtained for each standard solution
against the concentration of that solution. Calculate the calibration
factor as the inverse of the slope of this curve. If the product of the
arithmetic mean peak height for any standard solution and the
calibration factor differs from the actual concentration by more than 5
percent, remake and reanalyze that standard.
10.2 Preparation of Inorganic Carbon Standard Curve. Repeat the
procedures outlined in Sections 10.1.1 through 10.1.4, substituting the
inorganic carbon stock solution for the organic carbon stock solution,
and the inorganic carbon port of the analyzer for the total carbon
port.

11.0 Analytical Procedure

11.1 Record the data required on a sheet such as the one shown in
Figure 5-6 of Method 5.
11.2 Handle each sample container as follows:
11.2.1 Container No. 1. Same as Method 5, Section 11.2.1, except
that the filters must be dried at 20 6 deg.C (68
10 deg.F) and ambient pressure.
11.2.2 Containers No. 2 and No. 3. Same as Method 5, Section
11.2.2, except that evaporation of the samples must be at 20
6 deg.C (68 10 deg.F) and ambient pressure.
11.2.3 Container No. 4. Same as Method 5, Section 11.2.3.
11.2.4 ``Water Blank'' and ``Acetone Blank'' Containers. Determine
the water and acetone blank values following the procedures for the
``Acetone Blank'' container in Section 11.2.4 of Method 5. Evaporate
the samples at ambient temperature (20 6 deg.C (68
10 deg.F)) and pressure.
11.2.5 Container No. 5. For the determination of total organic
carbon, perform two analyses on successive identical samples, i.e.,
total carbon and inorganic carbon. The desired quantity is the
difference between the two values obtained. Both analyses are based on
conversion of sample carbon into carbon dioxide for measurement by a
nondispersive infrared analyzer. Results of analyses register as peaks
on a strip chart recorder.
11.2.5.1 The principal differences between the operating
parameters for the two channels involve the combustion tube packing
material and temperature. In the total carbon channel, a high
temperature (950 deg.C (1740 deg.F)) furnace heats a Hastelloy
combustion tube packed with cobalt oxide-impregnated asbestos fiber.
The oxygen in the carrier gas, the elevated temperature, and the
catalytic effect of the packing result in oxidation of both organic and
inorganic carbonaceous material to CO2, and steam. In the

[[Page 61864]]

inorganic carbon channel, a low temperature (150 deg.C (300 deg.F))
furnace heats a glass tube containing quartz chips wetted with 85
percent phosphoric acid. The acid liberates CO2 and steam
from inorganic carbonates. The operating temperature is below that
required to oxidize organic matter. Follow the manufacturer's
instructions for assembly, testing, calibration, and operation of the
analyzer.
11.2.5.2 As samples collected in 0.1 N NaOH often contain a high
measure of inorganic carbon that inhibits repeatable determinations of
TOC, sample pretreatment is necessary. Measure and record the liquid
volume of each sample (or impinger contents). If the sample contains
solids or immiscible liquid matter, homogenize the sample with a
blender or ultrasonics until satisfactory repeatability is obtained.
Transfer a representative portion of 10 to 15 ml to a 30-ml beaker, and
acidify with about 2 drops of concentrated HCl to a pH of 2 or less.
Warm the acidified sample at 50 deg.C (120 deg.F) in a water bath for
15 minutes.
11.2.5.3 While stirring the sample with a magnetic stirrer, use a
hypodermic syringe to withdraw a 20-to 50-1 aliquot from the
beaker. Analyze the sample for total carbon and calculate its corrected
mean peak height according to the procedures outlined in Sections
10.1.2 and 10.1.3. Similarly analyze an aliquot of the sample for
inorganic carbon. Repeat the analyses for all the samples and for the
0.1 N NaOH blank.
11.2.5.4 Ascertain the total carbon and inorganic carbon
concentrations (CTC and CIC, respectively) of
each sample and blank by comparing the corrected mean peak heights for
each sample and blank to the appropriate standard curve.

Note: If samples must be diluted for analysis, apply an
appropriate dilution factor.

12.0 Data Analysis and Calculations

Same as Method 5, Section 12.0, with the addition of the following:
12.1 Nomenclature.

Cc = Concentration of condensed particulate matter in stack
gas, gas dry basis, corrected to standard conditions, g/dscm (gr/dscf).
CIC = Concentration of condensed TOC in the liquid sample,
from Section 11.2.5, mg/L.
Ct = Total particulate concentration, dry basis, corrected
to standard conditions, g/dscm (gr/dscf).
CTC = Concentration of condensed TOC in the liquid sample,
from Section 11.2.5, mg/L.
CTOC = Concentration of condensed TOC in the liquid sample,
mg/L.
mTOC = Mass of condensed TOC collected in the impingers, mg.
Vm(std) = Volume of gas sample measured by the dry gas
meter, corrected to standard conditions, from Section 12.3 of Method 5,
dscm (dscf).
Vs = Total volume of liquid sample, ml.

12.2 Concentration of Condensed TOC in Liquid Sample.
[GRAPHIC] [TIFF OMITTED] TR17OC00.148

12.3 Mass of Condensed TOC Collected.
[GRAPHIC] [TIFF OMITTED] TR17OC00.149

Where:

0.001 = Liters per milliliter.

12.4 Concentration of Condensed Particulate Material.
[GRAPHIC] [TIFF OMITTED] TR17OC00.150

Where:

K4 = 0.001 g/mg for metric units.
= 0.0154 gr/mg for English units.

12.5 Total Particulate Concentration.
[GRAPHIC] [TIFF OMITTED] TR17OC00.151

13.0 Method Performance. [Reserved]

14.0 Pollution Prevention. [Reserved]

15.0 Waste Management. [Reserved]

16.0 References.

Same as Section 17.0 of Method 5, with the addition of the
following:

1. American Public Health Association, American Water Works
Association, Water Pollution Control Federation. Standard Methods
for the Examination of Water and Wastewater. Fifteenth Edition.
Washington, D.C. 1980.

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

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

1.0 Scope and Applications

1.1 Analyte. Nonsulfate particulate matter (PM). No CAS number
assigned.
1.2 Applicability. This method is applicable for the determination
of nonsulfate PM emissions from stationary sources. Use of this method
must be specified by an applicable subpart of the standards, or
approved by the Administrator for a particular application.
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 filter maintained at a temperature in the range 160
14 deg.C (320 25 deg.F). The collected
sample is extracted with water. A portion of the extract is analyzed
for sulfate content by ion chromatography. The remainder is neutralized
with ammonium hydroxide (NH4OH), dried, and weighed. The
weight of sulfate in the sample is calculated as ammonium sulfate
((NH4)2SO4), and is subtracted from
the total particulate weight; the result is reported as nonsulfate
particulate matter.

3.0 Definitions [Reserved]

4.0 Interferences [Reserved]

5.0 Safety

6.0 Equipment and Supplies

6.1 Sample Collection and Recovery. Same as Method 5, Sections 6.1
and 6.2, respectively.
6.2 Sample Analysis. Same as Method 5, Section 6.3, with the
addition of the following:
6.2.1 Erlenmeyer Flasks. 125-ml, with ground glass joints.
6.2.2 Air Condenser. With ground glass joint compatible with the
Erlenmeyer flasks.
6.2.3 Beakers. 600-ml.
6.2.4 Volumetric Flasks. 1-liter, 500-ml (one for each sample),
200-ml, and 50-ml (one for each sample and standard).
6.2.5 Pipet. 5-ml (one for each sample and standard).
6.2.6 Ion Chromatograph. The ion chromatograph should have at
least the following components.
6.2.6.1 Columns. An anion separation column or other column

[[Page 61865]]

capable of resolving the sulfate ion from other species present and a
standard anion suppressor column. Suppressor columns are produced as
proprietary items; however, one can be produced in the laboratory using
the resin available from BioRad Company, 32nd and Griffin Streets,
Richmond, California. Other systems which do not use suppressor columns
may also be used.
6.2.6.2 Pump. Capable of maintaining a steady flow as required by
the system.
6.2.6.3 Flow Gauges. Capable of measuring the specified system
flow rate.
6.2.6.4 Conductivity Detector.
6.2.6.5 Recorder. Compatible with the output voltage range of the
detector.

7.0 Reagents and Standards

Unless otherwise indicated, it is intended that all reagents
conform to the specifications established by the Committee on
Analytical Reagents of the American Chemical Society, where such
specifications are available; otherwise, use the best available grade.
7.1 Sample Collection. Same as Method 5, Section 7.1.
7.2 Sample Recovery. Same as Method 5, Section 7.2, with the
addition of the following:
7.2.1 Water. Deionized distilled, to conform to ASTM D 1193-77 or
91 Type 3 (incorporated by reference--see Sec. 60.17). The potassium
permanganate (KMnO4) test for oxidizable organic matter may
be omitted when high concentrations of organic matter are not expected
to be present.
7.3 Analysis. Same as Method 5, Section 7.3, with the addition of
the following:
7.3.1 Water. Same as in Section 7.2.1.
7.3.2 Stock Standard Solution, 1 mg
(NH4)2SO4/ml. Dry an adequate amount
of primary standard grade ammonium sulfate
((NH4)2SO4) at 105 to 110 deg.C (220
to 230 deg.F) for a minimum of 2 hours before preparing the standard
solution. Then dissolve exactly 1.000 g of dried
(NH4)2SO4 in water in a 1-liter
volumetric flask, and dilute to 1 liter. Mix well.
7.3.3 Working Standard Solution, 25 g
(NH4)2SO4/ml. Pipet 5 ml of the stock
standard solution into a 200-ml volumetric flask. Dilute to 200 ml with
water.
7.3.4 Eluent Solution. Weigh 1.018 g of sodium carbonate
(Na2CO3) and 1.008 g of sodium bicarbonate
(NaHCO3), and dissolve in 4 liters of water. This solution
is 0.0024 M Na2CO3/0.003 M NaHCO3.
Other eluents appropriate to the column type and capable of resolving
sulfate ion from other species present may be used.
7.3.5 Ammonium Hydroxide. Concentrated, 14.8 M.
7.3.6 Phenolphthalein Indicator. 3,3-Bis(4-hydroxyphenyl)-1-(3H)-
isobenzo-furanone. Dissolve 0.05 g in 50 ml of ethanol and 50 ml of
water.

8.0 Sample Collection, Preservation, Storage, and Transport

Same as Method 5, Section 8.0, with the exception of the following:
8.1 Sampling Train Operation. Same as Method 5, Section 8.5,
except that the probe outlet and filter temperatures shall be
maintained at 160 14 deg.C (320 25 deg.F).
8.2 Sample Recovery. Same as Method 5, Section 8.7, except that
the recovery solvent shall be water instead of acetone, and a clean
filter from the same lot as those used during testing shall be saved
for analysis as a blank.

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures

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

10.0 Calibration and Standardization

Same as Method 5, Section 10.0, with the addition of the following:
10.1 Determination of Ion Chromatograph Calibration Factor S.
Prepare a series of five standards by adding 1.0, 2.0, 4.0, 6.0, and
10.0 ml of working standard solution (25 g/ml) to a series of
five 50-ml volumetric flasks. (The standard masses will equal 25, 50,
100, 150, and 250 g.) Dilute each flask to the mark with
water, and mix well. Analyze each standard according to the
chromatograph manufacturer's instructions. Take peak height
measurements with symmetrical peaks; in all other cases, calculate peak
areas. Prepare or calculate a linear regression plot of the standard
masses in g (x-axis) versus their responses (y-axis). From
this line, or equation, determine the slope and calculate its
reciprocal which is the calibration factor, S. If any point deviates
from the line by more than 7 percent of the concentration at that
point, remake and reanalyze that standard. This deviation can be
determined by multiplying S times the response for each standard. The
resultant concentrations must not differ by more than 7 percent from
each known standard mass (i.e., 25, 50, 100, 150, and 250 g).
10.2 Conductivity Detector. Calibrate according to manufacturer's
specifications prior to initial use.

11.0 Analytical Procedure

11.1 Sample Extraction.
11.1.1 Note on the analytical data sheet, the level of the liquid
in the container, and whether any sample was lost during shipment. 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.
11.1.2 Cut the filter into small pieces, and place it in a 125-ml
Erlenmeyer flask with a ground glass joint equipped with an air
condenser. Rinse the shipping container with water, and pour the rinse
into the flask. Add additional water to the flask until it contains
about 75 ml, and place the flask on a hot plate. Gently reflux the
contents for 6 to 8 hours. Cool the solution, and transfer it to a 500-
ml volumetric flask. Rinse the Erlenmeyer flask with water, and
transfer the rinsings to the volumetric flask including the pieces of
filter.
11.1.3 Transfer the probe rinse to the same 500-ml volumetric
flask with the filter sample. Rinse the sample bottle with water, and
add the rinsings to the volumetric flask. Dilute the contents of the
flask to the mark with water.
11.1.4 Allow the contents of the flask to settle until all solid
material is at the bottom of the flask. If necessary, remove and
centrifuge a portion of the sample.
11.1.5 Repeat the procedures outlined in Sections 11.1.1 through
11.1.4 for each sample and for the filter blank.
11.2 Sulfate (SO4) Analysis.

[[Page 61866]]

11.2.1 Prepare a standard calibration curve according to the
procedures outlined in Section 10.1.
11.2.2 Pipet 5 ml of the sample into a 50-ml volumetric flask, and
dilute to 50 ml with water. (Alternatively, eluent solution may be used
instead of water in all sample, standard, and blank dilutions.) Analyze
the set of standards followed by the set of samples, including the
filter blank, using the same injection volume used for the standards.
11.2.3 Repeat the analyses of the standards and the samples, with
the standard set being done last. The two peak height or peak area
responses for each sample must agree within 5 percent of their
arithmetic mean for the analysis to be valid. Perform this analysis
sequence on the same day. Dilute any sample and the blank with equal
volumes of water if the concentration exceeds that of the highest
standard.
11.2.4 Document each sample chromatogram by listing the following
analytical parameters: injection point, injection volume, sulfate
retention time, flow rate, detector sensitivity setting, and recorder
chart speed.
11.3 Sample Residue.
11.3.1 Transfer the remaining contents of the volumetric flask to
a tared 600-ml beaker or similar container. Rinse the volumetric flask
with water, and add the rinsings to the tared beaker. Make certain that
all particulate matter is transferred to the beaker. Evaporate the
water in an oven at 105 deg.C (220 deg.F) until only about 100 ml of
water remains. Remove the beakers from the oven, and allow them to
cool.
11.3.2 After the beakers have cooled, add five drops of
phenolphthalein indicator, and then add concentrated ammonium hydroxide
until the solution turns pink. Return the samples to the oven at 105
deg.C (220 deg.F), and evaporate the samples to dryness. Cool the
samples in a desiccator, and weigh the samples to constant weight.

