[[pp. 62093-62142]] Amendments for Testing and Monitoring Provisions

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

[Federal Register: October 17, 2000 (Volume 65, Number 201)]
[Rules and Regulations]
[Page 62093-62142]
From the Federal Register Online via GPO Access [wais.access.gpo.gov]
[DOCID:fr17oc00-17]

[[Continued from page 62092]]

[[Page 62093]]

6.2.3 Funnels. Glass or high-density polyethylene, to aid in
sample recovery.
6.3 Sample Preparation and Analysis.
6.3.1 Volumetric Flasks. Class A, various sizes.
6.3.2 Volumetric Pipettes. Class A, assortment. To dilute samples
to calibration range of the ion chromatograph (IC).
6.3.3 Ion Chromatograph (IC). Suppressed or nonsuppressed, with a
conductivity detector and electronic integrator operating in the peak
area mode. Other detectors, a strip chart recorder, and peak heights
may be used.

7.0 Reagents and Standards

Note: Unless otherwise indicated, all reagents must conform to
the specifications established by the Committee on Analytical
Reagents of the American Chemical Society (ACS reagent grade). When
such specifications are not available, the best available grade
shall be used.

7.1 Sampling.
7.1.1 Filter. Teflon mat (e.g., Pallflex TX40HI45) filter. When
the stack gas temperature exceeds 210 deg.C (410 deg.F) a quartz fiber
filter may be used.
7.1.2 Water. Deionized, distilled water that conforms to American
Society of Testing and Materials (ASTM) Specification D 1193-77 or 91,
Type 3 (incorporated by reference--see Sec. 60.17).
7.1.3 Acidic Absorbing Solution, 0.1 N Sulfuric Acid
(H2SO4). To prepare 1 L, slowly add 2.80 ml of
concentrated 17.9 M H2SO4 to about 900 ml of water while stirring, and
adjust the final volume to 1 L using additional water. Shake well to
mix the solution.
7.1.4 Silica Gel, Crushed Ice, and Stopcock Grease. Same as Method
5, Sections 7.1.2, 7.1.4, and 7.1.5, respectively.
7.1.5 Alkaline Absorbing Solution, 0.1 N Sodium Hydroxide (NaOH).
To prepare 1 L, dissolve 4.00 g of solid NaOH in about 900 ml of water
and adjust the final volume to 1 L using additional water. Shake well
to mix the solution.
7.1.6 Sodium Thiosulfate,
(Na2S2O33.5
H2O).
7.2 Sample Preparation and Analysis.
7.2.1 Water. Same as in Section 7.1.2.
7.2.2 Absorbing Solution Blanks. A separate blank solution of each
absorbing reagent should be prepared for analysis with the field
samples. Dilute 200 ml of each absorbing solution (250 ml of the acidic
absorbing solution, if a condensate impinger is used) to the same final
volume as the field samples using the blank sample of rinse water. If a
particulate determination is conducted, collect a blank sample of
acetone.
7.2.3 Halide Salt Stock Standard Solutions. Prepare concentrated
stock solutions from reagent grade sodium chloride (NaCl), sodium
bromide (NaBr), and sodium fluoride (NaF). Each must be dried at
110 deg.C (230 deg.F) for two or more hours and then cooled to room
temperature in a desiccator immediately before weighing. Accurately
weigh 1.6 to 1.7 g of the dried NaCl to within 0.1 mg, dissolve in
water, and dilute to 1 liter. Calculate the exact
Cl-concentration using Equation 26A-1 in Section 12.2. In a
similar manner, accurately weigh and solubilize 1.2 to 1.3 g of dried
NaBr and 2.2 to 2.3 g of NaF to make 1-liter solutions. Use Equations
26A-2 and 26A-3 in Section 12.2, to calculate the Br-and
F-concentrations. Alternately, solutions containing a
nominal certified concentration of 1000 mg/L NaCl are commercially
available as convenient stock solutions from which standards can be
made by appropriate volumetric dilution. Refrigerate the stock standard
solutions and store no longer than one month.
7.2.4 Chromatographic Eluent. Same as Method 26, Section 7.2.4.
7.2.5 Water. Same as Section 7.1.1.
7.2.6 Acetone. Same as Method 5, Section 7.2.
7.3 Quality Assurance Audit Samples. When making compliance
determinations, and upon availability, audit samples may be obtained
from the appropriate EPA regional Office or from the responsible
enforcement authority.

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

8.0 Sample Collection, Preservation, Storage, and Transport

Note: Because of the complexity of this method, testers and
analysts should be trained and experienced with the procedures to
ensure reliable results.

8.1 Sampling.
8.1.1 Pretest Preparation. Follow the general procedure given in
Method 5, Section 8.1, except the filter need only be desiccated and
weighed if a particulate determination will be conducted.
8.1.2 Preliminary Determinations. Same as Method 5, Section 8.2.
8.1.3 Preparation of Sampling Train. Follow the general procedure
given in Method 5, Section 8.1.3, except for the following variations:
Add 50 ml of 0.1 N H2SO4 to the condensate
impinger, if used. Place 100 ml of 0.1 N H2SO4 in
each of the next two impingers. Place 100 ml of 0.1 N NaOH in each of
the following two impingers. Finally, transfer approximately 200-300 g
of preweighed silica gel from its container to the last impinger. Set
up the train as in Figure 26A-1. When used, the optional cyclone is
inserted between the probe liner and filter holder and located in the
heated filter box.
8.1.4 Leak-Check Procedures. Follow the leak-check procedures
given in Method 5, Sections 8.4.2 (Pretest Leak-Check), 8.4.3 (Leak-
Checks During the Sample Run), and 8.4.4 (Post-Test Leak-Check).
8.1.5 Sampling Train Operation. Follow the general procedure given
in Method 5, Section 8.5. It is important to maintain a temperature
around the probe, filter (and cyclone, if used) of greater than
120 deg.C (248 deg.F) since it is extremely difficult to purge acid
gases off these components. (These components are not quantitatively
recovered and hence any collection of acid gases on these components
would result in potential undereporting these emissions. The applicable
subparts may specify alternative higher temperatures.) For each run,
record the data required on a data sheet such as the one shown in
Method 5, Figure 5-3. If the condensate impinger becomes too full, it
may be emptied, recharged with 50 ml of 0.1 N
H2SO4, and replaced during the sample run. The
condensate emptied must be saved and included in the measurement of the
volume of moisture collected and included in the sample for analysis.
The additional 50 ml of absorbing reagent must also be considered in
calculating the moisture. Before the sampling train integrity is
compromised by removing the impinger, conduct a leak-check as described
in Method 5, Section 8.4.2.
8.1.6 Post-Test Moisture Removal (Optional). When the optional
cyclone is included in the sampling train or when liquid is visible on
the filter at the end of a sample run even in the absence of a cyclone,
perform the following procedure. Upon completion of the test run,
connect the ambient air conditioning tube at the probe inlet and
operate the train with the filter heating system at least 120 deg.C
(248 deg.F) at a low flow rate (e.g., H = 1 in.
H2O) to vaporize any liquid and hydrogen halides in the
cyclone or on the filter and pull them through the train into the
impingers. After 30 minutes, turn off the flow, remove the conditioning
tube, and examine the cyclone and filter for any visible liquid. If
liquid is visible, repeat this step for 15 minutes and observe again.
Keep repeating until the cyclone is dry.

[[Page 62094]]

Note: It is critical that this is repeated until the cyclone is
completely dry.

8.2 Sample Recovery. Allow the probe to cool. When the probe can
be handled safely, wipe off all the external surfaces of the tip of the
probe nozzle and place a cap loosely over the tip to prevent gaining or
losing particulate matter. Do not cap the probe tip tightly while the
sampling train is cooling down because this will create a vacuum in the
filter holder, drawing water from the impingers into the holder. Before
moving the sampling train to the cleanup site, remove the probe from
the sample train, wipe off any silicone grease, and cap the open outlet
of the impinger train, being careful not to lose any condensate that
might be present. Wipe off any silicone grease and cap the filter or
cyclone inlet. Remove the umbilical cord from the last impinger and cap
the impinger. If a flexible line is used between the first impinger and
the filter holder, disconnect it at the filter holder and let any
condensed water drain into the first impinger. Wipe off any silicone
grease and cap the filter holder outlet and the impinger inlet. Ground
glass stoppers, plastic caps, serum caps, Teflon tape, Parafilm, or
aluminum foil may be used to close these openings. Transfer the probe
and filter/impinger assembly to the cleanup area. This area should be
clean and protected from the weather to minimize sample contamination
or loss. Inspect the train prior to and during disassembly and note any
abnormal conditions. Treat samples as follows:
8.2.1 Container No. 1 (Optional; Filter Catch for Particulate
Determination). Same as Method 5, Section 8.7.6.1, Container No. 1.
8.2.2 Container No. 2 (Optional; Front-Half Rinse for Particulate
Determination). Same as Method 5, Section 8.7.6.2, Container No. 2.
8.2.3 Container No. 3 (Knockout and Acid Impinger Catch for
Moisture and Hydrogen Halide Determination). Disconnect the impingers.
Measure the liquid in the acid and knockout impingers to 1
ml by using a graduated cylinder or by weighing it to 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. Quantitatively transfer this liquid to a leak-free sample
storage container. Rinse these impingers and connecting glassware
including the back portion of the filter holder (and flexible tubing,
if used) with water and add these rinses to the storage container. Seal
the container, shake to mix, and label. The fluid level should be
marked so that if any sample is lost during transport, a correction
proportional to the lost volume can be applied. Retain rinse water and
acidic absorbing solution blanks to be analyzed with the samples.
8.2.4 Container No. 4 (Alkaline Impinger Catch for Halogen and
Moisture Determination). Measure and record the liquid in the alkaline
impingers as described in Section 8.2.3. Quantitatively transfer this
liquid to a leak-free sample storage container. Rinse these two
impingers and connecting glassware with water and add these rinses to
the container. Add 25 mg of sodium thiosulfate per ppm halogen
anticipated to be in the stack gas multiplied by the volume (dscm) of
stack gas sampled (0.7 mg/ppm-dscf). Seal the container, shake to mix,
and label; mark the fluid level. Retain alkaline absorbing solution
blank to be analyzed with the samples.

Note: 25 mg per sodium thiosulfate per ppm halogen anticipated
to be in the stack includes a safety factor of approximately 5 to
assure complete reaction with the hypohalous acid to form a second
Cl- ion in the alkaline solution.

8.2.5 Container No. 5 (Silica Gel for Moisture Determination).
Same as Method 5, Section 8.7.6.3, Container No. 3.
8.2.6 Container Nos. 6 through 9 (Reagent Blanks). Save portions
of the absorbing reagents (0.1 N H2SO4 and 0.1 N
NaOH) equivalent to the amount used in the sampling train; dilute to
the approximate volume of the corresponding samples using rinse water
directly from the wash bottle being used. Add the same ratio of sodium
thiosulfate solution used in container No. 4 to the 0.1 N NaOH
absorbing reagent blank. Also, save a portion of the rinse water alone
and a portion of the acetone equivalent to the amount used to rinse the
front half of the sampling train. Place each in a separate, prelabeled
sample container.
8.2.7 Prior to shipment, recheck all sample containers to ensure
that the caps are well-secured. Seal the lids of all containers around
the circumference with Teflon tape. Ship all liquid samples upright and
all particulate filters with the particulate catch facing upward.

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures.

------------------------------------------------------------------------
Quality control
Section measure Effect
------------------------------------------------------------------------
8.1.4, 10.1................... Sampling Ensure accurate
equipment leak- measurement of stack
check and gas flow rate,
calibration. sample volume.
11.5.......................... Audit sample Evaluate analyst's
analysis. technique and
standards
preparation.
------------------------------------------------------------------------

9.1 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 Probe Nozzle, Pitot Tube Assembly, Dry Gas Metering System,
Probe Heater, Temperature Sensors, Leak-Check of Metering System, and
Barometer. Same as Method 5, Sections 10.1, 10.2, 10.3, 10.4, 10.5,
8.4.1, and 10.6, respectively.

10.2 Ion Chromatograph.
10.2.1 To prepare the calibration standards, dilute given amounts
(1.0 ml or greater) of the stock standard solutions to convenient
volumes, using 0.1 N H2SO4 or 0.1 N NaOH, as
appropriate. Prepare at least four calibration standards for each
absorbing reagent containing the three stock solutions such that they
are within the linear range of the field samples.
10.2.2 Using one of the standards in each series, ensure adequate
baseline separation for the peaks of interest.
10.2.3 Inject the appropriate series of calibration standards,
starting with the lowest concentration standard first both before and
after injection of the quality control check sample, reagent blanks,
and field samples. This allows compensation for any instrument drift
occurring during sample analysis. The values from duplicate injections
of these calibration samples should agree within 5 percent of their
mean for the analysis to be valid.
10.2.4 Determine the peak areas, or height, of the standards and
plot individual values versus halide ion concentrations in g/
ml.
10.2.5 Draw a smooth curve through the points. Use linear
regression to calculate a formula describing the resulting linear
curve.

11.0 Analytical Procedures

Note: the liquid levels in the sample containers and confirm on
the analysis sheet

[[Page 62095]]

whether or not leakage occurred during transport. If a noticeable
leakage has occurred, either void the sample or use methods, subject
to the approval of the Administrator, to correct the final results.

11.1 Sample Analysis.
11.1.1 The IC conditions will depend upon analytical column type
and whether suppressed or non-suppressed IC is used. An example
chromatogram from a non-suppressed system using a 150-mm Hamilton PRP-
X100 anion column, a 2 ml/min flow rate of a 4 mM 4-hydroxy benzoate
solution adjusted to a pH of 8.6 using 1 N NaOH, a 50 l sample
loop, and a conductivity detector set on 1.0 S full scale is
shown in Figure 26-2.
11.1.2 Before sample analysis, establish a stable baseline. Next,
inject a sample of water, and determine if any Cl-,
Br-, or F- appears in the chromatogram. If any of
these ions are present, repeat the load/injection procedure until they
are no longer present. Analysis of the acid and alkaline absorbing
solution samples requires separate standard calibration curves; prepare
each according to Section 10.2. Ensure adequate baseline separation of
the analyses.
11.1.3 Between injections of the appropriate series of calibration
standards, inject in duplicate the reagent blanks, quality control
sample, and the field samples. Measure the areas or heights of the
Cl-, Br-, and F- peaks. Use the mean
response of the duplicate injections to determine the concentrations of
the field samples and reagent blanks using the linear calibration
curve. The values from duplicate injections should agree within 5
percent of their mean for the analysis to be valid. If the values of
duplicate injections are not within 5 percent of the mean, the
duplicator injections shall be repeated and all four values used to
determine the average response. Dilute any sample and the blank with
equal volumes of water if the concentration exceeds that of the highest
standard.
11.2 Container Nos. 1 and 2 and Acetone Blank (Optional;
Particulate Determination). Same as Method 5, Sections 11.2.1 and
11.2.2, respectively.
11.3 Container No. 5. Same as Method 5, Section 11.2.3 for silica
gel.
11.4 Audit Sample Analysis.
11.4.1 When the method is used to analyze samples to demonstrate
compliance with a source emission regulation, a set of two EPA audit
samples must be analyzed, subject to availability.
11.4.2 Concurrently analyze the audit samples and the compliance
samples in the same manner to evaluate the technique of the analyst and
the standards preparation.
11.4.3 The same analyst, analytical reagents, and analytical
system shall be used for the compliance samples and the EPA audit
samples. If this condition is met, duplicate auditing of subsequent
compliance analyses for the same enforcement agency within a 30-day
period is waived. An audit sample set may not be used to validate
different sets of compliance samples under the jurisdiction of separate
enforcement agencies, unless prior arrangements have been made with
both enforcement agencies.
11.5 Audit Sample Results.
11.5.1 Calculate the concentrations in mg/L of audit sample and
submit results following the instructions provided with the audit
samples.
11.5.2 Report the results of the audit samples and the compliance
determination samples along with their identification numbers, and the
analyst's name to the responsible enforcement authority. Include this
information with reports of any subsequent compliance analyses for the
same enforcement authority during the 30-day period.
11.5.3 The concentrations of the audit samples obtained by the
analyst shall agree within 10 percent of the actual concentrations. If
the 10 percent specification is not met, reanalyze the compliance and
audit samples, and include initial and reanalysis values in the test
report.
11.5.4 Failure to meet the 10 percent specification may require
retests until the audit problems are resolved. However, if the audit
results do not affect the compliance or noncompliance status of the
affected facility, the Administrator may waive the reanalysis
requirement, further audits, or retests and accept the results of the
compliance test. While steps are being taken to resolve audit analysis
problems, the Administrator may also choose to use the data to
determine the compliance or noncompliance status of the affected
facility.

12.0 Data Analysis and Calculations

Note: Retain at least one extra decimal figure beyond those
contained in the available data in intermediate calculations, and
round off only the final answer appropriately.

12.1 Nomenclature. Same as Method 5, Section 12.1. In addition:

BX- = Mass concentration of applicable absorbing solution
blank, g halide ion (Cl-, Br-,
F-)/ml, not to exceed 1 g/ml which is 10 times the
published analytical detection limit of 0.1 g/ml. (It is also
approximately 5 percent of the mass concentration anticipated to result
from a one hour sample at 10 ppmv HCl.)
C = Concentration of hydrogen halide (HX) or halogen (X2),
dry basis, mg/dscm.
K = 10-3 mg/g.
KHCl = 1.028 (g HCl/g-mole)/(g
Cl-/g-mole).
KHBr = 1.013 (g HBr/g-mole)/(g
Br-/g-mole).
KHF = 1.053 (g HF/g-mole)/(g
F-/g-mole).
mHX = Mass of HCl, HBr, or HF in sample, ug.
mX2 = Mass of Cl2 or Br2 in sample,
ug.
SX- = Analysis of sample, ug halide ion (Cl-,
Br-, F-)/ml.
Vs = Volume of filtered and diluted sample, ml.

12.2 Calculate the exact Cl-, Br-, and
F- concentration in the halide salt stock standard solutions
using the following equations.
[GRAPHIC] [TIFF OMITTED] TR17OC00.419

[GRAPHIC] [TIFF OMITTED] TR17OC00.420

12.3 Average Dry Gas Meter Temperature and Average Orifice
Pressure Drop. See data sheet (Figure 5-3 of Method 5).
12.4 Dry Gas Volume. Calculate Vm(std) and adjust for
leakage, if necessary, using the equation in Section 12.3 of Method 5.

[[Page 62096]]

12.5 Volume of Water Vapor and Moisture Content. Calculate the
volume of water vapor Vw(std) and moisture content
Bws from the data obtained in this method (Figure 5-3 of
Method 5); use Equations 5-2 and 5-3 of Method 5.
12.6 Isokinetic Variation and Acceptable Results. Use Method 5,
Section 12.11.
12.7 Acetone Blank Concentration, Acetone Wash Blank Residue
Weight, Particulate Weight, and Particulate Concentration. For
particulate determination.
12.8 Total g HCl, HBr, or HF Per Sample.
[GRAPHIC] [TIFF OMITTED] TR17OC00.421

12.9 Total g Cl2 or Br2 Per Sample.
[GRAPHIC] [TIFF OMITTED] TR17OC00.422

12.10 Concentration of Hydrogen Halide or Halogen in Flue Gas.
[GRAPHIC] [TIFF OMITTED] TR17OC00.423

12.11 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.

3.0 Method Performance

13.1 Precision and Bias. The method has a possible measurable
negative bias below 20 ppm HCl perhaps due to reaction with small
amounts of moisture in the probe and filter. Similar bias for the other
hydrogen halides is possible.
13.2 Sample Stability. The collected Cl-samples can be stored for
up to 4 weeks for analysis for HCl and Cl2.
13.3 Detection Limit. A typical analytical detection limit for HCl
is 0.2 g/ml. Detection limits for the other analyses should be
similar. Assuming 300 ml of liquid recovered for the acidified
impingers and a similar amounts recovered from the basic impingers, and
1 dscm of stack gas sampled, the analytical detection limits in the
stack gas would be about 0.04 ppm for HCl and Cl2, respectively.

14.0 Pollution Prevention, [Reserved]

15.0 Waste Management, [Reserved]

16.0 References

1. Steinsberger, S. C. and J. H. Margeson. Laboratory and Field
Evaluation of a Methodology for Determination of Hydrogen Chloride
Emissions from Municipal and Hazardous Waste Incinerators. U.S.
Environmental Protection Agency, Office of Research and Development.
Publication No. 600/3-89/064. April 1989. Available from National
Technical Information Service, Springfield, VA 22161 as PB89220586/
AS.
2. State of California Air Resources Board. Method 421--
Determination of Hydrochloric Acid Emissions from Stationary
Sources. March 18, 1987.
3. Cheney, J.L. and C.R. Fortune. Improvements in the
Methodology for Measuring Hydrochloric Acid in Combustion Source
Emissions. J. Environ. Sci. Health. A19(3): 337-350. 1984.
4. Stern, D.A., B.M. Myatt, J.F. Lachowski, and K.T. McGregor.
Speciation of Halogen and Hydrogen Halide Compounds in Gaseous
Emissions. In: Incineration and Treatment of Hazardous Waste:
Proceedings of the 9th Annual Research Symposium, Cincinnati, Ohio,
May 2-4, 1983. Publication No. 600/9-84-015. July 1984. Available
from National Technical Information Service, Springfield, VA 22161
as PB84-234525.
5. Holm, R.D. and S.A. Barksdale. Analysis of Anions in
Combustion Products. In: Ion Chromatographic Analysis of
Environmental Pollutants, E. Sawicki, J.D. Mulik, and E.
Wittgenstein (eds.). Ann Arbor, Michigan, Ann Arbor Science
Publishers. 1978. pp. 99-110.
BILLING CODE 6560-50-P

[[Page 62097]]

17.0 Tables, Diagrams, Flowcharts, and Validation Data
[GRAPHIC] [TIFF OMITTED] TR17OC00.424

BILLING CODE 6560-50-C

[[Page 62098]]

Method 27--Determination of Vapor Tightness of Gasoline Delivery
Tank Using Pressure Vaccuum Test

1.0 Scope and Application

1.1 Applicability. This method is applicable for the determination
of vapor tightness of a gasoline delivery collection equipment.

2.0 Summary of Method

2.1 Pressure and vacuum are applied alternately to the
compartments of a gasoline delivery tank and the change in pressure or
vacuum is recorded after a specified period of time.

3.0 Definitions

3.1 Allowable pressure change (p) means the allowable
amount of decrease in pressure during the static pressure test, within
the time period t, as specified in the appropriate regulation, in mm
H2O.
3.2 Allowable vacuum change (v) means the allowable
amount of decrease in vacuum during the static vacuum test, within the
time period t, as specified in the appropriate regulation, in mm
H2O.
3.3 Compartment means a liquid-tight division of a delivery tank.
3.4 Delivery tank means a container, including associated pipes
and fittings, that is attached to or forms a part of any truck,
trailer, or railcar used for the transport of gasoline.
3.5 Delivery tank vapor collection equipment means any piping,
hoses, and devices on the delivery tank used to collect and route
gasoline vapors either from the tank to a bulk terminal vapor control
system or from a bulk plant or service station into the tank.
3.6 Gasoline means a petroleum distillate or petroleum distillate/
alcohol blend having a Reid vapor pressure of 27.6 kilopascals or
greater which is used as a fuel for internal combustion engines.
3.7 Initial pressure (Pi) means the pressure applied to
the delivery tank at the beginning of the static pressure test, as
specified in the appropriate regulation, in mm H2O.
3.8 Initial vacuum (Vi) means the vacuum applied to the
delivery tank at the beginning of the static vacuum test, as specified
in the appropriate regulation, in mm H3.
3.9 Time period of the pressure or vacuum test (t) means the time
period of the test, as specified in the appropriate regulation, during
which the change in pressure or vacuum is monitored, in minutes.

4.0 Interferences [Reserved]

5.0 Safety

5.1 Gasoline contains several volatile organic compounds (e.g.
benzene and hexane) which presents a potential for fire and/or
explosions. It is advisable to take appropriate precautions when
testing a gasoline vessel's vapor tightness, such as refraining from
smoking and using explosion-proof equipment.
5.2 This method may involve hazardous materials, operations, and
equipment. This test method may not address all of the safety problems
associated with its use. It is the responsibility of the user of this
test method to establish appropriate safety and health practices and
determine the applicability of regulatory limitations prior to
performing this test method

6.0 Equipment and Supplies

The following equipment and supplies are required for testing:
6.1 Pressure Source. Pump or compressed gas cylinder of air or
inert gas sufficient to pressurize the delivery tank to 500 mm (20 in.)
H2O above atmospheric pressure.
6.2 Regulator. Low pressure regulator for controlling
pressurization of the delivery tank.
6.3 Vacuum Source. Vacuum pump capable of evacuating the delivery
tank to 250 mm (10 in.) H2O below atmospheric pressure.
6.4 Pressure-Vacuum Supply Hose.
6.5 Manometer. Liquid manometer, or equivalent instrument, capable
of measuring up to 500 mm (20 in.) H2O gauge pressure with
2.5 mm (0.1 in.) H2O precision.
6.6 Pressure-Vacuum Relief Valves. The test apparatus shall be
equipped with an inline pressure-vacuum relief valve set to activate at
675 mm (26.6 in.) H2O above atmospheric pressure or 250 mm
(10 in.) H2O below atmospheric pressure, with a capacity equal to the
pressurizing or evacuating pumps.
6.7 Test Cap for Vapor Recovery Hose. This cap shall have a tap
for manometer connection and a fitting with shut-off valve for
connection to the pressure-vacuum supply hose.
6.8 Caps for Liquid Delivery Hoses.

7.0 Reagents and Standards [Reserved]

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Pretest Preparations.
8.1.1 Summary. Testing problems may occur due to the presence of
volatile vapors and/or temperature fluctuations inside the delivery
tank. Under these conditions, it is often difficult to obtain a stable
initial pressure at the beginning of a test, and erroneous test results
may occur. To help prevent this, it is recommended that prior to
testing, volatile vapors be removed from the tank and the temperature
inside the tank be allowed to stabilize. Because it is not always
possible to completely attain these pretest conditions, a provision to
ensure reproducible results is included. The difference in results for
two consecutive runs must meet the criteria in Sections 8.2.2.5 and
8.2.3.5.
8.1.2 Emptying of Tank. The delivery tank shall be emptied of all
liquid.
8.1.3 Purging of Vapor. As much as possible the delivery tank
shall be purged of all volatile vapors by any safe, acceptable method.
One method is to carry a load of non-volatile liquid fuel, such as
diesel or heating oil, immediately prior to the test, thus flushing out
all the volatile gasoline vapors. A second method is to remove the
volatile vapors by blowing ambient air into each tank compartment for
at least 20 minutes. This second method is usually not as effective and
often causes stabilization problems, requiring a much longer time for
stabilization during the testing.
8.1.4 Temperature Stabilization. As much as possible, the test
shall be conducted under isothermal conditions. The temperature of the
delivery tank should be allowed to equilibrate in the test environment.
During the test, the tank should be protected from extreme
environmental and temperature variability, such as direct sunlight.
8.2 Test Procedure.
8.2.1 Preparations.
8.2.1.1 Open and close each dome cover.
8.2.1.2 Connect static electrical ground connections to the tank.
Attach the liquid delivery and vapor return hoses, remove the liquid
delivery elbows, and plug the liquid delivery fittings.

Note: The purpose of testing the liquid delivery hoses is to
detect tears or holes that would allow liquid leakage during a
delivery. Liquid delivery hoses are not considered to be possible
sources of vapor leakage, and thus, do not have to be attached for a
vapor leakage test. Instead, a liquid delivery hose could be either
visually inspected, or filled with water to detect any liquid
leakage.

8.2.1.3 Attach the test cap to the end of the vapor recovery hose.
8.2.1.4 Connect the pressure-vacuum supply hose and the pressure-
vacuum relief valve to the shut-off valve. Attach a manometer to the
pressure tap.
8.2.1.5 Connect compartments of the tank internally to each other
if possible.

