DEPARTMENT OF ENVIRONMENT, GREAT LAKES, AND ENERGY

AIR QUALITY DIVISION

AIR POLLUTION CONTROL

(By authority conferred on the director of the department of environment, Great Lakes, and

energy by sections 5503 and 5512 of the natural resource and environmental protection act,

1994 PA 451, MCL 324.5503 and 324.5512, and Executive Reorganization Order Nos.

1995-16, 2009-31, 2011-1, 2019-1, MCL 324.99903, 324.99919, 324.99921, and

324.99923)

PART 10. INTERMITTENT TESTING AND SAMPLING

R 336.2001 Performance tests by owner.

Rule 1001. (1) The department may require the owner or operator of a source of air

contaminant to conduct acceptable performance tests, at the owner's or operator's expense,

in accordance with R 336.2003 under any of the following conditions:

(a) Reserved.

(b) The source is determined to be in violation of R 336.1301 and the potential emissions

exceed 100 tons per year.

(c) The owner or operator of the source has not submitted an acceptable performance test,

in accordance with R 336.2003, that demonstrates the source complies with either the

department's rules or the conditions specified in the permit to install, or both.

(d) The source of air contaminant is located in an area designated as nonattainment for 1

or more air pollutants, and more than 12 months have expired since the date of the last

performance test for such designated nonattainment pollutants.

(e) The source of air contaminant has potential emissions in excess of 100 tons per year,

is located in an area designated as attainment for 1 or more air pollutants, and more than

36 months have expired since the date of the last performance test for the designated

attainment pollutants.

(f) After completion of a compliance program.

(2) Performance tests required by subrule (1) of this rule must be conducted within 60

days following receipt of written notification from the department, unless otherwise

authorized by the department.

(3) Not less than 30 days before a performance test, as required by subrule (1) of this rule,

the owner or operator, or an authorized agent, shall do both of the following:

(a) Submit a site-specific test plan for approval by the department. The plan must include

a test program summary, test schedule, and the quality assurance measures to be applied.

(b) Notify the department, in writing, of the time and place of the performance tests and

who shall conduct them as provided in the site-specific test plan required under subdivision

(a) of this subrule. A representative of the department shall have the opportunity to witness

these tests.

Page 1

(4) Results of performance tests must be submitted to the department in the format

prescribed by the applicable reference test method within 60 days after the last date of the

test.

History: 1980 AACS; 2002 AACS; 2009 AACS; 2025 AACS.

R 336.2002 Performance tests by department.

Rule 1002. (1) The department may conduct performance tests in accordance with R

336.2003 at any source of air contaminant, on behalf of the state, at a reasonable time and

at the state's expense. During the conduct of such tests, the department may obtain samples

of any air contaminant and samples of any material entering or exiting the source or

aircleaning device for the purpose of evaluating pollutant emissions with respect to process

operating conditions.

(2) The department shall provide written notification to the owner or operator of a source

of the department's intent to conduct performance tests pursuant to subrule (1). Within 30

days of receipt of such notification, the owner or operator shall provide, and bear the

expense of, performance test facilities as specified by the department, including the

following:

(a) Sampling ports adequate for reference test methods applicable to the source.

(b) Safe sampling platforms as required.

(c) Safe access to sampling platforms.

(d) A suitable power source within 50 feet of any sampling location designated by the

department. Upon request, additional time for installing the required performance test

facilities may be authorized by the department for special situations.

(3) The owner shall not be responsible for providing sampling instruments and sensing

devices.

(4) Results of performance tests shall be furnished to the owner or operator, or both, in

the format prescribed by the applicable reference test method within 60 days following the

last date of the test.

History: 1980 AACS; 2002 AACS.

R 336.2003 Performance test criteria.

Rule 1003. (1) Performance tests must be conducted and data reduced according to the

reference test methods listed in R 336.2004, unless the department does any of the

following:

(a) Specifies or approves, in specific cases, the use of a reference test method with minor

changes in procedures or equipment.

(b) Approves the use of an equivalent method.

(c) Specifies or approves the use of an alternative method if an applicable reference test

method does not exist for a specific air contaminant or source of air contaminant.

(2) Unless otherwise approved by the department, a performance test must consist of a

minimum of 3 separate samples of a specific air contaminant conducted within a 36-hour

period that starts once the probe enters the stack. Any data measured within the 36-hour

period must be recorded and provided to the department. Each of the 3 separate samples

Page 2

must be obtained while the source is operating at a similar production level, as described

under subrule (3) of this rule. For the purpose of determining compliance with an applicable

emission limit, rule, or permit condition, the arithmetic mean of results of the 3 samples

must apply. If a sample is accidentally lost or conditions occur in which 1 of the 3 samples

must be discontinued because of forced shutdown, failure of an irreplaceable portion of the

sampling train, extreme meteorological conditions, or other circumstances beyond the

owner's or operator's control, then compliance may, upon the approval of the department,

be determined using the arithmetic mean of the results of 2 samples.

(3) All performance tests must be conducted while the source of air contaminant is

operating at maximum routine operating conditions, or under other conditions, within the

capacity of the equipment, as may be requested by the department. Other conditions may

include source operating periods of startup, shutdown, or other operations, excluding

malfunction, specific to certain sources. Routine operating conditions must also include

those specified within a permit to install or a permit to operate. The owner or operator shall

make available to the department the records that may be necessary to determine the

conditions of source operation that occurred during the period of time of the performance

test.

(4) For sources that are subject to an emission limitation calculated to 50% excess air, the

multipoint, integrated sampling at every traverse point must be used with method 3, 3A, or

3Bfor gas analysis. For all other sources that require a determination of the molecular

weight of the exhaust, an optional sampling procedure of method 3, 3A, or 3B may be used.

Alternatives or modifications to procedures are subject to the approval of the department.

(5) For reference test method 5B, which is described in R 336.2011, reference test method

5C, which is described in R 336.2012, and reference test method 5E, which is described in

R 336.1014, the minimum volume per sample must be 30 cubic feet of dry gas corrected

to standard conditions, 68 degrees Fahrenheit, 29.92 inches mercury. Minimum sample

time must be 60 minutes, which may be continuous or a combination of shorter sampling

periods for sources that operate in a cyclic manner. Smaller sampling times or sample

volumes, when necessitated by process variables or other factors, may be approved by the

department.

History: 1980 AACS; 2002 AACS; 2025 AACS.

R 336.2004 Reference test methods; adoption of federal reference test methods.

Rule 1004. (1) The federal test methods described in the provisions of 40 CFR part 60,

appendix A, adopted by reference in R 336.1902, are test methods for performance tests

required pursuant to the provisions of this part and include, but are not limited to, the

following:

(a) Method 1 - Sample and velocity traverse for stationary sources.

(b) Method 1A - Sample and velocity traverses for stationary sources with small stacks

or ducts.

(c) Method 2 - Determination of stack gas velocity and volumetric flow rate (type-S pitot

tube).

(d) Method 2A - Direct measurement of gas volume through pipes and small ducts.

(e) Method 2C - Determination of stack gas velocity and volumetric flow rate in small

stacks and ducts (standard pitot tube).

Page 3

(f) Method 2D - Measurement of gas volumetric flow rates in small pipes and ducts.

(g) Method 3 - Gas analysis for the determination of dry molecular weight.

(h) Method 4 - Determination of moisture content in stack gases.

(i) Method 5 - Determination of particulate matter emissions from stationary sources.

(j) Method 6 - Determination of sulfur dioxide emissions from stationary sources.

(k) Method 7 - Determination of nitrogen oxide emissions from stationary sources.

(l) Method 8 - Determination of sulfuric acid mist and sulfur dioxide emissions from

stationary sources.

(m) Method 9 - Visual determination of the opacity of emissions from stationary sources.

(n) Method 10 - Determination of carbon monoxide emissions from stationary sources.

(o) Method 10B - Determination of carbon monoxide emissions from stationary sources.

(p) Method 18 - Measurement of gaseous organic compound emissions by gas

chromatography.

(q) Method 21 - Determination of volatile organic compound leaks.

(r) Method 24 - Determination of volatile matter content, water content, density, volume

solids, and weight solids of surface coatings.

(s) Method 24A - Determination of volatile matter content and density of printing inks

and related coatings.

(t) Method 25 - Determination of total gaseous nonmethane organic emissions as carbon.

(u) Method 25A - Determination of total gaseous organic concentration using a flame

ionization analyzer.

(v) Method 27 - Determination of vapor tightness of gasoline delivery tank using

pressure-vacuum test.

(w) Method 29 - Determination of metals emissions from stationary sources.

(x) Method 30A - Determination of total vapor phase mercury emissions from stationary

sources (instrumental analyzer procedure).

(y) Method 30B - Determination of total vapor phase mercury emissions from coal-fired

combustion sources using carbon sorbent traps.

(2) The federal test methods in the following provisions, adopted by reference in

R 336.1902, are test methods for performance tests required pursuant to the provisions of

this part:

(a) 40 CFR part 51, appendix M.

(b) 40 CFR part 61, appendix B.

(c) 40 CFR part 63, appendix A.

(3) All alternatives that are subject to the approval of the administrator in the adopted

federal reference methods are subject to the approval of the department.

(4) Determinations of compliance with visible emission standards for stationary sources

must be conducted as specified in 40 CFR part 60, appendix A, test method 9 or another

alternative method approved by the department, with the following exceptions:

(a) Visible emissions from a scarfing operation at a steel manufacturing facility must be

determined as specified in reference test method 9A, which is described in R 336.2030.

(b) Visible emissions from a coke oven pushing operation and fugitive coke oven visible

emissions must be determined as specified in reference test method 9B, which is described

in R 336.2031.

Page 4

(c) Visible emissions, fugitive and nonfugitive, from basic oxygen furnace operations,

hot metal transfer operations, and hot metal desulfurization operations must be determined

as specified in reference method 9C, which is described in R 336.2032.

(5) Determinations of particulate emission rates for stationary sources must be conducted

as specified in 1 or more of the following reference test methods:

(a) Reference test method 5B, which is described in R 336.2011.

(b) Reference test method 5C, which is described in R 336.2012.

(c) Reference test method 5D, which is described in R 336.2013.

(d) Reference test method 5E, which is described in R 336.2014.

(e) "Standard Methods for the Examination of Water and Wastewater," (23rd edition), as

described and modified in R 336.2033.

(6) Determinations of total gaseous nonmethane organic emissions as carbon, using the

alternate version of federal test method 25 under 40 CFR part 60, appendix A,

incorporating the Byron analysis, must be conducted as specified in R 336.2006.

History: 1980 AACS; 1985 AACS; 1989 AACS; 1993 AACS; 1998-2000 AACS; 2002 AACS; 2006

AACS; 2009 AACS; 2025 AACS.

Editor's Note: An obvious error in R 336.2004 was corrected at the request of the promulgating agency,

pursuant to Section 56 of 1969 PA 306, as amended by 2000 PA 262, MCL 24.256. The rule containing the

error was published in Annual Administrative Code Supplement 2025. The memorandum requesting the

correction was published in Michigan Register, 2026 MR 16.

R 336.2005 Reference test methods for state-requested tests of delivery vessels.

Rule 1005. The following reference test method shall be used to detect gasoline vapor

leaks by a combustible gas detector:

(a) Principle. A combustible gas detector is used to indicate any incidence of leakage from

gasoline delivery vessel tanks and vapor control systems. This qualitative monitoring

procedure is an enforcement tool to confirm the continuing existence of leak-tight

conditions.

(b) Applicability. This method is applicable to determining leak-tightness of gasoline

delivery vessel tanks during loading without taking the delivery vessel tank out of service.

The method is applicable only if the vapor control system does not create back pressure in

excess of the pressure limits of the delivery vessel tank compliance leak test. For vapor

control systems, this method is applicable to determining leak-tightness at any time.

(c) Apparatus and specifications. The following apparatus shall be used:

(i) Manometer. Liquid manometer, or equivalent, capable of measuring up to 0.9 pounds

per square inch (24.9 inches of water) gauge pressure within 0.003 pounds per square inch

(0.1 inches of water) precision.

(ii) Combustible gas detector. A portable hydrocarbon gas analyzer with associated

sampling line and probe which complies with all of the following provisions:

(A) Safety. The device is certified as safe for operation in explosive atmospheres.

(B) Range. The device shall have a minimum range of 0 to 100% of the lower explosive

limit (LEL) as propane.

(C) Probe diameter. The sampling probe shall have an internal diameter of 0.625

centimeters (1/4 inch).

Page 5

(D) Probe length. The probe sampling line shall be of sufficient length for easy

maneuverability during testing.

(E) Response time. The response time for full-scale deflection shall be less than 8 seconds

for a detector with a sampling line and probe attached.

(d) Test procedure. The following test procedure shall be complied with:

(i) Pressure. Place a pressure tap in the terminal, plant, or service station vapor control

system as close as possible to the connection with the delivery vessel tank. Record the

pressure periodically during testing.

(ii) Calibration. Calibrate the combustible gas detector with 2.2% propane, by volume, in

air for 100% lower explosive limit response.

(iii) Monitoring procedure. During loading or unloading, check the periphery of all

potential sources of leakage of the delivery vessel tank and of the terminal, plant, or service

station vapor collection system with a combustible gas detector. The check shall comply

with the following procedure:

(A) Probe distance. The probe inlet shall be 2.5 centimeters from the potential leak source.

