DEPARTMENT OF ENVIRONMENT, GREAT LAKES, AND ENERGY

AIR QUALITY DIVISION

AIR POLLUTION CONTROL

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

and energy by sections 5503 and 5512 of the natural resource and environmental

protection act, 1994 PA 451, MCL 324.5503 and 324.5512, and Executive

Reorganization Order Nos. 1995-16, 2009-31, 2011-1, 2019-1, MCL 324.99903,

324.99919, 324.99921, and 324.99923)

PART 10. INTERMITTENT TESTING AND SAMPLING

R 336.2001 Performance tests by owner.

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

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

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

(a) Reserved.

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

emissions exceed 100 tons per year.

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

performance test, in accordance with R 336.2003, that demonstrates the source complies

with either the department's rules or the conditions specified in the permit to install, or

both.

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

for 1 or more air pollutants, and more than 12 months have expired since the date of the

last performance test for such designated nonattainment pollutants.

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

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

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

attainment pollutants.

(f) After completion of a compliance program.

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

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

authorized by the department.

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

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

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

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

applied.

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

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

Page 1

Courtesy of Michigan Administrative Rules

subdivision (a) of this subrule. A representative of the department shall have the

opportunity to witness these tests.

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

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

test.

History: 1980 AACS; 2002 AACS; 2009 AACS; 2025 MR 17, Eff. Sept. 10, 2025.

R 336.2002 Performance tests by department.

Rule 1002. (1) The department may conduct performance

tests

in

accordance with R 336.2003 at any source of air contaminant, on behalf of the state, at

a reasonable time and at the state's expense. During the conduct of such tests, the

department may obtain samples of any air contaminant and samples of any material

entering or exiting the source or aircleaning device for the purpose of evaluating

pollutant emissions with respect to process operating conditions.

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

of a source of the department's intent to conduct performance tests pursuant to

subrule (1). Within 30 days of receipt of such notification, the owner or operator

shall provide, and bear the expense of, performance test facilities as specified by the

department, including the following:

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

(b) Safe sampling platforms as required.

(c) Safe access to sampling platforms.

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

designated by the department. Upon request, additional time for installing the required

performance test facilities may be authorized by the department for special situations.

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

and sensing devices.

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

both, in the format prescribed by the applicable reference test method within 60 days

following the last date of the test.

History: 1980 AACS; 2002 AACS.

R 336.2003 Performance test criteria.

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

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

following:

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

minor changes in procedures or equipment.

(b) Approves the use of an equivalent method.

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

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

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

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

Page 2

Courtesy of Michigan Administrative Rules

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

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

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

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

an applicable emission limit, rule, or permit condition, the arithmetic mean of results of

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

of the 3 samples must be discontinued because of forced shutdown, failure of an

irreplaceable portion of the sampling train, extreme meteorological conditions, or other

circumstances beyond the owner's or operator's control, then compliance may, upon the

approval of the department, be determined using the arithmetic mean of the results of 2

samples.

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

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

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

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

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

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

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

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

test.

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

air, the multipoint, integrated sampling at every traverse point must be used with method

3, 3A, or 3Bfor gas analysis. For all other sources that require a determination of the

molecular weight of the exhaust, an optional sampling procedure of method 3, 3A, or 3B

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

the department.

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

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

described in R 336.1014, the minimum volume per sample must be 30 cubic feet of dry

gas corrected to standard conditions, 68 degrees Fahrenheit, 29.92 inches mercury.

Minimum sample time must be 60 minutes, which may be continuous or a combination

of shorter sampling periods for sources that operate in a cyclic manner. Smaller sampling

times or sample volumes, when necessitated by process variables or other factors, may be

approved by the department.

History: 1980 AACS; 2002 AACS; 2025 MR 17, Eff. Sept. 10, 2025.

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

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

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

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

the following:

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

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

stacks or ducts.

Page 3

Courtesy of Michigan Administrative Rules

(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).

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

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

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

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

sources.

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

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

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

from stationary sources.

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

sources.

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

sources.

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

sources.

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

chromatography.

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

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

volume solids, and weight solids of surface coatings.

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

inks and related coatings.

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

carbon.

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

flame ionization analyzer.

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

pressure-vacuum test.

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

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

stationary sources (instrumental analyzer procedure).

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

fired combustion sources using carbon sorbent traps.

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

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

this part:

(a) 40 CFR part 51, appendix M.

(b) 40 CFR part 61, appendix B.

(c) 40 CFR part 63, appendix A.

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

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

Page 4

Courtesy of Michigan Administrative Rules

() Determinations of compliance with visible emission standards for stationary

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

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

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

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

R 336.2030.

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

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

described in R 336.2031.

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

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

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

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

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

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

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

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

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

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

edition), as described and modified in R 336.2033.

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

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

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

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

AACS; 2009 AACS; 2025 MR 17, Eff. Sept. 10, 2025.

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:

(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.

Page 5

Courtesy of Michigan Administrative Rules

(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:

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

Page 6

Courtesy of Michigan Administrative Rules

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.

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

Page 7

Courtesy of Michigan Administrative Rules

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

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.

Page 8

Courtesy of Michigan Administrative Rules

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

Page 9

Courtesy of Michigan Administrative Rules

FIGURE 25.1

History: 1993 AACS.

R 336.2007 Alternate version of procedure L, referenced

336.2040(10).

in R

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.

Page 10

Courtesy of Michigan Administrative Rules

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.

Page 11

Courtesy of Michigan Administrative Rules

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.

Page 12

Courtesy of Michigan Administrative Rules

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.

Page 13

Courtesy of Michigan Administrative Rules

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.

Page 14

Courtesy of Michigan Administrative Rules

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

Page 15

Courtesy of Michigan Administrative Rules

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.

Page 16

Courtesy of Michigan Administrative Rules

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.

Page 17

Courtesy of Michigan Administrative Rules

History: 1993 AACS; 2002 AACS.

R 336.2010 Rescinded.

History: 1985 AACS; 1992 AACS; 1997 AACS.

R 336.2011 Reference test method 5B.

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

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

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

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

mass is determined gravimetrically after removal of uncombined water.

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

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

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

to install, or a permit to operate.

(iii) Performance test criteria as follows:

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

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

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

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

Page 18

Courtesy of Michigan Administrative Rules

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

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

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

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

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

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

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

department.

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

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

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

method approved by the department.

(b) The following provisions apply to apparatus:

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

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

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

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

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

operating and maintenance procedures for many, but not all, of the sampling train are

described in APTD-0576, adopted by reference in R 336.1902. See subdivision (g)(iii) of

this rule. Since correct usage is important in obtaining valid results, all users shall read

APTD-0576 and adopt the applicable operating and maintenance procedures outlined in

it, unless otherwise specified. The sampling train must consist of the following

components:

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

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

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

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

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

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

isokinetic sampling must be available, for example, 0.32 to 1.27 centimeters, 1/8 to 1/2

inch, or larger if higher volume sampling trains are used inside diameter nozzles in

increments of 0.16 centimeters, 1/16 inches. Each nozzle must be calibrated according to

the procedures outlined in subdivision (e) of this rule.

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

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

experienced.

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

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

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

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

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

have a known coefficient, determined as outlined in method 2.

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

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

the other must be used for orifice differential pressure readings.

Page 19

Courtesy of Michigan Administrative Rules

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

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

contact with each other is not acceptable. Materials of construction may be stainless steel

316, glass, Teflon, or other material approved by the department.

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

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

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

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

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

or similar leak-free noncontaminating fittings. All impingers must be of the Greenburg-

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

inside diameter glass tube extending to about 1.3 centimeters, 1/2 inch, from the bottom

of the flask. Modifications, such as using flexible connections between the impingers or

using materials other than glass, are allowed, subject to the approval of the department.

The first impinger must contain a known quantity of water, as described in subdivision

(d)(i)(C) of this rule. The second impinger must be empty, and the third must contain a

known weight of silica gel or equivalent desiccant. Alternatively, a system that cools the

sample gas stream and allows measurement of the water condensed and moisture leaving

the condenser, each to within 1 milliliter or 1 gram, may be used, subject to the approval

of the department. In any case, the means for measuring the moisture leaving the

condenser must be by passing the sample gas stream through a tared silica gel, or

equivalent desiccant, trap with exit gases kept below 20 degrees Centigrade, 68 degrees

Fahrenheit, and determining the weight gain. If a determination of the particulate matter

collected in the impingers is required by the department’s rules, a permit to install, or a

permit to operate, then the impinger system described above must be used without

modification. Contact the department as to the sample recovery and analysis of the

impinger contents.

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

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

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

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

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

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

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

Sampling trains utilizing metering systems designed for higher flow rates than those

described in APTD-0581 or APTD-0576, both adopted by reference in R 336.1902, may

be used if the specifications of this method are met.

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

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

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

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

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

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

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

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

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

Page 20

Courtesy of Michigan Administrative Rules

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

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

leading edge of the probe sheath and does not touch any metal. Alternatively, the sensor

may be attached just before use in the field. If the temperature sensor is attached in the

field, then the sensor must be placed in an interference-free arrangement with respect to

the type S pitot tube openings, see method 2, figure 2-6 Velocity Traverse Data. As a

second alternative, if a difference of not more than 1% in the average velocity

measurement is to be introduced, then the temperature gauge need not be attached to the

probe or pitot tube. This alternative is subject to the approval of the department.

“Construction Details of Isokinetic Source Sampling Equipment,” APTD-0581, April

1971, PB203-060-LL, and “Maintenance, Calibration, and Operation of Isokinetic Source

Sampling Equipment,” APTD-0576, March 1972, PB209-022-LL, are adopted by

reference in R 336.1902.