[[Page 62099]]

If not possible, each compartment must be tested separately, as if it
were an individual delivery tank.
8.2.2 Pressure Test.
8.2.2.1 Connect the pressure source to the pressure-vacuum supply
hose.
8.2.2.2 Open the shut-off valve in the vapor recovery hose cap.
Apply air pressure slowly, pressurize the tank to Pi, the
initial pressure specified in the regulation.
8.2.2.3 Close the shut-off and allow the pressure in the tank to
stabilize, adjusting the pressure if necessary to maintain pressure of
Pi. When the pressure stabilizes, record the time and
initial pressure.
8.2.2.4 At the end of the time period (t) specified in the
regulation, record the time and final pressure.
8.2.2.5 Repeat steps 8.2.2.2 through 8.2.2.4 until the change in
pressure for two consecutive runs agrees within 12.5 mm (0.5 in.)
H2O. Calculate the arithmetic average of the two results.
8.2.2.6 Compare the average measured change in pressure to the
allowable pressure change, p, specified in the regulation. If
the delivery tank does not satisfy the vapor tightness criterion
specified in the regulation, repair the sources of leakage, and repeat
the pressure test until the criterion is met.
8.2.2.7 Disconnect the pressure source from the pressure-vacuum
supply hose, and slowly open the shut-off valve to bring the tank to
atmospheric pressure.
8.2.3 Vacuum Test.
8.2.3.1 Connect the vacuum source to the pressure-vacuum supply
hose.
8.2.3.2 Open the shut-off valve in the vapor recovery hose cap.
Slowly evacuate the tank to Vi, the initial vacuum specified
in the regulation.
8.2.3.3 Close the shut-off valve and allow the pressure in the
tank to stabilize, adjusting the pressure if necessary to maintain a
vacuum of Vi. When the pressure stabilizes, record the time
and initial vacuum.
8.2.3.4 At the end of the time period specified in the regulation
(t), record the time and final vacuum.
8.2.3.5 Repeat steps 8.2.3.2 through 8.2.3.4 until the change in
vacuum for two consecutive runs agrees within 12.5 mm (0.5 in.)
H2O. Calculate the arithmetic average of the two results.
8.2.3.6 Compare the average measured change in vacuum to the
allowable vacuum change, v, as specified in the regulation. If
the delivery tank does not satisfy the vapor tightness criterion
specified in the regulation, repair the sources of leakage, and repeat
the vacuum test until the criterion is met.
8.2.3.7 Disconnect the vacuum source from the pressure-vacuum
supply hose, and slowly open the shut-off valve to bring the tank to
atmospheric pressure.
8.2.4 Post-Test Clean-up. Disconnect all test equipment and return
the delivery tank to its pretest condition.

9.0 Quality Control

------------------------------------------------------------------------
Quality control
Section(s) measure Effect
------------------------------------------------------------------------
8.2.2.5, 8.3.3.5.............. Repeat test Ensures data
procedures until precision.
change in
pressure or
vacuum for two
consecutive runs
agrees within

12.5 mm (0.5
in.) H2O.
------------------------------------------------------------------------

10.0 Calibration and Standardization [Reserved]

11.0 Analytical Procedures [Reserved]

12.0 Data Analysis and Calculations [Reserved]

13.0 Method Performance

13.1 Precision. The vapor tightness of a gasoline delivery tank
under positive or negative pressure, as measured by this method, is
precise within 12.5 mm (0.5 in.) H2O
13.2 Bias. No bias has been identified.

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 Alternative Procedures

16.1 The pumping of water into the bottom of a delivery tank is an
acceptable alternative to the pressure source described above.
Likewise, the draining of water out of the bottom of a delivery tank
may be substituted for the vacuum source. Note that some of the
specific step-by-step procedures in the method must be altered slightly
to accommodate these different pressure and vacuum sources.
16.2 Techniques other than specified above may be used for purging
and pressurizing a delivery tank, if prior approval is obtained from
the Administrator. Such approval will be based upon demonstrated
equivalency with the above method.

17.0 References [Reserved]

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

Method 28--Certification and Auditing of Wood Heaters

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, Method 4,
Method 5, Method 5G, Method 5H, Method 6, Method 6C, and Method 16A.

1.0 Scope and Application

1.1 Analyte. Particulate matter (PM). No CAS number assigned.
1.2 Applicability. This method is applicable for the certification
and auditing of wood heaters, including pellet burning 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 emissions are measured from a wood heater
burning a prepared test fuel crib in a test facility maintained at a
set of prescribed conditions. Procedures for determining burn rates and
particulate emission rates and for reducing data are provided.

3.0 Definitions

3.1 2 x 4 or 4 x 4 means two inches by four inches or four
inches by four inches (50 mm by 100 mm or 100 mm by 100 mm), as nominal
dimensions for lumber.
3.2 Burn rate means the rate at which test fuel is consumed in a
wood heater. Measured in kilograms or lbs of wood (dry basis) per hour
(kg/hr or lb/hr).
3.3 Certification or audit test means a series of at least four
test runs conducted for certification or audit purposes that meets the
burn rate specifications in Section 8.4.
3.4 Firebox means the chamber in the wood heater in which the test
fuel charge is placed and combusted.
3.5 Height means the vertical distance extending above the loading
door, if fuel could reasonably occupy that space, but not more than 2
inches above the top (peak height) of the loading door, to the floor of
the firebox

[[Page 62100]]

(i.e., below a permanent grate) if the grate allows a 1-inch diameter
piece of wood to pass through the grate, or, if not, to the top of the
grate. Firebox height is not necessarily uniform but must account for
variations caused by internal baffles, air channels, or other permanent
obstructions.
3.6 Length means the longest horizontal fire chamber dimension
that is parallel to a wall of the chamber.
3.7 Pellet burning wood heater means a wood heater which meets the
following criteria: (1) The manufacturer makes no reference to burning
cord wood in advertising or other literature, (2) the unit is safety
listed for pellet fuel only, (3) the unit operating and instruction
manual must state that the use of cordwood is prohibited by law, and
(4) the unit must be manufactured and sold including the hopper and
auger combination as integral parts.
3.8 Secondary air supply means an air supply that introduces air
to the wood heater such that the burn rate is not altered by more than
25 percent when the secondary air supply is adjusted during the test
run. The wood heater manufacturer can document this through design
drawings that show the secondary air is introduced only into a mixing
chamber or secondary chamber outside the firebox.
3.9 Test facility means the area in which the wood heater is
installed, operated, and sampled for emissions.
3.10 Test fuel charge means the collection of test fuel pieces
placed in the wood heater at the start of the emission test run.
3.11 Test fuel crib means the arrangement of the test fuel charge
with the proper spacing requirements between adjacent fuel pieces.
3.12 Test fuel loading density means the weight of the as-fired
test fuel charge per unit volume of usable firebox.
3.13 Test fuel piece means the 2 x 4 or 4 x 4 wood piece cut
to the length required for the test fuel charge and used to construct
the test fuel crib.
3.14 Test run means an individual emission test which encompasses
the time required to consume the mass of the test fuel charge.
3.15 Usable firebox volume means the volume of the firebox
determined using its height, length, and width as defined in this
section.
3.16 Width means the shortest horizontal fire chamber dimension
that is parallel to a wall of the chamber.
3.17 Wood heater means an enclosed, woodburning appliance capable
of and intended for space heating or domestic water heating, as defined
in the applicable regulation.

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.

6.0 Equipment and Supplies

Same as Section 6.0 of either Method 5G or Method 5H, with the
addition of the following:
6.1 Insulated Solid Pack Chimney. For installation of wood
heaters. Solid pack insulated chimneys shall have a minimum of 2.5 cm
(1 in.) solid pack insulating material surrounding the entire flue and
possess a label demonstrating conformance to U.L. 103 (incorporated by
reference--see Sec. 60.17).
6.2 Platform Scale and Monitor. For monitoring of fuel load weight
change. The scale shall be capable of measuring weight to within 0.05
kg (0.1 lb) or 1 percent of the initial test fuel charge weight,
whichever is greater.
6.3 Wood Heater Temperature Monitors. Seven, each capable of
measuring temperature to within 1.5 percent of expected absolute
temperatures.
6.4 Test Facility Temperature Monitor. A thermocouple located
centrally in a vertically oriented 150 mm (6 in.) long, 50 mm (2 in.)
diameter pipe shield that is open at both ends, capable of measuring
temperature to within 1.5 percent of expected temperatures.
6.5 Balance (optional). Balance capable of weighing the test fuel
charge to within 0.05 kg (0.1 lb).
6.6 Moisture Meter. Calibrated electrical resistance meter for
measuring test fuel moisture to within 1 percent moisture content.
6.7 Anemometer. Device capable of detecting air velocities less
than 0.10 m/sec (20 ft/min), for measuring air velocities near the test
appliance.
6.8 Barometer. Mercury, aneroid or other barometer capable of
measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg).
6.9 Draft Gauge. Electromanometer or other device for the
determination of flue draft or static pressure readable to within 0.50
Pa (0.002 in. H2O).
6.10 Humidity Gauge. Psychrometer or hygrometer for measuring room
humidity.
6.11 Wood Heater Flue.
6.11.1 Steel flue pipe extending to 2.6 0.15 m (8.5
0.5 ft) above the top of the platform scale, and above
this level, insulated solid pack type chimney extending to 4.6
0.3 m (15 1 ft) above the platform scale, and
of the size specified by the wood heater manufacturer. This applies to
both freestanding and insert type wood heaters.
6.11.2 Other chimney types (e.g., solid pack insulated pipe) may
be used in place of the steel flue pipe if the wood heater
manufacturer's written appliance specifications require such chimney
for home installation (e.g., zero clearance wood heater inserts). Such
alternative chimney or flue pipe must remain and be sealed with the
wood heater following the certification test.
6.12 Test Facility. The test facility shall meet the following
requirements during testing:
6.12.1 The test facility temperature shall be maintained between
18 and 32 deg.C (65 and 90 deg.F) during each test run.
6.12.2 Air velocities within 0.6 m (2 ft) of the test appliance
and exhaust system shall be less than 0.25 m/sec (50 ft/min) without
fire in the unit.
6.12.3 The flue shall discharge into the same space or into a
space freely communicating with the test facility. Any hood or similar
device used to vent combustion products shall not induce a draft
greater than 1.25 Pa (0.005 in. H2O) on the wood heater
measured when the wood heater is not operating.
6.12.4 For test facilities with artificially induced barometric
pressures (e.g., pressurized chambers), the barometric pressure in the
test facility shall not exceed 775 mm Hg (30.5 in. Hg) during any test
run.

7.0 Reagents and Standards

Same as Section 6.0 of either Method 5G or Method 5H, with the
addition of the following:
7.1 Test Fuel. The test fuel shall conform to the following
requirements:
7.1.1 Fuel Species. Untreated, air-dried, Douglas fir lumber.
Kiln-dried lumber is not permitted. The lumber shall be certified C
grade (standard) or better Douglas fir by a lumber grader at the mill
of origin as specified in the West Coast Lumber Inspection Bureau
Standard No. 16 (incorporated by reference--see Sec. 60.17).
7.1.2 Fuel Moisture. The test fuel shall have a moisture content
range between 16 to 20 percent on a wet basis (19 to 25 percent dry
basis). Addition of moisture to previously dried wood is not allowed.
It is recommended that the test fuel be stored in a temperature and
humidity-controlled room.

[[Page 62101]]

7.1.3 Fuel Temperature. The test fuel shall be at the test
facility temperature of 18 to 32 deg.C (65 to 90 deg.F).
7.1.4 Fuel Dimensions. The dimensions of each test fuel piece
shall conform to the nominal measurements of 2 x 4 and 4 x 4 lumber.
Each piece of test fuel (not including spacers) shall be of equal
length, except as necessary to meet requirements in Section 8.8, and
shall closely approximate \5/6\ the dimensions of the length of the
usable firebox. The fuel piece dimensions shall be determined in
relation to the appliance's firebox volume according to guidelines
listed below:
7.1.4.1 If the usable firebox volume is less than or equal to
0.043 m3 (1.5 ft3), use 2 x 4 lumber.
7.1.4.2 If the usable firebox volume is greater than 0.043
m3 (1.5 ft3) and less than or equal to 0.085
m3 (3.0 ft3), use 2 x 4 and 4 x 4 lumber. About
half the weight of the test fuel charge shall be 2 x 4 lumber, and the
remainder shall be 4 x 4 lumber.
7.1.4.3 If the usable firebox volume is greater than 0.085
m3 (3.0 ft3), use 4 x 4 lumber.
7.2 Test Fuel Spacers. Air-dried, Douglas fir lumber meeting the
requirements outlined in Sections 7.1.1 through 7.1.3. The spacers
shall be 130 x 40 x 20 mm (5 x 1.5 x 0.75 in.).

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Test Run Requirements.
8.1.1 Burn Rate Categories. One emission test run is required in
each of the following burn rate categories:

Burn Rate Categories
[Average kg/hr (lb/hr), dry basis]
----------------------------------------------------------------------------------------------------------------
Category 1 Category 2 Category 3 Category 4
----------------------------------------------------------------------------------------------------------------
0.80................................. 0.80 to 1.25........... 1.25 to 1.90........... Maximum.
(1.76)............................... (1.76 to 2.76)......... (2.76 to 4.19)......... burn rate.
----------------------------------------------------------------------------------------------------------------

8.1.1.1 Maximum Burn Rate. For Category 4, the wood heater shall
be operated with the primary air supply inlet controls fully open (or,
if thermostatically controlled, the thermostat shall be set at maximum
heat output) during the entire test run, or the maximum burn rate
setting specified by the manufacturer's written instructions.
8.1.1.2 Other Burn Rate Categories. For burn rates in Categories 1
through 3, the wood heater shall be operated with the primary air
supply inlet control, or other mechanical control device, set at a
predetermined position necessary to obtain the average burn rate
required for the category.
8.1.1.3 Alternative Burn Rates for Burn Rate Categories 1 and 2.
8.1.1.3.1 If a wood heater cannot be operated at a burn rate below
0.80 kg/hr (1.76 lb/hr), two test runs shall be conducted with burn
rates within Category 2. If a wood heater cannot be operated at a burn
rate below 1.25 kg/hr (2.76 lb/hr), the flue shall be dampered or the
air supply otherwise controlled in order to achieve two test runs
within Category 2.
8.1.1.3.2 Evidence that a wood heater cannot be operated at a burn
rate less than 0.80 kg/hr shall include documentation of two or more
attempts to operate the wood heater in burn rate Category 1 and fuel
combustion has stopped, or results of two or more test runs
demonstrating that the burn rates were greater than 0.80 kg/hr when the
air supply controls were adjusted to the lowest possible position or
settings. Stopped fuel combustion is evidenced when an elapsed time of
30 minutes or more has occurred without a measurable ( 0.05 kg (0.1 lb)
or 1.0 percent, whichever is greater) weight change in the test fuel
charge. See also Section 8.8.3. Report the evidence and the reasoning
used to determine that a test in burn rate Category 1 cannot be
achieved; for example, two unsuccessful attempts to operate at a burn
rate of 0.4 kg/hr are not sufficient evidence that burn rate Category 1
cannot be achieved.

Note: After July 1, 1990, if a wood heater cannot be operated at
a burn rate less than 0.80 kg/hr, at least one test run with an
average burn rate of 1.00 kg/hr or less shall be conducted.
Additionally, if flue dampering must be used to achieve burn rates
below 1.25 kg/hr (or 1.0 kg/hr), results from a test run conducted
at burn rates below 0.90 kg/hr need not be reported or included in
the test run average provided that such results are replaced with
results from a test run meeting the criteria above.

8.2 Catalytic Combustor and Wood Heater Aging. The catalyst-
equipped wood heater or a wood heater of any type shall be aged before
the certification test begins. The aging procedure shall be conducted
and documented by a testing laboratory accredited according to
procedures in Sec. 60.535 of 40 CFR part 60.
8.2.1 Catalyst-equipped Wood Heater. Operate the catalyst-equipped
wood heater using fuel meeting the specifications outlined in Sections
7.1.1 through 7.1.3, or cordwood with a moisture content between 15 and
25 percent on a wet basis. Operate the wood heater at a medium burn
rate (Category 2 or 3) with a new catalytic combustor in place and in
operation for at least 50 hours. Record and report hourly catalyst exit
temperature data (Section 8.6.2) and the hours of operation.
8.2.2 Non-Catalyst Wood Heater. Operate the wood heater using the
fuel described in Section 8.4.1 at a medium burn rate for at least 10
hours. Record and report the hours of operation.
8.3 Pretest Recordkeeping. Record the test fuel charge dimensions
and weights, and wood heater and catalyst descriptions as shown in the
example in Figure 28-1.
8.4 Wood Heater Installation. Assemble the wood heater appliance
and parts in conformance with the manufacturer's written installation
instructions. Place the wood heater centrally on the platform scale and
connect the wood heater to the flue described in Section 6.11. Clean
the flue with an appropriately sized, wire chimney brush before each
certification test.
8.5 Wood Heater Temperature Monitors.
8.5.1 For catalyst-equipped wood heaters, locate a temperature
monitor (optional) about 25 mm (1 in.) upstream of the catalyst at the
centroid of the catalyst face area, and locate a temperature monitor
(mandatory) that will indicate the catalyst exhaust temperature. This
temperature monitor is centrally located within 25 mm (1 in.)
downstream at the centroid of catalyst face area. Record these
locations.
8.5.2 Locate wood heater surface temperature monitors at five
locations on the wood heater firebox exterior surface. Position the
temperature monitors centrally on the top surface, on two sidewall
surfaces, and on the bottom and back surfaces. Position the monitor
sensing tip on the firebox exterior surface inside of any heat shield,
air circulation walls, or other

[[Page 62102]]

wall or shield separated from the firebox exterior surface. Surface
temperature locations for unusual design shapes (e.g., spherical, etc.)
shall be positioned so that there are four surface temperature monitors
in both the vertical and horizontal planes passing at right angles
through the centroid of the firebox, not including the fuel loading
door (total of five temperature monitors).
8.6 Test Facility Conditions.
8.6.1 Locate the test facility temperature monitor on the
horizontal plane that includes the primary air intake opening for the
wood heater. Locate the temperature monitor 1 to 2 m (3 to 6 ft) from
the front of the wood heater in the 90 deg. sector in front of the wood
heater.
8.6.2 Use an anemometer to measure the air velocity. Measure and
record the room air velocity before the pretest ignition period
(Section 8.7) and once immediately following the test run completion.
8.6.3 Measure and record the test facility's ambient relative
humidity, barometric pressure, and temperature before and after each
test run.
8.6.4 Measure and record the flue draft or static pressure in the
flue at a location no greater than 0.3 m (1 ft) above the flue
connector at the wood heater exhaust during the test run at the
recording intervals (Section 8.8.2).
8.7 Wood Heater Firebox Volume.
8.7.1 Determine the firebox volume using the definitions for
height, width, and length in Section 3. Volume adjustments due to
presence of firebrick and other permanent fixtures may be necessary.
Adjust width and length dimensions to extend to the metal wall of the
wood heater above the firebrick or permanent obstruction if the
firebrick or obstruction extending the length of the side(s) or back
wall extends less than one-third of the usable firebox height. Use the
width or length dimensions inside the firebrick if the firebrick
extends more than one-third of the usable firebox height. If a log
retainer or grate is a permanent fixture and the manufacturer
recommends that no fuel be placed outside the retainer, the area
outside of the retainer is excluded from the firebox volume
calculations.
8.7.2 In general, exclude the area above the ash lip if that area
is less than 10 percent of the usable firebox volume. Otherwise, take
into account consumer loading practices. For instance, if fuel is to be
loaded front-to-back, an ash lip may be considered usable firebox
volume.
8.7.3 Include areas adjacent to and above a baffle (up to two
inches above the fuel loading opening) if four inches or more
horizontal space exist between the edge of the baffle and a vertical
obstruction (e.g., sidewalls or air channels).
8.8 Test Fuel Charge.
8.8.1 Prepare the test fuel pieces in accordance with the
specifications outlined in Sections 7.1 and 7.2. Determine the test
fuel moisture content with a calibrated electrical resistance meter or
other equivalent performance meter. If necessary, convert fuel moisture
content values from dry basis (%Md) to wet basis
(%Mw) in Section 12.2 using Equation 28-1. Determine fuel
moisture for each fuel piece (not including spacers) by averaging at
least three moisture meter readings, one from each of three sides,
measured parallel to the wood grain. Average all the readings for all
the fuel pieces in the test fuel charge. If an electrical resistance
type meter is used, penetration of insulated electrodes shall be one-
fourth the thickness of the test fuel piece or 19 mm (0.75 in.),
whichever is greater. Measure the moisture content within a 4-hour
period prior to the test run. Determine the fuel temperature by
measuring the temperature of the room where the wood has been stored
for at least 24 hours prior to the moisture determination.
8.8.2 Attach the spacers to the test fuel pieces with uncoated,
ungalvanized nails or staples as illustrated in Figure 28-2. Attachment
of spacers to the top of the test fuel piece(s) on top of the test fuel
charge is optional.
8.8.3 To avoid stacking difficulties, or when a whole number of
test fuel pieces does not result, all piece lengths shall be adjusted
uniformly to remain within the specified loading density. The shape of
the test fuel crib shall be geometrically similar to the shape of the
firebox volume without resorting to special angular or round cuts on
the individual fuel pieces.
8.8.4 The test fuel loading density shall be 112 11.2
kg/m3 (7 0.7
lb/ft3) of usable firebox volume on a wet basis.
8.9 Sampling Equipment. Prepare the sampling equipment as defined
by the selected method (i.e., either Method 5G or Method 5H). Collect
one particulate emission sample for each test run.
8.10 Secondary Air Adjustment Validation.
8.10.1 If design drawings do not show the introduction of
secondary air into a chamber outside the firebox (see ``secondary air
supply'' under Section 3.0, Definitions), conduct a separate test of
the wood heater's secondary air supply. Operate the wood heater at a
burn rate in Category 1 (Section 8.1.1) with the secondary air supply
operated following the manufacturer's written instructions. Start the
secondary air validation test run as described in Section 8.8.1, except
no emission sampling is necessary and burn rate data shall be recorded
at 5-minute intervals.
8.10.2 After the start of the test run, operate the wood heater
with the secondary air supply set as per the manufacturer's
instructions, but with no adjustments to this setting. After 25 percent
of the test fuel has been consumed, adjust the secondary air supply
controls to another setting, as per the manufacturer's instructions.
Record the burn rate data (5-minute intervals) for 20 minutes following
the air supply adjustment.
8.10.3 Adjust the air supply control(s) to the original
position(s), operate at this condition for at least 20 minutes, and
repeat the air supply adjustment procedure above. Repeat the procedure
three times at equal intervals over the entire burn period as defined
in Section 8.8. If the secondary air adjustment results in a burn rate
change of more than an average of 25 percent between the 20-minute
periods before and after the secondary adjustments, the secondary air
supply shall be considered a primary air supply, and no adjustment to
this air supply is allowed during the test run.
8.10.4 The example sequence below describes a typical secondary
air adjustment validation check. The first cycle begins after at least
25 percent of the test fuel charge has been consumed.

Cycle 1
Part 1, sec air adjusted to final position--20 min
Part 2, sec air adjusted to final position--20 min
Part 3, sec air adjusted to final position--20 min
Cycle 2
Part 1, sec air adjusted to final position--20 min
Part 2, sec air adjusted to final position--20 min
Part 3, sec air adjusted to final position--20 min
Cycle 3
Part 1, sec air adjusted to final position--20 min
Part 2, sec air adjusted to final position--20 min
Part 3, sec air adjusted to final position--20 min

Note that the cycles may overlap; that is, Part 3 of Cycle 1 may
coincide in part or in total with Part 1 of Cycle 2. The calculation of
the secondary air percent effect for this example is as follows:

[[Page 62103]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.425

8.11 Pretest Ignition. Build a fire in the wood heater in
accordance with the manufacturer's written instructions.
8.11.1 Pretest Fuel Charge. Crumpled newspaper loaded with
kindling may be used to help ignite the pretest fuel. The pretest fuel,
used to sustain the fire, shall meet the same fuel requirements
prescribed in Section 7.1. The pretest fuel charge shall consist of
whole 2 x 4's that are no less than \1/3\ the length of the test fuel
pieces. Pieces of 4 x 4 lumber in approximately the same weight ratio
as for the test fuel charge may be added to the pretest fuel charge.
8.11.2 Wood Heater Operation and Adjustments. Set the air inlet
supply controls at any position that will maintain combustion of the
pretest fuel load. At least one hour before the start of the test run,
set the air supply controls at the approximate positions necessary to
achieve the burn rate desired for the test run. Adjustment of the air
supply controls, fuel addition or subtractions, and coalbed raking
shall be kept to a minimum but are allowed up to 15 minutes prior to
the start of the test run. For the purposes of this method, coalbed
raking is the use of a metal tool (poker) to stir coals, break burning
fuel into smaller pieces, dislodge fuel pieces from positions of poor
combustion, and check for the condition of uniform charcoalization.
Record all adjustments made to the air supply controls, adjustments to
and additions or subtractions of fuel, and any other changes to wood
heater operations that occur during pretest ignition period. Record
fuel weight data and wood heater temperature measurements at 10-minute
intervals during the hour of the pretest ignition period preceding the
start of the test run. During the 15-minute period prior to the start
of the test run, the wood heater loading door shall not be open more
than a total of 1 minute. Coalbed raking is the only adjustment allowed
during this period.

Note: One purpose of the pretest ignition period is to achieve
uniform charcoalization of the test fuel bed prior to loading the
test fuel charge. Uniform charcoalization is a general condition of
the test fuel bed evidenced by an absence of large pieces of burning
wood in the coal bed and the remaining fuel pieces being brittle
enough to be broken into smaller charcoal pieces with a metal poker.
Manipulations to the fuel bed prior to the start of the test run
should be done to achieve uniform charcoalization while maintaining
the desired burn rate. In addition, some wood heaters (e.g., high
mass units) may require extended pretest burn time and fuel
additions to reach an initial average surface temperature sufficient
to meet the thermal equilibrium criteria in Section 8.3.

8.11.3 The weight of pretest fuel remaining at the start of the
test run is determined as the difference between the weight of the wood
heater with the remaining pretest fuel and the tare weight of the
cleaned, dry wood heater with or without dry ash or sand added
consistent with the manufacturer's instructions and the owner's manual.
The tare weight of the wood heater must be determined with the wood
heater (and ash, if added) in a dry condition.
8.12 Test Run. Complete a test run in each burn rate category, as
follows:
8.12.1 Test Run Start.
8.12.1.1 When the kindling and pretest fuel have been consumed to
leave a fuel weight between 20 and 25 percent of the weight of the test
fuel charge, record the weight of the fuel remaining and start the test
run. Record and report any other criteria, in addition to those
specified in this section, used to determine the moment of the test run
start (e.g., firebox or catalyst temperature), whether such criteria
are specified by the wood heater manufacturer or the testing
laboratory. Record all wood heater individual surface temperatures,
catalyst temperatures, any initial sampling method measurement values,
and begin the particulate emission sampling. Within 1 minute following
the start of the test run, open the wood heater door, load the test
fuel charge, and record the test fuel charge weight. Recording of
average, rather than individual, surface temperatures is acceptable for
tests conducted in accordance with Sec. 60.533(o)(3)(i) of 40 CFR part
60.
8.12.1.2 Position the fuel charge so that the spacers are parallel
to the floor of the firebox, with the spacer edges abutting each other.
If loading difficulties result, some fuel pieces may be placed on edge.
If the usable firebox volume is between 0.043 and 0.085 m3
(1.5 and 3.0 ft3), alternate the piece sizes in vertical
stacking layers to the extent possible. For example, place 2 x 4's on
the bottom layer in direct contact with the coal bed and 4 x 4's on
the next layer, etc. (See Figure 28-3). Position the fuel pieces
parallel to each other and parallel to the longest wall of the firebox
to the extent possible within the specifications in Section 8.8.
8.12.1.3 Load the test fuel in appliances having unusual or
unconventional firebox design maintaining air space intervals between
the test fuel pieces and in conformance with the manufacturer's written
instructions. For any appliance that will not accommodate the loading
arrangement specified in the paragraph above, the test facility
personnel shall contact the Administrator for an alternative loading
arrangement.
8.12.1.4 The wood heater door may remain open and the air supply
controls adjusted up to five minutes after the start of the test run in
order to make adjustments to the test fuel charge and to ensure
ignition of the test fuel charge has occurred. Within the five minutes
after the start of the test run, close the wood heater door and adjust
the air supply controls to the position determined to produce the
desired burn rate. No other adjustments to the air supply controls or
the test fuel charge are allowed (except as specified in Sections
8.12.3 and 8.12.4) after the first five minutes of the test run. Record
the length of time the wood heater door remains open, the adjustments
to the air supply controls, and any other operational adjustments.
8.12.2 Data Recording. Record on a data sheet similar to that
shown in Figure 28-4, at intervals no greater than 10 minutes, fuel
weight data, wood heater individual surface and catalyst temperature
measurements, other wood heater operational data (e.g., draft), test
facility temperature and sampling method data.
8.12.3 Test Fuel Charge Adjustment. The test fuel charge may be
adjusted (i.e., repositioned) once during a test run if more than 60
percent of the initial test fuel charge weight has been consumed and
more than 10 minutes have elapsed without a measurable (0.05 kg (0.1
lb) or 1.0 percent, whichever is greater) weight change. The time used
to make this adjustment shall be less than 15 seconds.
8.12.4 Air Supply Adjustment. Secondary air supply controls may be
adjusted once during the test run following the manufacturer's written
instructions (see Section 8.10). No other air supply adjustments are
allowed during the test run. Recording of wood heater flue draft during
the test run is optional for tests conducted in

[[Page 62104]]

accordance with Sec. 60.533(o)(3)(i) of 40 CFR part 60.
8.12.5 Auxiliary Wood Heater Equipment Operation. Heat exchange
blowers sold with the wood heater shall be operated during the test run
following the manufacturer's written instructions. If no manufacturer's
written instructions are available, operate the heat exchange blower in
the ``high'' position. (Automatically operated blowers shall be
operated as designed.) Shaker grates, by-pass controls, or other
auxiliary equipment may be adjusted only one time during the test run
following the manufacturer's written instructions.
Record all adjustments on a wood heater operational written record.

