Section

[Code of Federal Regulations]
[Title 40, Volume 7]
[Revised as of July 1, 2005]
From the U.S. Government Printing Office via GPO Access
[CITE: 40CFR60.A3]

[Page 160]

Appendix A-3 to Part 60--Test Methods 4 through 5I

Method 4--Determination of moisture content in stack gases
Method 5--Determination of particulate matter emissions from stationary
sources
Method 5A--Determination of particulate matter emissions from the
asphalt processing and asphalt roofing industry
Method 5B--Determination of nonsulfuric acid particulate matter
emissions from stationary sources
Method 5C [Reserved]
Method 5D--Determination of particulate matter emissions from positive
pressure fabric filters
Method 5E--Determination of particulate matter emissions from the wool
fiberglass insulation manufacturing industry
Method 5F--Determination of nonsulfate particulate matter emissions from
stationary sources
Method 5G--Determination of particulate matter emissions from wood
heaters (dilution tunnel sampling location)
Method 5H--Determination of particulate emissions from wood heaters from
a stack location
Method 5I--Determination of Low Level Particulate Matter Emissions From
Stationary Sources
The test methods in this appendix are referred to in Sec. 60.8
(Performance Tests) and Sec. 60.11 (Compliance With Standards and
Maintenance Requirements) of 40 CFR part 60, subpart A (General
Provisions). Specific uses of these test methods are described in the
standards of performance contained in the subparts, beginning with
Subpart D.
Within each standard of performance, a section title ``Test Methods
and Procedures'' is provided to: (1) Identify the test methods to be
used as reference methods to the facility subject to the respective
standard and (2) identify any special instructions or conditions to be
followed when applying a method to the respective facility. Such
instructions (for example, establish sampling rates, volumes, or
temperatures) are to be used either in addition to, or as a substitute
for procedures in a test method. Similarly, for sources subject to
emission monitoring requirements, specific instructions pertaining to
any use of a test method as a reference method are provided in the
subpart or in Appendix B.
Inclusion of methods in this appendix is not intended as an
endorsement or denial of their applicability to sources that are not
subject to standards of performance. The methods are potentially
applicable to other sources; however, applicability should be confirmed
by careful and appropriate evaluation of the conditions prevalent at
such sources.
The approach followed in the formulation of the test methods
involves specifications for equipment, procedures, and performance. In
concept, a performance specification approach would be preferable in all
methods because this allows the greatest flexibility to the user. In
practice, however, this approach is impractical in most cases because
performance specifications cannot be established. Most of the methods
described herein, therefore, involve specific equipment specifications
and procedures, and only a few methods in this appendix rely on
performance criteria.
Minor changes in the test methods should not necessarily affect the
validity of the results and it is recognized that alternative and
equivalent methods exist. Section 60.8 provides authority for the
Administrator to specify or approve (1) equivalent methods, (2)
alternative methods, and (3) minor changes in the methodology of the
test methods. It should be clearly understood that unless otherwise
identified all such methods and changes must have prior approval of the
Administrator. An owner employing such methods or deviations from the
test methods without obtaining prior approval does so at the risk of
subsequent disapproval and retesting with approved methods.
Within the test methods, certain specific equipment or procedures
are recognized as being acceptable or potentially acceptable and are
specifically identified in the methods. The items identified as
acceptable options may be used without approval but

must be identified in the test report. The potentially approvable
options are cited as ``subject to the approval of the Administrator'' or
as ``or equivalent.'' Such potentially approvable techniques or
alternatives may be used at the discretion of the owner without prior
approval. However, detailed descriptions for applying these potentially
approvable techniques or alternatives are not provided in the test
methods. Also, the potentially approvable options are not necessarily
acceptable in all applications. Therefore, an owner electing to use such
potentially approvable techniques or alternatives is responsible for:
(1) assuring that the techniques or alternatives are in fact applicable
and are properly executed; (2) including a written description of the
alternative method in the test report (the written method must be clear
and must be capable of being performed without additional instruction,
and the degree of detail should be similar to the detail contained in
the test methods); and (3) providing any rationale or supporting data
necessary to show the validity of the alternative in the particular
application. Failure to meet these requirements can result in the
Administrator's disapproval of the alternative.

Method 4--Determination of Moisture Content in Stack Gases

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

1.0 Scope and Application

1.1 Analytes.

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

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

2.0 Summary of Method

2.1 A gas sample is extracted at a constant rate from the source;
moisture is removed from the sample stream and determined either
volumetrically or gravimetrically.
2.2 The method contains two possible procedures: a reference method
and an approximation method.
2.2.1 The reference method is used for accurate determinations of
moisture content (such as are needed to calculate emission data). The
approximation method, provides estimates of percent moisture to aid in
setting isokinetic sampling rates prior to a pollutant emission
measurement run. The approximation method described herein is only a
suggested approach; alternative means for approximating the moisture
content (e.g., drying tubes, wet bulb-dry bulb techniques, condensation
techniques, stoichiometric calculations, previous experience, etc.) are
also acceptable.
2.2.2 The reference method is often conducted simultaneously with a
pollutant emission measurement run. When it is, calculation of percent
isokinetic, pollutant emission rate, etc., for the run shall be based
upon the results of the reference method or its equivalent. These
calculations shall not be based upon the results of the approximation
method, unless the approximation method is shown, to the satisfaction of
the Administrator, to be capable of yielding results within one percent
H2O of the reference method.

3.0 Definitions [Reserved]

4.0 Interferences

4.1 The moisture content of saturated gas streams or streams that
contain water droplets, as measured by the reference method, may be
positively biased. Therefore, when these conditions exist or are
suspected, a second determination of the moisture content shall be made
simultaneously with the reference method, as follows: Assume that the
gas stream is saturated. Attach a temperature sensor [capable of
measuring to 1 [deg]C (2 [deg]F)] to the reference
method probe. Measure the stack gas temperature at each traverse point
(see Section 8.1.1.1) during the reference method traverse, and
calculate the average stack gas temperature. Next, determine the
moisture percentage, either by: (1) Using a psychrometric chart and
making appropriate corrections if the stack pressure is different from
that of the chart, or (2) using saturation vapor pressure tables. In
cases where the psychrometric chart or the saturation vapor pressure
tables are not applicable (based on evaluation of the process),
alternative methods, subject to the approval of the Administrator, shall
be used.

5.0 Safety

[[Page 161]]

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

6.0 Equipment and Supplies

6.1 Reference Method. A schematic of the sampling train used in this
reference method is shown in Figure 4-1.
6.1.1 Probe. Stainless steel or glass tubing, sufficiently heated to
prevent water condensation, and equipped with a filter, either in-stack
(e.g., a plug of glass wool inserted into the end of the probe) or
heated out-of-stack (e.g., as described in Method 5), to remove
particulate matter. When stack conditions permit, other metals or
plastic tubing may be used for the probe, subject to the approval of the
Administrator.
6.1.2 Condenser. Same as Method 5, Section 6.1.1.8.
6.1.3 Cooling System. An ice bath container, crushed ice, and water
(or equivalent), to aid in condensing moisture.
6.1.4 Metering System. Same as in Method 5, Section 6.1.1.9, except
do not use sampling systems designed for flow rates higher than 0.0283
m\3\/min (1.0 cfm). Other metering systems, capable of maintaining a
constant sampling rate to within 10 percent and determining sample gas
volume to within 2 percent, may be used, subject to the approval of the
Administrator.
6.1.5 Barometer and Graduated Cylinder and/or Balance. Same as
Method 5, Sections 6.1.2 and 6.2.5, respectively.
6.2. Approximation Method. A schematic of the sampling train used in
this approximation method is shown in Figure 4-2.
6.2.1 Probe. Same as Section 6.1.1.
6.2.2 Condenser. Two midget impingers, each with 30-ml capacity, or
equivalent.
6.2.3 Cooling System. Ice bath container, crushed ice, and water, to
aid in condensing moisture in impingers.
6.2.4 Drying Tube. Tube packed with new or regenerated 6- to 16-mesh
indicating-type silica gel (or equivalent desiccant), to dry the sample
gas and to protect the meter and pump.
6.2.5 Valve. Needle valve, to regulate the sample gas flow rate.
6.2.6 Pump. Leak-free, diaphragm type, or equivalent, to pull the
gas sample through the train.
6.2.7 Volume Meter. Dry gas meter, sufficiently accurate to measure
the sample volume to within 2 percent, and calibrated over the range of
flow rates and conditions actually encountered during sampling.
6.2.8 Rate Meter. Rotameter, or equivalent, to measure the flow
range from 0 to 3 liters/min (0 to 0.11 cfm).
6.2.9 Graduated Cylinder. 25-ml.
6.2.10 Barometer. Same as Method 5, Section 6.1.2.
6.2.11 Vacuum Gauge. At least 760-mm (30-in.) Hg gauge, to be used
for the sampling leak check.

7.0 Reagents and Standards [Reserved]

8.0 Sample Collection, Preservation, Transport, and Storage

8.1 Reference Method. The following procedure is intended for a
condenser system (such as the impinger system described in Section
6.1.1.8 of Method 5) incorporating volumetric analysis to measure the
condensed moisture, and silica gel and gravimetric analysis to measure
the moisture leaving the condenser.
8.1.1 Preliminary Determinations.
8.1.1.1 Unless otherwise specified by the Administrator, a minimum
of eight traverse points shall be used for circular stacks having
diameters less than 0.61 m (24 in.), a minimum of nine points shall be
used for rectangular stacks having equivalent diameters less than 0.61 m
(24 in.), and a minimum of twelve traverse points shall be used in all
other cases. The traverse points shall be located according to Method 1.
The use of fewer points is subject to the approval of the Administrator.
Select a suitable probe and probe length such that all traverse points
can be sampled. Consider sampling from opposite sides of the stack (four
total sampling ports) for large stacks, to permit use of shorter probe
lengths. Mark the probe with heat resistant tape or by some other method
to denote the proper distance into the stack or duct for each sampling
point.
8.1.1.2 Select a total sampling time such that a minimum total gas
volume of 0.60 scm (21 scf) will be collected, at a rate no greater than
0.021 m\3\/min (0.75 cfm). When both moisture content and pollutant
emission rate are to be determined, the moisture determination shall be
simultaneous with, and for the same total length of time as, the
pollutant emission rate run, unless otherwise specified in an applicable
subpart of the standards.
8.1.2 Preparation of Sampling Train.
8.1.2.1 Place known volumes of water in the first two impingers;
alternatively, transfer water into the first two impingers and record
the weight of each impinger (plus water) to the nearest 0.5 g. Weigh and
record the weight of the silica gel to the nearest 0.5 g, and transfer
the silica gel to the fourth impinger; alternatively, the silica gel may
first be transferred to the impinger, and the weight of the silica gel
plus impinger recorded.
8.1.2.2 Set up the sampling train as shown in Figure 4-1. Turn on
the probe heater and (if applicable) the filter heating system to
temperatures of approximately 120 [deg]C (248 [deg]F), to prevent water
condensation ahead of the condenser. Allow time for the temperatures to
stabilize. Place crushed ice and water in the ice bath container.

[[Page 162]]

8.1.3 Leak Check Procedures. It is recommended, but not required,
that the volume metering system and sampling train be leak-checked as
follows:
8.1.3.1 Metering System. Same as Method 5, Section 8.4.1.
8.1.3.2 Sampling Train. Disconnect the probe from the first impinger
or (if applicable) from the filter holder. Plug the inlet to the first
impinger (or filter holder), and pull a 380 mm (15 in.) Hg vacuum. A
lower vacuum may be used, provided that it is not exceeded during the
test. A leakage rate in excess of 4 percent of the average sampling rate
or 0.00057 m\3\/min (0.020 cfm), whichever is less, is unacceptable.
Following the leak check, reconnect the probe to the sampling train.
8.1.4 Sampling Train Operation. During the sampling run, maintain a
sampling rate within 10 percent of constant rate, or as specified by the
Administrator. For each run, record the data required on a data sheet
similar to that shown in Figure 4-3. Be sure to record the dry gas meter
reading at the beginning and end of each sampling time increment and
whenever sampling is halted. Take other appropriate readings at each
sample point at least once during each time increment.