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

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

steel wire handles. The probe brush must have extensions, at least as long as the probe,

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

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

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

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

for longer than 1 month.

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

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

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

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

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

otherwise specified by the department.

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

milliliter or 1 gram, graduated cylinders must have subdivisions of not more than 2

milliliters. Most laboratory balances are capable of weighing to the nearest 0.5 gram or

less. Any of these balances may be used here and in paragraph (iii)(D) of this

subdivision.

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

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

but not necessary if silica gel is weighed in the field.

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

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

(A) Glass weighing dishes.

(B) Desiccator.

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

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

(E) Beakers. 250 milliliters.

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

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

environment.

(c) The following provisions must apply to reagents:

Page 21

Courtesy of Michigan Administrative Rules

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

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

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

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

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

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

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

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

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

to the approval of the department.

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

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

samples.

(D) Crushed ice.

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

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

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

department.

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

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

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

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

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

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

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

weight. If distilled water is used for washing solvent, use distilled water with less than

0.001% residue. Run blanks before field use to eliminate a high blank on test samples.

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

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

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

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

(d) The following provisions must apply to procedure:

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

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

comply with the following provisions:

(A) Pretest preparation provisions are as follows:

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

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

unless otherwise specified in this rule.

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

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

container. As an alternative, the silica gel need not be preweighed, but may be weighed

directly in its impinger or sampling holder just before train assembly.

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

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

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

Page 22

Courtesy of Michigan Administrative Rules

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

weighing.

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

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

calcium sulfate, and individually weigh and record each weight to the nearest 0.1

milligram. During the weighing, the filter must not be exposed to the laboratory

atmosphere for a period of more than 2 minutes and a relative humidity above 50%.

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

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

(B) Preliminary determinations provisions are as follows:

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

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

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

performed.

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

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

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

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

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

the particulate sample run.

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

necessary to change the nozzle size to maintain isokinetic sampling rates. During the run,

do not change the nozzle size. Ensure that the proper differential pressure gauge is chosen

for the range of velocity heads encountered, see method 2.

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

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

length of probes.

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

sampling time specified in the department’s rules so that the sampling time per point is

not less than 5 minutes, unless approved by the department, or some greater time interval

as specified by the department, and so that the sample volume taken, corrected to

standard conditions, exceeds the required minimum total gas sample volume. The latter is

based on an approximate average sampling rate. The number of minutes sampled at each

point may be an integer or an integer plus 1/2 minute to avoid timekeeping errors. In

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

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

department’s approval must first be obtained.

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

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

where contamination can occur covered until just before assembly or until sampling is

about to begin.

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

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

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

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

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

Page 23

Courtesy of Michigan Administrative Rules

weight of the silica gel plus impinger may be determined to the nearest 0.5 gram and

recorded.

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

identified, and weighed filter in each filter holder. Be sure that the filter is properly

centered and the gasket properly placed so as to prevent the sample gas stream from

circumventing the filter.

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

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

fiberglass, graphite, or other material string gasket when temperatures are higher. See

APTD-0576, adopted by reference in R 336.1902, for requirements. Other connecting

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

direct mechanical connection.

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

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

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

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

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

contamination by the silicone grease.

(VIII) Place crushed ice around the impingers.

(D) Leak check procedures:

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

required, to prevent invalid sampling and wasted time. If the tester opts to conduct the

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

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

380 millimeter mercury, 15 inch mercury, vacuum. Alternatively, a lower vacuum may

be used if it is not exceeded during the test. Leakage rates in excess of 4% of the average

sampling rate or 0.00057 cubic meters per minute, 0.02 cubic feet per minute, whichever

is less, are unacceptable. The following leak check instructions for the sampling train

described in APTD-0576 and APTD-0581, adopted by reference in R 336.1902, may be

helpful. Start the pump with the bypass valve fully open and the coarse adjust valve

completely closed. Partially open the coarse adjust valve and slowly close the bypass

valve until the desired vacuum is reached. Do not reverse the direction of the bypass

valve, as this will cause water to back up into the flexible sample tube and the probe. If

the desired vacuum is exceeded, either leak-check at this higher vacuum or end the leak

check and start over. When the leak check is completed, first slowly remove the plug

from the inlet to the nozzle and immediately turn off the vacuum pump. This prevents the

water in the first impinger from being forced backward into the sample tube and prevents

silica gel from being entrained backward into the second impinger.

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

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

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

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

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

that point in the test. If the leakage rate is not more than 0.00057 cubic meters per minute,

0.02 cubic feet per minute, or 4% of the average sampling rate, whichever is less, then the

results are acceptable and no correction need be applied to the total volume of dry gas

Page 24

Courtesy of Michigan Administrative Rules

metered. If a higher leakage rate is obtained, then the tester shall either record the leakage

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

void the sampling run. Immediately after component changes, leak checks may be

performed. If leak checks are done, then the procedure outlined in paragraph (i)(D)(I) of

this subdivision must be used.

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

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

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

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

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

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

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

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

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

sampling run.

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

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

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

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

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

changes in flow rates are made, before and after each leak check, and when sampling is

halted. Take other readings required by figure 104 under R 336.2021 at least once at each

sample point during each time increment, and take additional readings when significant

changes, 20% variation in velocity head readings, necessitate additional adjustments in

flow rate. Level and zero the manometer. Because the manometer level and zero may

drift due to vibrations and temperature changes, make periodic checks during the

traverse. Clean the portholes before the test run to minimize the chance of sampling

deposited material. To begin sampling, remove the nozzle cap and verify that the pitot

tube and probe are properly positioned. Position the nozzle at the first traverse point with

the tip pointing directly into the gas stream. Immediately start the pump and adjust the

flow to isokinetic conditions. Nomographs that aid in the rapid adjustment of the

isokinetic sampling rate without excessive computations are available. These nomographs

are designed for use when the type S pitot tube coefficient is 0.85 ±0.02 and the stack gas

equivalent density, dry molecular weight, is equal to 29 ±4. APTD-0576, adopted by

reference in R 336.1902, details the procedure for using the nomographs. If Cp and Md

are outside the above stated ranges, do not use the nomographs unless appropriate steps,

see subdivision (g)(iv) of this rule, are taken to compensate for the deviations. When the

stack is under significant negative pressure, height of impinger stem, take care to pull

low-flow when inserting the probe into the stack to prevent water from backing into the

sample tubing and to avoid pulsation through the filter and possible loss of materials.

When the probe is in position, block off the openings around the probe and porthole to

prevent unrepresentative dilution of the gas stream. Traverse the stack cross section, as

required by method 1 or as specified by the department, being careful not to bump the

probe nozzle into the stack walls when sampling near the walls or when removing or

inserting the probe through the portholes; this minimizes the chance of extracting

deposited material. During the test run, add more ice and, if necessary, salt to maintain a

Page 25

Courtesy of Michigan Administrative Rules

temperature of less than 20 degrees Centigrade, 68 degrees Fahrenheit, at the

condenser/silica gel outlet. Also, periodically check the level and zero of the manometer.

If the pressure drop across the filter becomes too high and makes isokinetic sampling

difficult to maintain, the filter may be replaced in the midst of a sample run. It is

recommended that another complete filter assembly be used rather than attempting to

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

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

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

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

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

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

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

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

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

nozzle sizes were used, the front-half catches from the individual trains may be

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

of impinger catch may be performed. Consult with the department for details concerning

the calculation of results when 2 or more trains are used. At the end of the sample run,

turn off the coarse adjust valve, remove the probe and nozzle from the stack, turn off the

pump, record the final dry-gas meter reading, and conduct a post-test leak check, as

outlined in paragraph (i)(D)(III) of this subdivision. Leak-check the pitot lines as

described in method 2. The lines must pass this leak check to validate the velocity head

data.

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

(f) of this rule, to determine if the run was valid or if another test run should be made. If

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

the department for possible variance on the isokinetic rates.

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

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

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

probe nozzle and place a cap over it to prevent losing or gaining particulate matter. Do

not cap off the probe tip tightly while the sampling train is cooling down as this creates a

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

Before moving the sampling train to the cleanup site, make sure all condensed water in

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

sample lines and remove the nozzle-filter set assembly from the probe. Cap all openings

to prevent contamination or accidental loss of sample. Remove all excess particulate from

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

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

area must be clean and protected from the wind so that the chances of contaminating or

losing the sample are minimized. Save a portion of the solvent used for cleanup as a

blank. Take 200 milliliters of this solvent directly from the wash bottle being used and

place it in a glass sample container labeled "solvent blank". Inspect the train before and

during disassembly and note any abnormal conditions. Treat the samples in the following

manner: Container numbers. 1, 1A. Carefully remove the filters from the filter holders

and place each filter in its identified container. Use a pair of tweezers or clean disposable

Page 26

Courtesy of Michigan Administrative Rules

surgical gloves, or both, to handle the filters. Carefully transfer to the container any

particulate matter or filter fibers, or both, that adhere to the filter holder gasket by using a

dry nylon bristle brush or sharp-edged blade, or both. Seal the containers. Container

number 2. Taking care to see that particulate on the outside of the nozzle and filter

holders does not get into the sample, the tester shall carefully remove the nozzle and

clean the inside surface by rinsing with solvent from a wash bottle and brushing with a

nylon bristle brush. Brush until the solvent rinse shows no visible particles and then make

a final rinse of the inside surface with solvent. After ensuring that all joints have been

cleaned of all extraneous material, the tester shall quantitatively remove particulate from

the filter holders by rubbing the surfaces with a nylon bristle brush and rinsing with

solvent. Rinse each surface 3 times, or more if needed, to remove visible particulate.