(B) Probe movement. Move the probe slowly (2.0 centimeters per second).If there is any

meter deflection at a potential leak source, move the probe to locate the point of highest

meter response.

(C) Probe position. As much as possible, the probe inlet shall be positioned in the path of

(parallel to) the vapor flow from a leak.

(D) Wind. Attempt, as much as possible, to block the wind from the area being monitored.

(iv) Recording. Record the highest detector reading and location for each incidence of

leakage.

History: 1981 AACS; 1989 AACS; 2002 AACS; 2006 AACS.

Editor's Note: An obvious error in R 336.2005 was corrected at the request of the promulgating agency,

pursuant to Section 56 of 1969 PA 306, as amended by 2000 PA 262, MCL 24.256. The rule containing the

error was published in Annual Administrative Code Supplement 2006. The memorandum requesting the

correction was published in Michigan Register, 2026 MR 16.

R 336.2006 Reference test method serving as alternate version of federal reference

test method 25 by incorporating Byron analysis.

Rule 1006. When using the alternate version of federal reference test method 25

incorporating the Byron analysis, the procedures in method 25, which are described in R

336.2004, shall be followed, except that all of the following parts in method 25 are

amended to read as follows:

1.2 Principle. An emission sample is withdrawn from a stack at a constant rate through a

stainless steel absorber tube packed with porasil; the gaseous portion of the sample is pulled

past a battery-operated sampling pump into a tedlar bag. After sampling is complete, the

contents of the tedlar bag are analyzed on an automated gas chromatograph (GC), and the

sample in the porasil packed tube is heated to remove all components for analysis on the

GC. The GC separates CO, CO2, and CH4 from the nonmethane organics (NMO), then

converts the NMOs to methane for analysis.

2. Apparatus. The sampling system consists of a nonmethane organic (NMO) absorber

tube, a sampling pump, and a sample bag (figure 25-1). The analytical system has 2 parts

Page 6

the oven for removing the sample from the absorber tube and an automated gas

chromatograph (GC).

2.1 Sampling. All of the following equipment is required, as shown in figure 25-1:

2.1.1 Heated probe. 6.4-millimeter (mm) (1/4-inch (in.)) outside diameter (o.d.) stainless

steel tubing with a heating system that is capable of maintaining a gas temperature at the

exit end of not less than 129 degrees Centigrade (265 degrees Fahrenheit). The probe shall

be equipped with a thermocouple at the exit end to monitor the gas temperature. The nozzle

is an elbow fitting that is attached to the front end of the probe while the thermocouple is

inserted in the side arm of a tee fitting that is attached to the rear of the probe. The probe

is wrapped with a suitable length of high-temperature heating tape and then covered with

2 layers of glass cloth insulation and 1 layer of aluminum foil.

2.1.2 Heated prefilter-only for stacks with possible particulate matter interference. A

stainless steel filter holder with a 47-mm type A/E fiberglass filter without organic binder.

The entire prefilter shall be maintained at 110 degrees Celsius. Note - if it is not possible

to use a heating system for safety reasons, an unheated system with an instack filter is a

suitable alternative.

2.1.3 NMO absorber tube. 1/2-inch inside diameter (i.d.) stainless steel tube packed with

porasil (thermally stable silica gel).

2.1.4 1/4-inch o.d. teflon line that is 2 to 4 feet long.

2.1.5 Battery-operated diaphragm sampling pump with kurz digital mass flow meter.

Total flow is integrated electronically to measure flow with an accuracy of 1% at any flow

rate. (Byron instruments model 90).

2.1.6 Sample bag. 0.3-mil tedlar, 1/2-cubic foot capacity. The sample bag undergoes

nitrogen purge cycle until analysis exhibits zero carbon content in the sample bag.

2.2 Analysis. The following equipment is required:

2.2.1 Sample recovery on the adsorber tube is done in a Byron model 75 oven in 2 stages,

each stage requiring a 0.3-mil tedlar bag that has a 1/2-cubic foot capacity.

2.2.2 Analysis is done on a Byron model 401 gas chromatograph (GC) that meets all

criteria specified in method 25, section 2.2.2.

2.3 NMO analyzer. The NMO analyzer is a Byron model 401 gas chromatograph (GC).

(Remainder of 2.3 as stated in method 25)

2.3.5.2 Range. A full scale range of 1 to 10,000 parts per million (ppm) CH4. Signal

attenuators shall be available to produce a minimum signal response of 10% of full scale.

3.1.1 Delete (dry ice is not required).

4.1.1 Model 90 and model 75 flow meter calibration. The model 90 sample pump inlet is

attached to the outlet of the model 75 oven. Air is passed through the system at the rate that

will be used in sampling and for the total volume anticipated to be sampled. If the flow

meters on the 2 instruments do not agree within 0.01 liters, then adjust the meter on the

model 90 until agreement is within 0.01 liters. After making any correction, run a full

calibration again.

4.1.2 Sample train assembly. Assemble the probe (prefilter if needed), adsorber tube, and

teflon line to the inlet of the model 90. Attach a short (8 to 10 inches) flexible line to the

outlet of model 90. Have a completely clean evacuated tedlar sample bag nearby for

collection of sample to be analyzed.

4.1.3 Pretest leak check. Stopper the inlet of the probe and place the flexible tube on the

outlet of the model 90 in a small open container of water. Turn on the sampling pump. For

Page 7

a satisfactory leak check, bubbling should cease within 1 minute. If the leak check is

unsatisfactory, tighten the fittings or change parts until a satisfactory leak check is obtained.

4.1.4 Sampling train operation. Place the probe and the front portion of the adsorption tube

in the stack. If the stack has a temperature higher than ambient, allow time for the probe to

heat before starting the sample pump. Start the model 90 pump and adjust to the desired

flow, usually about 90 ml/min. After about 0.1 liter of sampling, or equivalent to the

volume of air that is displaced in the sample system before the flowmeter, remove the

flexible tube from the outlet of the model 90 and install the evacuated tedlar bag. This

assures that gaseous components are undiluted by the air originally in the sampling system.

Record requested data on the data form during the sample time. The sampling is usually

done for 1 hour with a total of 5 to 6 liters sampled. When sampling is complete, record

the precise volume sampled. The process may require different sample times or sample

volumes. (Sampling form is figure 25-8.)

4.1.5 Post test leak check. Remove the tedlar bag and replace it with the flexible tube.

Stopper the probe and operate the same as the pretest leak check specified in section 4.1.3.

If the leak test is not acceptable, invalidate the sample.

4.2 Sample recovery. The tedlar bag is ready for direct analysis on the GC. The adsorber

tube shall undergo the following 2-stage preparation:

4.2.1 Sample purge. The absorber tube is placed in the Byron model 75 oven with a clean

tedlar bag attached directly to the tube. A volume of clean dry air is passed through the

adsorber tube while holding the oven temperature at about 130 degrees Celsius. The

volume of air should be precisely the same as that sampled. This purge is necessary to

remove any CO2 on the sample tube, and the elevated temperature is needed to assure CO2

removal from any absorbed water. The tedlar bag is now ready for direct analysis on the

GC.

4.2.2 Sample digest. The absorber tube, now free of CO2 and the lighter NMOs, is now

attached to an oxidation catalyst, and another tedlar bag is attached to the outlet of the

oxidation catalyst. A volume of clean dry air equal to that sampled is passed through this

system while the temperature on the sample tube is brought up to 600 degrees Celsius. If

the sampled volume was less than 3 liters, a larger volume shall be used in the digestion to

assure completion. Usually a multiple of precisely 1.5 or 2.0 of the sampled volume is

sufficient. This third tedlar bag is now ready for direct analysis on the GC. If anything other

than CO2 is found in this bag, the model 75 oxidation catalyst is probably in need of

replacement. In this case the test would be invalid and would have to be redone.

4.3 Analysis. Each of the 3 bags is analyzed on the GC. Each bag should be analyzed as

soon as possible after being filled. At the completion of analysis, the bags shall be cleaned

by repeated fillings with either clean air or nitrogen. Before being used again, the bags shall

be checked by filling with clean air and then analyzed on the GC to assure zero

concentrations of all analyzed substances. All pertinent calibration, performance, and

operational checks in sections 4.4 and 5 of method 25 apply to the Byron system.

6. Calculations.

6.1 Nomenclature.

C1 = Concentration of sample bag, ppm C, (NMO converted to methane).

C2 = Concentration of purge bag, ppm C, (NMO converted to methane).

C3 = Concentration of digest bag, ppm C, (CO2 converted to methane).

C = Ppm C (NMO).

Page 8

6.2-6.4 (Delete).

6.5 C1, C2, C3 calculated directly as: ppm C calibration gas x GC reading unknown =

ppm C GC reading calibration gas unknown 6.6 C = C1 + C2 + C3 Delete figures 25.3,

25.4, 25.9, and 25.10 from method 25. Amend figures 25.1 and 25.8 from method 25 to

read as follows:

FIGURE 25.1

SAMPLING TRAIN

FIGURE 25.1

Page 9

History: 1993 AACS.

R 336.2007 Alternate version of procedure L, referenced in R 336.2040(10).

Rule 1007. The alternate version of procedure L is as follows:

1. Introduction.

1.1 Applicability. This procedure is applicable for determining the input of volatile

organic compounds (voc), measured as equivalent propane as measured by a flame

ionization instrument. It is intended to be used as a segment in the development of

liquid/gas protocols for determining voc capture efficiency (ce) for surface coating and

printing operations.

1.2 Principle. The amount of voc introduced to the process (l) is the sum of products of

the weight (w) of each voc containing liquid (ink, paint, solvent, or similar material) used

and its voc content (v), corrected for a response factor (rf) to allow the input to be calculated

in terms of propane, the same calibration gas used in the gaseous voc measurements. A

sample of each coating used is distilled to separate the voc fraction. The distillate is used

to prepare a known standard for analysis by a flame ionization analyzer (fia), calibrated

against propane, to determine its rf.

2. Apparatus and reagents.

2.1 Liquid weight.

2.1.1 Balances/digital scales. To weigh drums of voc containing liquids to within 0.2 lb.

Page 10

2.1.2 Volume measurement apparatus (alternative). Volume meters, flow meters, density

measurement equipment, or similar material, as needed to achieve the same accuracy as

direct weight measurements.

2.2 Response factor (rf) determination (fia technique). The voc distillation and tedlar gas

bag generation systems apparatus are shown in figures 1 and 2. The following equipment

is required:

2.2.1 Sample collection can. An appropriately sized metal can to collect voc-containing

materials. The can shall be constructed in such a way that it can be grounded to the coating

container.

2.2.2 Needle valves. To control gas flow.

2.2.3 Regulators. For fia, calibration, dilution, and sweep gas cylinders.

2.2.4 Tubing and fittings. Teflon and stainless steel tubing and fittings with diameters and

lengths and sizes determined by connection requirements of the equipment.

2.2.5 Thermometer. Capable of measuring the temperature of the hot water and oil baths

to within 1 degree Celsius.

2.2.6 Analytical balance. To measure plus or minus 0.01 mg.

2.2.7 Microliter syringe. 10-microliter size.

2.2.8 Vacuum and pressure manometers. 0 to 760 mm (0 to 30 in.) hg.U-tube manometer,

vacuum or pressure.

2.2.9 Hot oil bath, with stirring hot plate. Capable of heating and maintaining a distillation

vessel at 110 plus or minus 3 degrees Celsius.

2.2.10 Vacuum/water aspirator. A device capable of drawing a vacuum to within 20 mm

hg from absolute.

2.2.11 Rotary evaporator system. Complete with folded inner coil, vertical style

condenser, rotary speed control, and teflon sweep gas delivery tube with valved inlet. Buchi

rotavapor or equivalent.

2.2.12 Ethylene glycol cooling/circulating bath. Capable of maintaining the condenser

coil fluid at minus 10 degrees Celsius.

2.2.13 Dry gas meter. For the precise measurement of dilution gas volume. It shall be

calibrated to a primary standard, either spirometer or bubble meter.

2.2.14 Activated charcoal/mole sieve trap. To remove any trace level of organics picked

up from the dry gas meter.

2.2.15 Gas coil heater. Sufficient length of 0.125-inch stainless steel tubing to allow

heating of the dilution gas to near the water bath temperature before entering the

volatilization vessel.

2.2.16 Water bath, with stirring hot plate. Capable of heating and maintaining a

volatilization vessel and coil heater at a temperature of 100 plus or minus 5 degrees Celsius.

2.2.17 Volatilization vessel. 50-milliliter midget impinger fitted with a septum top and

loosely filled with glass wool to increase volatilization surface.

2.2.18 Tedlar gas bag. Capable of holding 30 liters of gas, flushed clean with zero air,

leak tested and evacuated.

2.2.19 Cylinder of compressed zero air. Used to supply dilution air for making the tedlar

bag gas samples.

2.2.20 Cylinder of compressed thc free N2. Used as sweep gas in the rotary evaporator

system.