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

8.1.4.1 To begin sampling, position the probe tip at the first
traverse point. Immediately start the pump, and adjust the flow to the
desired rate. Traverse the cross section, sampling at each traverse
point for an equal length of time. Add more ice and, if necessary, salt
to maintain a temperature of less than 20 [deg]C (68 [deg]F) at the
silica gel outlet.
8.1.4.2 After collecting the sample, disconnect the probe from the
first impinger (or from the filter holder), and conduct a leak check
(mandatory) of the sampling train as described in Section 8.1.3.2.
Record the leak rate. If the leakage rate exceeds the allowable rate,
either reject the test results or correct the sample volume as in
Section 12.3 of Method 5.
8.2 Approximation Method.

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

8.2.1 Place exactly 5 ml water in each impinger. Leak check the
sampling train as follows: Temporarily insert a vacuum gauge at or near
the probe inlet. Then, plug the probe inlet and pull a vacuum of at
least 250 mm (10 in.) Hg. Note the time rate of change of the dry gas
meter dial; alternatively, a rotameter (0 to 40 ml/min) may be
temporarily attached to the dry gas meter outlet to determine the
leakage rate. A leak rate not in excess of 2 percent of the average
sampling rate is acceptable.

Note: Release the probe inlet plug slowly before turning off the
pump.

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

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures.

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

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

10.0 Calibration and Standardization

Note: Maintain a laboratory log of all calibrations.

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

11.0 Analytical Procedure

11.1 Reference Method. Measure the volume of the moisture condensed
in each of the impingers to the nearest ml. Alternatively, if the
impingers were weighed prior to sampling, weigh the impingers after
sampling

[[Page 163]]

and record the difference in weight to the nearest 0.5 g. Determine the
increase in weight of the silica gel (or silica gel plus impinger) to
the nearest 0.5 g. Record this information (see example data sheet,
Figure 4-5), and calculate the moisture content, as described in Section
12.0.
11.2 Approximation Method. Combine the contents of the two
impingers, and measure the volume to the nearest 0.5 ml.

12.0 Data Analysis and Calculations

Carry out the following calculations, retaining at least one extra
significant figure beyond that of the acquired data. Round off figures
after final calculation.
12.1 Reference Method.
12.1.1 Nomenclature.
Bws=Proportion of water vapor, by volume, in the gas stream.
Mw=Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb-
mole).
Pm=Absolute pressure (for this method, same as barometric
pressure) at the dry gas meter, mm Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
R=Ideal gas constant, 0.06236 (mm Hg)(m\3\)/(g-mole)([deg]K) for metric
units and 21.85 (in. Hg)(ft\3\)/(lb-mole)([deg]R) for English units.
Tm=Absolute temperature at meter, [deg]K ([deg]R).
Tstd=Standard absolute temperature, 293 [deg]K (528 [deg]R).
Vf=Final volume of condenser water, ml.
Vi=Initial volume, if any, of condenser water, ml.
Vm=Dry gas volume measured by dry gas meter, dcm (dcf).
Vm(std)=Dry gas volume measured by the dry gas meter,
corrected to standard conditions, dscm (dscf).
Vwc(std)=Volume of water vapor condensed, corrected to
standard conditions, scm (scf).
Vwsg(std)=Volume of water vapor collected in silica gel,
corrected to standard conditions, scm (scf).
Wf=Final weight of silica gel or silica gel plus impinger, g.
Wi=Initial weight of silica gel or silica gel plus impinger,
g.
Y=Dry gas meter calibration factor.
[Delta]Vm=Incremental dry gas volume measured by dry gas
meter at each traverse point, dcm (dcf).
[rho]w=Density of water, 0.9982 g/ml (0.002201 lb/ml).

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

Where:

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

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

Where:

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

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

Where:

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

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

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

12.1.6 Verification of Constant Sampling Rate. For each time
increment, determine the [Delta]Vm. Calculate the average. If
the value for any time increment differs from the average by more than
10 percent, reject the results, and repeat the run.
12.1.7 In saturated or moisture droplet-laden gas streams, two
calculations of the moisture content of the stack gas shall be made, one
using a value based upon the saturated conditions (see Section 4.1), and
another based upon the results of the impinger analysis. The lower of
these two values of Bws shall be considered correct.

[[Page 164]]

12.2 Approximation Method. The approximation method presented is
designed to estimate the moisture in the stack gas; therefore, other
data, which are only necessary for accurate moisture determinations, are
not collected. The following equations adequately estimate the moisture
content for the purpose of determining isokinetic sampling rate
settings.
12.2.1 Nomenclature.
Bwm=Approximate proportion by volume of water vapor in the
gas stream leaving the second impinger, 0.025.
Bws=Water vapor in the gas stream, proportion by volume.
Mw=Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb-
mole).
Pm=Absolute pressure (for this method, same as barometric
pressure) at the dry gas meter, mm Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
R=Ideal gas constant, 0.06236 [(mm Hg)(m\3\)]/[(g-mole)(K)] for metric
units and 21.85 [(in. Hg)(ft\3\)]/[(lb-mole)([deg]R)] for English units.
Tm=Absolute temperature at meter, [deg]K ([deg]R).
Tstd=Standard absolute temperature, 293 [deg]K (528 [deg]R).
Vf=Final volume of impinger contents, ml.
Vi=Initial volume of impinger contents, ml.
Vm=Dry gas volume measured by dry gas meter, dcm (dcf).
Vm(std)=Dry gas volume measured by dry gas meter, corrected
to standard conditions, dscm (dscf).
Vwc(std)=Volume of water vapor condensed, corrected to
standard conditions, scm (scf).
Y=Dry gas meter calibration factor.
[rho]w=Density of water, 0.09982 g/ml (0.002201 lb/ml).

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

Where:

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

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

Where:

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

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

13.0 Method Performance [Reserved]

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 Alternative Procedures

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

17.0 References

1. Air Pollution Engineering Manual (Second Edition). Danielson,
J.A. (ed.). U.S. Environmental Protection Agency, Office of Air Quality
Planning and Standards. Research Triangle Park, NC. Publication No. AP-
40. 1973.
2. Devorkin, Howard, et al. Air Pollution Source Testing Manual. Air
Pollution Control District, Los Angeles, CA. November 1963.
3. Methods for Determination of Velocity, Volume, Dust and Mist
Content of Gases. Western Precipitation Division of Joy Manufacturing
Co. Los Angeles, CA. Bulletin WP-50. 1968.

18.0 Tables, Diagrams, Flowcharts, and Validation Data

[[Page 165]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.105

[[Page 166]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.106

[[Page 167]]

Plant___________________________________________________________________
Location________________________________________________________________
Operator________________________________________________________________
Date____________________________________________________________________
Run No._________________________________________________________________
Ambient temperature_____________________________________________________
Barometric pressure_____________________________________________________
Probe Length____________________________________________________________

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

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

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

[[Page 168]]

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

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

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

[[Page 169]]

Location________________________________________________________________
Test____________________________________________________________________
Date____________________________________________________________________
Operator________________________________________________________________
Barometric pressure_____________________________________________________
Comments:_______________________________________________________________
________________________________________________________________________

Figure 4-3. Moisture Determination--Reference Method

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

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

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

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

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

Figure 4-5. Analytical Data--Reference Method

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

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

1.0 Scope and Application

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

2.0 Summary of Method

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

3.0 Definitions [Reserved]

4.0 Interferences [Reserved]

5.0 Safety

6.0 Equipment and Supplies

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

[[Page 170]]

models of this train are also available. For changes from APTD-0581 and
for allowable modifications of the train shown in Figure 5-1, see the
following subsections.

Note: The operating and maintenance procedures for the sampling
train are described in APTD-0576 (Reference 3 in Section 17.0). Since
correct usage is important in obtaining valid results, all users should
read APTD-0576 and adopt the operating and maintenance procedures
outlined in it, unless otherwise specified herein.

6.1.1.1 Probe Nozzle. Stainless steel (316) or glass with a sharp,
tapered leading edge. The angle of taper shall be <=30[deg], and the
taper shall be on the outside to preserve a constant internal diameter.
The probe nozzle shall be of the button-hook or elbow design, unless
otherwise specified by the Administrator. If made of stainless steel,
the nozzle shall be constructed from seamless tubing. Other materials of
construction may be used, subject to the approval of the Administrator.
A range of nozzle sizes suitable for isokinetic sampling should be
available. Typical nozzle sizes range from 0.32 to 1.27 cm (\1/8\ to \1/
2\ in) inside diameter (ID) in increments of 0.16 cm (\1/16\ in). Larger
nozzles sizes are also available if higher volume sampling trains are
used. Each nozzle shall be calibrated, according to the procedures
outlined in Section 10.1.
6.1.1.2 Probe Liner. Borosilicate or quartz glass tubing with a
heating system capable of maintaining a probe gas temperature during
sampling of 120 14 [deg]C (248 25 [deg]F), or such other temperature as specified by an
applicable subpart of the standards or as approved by the Administrator
for a particular application. Since the actual temperature at the outlet
of the probe is not usually monitored during sampling, probes
constructed according to APTD-0581 and utilizing the calibration curves
of APTD-0576 (or calibrated according to the procedure outlined in APTD-
0576) will be considered acceptable. Either borosilicate or quartz glass
probe liners may be used for stack temperatures up to about 480 [deg]C
(900 [deg]F); quartz glass liners shall be used for temperatures between
480 and 900 [deg]C (900 and 1,650 [deg]F). Both types of liners may be
used at higher temperatures than specified for short periods of time,
subject to the approval of the Administrator. The softening temperature
for borosilicate glass is 820 [deg]C (1500 [deg]F), and for quartz glass
it is 1500 [deg]C (2700 [deg]F). Whenever practical, every effort should
be made to use borosilicate or quartz glass probe liners. Alternatively,
metal liners (e.g., 316 stainless steel, Incoloy 825 or other corrosion
resistant metals) made of seamless tubing may be used, subject to the
approval of the Administrator.
6.1.1.3 Pitot Tube. Type S, as described in Section 6.1 of Method 2,
or other device approved by the Administrator. The pitot tube shall be
attached to the probe (as shown in Figure 5-1) to allow constant
monitoring of the stack gas velocity. The impact (high pressure) opening
plane of the pitot tube shall be even with or above the nozzle entry
plane (see Method 2, Figure 2-7) during sampling. The Type S pitot tube
assembly shall have a known coefficient, determined as outlined in
Section 10.0 of Method 2.
6.1.1.4 Differential Pressure Gauge. Inclined manometer or
equivalent device (two), as described in Section 6.2 of Method 2. One
manometer shall be used for velocity head ([Delta]p) readings, and the
other, for orifice differential pressure readings.
6.1.1.5 Filter Holder. Borosilicate glass, with a glass frit filter
support and a silicone rubber gasket. Other materials of construction
(e.g., stainless steel, Teflon, or Viton) may be used, subject to the
approval of the Administrator. The holder design shall provide a
positive seal against leakage from the outside or around the filter. The
holder shall be attached immediately at the outlet of the probe (or
cyclone, if used).
6.1.1.6 Filter Heating System. Any heating system capable of
maintaining a temperature around the filter holder of 120 14 [deg]C (248 25 [deg]F) during
sampling, or such other temperature as specified by an applicable
subpart of the standards or approved by the Administrator for a
particular application.
6.1.1.7 Temperature Sensor. A temperature sensor capable of
measuring temperature to within 3 [deg]C (5.4
[deg]F) shall be installed so that the sensing tip of the temperature
sensor is in direct contact with the sample gas, and the temperature
around the filter holder can be regulated and monitored during sampling.
6.1.1.8 Condenser. The following system shall be used to determine
the stack gas moisture content: Four impingers connected in series with
leak-free ground glass fittings or any similar leak-free
noncontaminating fittings. The first, third, and fourth impingers shall
be of the Greenburg-Smith design, modified by replacing the tip with a
1.3 cm (\1/2\ in.) ID glass tube extending to about 1.3 cm (\1/2\ in.)
from the bottom of the flask. The second impinger shall be of the
Greenburg-Smith design with the standard tip. Modifications (e.g., using
flexible connections between the impingers, using materials other than
glass, or using flexible vacuum lines to connect the filter holder to
the condenser) may be used, subject to the approval of the
Administrator. The first and second impingers shall contain known
quantities of water (Section 8.3.1), the third shall be empty, and the
fourth shall contain a known weight of silica gel, or equivalent
desiccant. A temperature sensor, capable of measuring temperature to
within 1 [deg]C (2 [deg]F) shall be placed at the outlet of the fourth
impinger for monitoring purposes. Alternatively, any system that cools
the sample

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gas stream and allows measurement of the water condensed and moisture
leaving the condenser, each to within 1 ml or 1 g may be used, subject
to the approval of the Administrator. An acceptable technique involves
the measurement of condensed water either gravimetrically or
volumetrically and the determination of the moisture leaving the
condenser by: (1) monitoring the temperature and pressure at the exit of
the condenser and using Dalton's law of partial pressures; or (2)
passing the sample gas stream through a tared silica gel (or equivalent
desiccant) trap with exit gases kept below 20 [deg]C (68 [deg]F) and
determining the weight gain. If means other than silica gel are used to
determine the amount of moisture leaving the condenser, it is
recommended that silica gel (or equivalent) still be used between the
condenser system and pump to prevent moisture condensation in the pump
and metering devices and to avoid the need to make corrections for
moisture in the metered volume.