Note: If the wood heater is sold with a heat exchange blower as
an option, test the wood heater with the heat exchange blower
operating as described in Sections 8.1 through 8.12 and report the
results. As an alternative to repeating all test runs without the
heat exchange blower operating, one additional test run may be
without the blower operating as described in Section 8.12.5 at a
burn rate in Category 2 (Section 8.1.1). If the emission rate
resulting from this test run without the blower operating is equal
to or less than the emission rate plus 1.0 g/hr (0.0022 lb/hr) for
the test run in burn rate Category 2 with the blower operating, the
wood heater may be considered to have the same average emission rate
with or without the blower operating. Additional test runs without
the blower operating are unnecessary.

8.13 Test Run Completion. Continue emission sampling and wood
heater operation for 2 hours. The test run is completed when the
remaining weight of the test fuel charge is 0.00 kg (0.0 lb). End the
test run when the scale has indicated a test fuel charge weight of 0.00
kg (0.0 lb) or less for 30 seconds. At the end of the test run, stop
the particulate sampling, and record the final fuel weight, the run
time, and all final measurement values.
8.14 Wood Heater Thermal Equilibrium. The average of the wood
heater surface temperatures at the end of the test run shall agree with
the average surface temperature at the start of the test run to within
70 deg.C (126 deg.F).
8.15 Consecutive Test Runs. Test runs on a wood heater may be
conducted consecutively provided that a minimum one-hour interval
occurs between test runs.
8.16 Additional Test Runs. The testing laboratory may conduct more
than one test run in each of the burn rate categories specified in
Section 8.1.1. If more than one test run is conducted at a specified
burn rate, the results from at least two-thirds of the test runs in
that burn rate category shall be used in calculating the weighted
average emission rate (see Section 12.2). The measurement data and
results of all test runs shall be reported regardless of which values
are used in calculating the weighted average emission rate (see Note in
Section 8.1).

9.0 Quality Control

Same as Section 9.0 of either Method 5G or Method 5H.

10.0 Calibration and Standardizations

Same as Section 10.0 of either Method 5G or Method 5H, with the
addition of the following:
10.1 Platform Scale. Perform a multi-point calibration (at least
five points spanning the operational range) of the platform scale
before its initial use. The scale manufacturer's calibration results
are sufficient for this purpose. Before each certification test, audit
the scale with the wood heater in place by weighing at least one
calibration weight (Class F) that corresponds to between 20 percent and
80 percent of the expected test fuel charge weight. If the scale cannot
reproduce the value of the calibration weight within 0.05 kg (0.1 lb)
or 1 percent of the expected test fuel charge weight, whichever is
greater, recalibrate the scale before use with at least five
calibration weights spanning the operational range of the scale.
10.2 Balance (optional). Calibrate as described in Section 10.1.
10.3 Temperature Monitor. Calibrate as in Method 2, Section 4.3,
before the first certification test and semiannually thereafter.
10.4 Moisture Meter. Calibrate as per the manufacturer's
instructions before each certification test.
10.5 Anemometer. Calibrate the anemometer as specified by the
manufacturer's instructions before the first certification test and
semiannually thereafter.
10.6 Barometer. Calibrate against a mercury barometer before the
first certification test and semiannually thereafter.
10.7 Draft Gauge. Calibrate as per the manufacturer's
instructions; a liquid manometer does not require calibration.
10.8 Humidity Gauge. Calibrate as per the manufacturer's
instructions before the first certification test and semiannually
thereafter.

11.0 Analytical Procedures

Same as Section 11.0 of either Method 5G or Method 5H.

12.0 Data Analysis and Calculations

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

BR = Dry wood burn rate, kg/hr (lb/hr)
Ei = Emission rate for test run, i, from Method 5G or 5H, g/
hr (lb/hr)
Ew = Weighted average emission rate, g/hr (lb/hr)
ki = Test run weighting factor = Pi+1 -
Pi-1
%Md = Fuel moisture content, dry basis, percent.
%Mw = Average moisture in test fuel charge, wet basis,
percent.
n = Total number of test runs.
Pi = Probability for burn rate during test run, i, obtained
from Table 28-1. Use linear interpolation to determine probability
values for burn rates between those listed on the table.
Wwd = Total mass of wood burned during the test run, kg
(lb).

12.2 Wet Basis Fuel Moisture Content.
[GRAPHIC] [TIFF OMITTED] TR17OC00.426

12.3 Weighted Average Emission Rate. Calculate the weighted
average emission rate (Ew) using Equation 28-1:
[GRAPHIC] [TIFF OMITTED] TR17OC00.427

Note: Po always equals 0, P(n+1) always
equals 1, P1 corresponds to the probability of the lowest
recorded burn rate, P2 corresponds to the probability of
the next lowest burn rate, etc. An example calculation is in Section
12.3.1.

12.3.1 Example Calculation of Weighted Average Emission Rate.

------------------------------------------------------------------------
Burn rate Emissions
Burn rate category Test No. (Dry-kg/hr) (g/hr)
------------------------------------------------------------------------
1................................ 1 0.65 5.0
2\1\............................. 2 0.85 6.7
2................................ 3 0.90 4.7

[[Page 62105]]

2................................ 4 1.00 5.3
3................................ 5 1.45 3.8
4................................ 6 2.00 5.1
------------------------------------------------------------------------
\1\ As permitted in Section 6.6, this test run may be omitted from the
calculation of the weighted average emission rate because three runs
were conducted for this burn rate category.

----------------------------------------------------------------------------------------------------------------
Test No. Burn rate Pi Ei Ki
----------------------------------------------------------------------------------------------------------------
0........................................................... ........... 0.000 ........... ...........
1........................................................... 0.65 0.121 5.0 0.300
2........................................................... 0.90 0.300 4.7 0.259
3........................................................... 1.00 0.380 5.3 0.422
4........................................................... 1.45 0.722 3.8 0.532
5........................................................... 2.00 0.912 5.1 0.278
6........................................................... ........... 1.000 ........... ...........
----------------------------------------------------------------------------------------------------------------
K1 = P2 - P0 = 0.300 - 0 = 0.300
K2 = P3 - P1 = 0.381 - 0.121 = 0.259
K3 = P4 - P2 = 0.722 - 0.300 = 0.422
K4 = P5 - P3 = 0.912 - 0.380 = 0.532
K5 = P6 - P4 = 1.000 - 0.722 = 0.278

Weighted Average Emission Rate, Ew, Calculation
[GRAPHIC] [TIFF OMITTED] TR17OC00.428

12.4 Average Wood Heater Surface Temperatures. Calculate the
average of the wood heater surface temperatures for the start of the
test run (Section 8.12.1) and for the test run completion (Section
8.13). If the two average temperatures do not agree within 70 deg.C
(125 deg.F), report the test run results, but do not include the test
run results in the test average. Replace such test run results with
results from another test run in the same burn rate category.
12.5 Burn Rate. Calculate the burn rate (BR) using Equation 28-3:
[GRAPHIC] [TIFF OMITTED] TR17OC00.429

12.6 Reporting Criteria. Submit both raw and reduced test data for
wood heater tests.
12.6.1 Suggested Test Report Format.
12.6.1.1 Introduction.
12.6.1.1.1 Purpose of test-certification, audit, efficiency,
research and development.
12.6.1.1.2 Wood heater identification-manufacturer, model number,
catalytic/noncatalytic, options.
12.6.1.1.3 Laboratory-name, location (altitude), participants.
12.6.1.1.4 Test information-date wood heater received, date of
tests, sampling methods used, number of test runs.
12.6.1.2 Summary and Discussion of Results
12.6.1.2.1 Table of results (in order of increasing burn rate)-
test run number, burn rate, particulate emission rate, efficiency (if
determined), averages (indicate which test runs are used).
12.6.1.2.2 Summary of other data-test facility conditions, surface
temperature averages, catalyst temperature averages, pretest fuel
weights, test fuel charge weights, run times.
12.6.1.2.3 Discussion-Burn rate categories achieved, test run
result selection, specific test run problems and solutions.
12.6.1.3 Process Description.
12.6.1.3.1 Wood heater dimensions-volume, height, width, lengths
(or other linear dimensions), weight, volume adjustments.
12.6.1.3.2 Firebox configuration-air supply locations and
operation, air supply introduction location, refractory location and
dimensions, catalyst location, baffle and by-pass location and
operation (include line drawings or photographs).
12.6.1.3.3 Process operation during test-air supply settings and
adjustments, fuel bed adjustments, draft.
12.6.1.3.4 Test fuel-test fuel properties (moisture and
temperature), test fuel crib description (include line drawing or
photograph), test fuel loading density.
12.6.1.4 Sampling Locations.
12.6.1.4.1 Describe sampling location relative to wood heater.
Include drawing or photograph.
12.6.1.5 Sampling and Analytical Procedures
12.6.1.5.1 Sampling methods-brief reference to operational and
sampling procedures and optional and alternative procedures used.
12.6.1.5.2 Analytical methods-brief description of sample recovery
and analysis procedures.
12.6.1.6 Quality Control and Assurance Procedures and Results
12.6.1.6.1 Calibration procedures and results-certification
procedures, sampling and analysis procedures.
12.6.1.6.2 Test method quality control procedures-leak-checks,
volume

[[Page 62106]]

meter checks, stratification (velocity) checks, proportionality
results.
12.6.1.7 Appendices
12.6.1.7.1 Results and Example Calculations. Complete summary
tables and accompanying examples of all calculations.
12.6.1.7.2 Raw Data. Copies of all uncorrected data sheets for
sampling measurements, temperature records and sample recovery data.
Copies of all pretest burn rate and wood heater temperature data.
12.6.1.7.3 Sampling and Analytical Procedures. Detailed
description of procedures followed by laboratory personnel in
conducting the certification test, emphasizing particular parts of the
procedures differing from the methods (e.g., approved alternatives).
12.6.1.7.4 Calibration Results. Summary of all calibrations,
checks, and audits pertinent to certification test results with dates.
12.6.1.7.5 Participants. Test personnel, manufacturer
representatives, and regulatory observers.
12.6.1.7.6 Sampling and Operation Records. Copies of uncorrected
records of activities not included on raw data sheets (e.g., wood
heater door open times and durations).
12.6.1.7.7 Additional Information. Wood heater manufacturer's
written instructions for operation during the certification test.
12.6.2.1 Wood Heater Identification. Report wood heater
identification information. An example data form is shown in Figure 28-
4.
12.6.2.2 Test Facility Information. Report test facility
temperature, air velocity, and humidity information. An example data
form is shown on Figure 28-4.
12.6.2.3 Test Equipment Calibration and Audit Information. Report
calibration and audit results for the platform scale, test fuel
balance, test fuel moisture meter, and sampling equipment including
volume metering systems and gaseous analyzers.
12.6.2.4 Pretest Procedure Description. Report all pretest
procedures including pretest fuel weight, burn rates, wood heater
temperatures, and air supply settings. An example data form is shown on
Figure 28-4.
12.6.2.5 Particulate Emission Data. Report a summary of test
results for all test runs and the weighted average emission rate.
Submit copies of all data sheets and other records collected during the
testing. Submit examples of all calculations.

13.0 Method Performance, [Reserved]

14.0 Pollution Prevention, [Reserved]

15.0 Waste Management, [Reserved]

16.0 Alternative Procedures

16.1 Pellet Burning Heaters. Certification testing requirements
and procedures for pellet burning wood heaters are identical to those
for other wood heaters, with the following exceptions:
16.1.1 Test Fuel Properties. The test fuel shall be all wood
pellets with a moisture content no greater than 20 percent on a wet
basis (25 percent on a dry basis). Determine the wood moisture content
with either ASTM D 2016-74 or 83, (Method A), ASTM D 4444-92, or ASTM D
4442-84 or 92 (all noted ASTM standards are incorporated by reference--
see Sec. 60.17).
16.1.2 Test Fuel Charge Specifications. The test fuel charge size
shall be as per the manufacturer's written instructions for maintaining
the desired burn rate.
16.1.3 Wood Heater Firebox Volume. The firebox volume need not be
measured or determined for establishing the test fuel charge size. The
firebox dimensions and other heater specifications needed to identify
the heater for certification purposes shall be reported.
16.1.4 Heater Installation. Arrange the heater with the fuel
supply hopper on the platform scale as described in Section 8.6.1.
16.1.5 Pretest Ignition. Start a fire in the heater as directed by
the manufacturer's written instructions, and adjust the heater controls
to achieve the desired burn rate. Operate the heater at the desired
burn rate for at least 1 hour before the start of the test run.
16.1.6 Test Run. Complete a test run in each burn rate category as
follows:
16.1.6.1 Test Run Start. When the wood heater has operated for at
least 1 hour at the desired burn rate, add fuel to the supply hopper as
necessary to complete the test run, record the weight of the fuel in
the supply hopper (the wood heater weight), and start the test run. Add
no additional fuel to the hopper during the test run.
Record all the wood heater surface temperatures, the initial
sampling method measurement values, the time at the start of the test,
and begin the emission sampling. Make no adjustments to the wood heater
air supply or wood supply rate during the test run.
16.1.6.2 Data Recording. Record the fuel (wood heater) weight
data, wood heater temperature and operational data, and emission
sampling data as described in Section 8.12.2.
16.1.6.3 Test Run Completion. Continue emission sampling and wood
heater operation for 2 hours. At the end of the test run, stop the
particulate sampling, and record the final fuel weight, the run time,
and all final measurement values, including all wood heater individual
surface temperatures.
16.1.7 Calculations. Determine the burn rate using the difference
between the initial and final fuel (wood heater) weights and the
procedures described in Section 12.4. Complete the other calculations
as described in Section 12.0.

17.0 References

Same as Method 5G, with the addition of the following:

1. Radian Corporation. OMNI Environmental Services, Inc.,
Cumulative Probability for a Given Burn Rate Based on Data Generated
in the CONEG and BPA Studies. Package of materials submitted to the
Fifth Session of the Regulatory Negotiation Committee, July 16-17,
1986.

18.0 Tables, Diagrams, Flowcharts, and Validation Data

Table 28-1.--Burn Rate Weighted Probabilities for Calculating Weighted Average Emission Rates
----------------------------------------------------------------------------------------------------------------
Cumulative Cumulative Cumulative
Burn rate (kg/hr-dry) probability Burn rate (kg/ probability Burn rate (kg/ probability
(P) hr-dry) (P) hr-dry) (P)
----------------------------------------------------------------------------------------------------------------
0.00............................ 0.000 1.70 0.840 3.40 0.989
0.05............................ 0.002 1.75 0.857 3.45 0.989
0.10............................ 0.007 1.80 0.875 3.50 0.990
0.15............................ 0.012 1.85 0.882 3.55 0.991
0.20............................ 0.016 1.90 0.895 3.60 0.991
0.25............................ 0.021 1.95 0.906 3.65 0.992
0.30............................ 0.028 2.00 0.912 3.70 0.992
0.35............................ 0.033 2.05 0.920 3.75 0.992

[[Page 62107]]

0.40............................ 0.041 2.10 0.925 3.80 0.993
0.45............................ 0.054 2.15 0.932 3.85 0.994
0.50............................ 0.065 2.20 0.936 3.90 0.994
0.55............................ 0.086 2.25 0.940 3.95 0.994
0.60............................ 0.100 2.30 0.945 4.00 0.994
0.65............................ 0.121 2.35 0.951 4.05 0.995
0.70............................ 0.150 2.40 0.956 4.10 0.995
0.75............................ 0.185 2.45 0.959 4.15 0.995
0.80............................ 0.220 2.50 0.964 4.20 0.995
0.85............................ 0.254 2.55 0.968 4.25 0.995
0.90............................ 0.300 2.60 0.972 4.30 0.996
0.95............................ 0.328 2.65 0.975 4.35 0.996
1.00............................ 0.380 2.70 0.977 4.40 0.996
1.05............................ 0.407 2.75 0.979 4.45 0.996
1.10............................ 0.460 2.80 0.980 4.50 0.996
1.15............................ 0.490 2.85 0.981 4.55 0.996
1.20............................ 0.550 2.90 0.982 4.60 0.996
1.25............................ 0.572 2.95 0.984 4.65 0.996
1.30............................ 0.620 3.00 0.984 4.70 0.996
1.35............................ 0.654 3.05 0.985 4.75 0.997
1.40............................ 0.695 3.10 0.986 4.80 0.997
1.45............................ 0.722 3.15 0.987 4.85 0.997
1.50............................ 0.750 3.20 0.987 4.90 0.997
1.55............................ 0.779 3.25 0.988 4.95 0.997
1.60............................ 0.800 3.30 0.988 5.0 1.000
0
1.65............................ 0.825 3.35 0.989 .............. ..............
----------------------------------------------------------------------------------------------------------------

BILLING CODE 6560-50-P

[[Page 62108]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.430

[[Page 62109]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.431

[[Page 62110]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.432

BILLING CODE 6560-50-C

[[Page 62111]]

Method 28A--Measurement of Air- to-Fuel Ratio and Mimimum
Achievable Burn Rates for Wood-Fired Appliances

Note: This method does not include all or the specifications
(e.g., equipment and supplies) and procedures (e.g., sampling and
analytical) essential to its performance. Some material is
incorporated by reference from other methods in this part.
Therefore, to obtain reliable results, persons using this method
should also have a thorough knowledge of at least the following
additional test methods: Method 3, Method 3A, Method 5H, Method 6C,
and Method 28.

1.0 Scope and Application

1.1 Analyte. Particulate matter (PM). No CAS number assigned.
1.2 Applicability. This method is applicable for the measurement
of air-to-fuel ratios and minimum achievable burn rates, for
determining whether a wood-fired appliance is an affected facility, as
specified in 40 CFR 60.530.
1.3 Data Quality Objectives. Adherence to the requirements of this
method will enhance the quality of the data obtained from air pollutant
sampling methods.

2.0 Summary of Method

2.1 A gas sample is extracted from a location in the stack of a
wood-fired appliance while the appliance is operating at a prescribed
set of conditions. The gas sample is analyzed for carbon dioxide
(CO2), oxygen (O2), and carbon monoxide (CO).
These stack gas components are measured for determining the dry
molecular weight of the exhaust gas. Total moles of exhaust gas are
determined stoichiometrically. Air-to-fuel ratio is determined by
relating the mass of dry combustion air to the mass of dry fuel
consumed.

3.0 Definitions

Same as Method 28, Section 3.0, with the addition of the following:
3.1 Air-to-fuel ratio means the ratio of the mass of dry combustion
air introduced into the firebox to the mass of dry fuel consumed (grams
of dry air per gram of dry wood burned).

4.0 Interferences [Reserved]

5.0 Safety

6.0 Equipment and Supplies

6.1 Test Facility. Insulated Solid Pack Chimney, Platform Scale
and Monitor, Test Facility Temperature Monitor, Balance, Moisture
Meter, Anemometer, Barometer, Draft Gauge, Humidity Gauge, Wood Heater
Flue, and Test Facility. Same as Method 28, Sections 6.1, 6.2, and 6.4
to 6.12, respectively.
6.2 Sampling System. Probe, Condenser, Valve, Pump, Rate Meter,
Flexible Bag, Pressure Gauge, and Vacuum Gauge. Same as Method 3,
Sections 6.2.1 to 6.2.8, respectively. Alternatively, the sampling
system described in Method 5H, Section 6.1 may be used.
6.3 Exhaust Gas Analysis. Use one or both of the following:
6.3.1 Orsat Analyzer. Same as Method 3, Section 6.1.3
6.3.2 Instrumental Analyzers. Same as Method 5H, Sections 6.1.3.4
and 6.1.3.5, for CO2 and CO analyzers, except use a CO
analyzer with a range of 0 to 5 percent and use a CO2
analyzer with a range of 0 to 5 percent. Use an O2 analyzer
capable of providing a measure of O2 in the range of 0 to 25
percent by volume at least once every 10 minutes.

7.0 Reagents and Standards

7.1 Test Fuel and Test Fuel Spacers. Same as Method 28, Sections
7.1 and 7.2, respectively.
7.2 Cylinder Gases. For each of the three analyzers, use the same
concentration as specified in Sections 7.2.1, 7.2.2, and 7.2.3 of
Method 6C.

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Wood Heater Air Supply Adjustments.
8.1.1 This section describes how dampers are to be set or adjusted
and air inlet ports closed or sealed during Method 28A tests. The
specifications in this section are intended to ensure that affected
facility determinations are made on the facility configurations that
could reasonably be expected to be employed by the user. They are also
intended to prevent circumvention of the standard through the addition
of an air port that would often be blocked off in actual use. These
specifications are based on the assumption that consumers will remove
such items as dampers or other closure mechanism stops if this can be
done readily with household tools; that consumers will block air inlet
passages not visible during normal operation of the appliance using
aluminum tape or parts generally available at retail stores; and that
consumers will cap off any threaded or flanged air inlets. They also
assume that air leakage around glass doors, sheet metal joints or
through inlet grilles visible during normal operation of the appliance
would not be further blocked or taped off by a consumer.
8.1.2 It is not the intention of this section to cause an
appliance that is clearly designed, intended, and, in most normal
installations, used as a fireplace to be converted into a wood heater
for purposes of applicability testing. Such a fireplace would be
identifiable by such features as large or multiple glass doors or
panels that are not gasketed, relatively unrestricted air inlets
intended, in large part, to limit smoking and fogging of glass
surfaces, and other aesthetic features not normally included in wood
heaters.
8.1.3 Adjustable Air Supply Mechanisms. Any commercially available
flue damper, other adjustment mechanism or other air inlet port that is
designed, intended or otherwise reasonably expected to be adjusted or
closed by consumers, installers, or dealers and which could restrict
air into the firebox shall be set so as to achieve minimum air into the
firebox (i.e., closed off or set in the most closed position).
8.1.3.1 Flue dampers, mechanisms and air inlet ports which could
reasonably be expected to be adjusted or closed would include:
8.1.3.1.1 All internal or externally adjustable mechanisms
(including adjustments that affect the tightness of door fittings) that
are accessible either before and/or after installation.
8.1.3.1.2 All mechanisms, other inlet ports, or inlet port stops
that are identified in the owner's manual or in any dealer literature
as being adjustable or alterable. For example, an inlet port that could
be used to provide access to an outside air duct but which is
identified as being closable through use of additional materials
whether or not they are supplied with the facility.
8.1.3.1.3 Any combustion air inlet port or commercially available
flue damper or mechanism stop, which would readily lend itself to
closure by consumers who are handy with household tools by the removal
of parts or the addition of parts generally available at retail stores
(e.g., addition of a pipe cap or plug, addition of a small metal plate
to an inlet hole on a nondecorative sheet metal surface, or removal of
riveted or screwed damper stops).
8.1.3.1.4 Any flue damper, other adjustment mechanisms or other
air inlet ports that are found and documented in several (e.g., a
number

[[Page 62112]]

sufficient to reasonably conclude that the practice is not unique or
uncommon) actual installations as having been adjusted to a more closed
position, or closed by consumers, installers, or dealers.
8.1.4 Air Supply Adjustments During Test. The test shall be
performed with all air inlets identified under this section in the
closed or most closed position or in the configuration which otherwise
achieves the lowest air inlet (i.e., greatest blockage).

Note: For the purposes of this section, air flow shall not be
minimized beyond the point necessary to maintain combustion or
beyond the point that forces smoke into the room.

8.1.5 Notwithstanding Section 8.1.1, any flue damper, adjustment
mechanism, or air inlet port (whether or not equipped with flue dampers
or adjusting mechanisms) that is visible during normal operation of the
appliance and which could not reasonably be closed further or blocked
except through means that would significantly degrade the aesthetics of
the facility (e.g., through use of duct tape) will not be closed
further or blocked.
8.2 Sampling System.
8.2.1 Sampling Location. Same as Method 5H, Section 8.1.2.
8.2.2 Sampling System Set Up. Set up the sampling equipment as
described in Method 3, Section 8.1.
8.3 Wood Heater Installation, Test Facility Conditions, Wood
Heater Firebox Volume, and Test Fuel Charge. Same as Method 28,
Sections 8.4 and 8.6 to 8.8, respectively.
8.4 Pretest Ignition. Same as Method 28, Section 8.11. Set the
wood heater air supply settings to achieve a burn rate in Category 1 or
the lowest achievable burn rate (see Section 8.1).
8.5 Test Run. Same as Method 28, Section 8.12. Begin sample
collection at the start of the test run as defined in Method 28,
Section 8.12.1.
8.5.1 Gas Analysis.
8.5.1.1 If Method 3 is used, collect a minimum of two bag samples
simultaneously at a constant sampling rate for the duration of the test
run. A minimum sample volume of 30 liters (1.1 ft3) per bag
is recommended.
8.5.1.2 If instrumental gas concentration measurement procedures
are used, conduct the gas measurement system performance tests,
analyzer calibration, and analyzer calibration error check outlined in
Method 6C, Sections 8.2.3, 8.2.4, 8.5, and 10.0, respectively. Sample
at a constant rate for the duration of the test run.
8.5.2 Data Recording. Record wood heater operational data, test
facility temperature, sample train flow rate, and fuel weight data at
intervals of no greater than 10 minutes.
8.5.3 Test Run Completion. Same as Method 28, Section 8.13.

9.0 Quality Control

9.1 Data Validation. The following quality control procedure is
suggested to provide a check on the quality of the data.
9.1.1 Calculate a fuel factor, Fo, using Equation 28A-1
in Section 12.2.
9.1.2 If CO is present in quantities measurable by this method,
adjust the O2 and CO2 values before performing
the calculation for Fo as shown in Section 12.3 and 12.4.
9.1.3 Compare the calculated Fo factor with the
expected Fo range for wood (1.000--1.120). Calculated
Fo values beyond this acceptable range should be
investigated before accepting the test results. For example, the
strength of the solutions in the gas analyzer and the analyzing
technique should be checked by sampling and analyzing a known
concentration, such as air. If no detectable or correctable measurement
error can be identified, the test should be repeated. Alternatively,
determine a range of air-to-fuel ratio results that could include the
correct value by using an Fo value of 1.05 and calculating a
potential range of CO2 and O2 values. Acceptance
of such results will be based on whether the calculated range includes
the exemption limit and the judgment of the Administrator.
9.2 Method 3 Analyses. Compare the results of the analyses of the
two bag samples. If all the gas components (O2, CO, and
CO2) values for the two analyses agree within 0.5 percent
(e.g., 6.0 percent O2 for bag 1 and 6.5 percent
O2 for bag 2, agree within 0.5 percent), the results of the
bag analyses may be averaged for the calculations in Section 12. If the
analysis results do not agree within 0.5 percent for each component,
calculate the air-to-fuel ratio using both sets of analyses and report
the results.

10.0 Calibration and Standardization, [Reserved]

11.0 Analytical Procedures

11.1 Method 3 Integrated Bag Samples. Within 4 hours after the
sample collection, analyze each bag sample for percent CO2,
O2, and CO using an Orsat analyzer as described in Method 3,
Section 11.0.
11.2 Instrumental Analyzers. Average the percent CO2,
CO, and O2 values for the test run.

12.0 Data Analyses and Calculations

Carry out calculations, retaining at least one extra significant
figure beyond that of the acquired data. Round off figure after the
final calculation. Other forms of the equations may be used as long as
they give equivalent results.
12.1 Nomenclature.