Make a final rinse of the brush and filter holder set. After all solvent washings and

particulate matter have been collected in the sample container, tighten the lid on the

sample container so that solvent will not leak out when it is shipped to the laboratory.

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

the container to clearly identify its contents. Container number 3. Note the color of the

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

its condition. Transfer the silica gel from the third impinger to its original container and

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

policeman may be used as an aid in removing the silica gel from the impinger. It is not

necessary to remove the small amount of dust particles that adhere to the impinger wall

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

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

available in the field, follow the procedure for container number 3 in paragraph (iii) of

this subdivision. Impinger water. Treat the impingers in the following manner: Make a

notation of any color or film in the liquid catch. Measure the liquid that is in the first 2

impingers to within ±1 milliliter by using a graduated cylinder or by weighing it to within

±1.0 gram by using a balance if one is available. Record the volume or weight of liquid

present. This information is required to calculate the moisture content of the effluent gas.

Discard the liquid after measuring and recording the volume or weight, unless analysis of

the impinger catch is required, see subdivision (b)(i)(G) of this rule. If a different type of

condenser is used, measure the amount of moisture condensed either volumetrically or

gravimetrically. If possible, containers must be shipped in a manner that keeps them

upright at all times.

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

under R 336.2021. Handle each sample container in the following manner: Container

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

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

oven at 105 degrees Centigrade, 220 degrees Fahrenheit, for a minimum of 2 hours, cool

for at least 1 hour in a desiccator containing anhydrous calcium sulfate, and weigh and

record its weight to the nearest 0.1 milligram. During the weighing the filter must not be

exposed to the laboratory atmosphere for a period greater than 2 minutes or a relative

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

humidity effects may be used, subject to the approval of the department. The method

used for drying and weighing of filters must be consistent before and after the test.

Container number 2. Note the level of liquid in the container and confirm on the analysis

Page 27

Courtesy of Michigan Administrative Rules

sheet if leakage occurred during transport. If a noticeable amount of leakage has

occurred, then either void the sample or use methods, subject to the approval of the

department, to correct the final results. Measure the liquid in this container either

volumetrically to ±1 milliliter or gravimetrically to ±1.0 gram. Transfer the contents to a

tared 250-milliliter beaker and evaporate to dryness either at ambient temperature and

pressure for acetone or at 95 degrees Centigrade, 203 degrees Fahrenheit, in an oven for

distilled water. Then subject the sample to 250 degrees Centigrade, 482 degrees

Fahrenheit, in an oven for 2 to 3 hours. Desiccate 24 hours and weigh to a constant

weight. Report the results to the nearest 0.1 milligram. Container number 3. Weigh the

spent silica gel, or silica gel plus impinger, to the nearest 0.5 gram using a balance. This

step may be conducted in the field. "Solvent blank" container. Measure solvent in this

container either volumetrically or gravimetrically. Transfer the contents to a tared 250-

milliliters beaker and evaporate to dryness either at ambient temperature and pressure for

acetone or at 95 degrees Centigrade, 203 degrees Fahrenheit, in an oven for distilled

water. Then subject the sample to 250 degrees Centigrade, 482 degrees Fahrenheit, in an

oven for 2 to 3 hours. Desiccate for 24 hours and weigh to a constant weight. Report the

results to the nearest 0.1 milligram. If acetone is used, the contents of Container number

2, as well as the acetone blank container, may be evaporated at temperatures higher than

ambient. If evaporation is done at an elevated temperature, then the temperature must be

closely supervised, and the contents of the beaker must be swirled occasionally to

maintain an even temperature. Use extreme care, as acetone is highly flammable and has

a low flash point.

(e) Calibration. Maintain a laboratory log of all calibrations. Calibrations must

comply with the following provisions:

(i) Probe nozzle. A probe nozzle must be calibrated before its initial use in the

field. Using a micrometer, measure the inside diameter of the nozzle to the nearest 0.025

millimeter, 0.001 inch. Make 3 separate measurements using different diameters each

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

low numbers must not exceed 0.1 millimeter, 0.004 inch. When nozzles become nicked,

dented, or corroded, the nozzles must be reshaped, sharpened, and recalibrated before

use. Each nozzle must be permanently and uniquely identified.

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

procedures in method 2.

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

be calibrated according to the procedure in APTD-0576, adopted by reference in R

336.1902. Instead of physically adjusting the dry-gas meter dial readings to correspond to

the wet-test meter readings, calibration factors may be used to mathematically correct the

gas meter dial readings to the proper values. Before calibrating the metering system, a

leak check may be conducted. For metering systems having diaphragm or rotary pumps,

the normal leak check procedure will not detect leakages within the pump. For these

cases, the following leak check procedure may be used: Make a 10-minute calibration run

at 0.00057 cubic meters per minute, 0.02 cubic feet per minute. At the end of the run,

take the difference of the measured wet-test meter and dry-gas meter volumes and divide

the difference by 10 to get the leak rate. The leak rate must not exceed 0.00057 cubic

meters per minute (0.02 cubic feet per minute). After each field use, the calibration of the

metering system must be checked by performing 3 calibration runs at a single,

Page 28

Courtesy of Michigan Administrative Rules

intermediate orifice setting, based on the previous field test, with the vacuum set at the

maximum value reached during the test series. To adjust the vacuum, insert a valve

between the wet-test meter and the inlet of the metering system. Calculate the average

value of the calibration factor. If the calibration has changed by more than 5%, then

recalibrate the meter over the full range of orifice settings, as outlined in APTD-0576.

Alternatively, a spirometer may be substituted for a wet-test meter in the above

calibration procedures. Alternative procedures, such as using the orifice meter

coefficients, may be used, subject to the approval of the department. If the dry-gas meter

coefficient values obtained before and after a test series differ by more than 5%, then the

test series must be performed using whichever meter coefficient value, before or after,

gives the lower value of total sample volume.

(iv) Temperature gauges. Use the procedure in method 2 to calibrate in-stack

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

condenser outlet, must be calibrated against mercury-in-glass thermometers or other

thermometers that are calibrated using a National Institute of Standards and Technology

calibrated reference thermometer.

(v) Leak check of metering system shown in figure 102 under R 336.2021. That

portion of the sampling train from the pump to the orifice meter must be leak-checked

before initial use and after each shipment. Leakage after the pump will result in less

volume being recorded than is actually sampled. The following procedure is suggested,

also see figure 107 under R 336.2021: Close the main valve on the meter box. Insert a 1-

hole rubber stopper with rubber tubing attached into the orifice exhaust pipe. Disconnect

and vent the low side of the orifice manometer. Close off the low side orifice tap.

Pressurize the system to 13 to 18 centimeters, 5 to 7 inches, water column by blowing

into the rubber tubing. Pinch off the tubing and observe the manometer for 1 minute. A

loss of pressure on the manometer indicates a leak in the meter box. Leaks, if present,

must be corrected.

(vi) Barometer. Calibrate against a mercury barometer.

(f) Calculations. When carrying out calculations, retain at least 1 extra decimal

figure beyond that of the acquired data. Round off figures after the final calculation.

Other forms of the equations may be used if the other forms of the equations give

equivalent results. The following provisions apply to calculations:

(i) Nomenclature:

A_n= Cross-sectional area of nozzle, meters² or the equivalent feet².

A = Cross-sectional area of stack or flue at the point of sampling, feet².

B

fraction.

B

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

ws

= Percent water vapor in gas entering source particulate control device

wi

determined by method 4.

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

C_a= Wash blank residue concentration, milligrams per gram.

C_s= Concentration of particulate matter in stack gas, pounds per 1,000 pounds of

actual stack gas.

C

= Concentration of particulate matter in stack gas, moisture excluded,

sD

pounds per 1000 pounds of dry stack gas.

Page 29

Courtesy of Michigan Administrative Rules

C_s50= Concentration of particulate matter corrected to 50% excess air, pounds per

1000 pounds of stack gas.

C_s50D= Concentration of particulate matter corrected to 50% excess air, excluding

any water addition from a collector, pounds per 1000 pounds of stack gas.

E = Mass emission rate of particulate, pounds/hour.

F₅₀= Concentration conversion factor to 50% excess air with no moisture

alterations in exhaust.

F_50D= Concentration conversion factor to 50% excess air, excluding any moisture

added to exhaust gas by pollution collection system.

F_D= Concentration conversion factor to dry basis, excluding any water in the

stack gas.

I = Percent of isokinetic sampling.

L _a= Maximum acceptable leakage rate for either a pretest leak check or for a leak

check following a component change; equal to 0.00057 meters³/minute (0.02 cubic feet

per minute) or 4% of the average sampling rate, whichever is less.

L_i= Individual leakage rate observed during the leak check conducted

before the "ith" component change (i = 1, 2, 3 . . . . n), meters³/minute (cubic feet per

minute).

L_p= Leakage rate observed during the post-test leak check, meters³/minute (cubic

feet per minute).

M_d= Molecular weight of dry stack gas, gram/gram mole (pound/pound-mole),

calculated

by method 3, equation 3-1, using data from integrated method 3.

m_n= Total amount of particulate matter collected, milligram.

M_w= Molecular weight of water, 18.0 gram/gram-mole (18.0 pound/pound-

mole).

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

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

P

= Barometric pressure at the sampling site, millimeter mercury (inches

bar

mercury).

P_s= Absolute stack gas pressure.

P_std

=

Standard absolute pressure, 760 millimeters mercury (29.92 inches

mercury).

R = Ideal gas constant, 0.06236 millimeters of mercury-cubic meters per kelvin-

gram-mole, (21.85 inches of mercury-cubic feet per Rankine-pound-mole).

