DEPARTMENT OF ENVIRONMENTAL QUALITY

AIR QUALITY DIVISION

AIR POLLUTION CONTROL

(By authority conferred on the director of the department of environmental quality

by sections 5503 and 5512 of 1994 PA 451, MCL 324.5503 and 324.5512, and

Executive Reorganization Order No. 1995-18, MCL 324.99903)

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 any 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 1 of the following conditions:

(a) Prior to issuance of a permit to operate.

(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 that the source is in

compliance with the department's rules and with the conditions specified in the permit to

install.

(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 such

designated attainment pollutants.

(f) After completion of a compliance program.

(2) Performance tests required by subrule (1) of this rule shall be conducted

within 60 days following receipt of written notification from the department, unless

otherwise authorized by the department.

(3) For a performance test required by subrule (1) of this rule, the owner or operator

shall submit a site-specific test plan not less than 30 days before a performance test for

approval of the department. The plan will include test program summary, test

schedule, and the quality assurance measures to be applied.

(4) Not less than 7 days before performance tests are conducted, the owner of a

source of air contaminant, or his or her authorized agent, shall notify the department, in

writing, of the time and place of the performance tests and who shall conduct them. A

representative of the department shall have the opportunity to witness these tests.

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(5) Results of performance tests shall 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; 2002 AACS; 2009 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 shall be conducted and data reduced

according to the reference test methods listed in

does any of the following:

R

336.2004, unless the department

(a) Specifies or approves, in specific cases, the use of

with minor changes in procedures or equipment.

(b) Approves the use of an equivalent method.

a

reference test 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) A performance test shall consist of a minimum of 3 separate samples of a

specific air contaminant conducted within a 36-hour period, unless otherwise

authorized by the department. Each of the 3 separate samples shall be obtained while

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the source is operating at a similar production level. For the purpose of determining

compliance with an applicable emission limit, rule, or permit condition, the arithmetic

mean of results of the 3 samples shall 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 shall be conducted while the source

contaminant is operating at maximum routine operating conditions, or under such

other conditions, within the capacity of the equipment, as may be requested by the

department. Other conditions may include source operating periods of startup,

of air

shutdown, or such other operations, excluding malfunction, specific to certain

sources. Routine operating conditions shall also include those specified within a permit

to install or a permit to operate. The owner or operator shall make available to the

department such records as may be necessary to determine the conditions of source

operation that occurred during the period of time of the performance test.

(4) For any source that is subject to an emission limitation calculated to 50%

excess air, the multipoint, integrated sampling procedure of method 3 shall be used for

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

weight of the exhaust, any optional sampling procedure of method 3 may be

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

department.

(5) For reference test methods 5B and 5C, the minimum volume per sample shall

be 30 cubic feet of dry gas corrected to standard conditions (70 degrees Fahrenheit,

29.92 in. Hg.). Minimum sample time shall 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.

R 336.2004 Appendix A; reference test methods; adoption of federal reference

test methods.

Rule 1004. (1) The following federal reference test methods, described in the

provisions of 40 C.F.R. part 60, appendix A (2007), are the reference test methods

for performance tests required pursuant to the provisions of this part:

(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).

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(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 reference test methods listed in subrule (1) of this rule are adopted by

reference in this rule. Copies of the test methods may be inspected at the Lansing

office of the air quality division of the department of environmental quality. A copy

of title 40 of the Code of Federal Regulations, part 60, appendix A, may be obtained

from the Department of Environmental Quality, Air Quality Division, P.0. Box

30260, Lansing, Michigan 48909 7760, at a cost at the time of adoption of these rules

of $67.00; from the Superintendent of Documents, United States Government

Printing Office, P.O. Box 979050, St. Louis, Missouri 63197-9000, at a cost at the

time of adoption of these rules of $57.00; or on the United States government printing

office internet web site at http://www.gpoaccess.gov.

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(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 shall be conducted as specified in reference test method 9 or other

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

(a) Visible emissions from a scarfing operation at

a

steel manufacturing

facility shall 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 shall be determined as specified in reference test method 9B,

which is described in R 336.2031.

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

operations, hot metal transfer operations, and hot metal desulfurization operations

shall be determined as specified in reference method 9C, which is described in R

336.2032.

(5) Determinations of particulate emission rates for stationary sources shall

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," (14th

edition), section 208C, as described and modified in R 336.2033.

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

using the alternate version of federal reference test method 25 incorporating the

Byron analysis, shall 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.

R 336.2005 Reference test methods for staterequested 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:

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(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

associated sampling line and probe which complies with all of

provisions:

gas

analyzer with

the following

(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).

(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.