Md = Dry molecular weight, g/g-mole (lb/lb-mole).
NT = Total gram-moles of dry exhaust gas per kg of wood
burned (lb-moles/lb).
%CO2 = Percent CO2 by volume (dry basis).
%CO = Percent CO by volume (dry basis).
%N2 = Percent N2 by volume (dry basis).
%O2 = Percent O2 by volume (dry basis).
YHC = Assumed mole fraction of HC (dry as CH4) =
0.0088 for catalytic wood heaters; = 0.0132 for noncatalytic wood
heaters. = 0.0080 for pellet-fired wood heaters.
YCO = Measured mole fraction of CO (e.g., 1 percent CO = .01
mole fraction), g/g-mole (lb/lb-mole).
YCO2 = Measured mole fraction of COCO2 (e.g., 10
percent CO2 = .10 mole fraction), g/g-mole (lb/lb-mole).
0.280 = Molecular weight of N2 or CO, divided by 100.
0.320 = Molecular weight of O2 divided by 100.
0.440 = Molecular weight of CO2 divided by 100.
20.9 = Percent O2 by volume in ambient air.
42.5 = Gram-moles of carbon in 1 kg of dry wood assuming 51 percent
carbon by weight dry basis (.0425 lb/lb-mole).
510 = Grams of carbon in exhaust gas per kg of wood burned.
1,000 = Grams in 1 kg.

12.2 Fuel Factor. Use Equation 28A-1 to calculate the fuel factor.
[GRAPHIC] [TIFF OMITTED] TR17OC00.433

12. 3 Adjusted %CO2. Use Equation 28A-2 to adjust
CO2 values if measurable CO is present.
[GRAPHIC] [TIFF OMITTED] TR17OC00.434

[[Page 62113]]

12.4 Adjusted %O2. Use Equation 28A-3 to adjust
O2 value if measurable CO is present.
[GRAPHIC] [TIFF OMITTED] TR17OC00.435

12.5 Dry Molecular Weight. Use Equation 28A-4 to calculate the dry
molecular weight of the stack gas.
[GRAPHIC] [TIFF OMITTED] TR17OC00.436

Note: The above equation does not consider argon in air (about
0.9 percent, molecular weight of 39.9). A negative error of about
0.4 percent is introduced. Argon may be included in the analysis
using procedures subject to approval of the Administrator.

12.6 Dry Moles of Exhaust Gas. Use Equation 28A-5 to calculate the
total moles of dry exhaust gas produced per kilogram of dry wood
burned.
[GRAPHIC] [TIFF OMITTED] TR17OC00.437

12.7 Air-to-Fuel Ratio. Use Equation 28A-6 to calculate the air-
to-fuel ratio on a dry mass basis.
[GRAPHIC] [TIFF OMITTED] TR17OC00.438

12.8 Burn Rate. Calculate the fuel burn rate as in Method 28,
Section 12.4.

13.0 Method Performance, [Reserved]

14.0 Pollution Prevention, [Reserved]

15.0 Waste Management, [Reserved]

16.0 References

Same as Section 16.0 of Method 3 and Section 17 of Method 5G.

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

Method 29--Determination of Metals 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 5 and Method 12.

1.0 Scope and Application

1.1 Analytes.

------------------------------------------------------------------------
Analyte CAS No.
------------------------------------------------------------------------
Antimony (Sb)........................................... 7440-36-0
Arsenic (As)............................................ 7440-38-2
Barium (Ba)............................................. 7440-39-3
Beryllium (Be).......................................... 7440-41-7
Cadmium (Cd)............................................ 7440-43-9
Chromium (Cr)........................................... 7440-47-3
Cobalt (Co)............................................. 7440-48-4
Copper (Cu)............................................. 7440-50-8
Lead (Pb)............................................... 7439-92-1
Manganese (Mn).......................................... 7439-96-5
Mercury (Hg)............................................ 7439-97-6
Nickel (Ni)............................................. 7440-02-0
Phosphorus (P).......................................... 7723-14-0
Selenium (Se)........................................... 7782-49-2
Silver (Ag)............................................. 7440-22-4
Thallium (Tl)........................................... 7440-28-0
Zinc (Zn)............................................... 7440-66-6
------------------------------------------------------------------------

1.2 Applicability. This method is applicable to the determination
of metals emissions from stationary sources. This method may be used to
determine particulate emissions in addition to the metals emissions if
the prescribed procedures and precautions are followed.
1.2.1 Hg emissions can be measured, alternatively, using EPA
Method 101A of Appendix B, 40 CFR Part 61. Method 101-A measures only
Hg but it can be of special interest to sources which need to measure
both Hg and Mn emissions.

2.0 Summary of Method

2.1 Principle. A stack sample is withdrawn isokinetically from the
source, particulate emissions are collected in the probe and on a
heated filter, and gaseous emissions are then collected in an aqueous
acidic solution of hydrogen peroxide (analyzed for all metals including
Hg) and an aqueous acidic solution of potassium permanganate (analyzed
only for Hg). The recovered samples are digested, and appropriate
fractions are analyzed for Hg by cold vapor atomic absorption
spectroscopy (CVAAS) and for Sb, As, Ba, Be, Cd, Cr, Co, Cu, Pb, Mn,
Ni, P, Se, Ag, Tl, and Zn by inductively coupled argon plasma emission
spectroscopy (ICAP) or atomic absorption spectroscopy (AAS). Graphite
furnace atomic absorption spectroscopy (GFAAS) is used for analysis of
Sb, As, Cd, Co, Pb, Se, and Tl if these elements require greater
analytical sensitivity than can be obtained by ICAP. If one so chooses,
AAS may be used for analysis of all listed metals if the resulting in-
stack method detection limits meet the goal of the testing program.
Similarly, inductively coupled plasma-mass spectroscopy (ICP-MS) may be
used for analysis of Sb, As, Ba, Be, Cd, Cr, Co, Cu, Pb, Mn, Ni, Ag, Tl
and Zn.

3.0 Definitions. [Reserved]

4.0 Interferences

4.1 Iron (Fe) can be a spectral interference during the analysis
of As, Cr, and Cd by ICAP. Aluminum (Al) can be a spectral interference
during the analysis of As and Pb by ICAP. Generally, these
interferences can be reduced by diluting the analytical sample, but
such dilution raises the in-stack detection limits. Background and
overlap corrections may be used to adjust for spectral interferences.
Refer to Method 6010 of Reference 2 in Section 16.0 or the other
analytical methods used for details on potential interferences to this
method. For all GFAAS analyses, use matrix modifiers to limit
interferences, and matrix match all standards.

5.0 Safety

[[Page 62114]]

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 Nitric Acid (HNO3). Highly corrosive to eyes,
skin, nose, and lungs. Vapors cause bronchitis, pneumonia, or edema of
lungs. Reaction to inhalation may be delayed as long as 30 hours and
still be fatal. Provide ventilation to limit exposure. Strong oxidizer.
Hazardous reaction may occur with organic materials such as solvents.
5.2.2 Sulfuric Acid (H2SO4). Rapidly
destructive to body tissue. Will cause third degree burns. Eye damage
may result in blindness. Inhalation may be fatal from spasm of the
larynx, usually within 30 minutes. May cause lung tissue damage with
edema. 1 mg/m\3\ for 8 hours will cause lung damage or, in higher
concentrations, death. Provide ventilation to limit inhalation. Reacts
violently with metals and organics.
5.2.3 Hydrochloric Acid (HC1). Highly corrosive liquid with toxic
vapors. 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 can be lethal
to humans in a few minutes. Provide ventilation to limit exposure.
Reacts with metals, producing hydrogen gas.
5.2.4 Hydrofluoric Acid (HF). Highly corrosive to eyes, skin,
nose, throat, and lungs. Reaction to exposure may be delayed by 24
hours or more. Provide ventilation to limit exposure.
5.2.5 Hydrogen Peroxide (H2O2). Irritating
to eyes, skin, nose, and lungs. 30% H2O2 is a
strong oxidizing agent. Avoid contact with skin, eyes, and combustible
material. Wear gloves when handling.
5.2.6 Potassium Permanganate (KMnO4). Caustic, strong
oxidizer. Avoid bodily contact with.
5.2.7 Potassium Persulfate. Strong oxidizer. Avoid bodily contact
with. Keep containers well closed and in a cool place.
5.3 Reaction Pressure. Due to the potential reaction of the
potassium permanganate with the acid, there could be pressure buildup
in the acidic KMnO4 absorbing solution storage bottle.
Therefore these bottles shall not be fully filled and shall be vented
to relieve excess pressure and prevent explosion potentials. Venting is
required, but not in a manner that will allow contamination of the
solution. A No. 70-72 hole drilled in the container cap and Teflon
liner has been used.

6.0 Equipment and Supplies

6.1 Sampling. A schematic of the sampling train is shown in Figure
29-1. It has general similarities to the Method 5 train.
6.1.1 Probe Nozzle (Probe Tip) and Borosilicate or Quartz Glass
Probe Liner. Same as Method 5, Sections 6.1.1.1 and 6.1.1.2, except
that glass nozzles are required unless alternate tips are constructed
of materials that are free from contamination and will not interfere
with the sample. If a probe tip other than glass is used, no correction
to the sample test results to compensate for the nozzle's effect on the
sample is allowed. Probe fittings of plastic such as Teflon,
polypropylene, etc. are recommended instead of metal fittings to
prevent contamination. If one chooses to do so, a single glass piece
consisting of a combined probe tip and probe liner may be used.
6.1.2 Pitot Tube and Differential Pressure Gauge. Same as Method
2, Sections 6.1 and 6.2, respectively.
6.1.3 Filter Holder. Glass, same as Method 5, Section 6.1.1.5,
except use a Teflon filter support or other non-metallic, non-
contaminating support in place of the glass frit.
6.1.4 Filter Heating System. Same as Method 5, Section 6.1.1.6.
6.1.5 Condenser. Use the following system for condensing and
collecting gaseous metals and determining the moisture content of the
stack gas. The condensing system shall consist of four to seven
impingers connected in series with leak-free ground glass fittings or
other leak-free, non-contaminating fittings. Use the first impinger as
a moisture trap. The second impinger (which is the first
HNO3/H2O2 impinger) shall be identical
to the first impinger in Method 5. The third impinger (which is the
second HNO3/H2O2 impinger) shall be a
Greenburg Smith impinger with the standard tip as described for the
second impinger in Method 5, Section 6.1.1.8. The fourth (empty)
impinger and the fifth and sixth (both acidified KMnO4)
impingers are the same as the first impinger in Method 5. Place a
temperature sensor capable of measuring to within 1 deg.C (2 deg.F)
at the outlet of the last impinger. If no Hg analysis is planned, then
the fourth, fifth, and sixth impingers are not used.
6.1.6 Metering System, Barometer, and Gas Density Determination
Equipment. Same as Method 5, Sections 6.1.1.9, 6.1.2, and 6.1.3,
respectively.
6.1.7 Teflon Tape. For capping openings and sealing connections,
if necessary, on the sampling train.
6.2 Sample Recovery. Same as Method 5, Sections 6.2.1 through
6.2.8 (Probe-Liner and Probe-Nozzle Brushes or Swabs, Wash Bottles,
Sample Storage Containers, Petri Dishes, Glass Graduated Cylinder,
Plastic Storage Containers, Funnel and Rubber Policeman, and Glass
Funnel), respectively, with the following exceptions and additions:
6.2.1 Non-metallic Probe-Liner and Probe-Nozzle Brushes or Swabs.
Use non-metallic probe-liner and probe-nozzle brushes or swabs for
quantitative recovery of materials collected in the front-half of the
sampling train.
6.2.2 Sample Storage Containers. Use glass bottles (see Section
8.1 of this Method) with Teflon-lined caps that are non-reactive to the
oxidizing solutions, with capacities of 1000- and 500-ml, for storage
of acidified KMnO4--containing samples and blanks. Glass or
polyethylene bottles may be used for other sample types.
6.2.3 Graduated Cylinder. Glass or equivalent.
6.2.4 Funnel. Glass or equivalent.
6.2.5 Labels. For identifying samples.
6.2.6 Polypropylene Tweezers and/or Plastic Gloves. For recovery
of the filter from the sampling train filter holder.
6.3 Sample Preparation and Analysis.
6.3.1 Volumetric Flasks, 100-ml, 250-ml, and 1000-ml. For
preparation of standards and sample dilutions.
6.3.2 Graduated Cylinders. For preparation of reagents.
6.3.3 Parr Bombs or Microwave Pressure Relief Vessels with Capping
Station (CEM Corporation model or equivalent). For sample digestion.
6.3.4 Beakers and Watch Glasses. 250-ml beakers, with watch glass
covers, for sample digestion.
6.3.5 Ring Stands and Clamps. For securing equipment such as
filtration apparatus.
6.3.6 Filter Funnels. For holding filter paper.
6.3.7 Disposable Pasteur Pipets and Bulbs.
6.3.8 Volumetric Pipets.
6.3.9 Analytical Balance. Accurate to within 0.1 mg.
6.3.10 Microwave or Conventional Oven. For heating samples at
fixed power levels or temperatures, respectively.
6.3.11 Hot Plates.
6.3.12 Atomic Absorption Spectrometer (AAS). Equipped with a
background corrector.
6.3.12.1 Graphite Furnace Attachment. With Sb, As, Cd, Co, Pb, Se,
and Tl hollow cathode lamps (HCLs) or electrodeless discharge lamps
(EDLs). Same as Reference 2 in Section 16.0.

[[Page 62115]]

Methods 7041 (Sb), 7060 (As), 7131 (Cd), 7201 (Co), 7421 (Pb), 7740
(Se), and 7841 (Tl).
6.3.12.2 Cold Vapor Mercury Attachment. With a mercury HCL or EDL,
an air recirculation pump, a quartz cell, an aerator apparatus, and a
heat lamp or desiccator tube. The heat lamp shall be capable of raising
the temperature at the quartz cell by 10 deg.C above ambient, so that
no condensation forms on the wall of the quartz cell. Same as Method
7470 in Reference 2 in Section 16.0. See Note 2: Section 11.1.3 for
other acceptable approaches for analysis of Hg in which analytical
detection limits of 0.002 ng/ml were obtained.
6.3.13 Inductively Coupled Argon Plasma Spectrometer. With either
a direct or sequential reader and an alumina torch. Same as EPA Method
6010 in Reference 2 in Section 16.0.
6.3.14 Inductively Coupled Plasma-Mass Spectrometer.
Same as EPA Method 6020 in Reference 2 in Section 16.0.

7.0 Reagents and Standards

7.1 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.
7.2 Sampling Reagents.
7.2.1 Sample Filters. Without organic binders. The filters shall
contain less than 1.3 g/in.\2\ of each of the metals to be
measured. Analytical results provided by filter manufacturers stating
metals content of the filters are acceptable. However, if no such
results are available, analyze filter blanks for each target metal
prior to emission testing. Quartz fiber filters meeting these
requirements are recommended. However, if glass fiber filters become
available which meet these requirements, they may be used. Filter
efficiencies and unreactiveness to sulfur dioxide (SO2) or
sulfur trioxide (SO3) shall be as described in Section 7.1.1
of Method 5.
7.2.2 Water. To conform to ASTM Specification D1193-77 or 91, Type
II (incorporated by reference--see Sec. 60.17). If necessary, analyze
the water for all target metals prior to field use. All target metals
should be less than 1 ng/ml.
7.2.3 HNO3, Concentrated. Baker Instra-analyzed or
equivalent.
7.2.4 HCl, Concentrated. Baker Instra-analyzed or equivalent.
7.2.5 H2O2, 30 Percent (V/V).
7.2.6 KMnO4.
7.2.7 H2SO4, Concentrated.
7.2.8 Silica Gel and Crushed Ice. Same as Method 5, Sections 7.1.2
and 7.1.4, respectively.
7.3 Pretest Preparation of Sampling Reagents.
7.3.1 HNO3/H2O2 Absorbing
Solution, 5 Percent HNO3/10 Percent
H2O2. Add carefully with stirring 50 ml of
concentrated HNO3 to a 1000-ml volumetric flask containing
approximately 500 ml of water, and then add carefully with stirring 333
ml of 30 percent H2O2. Dilute to volume with
water. Mix well. This reagent shall contain less than 2 ng/ml of each
target metal.
7.3.2 Acidic KMnO4 Absorbing Solution, 4 Percent
KMnO4 (W/V), 10 Percent H2SO4 (V/V).
Prepare fresh daily. Mix carefully, with stirring, 100 ml of
concentrated H2SO4 into approximately 800 ml of
water, and add water with stirring to make a volume of 1 liter: this
solution is 10 percent H2SO4 (V/V). Dissolve,
with stirring, 40 g of KMnO4 into 10 percent
H2SO4 (V/V) and add 10 percent
H2SO4 (V/V) with stirring to make a volume of 1
liter. Prepare and store in glass bottles to prevent degradation. This
reagent shall contain less than 2 ng/ml of Hg.
Precaution: To prevent autocatalytic decomposition of the
permanganate solution, filter the solution through Whatman 541 filter
paper.
7.3.3 HNO3, 0.1 N. Add with stirring 6.3 ml of
concentrated HNO3 (70 percent) to a flask containing
approximately 900 ml of water. Dilute to 1000 ml with water. Mix well.
This reagent shall contain less than 2 ng/ml of each target metal.
7.3.4 HCl, 8 N. Carefully add with stirring 690 ml of concentrated
HCl to a flask containing 250 ml of water. Dilute to 1000 ml with
water. Mix well. This reagent shall contain less than 2 ng/ml of Hg.
7.4 Glassware Cleaning Reagents.
7.4.1 HNO3, Concentrated. Fisher ACS grade or
equivalent.
7.4.2 Water. To conform to ASTM Specifications D1193, Type II.
7.4.3 HNO3, 10 Percent (V/V). Add with stirring 500 ml
of concentrated HNO3 to a flask containing approximately
4000 ml of water. Dilute to 5000 ml with water. Mix well. This reagent
shall contain less than 2 ng/ml of each target metal.
7.5 Sample Digestion and Analysis Reagents. The metals standards,
except Hg, may also be made from solid chemicals as described in
Reference 3 in Section 16.0. Refer to References 1, 2, or 5 in Section
16.0 for additional information on Hg standards. The 1000 g/ml
Hg stock solution standard may be made according to Section 7.2.7 of
Method 101A.
7.5.1 HCl, Concentrated.
7.5.2 HF, Concentrated.
7.5.3 HNO3, Concentrated. Baker Instra-analyzed or
equivalent.
7.5.4 HNO3, 50 Percent (V/V). Add with stirring 125 ml
of concentrated HNO3 to 100 ml of water. Dilute to 250 ml
with water. Mix well. This reagent shall contain less than 2 ng/ml of
each target metal.
7.5.5 HNO3, 5 Percent (V/V). Add with stirring 50 ml of
concentrated HNO3 to 800 ml of water. Dilute to 1000 ml with
water. Mix well. This reagent shall contain less than 2 ng/ml of each
target metal.
7.5.6 Water. To conform to ASTM Specifications D1193, Type II.
7.5.7 Hydroxylamine Hydrochloride and Sodium Chloride Solution.
See Reference 2 In Section 16.0 for preparation.
7.5.8 Stannous Chloride. See Reference 2 in Section 16.0 for
preparation.
7.5.9 KMnO4, 5 Percent (W/V). See Reference 2 in
Section 16.0 for preparation.
7.5.10 H2SO4, Concentrated.
7.5.11 Potassium Persulfate, 5 Percent (W/V). See Reference 2 in
Section 16.0 for preparation.
7.5.12 Nickel Nitrate, Ni(N03) 2
6H20.
7.5.13 Lanthanum Oxide, La203.
7.5.14 Hg Standard (AAS Grade), 1000 g/ml.
7.5.15 Pb Standard (AAS Grade), 1000 g/ml.
7.5.16 As Standard (AAS Grade), 1000 g/ml.
7.5.17 Cd Standard (AAS Grade), 1000 g/ml.
7.5.18 Cr Standard (AAS Grade), 1000 g/ml.
7.5.19 Sb Standard (AAS Grade), 1000 g/ml.
7.5.20 Ba Standard (AAS Grade), 1000 g/ml.
7.5.21 Be Standard (AAS Grade), 1000 g/ml.
7.5.22 Co Standard (AAS Grade), 1000 g/ml.
7.5.23 Cu Standard (AAS Grade), 1000 g/ml.
7.5.24 Mn Standard (AAS Grade), 1000 g/ml.
7.5.25 Ni Standard (AAS Grade), 1000 g/ml.
7.5.26 P Standard (AAS Grade), 1000 g/ml.
7.5.27 Se Standard (AAS Grade), 1000 g/ml.
7.5.28 Ag Standard (AAS Grade), 1000 g/ml.
7.5.29 Tl Standard (AAS Grade), 1000 g/ml.

[[Page 62116]]

7.5.30 Zn Standard (AAS Grade), 1000 g/ml.
7.5.31 Al Standard (AAS Grade), 1000 g/ml.
7.5.32 Fe Standard (AAS Grade), 1000 g/ml.
7.5.33 Hg Standards and Quality Control Samples. Prepare fresh
weekly a 10 g/ml intermediate Hg standard by adding 5 ml of
1000 g/ml Hg stock solution prepared according to Method 101A
to a 500-ml volumetric flask; dilute with stirring to 500 ml by first
carefully adding 20 ml of 15 percent HNO3 and then adding
water to the 500-ml volume. Mix well. Prepare a 200 ng/ml working Hg
standard solution fresh daily: add 5 ml of the 10 g/ml
intermediate standard to a 250-ml volumetric flask, and dilute to 250
ml with 5 ml of 4 percent KMnO4, 5 ml of 15 percent
HNO3, and then water. Mix well. Use at least five separate
aliquots of the working Hg standard solution and a blank to prepare the
standard curve. These aliquots and blank shall contain 0.0, 1.0, 2.0,
3.0, 4.0, and 5.0 ml of the working standard solution containing 0,
200, 400, 600, 800, and 1000 ng Hg, respectively. Prepare quality
control samples by making a separate 10 g/ml standard and
diluting until in the calibration range.
7.5.34 ICAP Standards and Quality Control Samples. Calibration
standards for ICAP analysis can be combined into four different mixed
standard solutions as follows:

Mixed Standard Solutions for ICAP Analysis
------------------------------------------------------------------------
Solution Elements
------------------------------------------------------------------------
I................................. As, Be, Cd, Mn, Pb, Se, Zn.
II................................ Ba, Co, Cu, Fe.
III............................... Al, Cr, Ni.
IV................................ Ag, P, Sb, Tl.
------------------------------------------------------------------------

Prepare these standards by combining and diluting the appropriate
volumes of the 1000 g/ml solutions with 5 percent
HNO3. A minimum of one standard and a blank can be used to
form each calibration curve. However, prepare a separate quality
control sample spiked with known amounts of the target metals in
quantities in the mid-range of the calibration curve. Suggested
standard levels are 25 g/ml for Al, Cr and Pb, 15 g/
ml for Fe, and 10 g/ml for the remaining elements. Prepare any
standards containing less than 1 g/ml of metal on a daily
basis. Standards containing greater than 1 g/ml of metal
should be stable for a minimum of 1 to 2 weeks. For ICP-MS, follow
Method 6020 in EPA Publication SW-846 Third Edition (November 1986)
including updates I, II, IIA, IIB and III, as incorporated by reference
in Sec. 60.17(i).
7.5.35 GFAAS Standards. Sb, As, Cd, Co, Pb, Se, and Tl. Prepare a
10 g/ml standard by adding 1 ml of 1000 g/ml standard
to a 100-ml volumetric flask. Dilute with stirring to 100 ml with 10
percent HNO3. For GFAAS, matrix match the standards. Prepare
a 100 ng/ml standard by adding 1 ml of the 10 g/ml standard to
a 100-ml volumetric flask, and dilute to 100 ml with the appropriate
matrix solution. Prepare other standards by diluting the 100 ng/ml
standards. Use at least five standards to make up the standard curve.
Suggested levels are 0, 10, 50, 75, and 100 ng/ml. Prepare quality
control samples by making a separate 10 g/ml standard and
diluting until it is in the range of the samples. Prepare any standards
containing less than 1 g/ml of metal on a daily basis.
Standards containing greater than 1 g/ml of metal should be
stable for a minimum of 1 to 2 weeks.
7.5.36 Matrix Modifiers.
7.5.36.1 Nickel Nitrate, 1 Percent (V/V). Dissolve 4.956 g of
Ni(N03)26H20 or other nickel
compound suitable for preparation of this matrix modifier in
approximately 50 ml of water in a 100-ml volumetric flask. Dilute to
100 ml with water.
7.5.36.2 Nickel Nitrate, 0.1 Percent (V/V). Dilute 10 ml of 1
percent nickel nitrate solution to 100 ml with water. Inject an equal
amount of sample and this modifier into the graphite furnace during
GFAAS analysis for As.
7.5.36.3 Lanthanum. Carefully dissolve 0.5864 g of
La203 in 10 ml of concentrated HN03,
and dilute the solution by adding it with stirring to approximately 50
ml of water. Dilute to 100 ml with water, and mix well. Inject an equal
amount of sample and this modifier into the graphite furnace during
GFAAS analysis for Pb.
7.5.37 Whatman 40 and 541 Filter Papers (or equivalent). For
filtration of digested samples.