T

= Absolute average dry-gas meter temperature, see figure 104 under R

m

336.2021, °Kelvin, (°Rankine).

T_s= Absolute average stack gas temperature, see figure 104 under R 336.2021,

°Kelvin, (°Rankine).

T_std= Standard absolute temperature, 294.I°Kelvin, (530°Rankine).

V _a= Volume of solvent blank, milliliters.

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

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

under R 336.2021), milliliters.

V_m= Volume of gas sample as measured by the dry-gas meter, deci-centimeter,

(deci-cubic-foot).

Page 30

Courtesy of Michigan Administrative Rules

V

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

standard conditions, deci-standard cubic meter, (deci-standard cubic foot).

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

conditions, standard cubic meter, (standard cubic foot).

= Stack gas velocity, calculated by method 2, using data obtained from

m(std)

V

w(std)

V

s

method 5, meters/second (feet/second).

W_a= Weight of residue in solvent wash, milligram.

Y = Dry-gas meter calibration factor.

ΔH = Average pressure differential across the orifice meter (see figure 104 under

R 336.2021), millimeter water (inches water).

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

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

p _a= Density of solvent, milligrams/milliliter.

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

p_w= Density of water, 0.9982 grams/milliliter (0.002201 pounds/milliliter).

θ = Total sample time, minute.

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

change, minute.

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

with the interval between the first and second changes, minute.

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

of the sampling run, minute.

13.6 = Specific gravity of mercury.

60 = Seconds/minute.

100 = Conversion to percent.

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

453.6 = Conversion of pounds to grams.

3600 = Conversion of hours to seconds.

1000 = Conversion of 1000 pound units to pound units.

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

See data sheet, figure 104 under R 336.2021.

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

standard conditions, 21.11 degrees Centigrade, 760 millimeters mercury or 68 degrees

Fahrenheit, 29.92 inches mercury, by using equation 5-1.

Equation 5-1:

Y

(

+ H / 13.6)

(

+ H / 13.6)

P_bar

V_mT_stdP_bar

=

Y

K₁V_m

V_m(std)

T_mP_std

T_m

Where:

K₁= 0.3869 °K/mm Hg for metric units.

= 17.71 °R/in. Hg for English units.

Page 31

Courtesy of Michigan Administrative Rules

Equation 5-1 may be used as written. However, if the leakage rate observed during

any of the mandatory leak checks, for example, the post-test leak check or leak checks

conducted before component changes, exceeds L_a, equation 5-1 must be modified as

follows:

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

V_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

=

( p_w/

) (R

/

) =

V_w(std)

V_1c

M_w

T_stdP_stdK₂V_1c

Where:

K₂= 0.001338 m³/ml for metric units.

= 0.04733 ft.³/ml for English units.

(v) Moisture content.

Equation 5-3

=

/ (

V_w(std)V_m(std)

+

)

v_w(std)

B_ws

In saturated or water droplet-laden gas streams, 2 calculations of the moisture content

of the stack gas must be made: 1 from the impinger analysis, equation 5-3, and a second

from the assumption of saturated conditions. The lower of the 2 values of B_wsmust be

considered correct. The procedure for determining the moisture content based on the

assumption of saturated conditions as described in 40 CFR part 60 appendix A method 4.

For the purpose of this method, the average stack gas temperature from figure 104 under

R 336.2021 may be used to make the determination, if the accuracy of the in-stack

temperature sensor is ±1 degree Centigrade, 2 degrees Fahrenheit.

(vi) Solvent blank concentration.

Equation 5-4

Page 32

Courtesy of Michigan Administrative Rules

=

/ ( )

V_aP_a

C_a

m

a

(vii) Solvent wash blank.

Equation 5-5

=

W _a

C _a

V

P _a

aw

(viii) Total particulate weight. Determine the total particulate catch from the sum

of the weights obtained from containers 1, 1A, and 2 less the wash solvent blank, see

figure 106 under R 336.2021. Refer to subdivision (d)(i)(E) of this rule to assist in the

calculation of results involving 2 or more pairs of filters or 2 or more sampling trains.

(ix) Sampled gas density. Determine the density of the gas sampled from the stack,

at standard conditions in pounds per cubic foot, lb/ft.³.

Equation 5-6

= (

(1-

) +

) / 386.9

M_wB_ws

P_s(std)

M_d

B_ws

(x) Total weight of gas sampled, lbs.

Equation 5-7

= (

+

) p

V _w(std)

s(std)

m_g

V_m(std)

(xi) Particulate concentration, lbs/1000 lbs.

Equation 5-8

=

/ (453.6

)

m_g

C_s

m_n

(xii) Excess air and moisture correction factors:

(A) Correction factor to 50% excess air for those sources with or without a

particulate collector where no increase in moisture content of the exhaust gas occurs after

the process and before the point of sampling.

Equation 5-9

+ 18

/ (100 -

)

M_d

- 2.0592 %

B_wo

+

B_wo

+ 18

=

F₅₀

0.1826 %

/ (100 -

)

B_wo

N₂

0₂

M_d

B_wo

(B) Correction factor to 50% excess air for those sources with a wet collection

device, scrubber, that increases the moisture content of the exhaust gas after the process

and before the point of sampling.

Page 33

Courtesy of Michigan Administrative Rules

Equation 5-10

+ 18

/ (100 -

)

M_d

- 2.0592 %

B_wo

+

B_wo

+ 18

=

F_50D

0.1826 %

/ (100 -

)

B_wi

N₂

0₂

M_d

B_wi

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

Equation 5-11

+ 18

/ (100 -

)

B_wo

M_d

B_wo

=

F_D

M_d

(xiii) Converted particulate concentrations, where applicable under the

department’s rules or permit.

Equation 5-12

=

C _s50

C _sF ₅₀

C_sF _50D

C_sF _D

Equation 5-13

=

C _s50D

Equation 5-14

=

C_sD

(xiv) Mass emission rate in pounds per hour, lb/hr.

Equation 5-15

3600 A

V_sC_sP_sT_stdP_s(std)

E =

=

A

/

K₃V_sC_sP_sP_s(std)T_s

1000

T_sP_std

Where:

K₃= 63.77 for English units.

(xv) Isokinetic variation using 1 of the following methods:

(A) Calculation from raw data.

Equation 5-16

Page 34

Courtesy of Michigan Administrative Rules

100

(

+ ( + H / 13.6))

/

)(

T_sK₄V_lc

V_mT_mP_bar

I =

60 

V_sP_sA_n

Where:

K₄= 0.003458 mm Hg - m³ml - °K for metric units.

= 0.002672 in. Hg - ft.³/ml - °R for English units.

(B) Calculation from intermediate values.

Equation 5-17

100

T_sV_m(std)P_std

T_sV_m(std)

 (1-

I =

=

K₅



60(1-

)

B_ws

T_stdV_sA_nP_s

B_ws

P_sV_sA_n

Where:

K5 = 4.307 for metric units.

= 0.09409 for English units.

(xvi) Acceptable results. If 90%=I=110%, then the results are acceptable. If the

results are low in comparison to the standard and I is beyond the acceptable range, or if I

is less than 90%, then the department may opt to accept the results. Otherwise, reject the

results and repeat the test.

(g) Bibliography:

(i) Federal Register, Volume 42, No. 160, Part 160, Chapter 1, Title 40, Appendix

A, Method 5, August 18, 1977.

(ii) Martin, Robert M. Construction Details of Isokinetic Source Sampling

Equipment. Environmental Protection Agency. Research Triangle Park, N.C. APTD-

0581. April, 1971.

(iii) Rom, Jerome J. Maintenance, Calibration, and Operation of Isokinetic Source

Sampling Equipment. Environmental Protection Agency. Research Triangle Park, N.C.

APTD-0576. March, 1972.

(iv) Shigehara, R. T. "Adjustments in the EPA Nomograph for Different Pitot Tube

Coefficients and Dry Molecular Weights." Stack Sampling News, 2:4 - 11. October,

1974.

(v) Guidelines for Source Testing of Particulate. Michigan Department of Natural

Resources, Air Quality Division. June 1, 1977.

History: 1985 AACS; 1992 AACS; 2002 AACS; 2005 AACS; 2025 MR 17, Eff. Sept. 10, 2025.

R 336.2012 Reference test method 5C.

Rule 1012. Reference test method 5C, out-stack filtration method, reads as follows:

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

(i) Principle. Particulate matter is withdrawn iso-kinetically from the source and

collected on solid filtering media maintained at a temperature in the range of 120 ±14

Page 35

Courtesy of Michigan Administrative Rules

degrees Centigrade, 248 ±25 degrees Fahrenheit, or another temperature as specified by

the department's rules or a permit condition, or as approved by the department for a

particular application. The particulate mass, which includes any material that condenses

at or above the filtration temperature, is determined gravimetrically after removal of

uncombined water.

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

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

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

to install, or a permit to operate.

(iii) Performance test criteria as follows:

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

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

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

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

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

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

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

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

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

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

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

department.

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

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

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

method approved by the department.

(b) The following provisions apply to apparatus:

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

in figure 103 under R 336.2021. Construction details for many, but not all, of the train

components are given in APTD-0581, subdivision (g)(ii) of this rule. For changes from

the APTD-0581 document and for allowable modifications to figure 103 under R

336.2021, consult with the department. The operating and maintenance procedures for

many, but not all, of the sampling train are described in APTD-0576, adopted by

reference in R 336.1902, and referenced under subdivision (g)(iii) of this rule. Since

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

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

otherwise specified. The sampling train consists of the following components:

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

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

preserve a constant internal diameter. The probe nozzle must be of the buttonhook

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

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

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

isokinetic sampling must be available, for example, 0.32 to 1.27 centimeters, 1/8 to 1/2

inch, or larger if higher volume sampling trains are used inside diameter nozzles in

Page 36

Courtesy of Michigan Administrative Rules

increments of 0.16 centimeters, 1/16 inches. Each nozzle must be calibrated according to

the procedures outlined in subdivision (e) of this rule.