Note: If a determination of the PM collected in the impingers is
desired in addition to moisture content, the impinger system described
above shall be used, without modification. Individual States or control
agencies requiring this information shall be contacted as to the sample
recovery and analysis of the impinger contents.

6.1.1.9 Metering System. Vacuum gauge, leak-free pump, temperature
sensors capable of measuring temperature to within 3 [deg]C (5.4
[deg]F), dry gas meter (DGM) capable of measuring volume to within 2
percent, and related equipment, as shown in Figure 5-1. Other metering
systems capable of maintaining sampling rates within 10 percent of
isokinetic and of determining sample volumes to within 2 percent may be
used, subject to the approval of the Administrator. When the metering
system is used in conjunction with a pitot tube, the system shall allow
periodic checks of isokinetic rates.
6.1.1.10 Sampling trains utilizing metering systems designed for
higher flow rates than that described in APTD-0581 or APTD-0576 may be
used provided that the specifications of this method are met.
6.1.2 Barometer. Mercury, aneroid, or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in.).

Note: The barometric pressure reading may be obtained from a nearby
National Weather Service station. In this case, the station value (which
is the absolute barometric pressure) shall be requested and an
adjustment for elevation differences between the weather station and
sampling point shall be made at a rate of minus 2.5 mm Hg (0.1 in.) per
30 m (100 ft) elevation increase or plus 2.5 mm Hg (0.1 in) per 30 m
(100 ft) elevation decrease.

6.1.3 Gas Density Determination Equipment. Temperature sensor and
pressure gauge, as described in Sections 6.3 and 6.4 of Method 2, and
gas analyzer, if necessary, as described in Method 3. The temperature
sensor shall, preferably, be permanently attached to the pitot tube or
sampling probe in a fixed configuration, such that the tip of the sensor
extends beyond the leading edge of the probe sheath and does not touch
any metal. Alternatively, the sensor may be attached just prior to use
in the field. Note, however, that if the temperature sensor is attached
in the field, the sensor must be placed in an interference-free
arrangement with respect to the Type S pitot tube openings (see Method
2, Figure 2-4). As a second alternative, if a difference of not more
than 1 percent in the average velocity measurement is to be introduced,
the temperature sensor need not be attached to the probe or pitot tube.
(This alternative is subject to the approval of the Administrator.)
6.2 Sample Recovery. The following items are required for sample
recovery:
6.2.1 Probe-Liner and Probe-Nozzle Brushes. Nylon bristle brushes
with stainless steel wire handles. The probe brush shall have extensions
(at least as long as the probe) constructed of stainless steel, Nylon,
Teflon, or similarly inert material. The brushes shall be properly sized
and shaped to brush out the probe liner and nozzle.
6.2.2 Wash Bottles. Two Glass wash bottles are recommended.
Alternatively, polyethylene wash bottles may be used. It is recommended
that acetone not be stored in polyethylene bottles for longer than a
month.
6.2.3 Glass Sample Storage Containers. Chemically resistant,
borosilicate glass bottles, for acetone washes, 500 ml or 1000 ml. Screw
cap liners shall either be rubber-backed Teflon or shall be constructed
so as to be leak-free and resistant to chemical attack by acetone.
(Narrow mouth glass bottles have been found to be less prone to
leakage.) Alternatively, polyethylene bottles may be used.
6.2.4 Petri Dishes. For filter samples; glass or polyethylene,
unless otherwise specified by the Administrator.
6.2.5 Graduated Cylinder and/or Balance. To measure condensed water
to within 1 ml or 0.5 g. Graduated cylinders shall have subdivisions no
greater than 2 ml.
6.2.6 Plastic Storage Containers. Air-tight containers to store
silica gel.
6.2.7 Funnel and Rubber Policeman. To aid in transfer of silica gel
to container; not necessary if silica gel is weighed in the field.
6.2.8 Funnel. Glass or polyethylene, to aid in sample recovery.
6.3 Sample Analysis. The following equipment is required for sample
analysis:
6.3.1 Glass Weighing Dishes.
6.3.2 Desiccator.

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6.3.3 Analytical Balance. To measure to within 0.1 mg.
6.3.4 Balance. To measure to within 0.5 g.
6.3.5 Beakers. 250 ml.
6.3.6 Hygrometer. To measure the relative humidity of the laboratory
environment.
6.3.7 Temperature Sensor. To measure the temperature of the
laboratory environment.

7.0 Reagents and Standards

7.1 Sample Collection. The following reagents are required for
sample collection:
7.1.1 Filters. Glass fiber filters, without organic binder,
exhibiting at least 99.95 percent efficiency (<0.05 percent penetration)
on 0.3 micron dioctyl phthalate smoke particles. The filter efficiency
test shall be conducted in accordance with ASTM Method D 2986-71, 78, or
95a (incorporated by reference--see Sec. 60.17). Test data from the
supplier's quality control program are sufficient for this purpose. In
sources containing SO2 or SO3, the filter material
must be of a type that is unreactive to SO2 or
SO3. Reference 10 in Section 17.0 may be used to select the
appropriate filter.
7.1.2 Silica Gel. Indicating type, 6 to 16 mesh. If previously used,
dry at 175 [deg]C (350 [deg]F) for 2 hours. New silica gel may be used
as received. Alternatively, other types of desiccants (equivalent or
better) may be used, subject to the approval of the Administrator.
7.1.3 Water. When analysis of the material caught in the impingers
is required, deionized distilled water (to conform to ASTM D 1193-77 or
91 Type 3 (incorporated by reference--see Sec. 60.17)) shall be used.
Run blanks prior to field use to eliminate a high blank on test samples.
7.1.4 Crushed Ice.
7.1.5 Stopcock Grease. Acetone-insoluble, heat-stable silicone
grease. This is not necessary if screw-on connectors with Teflon
sleeves, or similar, are used. Alternatively, other types of stopcock
grease may be used, subject to the approval of the Administrator.
7.2 Sample Recovery. Acetone, reagent grade, <=0.001 percent
residue, in glass bottles, is required. Acetone from metal containers
generally has a high residue blank and should not be used. Sometimes,
suppliers transfer acetone to glass bottles from metal containers; thus,
acetone blanks shall be run prior to field use and only acetone with low
blank values (<=0.001 percent) shall be used. In no case shall a blank
value of greater than 0.001 percent of the weight of acetone used be
subtracted from the sample weight.
7.3 Sample Analysis. The following reagents are required for sample
analysis:
7.3.1 Acetone. Same as in Section 7.2.
7.3.2 Desiccant. Anhydrous calcium sulfate, indicating type.
Alternatively, other types of desiccants may be used, subject to the
approval of the Administrator.

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Pretest Preparation. It is suggested that sampling equipment be
maintained according to the procedures described in APTD-0576.
8.1.1 Place 200 to 300 g of silica gel in each of several air-tight
containers. Weigh each container, including silica gel, to the nearest
0.5 g, and record this weight. As an alternative, the silica gel need
not be preweighed, but may be weighed directly in its impinger or
sampling holder just prior to train assembly.
8.1.2 Check filters visually against light for irregularities,
flaws, or pinhole leaks. Label filters of the proper diameter on the
back side near the edge using numbering machine ink. As an alternative,
label the shipping containers (glass or polyethylene petri dishes), and
keep each filter in its identified container at all times except during
sampling.
8.1.3 Desiccate the filters at 20 5.6 [deg]C
(68 10 [deg]F) and ambient pressure for at least
24 hours. Weigh each filter (or filter and shipping container) at
intervals of at least 6 hours to a constant weight (i.e., <=0.5 mg
change from previous weighing). Record results to the nearest 0.1 mg.
During each weighing, the period for which the filter is exposed to the
laboratory atmosphere shall be less than 2 minutes. Alternatively
(unless otherwise specified by the Administrator), the filters may be
oven dried at 105 [deg]C (220 [deg]F) for 2 to 3 hours, desiccated for 2
hours, and weighed. Procedures other than those described, which account
for relative humidity effects, may be used, subject to the approval of
the Administrator.
8.2 Preliminary Determinations.
8.2.1 Select the sampling site and the minimum number of sampling
points according to Method 1 or as specified by the Administrator.
Determine the stack pressure, temperature, and the range of velocity
heads using Method 2; it is recommended that a leak check of the pitot
lines (see Method 2, Section 8.1) be performed. Determine the moisture
content using Approximation Method 4 or its alternatives for the purpose
of making isokinetic sampling rate settings. Determine the stack gas dry
molecular weight, as described in Method 2, Section 8.6; if integrated
Method 3 sampling is used for molecular weight determination, the
integrated bag sample shall be taken simultaneously with, and for the
same total length of time as, the particulate sample run.
8.2.2 Select a nozzle size based on the range of velocity heads,
such that it is not necessary to change the nozzle size in order to
maintain isokinetic sampling rates. During the run, do not change the
nozzle size. Ensure that the proper differential pressure gauge is
chosen for the range of velocity

[[Page 173]]

heads encountered (see Section 8.3 of Method 2).
8.2.3 Select a suitable probe liner and probe length such that all
traverse points can be sampled. For large stacks, consider sampling from
opposite sides of the stack to reduce the required probe length.
8.2.4 Select a total sampling time greater than or equal to the
minimum total sampling time specified in the test procedures for the
specific industry such that (l) the sampling time per point is not less
than 2 minutes (or some greater time interval as specified by the
Administrator), and (2) the sample volume taken (corrected to standard
conditions) will exceed the required minimum total gas sample volume.
The latter is based on an approximate average sampling rate.
8.2.5 The sampling time at each point shall be the same. It is
recommended that the number of minutes sampled at each point be an
integer or an integer plus one-half minute, in order to avoid
timekeeping errors.
8.2.6 In some circumstances (e.g., batch cycles) it may be necessary
to sample for shorter times at the traverse points and to obtain smaller
gas sample volumes. In these cases, the Administrator's approval must
first be obtained.
8.3 Preparation of Sampling Train.
8.3.1 During preparation and assembly of the sampling train, keep
all openings where contamination can occur covered until just prior to
assembly or until sampling is about to begin. Place 100 ml of water in
each of the first two impingers, leave the third impinger empty, and
transfer approximately 200 to 300 g of preweighed silica gel from its
container to the fourth impinger. More silica gel may be used, but care
should be taken to ensure that it is not entrained and carried out from
the impinger during sampling. Place the container in a clean place for
later use in the sample recovery. Alternatively, the weight of the
silica gel plus impinger may be determined to the nearest 0.5 g and
recorded.
8.3.2 Using a tweezer or clean disposable surgical gloves, place a
labeled (identified) and weighed filter in the filter holder. Be sure
that the filter is properly centered and the gasket properly placed so
as to prevent the sample gas stream from circumventing the filter. Check
the filter for tears after assembly is completed.
8.3.3 When glass probe liners are used, install the selected nozzle
using a Viton A O-ring when stack temperatures are less than 260 [deg]C
(500 [deg]F) or a heat-resistant string gasket when temperatures are
higher. See APTD-0576 for details. Other connecting systems using either
316 stainless steel or Teflon ferrules may be used. When metal liners
are used, install the nozzle as discussed above or by a leak-free direct
mechanical connection. Mark the probe with heat resistant tape or by
some other method to denote the proper distance into the stack or duct
for each sampling point.
8.3.4 Set up the train as shown in Figure 5-1, using (if necessary)
a very light coat of silicone grease on all ground glass joints,
greasing only the outer portion (see APTD-0576) to avoid the possibility
of contamination by the silicone grease. Subject to the approval of the
Administrator, a glass cyclone may be used between the probe and filter
holder when the total particulate catch is expected to exceed 100 mg or
when water droplets are present in the stack gas.
8.3.5 Place crushed ice around the impingers.
8.4 Leak-Check Procedures.
8.4.1 Leak Check of Metering System Shown in Figure 5-1. That
portion of the sampling train from the pump to the orifice meter should
be leak-checked prior to initial use and after each shipment. Leakage
after the pump will result in less volume being recorded than is
actually sampled. The following procedure is suggested (see Figure 5-2):
Close the main valve on the meter box. Insert a one-hole rubber stopper
with rubber tubing attached into the orifice exhaust pipe. Disconnect
and vent the low side of the orifice manometer. Close off the low side
orifice tap. Pressurize the system to 13 to 18 cm (5 to 7 in.) water
column by blowing into the rubber tubing. Pinch off the tubing, and
observe the manometer for one minute. A loss of pressure on the
manometer indicates a leak in the meter box; leaks, if present, must be
corrected.
8.4.2 Pretest Leak Check. A pretest leak check of the sampling train
is recommended, but not required. If the pretest leak check is
conducted, the following procedure should be used.
8.4.2.1 After the sampling train has been assembled, turn on and set
the filter and probe heating systems to the desired operating
temperatures. Allow time for the temperatures to stabilize. If a Viton A
O-ring or other leak-free connection is used in assembling the probe
nozzle to the probe liner, leak-check the train at the sampling site by
plugging the nozzle and pulling a 380 mm (15 in.) Hg vacuum.