12.0 Data Analysis and Calculations

Same as Method 5, Section 12.0, with the addition of the following:
12.1 Nomenclature.

CW = Water blank residue concentration, mg/ml.
F = Dilution factor (required only if sample dilution was needed to
reduce the concentration into the range of calibration).
HS = Arithmetic mean response of duplicate sample analyses,
mm for height or mm2 for area.
Hb = Arithmetic mean response of duplicate filter blank
analyses, mm for height or mm2 for area.
mb = Mass of beaker used to dry sample, mg.
mf = Mass of sample filter, mg.
mn = Mass of nonsulfate particulate matter in the sample as
collected, mg.
ms = Mass of ammonium sulfate in the sample as collected,
mg.
mt = Mass of beaker, filter, and dried sample, mg.
mw = Mass of residue after evaporation of water blank, mg.
S = Calibration factor, g/mm.
Vb = Volume of water blank, ml.
VS = Volume of sample collected, 500 ml.

12.2 Water Blank Concentration.
[GRAPHIC] [TIFF OMITTED] TR17OC00.152

12.3 Mass of Ammonium Sulfate.
[GRAPHIC] [TIFF OMITTED] TR17OC00.153

Where:

100 = Aliquot factor, 495 ml/5 ml
1000 = Constant, g/mg

12.4 Mass of Nonsulfate Particulate Matter.
[GRAPHIC] [TIFF OMITTED] TR17OC00.154

13.0 Method Performance. [Reserved]

14.0 Pollution Prevention. [Reserved]

15.0 Waste Management. [Reserved]

16.0 Alternative Procedures

16.1 The following procedure may be used as an alternative to the
procedure in Section 11.0
16.1.1 Apparatus. Same as for Method 6, Sections 6.3.3 to 6.3.6
with the following additions.
16.1.1.1 Beakers. 250-ml, one for each sample, and 600-ml.
16.1.1.2 Oven. Capable of maintaining temperatures of 75
5 deg.C (167 9 deg.F) and 105
5 deg.C (221 9 deg.F).
16.1.1.3 Buchner Funnel.
16.1.1.4 Glass Columns. 25-mm x 305-mm (1-in. x 12-in.) with
Teflon stopcock.
16.1.1.5 Volumetric Flasks. 50-ml and 500-ml, one set for each
sample, and 100-ml, 200-ml, and 1000-ml.
16.1.1.6 Pipettes. Two 20-ml and one 200-ml, one set for each
sample, and 5-ml.
16.1.1.7 Filter Flasks. 500-ml.
16.1.1.8 Polyethylene Bottle. 500-ml, one for each sample.
16.1.2 Reagents. Same as Method 6, Sections 7.3.2 to 7.3.5 with
the following additions:
16.1.2.1 Water, Ammonium Hydroxide, and Phenolphthalein. Same as
Sections 7.2.1, 7.3.5, and 7.3.6 of this method, respectively.
16.1.2.2 Filter. Glass fiber to fit Buchner funnel.
16.1.2.3 Hydrochloric Acid (HCl), 1 m. Add 8.3 ml of concentrated
HCl (12 M) to 50 ml of water in a 100-ml volumetric flask. Dilute to
100 ml with water.
16.1.2.4 Glass Wool.
16.1.2.5 Ion Exchange Resin. Strong cation exchange resin,
hydrogen form, analytical grade.
16.1.2.6 pH Paper. Range of 1 to 7.
16.1.3 Analysis.
16.1.3.1 Ion Exchange Column Preparation. Slurry the resin with 1
M HCl in a 250-ml beaker, and allow to stand overnight. Place 2.5 cm (1
in.) of glass wool in the bottom of the glass column. Rinse the
slurried resin twice with water. Resuspend the resin in water, and pour
sufficient resin into the column to make a bed 5.1 cm (2 in.) deep. Do
not allow air bubbles to become entrapped in the resin or glass wool to
avoid channeling, which may produce erratic results. If necessary, stir
the resin with a glass rod to remove air bubbles, after the column has
been prepared, never let the liquid level fall below the top of the
upper glass wool plug. Place a 2.5-cm (1-in.) plug of glass wool on top
of the resin. Rinse the column with water until the eluate gives a pH
of 5 or greater as measured with pH paper.
16.1.3.2 Sample Extraction. Followup the procedure given in
Section 11.1.3 except do not dilute the sample to 500 ml.
16.1.3.3 Sample Residue.
16.1.3.3.1 Place at least one clean glass filter for each sample
in a Buchner funnel, and rinse the filters with water. Remove the
filters from the funnel, and dry them in an oven at 105
5 deg. C (221 9 deg.F); then cool in a desiccator. Weigh
each filter to constant weight according to the procedure in Method 5,
Section 11.0. Record the weight of each filter to the nearest 0.1 mg.

[[Page 61867]]

16.1.3.3.2 Assemble the vacuum filter apparatus, and place one of
the clean, tared glass fiber filters in the Buchner funnel. Decant the
liquid portion of the extracted sample (Section 16.1.3.2) through the
tared glass fiber filter into a clean, dry, 500-ml filter flask. Rinse
all the particulate matter remaining in the volumetric flask onto the
glass fiber filter with water. Rinse the particulate matter with
additional water. Transfer the filtrate to a 500-ml volumetric flask,
and dilute to 500 ml with water. Dry the filter overnight at 105
5 deg. C (221 9 deg.F), cool in a desiccator,
and weigh to the nearest 0.1 mg.
16.1.3.3.3 Dry a 250-ml beaker at 75 5 deg. C (167
9 deg. F), and cool in a desiccator; then weigh to
constant weight to the nearest 0.1 mg. Pipette 200 ml of the filtrate
that was saved into a tared 250-ml beaker; add five drops of
phenolphthalein indicator and sufficient concentrated ammonium
hydroxide to turn the solution pink. Carefully evaporate the contents
of the beaker to dryness at 75 5 deg. C (167
9 deg. F). Check for dryness every 30 minutes. Do not continue to bake
the sample once it has dried. Cool the sample in a desiccator, and
weigh to constant weight to the nearest 0.1 mg.
16.1.3.4 Sulfate Analysis. Adjust the flow rate through the ion
exchange column to 3 ml/min. Pipette a 20-ml aliquot of the filtrate
onto the top of the ion exchange column, and collect the eluate in a
50-ml volumetric flask. Rinse the column with two 15-ml portions of
water. Stop collection of the eluate when the volume in the flask
reaches 50-ml. Pipette a 20-ml aliquot of the eluate into a 250-ml
Erlenmeyer flask, add 80 ml of 100 percent isopropanol and two to four
drops of thorin indicator, and titrate to a pink end point using 0.0100
N barium perchlorate. Repeat and average the titration volumes. Run a
blank with each series of samples. Replicate titrations must agree
within 1 percent or 0.2 ml, whichever is larger. Perform the ion
exchange and titration procedures on duplicate portions of the
filtrate. Results should agree within 5 percent. Regenerate or replace
the ion exchange resin after 20 sample aliquots have been analyzed or
if the end point of the titration becomes unclear.

Note: Protect the 0.0100 N barium perchlorate solution from
evaporation at all times.

16.1.3.5 Blank Determination. Begin with a sample of water of the
same volume as the samples being processed and carry it through the
analysis steps described in Sections 16.1.3.3 and 16.1.3.4. A blank
value larger than 5 mg should not be subtracted from the final
particulate matter mass. Causes for large blank values should be
investigated and any problems resolved before proceeding with further
analyses.
16.1.4 Calibration. Calibrate the barium perchlorate solutions as
in Method 6, Section 10.5.
16.1.5 Calculations.
16.1.5.1 Nomenclature. Same as Section 12.1 with the following
additions:

ma = Mass of clean analytical filter, mg.
md = Mass of dissolved particulate matter, mg.
me = Mass of beaker and dissolved particulate matter after
evaporation of filtrate, mg.
mp = Mass of insoluble particulate matter, mg.
mr = Mass of analytical filter, sample filter, and insoluble
particulate matter, mg.
mbk = Mass of nonsulfate particulate matter in blank sample,
mg.
mn = Mass of nonsulfate particulate matter, mg.
ms = Mass of Ammonium sulfate, mg.
N = Normality of Ba(ClO4) titrant, meq/ml.
Va = Volume of aliquot taken for titration, 20 ml.
Vc = Volume of titrant used for titration blank, ml.
Vd = Volume of filtrate evaporated, 200 ml.
Ve = Volume of eluate collected, 50 ml.
Vf = Volume of extracted sample, 500 ml.
Vi = Volume of filtrate added to ion exchange column, 20 ml.
Vt = Volume of Ba(C104)2 titrant, ml.
W = Equivalent weight of ammonium sulfate, 66.07 mg/meq.
16.1.5.2 Mass of Insoluble Particulate Matter.
[GRAPHIC] [TIFF OMITTED] TR17OC00.155

16.1.5.3 Mass of Dissolved Particulate Matter.
[GRAPHIC] [TIFF OMITTED] TR17OC00.156

16.1.5.4 Mass of Ammonium Sulfate.
[GRAPHIC] [TIFF OMITTED] TR17OC00.157

16.1.5.5 Mass of Nonsulfate Particulate Matter.
[GRAPHIC] [TIFF OMITTED] TR17OC00.158

17.0 References

Same as Method 5, Section 17.0, with the addition of the following:

1. Mulik, J.D. and E. Sawicki. Ion Chromatographic Analysis of
Environmental Pollutants. Ann Arbor, Ann Arbor Science Publishers,
Inc. Vol. 2, 1979.
2. Sawicki, E., J.D. Mulik, and E. Wittgenstein. Ion
Chromatographic Analysis of Environmental Pollutants. Ann Arbor, Ann
Arbor Science Publishers, Inc. Vol. 1. 1978.
3. Siemer, D.D. Separation of Chloride and Bromide from Complex
Matrices Prior to Ion Chromatographic Determination. Analytical
Chemistry 52(12): 1874-1877. October 1980.
4. Small, H., T.S. Stevens, and W.C. Bauman. Novel Ion Exchange
Chromatographic Method Using Conductimetric Determination.
Analytical Chemistry. 47(11):1801. 1975.

18.0 Tables, Diagrams, Flowcharts, and Validation Data. [Reserved]

Method 5G--Determination of Particulate Matter Emissions From Wood
Heaters (Dilution Tunnel Sampling Location)

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 wood heaters.
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

2.1 The exhaust from a wood heater is collected with a total
collection hood, and is combined with ambient dilution air. Particulate
matter is withdrawn proportionally from a single point in a sampling
tunnel, and is collected on two glass fiber filters in series. The
filters are maintained at a temperature of no greater than 32 deg.C
(90 deg.F). The particulate mass is determined gravimetrically after
the removal of uncombined water.
2.2 There are three sampling train approaches described in this
method: (1) One dual-filter dry sampling train operated at about 0.015
m\3\/min (0.5 cfm), (2) One dual-filter plus impingers sampling train
operated at about 0.015 m\3\/min (0.5 cfm), and (3) two dual-filter dry
sampling trains operated simultaneously at any flow rate. Options

[[Page 61868]]

(2) and (3) are referenced in Section 16.0 of this method. The dual-
filter dry sampling train equipment and operation, option (1), are
described in detail in this method.

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. The sampling train configuration is shown in
Figure 5G-1 and consists of the following components:
6.1.1.1 Probe. Stainless steel (e.g., 316 or grade more corrosion
resistant) or glass about 9.5 mm (\3/8\ in.) I.D., 0.6 m (24 in.) in
length. If made of stainless steel, the probe shall be constructed from
seamless tubing.
6.1.1.2 Pitot Tube. Type S, as described in Section 6.1 of Method
2. The Type S pitot tube assembly shall have a known coefficient,
determined as outlined in Method 2, Section 10. Alternatively, a
standard pitot may be used as described in Method 2, Section 6.1.2.
6.1.1.3 Differential Pressure Gauge. Inclined manometer or
equivalent device, as described in Method 2, Section 6.2. One manometer
shall be used for velocity head (p) readings and another
(optional) for orifice differential pressure readings (H).
6.1.1.4 Filter Holders. Two each made of borosilicate glass,
stainless steel, or Teflon, with a glass frit or stainless steel filter
support and a silicone rubber, Teflon, or Viton gasket. The holder
design shall provide a positive seal against leakage from the outside
or around the filters. The filter holders shall be placed in series
with the backup filter holder located 25 to 100 mm (1 to 4 in.)
downstream from the primary filter holder. The filter holder shall be
capable of holding a filter with a 100 mm (4 in.) diameter, except as
noted in Section 16.
6.1.1.5 Filter Temperature Monitoring System. A temperature sensor
capable of measuring temperature to within 3 deg.C
( 5 deg.F). The sensor shall be installed at the exit side
of the front filter holder so that the sensing tip of the temperature
sensor is in direct contact with the sample gas or in a thermowell as
shown in Figure 5G-1. The temperature sensor shall comply with the
calibration specifications in Method 2, Section 10.3. Alternatively,
the sensing tip of the temperature sensor may be installed at the inlet
side of the front filter holder.
6.1.1.6 Dryer. Any system capable of removing water from the
sample gas to less than 1.5 percent moisture (volume percent) prior to
the metering system. The system shall include a temperature sensor for
demonstrating that sample gas temperature exiting the dryer is less
than 20 deg.C (68 deg.F).
6.1.1.7 Metering System. Same as Method 5, Section 6.1.1.9.
6.1.2 Barometer. Same as Method 5, Section 6.1.2.
6.1.3 Dilution Tunnel Gas Temperature Measurement. A temperature
sensor capable of measuring temperature to within 3 deg.C
( 5 deg.F).
6.1.4 Dilution Tunnel. The dilution tunnel apparatus is shown in
Figure 5G-2 and consists of the following components:
6.1.4.1 Hood. Constructed of steel with a minimum diameter of 0.3
m (1 ft) on the large end and a standard 0.15 to 0.3 m (0.5 to 1 ft)
coupling capable of connecting to standard 0.15 to 0.3 m (0.5 to 1 ft)
stove pipe on the small end.
6.1.4.2 90 deg. Elbows. Steel 90 deg. elbows, 0.15 to 0.3 m (0.5
to 1 ft) in diameter for connecting mixing duct, straight duct and
optional damper assembly. There shall be at least two 90 deg. elbows
upstream of the sampling section (see Figure 5G-2).
6.1.4.3 Straight Duct. Steel, 0.15 to 0.3 m (0.5 to 1 ft) in
diameter to provide the ducting for the dilution apparatus upstream of
the sampling section. Steel duct, 0.15 m (0.5 ft) in diameter shall be
used for the sampling section. In the sampling section, at least 1.2 m
(4 ft) downstream of the elbow, shall be two holes (velocity traverse
ports) at 90 deg. to each other of sufficient size to allow entry of
the pitot for traverse measurements. At least 1.2 m (4 ft) downstream
of the velocity traverse ports, shall be one hole (sampling port) of
sufficient size to allow entry of the sampling probe. Ducts of larger
diameter may be used for the sampling section, provided the
specifications for minimum gas velocity and the dilution rate range
shown in Section 8 are maintained. The length of duct from the hood
inlet to the sampling ports shall not exceed 9.1 m (30 ft).
6.1.4.4 Mixing Baffles. Steel semicircles (two) attached at
90 deg. to the duct axis on opposite sides of the duct midway between
the two elbows upstream of sampling section. The space between the
baffles shall be about 0.3 m (1 ft).
6.1.4.5 Blower. Squirrel cage or other fan capable of extracting
gas from the dilution tunnel of sufficient flow to maintain the
velocity and dilution rate specifications in Section 8 and exhausting
the gas to the atmosphere.
6.2 Sample Recovery. The following items are required for sample
recovery: probe brushes, wash bottles, sample storage containers, petri
dishes, and funnel. Same as Method 5, Sections 6.2.1 through 6.2.4, and
6.2.8, respectively.
6.3 Sample Analysis. The following items are required for sample
analysis: glass weighing dishes, desiccator, analytical balance,
beakers (250-ml or smaller), hygrometer, and temperature sensor. Same
as Method 5, Sections 6.3.1 through 6.3.3 and 6.3.5 through 6.3.7,
respectively.