(B) Probe liner. Borosilicate or quartz glass tubing with a heating system capable

of maintaining a gas temperature at the exit end during sampling of 120 ±14 degrees

Centigrade, 248 ±25 degrees Fahrenheit, another temperature as specified by the

department's rules, or a temperature approved by the department for a particular

application. The tester may opt to operate the equipment at a temperature lower than that

specified. Since the actual temperature at the outlet of the probe is not usually monitored

during sampling, probes constructed according to APTD-0581, adopted by reference in R

336.1902, which utilize the calibration curves of APTD-0576, or calibrated according to

the procedure outlined in APTD-0576, adopted by reference in R 336.1902, are

acceptable. Either borosilicate or quartz glass probe liners may be used for stack

temperatures up to about 480 degrees Centigrade, 900 degrees Fahrenheit; quartz liners

must be used for temperatures between 480 and 900 degrees Centigrade, 900 and 1,650

degrees Fahrenheit. Both types of liners may be used at higher temperatures than

specified for short periods of time, subject to the approval of the department. The

softening temperature for borosilicate is 820 degrees Centigrade, 1,508 degrees

Fahrenheit, and for quartz it is 1,500 degrees Centigrade, 2,732 degrees Fahrenheit.

When practical, every effort must be made to use borosilicate or quartz glass probe liners.

Alternatively, metal liners, such as 316 stainless steel, Incoloy 825, or other corrosion

resistant materials made of seamless tubing, may be used, subject to the approval of the

department.

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

the department. The pitot tube must be attached to the probe, as shown in figure 103

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

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

entry plane, see method 2, figure 2-6 Velocity Traverse Data, during sampling. The type

S pitot tube assembly must have a known coefficient, determined as outlined in method 2.

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

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

the other must be used for orifice differential pressure readings.

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

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

contact with each other is not acceptable. Materials of construction may be stainless steel

316, glass, Teflon, or another material approved by the department.

(F) Filter heating system. Any heating system capable of maintaining a

temperature around the filter holder during sampling of 120 ±14 degrees Centigrade, 248

±25 degrees Fahrenheit, another temperature as specified by the department's rules or a

permit condition, or a temperature approved by the department for a particular

application. Alternatively, the tester may opt to operate the equipment at a temperature

lower than that specified. A temperature gauge capable of measuring temperature to

within 3 degrees Centigrade, 5.4 degrees Fahrenheit, must be installed so that the

temperature around the filter holders can be regulated and monitored during sampling.

Heating systems other than the one shown in APTD-0581 may be used.

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

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

Page 37

Courtesy of Michigan Administrative Rules

or any similar leak-free non-contaminating fittings. All impingers must be of the

Greenburg-Smith design and must be modified by replacing the tip with a 1.3

centimeters, 1/2 inch, inside diameter glass tube extending to about 1.3 centimeters, 1/2

inch, from the bottom of the flask. Modifications, such as using flexible connections

between the impingers or using materials other than glass, are allowed subject to the

approval of the department’s staff. The first impinger must contain a known quantity of

water, as described in subdivision (d)(i)(C) of this rule, the second must be empty, and

the third must contain a known weight of silica gel or equivalent desiccant. Alternatively,

a system that cools the sample gas stream and allows measurement of the water

condensed and moisture leaving the condenser, to within 1 milliliter or 1 gram, may be

used subject to the approval of the department. In any case, the means for measuring the

moisture leaving the condenser must be by passing the sample gas stream through a tared

silica gel, or equivalent desiccant, trap with exit gases kept below 20 degrees Centigrade,

68 degrees Fahrenheit, and determining the weight gain. If a determination of the

particulate matter collected in the impingers is required by the department's rules, a

permit to install, or a permit to operate, the impinger system described in this

subparagraph must be used, without modification. Contact the department as to the

sample recovery and analysis of the impinger contents.

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

measuring temperature to within 3 degrees Centigrade, 5.4 degrees Fahrenheit, drygas

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

figure 103 under R 336.2021. Other metering systems capable of maintaining sampling

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

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

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

Sampling trains utilizing metering systems designed for higher flow rates than those

described in APTD-0581 or APTD-0576, both adopted by reference in R 336.1902, may

be used if the specifications of this method are met.

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

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

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

When obtained from this source, the station value, which is the absolute barometric

pressure, must be requested and an adjustment for elevation differences between the

weather station and sampling point must be applied at a rate of minus 2.5 millimeters

mercury per 30 meters, 0.1 inch mercury, per 100 foot, elevation increase or vice versa

for elevation decrease.

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

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

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

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

leading edge of the probe sheath and does not touch any metal. Alternatively, the sensor

may be attached just before use in the field. Note, however, that if the temperature sensor

is attached in the field, the sensor must be placed in an interference-free arrangement

with respect to the type S pitot tube openings, see method 2, figure 2.7. As a second

alternative, if a difference of not more than 1% in the average velocity measurement is to

Page 38

Courtesy of Michigan Administrative Rules

be introduced, the temperature gauge need not be attached to the probe or pitot tube. This

alternative is subject to the approval of the department.

(ii) Sample recovery. The following items :

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

steel wire handles. The probe brush must have extensions, at least as long as the probe,

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

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

(B) Wash bottles - 2. Glass wash bottles are recommended; polyethylene wash

bottles may be used at the option of the tester. It is recommended that acetone not be

stored in polyethylene bottles for longer than a month.

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

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

must be constructed so as to be leak-free and resistant to chemical attack by acetone.

Narrow-mouth glass bottles have been found to be less prone to leakage. Alternatively,

polyethylene bottles may be used.

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

otherwise specified by the department.

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

milliliter or 1 gram. Graduated cylinders must have subdivisions of not more than 2

milliliters. Most laboratory balances are capable of weighing to the nearest 0.5 gram or

less. Any of these balances are suitable for use here and in paragraph (iii)(D) of this

subdivision.

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

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

not necessary if silica gel is weighed in the field.

(H) Funnel made from glass or polyethylene, to aid in sample recovery.

(iii) Analysis must include the following equipment:

(A) Glass weighing dishes.

(B) Desiccator.

(C) Analytical balance, to measure to within 0.1 milligrams.

(D) Balance, to measure to within 0.5 milligrams.

(E) Beakers, 250 milliliters.

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

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

(c) The following provisions apply to reagents:

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

(A) Filters. Two outstack filters may be any combination of alundum ceramic

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

of the filters must allow proper sampling rates to maintain isokinetics using the nozzle

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

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

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

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

Alternatively, other types of desiccants, equivalent or better, may be used, subject to the

approval of the department.

Page 39

Courtesy of Michigan Administrative Rules

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

distilled water must be used. Run blanks prior to field use to eliminate a high blank on

test samples.

(D) Crushed ice.

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

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

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

department.

(ii) Sample recovery, washing solvent. Either acetone or distilled water may be

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

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

has a high residue blank and must not be used. Suppliers sometimes transfer acetone to

glass bottles from metal containers, so acetone blanks must be run before field use and

only acetone with low blank values, less than 0.001%, must be used. A blank value of

more than 0.001% of the weight of acetone used must not be subtracted from the sample

weight. If distilled water is used for washing solvent, use distilled water with less than

0.001% residue. Run blanks before field use to eliminate a high blank on test samples.

(iii) Two reagents are required for the analysis:

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

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

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

(d) The following provisions apply to procedure:

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

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

comply with the following provisions:

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

according to the applicable procedures described in APTD-0576, adopted by reference in

R 336.1902, unless otherwise specified in this rule. Weigh several 200 to 300 gram

portions of silica gel in airtight containers to the nearest 0.5 gram. Record the total weight

of the silica gel plus container on each container. As an alternative, the silica gel need not

be pre-weighed, but may be weighed directly in its impinger or sampling holder just

before train assembly. Check filters visually against light for irregularities, flaws, pinhole

leaks, or cracks. Label filters of the proper size on the back side using numbering

machine ink. As an alternative, label the shipping containers, described in subdivision

(b)(ii)(D) of this rule, and keep the filters in these containers at all times, except during

sampling and weighing. Dry the filters in an oven at 105 degrees Centigrade, 220 degrees

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

anhydrous calcium sulfate, and individually weigh and record each weight to the nearest

0.1 milligram. During the weighing, the filters must not be exposed to the laboratory

atmosphere for a period of more than 2 minutes and a relative humidity above 50%.

Procedures, other than those specified, that account for relative humidity effects may be

used, subject to the approval of the department.

(B) Preliminary determinations. Select the sampling site and the minimum number

of sampling points according to method 1 or as specified by the department. Determine

the stack pressure, temperature, and the range of velocity heads using method 2. It is

recommended that a leak check of the pitot lines, see method 2, be performed. Determine

Page 40

Courtesy of Michigan Administrative Rules

the moisture content using approximation method 4, or its alternatives, for the purpose of

making isokinetic sampling rate settings. Determine the stack gas dry molecular weight,

as described in method 2. If integrated method 3 sampling is used for molecular weight

determination, the integrated bag sample must be taken simultaneously with, and for the

same total length of time as, the particulate sample run. Select a nozzle size based on the

range of velocity heads so that it is not necessary to change the nozzle size in order to

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

that the proper differential pressure gauge is chosen for the range of velocity heads

encountered, see method 2. Select a suitable probe liner and probe length so that all

traverse points can be sampled. For large stacks, consider sampling from opposite sides

of the stack to reduce the length of probes. Select a total sampling time greater than or

equal to the minimum total sampling time specified in the test procedures for the specific

industry so that the sampling time per point is not less than 5 minutes, unless approved by

the department, or some greater time interval as specified by the department, and so that

the sample volume taken, corrected to standard conditions, exceeds the required

minimum total gas sample volume. The latter is based on an approximate average

sampling rate. It is recommended that the number of minutes sampled at each point be an

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

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

points and to obtain smaller gas sample volumes. In these cases, the department's

approval must first be obtained.