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:

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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 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

chromatograph (GC). (Remainder of 2.3 as stated in method 25)

401

gas

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.

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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 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

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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).

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

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FIGURE 25.1

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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.

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

0.2 lb.

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.

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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.

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.

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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.

(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.

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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.

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.

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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.

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

) ( )

T _MP_STD

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Where:

B_v

M_v

= Bag sample volume in standard liters.

= Indicated dry gas meter volume, in liters.

T_STD= 293⁰K.

T_M

P_M

= Meter gas temperature, in ⁰K.

= Meter gas pressure, in mm Hg absolute.

P_STD= 760 mm Hg.

6.2

6.3

Bag sample voc concentration, as voc, C_voc.

C_voc= M_l/B_v

Where:

C_voc= Bag sample voc concentration, as voc, mg/std. liters.

M_l

= Weight of voc liquid injected, mg.

Bag sample voc concentration, as propane, C_c3.

C_c3= R_c3*K

Where:

C_c3

R_c3

= Bag sample voc concentration, as propane, mg C₃/std. liter.

= 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.

V_IJ= Initial voc weight fraction of voc liquid J.

V_FJ= Final voc weight fraction of voc liquid J.

V_AJ= Voc weight fraction of voc liquid J added during the test.

W_IJ= Weight of voc containing liquid J at beginning of test, kg.

W_FG= Weight of voc containing liquid J at end of test, kg.

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W_AJ= Weight of voc containing liquid J added during the test, kg.

RF_J= Response factor for voc in liquid J, weight voc/weight propane.

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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:

(A) A performance test shall consist of a minimum of 3 separate samples of a

specific air contaminant conducted within a 36-hour period, unless otherwise

authorized by the department. Each of the 3 separate samples shall be obtained while the

source is operating at a similar production level. For the purpose of determining

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compliance with an applicable emission limit, rule, or permit condition, the arithmetic

mean of results of the 3 samples shall 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, compliance may, upon the approval of the department, be determined using the

arithmetic mean of the results of 2 samples.

(B) For any source that is subject to an emission limitation calculated to 50%

excess air, the multipoint, integrated sampling procedure of R 336.2004(1)(c) shall

be used for gas analysis. For all other sources that require a determination of the

molecular weight of the exhaust, any 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 shall be 30 cubic feet of dry gas

corrected to standard conditions (70 degrees Fahrenheit, 29.92 inches mercury).

Minimum sample time shall 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 any source whose emission control device alters the moisture content of

the exhaust gas, a moisture determination shall 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. Construction details for many, but not all, of the train components are

given in APTD-0581. (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. (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 herein. The sampling train shall consist of the

following components:

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

The angle of taper shall be less than 30 degrees and the taper shall be on the outside to

preserve a constant internal diameter. The probe nozzle shall be of the button-hook

design, unless otherwise specified by the department. If made of stainless steel, the

nozzle shall be constructed from seamless tubing. Other materials of construction may be

used, subject to the approval of the department. A range of nozzle sizes suitable for

isokinetic sampling shall be available, for example, 0.32 to 1.27 cm (1/8 to 1/2 in. or

larger if higher volume sampling trains are used inside diameter (ID) nozzles in

increments of 0.16 cm (1/16 in.). Each nozzle shall be calibrated according to the

procedures outlined in subdivision (e) of this rule.

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

grade), glass, teflon, or such other material that maintains proper flow at the stack

conditions experienced.

(C) Pitot tube. Type S, as described in section 2.1 of method 2, or other device

approved by the department. The pitot tube shall be attached to the probe, as shown in

figure 102, to allow constant monitoring of the stack gas velocity. The impact (high

pressure) opening plane of the pitot tube shall be even with or above the nozzle entry

plane (see method 2, figure 2-6b) during sampling. The type S pitot tube assembly

shall have a known coefficient, determined as outlined in section 4 of method 2.

(D) Differential pressure gauge. Incline manometer or equivalent devices (2) as

described in section 2.2 of method 2. One manometer shall be used for velocity head (p)

readings and the other shall 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 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 shall 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 noncontaminating fittings. All impingers shall be of the

Greenburg-Smith design and shall be modified by replacing the tip with a 1.3 cm (1/2 in.)

ID glass tube extending to about 1.3 cm (1/2 in.) from the bottom of the flask.

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

materials other than glass, are permitted, subject to the approval of the department. The

first impinger shall contain a known quantity of water (subdivision (d)(i)(C) of this

rule); the second shall be empty; and the third shall contain a known weight of silica gel

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

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

within 1 ml or 1 g, may be used, subject to the approval of the department. In any

case, the means for measuring the moisture leaving the condenser shall 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 shall 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. 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 shall enable checks of isokinetic rates.