Page 11

2.2.21 Organic concentration analyzer. An fia with a span value of 1.5 times the expected

concentration as propane; however, other span values may be used if it can be demonstrated

that they would provide more accurate measurements. The fia instrument shall be the same

instrument used in the gaseous analyses adjusted with the same fuel, combustion air, and

sample backpressure (flowrate) settings. The system shall be capable of meeting or

exceeding the following specifications:

2.2.21.1 Zero drift. Less than plus or minus 3.0% of the span value.

2.2.21.2 Calibration drift. Less than plus or minus 3.0% of span value.

2.2.21.3 Calibration error. Less than plus or minus 5.0% of the calibration gas value.

2.2.22 Integrator/data acquisition system. An analog or digital device or computerized

data acquisition system used to integrate the fia response or compute the average response

and record measurement data. The minimum data sampling frequency for computing

average or integrated values is 1 measurement value every 5 seconds. The device shall be

capable of recording average values at least once per minute.

2.2.23 Chart recorder (optional). A chart recorder or similar device is recommended to

provide a continuous analog display of the measurement results during the liquid sample

analysis.

2.2.24 Calibration and other gases. For calibration, fuel, and combustion air, if required,

contained in compressed gas cylinders. All calibration gases shall be traceable to NIST

standards and shall be certified by the manufacturer to plus or minus 1% of the tag

value.Additionally, the manufacturer of the cylinder should provide a recommended shelf

life for each calibration gas cylinder over which the concentration does not change more

than plus or minus 2% from the certified value. For calibration gas values that are not

generally available, alternative methods for preparing calibration gas mixtures, such as

dilution systems, may be used with prior approval.

2.2.24.1 Fuel. 99.995% hydrogen, 40% hydrogen/60% helium, or 40% hydrogen/60%

nitrogen. The fia manufacturer's recommended fuel shall be used. An attempt shall be made

to avoid fuels with oxygen to avoid an oxygen synergism effect that reportedly occurs when

oxygen concentration varies significantly from a mean value.

2.2.24.2 Carrier gas. High purity air with less than 1 ppm of organic material (as propane)

or less than 0.1% of the span value, whichever is greater.

2.2.24.3 Fia linearity calibration gases. Low-, mid-, and high-range gas mixture standards

with a nominal propane concentration of 20 to 30, 45 to 55, and 70 to 80% of the span

value in air, respectively. Other calibration values and other span values may be used if it

can be shown that more accurate measurements would be achieved.

2.2.24.4 System calibration gas. Gas mixture standard which contains propane in air and

which approximates the voc concentration expected for the tedlar gas bag samples.

3. Determination of liquid input weight. A capture efficiency test shall consist of not less

than 3 sampling runs. Each run shall cover at least 1 complete production or processing

cycle or shall be at least 1 hour in duration. For automotive surface coating operations, the

sampling time per run shall be based on coating a minimum of 3 representative vehicles.

3.1 Weight difference. Determine the amount of material introduced to the process as the

weight difference of the feed material before and after each sampling run. In determining

the total voc-containing liquid usage, account for all of the following:

(a) The initial (beginning) voc-containing liquid mixture.

(b) Any solvent added during the test run.

Page 12

(c) Any coating added during the test run.

(d) Any residual voc-containing liquid mixture remaining at the end of the sample run.

3.1.1 Identify all points where voc-containing liquids are introduced to the process. To

obtain an accurate measurement of voc-containing liquids, start with an empty fountain, if

applicable. After completing the run, drain the liquid in the fountain back into the liquid

drum, if possible, and weigh the drum again. Weigh the voc-containing liquids to plus or

minus 0.5% of the total weight (full) or plus or minus 0.1% of the total weight of voc-

containing liquid used during the sample run, whichever is less. If the residual liquid cannot

be returned to the drum, drain the fountain into a preweighed empty drum to determine the

final weight of the liquid.

3.1.2 If it is not possible to measure a single representative mixture, then weigh the various

components separately, for example, if solvent is added during the sampling run, weigh the

solvent before it is added to the mixture. If a fresh drum of voc-containing liquid is needed

during the run, then weigh both the empty drum and the fresh drum.

3.2 Volume measurement (alternative). If direct weight measurements are not feasible,

the tester may use volume meters, flow rate meters, and density measurements to determine

the weight of liquids that are used if it can be demonstrated that the technique produces

results equivalent to the direct weight measurements. If a single representative mixture

cannot be measured, measure the components separately.

4. Determination of voc content in input liquids.

4.1 Collection of liquid samples.

4.1.1 Collect a 1-pint or larger sample of the voc-containing liquid mixture at each

application location at the beginning and end of each test run. A separate sample shall be

taken of each voc-containing liquid that is added to the application mixture during the test

run. If a fresh drum is needed during the sampling run, then obtain a sample from the fresh

drum.

4.1.2 When collecting the sample, ground the sample container to the coating drum. Fill

the sample container as close to the rim as possible to minimize the amount of headspace.

4.1.3 After the sample is collected, seal the container so the sample cannot leak out or

evaporate.

4.1.4 Label the container to identify clearly the contents.

4.2 Distillation of voc.

4.2.1 Assemble the rotary evaporator as shown in figure 1.

4.2.2 Leak check the rotary evaporation system by aspirating a vacuum of approximately

20 mm hg from absolute. Close up the system and monitor the vacuum for approximately

1 minute. If the vacuum falls more than 125 mm hg in 1 minute, repair leaks and repeat.

4.2.3 Deposit approximately 20 mls of the sample (inks, paints, or similar material) into

the rotary evaporation distillation vessel.

4.2.4 Turn off the aspirator and gradually apply a vacuum to the evaporator of within 20

mm hg.

4.2.5 Begin heating the vessel at a rate of 2 to 3 degrees Centigrade per minute,

maintaining the vacuum specified in 4.2.3. Care shall be taken to prevent material bumping

from the distillation flask.

4.2.6 Continue heating until a temperature of 110 degrees Centigrade is achieved and

maintain this temperature for not less than 10 minutes or until the sample has dried in the

distillation flask.

Page 13

4.2.7 Slowly introduce the N2 sweep gas through the purge tube and into the distillation

flask, taking care to maintain not less than 125 mm hg vacuum at all times.

4.2.8 Continue sweeping the remaining solvent voc from the distillation flask and

condenser assembly for 10 minutes or until all traces of condensed solvent are gone from

the vessel and the still head.

4.2.9 Disassemble the apparatus and transfer the distillate to a labeled sealed vial.

4.3 Preparation of voc standard bag sample.

4.3.1 Assemble the bag sample generation system as shown in figure 2 and bring the water

bath up to a near-boiling temperature.

4.3.2 Inflate the tedlar bag and perform a leak check on the bag.

4.3.3 Evacuate the bag and close the bag inlet valve.

4.3.4 Record the current barometric pressure.

4.3.5 Record the starting reading on the dry gas meter, open the bag inlet valve, and start

the dilution zero air flowing into the tedlar bag at approximately 2 liters per minute.

4.3.6 The bag sample voc concentration shall be similar to the gaseous voc concentration

measured in the exhaust gas ducts. The amount of liquid voc required can be approximated

using the equations in section 6, the gaseous voc measurement results in terms of propane,

and an assumed response factor of 1.0. Let Cc3 equal the exhaust gas concentration in

terms of propane and rf=1.0. Calculate Cvoc. Let bv = 20 liters and calculate ml, the

approximate quantity of liquid to be used to prepare the bag gas sample.

4.3.7 Quickly withdraw an aliquot (approximately 5 microliters) of sample from the

distillate vial with the microliter syringe and record its weight from the analytical balance

to the nearest 0.01 mg.

4.3.8 Inject the contents of the syringe through the septum of the volatilization vessel into

the glass wool inside the vessel.

4.3.9 Reweigh and record the tare weight of the now empty syringe.

4.3.10 Record the pressure and temperature of the dilution gas as it is passed through the

dry gas meter, as shown in the figure 2 diagram.

4.3.11 After approximately 20 liters of dilution gas have passed into the tedlar bag, close

the valve to the dilution air source and record the exact final reading on the dry gas meter.

4.3.12 The gas bag is then analyzed by fia within 1 hour of bag preparation in accordance

with the procedures contained in section 4.4. 4.4 Determination of voc response factor.

4.4.1 Start up the fia instrument using the same settings as used for the gaseous voc

measurements.

4.4.2 Perform the fia analyzer calibration and linearity checks according to the procedure

in section 5.1. Record the responses to each of the calibration gases and the back-pressure

setting of the fia.

4.4.3 Connect the tedlar bag sample to the fia sample inlet and record the bag

concentration in terms of propane. Continue the analysis until a steady reading is obtained

for not less than 30 seconds. Record the final reading and proceed with the calculation of

the response factor.

4.5 Determination of coating voc content as voc (vu).

4.5.1 Determine the voc content of the coatings used in the process using EPA method 24

or 24a as applicable.

5. Calibration and quality assurance.

Page 14

5.1 Fia calibration and linearity check. Make necessary adjustments to the air and fuel

supplies for the fia and ignite the burner. Allow the fia to warm up for the period

recommended by the manufacturer. Inject a calibration gas into the measurement system

and adjust the back-pressure regulator to the value required to achieve the flow rates

specified by the manufacturer. Inject the zero- and the high-range calibration gases and

adjust the analyzer calibration to provide the proper responses. Inject the low and mid-

range gases and record the responses of the measurement system. The calibration and

linearity of the system are acceptable if the responses for all 4 gases are within 5% of the

respective gas values. If the performance of the system is not acceptable, repair or adjust

the system and repeat the linearity check. Conduct a calibration and linearity check after

assembling the analysis system and after a major change is made to the system. A

calibration curve consisting of zero gas and 2 calibration levelsshall be performed at the

beginning and end of each batch of samples.

5.2 Systems drift checks. After each sample, repeat the system calibration checks in

section 5.1 before any adjustments to the fia or measurement system are made. If the zero

or calibration drift is more than plus or minus 3% of the span value, discard the result and

repeat the analysis.

5.3 Quality control. A minimum of 1 sample in each batch shall be distilled and analyzed

in duplicate as a precision control. If the results of the 2 analyzed differ by more than plus

or minus 10% of the mean, then the system shall be reevaluated and the entire batch shall

be redistilled and analyzed.

6.

Calculations.

6.1 Bag sample volume, B_v.

(

) (

)

M_VT_STDP_M

) (

=

B_V

Where:

(

)

T _MP_STD

B_v

= Bag sample volume in

= Indicated dry gas meter

standard liters.

M_v

volume, in liters.

T_STD= 293⁰K.

T_M

= Meter gas temperature, in

⁰K.

P_M

= Meter gas pressure, in mm

Hg absolute.

P_STD= 760 mm Hg.

Bag sample voc concentration, as voc, C_voc.

C_voc= M_l/B_v

6.2

Where:

C_voc

=

Bag

sample

voc

concentration, as voc, mg/std. liters.

Page 15

M_l

= Weight of voc liquid

injected, mg.

6.3

Bag sample voc concentration, as propane, C_c3.

C_c3= R_c3*K

Where:

C_c3

=

Bag

sample

voc

concentration, as propane, mg C₃/std. liter.

R_c3

= FIA reading for bag gas

sample, ppm propane.

mg propane / std. liter

K = Conversion factor, 0.00183

Response factor, RF.

ppm propane

6.4

6.5

RF = C_voc/C_c3

Where:

RF

= Response factor, weight

voc/weight propane.

Total voc content of the input voc containing liquid, as propane, L.

n

V _IJW_IJ

RF_J

V _FJW_FJ

RF_J

V _AJW_AJ

RF_J

L =

-

+



J=1

Where:

L =

Total voc content of liquid

input, calculate as propane, kg.

voc liquid J.

V_IJ= Initial voc weight fraction of

V_FJ= Final voc weight fraction of

V_AJ= Voc weight fraction of voc

W_IJ= Weight of voc containing

W_FG= Weight of voc containing

W_AJ= Weight of voc containing

RF_J= Response factor for voc in

voc liquid J.

liquid J added during the test.

liquid J at beginning of test, kg.

liquid J at end of test, kg.

liquid J added during the test, kg.

liquid J, weight voc/weight propane.

Page 16

Page 17

History: 1993 AACS; 2002 AACS.

R 336.2010 Rescinded.

History: 1985 AACS; 1992 AACS; 1997 AACS.

R 336.2011 Reference test method 5B.

Rule 1011. Reference test method 5B, in-stack filtration method, reads as follows:

(a) The principle, applicability, and performance test criteria are as follows:

(i) Principle. Particulate matter is withdrawn isokinetically from the source and collected

on solid filtering media maintained at stack temperature. The particulate matter mass is

determined gravimetrically after removal of uncombined water.

(ii) Applicability. This method is applicable for the determination of particulate

emissions from stationary sources as identified in table 31 of R 336.1331. The method is

also applicable when specifically provided for in the department’s rules, orders, a permit

to install, or a permit to operate.

(iii) Performance test criteria as follows:

(A) A performance test must meet the requirements under R 336.2003(2).

(B) For sources that are subject to an emission limitation calculated to 50% excess air,

the multipoint, integrated sampling procedure of R 336.2004(1)(c) must be used for gas

analysis. For all other sources that require a determination of the molecular weight of the

Page 18

exhaust, an optional sampling procedure of R 336.2004(1)(c) may be used. Alternatives or

modifications to procedures are subject to the approval of the department.

(C) The minimum volume per sample must be 30 cubic feet of dry gas corrected to

standard conditions, 68 degrees Fahrenheit and 29.92 inches mercury. Minimum sample

time must be 60 minutes, which may be continuous or a combination of shorter sampling

periods for sources that operate in a cyclic manner. Smaller sampling times or sample

volumes, if necessitated by process variables or other factors, may be approved by the

department.