8.0 Sample Collection, Preservation, Transport, and Storage

8.1 Sampling. The complexity of this method is such that, to
obtain reliable results, both testers and analysts must be trained and
experienced with the test procedures, including source sampling;
reagent preparation and handling; sample handling; safety equipment and
procedures; analytical calculations; reporting; and the specific
procedural descriptions throughout this method.
8.1.1 Pretest Preparation. Follow the same general procedure given
in Method 5, Section 8.1, except that, unless particulate emissions are
to be determined, the filter need not be desiccated or weighed. First,
rinse all sampling train glassware with hot tap water and then wash in
hot soapy water. Next, rinse glassware three times with tap water,
followed by three additional rinses with water. Then soak all glassware
in a 10 percent (V/V) nitric acid solution for a minimum of 4 hours,
rinse three times with water, rinse a final time with acetone, and
allow to air dry. Cover all glassware openings where contamination can
occur until the sampling train is assembled for sampling.
8.1.2 Preliminary Determinations. Same as Method 5, Section 8.1.2.
8.1.3 Preparation of Sampling Train.
8.1.3.1 Set up the sampling train as shown in Figure 29-1. Follow
the same general procedures given in Method 5, Section 8.3, except
place 100 ml of the HNO3/H2O2 solution
(Section 7.3.1 of this method) in each of the second and third
impingers as shown in Figure 29-1. Place 100 ml of the acidic
KMnO4 absorbing solution (Section 7.3.2 of this method) in
each of the fifth and sixth impingers as shown in Figure 29-1, and
transfer approximately 200 to 300 g of pre-weighed silica gel from its
container to the last impinger. Alternatively, the silica gel may be
weighed directly in the impinger just prior to final train assembly.
8.1.3.2 Based on the specific source sampling conditions, the use
of an empty first impinger can be eliminated if the moisture to be
collected in the impingers will be less than approximately 100 ml.
8.1.3.3 If Hg analysis will not be performed, the fourth, fifth,
and sixth impingers as shown in Figure 29-1 are not required.
8.1.3.4 To insure leak-free sampling train connections and to
prevent possible sample contamination problems, use Teflon tape or
other non-contaminating material instead of silicone grease.
Precaution: Exercise extreme care to prevent contamination within
the train. Prevent the acidic KMnO4 from contacting any
glassware that contains sample material to be analyzed for Mn. Prevent
acidic H2O2 from mixing with the acidic
KMnO4.
8.1.4 Leak-Check Procedures. Follow the leak-check procedures
given in Method 5, Section 8.4.2 (Pretest Leak-Check), Section 8.4.3
(Leak-Checks During the Sample Run), and Section 8.4.4 (Post-Test Leak-
Checks).
8.1.5 Sampling Train Operation. Follow the procedures given in
Method 5, Section 8.5. When sampling for Hg, use a procedure analogous
to that

[[Page 62117]]

described in Section 8.1 of Method 101A, 40 CFR Part 61, Appendix B, if
necessary to maintain the desired color in the last acidified
permanganate impinger. For each run, record the data required on a data
sheet such as the one shown in Figure 5-3 of Method 5.
8.1.6 Calculation of Percent Isokinetic. Same as Method 5, Section
12.11.
8.2 Sample Recovery.
8.2.1 Begin cleanup procedures as soon as the probe is removed
from the stack at the end of a sampling period. The probe should be
allowed to cool prior to sample recovery. When it can be safely
handled, wipe off all external particulate matter near the tip of the
probe nozzle and place a rinsed, non-contaminating cap over the probe
nozzle to prevent losing or gaining particulate matter. Do not cap the
probe tip tightly while the sampling train is cooling; a vacuum can
form in the filter holder with the undesired result of drawing liquid
from the impingers onto the filter.
8.2.2 Before moving the sampling train to the cleanup site, remove
the probe from the sampling train and cap the open outlet. Be careful
not to lose any condensate that might be present. Cap the filter inlet
where the probe was fastened. Remove the umbilical cord from the last
impinger and cap the impinger. Cap the filter holder outlet and
impinger inlet. Use non-contaminating caps, whether ground-glass
stoppers, plastic caps, serum caps, or Teflon tape to close
these openings.
8.2.3 Alternatively, the following procedure may be used to
disassemble the train before the probe and filter holder/oven are
completely cooled: Initially disconnect the filter holder outlet/
impinger inlet and loosely cap the open ends. Then disconnect the probe
from the filter holder or cyclone inlet and loosely cap the open ends.
Cap the probe tip and remove the umbilical cord as previously
described.
8.2.4 Transfer the probe and filter-impinger assembly to a cleanup
area that is clean and protected from the wind and other potential
causes of contamination or loss of sample. Inspect the train before and
during disassembly and note any abnormal conditions. Take special
precautions to assure that all the items necessary for recovery do not
contaminate the samples. The sample is recovered and treated as follows
(see schematic in Figures 29-2a and 29-2b):
8.2.5 Container No. 1 (Sample Filter). Carefully remove the filter
from the filter holder and place it in its labeled petri dish
container. To handle the filter, use either acid-washed polypropylene
or Teflon coated tweezers or clean, disposable surgical gloves rinsed
with water and dried. If it is necessary to fold the filter, make
certain the particulate cake is inside the fold. Carefully transfer the
filter and any particulate matter or filter fibers that adhere to the
filter holder gasket to the petri dish by using a dry (acid-cleaned)
nylon bristle brush. Do not use any metal-containing materials when
recovering this train. Seal the labeled petri dish.
8.2.6 Container No. 2 (Acetone Rinse). Perform this procedure only
if a determination of particulate emissions is to be made.
Quantitatively recover particulate matter and any condensate from the
probe nozzle, probe fitting, probe liner, and front half of the filter
holder by washing these components with a total of 100 ml of acetone,
while simultaneously taking great care to see that no dust on the
outside of the probe or other surfaces gets in the sample. The use of
exactly 100 ml is necessary for the subsequent blank correction
procedures. 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.
8.2.6.1 Carefully remove the probe nozzle, and clean the inside
surface by rinsing with acetone from a wash bottle while brushing with
a non-metallic brush. Brush until the acetone rinse shows no visible
particles, then make a final rinse of the inside surface with acetone.
8.2.6.2 Brush and rinse the sample exposed inside parts of the
probe fitting with acetone in a similar way until no visible particles
remain. Rinse the probe liner with acetone by tilting and rotating the
probe while squirting acetone into its upper end so that all inside
surfaces will be wetted with acetone. Allow the acetone to drain from
the lower end into the sample container. A funnel may be used to aid in
transferring liquid washings to the container. Follow the acetone rinse
with a non-metallic 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 three times through the probe. Hold a
sample container underneath the lower end of the probe, and catch any
acetone and particulate matter which is brushed through the probe until
no visible particulate matter is carried out with the acetone or until
none remains in the probe liner on visual inspection. Rinse the brush
with acetone, and quantitatively collect these washings in the sample
container. After the brushing, make a final acetone rinse of the probe
as described above.
8.2.6.3 It is recommended that two people clean the probe to
minimize sample losses. Between sampling runs, keep brushes clean and
protected from contamination. Clean the inside of the front-half of the
filter holder by rubbing the surfaces with a non-metallic 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. After all acetone washings and particulate matter have
been collected in the sample container, tighten the lid so that acetone
will not leak out when shipped to the laboratory. Mark the height of
the fluid level to determine whether or not leakage occurred during
transport. Clearly label the container to identify its contents.
8.2.7 Container No. 3 (Probe Rinse). Keep the probe assembly clean
and free from contamination during the probe rinse. Rinse the probe
nozzle and fitting, probe liner, and front-half of the filter holder
thoroughly with a total of 100 ml of 0.1 N HNO3, and place
the wash into a sample storage container. Perform the rinses as
applicable and generally as described in Method 12, Section 8.7.1.
Record the volume of the rinses. Mark the height of the fluid level on
the outside of the storage container and use this mark to determine if
leakage occurs during transport. Seal the container, and clearly label
the contents. Finally, rinse the nozzle, probe liner, and front-half of
the filter holder with water followed by acetone, and discard these
rinses.

Note: The use of a total of exactly 100 ml is necessary for the
subsequent blank correction procedures.

8.2.8 Container No. 4 (Impingers 1 through 3, Moisture Knockout
Impinger, when used, HNO3/H2O2
Impingers Contents and Rinses). Due to the potentially large quantity
of liquid involved, the tester may place the impinger solutions from
impingers 1 through 3 in more than one container, if necessary. Measure
the liquid in the first three impingers to within 0.5 ml using a
graduated cylinder. Record the volume. This information is required to
calculate the moisture content of the sampled flue gas. Clean each of
the first three impingers, the filter support, the back half of the
filter housing, and connecting glassware by thoroughly rinsing with 100
ml of 0.1 N HNO3 using the procedure as applicable in Method
12, Section 8.7.3.

Note: The use of exactly 100 ml of 0.1 N HNO3 rinse
is necessary for the subsequent blank correction procedures. Combine
the rinses and impinger solutions, measure and

[[Page 62118]]

record the final total volume. Mark the height of the fluid level,
seal the container, and clearly label the contents.

8.2.9 Container Nos. 5A (0.1 N HNO3), 5B
(KMnO4/H2SO4 absorbing solution), and
5C (8 N HCl rinse and dilution).
8.2.9.1 When sampling for Hg, pour all the liquid from the
impinger (normally impinger No. 4) that immediately preceded the two
permanganate impingers into a graduated cylinder and measure the volume
to within 0.5 ml. This information is required to calculate the
moisture content of the sampled flue gas. Place the liquid in Container
No. 5A. Rinse the impinger with exactly 100 ml of 0.1 N HNO3
and place this rinse in Container No. 5A.
8.2.9.2 Pour all the liquid from the two permanganate impingers
into a graduated cylinder and measure the volume to within 0.5 ml. This
information is required to calculate the moisture content of the
sampled flue gas. Place this acidic KMnO4 solution into
Container No. 5B. Using a total of exactly 100 ml of fresh acidified
KMnO4 solution for all rinses (approximately 33 ml per
rinse), rinse the two permanganate impingers and connecting glassware a
minimum of three times. Pour the rinses into Container No. 5B,
carefully assuring transfer of all loose precipitated materials from
the two impingers. Similarly, using 100 ml total of water, rinse the
permanganate impingers and connecting glass a minimum of three times,
and pour the rinses into Container 5B, carefully assuring transfer of
any loose precipitated material. Mark the height of the fluid level,
and clearly label the contents. Read the Precaution: in Section 7.3.2.

Note: Due to the potential reaction of KMnO4 with
acid, pressure buildup can occur in the sample storage bottles. Do
not fill these bottles completely and take precautions to relieve
excess pressure. A No. 70-72 hole drilled in the container cap and
Teflon liner has been used successfully.

8.2.9.3 If no visible deposits remain after the water rinse, no
further rinse is necessary. However, if deposits remain on the impinger
surfaces, wash them with 25 ml of 8 N HCl, and place the wash in a
separate sample container labeled No. 5C containing 200 ml of water.
First, place 200 ml of water in the container. Then wash the impinger
walls and stem with the HCl by turning the impinger on its side and
rotating it so that the HCl contacts all inside surfaces. Use a total
of only 25 ml of 8 N HCl for rinsing both permanganate impingers
combined. Rinse the first impinger, then pour the actual rinse used for
the first impinger into the second impinger for its rinse. Finally,
pour the 25 ml of 8 N HCl rinse carefully into the container. Mark the
height of the fluid level on the outside of the container to determine
if leakage occurs during transport.
8.2.10 Container No. 6 (Silica Gel). Note the color of the
indicating silica gel to determine whether it has been completely spent
and make a notation of its condition. Transfer the silica gel from its
impinger to its original container and seal it. The tester may use a
funnel to pour the silica gel and a rubber policeman to remove the
silica gel from the impinger. The small amount of particles that might
adhere to the impinger wall need not be removed. Do not use water or
other liquids to transfer the silica gel since weight gained in the
silica gel impinger is used for moisture calculations. Alternatively,
if a balance is available in the field, record the weight of the spent
silica gel (or silica gel plus impinger) to the nearest 0.5 g.
8.2.11 Container No. 7 (Acetone Blank). If particulate emissions
are to be determined, at least once during each field test, place a
100-ml portion of the acetone used in the sample recovery process into
a container labeled No. 7. Seal the container.
8.2.12 Container No. 8A (0.1 N HNO3 Blank). At least
once during each field test, place 300 ml of the 0.1 N HNO3
solution used in the sample recovery process into a container labeled
No. 8A. Seal the container.
8.2.13 Container No. 8B (Water Blank). At least once during each
field test, place 100 ml of the water used in the sample recovery
process into a container labeled No. 8B. Seal the container.
8.2.14 Container No. 9 (5 Percent HNO3/10 Percent
H2O2 Blank). At least once during each field
test, place 200 ml of the 5 Percent HNO3/10 Percent
H2O2 solution used as the nitric acid impinger
reagent into a container labeled No. 9. Seal the container.
8.2.15 Container No. 10 (Acidified KMnO4 Blank). At
least once during each field test, place 100 ml of the acidified
KMnO4 solution used as the impinger solution and in the
sample recovery process into a container labeled No. 10. Prepare the
container as described in Section 8.2.9.2. Read the Precaution: in
Section 7.3.2 and read the NOTE in Section 8.2.9.2.
8.2.16 Container No. 11 (8 N HCl Blank). At least once during each
field test, place 200 ml of water into a sample container labeled No.
11. Then carefully add with stirring 25 ml of 8 N HCl. Mix well and
seal the container.
8.2.17 Container No. 12 (Sample Filter Blank). Once during each
field test, place into a petri dish labeled No. 12 three unused blank
filters from the same lot as the sampling filters. Seal the petri dish.
8.3 Sample Preparation. Note the level of the liquid in each of
the containers and determine if 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. A diagram illustrating sample preparation and
analysis procedures for each of the sample train components is shown in
Figure 29-3.
8.3.1 Container No. 1 (Sample Filter).
8.3.1.1 If particulate emissions are being determined, first
desiccate the filter and filter catch without added heat (do not heat
the filters to speed the drying) and weigh to a constant weight as
described in Section 11.2.1 of Method 5.
8.3.1.2 Following this procedure, or initially, if particulate
emissions are not being determined in addition to metals analysis,
divide the filter with its filter catch into portions containing
approximately 0.5 g each. Place the pieces in the analyst's choice of
either individual microwave pressure relief vessels or Parr Bombs. Add
6 ml of concentrated HNO3 and 4 ml of concentrated HF to
each vessel. For microwave heating, microwave the samples for
approximately 12 to 15 minutes total heating time as follows: heat for
2 to 3 minutes, then turn off the microwave for 2 to 3 minutes, then
heat for 2 to 3 minutes, etc., continue this alternation until the 12
to 15 minutes total heating time are completed (this procedure should
comprise approximately 24 to 30 minutes at 600 watts). Microwave
heating times are approximate and are dependent upon the number of
samples being digested simultaneously. Sufficient heating is evidenced
by sorbent reflux within the vessel. For conventional heating, heat the
Parr Bombs at 140 deg.C (285 deg.F) for 6 hours. Then cool the
samples to room temperature, and combine with the acid digested probe
rinse as required in Section 8.3.3.
8.3.1.3 If the sampling train includes an optional glass cyclone
in front of the filter, prepare and digest the cyclone catch by the
procedures described in Section 8.3.1.2 and then combine the digestate
with the digested filter sample.
8.3.2 Container No. 2 (Acetone Rinse). Note the level of liquid in
the

[[Page 62119]]

container and confirm on the analysis sheet whether or not leakage
occurred during transport. If a noticeable amount of leakage has
occurred, either void the sample or use methods, subject to the
approval of the Administrator, to correct the final results. Measure
the liquid in this container either volumetrically within 1 ml or
gravimetrically within 0.5 g. Transfer the contents to an acid-cleaned,
tared 250-ml beaker and evaporate to dryness at ambient temperature and
pressure. If particulate emissions are being determined, desiccate for
24 hours without added heat, weigh to a constant weight according to
the procedures described in Section 11.2.1 of Method 5, and report the
results to the nearest 0.1 mg. Redissolve the residue with 10 ml of
concentrated HNO3. Quantitatively combine the resultant
sample, including all liquid and any particulate matter, with Container
No. 3 before beginning Section 8.3.3.
8.3.3 Container No. 3 (Probe Rinse). Verify that the pH of this
sample is 2 or lower. If it is not, acidify the sample by careful
addition with stirring of concentrated HNO3 to pH 2. Use
water to rinse the sample into a beaker, and cover the beaker with a
ribbed watch glass. Reduce the sample volume to approximately 20 ml by
heating on a hot plate at a temperature just below boiling. Digest the
sample in microwave vessels or Parr Bombs by quantitatively
transferring the sample to the vessel or bomb, carefully adding the 6
ml of concentrated HNO3, 4 ml of concentrated HF, and then
continuing to follow the procedures described in Section 8.3.1.2. Then
combine the resultant sample directly with the acid digested portions
of the filter prepared previously in Section 8.3.1.2. The resultant
combined sample is referred to as ``Sample Fraction 1''. Filter the
combined sample using Whatman 541 filter paper. Dilute to 300 ml (or
the appropriate volume for the expected metals concentration) with
water. This diluted sample is ``Analytical Fraction 1''. Measure and
record the volume of Analytical Fraction 1 to within 0.1 ml.
Quantitatively remove a 50-ml aliquot and label as ``Analytical
Fraction 1B''. Label the remaining 250-ml portion as ``Analytical
Fraction 1A''. Analytical Fraction 1A is used for ICAP or AAS analysis
for all desired metals except Hg. Analytical Fraction 1B is used for
the determination of front-half Hg.
8.3.4 Container No. 4 (Impingers 1-3). Measure and record the
total volume of this sample to within 0.5 ml and label it ``Sample
Fraction 2''. Remove a 75- to 100-ml aliquot for Hg analysis and label
the aliquot ``Analytical Fraction 2B''. Label the remaining portion of
Container No. 4 as ``Sample Fraction 2A''. Sample Fraction 2A defines
the volume of Analytical Fraction 2A prior to digestion. All of Sample
Fraction 2A is digested to produce ``Analytical Fraction 2A''.
Analytical Fraction 2A defines the volume of Sample Fraction 2A after
its digestion and the volume of Analytical Fraction 2A is normally 150
ml. Analytical Fraction 2A is analyzed for all metals except Hg. Verify
that the pH of Sample Fraction 2A is 2 or lower. If necessary, use
concentrated HNO3 by careful addition and stirring to lower
Sample Fraction 2A to pH 2. Use water to rinse Sample Fraction 2A into
a beaker and then cover the beaker with a ribbed watchglass. Reduce
Sample Fraction 2A to approximately 20 ml by heating on a hot plate at
a temperature just below boiling. Then follow either of the digestion
procedures described in Sections 8.3.4.1 or 8.3.4.2.
8.3.4.1 Conventional Digestion Procedure. Add 30 ml of 50 percent
HNO3, and heat for 30 minutes on a hot plate to just below
boiling. Add 10 ml of 3 percent H2O2 and heat for
10 more minutes. Add 50 ml of hot water, and heat the sample for an
additional 20 minutes. Cool, filter the sample, and dilute to 150 ml
(or the appropriate volume for the expected metals concentrations) with
water. This dilution produces Analytical Fraction 2A. Measure and
record the volume to within 0.1 ml.
8.3.4.2 Microwave Digestion Procedure. Add 10 ml of 50 percent
HNO3 and heat for 6 minutes total heating time in
alternations of 1 to 2 minutes at 600 Watts followed by 1 to 2 minutes
with no power, etc., similar to the procedure described in Section
8.3.1. Allow the sample to cool. Add 10 ml of 3 percent
H2O2 and heat for 2 more minutes. Add 50 ml of
hot water, and heat for an additional 5 minutes. Cool, filter the
sample, and dilute to 150 ml (or the appropriate volume for the
expected metals concentrations) with water. This dilution produces
Analytical Fraction 2A. Measure and record the volume to within 0.1 ml.

Note: All microwave heating times given are approximate and are
dependent upon the number of samples being digested at a time.
Heating times as given above have been found acceptable for
simultaneous digestion of up to 12 individual samples. Sufficient
heating is evidenced by solvent reflux within the vessel.

8.3.5 Container No. 5A (Impinger 4), Container Nos. 5B and 5C
(Impingers 5 and 6). Keep the samples in Containers Nos. 5A, 5B, and 5C
separate from each other. Measure and record the volume of 5A to within
0.5 ml. Label the contents of Container No. 5A to be Analytical
Fraction 3A. To remove any brown MnO2 precipitate from the
contents of Container No. 5B, filter its contents through Whatman 40
filter paper into a 500 ml volumetric flask and dilute to volume with
water. Save the filter for digestion of the brown MnO2
precipitate. Label the 500 ml filtrate from Container No. 5B to be
Analytical Fraction 3B. Analyze Analytical Fraction 3B for Hg within 48
hours of the filtration step. Place the saved filter, which was used to
remove the brown MnO2 precipitate, into an appropriately
sized vented container, which will allow release of any gases including
chlorine formed when the filter is digested. In a laboratory hood which
will remove any gas produced by the digestion of the MnO2,
add 25 ml of 8 N HCl to the filter and allow to digest for a minimum of
24 hours at room temperature. Filter the contents of Container No. 5C
through a Whatman 40 filter into a 500-ml volumetric flask. Then filter
the result of the digestion of the brown MnO2 from Container
No. 5B through a Whatman 40 filter into the same 500-ml volumetric
flask, and dilute and mix well to volume with water. Discard the
Whatman 40 filter. Mark this combined 500-ml dilute HCl solution as
Analytical Fraction 3C.
8.3.6 Container No. 6 (Silica Gel). Weigh the spent silica gel (or
silica gel plus impinger) to the nearest 0.5 g using a balance.

9.0 Quality Control

9.1 Field Reagent Blanks, if analyzed. Perform the digestion and
analysis of the blanks in Container Nos. 7 through 12 that were
produced in Sections 8.2.11 through 8.2.17, respectively. For Hg field
reagent blanks, use a 10 ml aliquot for digestion and analysis.
9.1.1 Digest and analyze one of the filters from Container No. 12
per Section 8.3.1, 100 ml from Container No. 7 per Section 8.3.2, and
100 ml from Container No. 8A per Section 8.3.3. This step produces
blanks for Analytical Fractions 1A and 1B.
9.1.2 Combine 100 ml of Container No. 8A with 200 ml from
Container No. 9, and digest and analyze the resultant volume per
Section 8.3.4. This step produces blanks for Analytical Fractions 2A
and 2B.
9.1.3 Digest and analyze a 100-ml portion of Container No. 8A to
produce a blank for Analytical Fraction 3A.
9.1.4 Combine 100 ml from Container No. 10 with 33 ml from
Container No. 8B to produce a blank for Analytical Fraction 3B. Filter
the resultant 133 ml as described for

[[Page 62120]]

Container No. 5B in Section 8.3.5, except do not dilute the 133 ml.
Analyze this blank for Hg within 48 hr of the filtration step, and use
400 ml as the blank volume when calculating the blank mass value. Use
the actual volumes of the other analytical blanks when calculating
their mass values.
9.1.5 Digest the filter that was used to remove any brown
MnO2 precipitate from the blank for Analytical Fraction 3B
by the same procedure as described in Section 8.3.5 for the similar
sample filter. Filter the digestate and the contents of Container No.
11 through Whatman 40 paper into a 500-ml volumetric flask, and dilute
to volume with water. These steps produce a blank for Analytical
Fraction 3C.
9.1.6 Analyze the blanks for Analytical Fraction Blanks 1A and 2A
per Section 11.1.1 and/or Section 11.1.2. Analyze the blanks for
Analytical Fractions 1B, 2B, 3A, 3B, and 3C per Section 11.1.3.
Analysis of the blank for Analytical Fraction 1A produces the front-
half reagent blank correction values for the desired metals except for
Hg; Analysis of the blank for Analytical Fraction 1B produces the
front-half reagent blank correction value for Hg. Analysis of the blank
for Analytical Fraction 2A produces the back-half reagent blank
correction values for all of the desired metals except for Hg, while
separate analyses of the blanks for Analytical Fractions 2B, 3A, 3B,
and 3C produce the back-half reagent blank correction value for Hg.
9.2 Quality Control Samples. Analyze the following quality control
samples.
9.2.1 ICAP and ICP-MS Analysis. Follow the respective quality
control descriptions in Section 8 of Methods 6010 and 6020 in EPA
Publication SW-846 Third Edition (November 1986) including updates I,
II, IIA, IIB and III, as incorporated by reference in Sec. 60.17(i).
For the purposes of a source test that consists of three sample runs,
modify those requirements to include the following: two instrument
check standard runs, two calibration blank runs, one interference check
sample at the beginning of the analysis (analyze by Method of Standard
Additions unless within 25 percent), one quality control sample to
check the accuracy of the calibration standards (required to be within
25 percent of calibration), and one duplicate analysis (required to be
within 20 percent of average or repeat all analyses).
9.2.2 Direct Aspiration AAS and/or GFAAS Analysis for Sb, As, Ba,
Be, Cd, Cu, Cr, Co, Pb, Ni, Mn, Hg, P, Se, Ag, Tl, and Zn. Analyze all
samples in duplicate. Perform a matrix spike on at least one front-half
sample and one back-half sample, or one combined sample. If recoveries
of less than 75 percent or greater than 125 percent are obtained for
the matrix spike, analyze each sample by the Method of Standard
Additions. Analyze a quality control sample to check the accuracy of
the calibration standards. If the results are not within 20 percent,
repeat the calibration.
9.2.3 CVAAS Analysis for Hg. Analyze all samples in duplicate.
Analyze a quality control sample to check the accuracy of the
calibration standards (if not within 15 percent, repeat calibration).
Perform a matrix spike on one sample (if not within 25 percent, analyze
all samples by the Method of Standard Additions). Additional
information on quality control can be obtained from Method 7470 in EPA
Publication SW-846 Third Edition (November 1986) including updates I,
II, IIA, IIB and III, as incorporated by reference in Sec. 60.17(i), or
in Standard Methods for Water and Wastewater Method 303F.

10.0 Calibration and Standardization

Note: Maintain a laboratory log of all calibrations.

10.1 Sampling Train Calibration. Calibrate the sampling train
components according to the indicated sections of Method 5: Probe
Nozzle (Section 10.1); Pitot Tube (Section 10.2); Metering System
(Section 10.3); Probe Heater (Section 10.4); Temperature Sensors
(Section 10.5); Leak-Check of the Metering System (Section 8.4.1); and
Barometer (Section 10.6).
10.2 Inductively Coupled Argon Plasma Spectrometer Calibration.
Prepare standards as outlined in Section 7.5. Profile and calibrate the
instrument according to the manufacturer's recommended procedures using
those standards. Check the calibration once per hour. If the instrument
does not reproduce the standard concentrations within 10 percent,
perform the complete calibration procedures. Perform ICP-MS analysis by
following Method 6020 in EPA Publication SW-846 Third Edition (November
1986) including updates I, II, IIA, IIB and III, as incorporated by
reference in Sec. 60.17(i).
10.3 Atomic Absorption Spectrometer--Direct Aspiration AAS, GFAAS,
and CVAAS analyses. Prepare the standards as outlined in Section 7.5
and use them to calibrate the spectrometer. Calibration procedures are
also outlined in the EPA methods referred to in Table 29-2 and in
Method 7470 in EPA Publication SW-846 Third Edition (November 1986)
including updates I, II, IIA, IIB and III, as incorporated by reference
in Sec. 60.17(i), or in Standard Methods for Water and Wastewater
Method 303F (for Hg). Run each standard curve in duplicate and use the
mean values to calculate the calibration line. Recalibrate the
instrument approximately once every 10 to 12 samples.

11.0 Analytical Procedure

11.1 Sample Analysis. For each sampling train sample run, seven
individual analytical samples are generated; two for all desired metals
except Hg, and five for Hg. A schematic identifying each sample
container and the prescribed analytical preparation and analysis scheme
is shown in Figure 29-3. The first two analytical samples, labeled
Analytical Fractions 1A and 1B, consist of the digested samples from
the front-half of the train. Analytical Fraction 1A is for ICAP, ICP-MS
or AAS analysis as described in Sections 11.1.1 and 11.1.2,
respectively. Analytical Fraction 1B is for front-half Hg analysis as
described in Section 11.1.3. The contents of the back-half of the train
are used to prepare the third through seventh analytical samples. The
third and fourth analytical samples, labeled Analytical Fractions 2A
and 2B, contain the samples from the moisture removal impinger No. 1,
if used, and HNO3/H2O2 impingers Nos.
2 and 3. Analytical Fraction 2A is for ICAP, ICP-MS or AAS analysis for
target metals, except Hg. Analytical Fraction 2B is for analysis for
Hg. The fifth through seventh analytical samples, labeled Analytical
Fractions 3A, 3B, and 3C, consist of the impinger contents and rinses
from the empty impinger No. 4 and the H2SO4/
KMnO4 Impingers Nos. 5 and 6. These analytical samples are
for analysis for Hg as described in Section 11.1.3. The total back-half
Hg catch is determined from the sum of Analytical Fractions 2B, 3A, 3B,
and 3C. Analytical Fractions 1A and 2A can be combined proportionally
prior to analysis.
11.1.1 ICAP and ICP-MS Analysis. Analyze Analytical Fractions 1A
and 2A by ICAP using Method 6010 or Method 200.7 (40 CFR 136, Appendix
C). Calibrate the ICAP, and set up an analysis program as described in
Method 6010 or Method 200.7. Follow the quality control procedures
described in Section 9.2.1. Recommended wavelengths for analysis are as
shown in Table 29-2. These wavelengths represent the best combination
of specificity and potential detection limit. Other wavelengths may be
substituted if they can provide the needed specificity and detection
limit, and are treated with the same corrective techniques for

[[Page 62121]]

spectral interference. Initially, analyze all samples for the target
metals (except Hg) plus Fe and Al. If Fe and Al are present, the sample
might have to be diluted so that each of these elements is at a
concentration of less than 50 ppm so as to reduce their spectral
interferences on As, Cd, Cr, and Pb. Perform ICP-MS analysis by
following Method 6020 in EPA Publication SW-846 Third Edition (November
1986) including updates I, II, IIA, IIB and III, as incorporated by
reference in Sec. 60.17(i).

Note: When analyzing samples in a HF matrix, an alumina torch
should be used; since all front-half samples will contain HF, use an
alumina torch.

11.1.2 AAS by Direct Aspiration and/or GFAAS. If analysis of
metals in Analytical Fractions 1A and 2A by using GFAAS or direct
aspiration AAS is needed, use Table 29-3 to determine which techniques
and procedures to apply for each target metal. Use Table 29-3, if
necessary, to determine techniques for minimization of interferences.
Calibrate the instrument according to Section 10.3 and follow the
quality control procedures specified in Section 9.2.2.
11.1.3 CVAAS Hg analysis. Analyze Analytical Fractions 1B, 2B, 3A,
3B, and 3C separately for Hg using CVAAS following the method outlined
in Method 7470 in EPA Publication SW-846 Third Edition (November 1986)
including updates I, II, IIA, IIB and III, as incorporated by reference
in Sec. 60.17(i), or in Standard Methods for Water and Wastewater
Analysis, 15th Edition, Method 303F, or, optionally using Note No. 2 at
the end of this section. Set up the calibration curve (zero to 1000 ng)
as described in Method 7470 or similar to Method 303F using 300-ml BOD
bottles instead of Erlenmeyers. Perform the following for each Hg
analysis. From each original sample, select and record an aliquot in
the size range from 1 ml to 10 ml. If no prior knowledge of the
expected amount of Hg in the sample exists, a 5 ml aliquot is suggested
for the first dilution to 100 ml (see Note No. 1 at end of this
section). The total amount of Hg in the aliquot shall be less than 1
g and within the range (zero to 1000 ng) of the calibration
curve. Place the sample aliquot into a separate 300-ml BOD bottle, and
add enough water to make a total volume of 100 ml. Next add to it
sequentially the sample digestion solutions and perform the sample
preparation described in the procedures of Method 7470 or Method 303F.
(See Note No. 2 at the end of this section). If the maximum readings
are off-scale (because Hg in the aliquot exceeded the calibration
range; including the situation where only a 1-ml aliquot of the
original sample was digested), then dilute the original sample (or a
portion of it) with 0.15 percent HNO3 (1.5 ml concentrated
HNO3 per liter aqueous solution) so that when a 1- to 10-ml
aliquot of the ``0.15 HNO3 percent dilution of the original
sample'' is digested and analyzed by the procedures described above, it
will yield an analysis within the range of the calibration curve.