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Sampling trains utilizing metering systems designed for higher flow rates than

those described in APTD-0581 or APTD-0576 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 mm Hg (0.1 in. Hg). 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, shall be requested and an

adjustment for elevation differences between the weather station and sampling point

shall be applied at a rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 M (100 ft.) elevation

increase or vice versa for elevation decrease.

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

as described in sections 2.3 and 2.4 of method 2, and gas analyzer, if necessary, as

described in method 3. The temperature sensor shall, preferably, be permanently

attached to the pitot tube or sampling probe in a fixed configuration such that the tip of

the sensor extends beyond the leading edge of the probe sheath and does not

touch any metal. Alternatively, the sensor may be attached just before use in the field.

If the temperature sensor is attached in the field, then the sensor shall 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, 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 this rule. Copies of these documents may be inspected at the

Lansing office of the air quality division of the department of environmental quality.

Copies of APTD-0581 and APTD-0576 may be obtained from the Department of

Environmental Quality, Air Quality Division, P.O. Box 30260, Lansing, Michigan

48909-7760, or from the National Technical Information Service, U.S. Department

of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161, at a cost at the time

of adoption of these rules of $28.50 each.

(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 shall have extensions, at least as long as the

probe, made of stainless steel, nylon, teflon, or similarly inert material. The brushes

shall be properly sized and shaped to brush out the probe liner and nozzle.

(B) Wash bottles 2. 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, 500 ml or 1000 ml. Screw cap liners shall either be rubber-

backed teflon or shall be constructed so as to be leak-free and resistant to chemical attack

by acetone. Narrow-mouth glass bottles 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.

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

g., graduated cylinders shall have subdivisions of not more than 2 ml. Most laboratory

balances are capable of weighing to the nearest 0.5 g 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;

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 mg.

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

(E) Beakers. 250 ml.

(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 shall 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 such filters shall 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 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 shall 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 shall not be used. If suppliers transfer acetone to

glass bottles from metal containers, then acetone blanks shall be run before field use and

only acetone with low blank values (less than 0.001%) shall be used. In no case shall 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

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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 shall 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 shall comply with the following provisions:

(A) Pretest preparation. All the components shall be maintained and calibrated

according to the applicable procedures described in APTD-0576, unless otherwise

specified in this rule. Weigh several 200 to 300 g portions of silica gel in airtight

containers to the nearest 0.5 g. 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. 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 (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 their weights to the nearest 0.1 mg.

During the weighing, the filter shall 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, section

3.1) be performed. Determine the moisture content using approximation method 4, or its

alternatives, for the purpose of making isokinetic sampling rate settings. Determine

the stack gas dry molecular weight, as described in method 2, section 3.6; if integrated

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

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

particulate sample run. 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 section 2.2

of method 2).

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.

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

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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 shall 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 ml of water in the first

impinger, leave the second impinger empty, and transfer approximately 200 to 300 g of

preweighed silica gel from its container to the third impinger. More silica gel may be

used, but care shall be taken to ensure that it is not entrained and carried out from the

impinger during sampling. Place the container in a clean place for later use in the sample

recovery. Alternatively, the weight of the silica gel plus impinger may be determined

to the nearest 0.5 g and recorded. 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. Install the selected nozzle using a Viton A 0-ring

when stack temperatures are less than 260 degrees Centigrade (500 degrees Fahrenheit)

and an asbestos string gasket when temperatures are higher. See APTD-0576 for

requirements. Other connecting systems using either 310 stainless steel or teflon ferrules

may be used to form 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 102. 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.

Place crushed ice around the impingers.

(D) Leak check procedures:

(1) 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 shall be used: Perform the leak check on the

entire system, including filter housings and nozzle, by plugging the nozzle and pulling a

380 mm Hg (15 in. Hg) 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 m³/min (0.02 cfm), 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; 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

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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.

(2) 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 shall be

conducted immediately before the change is made. The leak check shall be done

according to the procedure outlined in paragraph (i)(D)(1) of this subdivision, except

that it shall be done at a vacuum equal to or greater than the maximum value recorded up

to that point in the test.If the leakage rate is not more than 0.00057 m³/min (0.02 cfm) 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 shall 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)(1) of this subdivision shall be used.