(D) For a source whose emission control device alters the moisture content of the

exhaust gas, a moisture determination must be performed in a location upstream from the

emission control device and in accordance with R 336.2004(1)(d) or an alternative method

approved by the department.

(b) The following provisions apply to apparatus:

(i) Sampling train. A schematic of the sampling train used in this method is shown in

figure 102 under R 336.2021. Construction details for many, but not all, of the train

components are given in APTD-0581, adopted by reference in R 336.1902. See subdivision

(g)(ii) of this rule. For changes from the APTD-0581 document and for allowable

modifications to figure 102, the user shall consult with the department. The operating and

maintenance procedures for many, but not all, of the sampling train are described in APTD-

0576, adopted by reference in R 336.1902. See subdivision (g)(iii) of this rule. Since

correct usage is important in obtaining valid results, all users shall read APTD-0576 and

adopt the applicable operating and maintenance procedures outlined in it, unless otherwise

specified. The sampling train must consist of the following components:

(A) Probe nozzle. Stainless steel 316 or glass with sharp, tapered leading edge. The

angle of taper must be less than 30 degrees and the taper must be on the outside to preserve

a constant internal diameter. The probe nozzle must be of the button-hook design, unless

otherwise specified by the department. If made of stainless steel, the nozzle must be

constructed from seamless tubing. Other materials of construction may be used, subject to

the approval of the department. A range of nozzle sizes suitable for isokinetic sampling

must be available, for example, 0.32 to 1.27 centimeters, 1/8 to 1/2 inch, or larger if higher

volume sampling trains are used inside diameter nozzles in increments of 0.16 centimeters,

1/16 inches. Each nozzle must be calibrated according to the procedures outlined in

subdivision (e) of this rule.

(B) Probe liner. Interior surface may be constructed of stainless steel, no specific grade,

glass, Teflon, or other material that maintains proper flow at the stack conditions

experienced.

(C) Pitot tube. Type S, as described in method 2, or other device approved by the

department. The pitot tube must be attached to the probe, as shown in figure 102 under R

336.2021, to allow constant monitoring of the stack gas velocity. The impact, high

pressure, opening plane of the pitot tube must be even with or above the nozzle entry plane,

see method 2, figure 2-6b, during sampling. The type S pitot tube assembly must have a

known coefficient, determined as outlined in method 2.

(D) Differential pressure gauge. Two incline manometer or equivalent devices as

described in method 2. One manometer must be used for velocity head (p) readings and the

other must be used for orifice differential pressure readings.

Page 19

(E) Filter holders. Two separate filter holders in series or 1 filter holder with separate

filter supports and seals for 2 filters. One filter holder with 2 filters held in contact with

each other is not acceptable. Materials of construction may be stainless steel 316, glass,

Teflon, or other material approved by the department.

(F) Filter heating system. Auxiliary heating of the filter media is not acceptable. For

saturated stack gases, the operator may opt to use filters that do not blind when wet and

that do not require heating, see subdivision (c)(i)(A) of this rule.

(G) Condenser. The following system must be used to determine the stack gas moisture

content: Three impingers connected in series with leak-free ground glass fittings or similar

leak-free noncontaminating fittings. All impingers must be of the Greenburg-Smith design

and must be modified by replacing the tip with a 1.3 centimeters, 1/2 inch, inside diameter

glass tube extending to about 1.3 centimeters, 1/2 inch, from the bottom of the flask.

Modifications, such as using flexible connections between the impingers or using materials

other than glass, are allowed, subject to the approval of the department. The first impinger

must contain a known quantity of water, as described in subdivision (d)(i)(C) of this rule.

The second impinger must be empty, and the third must contain a known weight of silica

gel or equivalent desiccant. Alternatively, a system that cools the sample gas stream and

allows measurement of the water condensed and moisture leaving the condenser, each to

within 1 milliliter or 1 gram, may be used, subject to the approval of the department. In

any case, the means for measuring the moisture leaving the condenser must be by passing

the sample gas stream through a tared silica gel, or equivalent desiccant, trap with exit

gases kept below 20 degrees Centigrade, 68 degrees Fahrenheit, and determining the

weight gain. If a determination of the particulate matter collected in the impingers is

required by the department’s rules, a permit to install, or a permit to operate, then the

impinger system described above must be used without modification. Contact the

department as to the sample recovery and analysis of the impinger contents.

(H) Metering system. Vacuum gauge, leak-free pump, thermometers capable of

measuring temperature to within 3 degrees Centigrade, 5.4 degrees Fahrenheit, dry-gas

meter capable of measuring volume to within 2%, and related equipment as shown in figure

102 under R 336.2021. Other metering systems capable of maintaining sampling rates

within 10% of isokinetic and capable of determining sample volumes to within 2% may be

used, subject to the approval of the department. When the metering system is used in

conjunction with a pitot tube, the system must enable checks of isokinetic rates. Sampling

trains utilizing metering systems designed for higher flow rates than those described in

APTD-0581 or APTD-0576, both adopted by reference in R 336.1902, may be used if the

specifications of this method are met.

(I) Barometer. Mercury, aneroid, or other barometer capable of measuring atmospheric

pressure to within 2.5 millimeters mercury, 0.1 inch mercury. In many cases, the

barometric reading may be obtained from a nearby national weather service station. In this

case, the station value, which is the absolute barometric pressure, must be requested and

an adjustment for elevation differences between the weather station and sampling point

must be applied at a rate of minus 2.5 millimeters mercury, 0.1 inch mercury, per 30 meters,

100 feet, elevation increase or vice versa for elevation decrease.

(J) Gas density determination equipment. Temperature sensor and pressure gauge, as

described in method 2, and gas analyzer, if necessary, as described in method 3. The

temperature sensor must, preferably, be permanently attached to the pitot tube or sampling

Page 20

probe in a fixed configuration so that the tip of the sensor extends beyond the leading edge

of the probe sheath and does not touch any metal. Alternatively, the sensor may be attached

just before use in the field. If the temperature sensor is attached in the field, then the sensor

must be placed in an interference-free arrangement with respect to the type S pitot tube

openings, see method 2, figure 2-6 Velocity Traverse Data. As a second alternative, if a

difference of not more than 1% in the average velocity measurement is to be introduced,

then the temperature gauge need not be attached to the probe or pitot tube. This alternative

is subject to the approval of the department. “Construction Details of Isokinetic Source

Sampling Equipment,” APTD-0581, April 1971, PB203-060-LL, and “Maintenance,

Calibration, and Operation of Isokinetic Source Sampling Equipment,” APTD-0576,

March 1972, PB209-022-LL, are adopted by reference in R 336.1902.

(ii) Sample recovery. The following items are required:

(A) Probe-liner and probe-nozzle brushes. Nylon bristle brushes with stainless steel wire

handles. The probe brush must have extensions, at least as long as the probe, made of

stainless steel, nylon, Teflon, or similarly inert material. The brushes must be properly

sized and shaped to brush out the probe liner and nozzle.

(B) Wash bottles. Two glass wash bottles are recommended. The tester may use

polyethylene wash bottles, but the acetone should not be stored in polyethylene bottles for

longer than 1 month.

(C) Glass sample storage containers. Chemically resistant, borosilicate glass bottles for

acetone washes. Screw cap liners must either be rubber-backed Teflon or must be

constructed to be leak-free and resistant to chemical attack by acetone. Narrow-mouth glass

bottles are less prone to leakage. Alternatively, polyethylene bottles may be used.

(D) Filter containers. Glass, polyethylene, or aluminum tube containers, unless

otherwise specified by the department.

(E) Graduated cylinder or balance. To measure condensed water to within 1 milliliter

or 1 gram, graduated cylinders must have subdivisions of not more than 2 milliliters. Most

laboratory balances are capable of weighing to the nearest 0.5 gram or less. Any of these

balances may be used here and in paragraph (iii)(D) of this subdivision.

(F) Plastic storage containers. Airtight containers to store silica gel.

(G) Funnel and rubber policeman. To aid in the transfer of silica gel to container, but

not necessary if silica gel is weighed in the field.

(H) Funnel. Glass or polyethylene, to aid in sample recovery.

(iii) Analysis. The following equipment is required for analysis:

(A) Glass weighing dishes.

(B) Desiccator.

(C) Analytical balance. To measure to within 0.1 milligram.

(D) Balance. To measure to within 0.5 milligram.

(E) Beakers. 250 milliliters.

(F) Hygrometer. To measure the relative humidity of the laboratory environment.

(G) Temperature gauge. To measure the temperature of the laboratory environment.

(c) The following provisions must apply to reagents:

(i) Sampling. The reagents used in sampling are as follows:

(A) Filters. Two in-stack filters may be any combination of alundum ceramic thimble

filters, type RA-98, or glass fiber filters, type A without organic binder. The size of the

filters must allow proper sampling rates to maintain iso-kinetics using the nozzle sizes

Page 21

specified in subdivision (b)(i)(A) of this rule. Alternatively, other types of filters may be

used, subject to the approval of the department.

(B) Silica gel. Indicating type, 6 to 16 mesh. If previously used, dry at 175 degrees

Centigrade, 350 degrees Fahrenheit, for 2 hours. New silica gel may be used as received.

Alternatively, other types of desiccants that are equivalent or better may be used, subject

to the approval of the department.

(C) Water. When analysis of the material caught in the impingers is required, distilled

water must be used. Run blanks before field use to eliminate a high blank of test samples.

(D) Crushed ice.

(E) Stopcock grease. Acetone-insoluble, heat-stable silicone grease. This is not

necessary if screw-on connectors with Teflon sleeves, or equivalent, are used.

Alternatively, other types of stopcock grease may be used, subject to the approval of the

department.

(ii) Sample recovery. Washing solvent. Either acetone or distilled water may be used for

sample recovery. If acetone is used for washing solvent, then reagent grade, less than

0.001% residue, in glass bottles is required. Acetone from metal containers generally has

a high residue blank and must not be used. If suppliers transfer acetone to glass bottles

from metal containers, then acetone blanks must be run before field use and only acetone

with low blank values, less than 0.001%, must be used. In no case must a blank value of

more than 0.001% of the weight of acetone used be subtracted from the sample weight. If

distilled water is used for washing solvent, use distilled water with less than 0.001%

residue. Run blanks before field use to eliminate a high blank on test samples.

(iii) Analysis. Two reagents are required for the analysis:

(A) Solvent. Same as paragraph (ii) of this subdivision for quantitative transfer.

(B) Desiccant. Anhydrous calcium sulfate, indicating type. Alternatively, other types of

desiccants may be used, subject to the approval of the department.

(d) The following provisions must apply to procedure:

(i) Sampling. The complexity of this method is such that, in order to obtain reliable

results, testers shall be trained and experienced with the test procedures. Sampling must

comply with the following provisions:

(A) Pretest preparation provisions are as follows:

(I). All the components must be maintained and calibrated according to the applicable

procedures described in APTD-0576, adopted by reference in R 336.1902, unless otherwise

specified in this rule.

(II) Weigh several 200 to 300 gram portions of silica gel in airtight containers to the

nearest 0.5 gram. Record the total weight of the silica gel plus container on each container.

As an alternative, the silica gel need not be preweighed, but may be weighed directly in its

impinger or sampling holder just before train assembly.

(III) Check filters visually against light for irregularities, flaws, pinhole leaks, or

cracks. Label filters of the proper size on the back side using numbering machine ink. As

an alternative, label the shipping containers, as described under subdivision (b)(ii)(D) of

this rule, and keep the filters in these containers at all times, except during sampling and

weighing.

(IV) Dry the filters in an oven at 105 degrees Centigrade, 220 degrees Fahrenheit, for

a minimum of 2 hours, cool for at least 1 hour in a desiccator containing anhydrous calcium

sulfate, and individually weigh and record each weight to the nearest 0.1 milligram. During

Page 22

the weighing, the filter must not be exposed to the laboratory atmosphere for a period of

more than 2 minutes and a relative humidity above 50%.

(V) Procedures, other than those specified, that account for relative humidity effects

may be used, subject to the approval of the department.

(B) Preliminary determinations provisions are as follows:

(I) Select the sampling site and the minimum number by the department.

(II) Determine the stack pressure, temperature, and the range of velocity heads using

method 2. It is recommended that a leak check of the pitot lines, see method 2, be

performed.

(III) Determine the moisture content using approximation method 4, or its alternatives,

for the purpose of making isokinetic sampling rate settings.

(IV) Determine the stack gas dry molecular weight, as described in method 2, if

integrated method 3 sampling is used for molecular weight determination, the integrated

bag sample must be taken simultaneously with, and for the same total length of time as, the

particulate sample run.

(V) Select a nozzle size based on the range of velocity heads so that it is not necessary

to change the nozzle size to maintain isokinetic sampling rates. During the run, do not

change the nozzle size. Ensure that the proper differential pressure gauge is chosen for the

range of velocity heads encountered, see method 2.

(VI) Select a suitable probe liner and probe length so that all traverse points may be

sampled. For large stacks, sampling from opposite sides of the stack may reduce the length

of probes.

(VII) Select a total sampling time greater than or equal to the minimum total sampling

time specified in the department’s rules so that the sampling time per point is not less than

5 minutes, unless approved by the department, or some greater time interval as specified

by the department, and so that the sample volume taken, corrected to standard conditions,

exceeds the required minimum total gas sample volume. The latter is based on an

approximate average sampling rate. The number of minutes sampled at each point may be

an integer or an integer plus 1/2 minute to avoid timekeeping errors. In some

circumstances, such as in batch cycles, it may be necessary to sample for shorter times at

the traverse points and to obtain smaller gas sample volumes. In these cases, the

department’s approval must first be obtained.