7.0 Reagents and Standards

7.1 Sample Collection. The following reagents are required for
sample collection:
7.1.1 Filters. Glass fiber filters with a minimum diameter of 100
mm (4 in.), without organic binder, exhibiting at least 99.95 percent
efficiency (0.05 percent penetration) on 0.3-micron dioctyl phthalate
smoke particles. Gelman A/E 61631 has been found acceptable for this
purpose.
7.1.2 Stopcock Grease. Same as Method 5, Section 7.1.5. 7.2 Sample
Recovery. Acetone-reagent grade, same as Method 5, Section 7.2.
7.3 Sample Analysis. Two reagents are required for the sample
analysis:
7.3.1 Acetone. Same as in Section 7.2.
7.3.2 Desiccant. Anhydrous calcium sulfate, calcium chloride, or
silica gel, indicating type.

8.0 Sample Collection, Preservation, Transport, and Storage

8.1 Dilution Tunnel Assembly and Cleaning. A schematic of a
dilution tunnel is shown in Figure 5G-2. The dilution tunnel dimensions
and other features are described in Section 6.1.4. Assemble the
dilution tunnel, sealing joints and seams to prevent air leakage. Clean
the dilution tunnel with an appropriately sized wire chimney brush
before each certification test.
8.2 Draft Determination. Prepare the wood heater as in Method 28,
Section 6.2.1. Locate the dilution tunnel hood centrally over the wood
heater stack

[[Page 61869]]

exhaust. Operate the dilution tunnel blower at the flow rate to be used
during the test run. Measure the draft imposed on the wood heater by
the dilution tunnel (i.e., the difference in draft measured with and
without the dilution tunnel operating) as described in Method 28,
Section 6.2.3. Adjust the distance between the top of the wood heater
stack exhaust and the dilution tunnel hood so that the dilution tunnel
induced draft is less than 1.25 Pa (0.005 in. H2O). Have no
fire in the wood heater, close the wood heater doors, and open fully
the air supply controls during this check and adjustment.
8.3 Pretest Ignition. Same as Method 28, Section 8.7.
8.4 Smoke Capture. During the pretest ignition period, operate the
dilution tunnel and visually monitor the wood heater stack exhaust.
Operate the wood heater with the doors closed and determine that 100
percent of the exhaust gas is collected by the dilution tunnel hood. If
less than 100 percent of the wood heater exhaust gas is collected,
adjust the distance between the wood heater stack and the dilution
tunnel hood until no visible exhaust gas is escaping. Stop the pretest
ignition period, and repeat the draft determination procedure described
in Section 8.2.
8.5 Velocity Measurements. During the pretest ignition period,
conduct a velocity traverse to identify the point of average velocity.
This single point shall be used for measuring velocity during the test
run.
8.5.1 Velocity Traverse. Measure the diameter of the duct at the
velocity traverse port location through both ports. Calculate the duct
area using the average of the two diameters. A pretest leak-check of
pitot lines as in Method 2, Section 8.1, is recommended. Place the
calibrated pitot tube at the centroid of the stack in either of the
velocity traverse ports. Adjust the damper or similar device on the
blower inlet until the velocity indicated by the pitot is approximately
220 m/min (720 ft/min). Continue to read the p and temperature
until the velocity has remained constant (less than 5 percent change)
for 1 minute. Once a constant velocity is obtained at the centroid of
the duct, perform a velocity traverse as outlined in Method 2, Section
8.3 using four points per traverse as outlined in Method 1. Measure the
p and tunnel temperature at each traverse point and record the
readings. Calculate the total gas flow rate using calculations
contained in Method 2, Section 12. Verify that the flow rate is 4
0.40 dscm/min (140 14 dscf/min); if not,
readjust the damper, and repeat the velocity traverse. The moisture may
be assumed to be 4 percent (100 percent relative humidity at 85
deg.F). Direct moisture measurements (e.g., according to Method 4) are
also permissible.

Note: If burn rates exceed 3 kg/hr (6.6 lb/hr), dilution tunnel
duct flow rates greater than 4 dscm/min (140 dscfm) and sampling
section duct diameters larger than 150 mm (6 in.) are allowed. If
larger ducts or flow rates are used, the sampling section velocity
shall be at least 220 m/min (720 fpm). In order to ensure measurable
particulate mass catch, it is recommended that the ratio of the
average mass flow rate in the dilution tunnel to the average fuel
burn rate be less than 150:1 if larger duct sizes or flow rates are
used.

8.5.2 Testing Velocity Measurements. After obtaining velocity
traverse results that meet the flow rate requirements, choose a point
of average velocity and place the pitot and temperature sensor at that
location in the duct. Alternatively, locate the pitot and the
temperature sensor at the duct centroid and calculate a velocity
correction factor for the centroidal position. Mount the pitot to
ensure no movement during the test run and seal the port holes to
prevent any air leakage. Align the pitot opening to be parallel with
the duct axis at the measurement point. Check that this condition is
maintained during the test run (about 30-minute intervals). Monitor the
temperature and velocity during the pretest ignition period to ensure
that the proper flow rate is maintained. Make adjustments to the
dilution tunnel flow rate as necessary.
8.6 Pretest Preparation. Same as Method 5, Section 8.1.
8.7 Preparation of Sampling Train. During preparation and assembly
of the sampling train, keep all openings where contamination can occur
covered until just prior to assembly or until sampling is about to
begin.
Using a tweezer or clean disposable surgical gloves, place one
labeled (identified) and weighed filter in each of the filter holders.
Be sure that each filter is properly centered and that the gasket is
properly placed so as to prevent the sample gas stream from
circumventing the filter. Check each filter for tears after assembly is
completed.
Mark the probe with heat resistant tape or by some other method to
denote the proper distance into the stack or duct. Set up the train as
shown in Figure 5G-1.
8.8 Leak-Check Procedures.
8.8.1 Leak-Check of Metering System Shown in Figure 5G-1. That
portion of the sampling train from the pump to the orifice meter shall
be leak-checked prior to initial use and after each certification or
audit test. Leakage after the pump will result in less volume being
recorded than is actually sampled. Use the procedure described in
Method 5, Section 8.4.1. Similar leak-checks shall be conducted for
other types of metering systems (i.e., without orifice meters).
8.8.2 Pretest Leak-Check. A pretest leak-check of the sampling
train is recommended, but not required. If the pretest leak check is
conducted, the procedures outlined in Method 5, Section 8.4.2 should be
used. A vacuum of 130 mm Hg (5 in. Hg) may be used instead of 380 mm Hg
(15 in. Hg).
8.8.3 Post-Test Leak-Check. A leak-check of the sampling train is
mandatory at the conclusion of each test run. The leak-check shall be
performed in accordance with the procedures outlined in Method 5,
Section 8.4.2. A vacuum of 130 mm Hg (5 in. Hg) or the highest vacuum
measured during the test run, whichever is greater, may be used instead
of 380 mm Hg (15 in. Hg).
8.9 Preliminary Determinations. Determine the pressure,
temperature and the average velocity of the tunnel gases as in Section
8.5. Moisture content of diluted tunnel gases is assumed to be 4
percent for making flow rate calculations; the moisture content may be
measured directly as in Method 4.
8.10 Sampling Train Operation. Position the probe inlet at the
stack centroid, and block off the openings around the probe and
porthole to prevent unrepresentative dilution of the gas stream. Be
careful not to bump the probe into the stack wall when removing or
inserting the probe through the porthole; this minimizes the chance of
extracting deposited material.
8.10.1 Begin sampling at the start of the test run as defined in
Method 28, Section 8.8.1. During the test run, maintain a sample flow
rate proportional to the dilution tunnel flow rate (within 10 percent
of the initial proportionality ratio) and a filter holder temperature
of no greater than 32 deg.C (90 deg.F). The initial sample flow rate
shall be approximately 0.015 m\3\/min (0.5 cfm).
8.10.2 For each test run, record the data required on a data sheet
such as the one shown in Figure 5G-3. Be sure to record the initial dry
gas meter reading. Record the dry gas meter readings at the beginning
and end of each sampling time increment and when sampling is halted.
Take other readings as indicated on Figure 5G-3 at least once each 10
minutes during the test run. Since the manometer level and zero may
drift because of vibrations and temperature changes, make periodic
checks during the test run.
8.10.3 For the purposes of proportional sampling rate

[[Page 61870]]

determinations, data from calibrated flow rate devices, such as glass
rotameters, may be used in lieu of incremental dry gas meter readings.
Proportional rate calculation procedures must be revised, but
acceptability limits remain the same.
8.10.4 During the test run, make periodic adjustments to keep the
temperature between (or upstream of) the filters at the proper level.
Do not change sampling trains during the test run.
8.10.5 At the end of the test run (see Method 28, Section 6.4.6),
turn off the coarse adjust valve, remove the probe from the stack, turn
off the pump, record the final dry gas meter reading, and conduct a
post-test leak-check, as outlined in Section 8.8.2. 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.
8.11 Calculation of Proportional Sampling Rate. Calculate percent
proportionality (see Section 12.7) to determine whether the run was
valid or another test run should be made.
8.12 Sample Recovery. Same as Method 5, Section 8.7, with the
exception of the following:
8.12.1 An acetone blank volume of about 50-ml or more may be used.
8.12.2 Treat the samples as follows:
8.12.2.1 Container Nos. 1 and 1A. Treat the two filters according
to the procedures outlined in Method 5, Section 8.7.6.1. The filters
may be stored either in a single container or in separate containers.
Use the sum of the filter tare weights to determine the sample mass
collected.
8.12.2.3 Container No. 2.
8.12.2.3.1 Taking care to see that dust on the outside of the
probe or other exterior surfaces does not get into the sample,
quantitatively recover particulate matter or any condensate from the
probe and filter holders by washing and brushing these components with
acetone and placing the wash in a labeled glass container. At least
three cycles of brushing and rinsing are required.
8.12.2.3.2 Between sampling runs, keep brushes clean and protected
from contamination.
8.12.2.3.3 After all acetone washings and particulate matter have
been collected in the sample containers, tighten the lids on the sample
containers so that the acetone will not leak out when transferred to
the laboratory weighing area. Mark the height of the fluid levels to
determine whether leakage occurs during transport. Label the containers
clearly to identify contents.
8.13 Sample Transport. Whenever possible, containers should be
shipped in such a way that they remain upright at all times.

Note: Requirements for capping and transport of sample
containers are not applicable if sample recovery and analysis occur
in the same room.

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures.

------------------------------------------------------------------------
Quality control
Section measure Effect
------------------------------------------------------------------------
8.8, 10.1-10.4................ Sampling Ensures accurate
equipment leak measurement of stack
check and gas flow rate,
calibration. sample volume.
10.5.......................... Analytical Ensure accurate and
balance precise measurement
calibration. of collected
particulate.
16.2.5........................ Simultaneous, Ensure precision of
dual-train measured particulate
sample concentration.
collection.
------------------------------------------------------------------------

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

10.0 Calibration and Standardization

Note: Maintain a laboratory record of all calibrations.

10.1 Pitot Tube. The Type S pitot tube assembly shall be
calibrated according to the procedure outlined in Method 2, Section
10.1, prior to the first certification test and checked semiannually,
thereafter. A standard pitot need not be calibrated but shall be
inspected and cleaned, if necessary, prior to each certification test.
10.2 Volume Metering System.
10.2.1 Initial and Periodic Calibration. Before its initial use
and at least semiannually thereafter, calibrate the volume metering
system as described in Method 5, Section 10.3.1, except that the wet
test meter with a capacity of 3.0 liters/rev (0.1 ft\3\/rev) may be
used. Other liquid displacement systems accurate to within
1 percent, may be used as calibration standards.

Note: Procedures and equipment specified in Method 5, Section
16.0, for alternative calibration standards, including calibrated
dry gas meters and critical orifices, are allowed for calibrating
the dry gas meter in the sampling train. A dry gas meter used as a
calibration standard shall be recalibrated at least once annually.