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

8.4.2.2 If a heat-resistant string is used, do not connect the probe
to the train during the leak check. Instead, leak-check the train by
first plugging the inlet to the filter holder (cyclone, if applicable)
and pulling a 380 mm (15 in.) Hg vacuum (see Note in Section 8.4.2.1).
Then connect the probe to the train, and leak-check at approximately 25
mm (1 in.) Hg vacuum; alternatively, the probe may be leak-checked with
the rest of the sampling train, in one step, at 380 mm (15 in.) Hg
vacuum. Leakage rates in excess of 4 percent

[[Page 174]]

of the average sampling rate or 0.00057 m\3\/min (0.020 cfm), whichever
is less, are unacceptable.
8.4.2.3 The following leak-check instructions for the sampling train
described in APTD-0576 and APTD-0581 may be helpful. Start the pump with
the bypass valve fully open and the coarse adjust valve completely
closed. Partially open the coarse adjust valve, and slowly close the
bypass valve until the desired vacuum is reached. Do not reverse the
direction of the bypass valve, as this will cause water to back up into
the filter holder. If the desired vacuum is exceeded, either leak-check
at this higher vacuum, or end the leak check and start over.
8.4.2.4 When the leak check is completed, first slowly remove the
plug from the inlet to the probe, filter holder, or cyclone (if
applicable), and immediately turn off the vacuum pump. This prevents the
water in the impingers from being forced backward into the filter holder
and the silica gel from being entrained backward into the third
impinger.
8.4.3 Leak Checks During Sample Run. If, during the sampling run, a
component (e.g., filter assembly or impinger) change becomes necessary,
a leak check shall be conducted immediately before the change is made.
The leak check shall be done according to the procedure outlined in
Section 8.4.2 above, except that it shall be done at a vacuum equal to
or greater than the maximum value recorded up to that point in the test.
If the leakage rate is found to be no greater than 0.00057
m³/min (0.020 cfm) or 4 percent of the average sampling rate
(whichever is less), the results are acceptable, and no correction will
need to be applied to the total volume of dry gas metered; if, however,
a higher leakage rate is obtained, either record the leakage rate and
plan to correct the sample volume as shown in Section 12.3 of this
method, or void the sample run.

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

8.4.4 Post-Test Leak Check. A leak check of the sampling train is
mandatory at the conclusion of each sampling run. The leak check shall
be performed in accordance with the procedures outlined in Section
8.4.2, except that it shall be conducted at a vacuum equal to or greater
than the maximum value reached during the sampling run. If the leakage
rate is found to be no greater than 0.00057 m³ min (0.020
cfm) or 4 percent of the average sampling rate (whichever is less), the
results are acceptable, and no correction need be applied to the total
volume of dry gas metered. If, however, a higher leakage rate is
obtained, either record the leakage rate and correct the sample volume
as shown in Section 12.3 of this method, or void the sampling run.
8.5 Sampling Train Operation. During the sampling run, maintain an
isokinetic sampling rate (within 10 percent of true isokinetic unless
otherwise specified by the Administrator) and a temperature around the
filter of 120 14 [deg]C (248 25 [deg]F), or such other temperature as specified by an
applicable subpart of the standards or approved by the Administrator.
8.5.1 For each run, record the data required on a data sheet such as
the one shown in Figure 5-3. Be sure to record the initial DGM reading.
Record the DGM readings at the beginning and end of each sampling time
increment, when changes in flow rates are made, before and after each
leak check, and when sampling is halted. Take other readings indicated
by Figure 5-3 at least once at each sample point during each time
increment and additional readings when significant changes (20 percent
variation in velocity head readings) necessitate additional adjustments
in flow rate. Level and zero the manometer. Because the manometer level
and zero may drift due to vibrations and temperature changes, make
periodic checks during the traverse.
8.5.2 Clean the portholes prior to the test run to minimize the
chance of collecting deposited material. To begin sampling, verify that
the filter and probe heating systems are up to temperature, remove the
nozzle cap, verify that the pitot tube and probe are properly
positioned. Position the nozzle at the first traverse point with the tip
pointing directly into the gas stream. Immediately start the pump, and
adjust the flow to isokinetic conditions. Nomographs are available which
aid in the rapid adjustment of the isokinetic sampling rate without
excessive computations. These nomographs are designed for use when the
Type S pitot tube coefficient (Cp) is 0.85 0.02, and the stack gas equivalent density [dry
molecular weight (Md)] is equal to 29 4. APTD-0576 details the procedure for using the
nomographs. If Cp and Md are outside the above
stated ranges, do not use the nomographs unless appropriate steps (see
Reference 7 in Section 17.0) are taken to compensate for the deviations.
8.5.3 When the stack is under significant negative pressure (i.e.,
height of impinger stem), take care to close the coarse adjust valve
before inserting the probe into the stack to prevent water from backing
into the filter holder. If necessary, the pump may be turned on with the
coarse adjust valve closed.
8.5.4 When the probe is in position, block off the openings around
the probe and porthole to prevent unrepresentative dilution of the gas
stream.
8.5.5 Traverse the stack cross-section, as required by Method 1 or
as specified by the Administrator, being careful not to bump the probe
nozzle into the stack walls when sampling near the walls or when
removing or

[[Page 175]]

inserting the probe through the portholes; this minimizes the chance of
extracting deposited material.
8.5.6 During the test run, make periodic adjustments to keep the
temperature around the filter holder at the proper level; add more ice
and, if necessary, salt to maintain a temperature of less than 20 [deg]C
(68 [deg]F) at the condenser/silica gel outlet. Also, periodically check
the level and zero of the manometer.
8.5.7 If the pressure drop across the filter becomes too high,
making isokinetic sampling difficult to maintain, the filter may be
replaced in the midst of the sample run. It is recommended that another
complete filter assembly be used rather than attempting to change the
filter itself. Before a new filter assembly is installed, conduct a leak
check (see Section 8.4.3). The total PM weight shall include the
summation of the filter assembly catches.
8.5.8 A single train shall be used for the entire sample run, except
in cases where simultaneous sampling is required in two or more separate
ducts or at two or more different locations within the same duct, or in
cases where equipment failure necessitates a change of trains. In all
other situations, the use of two or more trains will be subject to the
approval of the Administrator.

Note: When two or more trains are used, separate analyses of the
front-half and (if applicable) impinger catches from each train shall be
performed, unless identical nozzle sizes were used on all trains, in
which case, the front-half catches from the individual trains may be
combined (as may the impinger catches) and one analysis of front-half
catch and one analysis of impinger catch may be performed. Consult with
the Administrator for details concerning the calculation of results when
two or more trains are used.

8.5.9 At the end of the sample run, close the coarse adjust valve,
remove the probe and nozzle from the stack, turn off the pump, record
the final DGM meter reading, and conduct a post-test leak check, as
outlined in Section 8.4.4. Also, leak-check the pitot lines as described
in Method 2, Section 8.1. The lines must pass this leak check, in order
to validate the velocity head data.
8.6 Calculation of Percent Isokinetic. Calculate percent isokinetic
(see Calculations, Section 12.11) to determine whether the run was valid
or another test run should be made. If there was difficulty in
maintaining isokinetic rates because of source conditions, consult with
the Administrator for possible variance on the isokinetic rates.
8.7 Sample Recovery.
8.7.1 Proper cleanup procedure begins as soon as the probe is
removed from the stack at the end of the sampling period. Allow the
probe to cool.
8.7.2 When the probe can be safely handled, wipe off all external PM
near the tip of the probe nozzle, and place a cap over it to prevent
losing or gaining PM. Do not cap off the probe tip tightly while the
sampling train is cooling down. This would create a vacuum in the filter
holder, thereby drawing water from the impingers into the filter holder.
8.7.3 Before moving the sample train to the cleanup site, remove the
probe from the sample train, wipe off the silicone grease, and cap the
open outlet of the probe. Be careful not to lose any condensate that
might be present. Wipe off the silicone grease from the filter inlet
where the probe was fastened, and cap it. Remove the umbilical cord from
the last impinger, and cap the impinger. If a flexible line is used
between the first impinger or condenser and the filter holder,
disconnect the line at the filter holder, and let any condensed water or
liquid drain into the impingers or condenser. After wiping off the
silicone grease, cap off the filter holder outlet and impinger inlet.
Either ground-glass stoppers, plastic caps, or serum caps may be used to
close these openings.
8.7.4 Transfer the probe and filter-impinger assembly to the cleanup
area. This area should be clean and protected from the wind so that the
chances of contaminating or losing the sample will be minimized.
8.7.5 Save a portion of the acetone used for cleanup as a blank.
Take 200 ml of this acetone directly from the wash bottle being used,
and place it in a glass sample container labeled ``acetone blank.''
8.7.6 Inspect the train prior to and during disassembly, and note
any abnormal conditions. Treat the samples as follows:
8.7.6.1 Container No. 1. Carefully remove the filter from the filter
holder, and place it in its identified petri dish container. Use a pair
of tweezers and/or clean disposable surgical gloves to handle the
filter. If it is necessary to fold the filter, do so such that the PM
cake is inside the fold. Using a dry Nylon bristle brush and/or a sharp-
edged blade, carefully transfer to the petri dish any PM and/or filter
fibers that adhere to the filter holder gasket. Seal the container.
8.7.6.2 Container No. 2. Taking care to see that dust on the outside
of the probe or other exterior surfaces does not get into the sample,
quantitatively recover PM or any condensate from the probe nozzle, probe
fitting, probe liner, and front half of the filter holder by washing
these components with acetone and placing the wash in a glass container.
Deionized distilled water may be used instead of acetone when approved
by the Administrator and shall be used when specified by the
Administrator. In these cases, save a water blank, and follow the
Administrator's directions on analysis. Perform the acetone rinse as
follows:

[[Page 176]]