(C) Preparation of collection train. During preparation and assembly of the

sampling train, keep all openings where contamination can occur covered until just

before assembly or until sampling is about to begin. Place 100 milliliters of water in the

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

grams of pre-weighed silica gel from its container to the third impinger. More silica gel

may be used, but care should be taken to ensure that it is not entrained and carried out

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

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

determined to the nearest 0.5 gram and recorded. Using tweezers or clean disposable

surgical gloves, place a labeled, identified, and weighed filter in the filter holder. Be sure

that the filter is properly centered and the gasket properly placed so as to prevent the

sample gas stream from circumventing the filter. Check the filter for tears after assembly

is completed. When glass liners are used, install the selected nozzle using a Viton A O-

ring when stack temperatures are less than 260 degrees Centigrade, 500 degrees

Fahrenheit, and a heat-resistant fiberglass, graphite, or other material string gasket when

temperatures are higher. See APTD-0576, adopted by reference in R 336.1902, for

details. Other connecting systems using either 310 stainless steel or Teflon ferrules may

be used. When metal liners are used, install the nozzle in the same manner as for glass

liners or by a leak-free direct mechanical connection. Mark the probe with heat-resistant

tape or by some other method to denote the proper distance into the stack or duct for each

sampling point. Set up the train as in figure 103 under R 336.2021. If necessary, use a

very light coat of silicone grease on all ground glass joints. Grease only the outer portion,

see APTD-0576, adopted by reference in R 336.1902, to avoid the possibility of

contamination by the silicone grease. Place crushed ice around the impingers.

(D) Leak check procedures as follows:

Page 41

Courtesy of Michigan Administrative Rules

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

required, to prevent invalid sampling and wasted time. If the tester opts to conduct the

pretest leak check, the following procedure must be used: After the sampling train has

been assembled, turn it on and set the filter and probe heating systems at the desired

operating temperatures. Allow time for the temperatures to stabilize. If a Viton A O-ring

or other leak-free connection is used in assembling the probe nozzle to the probe liner,

leak check the train at the sampling site by plugging the nozzle and pulling a 380

millimeter mercury, 15 inch mercury, vacuum. A lower vacuum may be used, if it is not

exceeded during the test. If a heat-resistant fiberglass, graphite, or other material string is

used, do not connect the probe to the train during the leak check. Instead, leak check the

train by first plugging the inlet to the filter holder, and cyclone, if applicable, and pulling

a 380 millimeter mercury, 15 inch mercury, vacuum. A lower vacuum may be used if it is

not exceeded during the test. Then connect the probe to the train and leak check at about

a 25 millimeter mercury, 1 inch mercury, vacuum. Alternatively, the probe may be leak

checked with the rest of the sampling train, in 1 step, at a 380 millimeter mercury, 15

inch mercury, vacuum. Leakage rates in excess of 4% of the average sampling rate or

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

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

APTD-0576 and APTD-0581 may be helpful. Start the pump with the bypass valve fully

open and the coarse adjust valve completely closed. Partially open the coarse adjust valve

and slowly close the bypass valve until the desired vacuum is reached. Do not reverse the

direction of the bypass valve, as this will cause water to back up into the filter holder. If

the desired vacuum is exceeded, either leak check at this higher vacuum or end the leak

check and start over. When the leak check is completed, first slowly remove the plug

from the inlet to the probe, filter holder, or cyclone, if applicable, and immediately turn

off the vacuum pump. This prevents the water in the impingers from being forced

backward into the filter holder and prevents silica gel from being entrained backward into

the third impinger.

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

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

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

according to the procedure outlined in subparagraph (D) (I) of this paragraph, except that

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

that point in the test. If the leakage rate is found to be not more than 0.00057 cubic meters

per minute, 0.02 cubic feet per minute, or 4% of the average sampling rate, whichever is

less, the results are acceptable and no correction need be applied to the total volume of

dry gas metered. If, however, a higher leakage rate is obtained, the tester shall either

record the leakage rate and plan to correct the sample volume, as shown in subdivision

(f)(iii)

of

R 336.2011, or shall void the sampling run. Immediately after component changes, leak

checks are optional. If the leak checks are done, the procedure outlined in paragraph

(i)(D)(I) of this subdivision must be used.

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

sampling run. The leak check must be done in accordance with the procedures outlined in

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

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

Page 42

Courtesy of Michigan Administrative Rules

leakage rate is found to be not more than 0.00057 cubic meters per minute, 0.02 cubic

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

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

however, a higher leakage rate is obtained, the tester shall either record the leakage rate

and correct the sample volume, as shown in subdivision (f)(iii) of R 336.2011, or shall

void the sampling run.

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

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

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

in figure 104 under R 336.2021. Be sure to record the initial dry-gas meter reading.

Record the dry-gas meter readings at the beginning and end of each sampling time

increment, when changes in flow rates are made, before and after each leak check, and

when sampling is halted. Take other readings required by figure 104 under R 336.2021 at

least once at each sample point during each time increment, and take additional readings

when significant changes, 20% variation in velocity head readings, necessitate additional

adjustments in flow rate. Level and zero the manometer. Because the manometer level

and zero may drift due to vibrations and temperature changes, make periodic checks

during the traverse. Clean the portholes before the test run to minimize the chance of

sampling deposited material. To begin sampling, remove the nozzle cap and verify that

the pitot tube and probe are properly positioned. Position the nozzle at the first traverse

point with the tip pointing directly into the gas stream. Immediately start the pump and

adjust the flow to isokinetic conditions. Nomographs that aid in the rapid adjustment of

the isokinetic sampling rate without excessive computations are available. These

nomographs are designed for use when the type S pitot tube coefficient is 0.85 ±0.02 and

the stack gas equivalent density, dry molecular weight, is equal to 29 ±4. APTD-0576,

adopted by reference in R 336.1902, details the procedure for using the nomographs. If

Cp and Md are outside the above stated ranges, do not use the nomographs unless

appropriate steps, see subdivision (g)(iv) of this rule, are taken to compensate for the

deviations. When the stack is under significant negative pressure, height of impinger

stem, take care to pull low flow when inserting the probe into the stack to prevent water

from backing into the sample tubing and to avoid pulsation through the filter and possible

loss of materials. When the probe is in position, block off the openings around the probe

and porthole to prevent unrepresentative dilution of the gas stream. Traverse the stack

cross section, as required by method 1 or as specified by the department, being careful

not to bump the probe nozzle into the stack walls when sampling near the walls or when

removing or inserting the probe through the portholes. This minimizes the chance of

extracting deposited material. During the test run, add more ice and, if necessary, salt to

maintain a temperature of less than 20 degrees Centigrade,68 degrees Fahrenheit, at the

condenser/silica gel outlet. Also, periodically check the level and zero of the manometer.

If the pressure drop across the filter becomes too high and makes isokinetic sampling

difficult to maintain, the filter may be replaced in the midst of a sample run. It is

recommended that another complete filter assembly be used rather than attempting to

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

subparagraph (D)(II) of this paragraph . The total particulate weight must include the

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

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

Page 43

Courtesy of Michigan Administrative Rules

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

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

must be subject to the approval of the department. Note that when 2 or more trains are

used, separate analyses of the front half catches from the individual trains may be

combined, as may the impinger catches, and 1 analysis of the 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 subparagraph (D)(III) of this paragraph. Also, leak check the pitot

lines as described in method 2. The lines must pass this leak check to validate the

velocity head data.

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

(f) of this rule, to determine whether the run was valid or whether 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 filter holder.

Before moving the sample train to the cleanup site, remove the probe from the sample

train, wipe off the silicone grease, and cap the open outlet of the probe. Be careful not to

lose any condensate that might be present. Wipe off the silicone grease from the filter

inlet where the probe was fastened and cap it. Remove the umbilical cord from the last

impinger and cap the impinger. If a flexible line is used between the first impinger or

condenser and the filter holder, disconnect the line at the filter holder and let any

condensed water or liquid drain into the impingers or condenser. After wiping off the

silicone grease, cap off the filter holder outlet and impinger inlet. Ground-glass stoppers,

plastic caps, or serum caps may be used to close these openings. Transfer the probe and

filter-impinger assembly to the cleanup area. This area must be clean and protected from

the wind so that the chances of contaminating or losing the sample are minimized. Save a

portion of the solvent used for cleanup as a blank. Take 200 milliliters of this solvent

directly from the wash bottle being used and place it in a glass sample container labeled

"solvent blank." Inspect the train prior to and during disassembly and note abnormal

conditions. Treat the samples as follows:

(A) Container numbers 1, 1A. Carefully remove the filters from the filter holders

and place each filter in its identified container. Use a pair of tweezers or clean disposable

surgical gloves, or both, to handle the filters. Carefully transfer to the container any

particulate matter or filter fibers, or both, that adhere to the filter holder gasket by using a

dry nylon bristle brush or sharp-edged blade, or both. Seal the container.