10.2.2 Calibration After Use. After each certification or audit
test (four or more test runs conducted on a wood heater at the four
burn rates specified in Method 28), check calibration of the metering
system by performing three calibration runs at a single, intermediate
flow rate as described in Method 5, Section 10.3.2.

Note: Procedures and equipment specified in Method 5, Section
16.0, for alternative calibration standards are allowed for the
post-test dry gas meter calibration check.

10.2.3 Acceptable Variation in Calibration. If the dry gas meter
coefficient values obtained before and after a certification test
differ by more than 5 percent, the certification test shall either be
voided and repeated, or calculations for the certification test shall
be performed using whichever meter coefficient value (i.e., before or
after) gives the lower value of total sample volume.
10.3 Temperature Sensors. Use the procedure in Method 2, Section
10.3, to calibrate temperature sensors before the first certification
or audit test and at least semiannually, thereafter.
10.4 Barometer. Calibrate against a mercury barometer before the
first certification test and at least semiannually, thereafter. If a
mercury barometer is used, no calibration is necessary. Follow the
manufacturer's instructions for operation.
10.5 Analytical Balance. Perform a multipoint calibration (at
least five points spanning the operational range) of the analytical
balance before the first certification test and semiannually,
thereafter. Before each certification test, audit the balance by
weighing at least one calibration weight (class F) that corresponds to
50 to 150 percent of the weight of one filter. If the scale cannot
reproduce the value of the calibration weight to within 0.1 mg, conduct
the multipoint calibration before use.

11.0 Analytical Procedure

11.1 Record the data required on a sheet such as the one shown in
Figure 5G-4. Use the same analytical balance for determining tare
weights and final sample weights.
11.2 Handle each sample container as follows:

[[Page 61871]]

11.2.1 Container Nos. 1 and 1A. Treat the two filters according to
the procedures outlined in Method 5, Section 11.2.1.
11.2.2 Container No. 2. Same as Method 5, Section 11.2.2, except
that the beaker may be smaller than 250 ml.
11.2.3 Acetone Blank Container. Same as Method 5, Section 11.2.4,
except that the beaker may be smaller than 250 ml.

12.0 Data Analysis and Calculations

Bws = Water vapor in the gas stream, proportion by volume
(assumed to be 0.04).
cs = Concentration of particulate matter in stack gas, dry
basis, corrected to standard conditions, g/dscm (gr/dscf).
E = Particulate emission rate, g/hr (lb/hr).
Eadj = Adjusted particulate emission rate, g/hr (lb/hr).
La = Maximum acceptable leakage rate for either a pretest or
post-test leak-check, equal to 0.00057 m\3\/min (0.020 cfm) or 4
percent of the average sampling rate, whichever is less.
Lp = Leakage rate observed during the post-test leak-check,
m\3\/min (cfm).
ma = Mass of residue of acetone blank after evaporation, mg.
maw = Mass of residue from acetone wash after evaporation,
mg.
mn = Total amount of particulate matter collected, mg.
Mw = Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb-
mole).
Pbar = Barometric pressure at the sampling site, mm Hg (in.
Hg).
PR = Percent of proportional sampling rate.
Ps = Absolute gas pressure in dilution tunnel, mm Hg (in.
Hg).
Pstd = Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
Qsd = Average gas flow rate in dilution tunnel, calculated
as in Method 2, Equation 2-8, dscm/hr (dscf/hr).
Tm = Absolute average dry gas meter temperature (see Figure
5G-3), deg.K ( deg.R).
Tmi = Absolute average dry gas meter temperature during each
10-minute interval, i, of the test run, deg.K ( deg.R).
Ts = Absolute average gas temperature in the dilution tunnel
(see Figure 5G-3), deg.K ( deg.R).
Tsi = Absolute average gas temperature in the dilution
tunnel during each 10 minute interval, i, of the test run, deg.K
( deg.R).
Tstd = Standard absolute temperature, 293 deg.K (528
deg.R).
Va = Volume of acetone blank, ml.
Vaw = Volume of acetone used in wash, ml.
Vm = Volume of gas sample as measured by dry gas meter, dcm
(dcf).
Vmi = Volume of gas sample as measured by dry gas meter
during each 10-minute interval, i, of the test run, dcm.
Vm(std) = Volume of gas sample measured by the dry gas
meter, corrected to standard conditions, dscm (dscf).
Vs = Average gas velocity in the dilution tunnel, calculated
by Method 2, Equation 2-7, m/sec (ft/sec). The dilution tunnel dry gas
molecular weight may be assumed to be 29 g/g mole (lb/lb mole).
Vsi = Average gas velocity in dilution tunnel during each
10-minute interval, i, of the test run, calculated by Method 2,
Equation 2-7, m/sec (ft/sec).
Y = Dry gas meter calibration factor.
H = Average pressure differential across the orifice meter, if
used (see Figure 5G-2), mm H\2\O (in. H\2\O).
U = Total sampling time, min.
10 = 10 minutes, length of first sampling period.
13.6 = Specific gravity of mercury.
100 = Conversion to percent.
12.2 Dry Gas Volume. Same as Method 5, Section 12.2, except that
component changes are not allowable.
12.3 Solvent Wash Blank.
[GRAPHIC] [TIFF OMITTED] TR17OC00.159

12.4 Total Particulate Weight. Determine the total particulate
catch, mn, from the sum of the weights obtained from Container Nos. 1,
1A, and 2, less the acetone blank (see Figure 5G-4).
12.5 Particulate Concentration.
[GRAPHIC] [TIFF OMITTED] TR17OC00.160

Where:
K2 = 0.001 g/mg for metric units.
= 0.0154 gr/mg for English units.
12.6 Particulate Emission Rate.
[GRAPHIC] [TIFF OMITTED] TR17OC00.161

Note: Particulate emission rate results produced using the
sampling train described in Section 6 and shown in Figure 5G-1 shall
be adjusted for reporting purposes by the following method
adjustment factor:

[GRAPHIC] [TIFF OMITTED] TR17OC00.162

Where:

K3 = constant, 1.82 for metric units.
= constant, 0.643 for English units.

12.7 Proportional Rate Variation. Calculate PR for each 10-minute
interval, i, of the test run.
[GRAPHIC] [TIFF OMITTED] TR17OC00.163

Alternate calculation procedures for proportional rate variation
may be used if other sample flow rate data (e.g., orifice flow meters
or rotameters) are monitored to maintain proportional sampling rates.
The proportional rate variations shall be calculated for each 10-minute
interval by comparing the stack to nozzle velocity ratio for each 10-
minute interval to the average stack to nozzle velocity ratio for the
test run. Proportional rate variation may be calculated for intervals
shorter than 10 minutes with appropriate revisions to Equation 5G-5. If
no more than 10 percent of the PR values for all the intervals exceed
90 percent PR 110 percent, and if no PR value
for any interval exceeds 80 percent PR 120
percent, the results are acceptable. If the PR values for the test run
are judged to be unacceptable, report the test run emission results,
but do not include the results in calculating the weighted average
emission rate, and repeat the test run.

13.0 Method Performance. [Reserved]

14.0 Pollution Prevention. [Reserved]

15.0 Waste Management. [Reserved]

16.0 Alternative Procedures

16.1 Method 5H Sampling Train. The sampling train and sample
collection, recovery, and analysis procedures described in Method 5H,
Sections 6.1.1, 7.1, 7.2, 8.1, 8.10, 8.11, and 11.0, respectively, may
be used in lieu of similar sections in Method 5G.

[[Page 61872]]

Operation of the Method 5H sampling train in the dilution tunnel is as
described in Section 8.10 of this method. Filter temperatures and
condenser conditions are as described in Method 5H. No adjustment to
the measured particulate matter emission rate (Equation 5G-4, Section
12.6) is to be applied to the particulate emission rate measured by
this alternative method.
16.2 Dual Sampling Trains. Two sampling trains may be operated
simultaneously at sample flow rates other than that specified in
Section 8.10, provided that the following specifications are met.
16.2.1 Sampling Train. The sampling train configuration shall be
the same as specified in Section 6.1.1, except the probe, filter, and
filter holder need not be the same sizes as specified in the applicable
sections. Filter holders of plastic materials such as Nalgene or
polycarbonate materials may be used (the Gelman 1119 filter holder has
been found suitable for this purpose). With such materials, it is
recommended that solvents not be used in sample recovery. The filter
face velocity shall not exceed 150 mm/sec (30 ft/min) during the test
run. The dry gas meter shall be calibrated for the same flow rate range
as encountered during the test runs. Two separate, complete sampling
trains are required for each test run.
16.2.2 Probe Location. Locate the two probes in the dilution
tunnel at the same level (see Section 6.1.4.3). Two sample ports are
necessary. Locate the probe inlets within the 50 mm (2 in.) diameter
centroidal area of the dilution tunnel no closer than 25 mm (1 in.)
apart.
16.2.3 Sampling Train Operation. Operate the sampling trains as
specified in Section 8.10, maintaining proportional sampling rates and
starting and stopping the two sampling trains simultaneously. The pitot
values as described in Section 8.5.2 shall be used to adjust sampling
rates in both sampling trains.
16.2.4 Recovery and Analysis of Sample. Recover and analyze the
samples from the two sampling trains separately, as specified in
Sections 8.12 and 11.0, respectively.
16.2.4.1 For this alternative procedure, the probe and filter
holder assembly may be weighed without sample recovery (use no
solvents) described above in order to determine the sample weight
gains. For this approach, weigh the clean, dry probe and filter holder
assembly upstream of the front filter (without filters) to the nearest
0.1 mg to establish the tare weights. The filter holder section between
the front and second filter need not be weighed. At the end of the test
run, carefully clean the outside of the probe, cap the ends, and
identify the sample (label). Remove the filters from the filter holder
assemblies as described for container Nos. 1 and 1A in Section
8.12.2.1. Reassemble the filter holder assembly, cap the ends, identify
the sample (label), and transfer all the samples to the laboratory
weighing area for final weighing. Requirements for capping and
transport of sample containers are not applicable if sample recovery
and analysis occur in the same room.
16.2.4.2 For this alternative procedure, filters may be weighed
directly without a petri dish. If the probe and filter holder assembly
are to be weighed to determine the sample weight, rinse the probe with
acetone to remove moisture before desiccating prior to the test run.
Following the test run, transport the probe and filter holder to the
desiccator, and uncap the openings of the probe and the filter holder
assembly. Desiccate for 24 hours and weigh to a constant weight. Report
the results to the nearest 0.1 mg.
16.2.5 Calculations. Calculate an emission rate (Section 12.6) for
the sample from each sampling train separately and determine the
average emission rate for the two values. The two emission rates shall
not differ by more than 7.5 percent from the average emission rate, or
7.5 percent of the weighted average emission rate limit in the
applicable subpart of the regulations, whichever is greater. If this
specification is not met, the results are unacceptable. Report the
results, but do not include the results in calculating the weighted
average emission rate. Repeat the test run until acceptable results are
achieved, report the average emission rate for the acceptable test run,
and use the average in calculating the weighted average emission rate.

17.0 References

Same as Method 5, Section 17.0, References 1 through 11, with the
addition of the following:

1. Oregon Department of Environmental Quality. Standard Method
for Measuring the Emissions and Efficiencies of Woodstoves. June 8,
1984. Pursuant to Oregon Administrative Rules Chapter 340, Division
21.
2. American Society for Testing and Materials. Proposed Test
Methods for Heating Performance and Emissions of Residential Wood-
fired Closed Combustion-Chamber Heating Appliances. E-6 Proposal P
180. August 1986.
BILLING CODE 6560-50-P

[[Page 61873]]

18.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.164

[[Page 61874]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.165

[[Page 61875]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.166

[[Page 61876]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.167

BILLING CODE 6560-50-C

[[Page 61877]]

Method 5H--Determination of Particulate Matter Emissions From Wood
Heaters From a Stack Location

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 and condensible emissions from wood heaters.
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

2.1 Particulate matter is withdrawn proportionally from the wood
heater exhaust and is collected on two glass fiber filters separated by
impingers immersed in an ice water bath. The first filter is maintained
at a temperature of no greater than 120 deg.C (248 deg.F). The second
filter and the impinger system are cooled such that the temperature of
the gas exiting the second filter is no greater than 20 deg.C (68
deg.F). The particulate mass collected in the probe, on the filters,
and in the impingers is determined gravimetrically after the removal of
uncombined water.

3.0 Definitions

Same as in Method 6C, Section 3.0.

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. The sampling train configuration is shown in
Figure 5H-1. Same as Method 5, Section 6.1.1, with the exception of the
following:
6.1.1.1 Probe Nozzle. The nozzle is optional; a straight sampling
probe without a nozzle is an acceptable alternative.
6.1.1.2 Probe Liner. Same as Method 5, Section 6.1.1.2, except
that the maximum length of the sample probe shall be 0.6 m (2 ft) and
probe heating is optional.
6.1.1.3 Filter Holders. Two each of borosilicate glass, with a
glass frit or stainless steel filter support and a silicone rubber,
Teflon, or Viton gasket. The holder design shall provide a positive
seal against leakage from the outside or around the filter. The front
filter holder shall be attached immediately at the outlet of the probe
and prior to the first impinger. The second filter holder shall be
attached on the outlet of the third impinger and prior to the inlet of
the fourth (silica gel) impinger.
6.1.2 Barometer. Same as Method 5, Section 6.2.
6.1.3 Stack Gas Flow Rate Measurement System. A schematic of an
example test system is shown in Figure 5H-2. The flow rate measurement
system consists of the following components:
6.1.3.1 Sample Probe. A glass or stainless steel sampling probe.
6.1.3.2 Gas Conditioning System. A high density filter to remove
particulate matter and a condenser capable of lowering the dew point of
the gas to less than 5 deg.C (40 deg.F). Desiccant, such as Drierite,
may be used to dry the sample gas. Do not use silica gel.
6.1.3.3 Pump. An inert (e.g., Teflon or stainless steel heads)
sampling pump capable of delivering more than the total amount of
sample required in the manufacturer's instructions for the individual
instruments. A means of controlling the analyzer flow rate and a device
for determining proper sample flow rate (e.g., precision rotameter,
pressure gauge downstream of all flow controls) shall be provided at
the analyzer. The requirements for measuring and controlling the
analyzer flow rate are not applicable if data are presented that
demonstrate that the analyzer is insensitive to flow variations over
the range encountered during the test.
6.1.3.4 Carbon Monoxide (CO) Analyzer. Any analyzer capable of
providing a measure of CO in the range of 0 to 10 percent by volume at
least once every 10 minutes.
6.1.3.5 Carbon Dioxide (CO2) Analyzer. Any analyzer
capable of providing a measure of CO2 in the range of 0 to
25 percent by volume at least once every 10 minutes.