(C) Preparation of collection train provisions are as follows:

(I) During preparation and assembly of the sampling train, keep all openings where

contamination can occur covered until just before assembly or until sampling is about to

begin.

(II) Place 100 milliliters of water in the first impinger, leave the second impinger

empty, and transfer approximately 200 to 300 grams of preweighed silica gel from its

container to the third impinger. More silica gel may be used, but care must be taken to

ensure that it is not entrained and carried out from the impinger during sampling. Place the

container in a clean place for later use in the sample recovery. Alternatively, the weight of

the silica gel plus impinger may be determined to the nearest 0.5 gram and recorded.

(III) Using tweezers or clean disposable surgical gloves, place a labeled, identified, and

weighed filter in each filter holder. Be sure that the filter is properly centered and the gasket

properly placed so as to prevent the sample gas stream from circumventing the filter.

Page 23

(IV) Install the selected nozzle using a Viton A 0-ring when stack temperatures are less

than 260 degrees Centigrade, 500 degrees Fahrenheit, and a heat-resistant fiberglass,

graphite, or other material string gasket when temperatures are higher. See APTD-0576,

adopted by reference in R 336.1902, for requirements. Other connecting systems using

either 310 stainless steel or Teflon ferrules may be used to form a leak-free direct

mechanical connection.

(V) Mark the probe with heat-resistant tape or by some other method to denote the

proper distance into the stack or duct for each sampling point.

(VI) Set up the train as in figure 102 under R 336.2021.

(VII) If necessary, use a very light coat of silicone grease on all ground glass joints.

Grease only the outer portion, see APTD-0576, to avoid the possibility of contamination

by the silicone grease.

(VIII) Place crushed ice around the impingers.

(D) Leak check procedures:

(I) Pretest leak check. A pretest leak check is strongly recommended, but not required,

to prevent invalid sampling and wasted time. If the tester opts to conduct the pretest leak

check, the following procedure must be used: Perform the leak check on the entire system,

including filter housings and nozzle, by plugging the nozzle and pulling a 380 millimeter

mercury, 15 inch mercury, vacuum. Alternatively, a lower vacuum may be used if it is not

exceeded during the test. Leakage rates in excess of 4% of the average sampling rate or

0.00057 cubic meters per minute, 0.02 cubic feet per minute, whichever is less, are

unacceptable. The following leak check instructions for the sampling train described in

APTD-0576 and APTD-0581, adopted by reference in R 336.1902, may be helpful. Start

the pump with the bypass valve fully open and the coarse adjust valve completely closed.

Partially open the coarse adjust valve and slowly close the bypass valve until the desired

vacuum is reached. Do not reverse the direction of the bypass valve, as this will cause water

to back up into the flexible sample tube and the probe. If the desired vacuum is exceeded,

either leak-check at this higher vacuum or end the leak check and start over. When the leak

check is completed, first slowly remove the plug from the inlet to the nozzle and

immediately turn off the vacuum pump. This prevents the water in the first impinger from

being forced backward into the sample tube and prevents silica gel from being entrained

backward into the second impinger.

(II) Leak checks during sample run. If, during the sampling run, a component, such as

a filter assembly or impinger, change becomes necessary, a leak check must be conducted

immediately before the change is made. The leak check must be done according to the

procedure outlined in paragraph (i)(D)(I) of this subdivision, except that it must be done at

a vacuum equal to or greater than the maximum value recorded up to that point in the test.

If the leakage rate is not more than 0.00057 cubic meters per minute, 0.02 cubic feet per

minute, or 4% of the average sampling rate, whichever is less, then the results are

acceptable and no correction need be applied to the total volume of dry gas metered. If a

higher leakage rate is obtained, then the tester shall either record the leakage rate and plan

to correct the sample volume, as shown in subdivision (f)(iii) of this rule, or void the

sampling run. Immediately after component changes, leak checks may be performed. If

leak checks are done, then the procedure outlined in paragraph (i)(D)(I) of this subdivision

must be used.

Page 24

(III) Post-test leak check. A leak check is required at the conclusion of each sampling

run. The leak check must be performed in accordance with the procedures in paragraph

(i)(D)(I) of this subdivision, except that it must be conducted at a vacuum equal to or

greater than the maximum value reached during the sampling run. If the leakage rate is not

more than 0.00057 cubic meters per minute, 0.02 cubic feet per minute, or 4% of the

average sampling rate, whichever is less, then the results are acceptable and no correction

need be applied to the total volume of dry gas metered. If a higher leakage rate is obtained,

then the tester shall either record the leakage rate and correct the sample volume, as shown

in subdivision (f)(iii) of this rule, or void the sampling run.

(E) Particulate train operation. During the sampling run, maintain an isokinetic

sampling rate that is within 10% of true isokinetic, unless otherwise specified by the

department. For each run, record the data required on a data sheet such as the data sheet in

figure 104 under R 336.2021. Record the initial dry-gas meter reading. Record the dry-gas

meter readings at the beginning and end of each sampling time increment, when changes

in flow rates are made, before and after each leak check, and when sampling is halted. Take

other readings required by figure 104 under R 336.2021 at least once at each sample point

during each time increment, and take additional readings when significant changes, 20%

variation in velocity head readings, necessitate additional adjustments in flow rate. Level

and zero the manometer. Because the manometer level and zero may drift due to vibrations

and temperature changes, make periodic checks during the traverse. Clean the portholes

before the test run to minimize the chance of sampling deposited material. To begin

sampling, remove the nozzle cap and verify that the pitot tube and probe are properly

positioned. Position the nozzle at the first traverse point with the tip pointing directly into

the gas stream. Immediately start the pump and adjust the flow to isokinetic conditions.

Nomographs that aid in the rapid adjustment of the isokinetic sampling rate without

excessive computations are available. These nomographs are designed for use when the

type S pitot tube coefficient is 0.85 ±0.02 and the stack gas equivalent density, dry

molecular weight, is equal to 29 ±4. APTD-0576, adopted by reference in R 336.1902,

details the procedure for using the nomographs. If Cp and Md are outside the above stated

ranges, do not use the nomographs unless appropriate steps, see subdivision (g)(iv) of this

rule, are taken to compensate for the deviations. When the stack is under significant

negative pressure, height of impinger stem, take care to pull low-flow when inserting the

probe into the stack to prevent water from backing into the sample tubing and to avoid

pulsation through the filter and possible loss of materials. When the probe is in position,

block off the openings around the probe and porthole to prevent unrepresentative dilution

of the gas stream. Traverse the stack cross section, as required by method 1 or as specified

by the department, being careful not to bump the probe nozzle into the stack walls when

sampling near the walls or when removing or inserting the probe through the portholes;

this minimizes the chance of extracting deposited material. During the test run, add more

ice and, if necessary, salt to maintain a temperature of less than 20 degrees Centigrade, 68

degrees Fahrenheit, at the condenser/silica gel outlet. Also, periodically check the level and

zero of the manometer. If the pressure drop across the filter becomes too high and makes

isokinetic sampling difficult to maintain, the filter may be replaced in the midst of a sample

run. It is recommended that another complete filter assembly be used rather than attempting

to change the filter itself. Before a new filter assembly is installed, conduct a leak check,

as described under paragraph (i)(D)(II) of this subdivision. The total particulate weight

Page 25

must include the summation of all filter assembly catches. A single train must be used for

the entire sample run, except in cases where simultaneous sampling is required in 2 or more

separate ducts, at 2 or more different locations within the same duct, or where equipment

failure necessitates a change of trains. In all other situations, the use of 2 or more trains

must be subject to the approval of the department. When 2 or more trains are used, separate

analyses of the front-half and, if applicable, impinger catches from each train must be

performed, unless identical nozzle sizes were used on all trains. If identical nozzle sizes

were used, the front-half catches from the individual trains may be combined, as may the

impinger catches, and 1 analysis of front-half catch and 1 analysis of impinger catch may

be performed. Consult with the department for details concerning the calculation of results

when 2 or more trains are used. At the end of the sample run, turn off the coarse adjust

valve, remove the probe and nozzle from the stack, turn off the pump, record the final dry-

gas meter reading, and conduct a post-test leak check, as outlined in paragraph (i)(D)(III)

of this subdivision. Leak-check the pitot lines as described in method 2. The lines must

pass this leak check to validate the velocity head data.

(F) Calculation of percent isokinetic. Calculate percent isokinetic, see subdivision (f) of

this rule, to determine if the run was valid or if another test run should be made. If there

was difficulty in maintaining isokinetic rates due to source conditions, consult with the

department for possible variance on the isokinetic rates.

(ii) Sample recovery. Proper cleanup procedure begins as soon as the probe is removed

from the stack at the end of the sampling period. Allow the probe to cool. When the probe

can be safely handled, wipe off all external particulate matter near the tip of the probe

nozzle and place a cap over it to prevent losing or gaining particulate matter. Do not cap

off the probe tip tightly while the sampling train is cooling down as this creates a vacuum

in the filter holder and draws water from the impingers into the sample tube. Before moving

the sampling train to the cleanup site, make sure all condensed water in the probe and

flexible sample lines are drained into the first impinger. Disconnect all sample lines and

remove the nozzle-filter set assembly from the probe. Cap all openings to prevent

contamination or accidental loss of sample. Remove all excess particulate from the exterior

of the nozzle-filter assembly to prevent contamination during disassembly. Transfer the

nozzle-filter set assembly and impinger set to the cleanup area. The cleanup area must be

clean and protected from the wind so that the chances of contaminating or losing the sample

are minimized. Save a portion of the solvent used for cleanup as a blank. Take 200

milliliters of this solvent directly from the wash bottle being used and place it in a glass

sample container labeled "solvent blank". Inspect the train before and during disassembly

and note any abnormal conditions. Treat the samples in the following manner: Container

numbers. 1, 1A. Carefully remove the filters from the filter holders and place each filter in

its identified container. Use a pair of tweezers or clean disposable surgical gloves, or both,

to handle the filters. Carefully transfer to the container any particulate matter or filter fibers,

or both, that adhere to the filter holder gasket by using a dry nylon bristle brush or sharp-

edged blade, or both. Seal the containers. Container number 2. Taking care to see that

particulate on the outside of the nozzle and filter holders does not get into the sample, the

tester shall carefully remove the nozzle and clean the inside surface by rinsing with solvent

from a wash bottle and brushing with a nylon bristle brush. Brush until the solvent rinse

shows no visible particles and then make a final rinse of the inside surface with solvent.

After ensuring that all joints have been cleaned of all extraneous material, the tester shall

Page 26

quantitatively remove particulate from the filter holders by rubbing the surfaces with a

nylon bristle brush and rinsing with solvent. Rinse each surface 3 times, or more if needed,

to remove visible particulate. Make a final rinse of the brush and filter holder set. After all

solvent washings and particulate matter have been collected in the sample container,

tighten the lid on the sample container so that solvent will not leak out when it is shipped

to the laboratory. Mark the height of the fluid level to determine if leakage occurred during

transport. Label the container to clearly identify its contents. Container number 3. Note the

color of the indicating silica gel to determine if it has been completely spent and make a

notation of its condition. Transfer the silica gel from the third impinger to its original

container and seal. A funnel may make it easier to pour the silica gel without spilling it. A

rubber policeman may be used as an aid in removing the silica gel from the impinger. It is

not necessary to remove the small amount of dust particles that adhere to the impinger wall

and are difficult to remove. Since the gain in weight will be used for moisture calculations,

do not use any water or other liquids to transfer the silica gel. If a balance is available in

the field, follow the procedure for container number 3 in paragraph (iii) of this subdivision.

Impinger water. Treat the impingers in the following manner: Make a notation of any color

or film in the liquid catch. Measure the liquid that is in the first 2 impingers to within ±1

milliliter by using a graduated cylinder or by weighing it to within ±1.0 gram by using a

balance if one is available. Record the volume or weight of liquid present. This information

is required to calculate the moisture content of the effluent gas. Discard the liquid after

measuring and recording the volume or weight, unless analysis of the impinger catch is

required, see subdivision (b)(i)(G) of this rule. If a different type of condenser is used,

measure the amount of moisture condensed either volumetrically or gravimetrically. If

possible, containers must be shipped in a manner that keeps them upright at all times.

(iii) Analysis. Record the data required on a sheet such as the sheet in figure 106 under

R 336.2021. Handle each sample container in the following manner: Container numbers 1,

1A. Analyze and report each filter separately. Transfer the filter and any loose particulate

from the sample container to a tared-glass weighing dish. Dry the filter in an oven at 105

degrees Centigrade, 220 degrees Fahrenheit, for a minimum of 2 hours, cool for at least 1

hour in a desiccator containing anhydrous calcium sulfate, and weigh and record its weight

to the nearest 0.1 milligram. During the weighing the filter must not be exposed to the

laboratory atmosphere for a period greater than 2 minutes or a relative humidity above

50%. Procedures, other than those specified, that account for relative humidity effects may

be used, subject to the approval of the department. The method used for drying and

weighing of filters must be consistent before and after the test. Container number 2. Note

the level of liquid in the container and confirm on the analysis sheet if leakage occurred

during transport. If a noticeable amount of leakage has occurred, then either void the

sample or use methods, subject to the approval of the department, to correct the final

results. Measure the liquid in this container either volumetrically to ±1 milliliter or

gravimetrically to ±1.0 gram. Transfer the contents to a tared 250-milliliter beaker and

evaporate to dryness either at ambient temperature and pressure for acetone or at 95 degrees

Centigrade, 203 degrees Fahrenheit, in an oven for distilled water. Then subject the sample

to 250 degrees Centigrade, 482 degrees Fahrenheit, in an oven for 2 to 3 hours. Desiccate

24 hours and weigh to a constant weight. Report the results to the nearest 0.1 milligram.