Note No. 1: When Hg levels in the sample fractions are below the
in-stack detection limit given in Table 29-1, select a 10 ml aliquot
for digestion and analysis as described.

Note No. 2: Optionally, Hg can be analyzed by using the CVAAS
analytical procedures given by some instrument manufacturer's
directions. These include calibration and quality control procedures
for the Leeman Model PS200, the Perkin Elmer FIAS systems, and
similar models, if available, of other instrument manufacturers. For
digestion and analyses by these instruments, perform the following
two steps: (1), Digest the sample aliquot through the addition of
the aqueous hydroxylamine hydrochloride/sodium chloride solution the
same as described in this section: (The Leeman, Perkin Elmer, and
similar instruments described in this note add automatically the
necessary stannous chloride solution during the automated analysis
of Hg.); (2), Upon completion of the digestion described in (1),
analyze the sample according to the instrument manufacturer's
directions. This approach allows multiple (including duplicate)
automated analyses of a digested sample aliquot.

12.0 Data Analysis and Calculations

12.1 Nomenclature.

A = Analytical detection limit, g/ml.
B = Liquid volume of digested sample prior to aliquotting for analysis,
ml.
C = Stack sample gas volume, dsm\3\.
Ca1 = Concentration of metal in Analytical Fraction 1A as
read from the standard curve, g/ml.
Ca2 = Concentration of metal in Analytical Fraction 2A as
read from the standard curve, (g/ml).
Cs = Concentration of a metal in the stack gas, mg/dscm.
D = In-stack detection limit, g/m\3\.
Fa = Aliquot factor, volume of Sample Fraction 2 divided by
volume of Sample Fraction 2A (see Section 8.3.4.)
Fd = Dilution factor (Fd = the inverse of the
fractional portion of the concentrated sample in the solution actually
used in the instrument to produce the reading Ca1. For
example, if a 2 ml aliquot of Analytical Fraction 1A is diluted to 10
ml to place it in the calibration range, Fd = 5).
Hgbh = Total mass of Hg collected in the back-half of the
sampling train, g.
Hgbh2 = Total mass of Hg collected in Sample Fraction 2,
g.
Hgbh3(A,B,C) = Total mass of Hg collected separately in
Fraction 3A, 3B, or 3C, g.
Hgbhb = Blank correction value for mass of Hg detected in
back-half field reagent blanks, g.
Hgfh = Total mass of Hg collected in the front-half of the
sampling train (Sample Fraction 1), g.
Hgfhb = Blank correction value for mass of Hg detected in
front-half field reagent blank, g.
Hgt = Total mass of Hg collected in the sampling train,
g.
Mbh = Total mass of each metal (except Hg) collected in the
back-half of the sampling train (Sample Fraction 2), g.
Mbhb = Blank correction value for mass of metal detected in
back-half field reagent blank, g.
Mfh = Total mass of each metal (except Hg) collected in the
front half of the sampling train (Sample Fraction 1), g.
Mfhb = Blank correction value for mass of metal detected in
front-half field reagent blank, g.
Mt = Total mass of each metal (separately stated for each
metal) collected in the sampling train, g.
Mt = Total mass of that metal collected in the sampling
train, g; (substitute Hgt for Mt for the
Hg calculation).
Qbh2 = Quantity of Hg, g, TOTAL in the ALIQUOT of
Analytical Fraction 2B selected for digestion and analysis . NOTE: For
example, if a 10 ml aliquot of Analytical Fraction 2B is taken and
digested and analyzed (according to Section 11.1.3 and its NOTES Nos. 1
and 2), then calculate and use the total amount of Hg in the 10 ml
aliquot for Qbh2.
Qbh3(A,B,C) = Quantity of Hg, g, TOTAL, separately,
in the ALIQUOT of Analytical Fraction 3A, 3B, or 3C selected for
digestion and analysis (see NOTES in Sections 12.7.1 and 12.7.2
describing the quantity ``Q'' and calculate similarly).
Qfh = Quantity of Hg, g, TOTAL in the ALIQUOT of
Analytical Fraction 1B selected for digestion and analysis. NOTE: For
example, if a 10 ml aliquot of Analytical Fraction 1B is taken and
digested and analyzed (according to Section 11.1.3 and its NOTES Nos. 1
and 2), then calculate and use the total amount of Hg in the 10 ml
aliquot for Qfh.
Va = Total volume of digested sample solution (Analytical
Fraction 2A),

[[Page 62122]]

ml (see Section 8.3.4.1 or 8.3.4.2, as applicable).
Vf1B = Volume of aliquot of Analytical Fraction 1B analyzed,
ml. NOTE: For example, if a 1 ml aliquot of Analytical Fraction 1B was
diluted to 50 ml with 0.15 percent HNO3 as described in
Section 11.1.3 to bring it into the proper analytical range, and then 1
ml of that 50-ml was digested according to Section 11.1.3 and analyzed,
Vf1B would be 0.02 ml.
Vf2B = Volume of Analytical Fraction 2B analyzed, ml. NOTE:
For example, if 1 ml of Analytical Fraction 2B was diluted to 10 ml
with 0.15 percent HNO3 as described in Section 11.1.3 to
bring it into the proper analytical range, and then 5 ml of that 10 ml
was analyzed, Vf2B would be 0.5 ml.
Vf3(A,B,C) = Volume, separately, of Analytical Fraction 3A,
3B, or 3C analyzed, ml (see previous notes in Sections 12.7.1 and
12.7.2, describing the quantity ``V'' and calculate similarly).
Vm(std) = Volume of gas sample as measured by the dry gas
meter, corrected to dry standard conditions, dscm.
Vsoln,1 = Total volume of digested sample solution
(Analytical Fraction 1), ml.
Vsoln,1 = Total volume of Analytical Fraction 1, ml.
Vsoln,2 = Total volume of Sample Fraction 2, ml.
Vsoln,3(A,B,C) = Total volume, separately, of Analytical
Fraction 3A, 3B, or 3C, ml.
K4 = 10-\3\ mg/g.

12.2 Dry Gas Volume. Using the data from this test, calculate
Vm(std), the dry gas sample volume at standard conditions as
outlined in Section 12.3 of Method 5.
12.3 Volume of Water Vapor and Moisture Content. Using the total
volume of condensate collected during the source sampling, calculate
the volume of water vapor Vw(std) and the moisture content
Bws of the stack gas. Use Equations 5-2 and 5-3 of Method 5.
12.4 Stack Gas Velocity. Using the data from this test and
Equation 2-9 of Method 2, calculate the average stack gas velocity.
12.5 In-Stack Detection Limits. Calculate the in-stack method
detection limits shown in Table 29-4 using the conditions described in
Section 13.3.1 as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.439

12.6 Metals (Except Hg) in Source Sample.
12.6.1 Analytical Fraction 1A, Front-Half, Metals (except Hg).
Calculate separately the amount of each metal collected in Sample
Fraction 1 of the sampling train using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.440

Note: If Analytical Fractions 1A and 2A are combined, use
proportional aliquots. Then make appropriate changes in Equations
29-2 through 29-4 to reflect this approach.

12.6.2 Analytical Fraction 2A, Back-Half, Metals (except Hg).
Calculate separately the amount of each metal collected in Fraction 2
of the sampling train using the following equation:
[GRAPHIC] [TIFF OMITTED] TR17OC00.441

12.6.3 Total Train, Metals (except Hg). Calculate the total amount
of each of the quantified metals collected in the sampling train as
follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.442

Note: If the measured blank value for the front half
(Mfhb) is in the range 0.0 to ``A'' g (where
``A'' g equals the value determined by multiplying 1.4
g/in.2 times the actual area in in.2
of the sample filter), use Mfhb to correct the emission
sample value (Mfh); if Mfhb exceeds ``A''
g, use the greater of I or II:
I. ``A'' g.
II. The lesser of (a) Mfhb, or (b) 5 percent of
Mfh. If the measured blank value for the back-half
(Mbhb) is in the range 0.0 to 1 g, use
Mbhb to correct the emission sample value
(Mbh); if Mbhb exceeds 1 g, use the
greater of I or II:
I. 1 g.
II. The lesser of (a) Mbhb, or (b) 5 percent of
Mbh.

12.7 Hg in Source Sample.
12.7.1 Analytical Fraction 1B; Front-Half Hg. Calculate the amount
ofHg collected in the front-half, Sample Fraction 1, of the sampling
train by using Equation 29-5:
[GRAPHIC] [TIFF OMITTED] TR17OC00.443

12.7.2 Analytical Fractions 2B, 3A, 3B, and 3C; Back Half Hg.
12.7.2.1 Calculate the amount of Hg collected in Sample Fraction 2
by using Equation 29-6:
[GRAPHIC] [TIFF OMITTED] TR17OC00.444

12.7.2.2 Calculate each of the back-half Hg values for Analytical
Fractions 3A, 3B, and 3C by using Equation 29-7:
[GRAPHIC] [TIFF OMITTED] TR17OC00.445

12.7.2.3 Calculate the total amount of Hg collected in the back-
half of the sampling train by using Equation 29-8:
[GRAPHIC] [TIFF OMITTED] TR17OC00.446

12.7.3 Total Train Hg Catch. Calculate the total amount of Hg
collected in the sampling train by using Equation 29-9:

[[Page 62123]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.447

Note: If the total of the measured blank values
(Hgfhb + Hgbhb) is in the range of 0.0 to 0.6
g, then use the total to correct the sample value
(Hgfh + Hgbh); if it exceeds 0.6 g,
use the greater of I. or II:
I. 0.6 g.
II. The lesser of (a) (Hgfhb + Hgbhb), or
(b) 5 percent of the sample value (Hgfh +
Hgbh).

12.8 Individual Metal Concentrations in Stack Gas. Calculate the
concentration of each metal in the stack gas (dry basis, adjusted to
standard conditions) by using Equation 29-10:
[GRAPHIC] [TIFF OMITTED] TR17OC00.448

12.9 Isokinetic Variation and Acceptable Results. Same as Method
5, Sections 12.11 and 12.12, respectively.

13.0 Method Performance

13.1 Range. For the analysis described and for similar analyses,
the ICAP response is linear over several orders of magnitude. Samples
containing metal concentrations in the nanograms per ml (ng/ml) to
micrograms per ml (g/ml) range in the final analytical
solution can be analyzed using this method. Samples containing greater
than approximately 50 g/ml As, Cr, or Pb should be diluted to
that level or lower for final analysis. Samples containing greater than
approximately 20 g/ml of Cd should be diluted to that level
before analysis.
13.2 Analytical Detection Limits.

Note: See Section 13.3 for the description of in-stack detection
limits.

13.2.1 ICAP analytical detection limits for the sample solutions
(based on SW-846, Method 6010) are approximately as follows: Sb (32 ng/
ml), As (53 ng/ml), Ba (2 ng/ml), Be (0.3 ng/ml), Cd (4 ng/ml), Cr (7
ng/ml), Co (7 ng/ml), Cu (6 ng/ml), Pb (42 ng/ml), Mn (2 ng/ml), Ni (15
ng/ml), P (75 ng/ml), Se (75 ng/ml), Ag (7 ng/ml), Tl (40 ng/ml), and
Zn (2 ng/ml). ICP-MS analytical detection limits (based on SW-846,
Method 6020) are lower generally by a factor of ten or more. Be is
lower by a factor of three. The actual sample analytical detection
limits are sample dependent and may vary due to the sample matrix.
13.2.2 The analytical detection limits for analysis by direct
aspiration AAS (based on SW-846, Method 7000 series) are approximately
as follows: Sb (200 ng/ml), As (2 ng/ml), Ba (100 ng/ml), Be (5 ng/ml),
Cd (5 ng/ml), Cr (50 ng/ml), Co (50 ng/ml), Cu (20 ng/ml), Pb (100 ng/
ml), Mn (10 ng/ml), Ni (40 ng/ml), Se (2 ng/ml), Ag (10 ng/ml), Tl (100
ng/ml), and Zn (5 ng/ml).
13.2.3 The detection limit for Hg by CVAAS (on the resultant
volume of the digestion of the aliquots taken for Hg analyses) can be
approximately 0.02 to 0.2 ng/ml, depending upon the type of CVAAS
analytical instrument used. 13.2.4 The use of GFAAS can enhance the
detection limits compared to direct aspiration AAS as follows: Sb (3
ng/ml), As (1 ng/ml), Be (0.2 ng/ml), Cd (0.1 ng/ml), Cr (1 ng/ml), Co
(1 ng/ml), Pb (1 ng/ml), Se (2 ng/ml), and Tl (1 ng/ml).
13.3 In-stack Detection Limits.
13.3.1 For test planning purposes in-stack detection limits can be
developed by using the following information: (1) The procedures
described in this method, (2) the analytical detection limits described
in Section 13.2 and in SW-846,(3) the normal volumes of 300 ml
(Analytical Fraction 1) for the front-half and 150 ml (Analytical
Fraction 2A) for the back-half samples, and (4) a stack gas sample
volume of 1.25 m3. The resultant in-stack method detection
limits for the above set of conditions are presented in Table 29-1 and
were calculated by using Eq. 29-1 shown in Section 12.5.
13.3.2 To ensure optimum precision/resolution in the analyses, the
target concentrations of metals in the analytical solutions should be
at least ten times their respective analytical detection limits. Under
certain conditions, and with greater care in the analytical procedure,
these concentrations can be as low as approximately three times the
respective analytical detection limits without seriously impairing the
precision of the analyses. On at least one sample run in the source
test, and for each metal analyzed, perform either repetitive analyses,
Method of Standard Additions, serial dilution, or matrix spike
addition, etc., to document the quality of the data.
13.3.3 Actual in-stack method detection limits are based on actual
source sampling parameters and analytical results as described above.
If required, the method in-stack detection limits can be improved over
those shown in Table 29-1 for a specific test by either increasing the
sampled stack gas volume, reducing the total volume of the digested
samples, improving the analytical detection limits, or any combination
of the three. For extremely low levels of Hg only, the aliquot size
selected for digestion and analysis can be increased to as much as 10
ml, thus improving the in-stack detection limit by a factor of ten
compared to a 1 ml aliquot size.
13.3.3.1 A nominal one hour sampling run will collect a stack gas
sampling volume of about 1.25 m3. If the sampling time is
increased to four hours and 5 m3 are collected, the in-stack
method detection limits would be improved by a factor of four compared
to the values shown in Table 29-1.
13.3.3.2 The in-stack detection limits assume that all of the
sample is digested and the final liquid volumes for analysis are the
normal values of 300 ml for Analytical Fraction 1, and 150 ml for
Analytical Fraction 2A. If the volume of Analytical Fraction 1 is
reduced from 300 to 30 ml, the in-stack detection limits for that
fraction of the sample would be improved by a factor of ten. If the
volume of Analytical Fraction 2A is reduced from 150 to 25 ml, the in-
stack detection limits for that fraction of the sample would be
improved by a factor of six. Matrix effect checks are necessary on
sample analyses and typically are of much greater significance for
samples that have been concentrated to less than the normal original
sample volume. Reduction of Analytical Fractions 1 and 2A to volumes of
less than 30 and 25 ml, respectively, could interfere with the
redissolving of the residue and could increase interference by other
compounds to an intolerable level.
13.3.3.3 When both of the modifications described in Sections
13.3.3.1 and 13.3.3.2 are used simultaneously on one sample, the
resultant improvements are multiplicative. For example, an increase in
stack gas volume by a factor of four and a reduction in the total
liquid sample digested volume of both Analytical Fractions 1 and 2A by
a factor of six would result in an improvement by a factor of twenty-
four of the in-stack method detection limit.
13.4 Precision. The precision (relative standard deviation) for
each metal detected in a method development test performed at a sewage
sludge incinerator were found to be as follows:

Sb (12.7 percent), As (13.5 percent), Ba (20.6 percent), Cd (11.5
percent), Cr (11.2 percent), Cu (11.5 percent), Pb (11.6 percent), P
(14.6 percent), Se (15.3 percent), Tl (12.3 percent), and Zn (11.8
percent). The precision for Ni was 7.7 percent for another test
conducted at a source simulator. Be, Mn, and Ag were not detected in
the tests. However,

[[Page 62124]]

based on the analytical detection limits of the ICAP for these metals,
their precisions could be similar to those for the other metals when
detected at similar levels.

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 References

1. Method 303F in Standard Methods for the Examination of Water
Wastewater, 15th Edition, 1980. Available from the American Public
Health Association, 1015 18th Street N.W., Washington, D.C. 20036.
2. EPA Methods 6010, 6020, 7000, 7041, 7060, 7131, 7421, 7470,
7740, and 7841, Test Methods for Evaluating Solid Waste: Physical/
Chemical Methods. SW-846, Third Edition, November 1986, with updates
I, II, IIA, IIB and III. Office of Solid Waste and Emergency
Response, U. S. Environmental Protection Agency, Washington, D.C.
20460.
3. EPA Method 200.7, Code of Federal Regulations, Title 40, Part
136, Appendix C. July 1, 1987.
4. EPA Methods 1 through 5, Code of Federal Regulations, Title
40, Part 60, Appendix A, July 1, 1991.
5. EPA Method 101A, Code of Federal Regulations, Title 40, Part
61, Appendix B, July 1, 1991.

17.0 Tables, Diagrams, Flowcharts, and Validation Data

Table 29-1.--In Stack Method Detection Limits (ug/m3) for the Front-Half, the Back Half, and the Total Sampling
Train Using ICAP, GFAAS, and CVAAS
----------------------------------------------------------------------------------------------------------------
Front-half: Back-half:
Metal probe and Back-half: impringers 4- Total train
filter impinters 1-3 6 a
----------------------------------------------------------------------------------------------------------------
Antimony........................................ 1 7.7 (0.7) 1 3.8 (0.4) .............. 1 11.5 (1.1)
Arsenic......................................... 1 12.7 (0.3) 1 6.4 (0.1) .............. 1 19.1 (0.4)
Barium.......................................... 0.5 0.3 .............. 0.8
Beryllium....................................... 1 0.07 (0.05) 1 0.04 (0.03) .............. 1 0.11 (0.08)
Cadmium......................................... 1 1.0 (0.02) 1 0.5 (0.01) .............. 1 1.5 (0.03)
Chromium........................................ 1 1.7 (0.2) 1 0.8 (0.1) .............. 1 2.5 (0.3)
Cobalt.......................................... 1 1.7 (0.2) 1 0.8 (0.1) .............. 1 2.5 (0.3)
Copper.......................................... 1.4 0.7 .............. 2.1
Lead............................................ 1 10.1 (0.2) 1 5.0 (0.1) .............. 1 15.1 (0.3)
Manganese....................................... 1 0.5 (0.2) 1 0.2 (0.1) .............. 1 0.7 (0.3)
Mercury......................................... 2 0.06 2 0.3 2 0.2 2 0.56
Nickel.......................................... 3.6 1.8 .............. 5.4
Phosphorus...................................... 18 9 .............. 27
Selenium........................................ 1 18 (0.5) 1 9 (0.3) .............. 1 27 (0.8)
Silver.......................................... 1.7 0.9 (0.7) .............. 2.6
Thallium........................................ 1 9.6 (0.2) 1 4.8 (0.1) .............. 1 14.4 (0.3)
Zinc............................................ 0.5 0.3 .............. 0.8
----------------------------------------------------------------------------------------------------------------
\a\ Mercury analysis only.
\1\ Detection limit when analyzed by ICAP or GFAAS as shown in parentheses (see Section 11.1.2).
\2\ Detection limit when anaylzed by CVAAS, estimated for Back-half and Total Train. See Sections 13.2 and
11.1.3. Note: Actual method in-stack detection limits may vary from these values, as described in Section
13.3.3.

Table 29-2.--Recommended Wavelengths for ICAP Analysis
------------------------------------------------------------------------
Wavelength
Analyte (nm)
------------------------------------------------------------------------
Aluminum (Al)........................................... 308.215
Antimony (Sb)........................................... 206.833
Arsenic (As)............................................ 193.696
Barium (Ba)............................................. 455.403
Beryllium (Be).......................................... 313.042
Cadmium (Cd)............................................ 226.502
Chromium (Cr)........................................... 267.716
Cobalt (Co)............................................. 228.616
Copper (Cu)............................................. 328.754
Iron (Fe)............................................... 259.940
Lead (Pb)............................................... 220.353
Manganese (Mn).......................................... 257.610
Nickel (Ni)............................................. 231.604
Phosphorus (P).......................................... 214.914
Selenium (Se)........................................... 196.026
Silver (Ag)............................................. 328.068
Thallium (T1)........................................... 190,864
Zinc (Zn)............................................... 213,856
------------------------------------------------------------------------

Table 29-3.--Applicable Techniques, Methods and Minimization of Interferences for AAS Analysis
----------------------------------------------------------------------------------------------------------------
Interferences
Metal Technique SW-846 \1\ Wavelength ----------------------------------------------
Methods No. (nm) Cause Minimization
----------------------------------------------------------------------------------------------------------------
Fe............... Aspiration.......... 7380 248.3 Contamination...... Great care taken to
avoid contamination.
Pb............... Aspiration.......... 7420 283.3 217.0 nm alternate. Background correction
required.
Pb............... Furnace............. 7421 283.3 Poor recoveries.... Matrix modifier, add 10
l of
phosphorus acid to 1 ml
of prepared sample in
sampler cup.
Mn............... Aspiration.......... 7460 279.5 403.1 nm alternate. Background correction
required.
Ni............... Aspiration.......... 7520 232.0 352.4 nm alternate Background correction
Fe, Co, and Cr. required. Matrix
Nonlinear response. matching or nitrous-
oxide/acetylene flame
Sample dilution or use
352.3 nm line

[[Page 62125]]

Se............... Furnace............. 7740 196.0 Volatility......... Spike samples and
reference materials and
add nickel nitrate to
minimize
volatilization.
Adsorption & Background correction is
scatter. required and Zeeman
background correction
can be useful.
Ag............... Aspiration.......... 7760 328.1 Adsorption & Background correction is
scatter AgCl required. Avoid
insoluble. hydrochloric acid
unless silver is in
solution as a chloride
complex. Sample and
standards monitored for
aspiration rate.
Tl............... Aspiration.......... 7840 276.8 Background correction is
required. Hydrochloric
acid should not be
used.
Tl............... Furnace............. 7841 276.8 Hydrochloric acid Background correction is
or chloride. required. Verify that
losses are not
occurring for
volatilization by
spiked samples or
standard addition;
Palladium is a suitable
matrix modifier. 4
Zn............... Aspiration.......... 7950 213.9 High Si, Cu, & P Strontium removes Cu and
Contamination. phosphate.
Great care taken to
avoid contamination.
Sb............... Aspiration.......... 7040 217.6 1000 mg/ml Pb, Ni, Use secondary wavelength
Cu, or acid. of 231.1 nm; match
sample & standards acid
concentration or use
nitrous oxide/acetylene
flame.
Sb............... Furnace............. 7041 217.6 High Pb............ Secondary wavelength or
Zeeman correction.
As............... Furnace............. 7060 193.7 Arsenic Spike samples and add
Volatilization nickel nitrate solution
Aluminum. to digestates prior to
analysis. Use Zeeman
background correction.
Ba............... Aspiration.......... 7080 553.6
Calcium............
Barium Ionization.. High hollow cathode
current and narrow band
set.
2 ml of KCl per 100 m1
of sample.
Be............... Aspiration.......... 7090 234.9 500 ppm Al. High Mg Add 0.1% fluoride.
and Si.
Be............... Furnace............. 7091 234.9 Be in optical path. Optimize parameters to
minimize effects.
Cd............... Aspiration.......... 7130 228.8 Absorption and Background correction is
light scattering. required.
Cd............... Furnace............. 7131 228.8 As above........... As above.
Excess Chloride.... Ammonium phosphate used
................. as a matrix modifier.
Pipet Tips......... Use cadmium-free tips.
Cr............... Aspiration.......... 7190 357.9 Alkali metal....... KCl ionization
suppressant in samples
and standards--Consult
mfgs' literature.
Co............... Furnace............. 7201 240.7 Excess chloride.... Use Method of Standard
Additions.
Cr............... Furnace............. 7191 357.9 200 mg/L Ca and P.. All calcium nitrate for
a know constant effect
and to eliminate effect
of phosphate.
Cu............... Aspiration.......... 7210 324.7 Absorption and Consult manufacturer's
Scatter. manual.
----------------------------------------------------------------------------------------------------------------
\1\ Refer to EPA publication SW-846 (Reference 2 in Section 16.0).

[[Page 62126]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.449

[[Page 62127]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.450

[[Page 62128]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.451

[[Page 62129]]

[GRAPHIC] [TIFF OMITTED] TR17OC00.452

BILLING CODE 6560-50-C

217. In Part 60, Appendix B is amended by revising Performance
Specifications 2, 3, 4, 4A, 5, 6, 7, 8, and 9 to read as follows:

[[Page 62130]]

Performance Specification 2--Specifications and Test Procedures for
SO2 and NOX Continuous Emission Monitoring
Systems in Stationary Sources

1.0 Scope and Application

1.1 Analytes

------------------------------------------------------------------------
Analyte CAS Nos.
------------------------------------------------------------------------
Sulfur Dioxide (SO2).................................... 7449-09-5
Nitrogen Oxides (NOx)................................... 10102-44-0
(NO2), 10024-
97-2 (NO)
------------------------------------------------------------------------

1.2 Applicability.
1.2.1 This specification is for evaluating the acceptability of
SO2 and NOX continuous emission monitoring
systems (CEMS) at the time of installation or soon after and whenever
specified in the regulations. The CEMS may include, for certain
stationary sources, a diluent (O2 or CO2)
monitor.
1.2.2 This specification is not designed to evaluate the installed
CEMS performance over an extended period of time nor does it identify
specific calibration techniques and other auxiliary procedures to
assess the CEMS performance. The source owner or operator is
responsible to calibrate, maintain, and operate the CEMS properly. The
Administrator may require, under Section 114 of the Act, the operator
to conduct CEMS performance evaluations at other times besides the
initial test to evaluate the CEMS performance. See 40 CFR Part 60,
Sec. 60.13(c).

2.0 Summary of Performance Specification

Procedures for measuring CEMS relative accuracy and calibration
drift are outlined. CEMS installation and measurement location
specifications, equipment specifications, performance specifications,
and data reduction procedures are included. Conformance of the CEMS
with the Performance Specification is determined.

3.0 Definitions

3.1 Calibration Drift (CD) means the difference in the CEMS output
readings from the established reference value after a stated period of
operation during which no unscheduled maintenance, repair, or
adjustment took place.
3.2 Centroidal Area means a concentric area that is geometrically
similar to the stack or duct cross section and is no greater than l
percent of the stack or duct cross-sectional area.
3.3 Continuous Emission Monitoring System means the total
equipment required for the determination of a gas concentration or
emission rate. The sample interface, pollutant analyzer, diluent
analyzer, and data recorder are the major subsystems of the CEMS.
3.4 Data Recorder means that portion of the CEMS that provides a
permanent record of the analyzer output. The data recorder may include
automatic data reduction capabilities.
3.5 Diluent Analyzer means that portion of the CEMS that senses
the diluent gas (i.e., CO2 or O2) and generates
an output proportional to the gas concentration.
3.6 Path CEMS means a CEMS that measures the gas concentration
along a path greater than 10 percent of the equivalent diameter of the
stack or duct cross section.
3.7 Point CEMS means a CEMS that measures the gas concentration
either at a single point or along a path equal to or less than 10
percent of the equivalent diameter of the stack or duct cross section.
3.8 Pollutant Analyzer means that portion of the CEMS that senses
the pollutant gas and generates an output proportional to the gas
concentration.
3.9 Relative Accuracy (RA) means the absolute mean difference
between the gas concentration or emission rate determined by the CEMS
and the value determined by the reference method (RM), plus the 2.5
percent error confidence coefficient of a series of tests, divided by
the mean of the RM tests or the applicable emission limit.
3.10 Sample Interface means that portion of the CEMS used for one
or more of the following: sample acquisition, sample delivery, sample
conditioning, or protection of the monitor from the effects of the
stack effluent.
3.11 Span Value means the concentration specified for the affected
source category in an applicable subpart of the regulations that is
used to set the calibration gas concentration and in determining
calibration drift.

4.0 Interferences. [Reserved]

5.0 Safety

The procedures required under this performance specification may
involve hazardous materials, operations, and equipment. This
performance specification may not address all of the safety problems
associated with these procedures. It is the responsibility of the user
to establish appropriate safety and health practices and determine the
applicable regulatory limitations prior to performing these procedures.
The CEMS user's manual and materials recommended by the reference
method should be consulted for specific precautions to be taken.