Note: Analyzers with ranges less than those specified above may
be used provided actual concentrations do not exceed the range of
the analyzer.

6.1.3.6 Manifold. A sampling tube capable of delivering the sample
gas to two analyzers and handling an excess of the total amount used by
the analyzers. The excess gas is exhausted through a separate port.
6.1.3.7 Recorders (optional). To provide a permanent record of the
analyzer outputs.
6.1.4 Proportional Gas Flow Rate System. To monitor stack flow
rate changes and provide a measurement that can be used to adjust and
maintain particulate sampling flow rates proportional to the stack gas
flow rate. A schematic of the proportional flow rate system is shown in
Figure 5H-2 and consists of the following components:
6.1.4.1 Tracer Gas Injection System. To inject a known
concentration of sulfur dioxide (SO2) into the flue. The
tracer gas injection system consists of a cylinder of SO2, a
gas cylinder regulator, a stainless steel needle valve or flow
controller, a nonreactive (stainless steel and glass) rotameter, and an
injection loop to disperse the SO2 evenly in the flue.
6.1.4.2 Sample Probe. A glass or stainless steel sampling probe.
6.1.4.3 Gas Conditioning System. A combustor as described in
Method 16A, Sections 6.1.5 and 6.1.6, followed by a high density filter
to remove particulate matter, and a condenser capable of lowering the
dew point of the gas to less than 5 deg.C (40 deg.F). Desiccant, such
as Drierite, may be used to dry the sample gas. Do not use silica gel.
6.1.4.4 Pump. Same as described in Section 6.1.3.3.
6.1.4.5 SO2 Analyzer. Any analyzer capable of providing
a measure of the SO2 concentration in the range of 0 to
1,000 ppm by volume (or other range necessary to measure the
SO2 concentration) at least once every 10 minutes.
6.1.4.6 Recorder (optional). To provide a permanent record of the
analyzer outputs.

Note: Other tracer gas systems, including helium gas systems,
are acceptable for determination of instantaneous proportional
sampling rates.

6.2 Sample Recovery. Same as Method 5, Section 6.2.
6.3 Sample Analysis. Same as Method 5, Section 6.3, with the
addition of the following:
6.3.1 Separatory Funnel. Glass or Teflon, 500-ml or greater.

[[Page 61878]]

7.0 Reagents and Standards

7.1 Sample Collection. Same as Method 5, Section 7.1, including
deionized distilled water.
7.2 Sample Recovery. Same as Method 5, Section 7.2.
7.3 Sample Analysis. The following reagents and standards are
required for sample analysis:
7.3.1 Acetone. Same as Method 5 Section 7.2.
7.3.2 Dichloromethane (Methylene Chloride). Reagent grade, 0.001
percent residue in glass bottles.
7.3.3 Desiccant. Anhydrous calcium sulfate, calcium chloride, or
silica gel, indicating type.
7.3.4 Cylinder Gases. For the purposes of this procedure, span
value is defined as the upper limit of the range specified for each
analyzer as described in Section 6.1.3.4 or 6.1.3.5. If an analyzer
with a range different from that specified in this method is used, the
span value shall be equal to the upper limit of the range for the
analyzer used (see Note in Section 6.1.3.5).
7.3.4.1 Calibration Gases. The calibration gases for the
CO2, CO, and SO2 analyzers shall be
CO2 in nitrogen (N2), CO in N2, and
SO2 in N2, respectively. CO2 and CO
calibration gases may be combined in a single cylinder. Use three
calibration gases as specified in Method 6C, Sections 7.2.1 through
7.2.3.
7.3.4.2 SO2 Injection Gas. A known concentration of
SO2 in N2. The concentration must be at least 2
percent SO2 with a maximum of 100 percent SO2.

8.0 Sample Collection, Preservation, Transport, and Storage

8.1 Pretest Preparation. Same as Method 5, Section 8.1.
8.2 Calibration Gas and SO2 Injection Gas Concentration
Verification, Sampling System Bias Check, Response Time Test, and Zero
and Calibration Drift Tests. Same as Method 6C, Sections 8.2.1, 8.2.3,
8.2.4, and 8.5, respectively, except that for verification of CO and
CO2 gas concentrations, substitute Method 3 for Method 6.
8.3 Preliminary Determinations.
8.3.1 Sampling Location. The sampling location for the particulate
sampling probe shall be 2.45 0.15 m (8 0.5
ft) above the platform upon which the wood heater is placed (i.e., the
top of the scale).
8.3.2 Sampling Probe and Nozzle. Select a nozzle, if used, sized
for the range of velocity heads, such that it is not necessary to
change the nozzle size in order to maintain proportional sampling
rates. During the run, do not change the nozzle size. Select a suitable
probe liner and probe length to effect minimum blockage.
8.4 Preparation of Particulate Sampling Train. Same as Method 5,
Section 8.3, with the exception of the following:
8.4.1 The train should be assembled as shown in Figure 5H-1.
8.4.2 A glass cyclone may not be used between the probe and filter
holder.
8.5 Leak-Check Procedures.
8.5.1 Leak-Check of Metering System Shown in Figure 5H-1. That
portion of the sampling train from the pump to the orifice meter shall
be leak-checked after each certification or audit test. Use the
procedure described in Method 5, Section 8.4.1.
8.5.2 Pretest Leak-Check. A pretest leak-check of the sampling
train is recommended, but not required. If the pretest leak-check is
conducted, the procedures outlined in Method 5, Section 8.5.2 should be
used. A vacuum of 130 mm Hg (5 in. Hg) may be used instead of 380 mm Hg
(15 in. Hg).
8.5.2 Leak-Checks During Sample Run. If, during the sampling run,
a component (e.g., filter assembly or impinger) change becomes
necessary, conduct a leak-check as described in Method 5, Section
8.4.3.
8.5.3 Post-Test Leak-Check. A leak-check is mandatory at the
conclusion of each sampling run. The leak-check shall be performed in
accordance with the procedures outlined in Method 5, Section 8.4.4,
except that a vacuum of 130 mm Hg (5 in. Hg) or the greatest vacuum
measured during the test run, whichever is greater, may be used instead
of 380 mm Hg (15 in. Hg).
8.6 Tracer Gas Procedure. A schematic of the tracer gas injection
and sampling systems is shown in Figure 5H-2.
8.6.1 SO2 Injection Probe. Install the SO2
injection probe and dispersion loop in the stack at a location 2.9
0.15 m (9.5 0.5 ft) above the sampling
platform.
8.6.2 SO2 Sampling Probe. Install the SO2
sampling probe at the centroid of the stack at a location 4.1
0.15 m (13.5 0.5 ft) above the sampling
platform.
8.7 Flow Rate Measurement System. A schematic of the flow rate
measurement system is shown in Figure 5H-2. Locate the flow rate
measurement sampling probe at the centroid of the stack at a location
2.3 0.3 m (7.5 1 ft) above the sampling
platform.
8.8 Tracer Gas Procedure. Within 1 minute after closing the wood
heater door at the start of the test run (as defined in Method 28,
Section 8.8.1), meter a known concentration of SO2 tracer
gas at a constant flow rate into the wood heater stack. Monitor the
SO2 concentration in the stack, and record the
SO2 concentrations at 10-minute intervals or more often.
Adjust the particulate sampling flow rate proportionally to the
SO2 concentration changes using Equation 5H-6 (e.g., the
SO2 concentration at the first 10-minute reading is measured
to be 100 ppm; the next 10 minute SO2 concentration is
measured to be 75 ppm: the particulate sample flow rate is adjusted
from the initial 0.15 cfm to 0.20 cfm). A check for proportional rate
variation shall be made at the completion of the test run using
Equation 5H-10.
8.9 Volumetric Flow Rate Procedure. Apply stoichiometric
relationships to the wood combustion process in determining the exhaust
gas flow rate as follows:
8.9.1 Test Fuel Charge Weight. Record the test fuel charge weight
(wet) as specified in Method 28, Section 8.8.2. The wood is assumed to
have the following weight percent composition: 51 percent carbon, 7.3
percent hydrogen, 41 percent oxygen. Record the wood moisture for each
fuel charge as described in Method 28, Section 8.6.5. The ash is
assumed to have negligible effect on associated C, H, and O
concentrations after the test burn.
8.9.2 Measured Values. Record the CO and CO2
concentrations in the stack on a dry basis every 10 minutes during the
test run or more often. Average these values for the test run. Use as a
mole fraction (e.g., 10 percent CO2 is recorded as 0.10) in
the calculations to express total flow (see Equation 5H-6).
8.10 Sampling Train Operation.
8.10.1 For each run, record the data required on a data sheet such
as the one shown in Figure 5H-3. Be sure to record the initial dry gas
meter reading. Record the dry gas meter readings at the beginning and
end of each sampling time increment, when changes in flow rates are
made, before and after each leak-check, and when sampling is halted.
Take other readings as indicated on Figure 5H-3 at least once each 10
minutes during the test run.
8.10.2 Remove the nozzle cap, verify that the filter and probe
heating systems are up to temperature, and that the probe is properly
positioned. Position the nozzle, if used, facing into gas stream, or
the probe tip in the 50 mm (2 in.) centroidal area of the stack.
8.10.3 Be careful not to bump the probe tip into the stack wall
when removing or inserting the probe through the porthole; this
minimizes the chance of extracting deposited material.

[[Page 61879]]

8.10.4 When the probe is in position, block off the openings
around the probe and porthole to prevent unrepresentative dilution of
the gas stream.
8.10.5 Begin sampling at the start of the test run as defined in
Method 28, Section 8.8.1, start the sample pump, and adjust the sample
flow rate to between 0.003 and 0.014 m\3\/min (0.1 and 0.5 cfm). Adjust
the sample flow rate proportionally to the stack gas flow during the
test run according to the procedures outlined in Section 8. Maintain a
proportional sampling rate (within 10 percent of the desired value) and
a filter holder temperature no greater than 120 deg.C (248 deg.F).
8.10.6 During the test run, make periodic adjustments to keep the
temperature around the filter holder at the proper level. Add more ice
to the impinger box and, if necessary, salt to maintain a temperature
of less than 20 deg.C (68 deg.F) at the condenser/silica gel outlet.
8.10.7 If the pressure drop across the filter becomes too high,
making proportional sampling difficult to maintain, either filter may
be replaced during a sample run. It is recommended that another
complete filter assembly be used rather than attempting to change the
filter itself. Before a new filter assembly is installed, conduct a
leak-check (see Section 8.5.2). The total particulate weight shall
include the summation of all filter assembly catches. The total time
for changing sample train components shall not exceed 10 minutes. No
more than one component change is allowed for any test run.
8.10.8 At the end of the test run, turn off the coarse adjust
valve, remove the probe and nozzle from the stack, turn off the pump,
record the final dry gas meter reading, and conduct a post-test leak-
check, as outlined in Section 8.5.3.
8.11 Sample Recovery. Same as Method 5, Section 8.7, with the
exception of the following:
8.11.1 Blanks. The volume of the acetone blank may be about 50-ml,
rather than 200-ml; a 200-ml water blank shall also be saved for
analysis.
8.11.2 Samples.
8.11.2.1 Container Nos. 1 and 1A. Treat the two filters according
to the procedures outlined in Method 5, Section 8.7.6.1. The filters
may be stored either in a single container or in separate containers.
8.11.2.2 Container No. 2. Same as Method 5, Section 8.7.6.2,
except that the container should not be sealed until the impinger rinse
solution is added (see Section 8.10.2.4).
8.11.2.3 Container No. 3. Treat the impingers as follows: Measure
the liquid which is in the first three impingers to within 1-ml by
using a graduated cylinder or by weighing it to within 0.5 g by using a
balance (if one is available). Record the volume or weight of liquid
present. This information is required to calculate the moisture content
of the effluent gas. Transfer the water from the first, second, and
third impingers to a glass container. Tighten the lid on the sample
container so that water will not leak out.
8.11.2.4 Rinse impingers and graduated cylinder, if used, with
acetone three times or more. Avoid direct contact between the acetone
and any stopcock grease or collection of any stopcock grease in the
rinse solutions. Add these rinse solutions to sample Container No. 2.
8.11.2.5 Container No. 4. Same as Method 5, Section 8.7.6.3
8.12 Sample Transport. Whenever possible, containers should be
transferred in such a way that they remain upright at all times.

Note: Requirements for capping and transport of sample
containers are not applicable if sample recovery and analysis occur
in the same room.

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures.

------------------------------------------------------------------------
Quality control
Section measure Effect
------------------------------------------------------------------------
8.2........................... Sampling system Ensures that bias
bias check. introduced by
measurement system,
minus analyzer, is
no greater than 3
percent of span.
8.2........................... Analyzer zero and Ensures that bias
calibration introduced by drift
drift tests. in the measurement
system output during
the run is no
greater than 3
percent of span.
8.5, 10.1, 12.13.............. Sampling Ensures accurate
equipment leak- measurement of stack
check and gas flow rate,
calibration; sample volume.
proportional
sampling rate
verification.
10.1.......................... Analytical Ensure accurate and
balance precise measurement
calibration. of collected
particulate.
10.3.......................... Analyzer Ensures that bias
calibration introduced by
error check. analyzer calibration
error is no greater
than 2 percent of
span.
------------------------------------------------------------------------

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

10.0 Calibration and Standardization

Note: Maintain a laboratory record of all calibrations.

10.1 Volume Metering System, Temperature Sensors, Barometer, and
Analytical Balance. Same as Method 5G, Sections 10.2 through 10.5,
respectively.
10.2 SO2 Injection Rotameter. Calibrate the
SO2 injection rotameter system with a soap film flowmeter or
similar direct volume measuring device with an accuracy of 2 percent.
Operate the rotameter at a single reading for at least three
calibration runs for 10 minutes each. When three consecutive
calibration flow rates agree within 5 percent, average the three flow
rates, mark the rotameter at the calibrated setting, and use the
calibration flow rate as the SO2 injection flow rate during
the test run. Repeat the rotameter calibration before the first
certification test and semiannually thereafter.
10.3. Gas Analyzers. Same as Method 6C, Section 10.0.