Container number 3. Weigh the spent silica gel, or silica gel plus impinger, to the nearest

0.5 gram using a balance. This step may be conducted in the field. "Solvent blank"

Page 27

container. Measure solvent in this container either volumetrically or gravimetrically.

Transfer the contents to a tared 250-milliliters beaker and evaporate to dryness either at

ambient temperature and pressure for acetone or at 95 degrees Centigrade, 203 degrees

Fahrenheit, in an oven for distilled water. Then subject the sample to 250 degrees

Centigrade, 482 degrees Fahrenheit, in an oven for 2 to 3 hours. Desiccate for 24 hours and

weigh to a constant weight. Report the results to the nearest 0.1 milligram. If acetone is

used, the contents of Container number 2, as well as the acetone blank container, may be

evaporated at temperatures higher than ambient. If evaporation is done at an elevated

temperature, then the temperature must be closely supervised, and the contents of the

beaker must be swirled occasionally to maintain an even temperature. Use extreme care,

as acetone is highly flammable and has a low flash point.

(e) Calibration. Maintain a laboratory log of all calibrations. Calibrations must comply

with the following provisions:

(i) Probe nozzle. A probe nozzle must be calibrated before its initial use in the field.

Using a micrometer, measure the inside diameter of the nozzle to the nearest 0.025

millimeter, 0.001 inch. Make 3 separate measurements using different diameters each time

and obtain the average of the measurements. The difference between the high and low

numbers must not exceed 0.1 millimeter, 0.004 inch. When nozzles become nicked, dented,

or corroded, the nozzles must be reshaped, sharpened, and recalibrated before use. Each

nozzle must be permanently and uniquely identified.

(ii) Pitot tube. The type S pitot tube assembly must be calibrated according to the

procedures in method 2.

(iii) Metering system. Before its initial use in the field, the metering system must be

calibrated according to the procedure in APTD-0576, adopted by reference in R 336.1902.

Instead of physically adjusting the dry-gas meter dial readings to correspond to the wet-

test meter readings, calibration factors may be used to mathematically correct the gas meter

dial readings to the proper values. Before calibrating the metering system, a leak check

may be conducted. For metering systems having diaphragm or rotary pumps, the normal

leak check procedure will not detect leakages within the pump. For these cases, the

following leak check procedure may be used: Make a 10-minute calibration run at 0.00057

cubic meters per minute, 0.02 cubic feet per minute. At the end of the run, take the

difference of the measured wet-test meter and dry-gas meter volumes and divide the

difference by 10 to get the leak rate. The leak rate must not exceed 0.00057 cubic meters

per minute (0.02 cubic feet per minute). After each field use, the calibration of the metering

system must be checked by performing 3 calibration runs at a single, intermediate orifice

setting, based on the previous field test, with the vacuum set at the maximum value reached

during the test series. To adjust the vacuum, insert a valve between the wet-test meter and

the inlet of the metering system. Calculate the average value of the calibration factor. If the

calibration has changed by more than 5%, then recalibrate the meter over the full range of

orifice settings, as outlined in APTD-0576. Alternatively, a spirometer may be substituted

for a wet-test meter in the above calibration procedures. Alternative procedures, such as

using the orifice meter coefficients, may be used, subject to the approval of the department.

If the dry-gas meter coefficient values obtained before and after a test series differ by more

than 5%, then the test series must be performed using whichever meter coefficient value,

before or after, gives the lower value of total sample volume.

Page 28

(iv) Temperature gauges. Use the procedure in method 2 to calibrate in-stack

temperature gauges. Dial thermometers, such as those used for the dry-gas meter and

condenser outlet, must be calibrated against mercury-in-glass thermometers or other

thermometers that are calibrated using a National Institute of Standards and Technology

calibrated reference thermometer.

(v) Leak check of metering system shown in figure 102 under R 336.2021. That portion

of the sampling train from the pump to the orifice meter must be leak-checked before initial

use and after each shipment. Leakage after the pump will result in less volume being

recorded than is actually sampled. The following procedure is suggested, also see figure

107 under R 336.2021: Close the main valve on the meter box. Insert a 1-hole rubber

stopper with rubber tubing attached into the orifice exhaust pipe. Disconnect and vent the

low side of the orifice manometer. Close off the low side orifice tap. Pressurize the system

to 13 to 18 centimeters, 5 to 7 inches, water column by blowing into the rubber tubing.

Pinch off the tubing and observe the manometer for 1 minute. A loss of pressure on the

manometer indicates a leak in the meter box. Leaks, if present, must be corrected.

(vi) Barometer. Calibrate against a mercury barometer.

(f) Calculations. When carrying out calculations, retain at least 1 extra decimal figure

beyond that of the acquired data. Round off figures after the final calculation. Other forms

of the equations may be used if the other forms of the equations give equivalent results.

The following provisions apply to calculations:

(i) Nomenclature:

A_n= Cross-sectional area of nozzle, meters² or the equivalent feet².

A = Cross-sectional area of stack or flue at the point of sampling, feet².

B _ws= Water vapor in the gas stream, proportion by volume, expressed as a fraction.

B _wi= Percent water vapor in gas entering source particulate control device determined

by method 4.

B _wo= Percent water vapor in gas exiting source particulate control device.

C_a= Wash blank residue concentration, milligrams per gram.

C_s= Concentration of particulate matter in stack gas, pounds per 1,000 pounds of actual

stack gas.

C _sD= Concentration of particulate matter in stack gas, moisture excluded, pounds per

1000 pounds of dry stack gas.

C_s50= Concentration of particulate matter corrected to 50% excess air, pounds per 1000

pounds of stack gas.

C_s50D= Concentration of particulate matter corrected to 50% excess air, excluding any

water addition from a collector, pounds per 1000 pounds of stack gas.

E = Mass emission rate of particulate, pounds/hour.

F₅₀= Concentration conversion factor to 50% excess air with no moisture alterations

in exhaust.

F_50D= Concentration conversion factor to 50% excess air, excluding any moisture

added to exhaust gas by pollution collection system.

F_D= Concentration conversion factor to dry basis, excluding any water in the stack gas.

I = Percent of isokinetic sampling.

L _a= Maximum acceptable leakage rate for either a pretest leak check or for a leak

check following a component change; equal to 0.00057 meters³/minute (0.02 cubic feet per

minute) or 4% of the average sampling rate, whichever is less.

Page 29

L_i= Individual leakage rate observed during the leak check conducted

before the "ith" component change (i = 1, 2, 3 . . . . n), meters³/minute (cubic feet per

minute).

L_p= Leakage rate observed during the post-test leak check, meters³/minute (cubic feet

per minute).

M_d= Molecular weight of dry stack gas, gram/gram mole (pound/pound-mole),

calculated

by method 3, equation 3-1, using data from integrated method 3.

m_n= Total amount of particulate matter collected, milligram.

M_w= Molecular weight of water, 18.0 gram/gram-mole (18.0 pound/pound-mole).

m_a= Mass of residue of solvent after evaporation, milligram.

m_g= Total weight of gas samples through nozzle, pound.

P _bar= Barometric pressure at the sampling site, millimeter mercury (inches mercury).

P_s= Absolute stack gas pressure.

P_std= Standard absolute pressure, 760 millimeters mercury (29.92 inches mercury).

R = Ideal gas constant, 0.06236 millimeters of mercury-cubic meters per kelvin-gram-

mole, (21.85 inches of mercury-cubic feet per Rankine-pound-mole).

T _m= Absolute average dry-gas meter temperature, see figure 104 under R 336.2021,

°Kelvin, (°Rankine).

T_s= Absolute average stack gas temperature, see figure 104 under R 336.2021, °Kelvin,

(°Rankine).

T_std= Standard absolute temperature, 294.I°Kelvin, (530°Rankine).

V _a= Volume of solvent blank, milliliters.

V _aw= Volume of solvent used in wash, milliliters.

V _lc= Total volume of liquid collected in impingers and silica gel (see figure 106 under

R 336.2021), milliliters.

V_m= Volume of gas sample as measured by the dry-gas meter, deci-centimeter, (deci-

cubic-foot).

V _m(std)= Volume of gas sample measured by the dry-gas meter, corrected to standard

conditions, deci-standard cubic meter, (deci-standard cubic foot).

V _w(std)= Volume of water vapor in the gas sample, corrected to standard conditions,

standard cubic meter, (standard cubic foot).

V _s= Stack gas velocity, calculated by method 2, using data obtained from method 5,

meters/second (feet/second).

W_a= Weight of residue in solvent wash, milligram.

Y = Dry-gas meter calibration factor.

ΔH = Average pressure differential across the orifice meter (see figure 104 under R

336.2021), millimeter water (inches water).

%0₂= Percent oxygen in stack gas by volume (dry basis).

%N₂= Percent nitrogen in stack gas by volume (dry basis).

p _a= Density of solvent, milligrams/milliliter.

p _s(std)= Density of all sampled gas at standard conditions, pounds/feet.³

p_w= Density of water, 0.9982 grams/milliliter (0.002201 pounds/milliliter).

θ = Total sample time, minute.

θ1 = Sample time, interval, from the beginning of a run until the first component

change, minute.

Page 30

θi = Sampling time interval, between 2 successive component changes, beginning with

the interval between the first and second changes, minute.

θp = Sampling time interval, from the final (nth) component change until the end of the

sampling run, minute.

13.6 = Specific gravity of mercury.

60 = Seconds/minute.

100 = Conversion to percent.

386.9 = Cubic feet per pound-mole of ideal gas at standard conditions.

453.6 = Conversion of pounds to grams.

3600 = Conversion of hours to seconds.

1000 = Conversion of 1000 pound units to pound units.

(ii) Average the dry-gas meter temperature and average the orifice pressure drop. See

data sheet, figure 104 under R 336.2021.

(iii) Dry gas volume. Correct the sample volume measured by the dry-gas meter to

standard conditions, 21.11 degrees Centigrade, 760 millimeters mercury or 68 degrees

Fahrenheit, 29.92 inches mercury, by using equation 5-1.

Equation 5-1:

Y

(

+ H / 13.6)

(

+ H / 13.6)

P_bar

V _mT_stdP_bar

=

Y

K₁V _m

V _m(std)

T_mP_std

T_m

Where:

K₁

= 0.3869 °K/mm Hg for metric units.

= 17.71 °R/in. Hg for English units.

Equation 5-1 may be used as written. However, if the leakage rate observed during any of

the mandatory leak checks, for example, the post-test leak check or leak checks conducted

before component changes, exceeds L_a, equation 5-1 must be modified as follows:

(A) Case I. No component changes made during sampling run. In this case, replace V_m

in equation 5-1 with the following expression:

Vm

-(L

p

-L)

a

(B) Case II. One or more component changes made during the sampling run. In this

case, replace V in equation 5-1 by the following expression:

m

n

Vm

- (L

1

- L

a

)

1

−

(L

i

- L

a

)

i

− (L

p

- L

a

)

p



i=2

and substitute only for those leakage rates (L_ior L_p) that exceed L_a.

(iv) Volume of water vapor.

Equation 5-2

Page 31

=

( p_w/

) (R

/

) =

V_w(std)

V_1c

M_w

T_stdP_stdK₂V_1c

Where:

K₂= 0.001338 m³/ml for metric units.

= 0.04733 ft.³/ml for English units.

(v) Moisture content.

Equation 5-3

=

/ (

V_w(std)V_m(std)

+

)

v_w(std)

B_ws

In saturated or water droplet-laden gas streams, 2 calculations of the moisture content of

the stack gas must be made: 1 from the impinger analysis, equation 5-3, and a second from

the assumption of saturated conditions. The lower of the 2 values of B_wsmust be considered

correct. The procedure for determining the moisture content based on the assumption of

saturated conditions as described in 40 CFR part 60 appendix A method 4. For the purpose

of this method, the average stack gas temperature from figure 104 under R 336.2021 may

be used to make the determination, if the accuracy of the in-stack temperature sensor is ±1

degree Centigrade, 2 degrees Fahrenheit.

(vi) Solvent blank concentration.

Equation 5-4

=

/ ( )

m_aV_aP_a

C_a

(vii) Solvent wash blank.

Equation 5-5

=

W_a

C_aV_awP_a

(viii) Total particulate weight. Determine the total particulate catch from the sum of the

weights obtained from containers 1, 1A, and 2 less the wash solvent blank, see figure 106

under R 336.2021. Refer to subdivision (d)(i)(E) of this rule to assist in the calculation of

results involving 2 or more pairs of filters or 2 or more sampling trains.

(ix) Sampled gas density. Determine the density of the gas sampled from the stack, at

standard conditions in pounds per cubic foot, lb/ft.³.

Equation 5-6

= (

(1-

) +

) / 386.9

M_wB_ws

P_s(std)

M_d

B_ws

(x) Total weight of gas sampled, lbs.