(B) Container number 2. Taking care to see that dust on the outside of the probe or

other exterior surfaces does not get into the sample, the tester shall quantitatively recover

from particulate matter or any condensate from the nozzle, probe fitting, probe liner, and

from both filter holders by washing these components with solvent and placing the wash

Page 44

Courtesy of Michigan Administrative Rules

in a glass container. Perform the solvent rinses as follows: Carefully remove the probe

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. Brush and rinse

the inside parts of the Swagelok fitting with solvent in a similar way until no visible

particles remain. Rinse the probe liner with solvent by tilting and rotating the probe while

squirting solvent into its upper end so that all inside surfaces are wetted with acetone. Let

the solvent drain from the lower end into the sample container. A glass or polyethylene

funnel may be used to aid in transferring liquid washes to the container. Follow the

solvent rinse with a probe brush. Hold the probe in an inclined position and squirt solvent

into the upper end as the probe brush is being pushed with a twisting action through the

probe. Hold a sample container underneath the lower end of the probe and catch any

solvent and particulate matter that is brushed from the probe. Run the brush through the

probe 3 or more times until no visible particulate matter is carried out with the solvent or

until none remains in the probe liner on visual inspection. With stainless steel or other

metal probes, run the brush through, in the above prescribed manner, not less than 6

times, since metal probes have small crevices in which particulate matter can be

entrapped. Rinse the brush with solvent and quantitatively collect these washings in the

sample container. After the brushing, make a final solvent rinse of the probe as described

above. It is recommended that 2 people clean the probe to minimize sample losses.

Between sampling runs, keep brushes clean and protected from contamination. After

ensuring that all joints have been wiped clean of silicone grease, clean the inside of both

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. 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 whether or not leakage occurred during transport. Label the container

to clearly identify its contents.

(C) Container number 3. Note the color of the indicating silica gel to determine if

it has been completely spent and make a notation of its condition. Transfer the silica gel

from the third impinger to its original container and seal. A funnel may make it easier to

pour the silica gel without spilling it. A rubber policeman may be used as an aid in

removing the silica gel from the impinger. It is not necessary to remove the small amount

of dust particles that adhere to the impinger wall and are difficult to remove. Since the

gain in weight is to be used for moisture calculations, do not use any water or other

liquids to transfer the silica gel. If a balance is available in the field, follow the procedure

for container number 3 in paragraph (iii)(C) of this subdivision. Impinger water. Treat the

impingers as follows: Make a notation of any color or film in the liquid catch. Measure

the liquid that is in the first 2 impingers to within ±1 milliliter by using a graduated

cylinder or by weighing it to within ±1.0 gram by using a balance if none is available.

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

the moisture content of the effluent gas. Discard the liquid after measuring and recording

the volume or weight, unless analysis of the impinger catch is required, see subdivision

(b)(i)(G) of this rule. If a different type of condenser is used, measure the amount of

Page 45

Courtesy of Michigan Administrative Rules

moisture condensed either volumetrically or gravimetrically. Whenever possible,

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

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

106 under R 336.2021. Handle each sample container as follows:

(A) Container numbers 1, 1A. Analyze and report each filter separately. Transfer

the filter and any loose particulate from the sample container to a tared-glass weighing

dish. Dry the filter in an oven at 105 degrees Centigrade, 220 degrees Fahrenheit, for a

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

calcium sulfate, and weigh and record its weight to the nearest 0.1 milligram. During the

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

more 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 the drying and weighing of filters must be

consistent before and after the test.

(B) Container number 2. Note the level of liquid in the container and confirm on

the analysis sheet whether or not leakage occurred during transport. If a noticeable

amount of leakage has occurred, either void the sample or use methods, subject to the

approval of the department, to correct the final results. Measure the liquid in this

container either volumetrically to ±1 milliliter or gravimetrically to ±1.0 gram. Transfer

the contents to a tared 250 milliliter beaker and evaporate to dryness either at ambient

temperature and pressure for acetone or at 95 degrees Centigrade, 203 degrees

Fahrenheit, in an oven for distilled water. Then subject the sample to 250 degrees

Centigrade, 482 degrees Fahrenheit, in an oven for 2 to 3 hours. Desiccate for 24 hours

and weigh to a constant weight. Report the results to the nearest 0.1 milligram.

(C) Container number 3. Weigh the spent silica gel, or silica gel plus impinger, to

the nearest 0.5 gram using a balance. This step may be conducted in the field. "Solvent

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

gravimetrically. Transfer the contents to a tared 250 milliliter beaker and evaporate to

dryness either at ambient temperature and pressure for acetone or at 95 degrees

Centigrade, 203 degrees Fahrenheit, in an oven for distilled water. Then subject the

sample to 250 degrees Centigrade, 482 degrees Fahrenheit, in an oven for 2 to 3 hours.

Desiccate for 24-hours and weigh to a constant weight. Report the results to the nearest

0.1 milligram. If acetone is used, the contents of container number 2, as well as the

acetone blank container, may be evaporated at temperatures higher than ambient. If

evaporation is done at an elevated temperature, the temperature must be closely

supervised, and the contents of the beaker must be swirled occasionally to maintain an

even temperature. Use extreme care, as acetone is highly flammable and has a low flash

point.

(e) Calibration. Maintain a laboratory log of all calibrations. Calibrations must

comply with all of the following provisions:

(i) Probe nozzle. A probe nozzle must be calibrated before its initial use in the

field. Using a micrometer, measure the inside diameter of the nozzle to the nearest 0.025

millimeter, 0.001 inch. Make 3 separate measurements using different diameters each

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

low numbers must not exceed 0.1 millimeter, 0.004 inch. When nozzles become nicked,

Page 46

Courtesy of Michigan Administrative Rules

dented, or corroded, the nozzles must be reshaped, sharpened, and recalibrated before

use. Each nozzle must be permanently and uniquely identified.

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

procedure outlined in method 2.

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

be calibrated according to the procedure outlined in APTD -0576, adopted by reference in

R 336.1902. Instead of physically adjusting the dry gas meter dial readings to correspond

to the wet test meter readings, calibration factors may be used to mathematically correct

the gas meter dial readings to the proper values. Before calibrating the metering system, it

is suggested that a leak check be conducted. For metering systems having diaphragm or

rotary pumps, the normal leak check procedure will not detect leakages within the pump.

For these cases, the following leak check procedure is suggested: Make a 10-minute

calibration run at 0.00057 cubic meters per minute, 0.02 cubic feet per minute. At the end

of the run, take the difference of the measured wet test meter and dry gas meter volumes,

and divide the difference by 10 to get the leak rate. The leak rate must not exceed

0.00057 cubic meters per minute, 0.02 cubic feet per minute. After each field use, the

calibration of the metering system must be checked by performing 3 calibration runs at a

single, intermediate orifice setting, based on the previous field test, with the vacuum set

at the maximum value reached during the test series. To adjust the vacuum, insert a valve

between the wet test meter and the inlet of the metering system. Calculate the average

value of the calibration factor. If the calibration has changed by more than 5%, recalibrate

the meter over the full range of orifice settings, as outlined in APTD-0576. Alternatively,

a spirometer may be substituted for a wettest meter in the above mentioned 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%, the test series must be

performed using whichever meter coefficient value, before or after, gives the lower value

of total sample volume.

(iv) Probe heater calibration. The probe heating system must be calibrated before

its initial use in the field according to the procedures outlined in APTD-0576, adopted by

reference in R 336.1902. Probes constructed according to APTD-0581 need not be

calibrated if the calibration curves in APTD-0576 are used.

(v) Temperature gauges. Use the procedure in method 2 to calibrate in stack

temperature gauges. Dial thermometers, such as those used for the dry gas meter and

condenser outlet, must be calibrated against mercury in glass thermometers or other

thermometers that are calibrated using a National Institute of Standards and Technology

calibrated reference thermometer.

(vi) Leak check of metering system shown in figure 103 under R 336.2021. That

portion of the sampling train from the pump to the orifice meter must be leak checked

before initial use and after each shipment. Leakage after the pump results in less volume

being recorded than is actually sampled. The following procedure is suggested, also see

figure 107 under R 336.2021: Close the main valve on the meter box. Insert a 1-hole

rubber stopper with rubber tubing attached into the orifice exhaust pipe. Disconnect and

vent the low side of the orifice manometer. Close off the low side orifice tap. Pressurize

the system to 13 to 18 centimeters, 5 to 7 inches, water column by blowing into the

rubber tubing. Pinch off the tubing and observe the manometer for 1 minute. A loss of

Page 47

Courtesy of Michigan Administrative Rules

pressure on the manometer indicates a leak in the meter box. Leaks, if present, must be

corrected.

(vii) Barometer. Calibrate against a mercury barometer.

(f) Calculations. When carrying out calculations, retain at least 1 extra decimal

figure beyond that of the acquired data. Round off figures after the final calculation.

Other forms of the equations may be used if the other forms of the equations give

equivalent results. All of the provisions under R 336.2011 (f) apply to calculations for

this rule.

(g) Bibliography:

(i) Federal Register, Volume 42, No. 160, Part 60, Chapter 1, Title 40, Appendix

A, Method 5. August 18, 1977.

(ii) Martin, Robert M. Construction Details of Isokinetic Source Sampling

Equipment. Environmental Protection Agency. Research Triangle Park, N.C.APTD-

0581. April, 1971.

(iii) Rom, Jerome J. Maintenance, Calibration, and Operation of Isokinetic Source

Sampling Equipment. Environmental Protection Agency. Research Triangle Park, N.C.

APTD-0576. March, 1972.