11.0 Analytical Procedure

11.1 Record the data required on a sheet such as the one shown in
Figure 5H-4.
11.2 Handle each sample container as follows:
11.2.1 Container Nos. 1 and 1A. Treat the two filters according to
the procedures outlined in Method 5, Section 11.2.1.
11.2.2 Container No. 2. Same as Method 5, Section 11.2.2, except
that the beaker may be smaller than 250-ml.
11.2.3 Container No. 3. Note the level of liquid in the container
and confirm on the analysis sheet whether leakage occurred during
transport. If a noticeable amount of leakage has occurred, either void
the sample or use methods, subject to the approval of the
Administrator, to correct the final results. Determination of sample
leakage is not applicable if sample recovery and analysis occur in the
same room. Measure the liquid in this container either volumetrically
to within 1-ml or gravimetrically to within 0.5 g. Transfer the
contents to a 500-ml or larger separatory funnel. Rinse the container
with water, and add to the separatory

[[Page 61880]]

funnel. Add 25-ml of dichloromethane to the separatory funnel, stopper
and vigorously shake 1 minute, let separate and transfer the
dichloromethane (lower layer) into a tared beaker or evaporating dish.
Repeat twice more. It is necessary to rinse Container No. 3 with
dichloromethane. This rinse is added to the impinger extract container.
Transfer the remaining water from the separatory funnel to a tared
beaker or evaporating dish and evaporate to dryness at 104 deg.C (220
deg.F). Desiccate and weigh to a constant weight. Evaporate the
combined impinger water extracts at ambient temperature and pressure.
Desiccate and weigh to a constant weight. Report both results to the
nearest 0.1 mg.
11.2.4 Container No. 4. Weigh the spent silica gel (or silica gel
plus impinger) to the nearest 0.5 g using a balance.
11.2.5 Acetone Blank Container. Same as Method 5, Section 11.2.4,
except that the beaker may be smaller than 250 ml.
11.2.6 Dichloromethane Blank Container. Treat the same as the
acetone blank.
11.2.7 Water Blank Container. Transfer the water to a tared 250 ml
beaker and evaporate to dryness at 104 deg.C (220 deg.F). Desiccate
and weigh to a constant weight.

12.0 Data Analysis and Calculations

a = Sample flow rate adjustment factor.
BR = Dry wood burn rate, kg/hr (lb/hr), from Method 28, Section 8.3.
Bws = Water vapor in the gas stream, proportion by volume.
Cs = Concentration of particulate matter in stack gas, dry
basis, corrected to standard conditions, g/dscm (g/dscf).
E = Particulate emission rate, g/hr (lb/hr).
H = Average pressure differential across the orifice meter
(see Figure 5H-1), mm H2O (in. H2O).
La = Maximum acceptable leakage rate for either a post-test
leak-check or for a leak-check following a component change; equal to
0.00057 cmm (0.020 cfm) or 4 percent of the average sampling rate,
whichever is less.
L1 = Individual leakage rate observed during the leak-check
conducted before a component change, cmm (cfm).
Lp = Leakage rate observed during the post-test leak-check,
cmm (cfm).
mn = Total amount of particulate matter collected, mg.
Ma = Mass of residue of solvent after evaporation, mg.
NC = Grams of carbon/gram of dry fuel (lb/lb), equal to
0.0425.
NT = Total dry moles of exhaust gas/kg of dry wood burned,
g-moles/kg (lb-moles/lb).
PR = Percent of proportional sampling rate.
Pbar = Barometric pressure at the sampling site, mm Hg
(in.Hg).
Pstd = Standard absolute pressure, 760 mm Hg (29.92 in.Hg).
Qsd = Total gas flow rate, dscm/hr (dscf/hr).
S1 = Concentration measured at the SO2 analyzer
for the first 10-minute interval, ppm.
Si = Concentration measured at the SO2 analyzer
for the ``ith'' 10 minute interval, ppm.
Tm = Absolute average dry gas meter temperature (see Figure
5H-3), deg.K ( deg.R).
Tstd = Standard absolute temperature, 293 deg.K (528
deg.R).
Va = volume of solvent blank, ml.
Vaw = Volume of solvent used in wash, ml.
Vlc = Total volume of liquid collected in impingers and
silica gel (see Figure 5H-4), ml.
Vm = Volume of gas sample as measured by dry gas meter, dcm
(dcf).
Vm(std) = Volume of gas sample measured by the dry gas
meter, corrected to standard conditions, dscm (dscf).
Vmi(std) = Volume of gas sample measured by the dry gas
meter during the ``ith'' 10-minute interval, dscm (dscf).
Vw(std) = Volume of water vapor in the gas sample, corrected
to standard conditions, scm (scf).
Wa = Weight of residue in solvent wash, mg.
Y = Dry gas meter calibration factor.
YCO = Measured mole fraction of CO (dry), average from
Section 8.2, g/g-mole (lb/lb-mole).
YCO2 = Measured mole fraction of CO2 (dry),
average from Section 8.2, g/g-mole (lb/lb-mole).
YHC = Assumed mole fraction of HC (dry), g/g-mole (lb/lb-
mole); = 0.0088 for catalytic wood heaters; = 0.0132 for non-catalytic
wood heaters; = 0.0080 for pellet-fired wood heaters.
10 = Length of first sampling period, min.
13.6 = Specific gravity of mercury.
100 = Conversion to percent.
= Total sampling time, min.
1 = Sampling time interval, from the beginning of
a run until the first component change, min.
12.2 Average Dry Gas Meter Temperature and Average Orifice
Pressure Drop. See data sheet (Figure 5H-3).
12.3 Dry Gas Volume. Same as Method 5, Section 12.3.
12.4 Volume of Water Vapor.
[GRAPHIC] [TIFF OMITTED] TR17OC00.168

Where:

K2 = 0.001333 m3/ml for metric units.
K2 = 0.04707 ft3/ml for English units.

12.5 Moisture Content.
[GRAPHIC] [TIFF OMITTED] TR17OC00.169

12.6 Solvent Wash Blank.
[GRAPHIC] [TIFF OMITTED] TR17OC00.170

12.7 Total Particulate Weight. Determine the total particulate
catch from the sum of the weights obtained from containers 1, 2, 3, and
4 less the appropriate solvent blanks (see Figure 5H-4).

Note: Refer to Method 5, Section 8.5 to assist in calculation of
results involving two filter assemblies.

12.8 Particulate Concentration.

[GRAPHIC] [TIFF OMITTED] TR17OC00.171

12.9 Sample Flow Rate Adjustment.
[GRAPHIC] [TIFF OMITTED] TR17OC00.172

12.10 Carbon Balance for Total Moles of Exhaust Gas (dry)/kg of
Wood Burned in the Exhaust Gas.
[GRAPHIC] [TIFF OMITTED] TR17OC00.173

Where:

K3 = 1000 g/kg for metric units.
K3 = 1.0 lb/lb for English units.

Note: The NOX/SOX portion of the gas is
assumed to be negligible.

12.11 Total Stack Gas Flow Rate.
[GRAPHIC] [TIFF OMITTED] TR17OC00.174

Where:
K4 = 0.02406 dscm/g-mole for metric units.
K4 = 384.8 dscf/lb-mole for English units.
12.12 Particulate Emission Rate.
[GRAPHIC] [TIFF OMITTED] TR17OC00.175

[[Page 61881]]

12.13 Proportional Rate Variation. Calculate PR for each 10-minute
interval, i, of the test run.
[GRAPHIC] [TIFF OMITTED] TR17OC00.176

12.14 Acceptable Results. If no more than 15 percent of the PR
values for all the intervals fall outside the range 90 percent
PR 110 percent, and if no PR value for any
interval falls outside the range 75 PR 125
percent, the results are acceptable. If the PR values for the test runs
are judged to be unacceptable, report the test run emission results,
but do not include the test run results in calculating the weighted
average emission rate, and repeat the test.

13.0 Method Performance. [Reserved]

14.0 Pollution Prevention. [Reserved]

15.0 Waste Management. [Reserved]

16.0 References

Same as Method 5G, Section 17.0.
BILLING CODE 6560-50-P

[[Page 61882]]

17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.177

[[Page 61883]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.178

[[Page 61884]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.179

[[Page 61885]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.180

[[Page 61886]]

Method 6--Determination of Sulfur Dioxide Emissions From Stationary
Sources

1.0 Scope and Application

1.1 Analytes.

------------------------------------------------------------------------
Analyte CAS No. Sensitivity
------------------------------------------------------------------------
SO2............................... 7449-09-5 3.4 mg SO2/m3
(2.12 x 10)-7 lb/
ft3
------------------------------------------------------------------------

1.2 Applicability. This method applies to the measurement of
sulfur dioxide (SO2) 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

2.1 A gas sample is extracted from the sampling point in the
stack. The SO2 and the sulfur trioxide, including those
fractions in any sulfur acid mist, are separated. The SO2
fraction is measured by the barium-thorin titration method.

3.0 Definitions. [Reserved]

4.0 Interferences

4.1 Free Ammonia. Free ammonia interferes with this method by
reacting with SO2 to form particulate sulfite and by
reacting with the indicator. If free ammonia is present (this can be
determined by knowledge of the process and/or noticing white
particulate matter in the probe and isopropanol bubbler), alternative
methods, subject to the approval of the Administrator are required. One
approved alternative is listed in Reference 13 of Section 17.0.
4.2 Water-Soluble Cations and Fluorides. The cations and fluorides
are removed by a glass wool filter and an isopropanol bubbler;
therefore, they do not affect the SO2 analysis. When samples
are collected from a gas stream with high concentrations of metallic
fumes (i.e., very fine cation aerosols) a high-efficiency glass fiber
filter must be used in place of the glass wool plug (i.e., the one in
the probe) to remove the cation interferent.

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 to establish appropriate safety and health practices and
determine the applicability of regulatory limitations before performing
this test method.
5.2 Corrosive reagents. The following reagents are hazardous.
Personal protective equipment and safe procedures are useful in
preventing chemical splashes. If contact occurs, immediately flush with
copious amounts of water for at least 15 minutes. Remove clothing under
shower and decontaminate. Treat residual chemical burns as thermal
burns.
5.2.1 Hydrogen Peroxide (H2O2). Irritating
to eyes, skin, nose, and lungs. 30% H2O2 is a
strong oxidizing agent. Avoid contact with skin, eyes, and combustible
material. Wear gloves when handling.
5.2.2 Sodium Hydroxide (NaOH). Causes severe damage to eyes and
skin. Inhalation causes irritation to nose, throat, and lungs. Reacts
exothermically with limited amounts of water.
5.2.3 Sulfuric Acid (H2SO4). Rapidly
destructive to body tissue. Will cause third degree burns. Eye damage
may result in blindness. Inhalation may be fatal from spasm of the
larynx, usually within 30 minutes. May cause lung tissue damage with
edema. 1 mg/m3 for 8 hours will cause lung damage or, in
higher concentrations, death. Provide ventilation to limit inhalation.
Reacts violently with metals and organics.

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 is shown
in Figure 6-1. The sampling equipment described in Method 8 may be
substituted in place of the midget impinger equipment of Method 6.
However, the Method 8 train must be modified to include a heated filter
between the probe and isopropanol impinger, and the operation of the
sampling train and sample analysis must be at the flow rates and
solution volumes defined in Method 8. Alternatively, SO2 may
be determined simultaneously with particulate matter and moisture
determinations by either (1) replacing the water in a Method 5 impinger
system with a 3 percent H2O2 solution, or (2)
replacing the Method 5 water impinger system with a Method 8
isopropanol-filter-H2O2 system. The analysis for
SO2 must be consistent with the procedure of Method 8. The
Method 6 sampling train consists of the following components:
6.1.1.1 Probe. Borosilicate glass or stainless steel (other
materials of construction may be used, subject to the approval of the
Administrator), approximately 6 mm (0.25 in.) inside diameter, with a
heating system to prevent water condensation and a filter (either in-
stack or heated out-of-stack) to remove particulate matter, including
sulfuric acid mist. A plug of glass wool is a satisfactory filter.
6.1.1.2 Bubbler and Impingers. One midget bubbler with medium-
coarse glass frit and borosilicate or quartz glass wool packed in top
(see Figure 6-1) to prevent sulfuric acid mist carryover, and three 30-
ml midget impingers. The midget bubbler and midget impingers must be
connected in series with leak-free glass connectors. Silicone grease
may be used, if necessary, to prevent leakage. A midget impinger may be
used in place of the midget bubbler.

Note: Other collection absorbers and flow rates may be used,
subject to the approval of the Administrator, but the collection
efficiency must be shown to be at least 99 percent for each test run
and must be documented in the report. If the efficiency is found to
be acceptable after a series of three tests, further documentation
is not required. To conduct the efficiency test, an extra absorber
must be added and analyzed separately. This extra absorber must not
contain more than 1 percent of the total SO2.