Page 32

Equation 5-7

= (

+

V _w(std)

) p

s(std)

m_g

V_m(std)

(xi) Particulate concentration, lbs/1000 lbs.

Equation 5-8

=

/ (453.6

)

m_g

C_s

m_n

(xii) Excess air and moisture correction factors:

(A) Correction factor to 50% excess air for those sources with or without a particulate

collector where no increase in moisture content of the exhaust gas occurs after the process

and before the point of sampling.

Equation 5-9

+ 18

/ (100 -

)

M_d

- 2.0592 %

B_wo

+

B_wo

+ 18

=

F₅₀

0.1826 %

/ (100 -

)

B_wo

N₂

0₂

M_d

B_wo

(B) Correction factor to 50% excess air for those sources with a wet collection device,

scrubber, that increases the moisture content of the exhaust gas after the process and before

the point of sampling.

Equation 5-10

+ 18

/ (100 -

)

M_d

- 2.0592 %

B_wo

+

B_wo

+ 18

=

F_50D

0.1826 %

/ (100 -

)

B_wi

N₂

0₂

M_d

B_wi

(C) Correction factor to convert the actual concentration, C_s, to dry conditions.

Equation 5-11

+ 18

/ (100 -

)

B_wo

M_d

B_wo

=

F_D

M_d

(xiii) Converted particulate concentrations, where applicable under the department’s

rules or permit.

Equation 5-12

=

C_s50

C_sF₅₀

Page 33

Equation 5-13

=

C_s50D

C_sF_50D

Equation 5-14

=

C_sD

C_sF_D

(xiv) Mass emission rate in pounds per hour, lb/hr.

Equation 5-15

3600 A

V_sC_sP_sT_stdP_s(std)

E =

=

A

/

K₃V_sC_sP_sP_s(std)T_s

1000

T_sP_std

Where:

K₃

= 63.77 for English units.

(xv) Isokinetic variation using 1 of the following methods:

(A) Calculation from raw data.

Equation 5-16

100

(

+ (

/

)( + H / 13.6))

T_sK₄V _lc

V _mT_mP_bar

I =

60 

V _sP_sA_n

Where:

K₄

= 0.003458 mm Hg - m³ml - °K for metric units.

= 0.002672 in. Hg - ft.³/ml - °R for English units.

(B) Calculation from intermediate values.

Equation 5-17

100

T_sV_m(std)P_std

T_sV_m(std)

 (1-

I =

=

K₅



60(1-

)

B_ws

T_stdV_sA_nP_s

B_ws

P_sV_sA_n

Where:

K5 = 4.307 for metric units.

= 0.09409 for English units.

(xvi) Acceptable results. If 90%=I=110%, then the results are acceptable. If the results

are low in comparison to the standard and I is beyond the acceptable range, or if I is less

Page 34

than 90%, then the department may opt to accept the results. Otherwise, reject the results

and repeat the test.

(g) Bibliography:

(i) Federal Register, Volume 42, No. 160, Part 160, Chapter 1, Title 40, Appendix A,

Method 5, August 18, 1977.

(ii) Martin, Robert M. Construction Details of Isokinetic Source Sampling Equipment.

Environmental Protection Agency. Research Triangle Park, N.C. APTD-0581. April, 1971.

(iii) Rom, Jerome J. Maintenance, Calibration, and Operation of Isokinetic Source

Sampling Equipment. Environmental Protection Agency. Research Triangle Park, N.C.

APTD-0576. March, 1972.

(iv) Shigehara, R. T. "Adjustments in the EPA Nomograph for Different Pitot Tube

Coefficients and Dry Molecular Weights." Stack Sampling News, 2:4 - 11. October, 1974.

(v) Guidelines for Source Testing of Particulate. Michigan Department of Natural

Resources, Air Quality Division. June 1, 1977.

History: 1985 AACS; 1992 AACS; 2002 AACS; 2005 AACS; 2025 AACS.

R 336.2012 Reference test method 5C.

Rule 1012. Reference test method 5C, out-stack filtration method, reads as follows:

(a) The principle, applicability, and performance test criteria are as follows:

(i) Principle. Particulate matter is withdrawn iso-kinetically from the source and

collected on solid filtering media maintained at a temperature in the range of 120 ±14

degrees Centigrade, 248 ±25 degrees Fahrenheit, or another temperature as specified by

the department's rules or a permit condition, or as approved by the department for a

particular application. The particulate mass, which includes any material that condenses at

or above the filtration temperature, is determined gravimetrically after removal of

uncombined water.

(ii) Applicability. This method is applicable for the determination of particulate

emissions from stationary sources as identified in table 31 of R 336.1331. The method is

also applicable when specifically provided for in the department’s rules, orders, a permit

to install, or a permit to operate.

(iii) Performance test criteria as follows:

(A) A performance test must meet the requirements under R 336.2003(2).

(B) For sources that are subject to an emission limitation calculated to 50% excess air,

the multipoint, integrated sampling procedure of R 336.2004(1)(c) must be used for gas

analysis. For all other sources that require a determination of the molecular weight of the

exhaust, an optional sampling procedure of R 336.2004(1)(c) may be used. Alternatives or

modifications to procedures are subject to the approval of the department.

(C) The minimum volume per sample must be 30 cubic feet of dry gas corrected to

standard conditions, 68 degrees Fahrenheit, 29.92 inches mercury. Minimum sample time

must be 60 minutes, which may be continuous or a combination of shorter sampling periods

for sources that operate in a cyclic manner. Smaller sampling times or sample volumes,

when necessitated by process variables or other factors, may be approved by the

department.

(D) For a source whose emission control device alters the moisture content of the

exhaust gas, a moisture determination must be performed in a location upstream from the

Page 35

emission control device and in accordance with R 336.2004(1)(d) or an alternative method

approved by the department.

(b) The following provisions apply to apparatus:

(i) Sampling train. A schematic of the sampling train used in this method is shown in

figure 103 under R 336.2021. Construction details for many, but not all, of the train

components are given in APTD-0581, subdivision (g)(ii) of this rule. For changes from the

APTD-0581 document and for allowable modifications to figure 103 under R 336.2021,

consult with the department. The operating and maintenance procedures for many, but not

all, of the sampling train are described in APTD-0576, adopted by reference in R 336.1902,

and referenced under subdivision (g)(iii) of this rule. Since correct usage is important in

obtaining valid results, all users shall read APTD-0576 and adopt the applicable operating

and maintenance procedures outlined in it, unless otherwise specified. The sampling train

consists of the following components:

(A) Probe nozzle. Stainless steel 316 or glass with sharp, tapered leading edge. The

angle of taper must be less than 30 degrees and the taper must be on the outside to preserve

a constant internal diameter. The probe nozzle must be of the buttonhook design, unless

otherwise specified by the department. If made of stainless steel, the nozzle must be

constructed from seamless tubing. Other materials of construction may be used, subject to

the approval of the department. A range of nozzle sizes suitable for isokinetic sampling

must be available, for example, 0.32 to 1.27 centimeters, 1/8 to 1/2 inch, or larger if higher

volume sampling trains are used inside diameter nozzles in increments of 0.16 centimeters,

1/16 inches. Each nozzle must be calibrated according to the procedures outlined in

subdivision (e) of this rule.

(B) Probe liner. Borosilicate or quartz glass tubing with a heating system capable of

maintaining a gas temperature at the exit end during sampling of 120 ±14 degrees

Centigrade, 248 ±25 degrees Fahrenheit, another temperature as specified by the

department's rules, or a temperature approved by the department for a particular

application. The tester may opt to operate the equipment at a temperature lower than that

specified. Since the actual temperature at the outlet of the probe is not usually monitored

during sampling, probes constructed according to APTD-0581, adopted by reference in R

336.1902, which utilize the calibration curves of APTD-0576, or calibrated according to

the procedure outlined in APTD-0576, adopted by reference in R 336.1902, are acceptable.

Either borosilicate or quartz glass probe liners may be used for stack temperatures up to

about 480 degrees Centigrade, 900 degrees Fahrenheit; quartz liners must be used for

temperatures between 480 and 900 degrees Centigrade, 900 and 1,650 degrees Fahrenheit.

Both types of liners may be used at higher temperatures than specified for short periods of

time, subject to the approval of the department. The softening temperature for borosilicate

is 820 degrees Centigrade, 1,508 degrees Fahrenheit, and for quartz it is 1,500 degrees

Centigrade, 2,732 degrees Fahrenheit. When practical, every effort must be made to use

borosilicate or quartz glass probe liners. Alternatively, metal liners, such as 316 stainless

steel, Incoloy 825, or other corrosion resistant materials made of seamless tubing, may be

used, subject to the approval of the department.

(C) Pitot tube. Type S, as described in method 2, or another device approved by the

department. The pitot tube must be attached to the probe, as shown in figure 103 under R

336.2021, to allow constant monitoring of the stack gas velocity. The impact, high

pressure, opening plane of the pitot tube must be even with or above the nozzle entry plane,

Page 36

see method 2, figure 2-6 Velocity Traverse Data, during sampling. The type S pitot tube

assembly must have a known coefficient, determined as outlined in method 2.

(D) Differential pressure gauge. Incline manometer or equivalent devices (2), as

described in method 2. One manometer must be used for velocity head (p) readings, and

the other must be used for orifice differential pressure readings.

(E) Filter holders. Two separate filter holders in series or 1 filter holder with separate

filter supports and seals for 2 filters. One filter holder with 2 filters held in contact with

each other is not acceptable. Materials of construction may be stainless steel 316, glass,

Teflon, or another material approved by the department.

(F) Filter heating system. Any heating system capable of maintaining a temperature

around the filter holder during sampling of 120 ±14 degrees Centigrade, 248 ±25 degrees

Fahrenheit, another temperature as specified by the department's rules or a permit

condition, or a temperature approved by the department for a particular application.

Alternatively, the tester may opt to operate the equipment at a temperature lower than that

specified. A temperature gauge capable of measuring temperature to within 3 degrees

Centigrade, 5.4 degrees Fahrenheit, must be installed so that the temperature around the

filter holders can be regulated and monitored during sampling. Heating systems other than

the one shown in APTD-0581 may be used.

(G) Condenser. The following system must be used to determine the stack gas moisture

content: Three impingers connected in series with leak-free ground glass fittings or any

similar leak-free non-contaminating fittings. All impingers must be of the Greenburg-

Smith design and must be modified by replacing the tip with a 1.3 centimeters, 1/2 inch,

inside diameter glass tube extending to about 1.3 centimeters, 1/2 inch, from the bottom of

the flask. Modifications, such as using flexible connections between the impingers or using

materials other than glass, are allowed subject to the approval of the department’s staff.

The first impinger must contain a known quantity of water, as described in subdivision

(d)(i)(C) of this rule, the second must be empty, and the third must contain a known weight

of silica gel or equivalent desiccant. Alternatively, a system that cools the sample gas

stream and allows measurement of the water condensed and moisture leaving the

condenser, to within 1 milliliter or 1 gram, may be used subject to the approval of the

department. In any case, the means for measuring the moisture leaving the condenser must

be by passing the sample gas stream through a tared silica gel, or equivalent desiccant, trap

with exit gases kept below 20 degrees Centigrade, 68 degrees Fahrenheit, and determining

the weight gain. If a determination of the particulate matter collected in the impingers is

required by the department's rules, a permit to install, or a permit to operate, the impinger

system described in this subparagraph must be used, without modification. Contact the

department as to the sample recovery and analysis of the impinger contents.

(H) Metering system. Vacuum gauge, leak-free pump, thermometers capable of

measuring temperature to within 3 degrees Centigrade, 5.4 degrees Fahrenheit, drygas

meter capable of measuring volume to within 2%, and related equipment as shown in figure

103 under R 336.2021. Other metering systems capable of maintaining sampling rates

within 10% of isokinetic and capable of determining sample volumes to within 2% may be

used, subject to the approval of the department. When the metering system is used in

conjunction with a pitot tube, the system must enable checks of isokinetic rates. Sampling

trains utilizing metering systems designed for higher flow rates than those described in

Page 37

APTD-0581 or APTD-0576, both adopted by reference in R 336.1902, may be used if the

specifications of this method are met.

(I) Barometer. Mercury, aneroid, or other barometer capable of measuring atmospheric

pressure to within 2.5 millimeters mercury, 0.1 inch mercury. In many cases, the

barometric reading may be obtained from a nearby national weather service station. When

obtained from this source, the station value, which is the absolute barometric pressure, must

be requested and an adjustment for elevation differences between the weather station and

sampling point must be applied at a rate of minus 2.5 millimeters mercury per 30 meters,

0.1 inch mercury, per 100 foot, elevation increase or vice versa for elevation decrease.

(J) Gas density determination equipment. Temperature sensor and pressure gauge, as

described in method 2, and gas analyzer, if necessary, as described in method 3. The

temperature sensor must, preferably, be permanently attached to the pitot tube or sampling

probe in a fixed configuration so that the tip of the sensor extends beyond the leading edge

of the probe sheath and does not touch any metal. Alternatively, the sensor may be attached

just before use in the field. Note, however, that if the temperature sensor is attached in the

field, the sensor must be placed in an interference-free arrangement with respect to the type

S pitot tube openings, see method 2, figure 2.7. As a second alternative, if a difference of

not more than 1% in the average velocity measurement is to be introduced, the temperature

gauge need not be attached to the probe or pitot tube. This alternative is subject to the

approval of the department.