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

sampling run. The leak check shall be performed in accordance with the procedures in

paragraph (i)(D)(1) of this subdivision, except that it shall be conducted at a vacuum

equal to or greater than the maximum value reached during the sampling run. If the

leakage rate is not more than 0.00057 m³/min (0.02 cfm) 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 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 data

sheet in figure 104. 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 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 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 (subdivision (g)(iv) of this rule)

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

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pressure (height of impinger stem), take care to pull lowflow 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 (paragraph (i)(D)(2) of this

subdivision). The total particulate weight shall include the summation of all filter

assembly catches. A single train shall 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 shall 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 shall 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)(3) of this subdivision. Leak-check the pitot lines as described in method 2,

section 3.1; the lines shall 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

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contamination during disassembly. Transfer the nozzle-filter set assembly and impinger

set to the cleanup area. The cleanup area shall 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 ml 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 Nos. 1, 1A. Carefully remove the

filters from the filter holders and place in their identified containers. 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 No. 2. Taking care to see that particulate on the

outside of the nozzle and filter holders does not get into the sample, the testor 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 testor shall 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 No. 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 No. 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 ml by

using a graduated cylinder or by weighing it to within ±1.0 g by using a balance if one

is available. Record the volume or weight of liquid present. This information is required

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

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

(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 shall 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.

Handle each sample container in the following manner: Container Nos. 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

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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 mg. During the weighing the filter shall 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 shall be consistent before and after the test. Container No.

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 ml

or gravimetrically to ±1.0 g. Transfer the contents to a tared 250 ml 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 mg. Container No. 3. Weigh the spent silica gel, or silica gel plus

impinger, to the nearest 0.5 g using a balance. This step may be conducted in the field.

"Solvent blank" container. Measure solvent in this container either volumetrically or

gravimetrically. Transfer the contents to a tared 250 ml 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 mg. If

acetone is used, the contents of Container No. 2, as well as the acetone blank container,

may be evaporated at temperatures higher than ambient. If evaporation is done at an

elevated temperature, then the temperature shall be closely supervised, and the

contents of the beaker shall 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

shall comply with the following provisions:

(i) Probe nozzle. Probe nozzles shall be calibrated before their initial use in the

field. Using a micrometer, measure the inside diameter of the nozzle to the nearest

0.025 mm (0.001 in.). Make 3 separate measurements using different diameters each

time and obtain the average of the measurements. The difference between the high and

low numbers shall not exceed 0.1 mm (0.004 in.). When nozzles become nicked,

dented, or corroded, they shall be reshaped, sharpened, and recalibrated before use.

Each nozzle shall be permanently and uniquely identified.

(ii) Pitot tube. The type S pitot tube assembly shall be calibrated according to

the procedures in section 4 of method 2.

(iii) Metering system. Before its initial use in the field, the metering system shall

be calibrated according to the procedure in APTD-0576. 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

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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 m³/min (0.02

cfm); at the end of the run, take the difference of the measured wet-test meter and

dry-gas meter volumes; divide the difference by 10 to get the leak rate. The leak rate

shall not exceed 0.00057 m³/min (0.02 cfm). After each field use, the calibration of the

metering system shall 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 shall be performed using whichever meter coefficient value

(before or after) gives the lower value of total sample volume.

(iv) Temperature gauges. Use the procedure in section 4.3 of method 2 to calibrate

in-stack temperature gauges. Dial thermometers, such as those used for the dry-gas meter

and condenser outlet, shall be calibrated against mercury-in-glass thermometers.

(v) Leak check of metering system shown in figure 102. That portion of the

sampling train from the pump to the orifice meter shall 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 (see figure

107): 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 cm (5 to 7 in.) 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, shall 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 they give equivalent results. The

following provisions apply to calculations:

(i) Nomenclature:

A_n= Cross-sectional area of nozzle, m²(ft.²).

A = Cross-sectional area of stack or flue at the point of sampling, ft².

B

= Water vapor in the gas stream, proportion by volume, expressed as a

ws

fraction.

B

= Percent water vapor in gas entering source particulate control device

wi

determined by method 4.

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B

_wo= Percent water vapor in gas exiting source particulate control device.

C_a= Wash blank residue concentration, mg/g.

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, lb/hr.

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 m³/min (0.02 cfm) or 4% of the

average sampling rate, whichever is less.

L_i= Individual leakage rate observed during the leak check conducted

before the "ith" component change (i = 1, 2, 3 . . . . n), m³/min (cfm).

L_p= Leakage rate observed during the post-test leak check, m³/min (cfm).

M_d= Molecular weight of dry stack gas, g/g mole (lb/lb-mole), calculated

by method 3, equation 3-2, using data from integrated method 3.

m_n= Total amount of particulate matter collected, mg.

M_w= Molecular weight of water, 18.0 g/g-mole (18.0 lb/lb-mole).

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m_a= Mass of residue of solvent after evaporation, mg.

m_g= Total weight of gas samples through nozzle, lb.