8.7.6.2.1 Carefully remove the probe nozzle. Clean the inside
surface by rinsing with acetone from a wash bottle and brushing with a
Nylon bristle brush. Brush until the acetone rinse shows no visible
particles, after which make a final rinse of the inside surface with
acetone.
8.7.6.2.2 Brush and rinse the inside parts of the fitting with
acetone in a similar way until no visible particles remain.
8.7.6.2.3 Rinse the probe liner with acetone by tilting and rotating
the probe while squirting acetone into its upper end so that all inside
surfaces will be wetted with acetone. Let the acetone drain from the
lower end into the sample container. A funnel (glass or polyethylene)
may be used to aid in transferring liquid washes to the container.
Follow the acetone rinse with a probe brush. Hold the probe in an
inclined position, squirt acetone into the upper end as the probe brush
is being pushed with a twisting action through the probe; hold a sample
container underneath the lower end of the probe, and catch any acetone
and particulate matter that is brushed from the probe. Run the brush
through the probe three times or more until no visible PM is carried out
with the acetone or until none remains in the probe liner on visual
inspection. With stainless steel or other metal probes, run the brush
through in the above prescribed manner at least six times since metal
probes have small crevices in which particulate matter can be entrapped.
Rinse the brush with acetone, and quantitatively collect these washings
in the sample container. After the brushing, make a final acetone rinse
of the probe.
8.7.6.2.4 It is recommended that two people clean the probe to
minimize sample losses. Between sampling runs, keep brushes clean and
protected from contamination.
8.7.6.2.5 After ensuring that all joints have been wiped clean of
silicone grease, clean the inside of the front half of the filter holder
by rubbing the surfaces with a Nylon bristle brush and rinsing with
acetone. Rinse each surface three times or more if needed to remove
visible particulate. Make a final rinse of the brush and filter holder.
Carefully rinse out the glass cyclone, also (if applicable). After all
acetone washings and particulate matter have been collected in the
sample container, tighten the lid on the sample container so that
acetone will not leak out when it is shipped to the laboratory. Mark the
height of the fluid level to allow determination of whether leakage
occurred during transport. Label the container to identify clearly its
contents.
8.7.6.3 Container No. 3. Note the color of the indicating silica gel
to determine whether it has been completely spent, and make a notation
of its condition. Transfer the silica gel from the fourth impinger to
its original container, and seal. A funnel may make it easier to pour
the silica gel without spilling. A rubber policeman may be used as an
aid in removing the silica gel from the impinger. It is not necessary to
remove the small amount of dust particles that may adhere to the
impinger wall and are difficult to remove. Since the gain in weight is
to be used for moisture calculations, do not use any water or other
liquids to transfer the silica gel. If a balance is available in the
field, follow the procedure for Container No. 3 in Section 11.2.3.
8.7.6.4 Impinger Water. Treat the impingers as follows: Make a
notation of any color or film in the liquid catch. Measure the liquid
that is in the first three impingers to within 1 ml by using a graduated
cylinder or by weighing it to within 0.5 g by using a balance. Record
the volume or weight of liquid present. This information is required to
calculate the moisture content of the effluent gas. Discard the liquid
after measuring and recording the volume or weight, unless analysis of
the impinger catch is required (see NOTE, Section 6.1.1.8). If a
different type of condenser is used, measure the amount of moisture
condensed either volumetrically or gravimetrically.
8.8 Sample Transport. Whenever possible, containers should be
shipped in such a way that they remain upright at all times.

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures.

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

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

[[Page 177]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.107

Where:

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

9.2.1.1 Before beginning the field test (a set of three runs usually
constitutes a field test), operate the metering system (i.e., pump,
volume meter, and orifice) at the [Delta]H@ pressure differential for 10
minutes. Record the volume collected, the DGM temperature, and the
barometric pressure. Calculate a DGM calibration check value,
Yc, as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.108

where:

Yc=DGM calibration check value, dimensionless.
10=Run time, min.
9.2.1.2 Compare the Yc value with the dry gas meter
calibration factor Y to determine that: 0.97Y < Yc < 1.03Y.
If the Yc value is not within this range, the volume metering
system should be investigated before beginning the test.
9.2.2 Calibrated Critical Orifice. A critical orifice, calibrated
against a wet test meter or spirometer and designed to be inserted at
the inlet of the sampling meter box, may be used as a check by following
the procedure of Section 16.2.

10.0 Calibration and Standardization

Note: Maintain a laboratory log of all calibrations.

10.1 Probe Nozzle. Probe nozzles shall be calibrated before their
initial use in the field. Using a micrometer, measure the ID of the
nozzle to the nearest 0.025 mm (0.001 in.). Make three separate
measurements using different diameters each time, and obtain the average
of the measurements. The difference between the high and low numbers
shall not exceed 0.1 mm (0.004 in.). When nozzles become nicked, dented,
or corroded, they shall be reshaped, sharpened, and recalibrated before
use. Each nozzle shall be permanently and uniquely identified.
10.2 Pitot Tube Assembly. The Type S pitot tube assembly shall be
calibrated according to the procedure outlined in Section 10.1 of Method
2.
10.3 Metering System.
10.3.1 Calibration Prior to Use. Before its initial use in the
field, the metering system shall be calibrated as follows: Connect the
metering system inlet to the outlet of a wet test meter that is accurate
to within 1 percent. Refer to Figure 5-4. The wet test meter should have
a capacity of 30 liters/rev (1 ft³/rev). A spirometer of 400
liters (14 ft³) or more capacity, or equivalent, may be used
for this calibration, although a wet test meter is usually more
practical. The wet test meter should be periodically calibrated with a
spirometer or a liquid displacement meter to ensure the accuracy of the
wet test meter. Spirometers or wet test meters of other sizes may be
used, provided that the specified accuracies of the procedure are
maintained. Run the metering system pump for about 15 minutes with the
orifice manometer indicating a median reading as expected in field use
to allow the pump to warm up and to permit the interior surface of the
wet test meter to be thoroughly wetted. Then, at each of a minimum of
three orifice manometer settings, pass an exact quantity of gas through
the wet test meter and note the gas volume indicated by the DGM. Also
note the barometric pressure and the temperatures of the wet test meter,
the inlet of the DGM, and the outlet of the DGM. Select the highest and
lowest orifice settings to bracket the expected field operating range of
the orifice. Use a minimum volume of 0.14 m³ (5
ft³) at all orifice settings. Record all the data on a form
similar to Figure 5-5 and calculate Y, the DGM calibration factor, and
[Delta]H@, the orifice calibration factor, at each orifice
setting as shown on Figure 5-5. Allowable tolerances for individual Y
and [Delta]H@ values are given in Figure 5-5. Use the average
of the Y values in the calculations in Section 12.0.
10.3.1.1 Before calibrating the metering system, it is suggested
that a leak check be conducted. For metering systems having diaphragm
pumps, the normal leak-check procedure will not detect leakages within
the pump. For these cases the following leak-check procedure is
suggested: make a 10-minute calibration run at 0.00057 m³/min
(0.020 cfm). At the end of the run, take the difference of the measured
wet test meter and DGM volumes. Divide the difference by 10 to get the
leak rate. The leak rate should not exceed 0.00057 m³/min
(0.020 cfm).
10.3.2 Calibration After Use. After each field use, the calibration
of the metering system shall be checked by performing three calibration
runs at a single, intermediate orifice setting (based on the previous
field test), with the vacuum set at the maximum value reached during the
test series. To adjust the vacuum, insert a valve between the wet test
meter and the inlet of the metering system. Calculate the average value
of the DGM calibration factor. If the value has changed by more than 5
percent, recalibrate

[[Page 178]]

the meter over the full range of orifice settings, as detailed in
Section 10.3.1.

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

10.3.3 Acceptable Variation in Calibration. If the DGM coefficient
values obtained before and after a test series differ by more than 5
percent, the test series shall either be voided, or calculations for the
test series shall be performed using whichever meter coefficient value
(i.e., before or after) gives the lower value of total sample volume.
10.4 Probe Heater Calibration. Use a heat source to generate air
heated to selected temperatures that approximate those expected to occur
in the sources to be sampled. Pass this air through the probe at a
typical sample flow rate while measuring the probe inlet and outlet
temperatures at various probe heater settings. For each air temperature
generated, construct a graph of probe heating system setting versus
probe outlet temperature. The procedure outlined in APTD-0576 can also
be used. Probes constructed according to APTD-0581 need not be
calibrated if the calibration curves in APTD-0576 are used. Also, probes
with outlet temperature monitoring capabilities do not require
calibration.

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

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

11.0 Analytical Procedure

11.1 Record the data required on a sheet such as the one shown in
Figure 5-6.
11.2 Handle each sample container as follows:
11.2.1 Container No. 1. Leave the contents in the shipping container
or transfer the filter and any loose PM from the sample container to a
tared glass weighing dish. Desiccate for 24 hours in a desiccator
containing anhydrous calcium sulfate. Weigh to a constant weight, and
report the results to the nearest 0.1 mg. For the purposes of this
section, the term ``constant weight'' means a difference of no more than
0.5 mg or 1 percent of total weight less tare weight, whichever is
greater, between two consecutive weighings, with no less than 6 hours of
desiccation time between weighings. Alternatively, the sample may be
oven dried at 104 [deg]C (220 [deg]F) for 2 to 3 hours, cooled in the
desiccator, and weighed to a constant weight, unless otherwise specified
by the Administrator. The sample may be oven dried at 104 [deg]C (220
[deg]F) for 2 to 3 hours. Once the sample has cooled, weigh the sample,
and use this weight as a final weight.
11.2.2 Container No. 2. Note the level of liquid in the container,
and confirm on the analysis sheet whether leakage occurred during
transport. If a noticeable amount of leakage has occurred, either void
the sample or use methods, subject to the approval of the Administrator,
to correct the final results. Measure the liquid in this container
either volumetrically to 1 ml or gravimetrically
to 0.5 g. Transfer the contents to a tared 250 ml
beaker, and evaporate to dryness at ambient temperature and pressure.
Desiccate for 24 hours, and weigh to a constant weight. Report the
results to the nearest 0.1 mg.
11.2.3 Container No. 3. Weigh the spent silica gel (or silica gel
plus impinger) to the nearest 0.5 g using a balance. This step may be
conducted in the field.
11.2.4 Acetone Blank Container. Measure the acetone in this
container either volumetrically or gravimetrically. Transfer the acetone
to a tared 250 ml beaker, and evaporate to dryness at ambient
temperature and pressure. Desiccate for 24 hours, and weigh to a
constant weight. Report the results to the nearest 0.1 mg.

Note: The contents of Container No. 2 as well as the acetone blank
container may be evaporated at temperatures higher than ambient. If
evaporation is done at an elevated temperature, the temperature must be
below the boiling point of the solvent; also, to prevent ``bumping,''
the evaporation process must be closely supervised, and the contents of
the beaker must be swirled occasionally to maintain an even temperature.
Use extreme care, as acetone is highly flammable and has a low flash
point.

12.0 Data Analysis and Calculations

An=Cross-sectional area of nozzle, m²
(ft²).
Bws=Water vapor in the gas stream, proportion by volume.
Ca=Acetone blank residue concentration, mg/mg.
cs=Concentration of particulate matter in stack gas, dry
basis, corrected to standard conditions, g/dscm (gr/dscf).
I=Percent of isokinetic sampling.
L1=Individual leakage rate observed during the leak-check
conducted prior to the first component change, m³/min
(ft³/min)
La=Maximum acceptable leakage rate for either a pretest leak-
check or for a leak-check following a component change; equal

[[Page 179]]

to 0.00057 m³/min (0.020 cfm) or 4 percent of the average
sampling rate, whichever is less.
Li=Individual leakage rate observed during the leak-check
conducted prior to the ``i\th\'' component change (i=1, 2, 3 . . . n),
m³/min (cfm).
Lp=Leakage rate observed during the post-test leak-check,
m³/min (cfm).
ma=Mass of residue of acetone after evaporation, mg.
mn=Total amount of particulate matter collected, mg.
Mw=Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb-
mole).
Pbar=Barometric pressure at the sampling site, mm Hg (in.
Hg).
Ps=Absolute stack gas pressure, mm Hg (in. Hg).
Pstd=Standard absolute pressure, 760 mm Hg (29.92 in. Hg).
R=Ideal gas constant, 0.06236 ((mm Hg)(m \3\))/((K)(g-mole)) {21.85
((in. Hg) (ft \3\))/(([deg]R) (lb-mole)){time} .
Tm=Absolute average DGM temperature (see Figure 5-3), K
([deg]R).
Ts=Absolute average stack gas temperature (see Figure 5-3), K
([deg]R).
Tstd=Standard absolute temperature, 293 K (528 [deg]R).
Va=Volume of acetone blank, ml.
Vaw=Volume of acetone used in wash, ml.
V1c=Total volume of liquid collected in impingers and silica
gel (see Figure 5-6), ml.
Vm=Volume of gas sample as measured by dry gas meter, dcm
(dcf).
Vm(std)=Volume of gas sample measured by the dry gas meter,
corrected to standard conditions, dscm (dscf).
Vw(std)=Volume of water vapor in the gas sample, corrected to
standard conditions, scm (scf).
Vs=Stack gas velocity, calculated by Method 2, Equation 2-7,
using data obtained from Method 5, m/sec (ft/sec).
Wa=Weight of residue in acetone wash, mg.
Y=Dry gas meter calibration factor.
[Delta]H=Average pressure differential across the orifice meter (see
Figure 5-4), mm H2O (in. H2O).
[rho]a=Density of acetone, mg/ml (see label on bottle).
[rho]w=Density of water, 0.9982 g/ml. (0.002201 lb/ml).
[thetas]=Total sampling time, min.
[thetas]1=Sampling time interval, from the beginning of a run
until the first component change, min.
[thetas]i=Sampling time interval, between two successive
component changes, beginning with the interval between the first and
second changes, min.
[thetas]p=Sampling time interval, from the final (n \th\)
component change until the end of the sampling run, min.
13.6 =Specific gravity of mercury.
60=Sec/min.
100=Conversion to percent.