(ii) Sample recovery. The following items :

(A) Probe-liner and probe-nozzle brushes. Nylon bristle brushes with stainless steel wire

handles. The probe brush must have extensions, at least as long as the probe, made of

stainless steel, nylon, Teflon, or similarly inert material. The brushes must be properly

sized and shaped to brush out the probe liner and nozzle.

(B) Wash bottles - 2. Glass wash bottles are recommended; polyethylene wash bottles

may be used at the option of the tester. It is recommended that acetone not be stored in

polyethylene bottles for longer than a month.

(C) Glass sample storage containers. Chemically resistant, borosilicate glass bottles, for

acetone washes. Screw cap liners must either be rubber-backed Teflon or must be

constructed so as to be leak-free and resistant to chemical attack by acetone. Narrow-mouth

glass bottles have been found to be less prone to leakage. Alternatively, polyethylene

bottles may be used.

(D) Filter containers. Glass, polyethylene, or aluminum tube containers, unless

otherwise specified by the department.

(E) Graduated cylinder or balance. To measure condensed water to within 1 milliliter

or 1 gram. Graduated cylinders must have subdivisions of not more than 2 milliliters. Most

laboratory balances are capable of weighing to the nearest 0.5 gram or less. Any of these

balances are suitable for use here and in paragraph (iii)(D) of this subdivision.

(F) Plastic storage containers. Airtight containers to store silica gel.

(G) Funnel and rubber policeman, to aid in the transfer of silica gel to container; not

necessary if silica gel is weighed in the field.

(H) Funnel made from glass or polyethylene, to aid in sample recovery.

(iii) Analysis must include the following equipment:

(A) Glass weighing dishes.

(B) Desiccator.

Page 38

(C) Analytical balance, to measure to within 0.1 milligrams.

(D) Balance, to measure to within 0.5 milligrams.

(E) Beakers, 250 milliliters.

(F) Hygrometer, to measure the relative humidity of the laboratory environment.

(G) Temperature gauge, to measure the temperature of the laboratory environment.

(c) The following provisions apply to reagents:

(i) The reagents used in sampling are as follows:

(A) Filters. Two outstack filters may be any combination of alundum ceramic thimble

filters, type RA-98 or glass fiber filters, type A without organic binder. The size of the

filters must allow proper sampling rates to maintain isokinetics using the nozzle sizes

specified in subdivision (b)(i)(A) of this rule. Alternatively, other types of filters may be

used, subject to the approval of the department.

(B) Silica gel. Indicating type, 6 to 16 mesh. If previously used, dry at 175 degrees

Centigrade, 350 degrees Fahrenheit, for 2 hours. New silica gel may be used as received.

Alternatively, other types of desiccants, equivalent or better, may be used, subject to the

approval of the department.

(C) Water. When analysis of the material caught in the impingers is required, distilled

water must be used. Run blanks prior to field use to eliminate a high blank on test samples.

(D) Crushed ice.

(E) Stopcock grease. Acetone-insoluble, heatstable silicone grease. This is not

necessary if screw on connectors with Teflon sleeves, or equivalent, are used.

Alternatively, other types of stopcock grease may be used, subject to the approval of the

department.

(ii) Sample recovery, washing solvent. Either acetone or distilled water may be used for

sample recovery. If acetone is used for washing solvent, then reagent grade, less than

0.001% residue, in glass bottles is required. Acetone from metal containers generally has

a high residue blank and must not be used. Suppliers sometimes transfer acetone to glass

bottles from metal containers, so acetone blanks must be run before field use and only

acetone with low blank values, less than 0.001%, must be used. A blank value of more than

0.001% of the weight of acetone used must not be subtracted from the sample weight. If

distilled water is used for washing solvent, use distilled water with less than 0.001%

residue. Run blanks before field use to eliminate a high blank on test samples.

(iii) Two reagents are required for the analysis:

(A) Solvent. Same as paragraph (ii) of this subdivision for quantitative transfer.

(B) Desiccant. Anhydrous calcium sulfate, indicating type. Alternatively, other types of

desiccants may be used, subject to the approval of the department.

(d) The following provisions apply to procedure:

(i) Sampling. The complexity of this method is such that, in order to obtain reliable

results, testers shall be trained and experienced with the test procedures. Sampling must

comply with the following provisions:

(A) Pretest preparation. All the components must be maintained and calibrated

according to the applicable procedures described in APTD-0576, adopted by reference in

R 336.1902, unless otherwise specified in this rule. Weigh several 200 to 300 gram portions

of silica gel in airtight containers to the nearest 0.5 gram. Record the total weight of the

silica gel plus container on each container. As an alternative, the silica gel need not be pre-

weighed, but may be weighed directly in its impinger or sampling holder just before train

Page 39

assembly. Check filters visually against light for irregularities, flaws, pinhole leaks, or

cracks. Label filters of the proper size on the back side using numbering machine ink. As

an alternative, label the shipping containers, described in subdivision (b)(ii)(D) of this rule,

and keep the filters in these containers at all times, except during sampling and weighing.

Dry the filters in an oven at 105 degrees Centigrade, 220 degrees Fahrenheit, for a

minimum of 2 hours, cool for at least 1 hour in a desiccator containing anhydrous calcium

sulfate, and individually weigh and record each weight to the nearest 0.1 milligram. During

the weighing, the filters must not be exposed to the laboratory atmosphere for a period of

more than 2 minutes and a relative humidity above 50%. Procedures, other than those

specified, that account for relative humidity effects may be used, subject to the approval of

the department.

(B) Preliminary determinations. Select the sampling site and the minimum number of

sampling points according to method 1 or as specified by the department. Determine the

stack pressure, temperature, and the range of velocity heads using method 2. It is

recommended that a leak check of the pitot lines, see method 2, be performed. Determine

the moisture content using approximation method 4, or its alternatives, for the purpose of

making isokinetic sampling rate settings. Determine the stack gas dry molecular weight, as

described in method 2. If integrated method 3 sampling is used for molecular weight

determination, the integrated bag sample must be taken simultaneously with, and for the

same total length of time as, the particulate sample run. Select a nozzle size based on the

range of velocity heads so that it is not necessary to change the nozzle size in order to

maintain isokinetic sampling rates. During the run, do not change the nozzle size. Ensure

that the proper differential pressure gauge is chosen for the range of velocity heads

encountered, see method 2. Select a suitable probe liner and probe length so that all traverse

points can be sampled. For large stacks, consider sampling from opposite sides of the stack

to reduce the length of probes. Select a total sampling time greater than or equal to the

minimum total sampling time specified in the test procedures for the specific industry so

that the sampling time per point is not less than 5 minutes, unless approved by the

department, or some greater time interval as specified by the department, and so that the

sample volume taken, corrected to standard conditions, exceeds the required minimum total

gas sample volume. The latter is based on an approximate average sampling rate. It is

recommended that the number of minutes sampled at each point be an integer or an integer

plus 1/2 minute to avoid timekeeping errors. In some circumstances, such as in batch

cycles, it may be necessary to sample for shorter times at the traverse points and to obtain

smaller gas sample volumes. In these cases, the department's approval must first be

obtained.

(C) Preparation of collection train. During preparation and assembly of the sampling

train, keep all openings where contamination can occur covered until just before assembly

or until sampling is about to begin. Place 100 milliliters of water in the first impinger, leave

the second impinger empty, and transfer approximately 200 to 300 grams of pre-weighed

silica gel from its container to the third impinger. More silica gel may be used, but care

should be taken to ensure that it is not entrained and carried out from the impinger during

sampling. Place the container in a clean place for later use in the sample recovery.

Alternatively, the weight of the silica gel plus impinger may be determined to the nearest

0.5 gram and recorded. Using tweezers or clean disposable surgical gloves, place a labeled,

identified, and weighed filter in the filter holder. Be sure that the filter is properly centered

Page 40

and the gasket properly placed so as to prevent the sample gas stream from circumventing

the filter. Check the filter for tears after assembly is completed. When glass liners are used,

install the selected nozzle using a Viton A O-ring when stack temperatures are less than

260 degrees Centigrade, 500 degrees Fahrenheit, and a heat-resistant fiberglass, graphite,

or other material string gasket when temperatures are higher. See APTD-0576, adopted by

reference in R 336.1902, for details. Other connecting systems using either 310 stainless

steel or Teflon ferrules may be used. When metal liners are used, install the nozzle in the

same manner as for glass liners or by a leak-free direct mechanical connection. Mark the

probe with heat-resistant tape or by some other method to denote the proper distance into

the stack or duct for each sampling point. Set up the train as in figure 103 under R 336.2021.

If necessary, use a very light coat of silicone grease on all ground glass joints. Grease only

the outer portion, see APTD-0576, adopted by reference in R 336.1902, to avoid the

possibility of contamination by the silicone grease. Place crushed ice around the impingers.

(D) Leak check procedures as follows:

(I) Pretest leak check. A pretest leak check is strongly recommended, but not required,

to prevent invalid sampling and wasted time. If the tester opts to conduct the pretest leak

check, the following procedure must be used: After the sampling train has been assembled,

turn it on and set the filter and probe heating systems at the desired operating temperatures.

Allow time for the temperatures to stabilize. If a Viton A O-ring or other leak-free

connection is used in assembling the probe nozzle to the probe liner, leak check the train

at the sampling site by plugging the nozzle and pulling a 380 millimeter mercury, 15 inch

mercury, vacuum. A lower vacuum may be used, if it is not exceeded during the test. If a

heat-resistant fiberglass, graphite, or other material string is used, do not connect the probe

to the train during the leak check. Instead, leak check the train by first plugging the inlet to

the filter holder, and cyclone, if applicable, and pulling a 380 millimeter mercury, 15 inch

mercury, vacuum. A lower vacuum may be used if it is not exceeded during the test. Then

connect the probe to the train and leak check at about a 25 millimeter mercury, 1 inch

mercury, vacuum. Alternatively, the probe may be leak checked with the rest of the

sampling train, in 1 step, at a 380 millimeter mercury, 15 inch mercury, vacuum. Leakage

rates in excess of 4% of the average sampling rate or 0.00057 cubic meters per minute

(0.02 cubic feet per minute), whichever is less, are unacceptable. The following leak check

instructions for the sampling train described in APTD-0576 and APTD-0581 may be

helpful. Start the pump with the bypass valve fully open and the coarse adjust valve

completely closed. Partially open the coarse adjust valve and slowly close the bypass valve

until the desired vacuum is reached. Do not reverse the direction of the bypass valve, as

this will cause water to back up into the filter holder. If the desired vacuum is exceeded,

either leak check at this higher vacuum or end the leak check and start over. When the leak

check is completed, first slowly remove the plug from the inlet to the probe, filter holder,

or cyclone, if applicable, and immediately turn off the vacuum pump. This prevents the

water in the impingers from being forced backward into the filter holder and prevents silica

gel from being entrained backward into the third impinger.

(II) Leak checks during sample run. If, during the sampling run, a component, such as

a filter assembly or impinger, change becomes necessary, a leak check must be conducted

immediately before the change is made. The leak check must be done according to the

procedure outlined in subparagraph (D) (I) of this paragraph, except that it must be done at

a vacuum equal to or greater than the maximum value recorded up to that point in the test.

Page 41

If the leakage rate is found to be not more than 0.00057 cubic meters per minute, 0.02 cubic

feet per minute, or 4% of the average sampling rate, whichever is less, the results are

acceptable and no correction need be applied to the total volume of dry gas metered. If,

however, a higher leakage rate is obtained, the tester shall either record the leakage rate

and plan to correct the sample volume, as shown in subdivision (f)(iii) of

R 336.2011, or shall void the sampling run. Immediately after component changes, leak

checks are optional. If the leak checks are done, the procedure outlined in paragraph

(i)(D)(I) of this subdivision must be used.

(III) Post-test leak check. A leak check is mandatory at the conclusion of each sampling

run. The leak check must be done in accordance with the procedures outlined in paragraph

(i)(D)(I) of this subdivision, except that it must be conducted at a vacuum equal to or

greater than the maximum value reached during the sampling run. If the leakage rate is

found to be not more than 0.00057 cubic meters per minute, 0.02 cubic feet per minute, or

4% of the average sampling rate, whichever is less, the results are acceptable and no

correction need be applied to the total volume of dry gas metered. If, however, a higher

leakage rate is obtained, the tester shall either record the leakage rate and correct the sample

volume, as shown in subdivision (f)(iii) of R 336.2011, or shall void the sampling run.

(E) Particulate train operation. During the sampling run, maintain an isokinetic

sampling rate that is within 10% of true isokinetic, unless otherwise specified by the

department. For each run, record the data required on a data sheet such as the one shown

in figure 104 under R 336.2021. Be sure to record the initial dry-gas meter reading. Record

the dry-gas meter readings at the beginning and end of each sampling time increment, when

changes in flow rates are made, before and after each leak check, and when sampling is

halted. Take other readings required by figure 104 under R 336.2021 at least once at each

sample point during each time increment, and take additional readings when significant

changes, 20% variation in velocity head readings, necessitate additional adjustments in

flow rate. Level and zero the manometer. Because the manometer level and zero may drift

due to vibrations and temperature changes, make periodic checks during the traverse. Clean

the portholes before the test run to minimize the chance of sampling deposited material. To

begin sampling, remove the nozzle cap and verify that the pitot tube and probe are properly