6.0 Equipment and Supplies

6.1 CEMS Equipment Specifications.
6.1.1 Data Recorder Scale. The CEMS data recorder output range
must include zero and a high-level value. The high-level value is
chosen by the source owner or operator and is defined as follows:
6.1.1.1 For a CEMS intended to measure an uncontrolled emission
(e.g., SO2 measurements at the inlet of a flue gas
desulfurization unit), the high-level value should be between 1.25 and
2 times the maximum potential emission level over the appropriate
averaging time, unless otherwise specified in an applicable subpart of
the regulations.
6.1.1.2 For a CEMS installed to measure controlled emissions or
emissions that are in compliance with an applicable regulation, the
high-level value between 1.5 times the pollutant concentration
corresponding to the emission standard level and the span value given
in the applicable regulations is adequate.
6.1.1.3 Alternative high-level values may be used, provided the
source can measure emissions which exceed the full-scale limit in
accordance with the requirements of applicable regulations.
6.1.1.4 If an analog data recorder is used, the data recorder
output must be established so that the high-level value would read
between 90 and 100 percent of the data recorder full scale. (This scale
requirement may not be applicable to digital data recorders.) The zero
and high level calibration gas, optical filter, or cell values should
be used to establish the data recorder scale.
6.1.2 The CEMS design should also allow the determination of
calibration drift at the zero and high-level values. If this is not
possible or practical, the design must allow these determinations to be
conducted at a low-level value (zero to 20 percent of the high-level
value) and at a value between 50 and 100 percent of the high-level
value. In special cases, the Administrator may approve a single-point
calibration-drift determination.
6.2 Other equipment and supplies, as needed by the applicable
reference method(s) (see Section 8.4.2 of this Performance
Specification), may be required.

7.0 Reagents and Standards

7.1 Reference Gases, Gas Cells, or Optical Filters. As specified
by the CEMS manufacturer for calibration of the CEMS (these need not be
certified).
7.2 Reagents and Standards. May be required as needed by the
applicable reference method(s) (see Section 8.4.2 of this Performance
Specification).

[[Page 62131]]

8.0 Performance Specification Test Procedure
8.1 Installation and Measurement Location Specifications.
8.1.1 CEMS Installation. Install the CEMS at an accessible
location where the pollutant concentration or emission rate
measurements are directly representative or can be corrected so as to
be representative of the total emissions from the affected facility or
at the measurement location cross section. Then select representative
measurement points or paths for monitoring in locations that the CEMS
will pass the RA test (see Section 8.4). If the cause of failure to
meet the RA test is determined to be the measurement location and a
satisfactory correction technique cannot be established, the
Administrator may require the CEMS to be relocated. Suggested
measurement locations and points or paths that are most likely to
provide data that will meet the RA requirements are listed below.
8.1.2 CEMS Measurement Location. It is suggested that the
measurement location be (1) at least two equivalent diameters
downstream from the nearest control device, the point of pollutant
generation, or other point at which a change in the pollutant
concentration or emission rate may occur and (2) at least a half
equivalent diameter upstream from the effluent exhaust or control
device.
8.1.2.1 Point CEMS. It is suggested that the measurement point be
(1) no less than 1.0 meter (3.3 ft) from the stack or duct wall or (2)
within or centrally located over the centroidal area of the stack or
duct cross section.
8.1.2.2 Path CEMS. It is suggested that the effective measurement
path (1) be totally within the inner area bounded by a line 1.0 meter
(3.3 ft) from the stack or duct wall, or (2) have at least 70 percent
of the path within the inner 50 percent of the stack or duct cross-
sectional area, or (3) be centrally located over any part of the
centroidal area.
8.1.3 Reference Method Measurement Location and Traverse Points.
8.1.3.1 Select, as appropriate, an accessible RM measurement point
at least two equivalent diameters downstream from the nearest control
device, the point of pollutant generation, or other point at which a
change in the pollutant concentration or emission rate may occur, and
at least a half equivalent diameter upstream from the effluent exhaust
or control device. When pollutant concentration changes are due solely
to diluent leakage (e.g., air heater leakages) and pollutants and
diluents are simultaneously measured at the same location, a half
diameter may be used in lieu of two equivalent diameters. The CEMS and
RM locations need not be the same.
8.1.3.2 Select traverse points that assure acquisition of
representative samples over the stack or duct cross section. The
minimum requirements are as follows: Establish a ``measurement line''
that passes through the centroidal area and in the direction of any
expected stratification. If this line interferes with the CEMS
measurements, displace the line up to 30 cm (12 in.) (or 5 percent of
the equivalent diameter of the cross section, whichever is less) from
the centroidal area. Locate three traverse points at 16.7, 50.0, and
83.3 percent of the measurement line. If the measurement line is longer
than 2.4 meters (7.8 ft) and pollutant stratification is not expected,
the three traverse points may be located on the line at 0.4, 1.2, and
2.0 meters from the stack or duct wall. This option must not be used
after wet scrubbers or at points where two streams with different
pollutant concentrations are combined. If stratification is suspected,
the following procedure is suggested. For rectangular ducts, locate at
least nine sample points in the cross section such that sample points
are the centroids of similarly-shaped, equal area divisions of the
cross section. Measure the pollutant concentration, and, if applicable,
the diluent concentration at each point using appropriate reference
methods or other appropriate instrument methods that give responses
relative to pollutant concentrations. Then calculate the mean value for
all sample points. For circular ducts, conduct a 12-point traverse
(i.e., six points on each of the two perpendicular diameters) locating
the sample points as described in 40 CFR 60, Appendix A, Method 1.
Perform the measurements and calculations as described above. Determine
if the mean pollutant concentration is more than 10% different from any
single point. If so, the cross section is considered to be stratified,
and the tester may not use the alternative traverse point locations
(...0.4, 1.2, and 2.0 meters from the stack or duct wall.) but must use
the three traverse points at 16.7, 50.0, and 83.3 percent of the entire
measurement line. Other traverse points may be selected, provided that
they can be shown to the satisfaction of the Administrator to provide a
representative sample over the stack or duct cross section. Conduct all
necessary RM tests within 3 cm (1.2 in.) of the traverse points, but no
closer than 3 cm (1.2 in.) to the stack or duct wall.
8.2 Pretest Preparation. Install the CEMS, prepare the RM test
site according to the specifications in Section 8.1, and prepare the
CEMS for operation according to the manufacturer's written
instructions.
8.3 Calibration Drift Test Procedure.
8.3.1 CD Test Period. While the affected facility is operating at
more than 50 percent of normal load, or as specified in an applicable
subpart, determine the magnitude of the CD once each day (at 24-hour
intervals) for 7 consecutive days according to the procedure given in
Sections 8.3.2 through 8.3.4.
8.3.2 The purpose of the CD measurement is to verify the ability
of the CEMS to conform to the established CEMS calibration used for
determining the emission concentration or emission rate. Therefore, if
periodic automatic or manual adjustments are made to the CEMS zero and
calibration settings, conduct the CD test immediately before these
adjustments, or conduct it in such a way that the CD can be determined.
8.3.3 Conduct the CD test at the two points specified in Section
6.1.2. Introduce to the CEMS the reference gases, gas cells, or optical
filters (these need not be certified). Record the CEMS response and
subtract this value from the reference value (see example data sheet in
Figure 2-1).
8.4 Relative Accuracy Test Procedure.
8.4.1 RA Test Period. Conduct the RA test according to the
procedure given in Sections 8.4.2 through 8.4.6 while the affected
facility is operating at more than 50 percent of normal load, or as
specified in an applicable subpart. The RA test may be conducted during
the CD test period.
8.4.2 Reference Methods. Unless otherwise specified in an
applicable subpart of the regulations, Methods 3B, 4, 6, and 7, or
their approved alternatives, are the reference methods for diluent
(O2 and CO2), moisture, SO2, and
NOx, respectively.
8.4.3 Sampling Strategy for RM Tests. Conduct the RM tests in such
a way that they will yield results representative of the emissions from
the source and can be correlated to the CEMS data. It is preferable to
conduct the diluent (if applicable), moisture (if needed), and
pollutant measurements simultaneously. However, diluent and moisture
measurements that are taken within an hour of the pollutant
measurements may be used to calculate dry pollutant concentration and
emission rates. In order to correlate the CEMS and RM data properly,
note the beginning and end of each RM test period of each run
(including the exact time of day) on the CEMS chart recordings or other
permanent record of

[[Page 62132]]

output. Use the following strategies for the RM tests:
8.4.3.1 For integrated samples (e.g., Methods 6 and Method 4),
make a sample traverse of at least 21 minutes, sampling for an equal
time at each traverse point (see Section 8.1.3.2 for discussion of
traverse points.
8.4.3.2 For grab samples (e.g., Method 7), take one sample at each
traverse point, scheduling the grab samples so that they are taken
simultaneously (within a 3-minute period) or at an equal interval of
time apart over the span of time the CEM pollutant is measured. A test
run for grab samples must be made up of at least three separate
measurements.

Note: At times, CEMS RA tests are conducted during new source
performance standards performance tests. In these cases, RM results
obtained during CEMS RA tests may be used to determine compliance as
long as the source and test conditions are consistent with the
applicable regulations.

8.4.4 Number of RM Tests. Conduct a minimum of nine sets of all
necessary RM test runs.

Note: More than nine sets of RM tests may be performed. If this
option is chosen, a maximum of three sets of the test results may be
rejected so long as the total number of test results used to
determine the RA is greater than or equal to nine. However, all data
must be reported, including the rejected data.

8.4.5 Correlation of RM and CEMS Data. Correlate the CEMS and the
RM test data as to the time and duration by first determining from the
CEMS final output (the one used for reporting) the integrated average
pollutant concentration or emission rate for each pollutant RM test
period. Consider system response time, if important, and confirm that
the pair of results are on a consistent moisture, temperature, and
diluent concentration basis. Then, compare each integrated CEMS value
against the corresponding average RM value. Use the following
guidelines to make these comparisons.
8.4.5.1 If the RM has an integrated sampling technique, make a
direct comparison of the RM results and CEMS integrated average value.
8.4.5.2 If the RM has a grab sampling technique, first average the
results from all grab samples taken during the test run, and then
compare this average value against the integrated value obtained from
the CEMS chart recording or output during the run. If the pollutant
concentration is varying with time over the run, the arithmetic average
of the CEMS value recorded at the time of each grab sample may be used.
8.4.6 Calculate the mean difference between the RM and CEMS values
in the units of the emission standard, the standard deviation, the
confidence coefficient, and the relative accuracy according to the
procedures in Section 12.0.
8.5 Reporting. At a minimum (check with the appropriate regional
office, State, or Local agency for additional requirements, if any),
summarize in tabular form the results of the CD tests and the RA tests
or alternative RA procedure, as appropriate. Include all data sheets,
calculations, charts (records of CEMS responses), cylinder gas
concentration certifications, and calibration cell response
certifications (if applicable) necessary to confirm that the
performance of the CEMS met the performance specifications.

9.0 Quality Control [Reserved]

10.0 Calibration and Standardization [Reserved]

11.0 Analytical Procedure

Sample collection and analysis are concurrent for this Performance
Specification (see Section 8.0). Refer to the RM for specific
analytical procedures.

12.0 Calculations and Data Analysis

Summarize the results on a data sheet similar to that shown in
Figure 2-2 (in Section 18.0).
12.1 All data from the RM and CEMS must be on a consistent dry
basis and, as applicable, on a consistent diluent basis and in the
units of the emission standard. Correct the RM and CEMS data for
moisture and diluent as follows:
12.1.1 Moisture Correction (as applicable). Correct each wet RM
run for moisture with the corresponding Method 4 data; correct each wet
CEMS run using the corresponding CEMS moisture monitor date using
Equation 2-1.
[GRAPHIC] [TIFF OMITTED] TR17OC00.453

12.1.2 Correction to Units of Standard (as applicable). Correct
each dry RM run to the units of the emission standard with the
corresponding Method 3B data; correct each dry CEMS run using the
corresponding CEMS diluent monitor data as follows:
12.1.2.1 Correct to Diluent Basis. The following is an example of
concentration (ppm) correction to 7% oxygen.
[GRAPHIC] [TIFF OMITTED] TR17OC00.454

The following is an example of mass/gross calorific value (lbs/
million Btu) correction.

lbs/MMBtu = Conc(dry) (F-factor) (20.9/20.9-%02)

12.2 Arithmetic Mean. Calculate the arithmetic mean of the
difference, d, of a data set as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.455

Where:

n = Number of data points.
[GRAPHIC] [TIFF OMITTED] TR17OC00.456

[[Page 62133]]

12.3 Standard Deviation. Calculate the standard deviation,
Sd, as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.457

12.4 Confidence Coefficient. Calculate the 2.5 percent error
confidence coefficient (one-tailed), CC, as follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.458

Where:

t0.975 = t-value (see Table 2-1).

12.5 Relative Accuracy. Calculate the RA of a set of data as
follows:
[GRAPHIC] [TIFF OMITTED] TR17OC00.459

Where:

|d| = Absolute value of the mean differences (from Equation 2-3).
|CC| = Absolute value of the confidence coefficient (from Equation 2-
3).
RM = Average RM value. In cases where the average emissions for the
test are less than 50 percent of the applicable standard, substitute
the emission standard value in the denominator of Eq. 2-6 in place of
RM. In all other cases, use RM.

13.0 Method Performance

13.1 Calibration Drift Performance Specification. The CEMS
calibration must not drift or deviate from the reference value of the
gas cylinder, gas cell, or optical filter by more than 2.5 percent of
the span value. If the CEMS includes pollutant and diluent monitors,
the CD must be determined separately for each in terms of
concentrations (See Performance Specification 3 for the diluent
specifications), and none of the CDs may exceed the specification.
13.2 Relative Accuracy Performance Specification. The RA of the
CEMS must be no greater than 20 percent when RM is used in the
denominator of Eq. 2-6 (average emissions during test are greater than
50 percent of the emission standard) or 10 percent when the applicable
emission standard is used in the denominator of Eq. 2-6 (average
emissions during test are less than 50 percent of the emission
standard).
13.3 For instruments that use common components to measure more
than one effluent gas constituent, all channels must simultaneously
pass the RA requirement, unless it can be demonstrated that any
adjustments made to one channel did not affect the others.

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 Alternative Procedures

Paragraphs 60.13(j)(1) and (2) of 40 CFR part 60 contain criteria
for which the reference method procedure for determining relative
accuracy (see Section 8.4 of this Performance Specification) may be
waived and the following procedure substituted.
16.1 Conduct a complete CEMS status check following the
manufacturer's written instructions. The check should include operation
of the light source, signal receiver, timing mechanism functions, data
acquisition and data reduction functions, data recorders, mechanically
operated functions (mirror movements, zero pipe operation, calibration
gas valve operations, etc.), sample filters, sample line heaters,
moisture traps, and other related functions of the CEMS, as applicable.
All parts of the CEMS shall be functioning properly before proceeding
to the alternative RA procedure.
16.2 Alternative RA Procedure.
16.2.1 Challenge each monitor (both pollutant and diluent, if
applicable) with cylinder gases of known concentrations or calibration
cells that produce known responses at two measurement points within the
ranges shown in Table 2-2 (Section 18).
16.2.2 Use a separate cylinder gas (for point CEMS only) or
calibration cell (for path CEMS or where compressed gas cylinders can
not be used) for measurement points 1 and 2. Challenge the CEMS and
record the responses three times at each measurement point. The
Administrator may allow dilution of cylinder gas using the performance
criteria in Test Method 205, 40 CFR Part 51, Appendix M. Use the
average of the three responses in determining relative accuracy.
16.2.3 Operate each monitor in its normal sampling mode as nearly
as possible. When using cylinder gases, pass the cylinder gas through
all filters, scrubbers, conditioners, and other monitor components used
during normal sampling and as much of the sampling probe as practical.
When using calibration cells, the CEMS components used in the normal
sampling mode should not be by-passed during the RA determination.
These include light sources, lenses, detectors, and reference cells.
The CEMS should be challenged at each measurement point for a
sufficient period of time to assure adsorption-desorption reactions on
the CEMS surfaces have stabilized.
16.2.4 Use cylinder gases that have been certified by comparison
to National Institute of Standards and Technology (NIST) gaseous
standard reference material (SRM) or NIST/EPA approved gas
manufacturer's certified reference material (CRM) (See Reference 2 in
Section 17.0) following EPA Traceability Protocol Number 1 (See
Reference 3 in Section 17.0). As an alternative to Protocol Number 1
gases, CRM's may be used directly as alternative RA cylinder gases. A
list of gas manufacturers that have prepared approved CRM's is
available from EPA at the address shown in Reference 2. Procedures for
preparation of CRM's are described in Reference 2.
16.2.5 Use calibration cells certified by the manufacturer to
produce a known response in the CEMS. The cell certification procedure
shall include determination of CEMS response produced by the
calibration cell in direct comparison with measurement of gases of
known concentration. This can be accomplished using SRM or CRM gases in
a laboratory source simulator or through extended tests using reference
methods at the CEMS location in the exhaust stack. These procedures are
discussed in Reference 4 in Section 17.0. The calibration cell
certification procedure is subject to approval of the Administrator.
16.3 The differences between the known concentrations of the
cylinder gases and the concentrations indicated by the CEMS are used to
assess the accuracy of the CEMS. The calculations and limits of
acceptable relative accuracy are as follows:
16.3.1 For pollutant CEMS:
[GRAPHIC] [TIFF OMITTED] TR17OC00.460

[[Page 62134]]

Where:

d = Average difference between responses and the concentration/
responses (see Section 16.2.2).
AC = The known concentration/response of the cylinder gas or
calibration cell.

16.3.2 For diluent CEMS:

RA = |d| O.7 percent O2 or CO2, as
applicable.

Note: Waiver of the relative accuracy test in favor of the
alternative RA procedure does not preclude the requirements to
complete the CD tests nor any other requirements specified in an
applicable subpart for reporting CEMS data and performing CEMS drift
checks or audits.

17.0 References

1. Department of Commerce. Experimental Statistics. Handbook 91.
Washington, D.C. p. 3-31, paragraphs 3-3.1.4.
2. ``A Procedure for Establishing Traceability of Gas Mixtures
to Certain National Bureau of Standards Standard Reference
Materials.'' Joint publication by NBS and EPA. EPA 600/7-81-010.
Available from U.S. Environmental Protection Agency, Quality
Assurance Division (MD-77), Research Triangle Park, North Carolina
27711.
3. ``Traceability Protocol for Establishing True Concentrations
of Gases Used for Calibration and Audits of Continuous Source
Emission Monitors. (Protocol Number 1).'' June 1978. Protocol Number
1 is included in the Quality Assurance Handbook for Air Pollution
Measurement Systems, Volume III, Stationary Source Specific Methods.
EPA-600/4-77-027b. August 1977.
4. ``Gaseous Continuous Emission Monitoring Systems--Performance
Specification Guidelines for SO2, NOX,
CO2, O2, and TRS.'' EPA-450/3-82-026.
Available from the U.S. EPA, Emission Measurement Center, Emission
Monitoring and Data Analysis Division (MD-19), Research Triangle
Park, North Carolina 27711.

18.0 Tables, Diagrams, Flowcharts, and Validation Data

Table 2-1.--t-Values
----------------------------------------------------------------------------------------------------------------
na t0.975 na t0.975 na t0.975
----------------------------------------------------------------------------------------------------------------
2.............................................. 12.706 7 2.447 12 2.201
3.............................................. 4.303 8 2.365 13 2.179
4.............................................. 3.182 9 2.306 14 2.160
5.............................................. 2.776 10 2.262 15 2.145
6.............................................. 2.571 11 2.228 16 2.131
----------------------------------------------------------------------------------------------------------------
a The values in this table are already corrected for n-1 degrees of freedom. Use n equal to the number of
individual values.

Table 2-2.--Measurement Range
--------------------------------------------------------------------------------------------------------------------------------------------------------
Diluent monitor for
Measurement point Pollutant monitor -----------------------------------------------------------------------
CO2 O2
--------------------------------------------------------------------------------------------------------------------------------------------------------
1.................................. 20-30% of span value....................... 5-8% by volume.................... 4-6% by volume.
2.................................. 50-60% of span value....................... 10-14% by volume.................. 8-12% by volume.

------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Percent of span value (C-M)/
Day Date and time Calibration value (C) Monitor value (M) Difference (C-M) span value x 100
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Low-level........................ ........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
High-level....................... ........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
........... .......................... ................................. .......................... ..................... ..............................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------

Figure 2-1. Calibration Drift Determination

[[Page 62135]]

Figure 2-2. Relative Accuracy Determination.
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
SO2 NOXb CO2 or O2a SO2a NOXa
Run No. Date and time ---------------------------------------------------------------------------------------------------------------------------------------------------
RM CEMS Diff RM CEMS Diff RM CEMS RM CEMS Diff RM CEMS Diff
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
ppmc
ppmc %c %c mass/GCV
mass/GCV
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1............................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
2............................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
3............................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
4............................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
5............................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
6............................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
7............................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
8............................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
9............................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
10...........................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
11...........................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
12...........................
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Average
Confidence Interval
Accuracy
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
a For steam generators.
b Average of three samples.
c Make sure that RM and CEMS data are on a consistent basis, either wet or dry.

[[Page 62136]]

Performance Specification 3--Specifications and Test Procedures for
O2 and CO2 Continuous Emission Monitoring
Systems in Stationary Sources

1.0 Scope and Application

1.1 Analytes.

------------------------------------------------------------------------
Analytes CAS No.
------------------------------------------------------------------------
Carbon Dioxide (CO2).................................... 124-38-9
Oxygen (O2)............................................. 7782-44-7
------------------------------------------------------------------------

1.2 Applicability.
1.2.1 This specification is for evaluating acceptability of
O2 and CO2 continuous emission monitoring systems
(CEMS) at the time of installation or soon after and whenever specified
in an applicable subpart of the regulations. This specification applies
to O2 or CO2 monitors that are not included under
Performance Specification 2 (PS 2).
1.2.2 This specification is not designed to evaluate the installed
CEMS performance over an extended period of time, nor does it identify
specific calibration techniques and other auxiliary procedures to
assess the CEMS performance. The source owner or operator, is
responsible to calibrate, maintain, and operate the CEMS properly. The
Administrator may require, under Section 114 of the Act, the operator
to conduct CEMS performance evaluations at other times besides the
initial test to evaluate the CEMS performance. See 40 CFR part 60,
Section 60.13(c).
1.2.3 The definitions, installation and measurement location
specifications, calculations and data analysis, and references are the
same as in PS 2, Sections 3, 8.1, 12, and 17, respectively, and also
apply to O2 and CO2 CEMS under this
specification. The performance and equipment specifications and the
relative accuracy (RA) test procedures for O2 and
CO2 CEMS do not differ from those for SO2 and
NOx CEMS (see PS 2), except as noted below.

2.0 Summary of Performance Specification

The RA and calibration drift (CD) tests are conducted to determine
conformance of the CEMS to the specification.

3.0 Definitions

Same as in Section 3.0 of PS 2.

4.0 Interferences [Reserved]

5.0 Safety

This performance specification may involve hazardous materials,
operations, and equipment. This performance specification may not
address all of the safety problems associated with its use. It is the
responsibility of the user to establish appropriate safety and health
practices and determine the applicable regulatory limitations prior to
performing this performance specification. The CEMS users manual should
be consulted for specific precautions to be taken with regard to the
analytical procedures.

6.0 Equipment and Supplies

Same as Section 6.0 of PS2.

7.0 Reagents and Standards

Same as Section 7.0 of PS2.

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Relative Accuracy Test Procedure. Sampling Strategy for
reference method (RM) Tests, Correlation of RM and CEMS Data, and
Number of RM Tests. Same as PS 2, Sections 8.4.3, 8.4.5, and 8.4.4,
respectively.
8.2 Reference Method. Unless otherwise specified in an applicable
subpart of the regulations, Method 3B or other approved alternative is
the RM for O2 or CO2.

9.0 Quality Control [Reserved]

10.0 Calibration and Standardization [Reserved]

11.0 Analytical Procedure

Sample collection and analyses are concurrent for this performance
specification (see Section 8). Refer to the RM for specific analytical
procedures.

12.0 Calculations and Data Analysis

Summarize the results on a data sheet similar to that shown in
Figure 2.2 of PS2. Calculate the arithmetic difference between the RM
and the CEMS output for each run. The average difference of the nine
(or more) data sets constitute the RA.

13.0 Method Performance

13.1 Calibration Drift Performance Specification. The CEMS
calibration must not drift by more than 0.5 percent O2 or
CO2 from the reference value of the gas, gas cell, or
optical filter.
13.2 CEMS Relative Accuracy Performance Specification. The RA of
the CEMS must be no greater than 1.0 percent O2 or
CO2.

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 References

Same as in Section 17.0 of PS 2.

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

Performance Specification 4--Specifications and Test Procedures for
Carbon Monoxide Continuous Emission Monitoring Systems in
Stationary Sources

1.0 Scope and Application

1.1 Analytes.

------------------------------------------------------------------------
Analyte CAS No.
------------------------------------------------------------------------
Carbon Monoxide (CO)................................... 630-08-0
------------------------------------------------------------------------

1.2 Applicability.
1.2.1 This specification is for evaluating the acceptability of
carbon monoxide (CO) continuous emission monitoring systems (CEMS) at
the time of installation or soon after and whenever specified in an
applicable subpart of the regulations. This specification was developed
primarily for CEMS having span values of 1,000 ppmv CO.
1.2.2 This specification is not designed to evaluate the installed
CEMS performance over an extended period of time nor does it identify
specific calibration techniques and other auxiliary procedures to
assess CEMS performance. The source owner or operator, is responsible
to calibrate, maintain, and operate the CEMS. The Administrator may
require, under Section 114 of the Act, the source owner or operator to
conduct CEMS performance evaluations at other times besides the initial
test to evaluate the CEMS performance. See 40 CFR part 60, Section
60.13(c).
1.2.3 The definitions, performance specification test procedures,
calculations, and data analysis procedures for determining calibration
drift (CD) and relative accuracy (RA) of Performance Specification 2
(PS 2), Sections 3, 8.0, and 12, respectively, apply to this
specification.

2.0 Summary of Performance Specification

The CD and RA tests are conducted to determine conformance of the
CEMS to the specification.

[[Page 62137]]

3.0 Definitions

Same as in Section 3.0 of PS 2.

4.0 Interferences [Reserved]

5.0 Safety

6.0 Equipment and Supplies

Same as Section 6.0 of PS 2.

7.0 Reagents and Standards

Same as Section 7.0 of PS 2.

8.0 Sample Collection, Preservation, Storage, and Transport

9.0 Quality Control [Reserved]

10.0 Calibration and Standardization [Reserved]

11.0 Analytical Procedure

Sample collection and analysis are concurrent for this performance
specification (see Section 8.0). Refer to the RM for specific
analytical procedures.

12.0 Calculations and Data Analysis

Same as Section 12.0 of PS 2.

13.0 Method Performance

13.1 Calibration Drift. The CEMS calibration must not drift or
deviate from the reference value of the calibration gas, gas cell, or
optical filter by more than 5 percent of the established span value for
6 out of 7 test days (e.g., the established span value is 1000 ppm for
Subpart J affected facilities).
13.2 Relative Accuracy. The RA of the CEMS must be no greater than
10 percent when the average RM value is used to calculate RA or 5
percent when the applicable emission standard is used to calculate RA.

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 Alternative Procedures [Reserved]

17.0 References

1. Ferguson, B.B., R.E. Lester, and W.J. Mitchell. Field
Evaluation of Carbon Monoxide and Hydrogen Sulfide Continuous
Emission Monitors at an Oil Refinery. U.S. Environmental Protection
Agency. Research Triangle Park, N.C. Publication No. EPA-600/4-82-
054. August 1982. 100 p.
2. ``Gaseous Continuous Emission Monitoring Systems--Performance
Specification Guidelines for SO2, NOx,
CO2, O2, and TRS.'' EPA-450/3-82-026. U.S.
Environmental Protection Agency, Technical Support Division (MD-19),
Research Triangle Park, NC 27711.
3. Repp, M. Evaluation of Continuous Monitors for Carbon
Monoxide in Stationary Sources. U.S. Environmental Protection
Agency. Research Triangle Park, N.C. Publication No. EPA-600/2-77-
063. March 1977. 155 p.
4. Smith, F., D.E. Wagoner, and R.P. Donovan. Guidelines for
Development of a Quality Assurance Program: Volume VIII--
Determination of CO Emissions from Stationary Sources by NDIR
Spectrometry. U.S. Environmental Protection Agency. Research
Triangle Park, N.C. Publication No. EPA-650/4-74-005-h. February
1975. 96 p.