P _bar= Barometric pressure at the sampling site, mm Hg (in. Hg).

P_s= Absolute stack gas pressure.

P_std= Standard absolute pressure, 760 mm Hg (29.92 in. Hg).

R

=

Ideal gas constant, 0.06236 mm Hg-m³/°K-g-mole (21.85 in.Hg-

ft.³/°R?lb-mole).

T _m= Absolute average dry-gas meter temperature (see figure 104), °K (°R).

T_s= Absolute average stack gas temperature (see figure 104), °K (°R).

T_std= Standard absolute temperature, 294.I°K (530°R).

V _a= Volume of solvent blank, ml.

V _aw= Volume of solvent used in wash, ml.

V _lc= Total volume of liquid collected in impingers and silica gel (see figure 106),

ml.

V_m= Volume of gas sample as measured by the dry-gas meter, dcm (dcf).

V

= Volume of gas sample measured by the dry-gas meter, corrected to

m(std)

standard conditions, dscm (dscf).

V

=

Volume of water vapor in the gas sample, corrected to standard

w(std)

conditions, scm (scf).

V _s= Stack gas velocity, calculated by method 2, equation 2-9, using data obtained

from method 5, m/sec (ft./sec).

W_a= Weight of residue in solvent wash, mg.

Y = Dry-gas meter calibration factor.

ΔH = Average pressure differential across the orifice meter (see figure 104), mm

H20 (in. H20).

%0₂= Percent oxygen in stack gas by volume (dry basis).

%N₂= Percent nitrogen in stack gas by volume (dry basis).

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p _a= Density of solvent, mg/ml.

p _s(std)= Density of all sampled gas at standard conditions, lb/ft.³

p_w= Density of water, 0.9982 g/ml (0.002201 lb/ml).

θ = Total sample time, min.

θ1 = Sample time, interval, from the beginning of a run until the first component

change, min.

θi = Sampling time interval, between 2 successive component changes,

beginning with the interval between the first and second changes, min.

θp = Sampling time interval, from the final (nth) component change until the end

of the sampling run, min.

13.6 = Specific gravity of mercury.

60 = Sec/min.

100 = Conversion to percent.

386.9 = Cubic feet per lb-mole of ideal gas at standard conditions.

453.6 = Conversion of pounds to grams.

3600 = Conversion of hours to sec.

1000 = Conversion of 1000 lb units to lb units.

(ii) Average the dry-gas meter temperature and average the orifice pressure

drop. See data sheet (figure 5-2).

(iii) Dry gas volume. Correct the sample volume measured by the dry-gas meter

to standard conditions (21.11 degrees Centigrade, 760 mm Hg or 70 degrees

Fahrenheit, 29.92 in. Hg) 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.

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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 shall be modified in the following manner:

(A) Case I. No component changes made during sampling run. In this

case, replace V_min 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

equation 5-3

=

( p_w/

) (R

/

) =

V _w(std)

V_1c

M_w

T_stdP_stdK₂V_1c

Where:

K₂= 0.001338 m³/ml for metric units.

(v) Moisture content.

=

/ (

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 shall 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_wsshall be considered correct. The procedure for

determining the moisture content based upon assumption of saturated conditions is

given in the note of section 1.2 of method 4. For the purpose of this method, the

average stack gas temperature from figure 104 may be used to make the

determination, if the accuracy of the instack temperature sensor is ±1 degree

Centigrade (2 degrees Fahrenheit).

(vi) Solvent blank concentration.

equation 5-4

=

/ (

)

C_a

m_aV _aP_a

(vii) Solvent wash blank.

equation 5-5

=

W_a

C_aV _awP_a

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(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). 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 (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).

equation 5-7

equation 5-8

= (

+

V _w(std)

) p

s(std)

m_g

V _m(std)

(xi) Particulate concentration (lbs/1000 lbs).

=

/ (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

any 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

(C) Correction factor to convert the actual concentration, C_s, to dry

conditions.

0₂

M_d

B_wi

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.

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equation 5-12

equation 5-13

equation 5-14

=

C_s50

C_s50D

C_sD

C_sF₅₀

C_sF_50D

C_sF_D

(xiv) Mass emission rate (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:

(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

60(1-

T_sV _m(std)

 (1-

I =

=

K₅



)

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 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.

Page 36

Courtesy of www.michigan.gov/orr

(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.

R 336.2012 Reference test method 5C.

Rule 1012. Reference test method 5C, outstack 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 a temperature in the range of 120 ±14

degrees Centigrade (248 ±25 degrees Fahrenheit) or such other 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.