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

Where:

K1=0.3858 [deg]K/mm Hg for metric units,=17.64 [deg]R/in. Hg
for English units.

Note: Equation 5-1 can be used as written unless the leakage rate
observed during any of the mandatory leak checks (i.e., the post-test
leak check or leak checks conducted prior to component changes) exceeds
La. If Lp or Li exceeds La,
Equation 5-1 must be modified as follows:

(a) Case I. No component changes made during sampling run. In this
case, replace Vm in Equation 5-1 with the expression:
[GRAPHIC] [TIFF OMITTED] TR17OC00.110

(b) Case II. One or more component changes made during the sampling
run. In this case, replace Vm in Equation 5-1 by the
expression:

[[Page 180]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.111

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

Where:

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

12.5 Moisture Content.
[GRAPHIC] [TIFF OMITTED] TR17OC00.113

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

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

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

12.8 Total Particulate Weight. Determine the total particulate
matter catch from the sum of the weights obtained from Containers 1 and
2 less the acetone blank (see Figure 5-6).

Note: In no case shall a blank value of greater than 0.001 percent
of the weight of acetone used be subtracted from the sample weight.
Refer to Section 8.5.8 to assist in calculation of results involving two
or more filter assemblies or two or more sampling trains.
12.9 Particulate Concentration.
[GRAPHIC] [TIFF OMITTED] TR17OC00.116

Where:

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

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

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

Where:

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

[[Page 181]]

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

Where:

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

12.11.3 Acceptable Results. If 90 percent <= I <= 110 percent, the
results are acceptable. If the PM results are low in comparison to the
standard, and ``I'' is over 110 percent or less than 90 percent, the
Administrator may opt to accept the results. Reference 4 in Section 17.0
may be used to make acceptability judgments. If ``I'' is judged to be
unacceptable, reject the results, and repeat the sampling run.
12.12 Stack Gas Velocity and Volumetric Flow Rate. Calculate the
average stack gas velocity and volumetric flow rate, if needed, using
data obtained in this method and the equations in Sections 12.3 and 12.4
of Method 2.

13.0 Method Performance [Reserved]

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 Alternative Procedures

16.1 Dry Gas Meter as a Calibration Standard. A DGM may be used as a
calibration standard for volume measurements in place of the wet test
meter specified in Section 10.3, provided that it is calibrated
initially and recalibrated periodically as follows:
16.1.1 Standard Dry Gas Meter Calibration.
16.1.1.1. The DGM to be calibrated and used as a secondary reference
meter should be of high quality and have an appropriately sized capacity
(e.g., 3 liters/rev (0.1 ft\3\/rev)). A spirometer (400 liters (14
ft\3\) or more capacity), or equivalent, may be used for this
calibration, although a wet test meter is usually more practical. The
wet test meter should have a capacity of 30 liters/rev (1 ft\3\/rev) and
capable of measuring volume to within 1.0 percent. Wet test meters
should be checked against a spirometer or a liquid displacement meter to
ensure the accuracy of the wet test meter. Spirometers or wet test
meters of other sizes may be used, provided that the specified
accuracies of the procedure are maintained.
16.1.1.2 Set up the components as shown in Figure 5-7. A spirometer,
or equivalent, may be used in place of the wet test meter in the system.
Run the pump for at least 5 minutes at a flow rate of about 10 liters/
min (0.35 cfm) to condition the interior surface of the wet test meter.
The pressure drop indicated by the manometer at the inlet side of the
DGM should be minimized (no greater than 100 mm H2O (4 in.
H2O) at a flow rate of 30 liters/min (1 cfm)). This can be
accomplished by using large diameter tubing connections and straight
pipe fittings.
16.1.1.3 Collect the data as shown in the example data sheet (see
Figure 5-8). Make triplicate runs at each of the flow rates and at no
less than five different flow rates. The range of flow rates should be
between 10 and 34 liters/min (0.35 and 1.2 cfm) or over the expected
operating range.
16.1.1.4 Calculate flow rate, Q, for each run using the wet test
meter volume, VW, and the run time, [thetas]. Calculate the
DGM coefficient, Yds, for each run. These calculations are as
follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.119

[GRAPHIC] [TIFF OMITTED] TR17OC00.120

Where:

K1=0.3858 [deg]C/mm Hg for metric units=17.64 [deg]F/in. Hg
for English units.
VW=Wet test meter volume, liter (ft\3\).
Vds=Dry gas meter volume, liter (ft\3\).
Tds=Average dry gas meter temperature, [deg]C ( [deg]F).
Tadj=273 [deg]C for metric units=460 [deg]F for English
units.
TW=Average wet test meter temperature, [deg]C ( [deg]F)
Pbar=Barometric pressure, mm Hg (in. Hg).
[Delta]p=Dry gas meter inlet differential pressure, mm H2O
(in. H2O).

[[Page 182]]

[thetas]=Run time, min.

16.1.1.5 Compare the three Yds values at each of the flow
rates and determine the maximum and minimum values. The difference
between the maximum and minimum values at each flow rate should be no
greater than 0.030. Extra sets of triplicate runs may be made in order
to complete this requirement. In addition, the meter coefficients should
be between 0.95 and 1.05. If these specifications cannot be met in three
sets of successive triplicate runs, the meter is not suitable as a
calibration standard and should not be used as such. If these
specifications are met, average the three Yds values at each
flow rate resulting in no less than five average meter coefficients,
Yds.
16.1.1.6 Prepare a curve of meter coefficient, Yds,
versus flow rate, Q, for the DGM. This curve shall be used as a
reference when the meter is used to calibrate other DGMs and to
determine whether recalibration is required.
16.1.2 Standard Dry Gas Meter Recalibration.
16.1.2.1 Recalibrate the standard DGM against a wet test meter or
spirometer annually or after every 200 hours of operation, whichever
comes first. This requirement is valid provided the standard DGM is kept
in a laboratory and, if transported, cared for as any other laboratory
instrument. Abuse to the standard meter may cause a change in the
calibration and will require more frequent recalibrations.
16.1.2.2 As an alternative to full recalibration, a two-point
calibration check may be made. Follow the same procedure and equipment
arrangement as for a full recalibration, but run the meter at only two
flow rates [suggested rates are 14 and 30 liters/min (0.5 and 1.0 cfm)].
Calculate the meter coefficients for these two points, and compare the
values with the meter calibration curve. If the two coefficients are
within 1.5 percent of the calibration curve values at the same flow
rates, the meter need not be recalibrated until the next date for a
recalibration check.
16.2 Critical Orifices As Calibration Standards. Critical orifices
may be used as calibration standards in place of the wet test meter
specified in Section 16.1, provided that they are selected, calibrated,
and used as follows:
16.2.1 Selection of Critical Orifices.
16.2.1.1 The procedure that follows describes the use of hypodermic
needles or stainless steel needle tubings which have been found suitable
for use as critical orifices. Other materials and critical orifice
designs may be used provided the orifices act as true critical orifices
(i.e., a critical vacuum can be obtained, as described in Section
16.2.2.2.3). Select five critical orifices that are appropriately sized
to cover the range of flow rates between 10 and 34 liters/min (0.35 and
1.2 cfm) or the expected operating range. Two of the critical orifices
should bracket the expected operating range. A minimum of three critical
orifices will be needed to calibrate a Method 5 DGM; the other two
critical orifices can serve as spares and provide better selection for
bracketing the range of operating flow rates. The needle sizes and
tubing lengths shown in Table 5-1 in Section 18.0 give the approximate
flow rates.
16.2.1.2 These needles can be adapted to a Method 5 type sampling
train as follows: Insert a serum bottle stopper, 13 by 20 mm sleeve
type, into a \1/2\-inch Swagelok (or equivalent) quick connect. Insert
the needle into the stopper as shown in Figure 5-9.
16.2.2 Critical Orifice Calibration. The procedure described in this
section uses the Method 5 meter box configuration with a DGM as
described in Section 6.1.1.9 to calibrate the critical orifices. Other
schemes may be used, subject to the approval of the Administrator.
16.2.2.1 Calibration of Meter Box. The critical orifices must be
calibrated in the same configuration as they will be used (i.e., there
should be no connections to the inlet of the orifice).
16.2.2.1.1 Before calibrating the meter box, leak check the system
as follows: Fully open the coarse adjust valve, and completely close the
by-pass valve. Plug the inlet. Then turn on the pump, and determine
whether there is any leakage. The leakage rate shall be zero (i.e., no
detectable movement of the DGM dial shall be seen for 1 minute).
16.2.2.1.2 Check also for leakages in that portion of the sampling
train between the pump and the orifice meter. See Section 8.4.1 for the
procedure; make any corrections, if necessary. If leakage is detected,
check for cracked gaskets, loose fittings, worn O-rings, etc., and make
the necessary repairs.
16.2.2.1.3 After determining that the meter box is leakless,
calibrate the meter box according to the procedure given in Section
10.3. Make sure that the wet test meter meets the requirements stated in
Section 16.1.1.1. Check the water level in the wet test meter. Record
the DGM calibration factor, Y.
16.2.2.2 Calibration of Critical Orifices. Set up the apparatus as
shown in Figure 5-10.
16.2.2.2.1 Allow a warm-up time of 15 minutes. This step is
important to equilibrate the temperature conditions through the DGM.
16.2.2.2.2 Leak check the system as in Section 16.2.2.1.1. The
leakage rate shall be zero.
16.2.2.2.3 Before calibrating the critical orifice, determine its
suitability and the appropriate operating vacuum as follows: Turn on the
pump, fully open the coarse adjust valve, and adjust the by-pass valve
to give a vacuum reading corresponding to about half of atmospheric
pressure. Observe the meter box orifice manometer reading, [Delta]H.
Slowly increase the vacuum reading until a stable

[[Page 183]]

reading is obtained on the meter box orifice manometer. Record the
critical vacuum for each orifice. Orifices that do not reach a critical
value shall not be used.
16.2.2.2.4 Obtain the barometric pressure using a barometer as
described in Section 6.1.2. Record the barometric pressure,
Pbar, in mm Hg (in. Hg).
16.2.2.2.5 Conduct duplicate runs at a vacuum of 25 to 50 mm Hg (1
to 2 in. Hg) above the critical vacuum. The runs shall be at least 5
minutes each. The DGM volume readings shall be in increments of complete
revolutions of the DGM. As a guideline, the times should not differ by
more than 3.0 seconds (this includes allowance for changes in the DGM
temperatures) to achieve 0.5 percent in K' (see
Eq. 5-11). Record the information listed in Figure 5-11.
16.2.2.2.6 Calculate K' using Equation 5-11.
[GRAPHIC] [TIFF OMITTED] TR17OC00.121

Where:

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

[[Page 184]]

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

Table 5-1 Flor Rates for Various needle Sizes and Tube Lengths
----------------------------------------------------------------------------------------------------------------
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
----------------------------------------------------------------------------------------------------------------

[[Page 185]]

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[[Page 186]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.126

[[Page 187]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.127

[[Page 188]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.128

[[Page 189]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.129

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)

[[Page 190]]

________________________________________________________________________

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

[[Page 191]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.130

[[Page 192]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.131

[[Page 193]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.132

[[Page 194]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.133

Date____________________________________________________________________
Train ID________________________________________________________________
DGM cal. factor_________________________________________________________
Critical orifice ID_____________________________________________________

[[Page 195]]

Temperatures:............ [deg]C ( / /
[deg]F).
Initial.................. [deg]C ( / /
[deg]F).
Final.................... min/sec........ / /
Av. Temeperature, t m.... min............ ........... ...........
Time, [thetas]............... ............... ........... ...........
Orifice man. rdg., [Delta]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, [thetas]............... min............ ........... ...........
Orifice man. rdg., [Delta]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

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 196]]

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

[[Page 197]]

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.