18.0 Tables, Diagrams, Flowcharts, and Validation Data

Same as Section 18.0 of PS 2.

Performance Specification 4A--Specifications and Test Procedures
for Carbon Monoxide Continuous Emission Monitoring Systems in
Stationary Sources

1.0 Scope and Application

1.1 Analytes.

------------------------------------------------------------------------
Analyte CAS No.
------------------------------------------------------------------------
Carbon Monoxide (CO)................................... 630-80-0
------------------------------------------------------------------------

1.2 Applicability.
1.2.1 This specification is for evaluating the acceptability of
carbon monoxide (CO) continuous emission monitoring systems (CEMS) at
the time of installation or soon after and whenever specified in an
applicable subpart of the regulations. This specification was developed
primarily for CEMS that comply with low emission standards (less than
200 ppmv).
1.2.2 This specification is not designed to evaluate the installed
CEMS performance over an extended period of time nor does it identify
specific calibration techniques and other auxiliary procedures to
assess CEMS performance. The source owner or operator is responsible to
calibrate, maintain, and operate the CEMS. The Administrator may
require, under Section 114 of the Act, the source owner or operator to
conduct CEMS performance evaluations at other times besides the initial
test to evaluate CEMS performance. See 40 CFR Part 60, Section
60.13(c).
1.2.3 The definitions, performance specification, test procedures,
calculations and data analysis procedures for determining calibration
drifts (CD) and relative accuracy (RA), of Performance Specification 2
(PS 2), Sections 3, 8.0, and 12, respectively, apply to this
specification.

2.0 Summary of Performance Specification

The CD and RA tests are conducted to determine conformance of the
CEMS to the specification.

3.0 Definitions

Same as in Section 3.0 of PS 2.

4.0 Interferences. [Reserved]

5.0 Safety

6.0 Equipment and Supplies

Same as Section 6.0 of PS 2 with the following additions.
6.1 Data Recorder Scale.
6.1.1 This specification is the same as Section 6.1 of PS 2. The
CEMS shall be capable of measuring emission levels under normal
conditions and under periods of short-duration peaks of high
concentrations. This dual-range capability may be met using two
separate analyzers (one for each range) or by using dual-range units
which have the capability of measuring both levels with a single unit.
In the latter case, when the reading goes above the full-scale
measurement value of the lower range, the higher-range operation shall
be started automatically. The CEMS recorder range must include zero and
a

[[Page 62138]]

high-level value. Under applications of consistent low emissions, a
single-range analyzer is allowed provided normal and spike emissions
can be quantified. In this case, set an appropriate high-level value to
include all emissions.
6.1.2 For the low-range scale of dual-range units, the high-level
value shall be between 1.5 times the pollutant concentration
corresponding to the emission standard level and the span value. For
the high-range scale, the high-level value shall be set at 2000 ppm, as
a minimum, and the range shall include the level of the span value.
There shall be no concentration gap between the low-and high-range
scales.

7.0 Reagents and Standards

Same as Section 7.0 of PS 2.

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Relative Accuracy Test Procedure. Sampling Strategy for
reference method (RM) Tests, Number of RM Tests, and Correlation of RM
and CEMS Data are the same as PS 2, Sections 8.4.3, 8.4.4, and 8.4.5,
respectively.
8.2 Reference Methods. Unless otherwise specified in an applicable
subpart of the regulation, Methods 10, 10A, 10B, or other approved
alternative is the RM for this PS. When evaluating nondispersive
infrared CEMS using Method 10 as the RM, the alternative interference
trap specified in Section 16.0 of Method 10 shall be used.
8.3 Response Time Test Procedure. The response time test applies
to all types of CEMS, but will generally have significance only for
extractive systems.
8.3.1 Introduce zero gas into the analyzer. When the system output
has stabilized (no change greater than 1 percent of full scale for 30
sec), introduce an upscale calibration gas and wait for a stable value.
Record the time (upscale response time) required to reach 95 percent of
the final stable value. Next, reintroduce the zero gas and wait for a
stable reading before recording the response time (downscale response
time). Repeat the entire procedure three times and determine the mean
upscale and downscale response times. The slower or longer of the two
means is the system response time.
8.4 Interference Check. The CEMS must be shown to be free from the
effects of any interferences.

9.0 Quality Control. [Reserved]

10.0 Calibration and Standardization. [Reserved]

11.0 Analytical Procedure

Sample collection and analysis are concurrent for this performance
specification (see Section 8.0). Refer to the RM for specific
analytical procedures.

12.0 Calculations and Data Analysis. Same as Section 12.0 of PS 2

13.0 Method Performance

13.1 Calibration Drift. The CEMS calibration must not drift or
deviate from the reference value of the calibration gas, gas cell, or
optical filter by more than 5 percent of the established span value for
6 out of 7 test days.
13.2 Relative Accuracy. The RA of the CEMS must be no greater than
10 percent when the average RM value is used to calculate RA, 5 percent
when the applicable emission standard is used to calculate RA, or
within 5 ppmv when the RA is calculated as the absolute average
difference between the RM and CEMS plus the 2.5 percent confidence
coefficient.
13.3 Response Time. The CEMS response time shall not exceed 1.5
min to achieve 95 percent of the final stable value.

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 Alternative Procedures

16.1 Under conditions where the average CO emissions are less than
10 percent of the standard and this is verified by Method 10, a
cylinder gas audit may be performed in place of the RA test to
determine compliance with these limits. In this case, the cylinder gas
shall contain CO in 12 percent carbon dioxide as an interference check.
If this option is exercised, Method 10 must be used to verify that
emission levels are less than 10 percent of the standard.

17.0 References

Same as Section 17 of PS 4.

18.0 Tables, Diagrams, Flowcharts, and Validation Data

Same as Section 18.0 of PS 2.

Performance Specification 5--Specifications and Test Procedures for
TRS Continuous Emission Monitoring Systems in Stationary Sources

1.0 Scope and Application

1.1 Analytes.

------------------------------------------------------------------------
Analyte CAS No.
------------------------------------------------------------------------
Total Reduced Sulfur (TRS)............................. NA
------------------------------------------------------------------------

1.2 Applicability. This specification is for evaluating the
applicability of TRS continuous emission monitoring systems (CEMS) at
the time of installation or soon after and whenever specified in an
applicable subpart of the regulations. The CEMS may include oxygen
monitors which are subject to Performance Specification 3 (PS 3).
1.3 The definitions, performance specification, test procedures,
calculations and data analysis procedures for determining calibration
drifts (CD) and relative accuracy (RA) of PS 2, Sections 3.0, 8.0, and
12.0, respectively, apply to this specification.

2.0 Summary of Performance Specification

The CD and RA tests are conducted to determine conformance of the
CEMS to the specification.

3.0 Definitions

Same as in Section 3.0 of PS 2.

4.0 Interferences [Reserved]

5.0 Safety

6.0 Equipment and Supplies

Same as Section 6.0 of PS 2.

7.0 Reagents and Standards

Same as Section 7.0 of PS 2.

8.0 Sample Collection, Preservation, Storage, and Transport

Note: For Method 16, a sample is made up of at least three
separate injects equally space over time. For Method 16A, a sample
is collected for at least 1 hour.

8.2 Reference Methods. Unless otherwise specified in the
applicable subpart of the regulations, Method 16,

[[Page 62139]]

Method 16A, 16B or other approved alternative is the RM for TRS.

9.0 Quality Control [Reserved]

10.0 Calibration and Standardization [Reserved]

11.0 Analytical Procedure

Sample collection and analysis are concurrent for this performance
specification (see Section 8.0). Refer to the reference method for
specific analytical procedures.

12.0 Calculations and Data Analysis

Same as Section 12.0 of PS 2.

13.0 Method Performance

13.1 Calibration Drift. The CEMS detector calibration must not
drift or deviate from the reference value of the calibration gas by
more than 5 percent of the established span value for 6 out of 7 test
days. This corresponds to 1.5 ppm drift for Subpart BB sources where
the span value is 30 ppm. If the CEMS includes pollutant and diluent
monitors, the CD must be determined separately for each in terms of
concentrations (see PS 3 for the diluent specifications).
13.2 Relative Accuracy. The RA of the CEMS must be no greater than
20 percent when the average RM value is used to calculate RA or 10
percent when the applicable emission standard is used to calculate RA.

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 Alternative Procedures [Reserved]

17.0 References

1. Department of Commerce. Experimental Statistics, National
Bureau of Standards, Handbook 91. 1963. Paragraphs 3-3.1.4, p. 3-31.
2. A Guide to the Design, Maintenance and Operation of TRS
Monitoring Systems. National Council for Air and Stream Improvement
Technical Bulletin No. 89. September 1977.
3. Observation of Field Performance of TRS Monitors on a Kraft
Recovery Furnace. National Council for Air and Stream Improvement
Technical Bulletin No. 91. January 1978.

18.0 Tables, Diagrams, Flowcharts, and Validation Data

Same as Section 18.0 of PS 2.

Performance Specification 6--Specifications and Test Procedures for
Continuous Emission Rate Monitoring Systems in Stationary Sources

1.0 Scope and Application

1.1 Applicability. This specification is used for evaluating the
acceptability of continuous emission rate monitoring systems (CERMSs).
1.2 The installation and measurement location specifications,
performance specification test procedure, calculations, and data
analysis procedures, of Performance Specifications (PS 2), Sections 8.0
and 12, respectively, apply to this specification.

2.0 Summary of Performance Specification

The calibration drift (CD) and relative accuracy (RA) tests are
conducted to determine conformance of the CERMS to the specification.

3.0 Definitions

The definitions are the same as in Section 3 of PS 2, except this
specification refers to the continuous emission rate monitoring system
rather than the continuous emission monitoring system. The following
definitions are added:
3.1 Continuous Emission Rate Monitoring System (CERMS). The total
equipment required for the determining and recording the pollutant mass
emission rate (in terms of mass per unit of time).
3.2 Flow Rate Sensor. That portion of the CERMS that senses the
volumetric flow rate and generates an output proportional to that flow
rate. The flow rate sensor shall have provisions to check the CD for
each flow rate parameter that it measures individually (e.g., velocity,
pressure).

4.0 Interferences [Reserved]

5.0 Safety

This performance specification may involve hazardous materials,
operations, and equipment. This performance specification may not
address all of the safety problems associated with its use. It is the
responsibility of the user to establish appropriate safety and health
practices and determine the applicable regulatory limitations prior to
performing this performance specification. The CERMS users manual
should be consulted for specific precautions to be taken with regard to
the analytical procedures.

6.0 Equipment and Supplies

Same as Section 6.0 of PS 2.

7.0 Reagents and Standards

Same as Section 7.0 of PS 2.

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Calibration Drift Test Procedure.
8.1.1 The CD measurements are to verify the ability of the CERMS
to conform to the established CERMS calibrations used for determining
the emission rate. Therefore, if periodic automatic or manual
adjustments are made to the CERMS zero and calibration settings,
conduct the CD tests immediately before these adjustments, or conduct
them in such a way that CD can be determined.
8.1.2 Conduct the CD tests for pollutant concentration at the two
values specified in Section 6.1.2 of PS 2. For other parameters that
are selectively measured by the CERMS (e.g., velocity, pressure, flow
rate), use two analogous values (e.g., Low: 0-20% of full scale, High:
50-100% of full scale). Introduce to the CERMS the reference signals
(these need not be certified). Record the CERMS response to each and
subtract this value from the respective reference value (see example
data sheet in Figure 6-1).
8.2 Relative Accuracy Test Procedure.
8.2.1 Sampling Strategy for reference method (RM) Tests,
Correlation of RM and CERMS Data, and Number of RM Tests are the same
as PS 2, Sections 8.4.3, 8.4.5, and 8.4.4, respectively. Summarize the
results on a data sheet. An example is shown in Figure 6-1. The RA test
may be conducted during the CD test period.
8.2.2 Reference Methods. Unless otherwise specified in the
applicable subpart of the regulations, the RM for the pollutant gas is
the Appendix A method that is cited for compliance test purposes, or
its approved alternatives. Methods 2, 2A, 2B, 2C, or 2D, as applicable,
are the RMs for the determination of volumetric flow rate.

9.0 Quality Control [Reserved]

10.0 Calibration and Standardization [Reserved]

11.0 Analytical Procedure

Same as Section 11.0 of PS 2.

12.0 Calculations and Data Analysis

Same as Section 12.0 of PS 2.

13.0 Method Performance

13.1 Calibration Drift. Since the CERMS includes analyzers for
several measurements, the CD shall be determined separately for each
analyzer in terms of its specific measurement. The calibration for each
analyzer associated with the measurement of flow rate shall not drift
or deviate from each reference value of flow rate by more than 3
percent of the respective high-level value. The CD specification for
each analyzer for which other PSs have been established (e.g., PS 2 for
SO2

[[Page 62140]]

and NOX), shall be the same as in the applicable PS.
13.2 CERMS Relative Accuracy. The RA of the CERMS shall be no
greater than 20 percent of the mean value of the RM's test data in
terms of the units of the emission standard, or 10 percent of the
applicable standard, whichever is greater.

14.0 Pollution Prevention [Reserved]

15.0 Waste Management [Reserved]

16.0 Alternative Procedures

Same as in Section 16.0 of PS 2.

17.0 References

1. Brooks, E.F., E.C. Beder, C.A. Flegal, D.J. Luciani, and R.
Williams. Continuous Measurement of Total Gas Flow Rate from
Stationary Sources. U.S. Environmental Protection Agency. Research
Triangle Park, North Carolina. Publication No. EPA-650/2-75-020.
February 1975. 248 p.

18.0 Tables, Diagrams, Flowcharts, and Validation Data

----------------------------------------------------------------------------------------------------------------
Emission rate (kg/hr)a
--------------------------------------------------------------------
Run No. Date and time Difference (RMs-
CERMS RMs CERMS)
----------------------------------------------------------------------------------------------------------------
1 .....................
----------------------------------------------------------------------------------------------------------------
2 .....................
----------------------------------------------------------------------------------------------------------------
3 .....................
----------------------------------------------------------------------------------------------------------------
4 .....................
----------------------------------------------------------------------------------------------------------------
5 .....................
----------------------------------------------------------------------------------------------------------------
6 .....................
----------------------------------------------------------------------------------------------------------------
7 .....................
----------------------------------------------------------------------------------------------------------------
8 .....................
----------------------------------------------------------------------------------------------------------------
9 .....................
----------------------------------------------------------------------------------------------------------------
\a\ The RMs and CERMS data as corrected to a consistent basis (i.e., moisture, temperature, and pressure
conditions).

Figure 6-1.--Emission Rate Determinations

Performance Specification 7--Specifications and Test Procedures for
Hydrogen Sulfide Continuous Emission Monitoring Systems in
Stationary Sources

1.0 Scope and Application

1.1 Analytes.

------------------------------------------------------------------------
Analyte CAS No.
------------------------------------------------------------------------
Hydrogen Sulfide........................................ 7783-06-4
------------------------------------------------------------------------

1.2 Applicability.
1.2.1 This specification is to be used for evaluating the
acceptability of hydrogen sulfide (H2S) continuous emission
monitoring systems (CEMS) at the time of or soon after installation and
whenever specified in an applicable subpart of the regulations.
1.2.2 This specification is not designed to evaluate the installed
CEMS performance over an extended period of time nor does it identify
specific calibration techniques and other auxiliary procedures to
assess CEMS performance. The source owner or operator, however, is
responsible to calibrate, maintain, and operate the CEMS. To evaluate
CEMS performance, the Administrator may require, under Section 114 of
the Act, the source owner or operator to conduct CEMS performance
evaluations at other times besides the initial test. See Section
60.13(c).

2.0 Summary

Calibration drift (CD) and relative accuracy (RA) tests are
conducted to determine that the CEMS conforms to the specification.

3.0 Definitions

Same as Section 3.0 of PS 2.

4.0 Interferences. [Reserved]

5.0 Safety

The procedures required under this performance specification may
involve hazardous materials, operations, and equipment. This
performance specification may not address all of the safety problems
associated with these procedures. It is the responsibility of the user
to establish appropriate safety problems associated with these
procedures. It is the responsibility of the user to establish
appropriate safety and health practices and determine the application
regulatory limitations prior to performing these procedures. The CEMS
user's manual and materials recommended by the reference method should
be consulted for specific precautions to be taken.

6.0 Equipment and Supplies

6.1 Instrument Zero and Span. This specification is the same as
Section 6.1 of PS 2.
6.2 Calibration Drift. The CEMS calibration must not drift or
deviate from the reference value of the calibration gas or reference
source by more than 5 percent of the established span value for 6 out
of 7 test days (e.g., the established span value is 300 ppm for Subpart
J fuel gas combustion devices).
6.3 Relative Accuracy. The RA of the CEMS must be no greater than
20 percent when the average reference method (RM) value is used to
calculate RA or 10 percent when the applicable emission standard is
used to calculate RA.

7.0 Reagents and Standards

Same as Section 7.0 of PS 2.

8.0 Sample Collection, Preservation, Storage, and Transport.

8.1 Installation and Measurement Location Specification. Same as
Section 8.1 of PS 2.
8.2 Pretest Preparation. Same as Section 8.2 of PS 2.
8.3 Calibration Drift Test Procedure. Same as Section 8.3 of PS 2.
8.4 Relative Accuracy Test Procedure.

[[Page 62141]]

8.4.1 Sampling Strategy for RM Tests, Correlation of RM and CEMS
Data, and Number of RM Tests. These are the same as that in PS 2,
Sections 8.4.3, 8.4.5, and 8.4.4, respectively.
8.4.2 Reference Methods. Unless otherwise specified in an
applicable subpart of the regulation, Method 11 is the RM for this PS.
8.5 Reporting. Same as Section 8.5 of PS 2.

9.0 Quality Control. [Reserved]

10.0 Calibration and Standardizations. [Reserved]

11.0 Analytical Procedures

Sample Collection and analysis are concurrent for this PS (see
Section 8.0). Refer to the RM for specific analytical procedures.

12.0 Data Analysis and Calculations

Same as Section 12.0 of PS 2.

13.0 Method Performance. [Reserved]

14.0 Pollution Prevention. [Reserved]

15.0 Waste Management. [Reserved]

16.0 References

1. U.S. Environmental Protection Agency. Standards of
Performance for New Stationary Sources; Appendix B; Performance
Specifications 2 and 3 for SO2, NOX,
CO2, and O2 Continuous Emission Monitoring
Systems; Final Rule. 48 CFR 23608. Washington, D.C. U.S. Government
Printing Office. May 25, 1983.
2. U.S. Government Printing Office. Gaseous Continuous Emission
Monitoring Systems--Performance Specification Guidelines for
SO2, NOX, CO2, O2, and
TRS. U.S. Environmental Protection Agency. Washington, D.C. EPA-450/
3-82-026. October 1982. 26 p.
3. Maines, G.D., W.C. Kelly (Scott Environmental Technology,
Inc.), and J.B. Homolya. Evaluation of Monitors for Measuring
H2S in Refinery Gas. Prepared for the U.S. Environmental
Protection Agency. Research Triangle Park, N.C. Contract No. 68-02-
2707. 1978. 60 p.
4. Ferguson, B.B., R.E. Lester (Harmon Engineering and Testing),
and W.J. Mitchell. Field Evaluation of Carbon Monoxide and Hydrogen
Sulfide Continuous Emission Monitors at an Oil Refinery. Prepared
for the U.S. Environmental Protection Agency. Research Triangle
Park, N.C. Publication No. EPA-600/4-82-054. August 1982. 100 p.

17.0 Tables, Diagrams, Flowcharts, and Validation Data

Same as Section 18.0 of PS 2.

Performance Specification 8 Performance Specifications for Volatile
Organic Compound Continuous Emission Monitoring Systems in
Stationary Sources

1.0 Scope and Application

1.1 Analytes. Volatile Organic Compounds (VOCs).
1.2 Applicability.
1.2.1 This specification is to be used for evaluating a continuous
emission monitoring system (CEMS) that measures a mixture of VOC's and
generates a single combined response value. The VOC detection principle
may be flame ionization (FI), photoionization (PI), non-dispersive
infrared absorption (NDIR), or any other detection principle that is
appropriate for the VOC species present in the emission gases and that
meets this performance specification. The performance specification
includes procedures to evaluate the acceptability of the CEMS at the
time of or soon after its installation and whenever specified in
emission regulations or permits. This specification is not designed to
evaluate the installed CEMS performance over an extended period of
time, nor does it identify specific calibration techniques and other
auxiliary procedures to assess the CEMS performance. The source owner
or operator, however, is responsible to calibrate, maintain, and
operate the CEMS properly. To evaluate the CEMS performance, the
Administrator may require, under Section 114 of the Act, the operator
to conduct CEMS performance evaluations in addition to the initial
test. See Section 60.13(c).
1.2.2 In most emission circumstances, most VOC monitors can
provide only a relative measure of the total mass or volume
concentration of a mixture of organic gases, rather than an accurate
quantification. This problem is removed when an emission standard is
based on a total VOC measurement as obtained with a particular
detection principle. In those situations where a true mass or volume
VOC concentration is needed, the problem can be mitigated by using the
VOC CEMS as a relative indicator of total VOC concentration if
statistical analysis indicates that a sufficient margin of compliance
exists for this approach to be acceptable. Otherwise, consideration can
be given to calibrating the CEMS with a mixture of the same VOC's in
the same proportions as they actually occur in the measured source. In
those circumstances where only one organic species is present in the
source, or where equal incremental amounts of each of the organic
species present generate equal CEMS responses, the latter choice can be
more easily achieved.

2.0 Summary of Performance Specification

2.1 Calibration drift and relative accuracy tests are conducted to
determine adherence of the CEMS with specifications given for those
items. The performance specifications include criteria for installation
and measurement location, equipment and performance, and procedures for
testing and data reduction.

3.0 Definitions.

Same as Section 3.0 of PS 2.

4.0 Interferences. [Reserved]

5.0 Safety

The procedures required under this performance specification may
involve hazardous materials, operations, and equipment. This
performance specification may not address all of the safety problems
associated with these procedures. It is the responsibility of the user
to establish appropriate safety problems associated with these
procedures. It is the responsibility of the user to establish
appropriate safety and health practices and determine the application
regulatory limitations prior to performing these procedures. The CEMS
user's manual and materials recommended by the reference method should
be consulted for specific precautions to be taken.

6.0 Equipment and Supplies

6.1 VOC CEMS Selection. When possible, select a VOC CEMS with the
detection principle of the reference method specified in the regulation
or permit (usually either FI, NDIR, or PI). Otherwise, use knowledge of
the source process chemistry, previous emission studies, or gas
chromatographic analysis of the source gas to select an appropriate VOC
CEMS. Exercise extreme caution in choosing and installing any CEMS in
an area with explosive hazard potential.
6.2 Data Recorder Scale. Same as Section 6.1 of PS 2.

7.0 Reagents and Standards. [Reserved]

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Installation and Measurement Location Specifications. Same as
Section 8.1 of PS 2.
8.2 Pretest Preparation. Same as Section 8.2 of PS 2.
8.3 Reference Method (RM). Use the method specified in the
applicable regulation or permit, or any approved alternative, as the
RM.
8.4 Sampling Strategy for RM Tests, Correlation of RM and CEMS
Data, and Number of RM Tests. Follow PS 2, Sections 8.4.3, 8.4.5, and
8.4.4, respectively.
8.5 Reporting. Same as Section 8.5 of PS 2.

[[Page 62142]]

9.0 Quality Control. [Reserved]

10.0 Calibration and Standardization. [Reserved]

11.0 Analytical Procedure

Sample collection and analysis are concurrent for this PS (see
Section 8.0). Refer to the RM for specific analytical procedures.

12.0 Calculations and Data Analysis

Same as Section 12.0 of PS 2.

13.0 Method Performance

13.1 Calibration Drift. The CEMS calibration must not drift by
more than 2.5 percent of the span value.
13.2 CEMS Relative Accuracy. Unless stated otherwise in the
regulation or permit, the RA of the CEMS must not be greater than 20
percent of the mean value of the RM test data in terms of the units of
the emission standard, or 10 percent of the applicable standard,
whichever is greater.

14.0 Pollution Prevention. [Reserved]

15.0 Waste Management. [Reserved]

16.0 References

Same as Section 17.0 of PS 2.

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

Performance Specification 9--Specifications and Test Procedures for
Gas Chromatographic Continuous Emission Monitoring Systems in
Stationary Sources

1.0 Scope and Application

1.1 Applicability. These requirements apply to continuous emission
monitoring systems (CEMSs) that use gas chromatography (GC) to measure
gaseous organic compound emissions. The requirements include procedures
intended to evaluate the acceptability of the CEMS at the time of its
installation and whenever specified in regulations or permits. Quality
assurance procedures for calibrating, maintaining, and operating the
CEMS properly at all times are also given in this procedure.

2.0 Summary of Performance Specification

2.1 Calibration precision, calibration error, and performance
audit tests are conducted to determine conformance of the CEMS with
these specifications. Daily calibration and maintenance requirements
are also specified.

3.0 Definitions

3.1 Gas Chromatograph (GC). That portion of the system that
separates and detects organic analytes and generates an output
proportional to the gas concentration. The GC must be temperature
controlled.

Note: The term temperature controlled refers to the ability to
maintain a certain temperature around the column. Temperature-
programmable GC is not required for this performance specification,
as long as all other requirements for precision, linearity and
accuracy listed in this performance specification are met. It should
be noted that temperature programming a GC will speed up peak
elution, thus allowing increased sampling frequency.

3.1.1 Column. Analytical column capable of separating the analytes
of interest.
3.1.2 Detector. A detection system capable of detecting and
quantifying all analytes of interest.
3.1.3 Integrator. That portion of the system that quantifies the
area under a particular sample peak generated by the GC.
3.1.4 Data Recorder. A strip chart recorder, computer, or digital
recorder capable of recording all readings within the instrument's
calibration range.
3.2 Calibration Precision. The error between triplicate injections
of each calibration standard.

4.0 Interferences [Reserved]

5.0 Safety

The procedures required under this performance specification may
involve hazardous materials, operations, and equipment. This
performance specification does not purport to address all of the safety
problems associated with these procedures. It is the responsibility of
the user to establish appropriate safety problems associated with these
procedures. It is the responsibility of the user to establish
appropriate safety and health practices and determine the application
regulatory limitations prior to performing these procedures. The CEMS
user's manual and materials recommended by the reference method should
be consulted for specific precautions to be taken.

6.0 Equipment and Supplies

6.1 Presurvey Sample Analysis and GC Selection. Determine the
pollutants to be monitored from the applicable regulation or permit and
determine the approximate concentration of each pollutant (this
information can be based on past compliance test results). Select an
appropriate GC configuration to measure the organic compounds. The GC
components should include a heated sample injection loop (or other
sample introduction systems), separatory column, temperature-controlled
oven, and detector. If the source chooses dual column and/or dual
detector configurations, each column/detector is considered a separate
instrument for the purpose of this performance specification and thus
the procedures in this performance specification shall be carried out
on each system. If this method is applied in highly explosive areas,
caution should be exercised in selecting the equipment and method of
installation.
6.2 Sampling System. The sampling system shall be heat traced and
maintained at a minimum of 120 deg.C with no cold spots. All system
components shall be heated, including the probe, calibration valve,
sample lines, sampling loop (or sample introduction system), GC oven,
and the detector block (when appropriate for the type of detector being
utilized, e.g., flame ionization detector).

7.0 Reagents and Standards

7.1 Calibration Gases. Obtain three concentrations of calibration
gases certified by the manufacturer to be accurate to within 2 percent
of the value on the label. A gas dilution system may be used to prepare
the calibration gases from a high concentration certified standard if
the gas dilution system meets the requirements specified in Test Method
205, 40 CFR Part 51, Appendix M. The performance test specified in Test
Method 205 shall be repeated quarterly, and the results of the Method
205 test shall be included in the report. The calibration gas
concentration of each target analyte shall be as follows (measured
concentration is based on the presurvey concentration determined in
Section 6.1).

Note: If the low level calibration gas concentration falls at or
below the limit of detection for the instrument for any target
pollutant, a calibration gas with a concentration at 4 to 5 times
the limit of detection for the instrument may be substituted for the
low-level calibration gas listed in Section 7.1.1.

7.1.1 Low-level. 40-60 percent of measured concentration.
7.1.2 Mid-level. 90-110 percent of measured concentration.
7.1.3 High-level. 140-160 percent of measured concentration, or
select highest expected concentration.
7.2 Performance Audit Gas. A certified EPA audit gas shall be
used, when possible. A gas mixture containing all the target compounds
within the calibration range and certified by EPA's Traceability
Protocol for Assay and Certification of Gaseous Calibration Standards
may be used when EPA performance audit materials

[[Continued on page 62143]]

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