6.1.1.3 Glass Wool. Borosilicate or quartz.
6.1.1.4 Stopcock Grease. Acetone-insoluble, heat-stable silicone
grease may be used, if necessary.
6.1.1.5 Temperature Sensor. Dial thermometer, or equivalent, to
measure temperature of gas leaving impinger train to within 1 deg.C (2
deg.F).
6.1.1.6 Drying Tube. Tube packed with 6- to 16- mesh indicating-
type silica gel, or equivalent, to dry the gas sample and to protect
the meter and pump. If silica gel is previously used, dry at 177 deg.C
(350 deg.F) for 2 hours. New silica gel may be used as received.
Alternatively, other types of desiccants

[[Page 61887]]

(equivalent or better) may be used, subject to the approval of the
Administrator.
6.1.1.7 Valve. Needle valve, to regulate sample gas flow rate.
6.1.1.8 Pump. Leak-free diaphragm pump, or equivalent, to pull gas
through the train. Install a small surge tank between the pump and rate
meter to negate the pulsation effect of the diaphragm pump on the rate
meter.
6.1.1.9 Rate Meter. Rotameter, or equivalent, capable of measuring
flow rate to within 2 percent of the selected flow rate of about 1
liter/min (0.035 cfm).
6.1.1.10 Volume Meter. Dry gas meter (DGM), sufficiently accurate
to measure the sample volume to within 2 percent, calibrated at the
selected flow rate and conditions actually encountered during sampling,
and equipped with a temperature sensor (dial thermometer, or
equivalent) capable of measuring temperature accurately to within 3
deg.C (5.4 deg.F). A critical orifice may be used in place of the DGM
specified in this section provided that it is selected, calibrated, and
used as specified in Section 16.0.
6.1.2 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg). See
the Note in Method 5, Section 6.1.2.
6.1.3 Vacuum Gauge and Rotameter. At least 760-mm Hg (30-in. Hg)
gauge and 0- to 40-ml/min rotameter, to be used for leak-check of the
sampling train.
6.2 Sample Recovery. The following items are needed for sample
recovery:
6.2.1 Wash Bottles. Two polyethylene or glass bottles, 500-ml.
6.2.2 Storage Bottles. Polyethylene bottles, 100-ml, to store
impinger samples (one per sample).
6.3 Sample Analysis. The following equipment is needed for sample
analysis:
6.3.1 Pipettes. Volumetric type, 5-ml, 20-ml (one needed per
sample), and 25-ml sizes.
6.3.2 Volumetric Flasks. 100-ml size (one per sample) and 1000-ml
size.
6.3.3 Burettes. 5- and 50-ml sizes.
6.3.4 Erlenmeyer Flasks. 250-ml size (one for each sample, blank,
and standard).
6.3.5 Dropping Bottle. 125-ml size, to add indicator.
6.3.6 Graduated Cylinder. 100-ml size.
6.3.7 Spectrophotometer. To measure absorbance at 352 nm.

7.0 Reagents and Standards

Note: Unless otherwise indicated, all reagents must conform to
the specifications established by the Committee on Analytical
Reagents of the American Chemical Society. Where such specifications
are not available, use the best available grade.

7.1 Sample Collection. The following reagents are required for
sample collection:
7.1.1 Water. Deionized distilled to conform to ASTM Specification
D 1193-77 or 91 Type 3 (incorporated by reference--see Sec. 60.17). The
KMnO4 test for oxidizable organic matter may be omitted when
high concentrations of organic matter are not expected to be present.
7.1.2 Isopropanol, 80 Percent by Volume. Mix 80 ml of isopropanol
with 20 ml of water.
7.1.2.1 Check each lot of isopropanol for peroxide impurities as
follows: Shake 10 ml of isopropanol with 10 ml of freshly prepared 10
percent potassium iodide solution. Prepare a blank by similarly
treating 10 ml of water. After 1 minute, read the absorbance at 352 nm
on a spectrophotometer using a 1-cm path length. If absorbance exceeds
0.1, reject alcohol for use.
7.1.2.2 Peroxides may be removed from isopropanol by redistilling
or by passage through a column of activated alumina; however, reagent
grade isopropanol with suitably low peroxide levels may be obtained
from commercial sources. Rejection of contaminated lots may, therefore,
be a more efficient procedure.
7.1.3 Hydrogen Peroxide (H2O2), 3 Percent by
Volume. Add 10 ml of 30 percent H2O2 to 90 ml of
water. Prepare fresh daily.
7.1.4 Potassium Iodide Solution, 10 Percent Weight by Volume (w/
v). Dissolve 10.0 g of KI in water, and dilute to 100 ml. Prepare when
needed.
7.2 Sample Recovery. The following reagents are required for
sample recovery:
7.2.1 Water. Same as in Section 7.1.1.
7.2.2 Isopropanol, 80 Percent by Volume. Same as in Section 7.1.2.
7.3 Sample Analysis. The following reagents and standards are
required for sample analysis:
7.3.1 Water. Same as in Section 7.1.1.
7.3.2 Isopropanol, 100 Percent.
7.3.3 Thorin Indicator. 1-(o-arsonophenylazo)-2-naphthol-3,6-
disulfonic acid, disodium salt, or equivalent. Dissolve 0.20 g in 100
ml of water.
7.3.4 Barium Standard Solution, 0.0100 N. Dissolve 1.95 g of
barium perchlorate trihydrate [Ba(ClO4)2
3H2O] in 200 ml water, and dilute to 1 liter with
isopropanol. Alternatively, 1.22 g of barium chloride dihydrate
[BaCl2 2H2O] may be used instead of the barium
perchlorate trihydrate. Standardize as in Section 10.5.
7.3.5 Sulfuric Acid Standard, 0.0100 N. Purchase or standardize to
0.0002 N against 0.0100 N NaOH which has previously been
standardized against potassium acid phthalate (primary standard grade).
7.3.6 Quality Assurance Audit Samples. When making compliance
determinations, audit samples, if available must be obtained from the
appropriate EPA Regional Office or from the responsible enforcement
authority and analyzed in conjunction with the field samples.

Note: The responsible enforcement authority should be notified
at least 30 days prior to the test date to allow sufficient time for
sample delivery.

8.0 Sample Collection, Preservation, Storage and Transport

8.1 Preparation of Sampling Train. Measure 15 ml of 80 percent
isopropanol into the midget bubbler and 15 ml of 3 percent
H2O2 into each of the first two midget impingers.
Leave the final midget impinger dry. Assemble the train as shown in
Figure 6-1. Adjust the probe heater to a temperature sufficient to
prevent water condensation. Place crushed ice and water around the
impingers.
8.2 Sampling Train Leak-Check Procedure. A leak-check prior to the
sampling run is recommended, but not required. A leak-check after the
sampling run is mandatory. The leak-check procedure is as follows:
8.2.1 Temporarily attach a suitable (e.g., 0- to 40- ml/min)
rotameter to the outlet of the DGM, and place a vacuum gauge at or near
the probe inlet. Plug the probe inlet, pull a vacuum of at least 250 mm
Hg (10 in. Hg), and note the flow rate as indicated by the rotameter. A
leakage rate in excess of 2 percent of the average sampling rate is not
acceptable.

Note: Carefully (i.e., slowly) release the probe inlet plug
before turning off the pump.

8.2.2 It is suggested (not mandatory) that the pump be leak-
checked separately, either prior to or after the sampling run. To leak-
check the pump, proceed as follows: Disconnect the drying tube from the
probe-impinger assembly. Place a vacuum gauge at the inlet to either
the drying tube or the pump, pull a vacuum of 250 mm Hg (10 in. Hg),
plug or pinch off the outlet of the flow meter, and then turn off the
pump. The vacuum should remain stable for at least 30 seconds.

[[Page 61888]]

If performed prior to the sampling run, the pump leak-check shall
precede the leak-check of the sampling train described immediately
above; if performed after the sampling run, the pump leak-check shall
follow the sampling train leak-check.
8.2.3 Other leak-check procedures may be used, subject to the
approval of the Administrator.
8.3 Sample Collection.
8.3.1 Record the initial DGM reading and barometric pressure. To
begin sampling, position the tip of the probe at the sampling point,
connect the probe to the bubbler, and start the pump. Adjust the sample
flow to a constant rate of approximately 1.0 liter/min as indicated by
the rate meter. Maintain this constant rate ( 10 percent)
during the entire sampling run.
8.3.2 Take readings (DGM volume, temperatures at DGM and at
impinger outlet, and rate meter flow rate) at least every 5 minutes.
Add more ice during the run to keep the temperature of the gases
leaving the last impinger at 20 deg.C (68 deg.F) or less.
8.3.3 At the conclusion of each run, turn off the pump, remove the
probe from the stack, and record the final readings. Conduct a leak-
check as described in Section 8.2. (This leak-check is mandatory.) If a
leak is detected, void the test run or use procedures acceptable to the
Administrator to adjust the sample volume for the leakage.
8.3.4 Drain the ice bath, and purge the remaining part of the
train by drawing clean ambient air through the system for 15 minutes at
the sampling rate. Clean ambient air can be provided by passing air
through a charcoal filter or through an extra midget impinger
containing 15 ml of 3 percent H2O2.
Alternatively, ambient air without purification may be used.
8.4 Sample Recovery. Disconnect the impingers after purging.
Discard the contents of the midget bubbler. Pour the contents of the
midget impingers into a leak-free polyethylene bottle for shipment.
Rinse the three midget impingers and the connecting tubes with water,
and add the rinse to the same storage container. Mark the fluid level.
Seal and identify the sample container.

9.0 Quality Control

------------------------------------------------------------------------
Quality control
Section measure Effect
------------------------------------------------------------------------
7.1.2.................... Isopropanol check.. Ensure acceptable level
of peroxide impurities
in isopropanol.
8.2, 10.1-10.4........... Sampling equipment Ensure accurate
leak-check and measurement of stack
calibration. gas flow rate, sample
volume.
10.5..................... Barium standard Ensure precision of
solution normality
standardization. determination.
11.2.3................... Replicate Ensure precision of
titrations. titration
determinations
11.3..................... Audit sample Evaluate analyst's
analysis. technique and standards
preparation.
------------------------------------------------------------------------

10.0 Calibration and Standardization

10.1 Volume Metering System.
10.1.1 Initial Calibration.
10.1.1.1 Before its initial use in the field, leak-check the
metering system (drying tube, needle valve, pump, rate meter, and DGM)
as follows: Place a vacuum gauge at the inlet to the drying tube and
pull a vacuum of 250 mm Hg (10 in. Hg). Plug or pinch off the outlet of
the flow meter, and then turn off the pump. The vacuum must remain
stable for at least 30 seconds. Carefully release the vacuum gauge
before releasing the flow meter end.
10.1.1.2 Remove the drying tube, and calibrate the metering system
(at the sampling flow rate specified by the method) as follows: Connect
an appropriately sized wet-test meter (e.g., 1 liter per revolution) to
the inlet of the needle valve. Make three independent calibration runs,
using at least five revolutions of the DGM per run. Calculate the
calibration factor Y (wet-test meter calibration volume divided by the
DGM volume, both volumes adjusted to the same reference temperature and
pressure) for each run, and average the results (Yi). If any
Y-value deviates by more than 2 percent from (Yi), the
metering system is unacceptable for use. If the metering system is
acceptable, use (Yi) as the calibration factor for
subsequent test runs.
10.1.2 Post-Test Calibration Check. After each field test series,
conduct a calibration check using the procedures outlined in Section
10.1.1.2, except that three or more revolutions of the DGM may be used,
and only two independent runs need be made. If the average of the two
post-test calibration factors does not deviate by more than 5 percent
from Yi, then Yi is accepted as the DGM
calibration factor (Y), which is used in Equation 6-1 to calculate
collected sample volume (see Section 12.2). If the deviation is more
than 5 percent, recalibrate the metering system as in Section 10.1.1,
and determine a post-test calibration factor (Yf). Compare
Yi and Yf; the smaller of the two factors is
accepted as the DGM calibration factor. If recalibration indicates that
the metering system is unacceptable for use, either void the test run
or use methods, subject to the approval of the Administrator, to
determine an acceptable value for the collected sample volume.
10.1.3 DGM 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 10.1.1.2, provided that it is calibrated
initially and recalibrated periodically according to the same
procedures outlined in Method 5, Section 10.3 with the following
exceptions: (a) the DGM is calibrated against a wet-test meter having a
capacity of 1 liter/rev (0.035 ft3/rev) or 3 liters/rev (0.1
ft3/rev) and having the capability of measuring volume to
within 1 percent; (b) the DGM is calibrated at 1 liter/min (0.035 cfm);
and (c) the meter box of the Method 6 sampling train is calibrated at
the same flow rate.
10.2 Temperature Sensors. Calibrate against mercury-in-glass
thermometers.
10.3 Rate Meter. The rate meter need not be calibrated, but should
be cleaned and maintained according to the manufacturer's instructions.
10.4 Barometer. Calibrate against a mercury barometer.
10.5 Barium Standard Solution. Standardize the barium perchlorate
or chloride solution against 25 ml of standard sulfuric acid to which
100 ml of 100 percent isopropanol has been added. Run duplicate
analyses. Calculate the normality using the average of duplicate
analyses where the titrations agree within 1 percent or 0.2 ml,
whichever is larger.

11.0 Analytical Procedure

11.1 Sample Loss Check. Note level of liquid in container and
confirm whether any sample was lost during shipment; note this finding
on the analytical data sheet. If a noticeable amount of leakage has
occurred, either void the sample or use methods, subject to the
approval of the Administrator, to correct the final results.
11.2 Sample Analysis.
11.2.1 Transfer the contents of the storage container to a 100-ml
volumetric flask, dilute to exactly 100 ml with water, and mix the
diluted sample.

[[Page 61889]]

11.2.2 Pipette a 20-ml aliquot of the diluted sample into a 250-ml
Erlenmeyer flask and add 80 ml of 100 percent isopropanol plus two to
four drops of thorin indicator. While stirring the solution, titrate to
a pink endpoint using 0.0100 N barium standard solution.
11.2.3 Repeat the procedures in Section 11.2.2, and average the
titration volumes. Run a blank with each series of samples. Replicate
titrations must agree within 1 percent or 0.2 ml, whichever is larger.

Note: Protect the 0.0100 N barium standard solution from
evaporation at all times.

11.3 Audit Sample Analysis.
11.3.1 When the method is used to analyze samples to demonstrate
compliance with a source emission regulation, an audit sample, if
available, must be analyzed.
11.3.2 Concurrently analyze the audit sample and the compliance
samples in the same manner to evaluate the technique of the analyst and
the standards preparation.
11.3.3 The same analyst, analytical reagents, and analytical
system must be used for the compliance samples and the audit sample. If
this condition is met, duplicate auditing of subsequent compliance
analyses for the same enforcement agency within a 30-day period is
waived. An audit sample set may not be used to validate different sets
of compliance samples under the jurisdiction of separate enforcement
agencies, unless prior arrangements have been made with both
enforcement agencies.
11.4 Audit Sample Results.
11.4.1 Calculate the audit sample concentrations and submit
results using the instructions provided with the audit samples.
11.4.2 Report the results of the audit samples and the compliance
determination samples along with their identification numbers, and the
analyst's name to the responsible enforcement authority. Include this
information with reports of any subsequent compliance analyses for the
same enforcement authority during the 30-day period.
11.4.3 The concentrations of the audit samples obtained by the
analyst must agree within 5 percent of the actual concentration. If the
5 percent specification is not met, reanalyze the compliance and audit
samples, and include initial and reanalysis values in the test report.
11.4.4 Failure to meet the 5-percent specification may require
retests until the audit problems are resolved. However, if the audit
results do not affect the compliance or noncompliance status of the
affected facility, the Administrator may waive the reanalysis
requirement, further audits, or retests and accept the results of the
compliance test. While steps are being taken to resolve audit analysis
problems, the Administrator may also choose to use the data to
determine the compliance or noncompliance status of the affected
facility.