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.

[[Page 198]]

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

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.
[rho]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 199]]

Weight of particulate matter.
----------------------------------------------------------------------------------------------------------------

[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.

[[Page 200]]

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 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 5C [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

[[Page 201]]

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 5x5
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 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 3x3 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.

[[Page 202]]

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.

17.0 Tables, Diagrams, Flowcharts, and Validation Data

[[Page 203]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.144

[[Page 204]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.145

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.

[[Page 205]]

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-[micro]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

[[Page 206]]

(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.
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-[micro]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:

[[Page 207]]

[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 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-[micro]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.

[[Page 208]]

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).

[[Page 209]]

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 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 [micro]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 [micro]g/ml) to a series of
five 50-ml volumetric flasks. (The standard masses will equal 25, 50,
100, 150, and 250 [micro]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 [micro]g
(x-axis) versus their responses (y-axis). From this line, or equation,
determine the slope

[[Page 210]]

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 [micro]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.
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, [micro]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.

[[Page 211]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.153

Where:

100=Aliquot factor, 495 ml/5 ml
1000=Constant, [micro]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-mmx305-mm (1-in.x12-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.
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.

[[Page 212]]

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)

[[Page 213]]

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 (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 ([Delta]p) readings and another
(optional) for orifice differential pressure readings ([Delta]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

[[Page 214]]

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 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 [Delta]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

[[Page 215]]

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
[Delta]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
determinations, data from

[[Page 216]]

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.

[[Page 217]]

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:
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.
[Delta]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.

[[Page 218]]

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. 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.

[[Page 219]]

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.

18.0 Tables, Diagrams, Flowcharts, and Validation Data

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[[Page 221]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.165

[[Page 222]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.166

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[GRAPHIC] [TIFF OMITTED] TR17OC00.167

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.

[[Page 224]]

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.

[[Page 225]]

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.

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).

[[Page 226]]

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.
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.

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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 funnel. Add 25-ml of dichloromethane to the separatory
funnel, stopper and vigorously shake 1 minute, let

[[Page 228]]

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

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.
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).
[Delta]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.
[thetas]=Total sampling time, min.
[thetas]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.

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[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

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.

17.0 Tables, Diagrams, Flowcharts, and Validation Data

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[[Page 233]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.180

Method 5I--Determination of Low Level Particulate Matter Emissions From
Stationary Sources

Note: This method does not include all of the specifications (e.g.,
equipment and supplies) and procedures (e.g., sampling and analytical)
essential to its performance. Certain information is contained in other
EPA procedures found in this part. Therefore, to obtain reliable
results, persons using this method should have experience with and a
thorough knowledge of the following Methods: Methods 1, 2, 3, 4 and 5.

1. Scope and Application.

1.1 Analyte. Particulate matter (PM). No CAS number assigned.

[[Page 234]]

1.2 Applicability. This method is applicable for the determination
of low level particulate matter (PM) emissions from stationary sources.
The method is most effective for total PM catches of 50 mg or less. This
method was initially developed for performing correlation of manual PM
measurements to PM continuous emission monitoring systems (CEMS),
however it is also useful for other low particulate concentration
applications.
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. Method 5I requires the use of paired trains.
Acceptance criteria for the identification of data quality outliers from
the paired trains are provided in Section 12.2 of this Method.

2. Summary of Method.

2.1. Description. The system setup and operation is essentially
identical to Method 5. Particulate is withdrawn isokinetically from the
source and collected on a 47 mm glass fiber filter maintained at a
temperature of 120 14[deg]C (248 25[deg]F). The PM mass is determined by gravimetric
analysis after the removal of uncombined water. Specific measures in
this procedure designed to improve system performance at low particulate
levels include:
1. Improved sample handling procedures
2 Light weight sample filter assembly
3. Use of low residue grade acetone
Accuracy is improved through the minimization of systemic errors
associated with sample handling and weighing procedures. High purity
reagents, all glass, grease free, sample train components, and light
weight filter assemblies and beakers, each contribute to the overall
objective of improved precision and accuracy at low particulate
concentrations.
2.2 Paired Trains. This method must be performed using a paired
train configuration. These trains may be operated as co-located trains
(to trains operating collecting from one port) or as simultaneous trains
(separate trains operating from different ports at the same time).
Procedures for calculating precision of the paired trains are provided
in Section 12.
2.3 Detection Limit. a. Typical detection limit for manual
particulate testing is 0.5 mg. This mass is also cited as the accepted
weight variability limit in determination of ``constant weight'' as
cited in Section 8.1.2 of this Method. EPA has performed studies to
provide guidance on minimum PM catch. The minimum detection limit (MDL)
is the minimum concentration or amount of an analyte that can be
determined with a specified degree of confidence to be different from
zero. We have defined the minimum or target catch as a concentration or
amount sufficiently larger than the MDL to ensure that the results are
reliable and repeatable. The particulate matter catch is the product of
the average particulate matter concentration on a mass per volume basis
and the volume of gas collected by the sample train. The tester can
generally control the volume of gas collected by increasing the sampling
time or to a lesser extent by increasing the rate at which sample is
collected. If the tester has a reasonable estimate of the PM
concentration from the source, the tester can ensure that the target
catch is collected by sampling the appropriate gas volume.
b. However, if the source has a very low particulate matter
concentration in the stack, the volume of gas sampled may need to be
very large which leads to unacceptably long sampling times. When
determining compliance with an emission limit, EPA guidance has been
that the tester does not always have to collect the target catch.
Instead, we have suggested that the tester sample enough stack gas, that
if the source were exactly at the level of the emission standard, the
sample catch would equal the target catch. Thus, if at the end of the
test the catch were smaller than the target, we could still conclude
that the source is in compliance though we might not know the exact
emission level. This volume of gas becomes a target volume that can be
translated into a target sampling time by assuming an average sampling
rate. Because the MDL forms the basis for our guidance on target
sampling times, EPA has conducted a systematic laboratory study to
define what is the MDL for Method 5 and determined the Method to have a
calculated practical quantitation limit (PQL) of 3 mg of PM and an MDL
of 1 mg.
c. Based on these results, the EPA has concluded that for PM
testing, the target catch must be no less than 3 mg. Those sample
catches between 1 mg and 3 mg are between the detection limit and the
limit of quantitation. If a tester uses the target catch to estimate a
target sampling time that results in sample catches that are less than 3
mg, you should not automatically reject the results. If the tester
calculated the target sampling time as described above by assuming that
the source was at the level of the emission limit, the results would
still be valid for determining that the source was in compliance. For
purposes other than determining compliance, results should be divided
into two categories--those that fall between 3 mg and 1 mg and those
that are below 1 mg. A sample catch between 1 and 3 mg may be used for
such purposes as calculating emission rates with the understanding that
the resulting emission rates can have a high degree of uncertainty.
Results of less than 1 mg should not be used for calculating emission
rates or pollutant concentrations.
d. When collecting small catches such as 3 mg, bias becomes an
important issue. Source testers must use extreme caution to reach the
PQL of 3 mg by assuring that sampling

[[Page 235]]

probes are very clean (perhaps confirmed by low blank weights) before
use in the field. They should also use low tare weight sample
containers, and establish a well-controlled balance room to weigh the
samples.

3. Definitions.

3.1 Light Weight Filter Housing. A smaller housing that allows the
entire filtering system to be weighed before and after sample
collection. (See. 6.1.3)
3.2 Paired Train. Sample systems trains may be operated as co-
located trains (two sample probes attached to each other in the same
port) or as simultaneous trains (two separate trains operating from
different ports at the same time).

4. Interferences.

a. There are numerous potential interferents that may be encountered
during performance of Method 5I sampling and analyses. This Method
should be considered more sensitive to the normal interferents typically
encountered during particulate testing because of the low level
concentrations of the flue gas stream being sampled.
b. Care must be taken to minimize field contamination, especially to
the filter housing since the entire unit is weighed (not just the filter
media). Care must also be taken to ensure that no sample is lost during
the sampling process (such as during port changes, removal of the filter
assemblies from the probes, etc.).
c. Balance room conditions are a source of concern for analysis of
the low level samples. Relative humidity, ambient temperatures
variations, air draft, vibrations and even barometric pressure can
affect consistent reproducible measurements of the sample media.
Ideally, the same analyst who performs the tare weights should perform
the final weights to minimize the effects of procedural differences
specific to the analysts.
d. Attention must also be provided to weighing artifacts caused by
electrostatic charges which may have to be discharged or neutralized
prior to sample analysis. Static charge can affect consistent and
reliable gravimetric readings in low humidity environments. Method 5I
recommends a relative humidity of less than 50 percent in the weighing
room environment used for sample analyses. However, lower humidity may
be encountered or required to address sample precision problems. Low
humidity conditions can increase the effects of static charge.
e. Other interferences associated with typical Method 5 testing
(sulfates, acid gases, etc.) are also applicable to Method 5I.

5. Safety.

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

6. Equipment and Supplies.

6.1 Sample Collection Equipment and Supplies. The sample train is
nearly identical in configuration to the train depicted in Figure 5-1 of
Method 5. The primary difference in the sample trains is the lightweight
Method 5I filter assembly that attaches directly to the exit to the
probe. Other exceptions and additions specific to Method 5I include:
6.1.1 Probe Nozzle. Same as Method 5, with the exception that it
must be constructed of borosilicate or quartz glass tubing.
6.1.2 Probe Liner. Same as Method 5, with the exception that it must
be constructed of borosilicate or quartz glass tubing.
6.1.3 Filter Holder. The filter holder is constructed of
borosilicate or quartz glass front cover designed to hold a 47-mm glass
fiber filter, with a wafer thin stainless steel (SS) filter support, a
silicone rubber or Viton O-ring, and Teflon tape seal. This holder
design will provide a positive seal against leakage from the outside or
around the filter. The filter holder assembly fits into a SS filter
holder and attaches directly to the outlet of the probe. The tare weight
of the filter, borosilicate or quartz glass holder, SS filter support,
O-ring and Teflon tape seal generally will not exceed approximately 35
grams. The filter holder is designed to use a 47-mm glass fiber filter
meeting the quality criteria in of Method 5. These units are
commercially available from several source testing equipment vendors.
Once the filter holder has been assembled, desiccated and tared, protect
it from external sources of contamination by covering the front socket
with a ground glass plug. Secure the plug with an impinger clamp or
other item that will ensure a leak-free fitting.
6.2 Sample Recovery Equipment and Supplies. Same as Method 5, with
the following exceptions:
6.2.1 Probe-Liner and Probe-Nozzle Brushes. Teflon or nylon bristle
brushes with stainless steel wire handles, should be used to clean the
probe. The probe brush must have extensions (at least as long as the
probe) of Teflon, nylon or similarly inert material. The brushes must be
properly sized and shaped for brushing out the probe liner and nozzle.
6.2.2 Wash Bottles. Two Teflon wash bottles are recommended however,
polyethylene wash bottles may be used at the option of the tester.
Acetone should not be stored in polyethylene bottles for longer than one
month.

[[Page 236]]

6.2.3 Filter Assembly Transport. A system should be employed to
minimize contamination of the filter assemblies during transport to and
from the field test location. A carrying case or packet with clean
compartments of sufficient size to accommodate each filter assembly can
be used. This system should have an air tight seal to further minimize
contamination during transport to and from the field.
6.3 Analysis Equipment and Supplies. Same as Method 5, with the
following exception:
6.3.1 Lightweight Beaker Liner. Teflon or other lightweight beaker
liners are used for the analysis of the probe and nozzle rinses. These
light weight liners are used in place of the borosilicate glass beakers
typically used for the Method 5 weighings in order to improve sample
analytical precision.
6.3.2 Anti-static Treatment. Commercially available gaseous anti-
static rinses are recommended for low humidity situations that
contribute to static charge problems.

7. Reagents and Standards.

7.1 Sampling Reagents. The reagents used in sampling are the same as
Method 5 with the following exceptions:
7.1.1 Filters. The quality specifications for the filters are
identical to those cited for Method 5. The only difference is the filter
diameter of 47 millimeters.
7.1.2 Stopcock Grease. Stopcock grease cannot be used with this
sampling train. We recommend that the sampling train be assembled with
glass joints containing O-ring seals or screw-on connectors, or similar.
7.1.3 Acetone. Low residue type acetone, <=0.001 percent residue,
purchased in glass bottles is used for the recovery of particulate
matter from the probe and nozzle. Acetone from metal containers
generally has a high residue blank and should not be used. Sometimes,
suppliers transfer acetone to glass bottles from metal containers; thus,
acetone blanks must be run prior to field use and only acetone with low
blank values (<=0.001 percent residue, as specified by the manufacturer)
must be used. Acetone blank correction is not allowed for this method;
therefore, it is critical that high purity reagents be purchased and
verified prior to use.
7.1.4 Gloves. Disposable, powder-free, latex surgical gloves, or
their equivalent are used at all times when handling the filter housings
or performing sample recovery.
7.2 Standards. There are no applicable standards or audit samples
commercially available for Method 5I analyses.

8. Sample Collection, Preservation, Storage, and Transport.

8.1 Pretest Preparation. Same as Method 5 with several exceptions
specific to filter assembly and weighing.
8.1.1 Filter Assembly. Uniquely identify each filter support before
loading filters into the holder assembly. This can be done with an
engraving tool or a permanent marker. Use powder free latex surgical
gloves whenever handling the filter holder assemblies. Place the O-ring
on the back of the filter housing in the O-ring groove. Place a 47 mm
glass fiber filter on the O-ring with the face down. Place a stainless
steel filter holder against the back of the filter. Carefully wrap 5 mm
(\1/4\ inch) wide Teflon'' tape one timearound the outside of the filter
holder overlapping the stainless steel filter support by approximately
2.5 mm (\1/8\ inch). Gently brush the Teflon tape down on the back of
the stainless steel filter support. Store the filter assemblies in their
transport case until time for weighing or field use.
8.1.2 Filter Weighing Procedures. a. Desiccate the entire filter
holder assemblies at 20 5.6[deg]C (68 10[deg]F) and ambient pressure for at least 24 hours.
Weigh at intervals of at least 6 hours to a constant weight, i.e., 0.5
mg change from previous weighing. Record the results to the nearest 0.1
mg. During each weighing, the filter holder assemblies must not be
exposed to the laboratory atmosphere for a period greater than 2 minutes
and a relative humidity above 50 percent. Lower relative humidity may be
required in order to improve analytical precision. However, low humidity
conditions increase static charge to the sample media.
b. Alternatively (unless otherwise specified by the Administrator),
the filters holder assemblies may be oven dried at 105[deg]C (220[deg]F)
for a minimum of 2 hours, desiccated for 2 hours, and weighed. The
procedure used for the tare weigh must also be used for the final weight
determination.
c. Experience has shown that weighing uncertainties are not only
related to the balance performance but to the entire weighing procedure.
Therefore, before performing any measurement, establish and follow
standard operating procedures, taking into account the sampling
equipment and filters to be used.
8.2 Preliminary Determinations. Select the sampling site, traverse
points, probe nozzle, and probe length as specified in Method 5.
8.3 Preparation of Sampling Train. Same as Method 5, Section 8.3,
with the following exception: During preparation and assembly of the
sampling train, keep all openings where contamination can occur covered
until justbefore assembly or until sampling is about to begin. Using
gloves, place a labeled

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(identified) and weighed filter holder assembly into the stainless steel
holder. Then place this whole unit in the Method 5 hot box, and attach
it to the probe. Do not use stopcock grease.
8.4 Leak-Check Procedures. Same as Method 5.
8.5 Sampling Train Operation.
8.5.1. Operation. Operate the sampling train in a manner consistent
with those described in Methods 1, 2, 4 and 5 in terms of the number of
sample points and minimum time per point. The sample rate and total gas
volume should be adjusted based on estimated grain loading of the source
being characterized. The total sampling time must be a function of the
estimated mass of particulate to be collected for the run. Targeted mass
to be collected in a typical Method 5I sample train should be on the
order of 10 to 20 mg. Method 5I is most appropriate for total collected
masses of less than 50 milligrams, however, there is not an exact
particulate loading cutoff, and it is likely that some runs may exceed
50 mg. Exceeding 50 mg (or less than 10 mg) for the sample mass does not
necessarily justify invalidating a sample run if all other Method
criteria are met.
8.5.2 Paired Train. This Method requires PM samples be collected
with paired trains.
8.5.2.1 It is important that the systems be operated truly
simultaneously. This implies that both sample systems start and stop at
the same times. This also means that if one sample system is stopped
during the run, the other sample systems must also be stopped until the
cause has been corrected.
8.5.2.2 Care should be taken to maintain the filter box temperature
of the paired trains as close as possible to the Method required
temperature of 120 14[deg]C (248 25[deg]F). If separate ovens are being used for
simultaneously operated trains, it is recommended that the oven
temperature of each train be maintained within 14[deg]C ( 25[deg]F) of each
other.
8.5.2.3 The nozzles for paired trains need not be identically sized.
8.5.2.4 Co-located sample nozzles must be within the same plane
perpendicular to the gas flow. Co-located nozzles and pitot assemblies
should be within a 6.0 cm x 6.0 cm square (as cited for a quadruple
train in Reference Method 301).
8.5.3 Duplicate gas samples for molecular weight determination need
not be collected.
8.6 Sample Recovery. Same as Method 5 with several exceptions
specific to the filter housing.
8.6.1 Before moving the sampling train to the cleanup site, remove
the probe from the train and seal the nozzle inlet and outlet of the
probe. Be careful not to lose any condensate that might be present. Cap
the filter inlet using a standard ground glass plug and secure the cap
with an impinger clamp. Remove the umbilical cord from the last impinger
and cap the impinger. If a flexible line is used between the first
impinger condenser and the filter holder, disconnect the line at the
filter holder and let any condensed water or liquid drain into the
impingers or condenser.
8.6.2 Transfer the probe and filter-impinger assembly to the cleanup
area. This area must be clean and protected from the wind so that the
possibility of losing any of the sample will be minimized.
8.6.3 Inspect the train prior to and during disassembly and note any
abnormal conditions such as particulate color, filter loading, impinger
liquid color, etc.
8.6.4 Container No. 1, Filter Assembly. Carefully remove the cooled
filter holder assembly from the Method 5 hot box and place it in the
transport case. Use a pair of clean gloves to handle the filter holder
assembly.
8.6.5 Container No. 2, Probe Nozzle and Probe Liner Rinse. Rinse the
probe and nozzle components with acetone. Be certain that the probe and
nozzle brushes have been thoroughly rinsed prior to use as they can be a
source of contamination.
8.6.6 All Other Train Components. (Impingers) Same as Method 5.
8.7 Sample Storage and Transport. Whenever possible, containers
should be shipped in such a way that they remain upright at all times.
All appropriate dangerous goods shipping requirements must be observed
since acetone is a flammable liquid.

9. Quality Control.

9.1 Miscellaneous Field Quality Control Measures.
9.1.1 A quality control (QC) check of the volume metering system at
the field site is suggested before collecting the sample using the
procedures in Method 5, Section 4.4.1.
9.1.2 All other quality control checks outlined in Methods 1, 2, 4
and 5 also apply to Method 5I. This includes procedures such as leak-
checks, equipment calibration checks, and independent checks of field
data sheets for reasonableness and completeness.
9.2 Quality Control Samples.
9.2.1 Required QC Sample. A laboratory reagent blank must be
collected and analyzed for each lot of acetone used for a field program
to confirm that it is of suitable purity. The particulate samples cannot
be blank corrected.
9.2.2 Recommended QC Samples. These samples may be collected and
archived for future analyses.
9.2.2.1 A field reagent blank is a recommended QC sample collected
from a portion of the acetone used for cleanup of the probe and nozzle.
Take 100 ml of this acetone directly from the wash bottle being used and
place it in a glass sample container labeled ``field acetone reagent
blank.'' At least one field reagent blank is recommended for every

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five runs completed. The field reagent blank samples demonstrate the
purity of the acetone was maintained throughout the program.
9.2.2.2 A field bias blank train is a recommended QC sample. This
sample is collected by recovering a probe and filter assembly that has
been assembled, taken to the sample location, leak checked, heated,
allowed to sit at the sample location for a similar duration of time as
a regular sample run, leak-checked again, and then recovered in the same
manner as a regular sample. Field bias blanks are not a Method
requirement, however, they are recommended and are very useful for
identifying sources of contamination in emission testing samples. Field
bias blank train results greater than 5 times the method detection limit
may be considered problematic.

10. Calibration and Standardization Same as Method 5, Section 5.

11. Analytical Procedures.

11.1 Analysis. Same as Method 5, Sections 11.1--11.2.4, with the
following exceptions:
11.1.1 Container No. 1. Same as Method 5, Section 11.2.1, with the
following exception: Use disposable gloves to remove each of the filter
holder assemblies from the desiccator, transport container, or sample
oven (after appropriate cooling).
11.1.2 Container No. 2. Same as Method 5, Section 11.2.2, with the
following exception: It is recommended that the contents of Container
No. 2 be transferred to a 250 ml beaker with a Teflon liner or similar
container that has a minimal tare weight before bringing to dryness.

12. Data Analysis and Calculations.

12.1 Particulate Emissions. The analytical results cannot be blank
corrected for residual acetone found in any of the blanks. All other
sample calculations are identical to Method 5.
12.2 Paired Trains Outliers. a. Outliers are identified through the
determination of precision and any systemic bias of the paired trains.
Data that do not meet this criteria should be flagged as a data quality
problem. The primary reason for performing dual train sampling is to
generate information to quantify the precision of the Reference Method
data. The relative standard deviation (RSD) of paired data is the
parameter used to quantify data precision. RSD for two simultaneously
gathered data points is determined according to:
[GRAPHIC] [TIFF OMITTED] TR30SE99.008

where, Ca and Cb are concentration values determined from trains A and B
respectively. For RSD calculation, the concentration units are
unimportant so long as they are consistent.
b. A minimum precision criteria for Reference Method PM data is that
RSD for any data pair must be less than 10% as long as the mean PM
concentration is greater than 10 mg/dscm. If the mean PM concentration
is less than 10 mg/dscm higher RSD values are acceptable. At mean PM
concentration of 1 mg/dscm acceptable RSD for paired trains is 25%.
Between 1 and 10 mg/dscm acceptable RSD criteria should be linearly
scaled from 25% to 10%. Pairs of manual method data exceeding these RSD
criteria should be eliminated from the data set used to develop a PM
CEMS correlation or to assess RCA. If the mean PM concentration is less
than 1 mg/dscm, RSD does not apply and the mean result is acceptable.

13. Method Performance [Reserved]

14. Pollution Prevention [Reserved]

15. Waste Management [Reserved]

16. Alternative Procedures. Same as Method 5.
17. Bibliography. Same as Method 5.
18. Tables, Diagrams, Flowcharts and Validation Data. Figure 5I-1 is
a schematic of the sample train.

[[Page 239]]

[GRAPHIC] [TIFF OMITTED] TR30SE99.009

[36 FR 24877, Dec. 23, 1971]

Editorial Note: For Federal Register citations affecting part 60,
appendix A-3, see the List of CFR Sections Affected, which appears in
the Finding Aids section of the printed volume and on GPO Access.

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