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.

Ca = Actual concentration of SO2 in audit sample,
mg/dscm.
Cd = Determined concentration of SO2 in audit
sample, mg/dscm.
CSO2 = Concentration of SO2, dry basis, corrected
to standard conditions, mg/dscm (lb/dscf).
N = Normality of barium standard titrant, meq/ml.
Pbar = Barometric pressure, mm Hg (in. Hg).
Pstd = Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
RE = Relative error of QA audit sample analysis, percent
Tm = Average DGM absolute temperature, deg.K ( deg.R).
Tstd = Standard absolute temperature, 293 deg.K (528
deg.R).
Va = Volume of sample aliquot titrated, ml.
Vm = Dry gas volume as measured by the DGM, dcm (dcf).
Vm(std) = Dry gas volume measured by the DGM, corrected to
standard conditions, dscm (dscf).
Vsoln = Total volume of solution in which the SO2 sample is
contained, 100 ml.
Vt = Volume of barium standard titrant used for the sample
(average of replicate titration), ml.
Vtb = Volume of barium standard titrant used for the blank,
ml.
Y = DGM calibration factor.

12.2 Dry Sample Gas Volume, Corrected to Standard Conditions.
[GRAPHIC] [TIFF OMITTED] TR17OC00.181

Where:

K1 = 0.3855 deg.K/mm Hg for metric units,
K1 = 17.65 deg.R/in. Hg for English units.

12.3 SO2 Concentration.
[GRAPHIC] [TIFF OMITTED] TR17OC00.182

Where:

K2 = 32.03 mg SO2/meq for metric units,
K2 = 7.061 x 10-5 lb SO2/meq for
English units.

12.4 Relative Error for QA Audit Samples.
[GRAPHIC] [TIFF OMITTED] TR17OC00.183

13.0 Method Performance

13.1 Range. The minimum detectable limit of the method has been
determined to be 3.4 mg SO2/m3 (2.12 x
10-7 lb/ft3). Although no upper limit has been
established, tests have shown that concentrations as high as 80,000 mg/
m3 (0.005 lb/ft3) of SO2 can be
collected efficiently at a rate of 1.0 liter/min (0.035 cfm) for 20
minutes in two midget impingers, each containing 15 ml of 3 percent
H2O2. Based on theoretical calculations, the
upper concentration limit in a 20 liter (0.7 ft3) sample is
about 93,300 mg/m3 (0.00583 lb/ft3).

14.0 Pollution Prevention. [Reserved]

15.0 Waste Management. [Reserved]

16.0 Alternative Procedures

16.1 Nomenclature. Same as Section 12.1, with the following
additions:

Bwa = Water vapor in ambient air, proportion by volume.
Ma = Molecular weight of the ambient air saturated at
impinger temperature, g/g-mole (lb/lb-mole).
Ms = Molecular weight of the sample gas saturated at
impinger temperature, g/g-mole (lb/lb-mole).

[[Page 61890]]

Pc = Inlet vacuum reading obtained during the calibration
run, mm Hg (in. Hg).
Psr = Inlet vacuum reading obtained during the sampling run,
mm Hg (in. Hg).
Qstd = Volumetric flow rate through critical orifice, scm/
min (scf/min).
Qstd = Average flow rate of pre-test and post-test
calibration runs, scm/min (scf/min).
Tamb = Ambient absolute temperature of air, deg.K ( deg.R).
Vsb = Volume of gas as measured by the soap bubble meter,
m\3\ (ft\3\).

Vsb(std) = Volume of gas as measured by the soap bubble
meter, corrected to standard conditions, scm (scf).
= Soap bubble travel time, min.
s = Time, min.

16.2 Critical Orifices for Volume and Rate Measurements. A
critical orifice may be used in place of the DGM specified in Section
6.1.1.10, provided that it is selected, calibrated, and used as
follows:
16.2.1 Preparation of Sampling Train. Assemble the sampling train
as shown in Figure 6-2. The rate meter and surge tank are optional but
are recommended in order to detect changes in the flow rate.

Note: The critical orifices can be adapted to a Method 6 type
sampling train as follows: Insert sleeve type, serum bottle stoppers
into two reducing unions. Insert the needle into the stoppers as
shown in Figure 6-3.

16.2.2 Selection of Critical Orifices.
16.2.2.1 The procedure that follows describes the use of
hypodermic needles and stainless steel needle tubings, which have been
found suitable for use as critical orifices. Other materials and
critical orifice designs may be used provided the orifices act as true
critical orifices, (i.e., a critical vacuum can be obtained) as
described in this section. Select a critical orifice that is sized to
operate at the desired flow rate. The needle sizes and tubing lengths
shown in Table 6-1 give the following approximate flow rates.
16.2.2.2 Determine the suitability and the appropriate operating
vacuum of the critical orifice as follows: If applicable, temporarily
attach a rate meter and surge tank to the outlet of the sampling train,
if said equipment is not present (see Section 16.2.1). Turn on the pump
and adjust the valve to give an outlet vacuum reading corresponding to
about half of the atmospheric pressure. Observe the rate meter reading.
Slowly increase the vacuum until a stable reading is obtained on the
rate meter. Record the critical vacuum, which is the outlet vacuum when
the rate meter first reaches a stable value. Orifices that do not reach
a critical value must not be used.
16.2.3 Field Procedures.
16.2.3.1 Leak-Check Procedure. A leak-check before the sampling
run is recommended, but not required. The leak-check procedure is as
follows: Temporarily attach a suitable (e.g., 0-40 ml/min) rotameter
and surge tank, or a soap bubble meter and surge tank to the outlet of
the pump. Plug the probe inlet, pull an outlet vacuum of at least 250
mm Hg (10 in. Hg), and note the flow rate as indicated by the rotameter
or bubble meter. A leakage rate in excess of 2 percent of the average
sampling rate (Qstd) is not acceptable. Carefully release
the probe inlet plug before turning off the pump.
16.2.3.2 Moisture Determination. At the sampling location, prior
to testing, determine the percent moisture of the ambient air using the
wet and dry bulb temperatures or, if appropriate, a relative humidity
meter.
16.2.3.3 Critical Orifice Calibration. At the sampling location,
prior to testing, calibrate the entire sampling train (i.e., determine
the flow rate of the sampling train when operated at critical
conditions). Attach a 500-ml soap bubble meter to the inlet of the
probe, and operate the sampling train at an outlet vacuum of 25 to 50
mm Hg (1 to 2 in. Hg) above the critical vacuum. Record the information
listed in Figure 6-4. Calculate the standard volume of air measured by
the soap bubble meter and the volumetric flow rate using the equations
below:
[GRAPHIC] [TIFF OMITTED] TR17OC00.184

[GRAPHIC] [TIFF OMITTED] TR17OC00.185

16.2.3.4 Sampling.
16.2.3.4.1 Operate the sampling train for sample collection at the
same vacuum used during the calibration run. Start the watch and pump
simultaneously. Take readings (temperature, rate meter, inlet vacuum,
and outlet vacuum) at least every 5 minutes. At the end of the sampling
run, stop the watch and pump simultaneously.
16.2.3.4.2 Conduct a post-test calibration run using the
calibration procedure outlined in Section 16.2.3.3. If the
Qstd obtained before and after the test differ by more than
5 percent, void the test run; if not, calculate the volume of the gas
measured with the critical orifice using Equation 6-6 as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.186

16.2.3.4.3 If the percent difference between the molecular weight
of the ambient air at saturated conditions and the sample gas is more
that 3 percent, then the molecular weight of the gas
sample must be considered in the calculations using the following
equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.187

Note: A post-test leak-check is not necessary because the post-
test calibration run results will indicate whether there is any
leakage.

16.2.3.4.4 Drain the ice bath, and purge the sampling train using
the procedure described in Section 8.3.4.
16.3 Elimination of Ammonia Interference. The following
alternative procedures must be used in addition to those specified in
the method when

[[Page 61891]]

sampling at sources having ammonia emissions.
16.3.1 Sampling. The probe shall be maintained at 275 deg.C (527
deg.F) and equipped with a high-efficiency in-stack filter (glass
fiber) to remove particulate matter. The filter material shall be
unreactive to SO2. Whatman 934AH (formerly Reeve Angel
934AH) filters treated as described in Reference 10 in Section 17.0 of
Method 5 is an example of a filter that has been shown to work. Where
alkaline particulate matter and condensed moisture are present in the
gas stream, the filter shall be heated above the moisture dew point but
below 225 deg.C (437 deg.F).
16.3.2 Sample Recovery. Recover the sample according to Section
8.4 except for discarding the contents of the midget bubbler. Add the
bubbler contents, including the rinsings of the bubbler with water, to
a separate polyethylene bottle from the rest of the sample. Under
normal testing conditions where sulfur trioxide will not be present
significantly, the tester may opt to delete the midget bubbler from the
sampling train. If an approximation of the sulfur trioxide
concentration is desired, transfer the contents of the midget bubbler
to a separate polyethylene bottle.
16.3.3 Sample Analysis. Follow the procedures in Sections 11.1 and
11.2, except add 0.5 ml of 0.1 N HCl to the Erlenmeyer flask and mix
before adding the indicator. The following analysis procedure may be
used for an approximation of the sulfur trioxide concentration. The
accuracy of the calculated concentration will depend upon the ammonia
to SO2 ratio and the level of oxygen present in the gas
stream. A fraction of the SO2 will be counted as sulfur
trioxide as the ammonia to SO2 ratio and the sample oxygen
content increases. Generally, when this ratio is 1 or less and the
oxygen content is in the range of 5 percent, less than 10 percent of
the SO2 will be counted as sulfur trioxide. Analyze the
peroxide and isopropanol sample portions separately. Analyze the
peroxide portion as described above. Sulfur trioxide is determined by
difference using sequential titration of the isopropanol portion of the
sample. Transfer the contents of the isopropanol storage container to a
100-ml volumetric flask, and dilute to exactly 100 ml with water.
Pipette a 20-ml aliquot of this solution into a 250-ml Erlenmeyer
flask, add 0.5 ml of 0.1 N HCl, 80 ml of 100 percent isopropanol, and
two to four drops of thorin indicator. Titrate to a pink endpoint using
0.0100 N barium perchlorate. Repeat and average the titration volumes
that agree within 1 percent or 0.2 ml, whichever is larger. Use this
volume in Equation 6-2 to determine the sulfur trioxide concentration.
From the flask containing the remainder of the isopropanol sample,
determine the fraction of SO2 collected in the bubbler by
pipetting 20-ml aliquots into 250-ml Erlenmeyer flasks. Add 5 ml of 3
percent H2O2, 100 ml of 100 percent isopropanol,
and two to four drips of thorin indicator, and titrate as before. From
this titration volume, subtract the titrant volume determined for
sulfur trioxide, and add the titrant volume determined for the peroxide
portion. This final volume constitutes Vt, the volume of
barium perchlorate used for the SO2 sample.

17.0 References

1. Atmospheric Emissions from Sulfuric Acid Manufacturing
Processes. U.S. DHEW, PHS, Division of Air Pollution. Public Health
Service Publication No. 999-AP-13. Cincinnati, OH. 1965.
2. Corbett, P.F. The Determination of SO2 and
SO3 in Flue Gases. Journal of the Institute of Fuel.
24:237-243. 1961.
3. Matty, R.E., and E.K. Diehl. Measuring Flue-Gas
SO2 and SO3. Power. 101:94-97. November 1957.
4. Patton, W.F., and J.A. Brink, Jr. New Equipment and
Techniques for Sampling Chemical Process Gases. J. Air Pollution
Control Association. 13:162. 1963.
5. Rom, J.J. Maintenance, Calibration, and Operation of
Isokinetic Source Sampling Equipment. Office of Air Programs, U.S.
Environmental Protection Agency. Research Triangle Park, NC. APTD-
0576. March 1972.
6. Hamil, H.F., and D.E. Camann. Collaborative Study of Method
for the Determination of Sulfur Dioxide Emissions from Stationary
Sources (Fossil-Fuel Fired Steam Generators). U.S. Environmental
Protection Agency, Research Triangle Park, NC. EPA-650/4-74-024.
December 1973.
7. Annual Book of ASTM Standards. Part 31; Water, Atmospheric
Analysis. American Society for Testing and Materials. Philadelphia,
PA. 1974. pp. 40-42.
8. Knoll, J.E., and M.R. Midgett. The Application of EPA Method
6 to High Sulfur Dioxide Concentrations. U.S. Environmental
Protection Agency. Research Triangle Park, NC. EPA-600/4-76-038.
July 1976.
9. Westlin, P.R., and R.T. Shigehara. Procedure for Calibrating
and Using Dry Gas Volume Meters as Calibration Standards. Source
Evaluation Society Newsletter. 3(1):17-30. February 1978.
10. Yu, K.K. Evaluation of Moisture Effect on Dry Gas Meter
Calibration. Source Evaluation Society Newsletter. 5(1):24-28.
February 1980.
11. Lodge, J.P., Jr., et al. The Use of Hypodermic Needles as
Critical Orifices in Air Sampling. J. Air Pollution Control
Association. 16:197-200. 1966.
12. Shigehara, R.T., and C.B. Sorrell. Using Critical Orifices
as Method 5 CalibrationStandards. Source Evaluation Society
Newsletter. 10:4-15. August 1985.
13. Curtis, F., Analysis of Method 6 Samples in the Presence of
Ammonia. Source Evaluation Society Newsletter. 13(1):9-15 February
1988.

18.0 Tables, Diagrams, Flowcharts and Validation Data

Table 6-1.--Approximate Flow Rates for Various Needle Sizes
------------------------------------------------------------------------
Needle
Needle size (gauge) length Flow rate
(cm) (ml/min)
------------------------------------------------------------------------
21............................................ 7.6 1,100
22............................................ 2.9 1,000
22............................................ 3.8 900
23............................................ 3.8 500
23............................................ 5.1 450
24............................................ 3.2 400
------------------------------------------------------------------------

BILLING CODE 6560-50-P

[[Page 61892]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.188

[[Continued on page 61893]]

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

[[pp. 61843-61892]] Amendments for Testing and Monitoring Provisions

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