(iv) Shigehara, R. T. "Adjustments in the EPA Nomograph for Different Pitot Tube

Coefficients and Dry Molecular Weights." Stack Sampling News 2:4-11.October, 1974.

(v) Guidelines for Source Testing of Particulate. Michigan Department of Natural

Resources, Air Quality Division. June 1, 1977.

History: 1985 AACS; 1992 AACS; 2002 AACS; 2025 MR 17, Eff. Sept. 10, 2025.

R 336.2013 Reference test method 5D.

Rule 1013. Reference test method 5D, testing of steel manufacturing sources,

reads as follows:

(a) General description. Emission testing procedures shall

follow the

methodology specified in R 336.2004(1)(c) and (d) and

otherwise provided in this rule.

R

336.2012, unless

(b) Coke battery pushing emission control equipment outlet test procedure for

scrubbers. Outlet emission tests for any scrubber emission control equipment

controlling coke battery emissions shall be conducted as follows:

(i) The pushing emission control system is operated on a batch type process and

shall be tested as such using the reference test methods specified in subdivision (a)

of this rule.

(ii) Each sampling point shall be sampled for 1 cycle operation, which is defined

as beginning when the coke guide and snorkels are engaged and continuing until the

quench car leaves the hood.

(iii) For a shed, the sampling period shall begin with the first movement of coke

and shall end when the car enters the quench tower.

(iv) Integrated gas samples shall be taken over the entire test period. The samples

shall be analyzed for carbon monoxide, carbon dioxide, oxygen, and nitrogen by means

of an Orsat analyzer. The sampling and sample analysis shall be performed in

accordance with R 336.2004(1)(c). The average values from the 3 samples shall be

Page 48

Courtesy of Michigan Administrative Rules

used in determining the dry molecular weight of the exhaust gas. If a complete test is

not performed during the day, at least 1 sample shall be taken.

(v) Based on design and previous data, saturated conditions shall be assumed.

The moisture content shall be calculated as per R 336.2004(1)(d), based on stack

conditions during the preliminary and sampling traverses.

(vi) The stack sampling equipment and procedures as described in method 5C

shall be used in performing a particulate emission test, with the following variations:

(A) Due to the varying time required for pushing operations, an integer

sampling time increment shall not be required.

(B) Because of the shorter sampling periods at each sampling point, a specific

gas volume cannot be guaranteed. Therefore, an average sampling rate of not less than

0.90 dry standard cubic feet per minute shall be used during each sampling run.

(C) A stainless steel probe liner after the nozzle may be used.

(D) Glass or glass-lined stainless steel tubing and a glass cyclone between the

probe and filter holder may be used.

(E) The probe and filter heating system may be heated at 248 ±25 degrees

Fahrenheit.

(c) Basic oxygen furnace primary emissions control

equipment

outlet test

procedure. Outlet emission tests for any emission control equipment controlling

only the primary emissions from a basic oxygen furnace shall be conducted as follows:

(i) The testing program shall consist of 3 valid sampling runs. A sampling run

is the composite of those portions of 4 heats starting with oxygen blowing and

ending not more than 180 seconds following the last oxygen blow or the beginning of

the tap, whichever occurs first. Each process cycle shall be used to obtain the sample

for 1 quadrant of the traverse.

(ii) When testing a wet scrubber outlet, saturated conditions shall be assumed

and moisture content shall be calculated based on stack conditions during the

preliminary and sampling traverses.

(iii) The particulate emission rate shall be determined as specified in reference

test method 5C, with the following variations:

(A) A stainless steel probe liner after the nozzle may be used.

(B) Glass or glass-lined stainless steel tubing and a glass cyclone between the

probe and filter holder may be used.

(C) The probe and filter heating system may be heated to 248 ±25 degrees

Fahrenheit.

(d) Basic oxygen furnace secondary emissions control

equipment

outlet test

procedure. Outlet emission tests for any emission control equipment controlling

only the secondary emissions from a basic oxygen furnace shall be conducted as

follows:

(i) The testing program shall consist of 3 valid sampling runs. A sampling run

shall be defined as the composite of the following portions of 4 heats:

(A) Charging.

(B) Tapping.

(C) Turndown.

(D) Slagging.

Page 49

Courtesy of Michigan Administrative Rules

(E) The first 5 minutes of oxygen blowing for those systems with a separate

secondary collector.

(ii) When testing a wet scrubber outlet, saturated conditions shall be assumed

and moisture content shall be calculated based on stack conditions during the

preliminary and sampling traverses.

(iii) The particulate emission rate shall be determined as specified in reference

test method 5C, with the following variations:

(A) A stainless steel probe liner after the nozzle may be used.

(B) Glass or glass-lined stainless steel tubing and a glass cyclone between the

probe and filter holder may be used.

(C) The probe and filter heating system may be heated to 248 ±25 degrees

Fahrenheit.

(e) Basic oxygen furnace primary and secondary emissions control equip-

ment outlet test procedures. Outlet emission tests for any emission control

equipment controlling both the primary and secondary emissions from a basic

oxygen furnace shall be conducted as follows:

(i) One vessel:

(A) For testing of primary control equipment that captures secondary

emissions from a single vessel, the testing program shall consist of 3 valid sampling

runs. A sampling run is the composite of the following portions of 8 heats:

(1) Charging.

(2) Oxygen blowing.

(3) Tapping.

(4) Turndown.

(5) Slagging.

Four heats are to be sampled only during oxygen blowing, with each heat used to

obtain the sample from 1 quadrant. The remaining 4 heats are to be sampled only during

the portions of the heat other than oxygen blowing, with each heat used to obtain the

sample from 1 quadrant.

(B) When testing a wet scrubber outlet, saturated conditions shall be assumed

and moisture content shall be calculated based on stack conditions during the

preliminary and sampling traverses.

(C) The particulate emission rate shall be determined as specified in reference

test method 5C, with the following variations:

(1) A stainless steel probe liner after the nozzle may be used.

(2) Glass or glass-lined stainless steel tubing and a glass cyclone between the

probe and filter holder may be used.

(3) The probe and filter heating system may be heated to 248 ±25 degrees

Fahrenheit.

(ii) More than one vessel:

(A) For testing of control equipment that captures both primary and secondary

emissions from more than 1 vessel, the testing program shall consist of 3 valid

sampling runs. A sampling run is the composite of the following portions of 4 heats

for 1 or more vessels:

(1) Charging.

(2) Oxygen blowing.

Page 50

Courtesy of Michigan Administrative Rules

(3) Tapping.

(4) Turndown.

(5) Slagging.

At least 1 heat shall be used to obtain the sample from each quadrant of the traverse.

(B) When testing a wet scrubber outlet, saturated conditions shall be assumed

and moisture content shall be calculated based on stack conditions during the

preliminary and sampling traverses.

(C) The particulate emission rate shall be determined as specified in reference

test method 5C, with the following variations:

(1) A stainless steel probe liner after the nozzle may be used.

(2) Glass or glass-lined stainless steel tubing and a glass cyclone between the

probe and filter holder may be used.

(3) The probe and filter heating system may be heated to 248 ±25 degrees

Fahrenheit.

(f) Blast furnace casthouse air-cleaning device outlet test procedure. Outlet

emission tests for any air-cleaning device controlling fugitive emissions from a blast

furnace casthouse shall be conducted as follows:

(i) The testing program shall consist of 3 sampling runs. A sampling run shall be

performed during a 2-hour period, sampling only when casting takes place. If 50 dry

standard cubic feet are not sampled during this period, the sampling run shall be

extended so as to fulfill this condition.

(ii) The particulate emission rate shall be determined as specified in reference

test method 5C, with the following variations:

(A) A stainless steel probe liner after the nozzle may be used.

(B) Glass or glass-lined stainless steel tubing and a glass cyclone between the

probe and filter holder may be used.

(C) The probe and filter heating system may be heated to 248 ±25 degrees

Fahrenheit.

(g) Coke oven combustion stack test procedures. Emissions from any coke oven

combustion stack shall be tested as follows:

(i) The testing program shall consist of 3 valid sampling runs.

(ii) Saturated conditions shall be assumed for stacks controlled

by wet

scrubbers. The moisture content shall be calculated as per R 336.2004(1)(d) based

on stack conditions during the preliminary and sampling traverses.

(iii) The stack sampling equipment and procedures described in method 5C shall

be used in performing a particulate emission test with the following variations:

(A) A stainless steel probe liner after the nozzle may be used.

(B) Heated flexible teflon tubing and a glass cyclone between the probe and filter

holder may be used.

(C) The probe and filter heating system may be heated at 248 ±25 degrees

Fahrenheit.

(D) All filters shall be cooled and stored in a dessicator previous to weighing.

Exposure to the ambient air shall be minimized to the extent that it is practical. This

same procedure shall be used if any subsequent weighing is necessary.

(iv) The sampling time shall correspond to a minimum of 5 coke oven pushes per

battery.

Page 51

Courtesy of Michigan Administrative Rules

(h) Coke oven coal preheater scrubber outlet test procedures. Outlet emission

tests for any scrubber emission control equipment controlling emissions from a coke

oven coal preheater shall be conducted as follows:

(i) The testing program shall consist of 3 valid sampling runs.

(ii) Based on design and previous data, saturated conditions shall be assumed.

The moisture content shall be calculated as per R 336.2004(1)(d) based on stack

conditions during the preliminary and sampling traverses.

(iii) The stack sampling equipment and procedures described in method 5C shall

be used in performing a particulate emission test with the following variations:

(A) A stainless steel probe liner after the nozzle may be used.

(B) Glass or glass-lined stainless steel tubing and a glass cyclone between the

probe and filter holder may be used.

(C) The probe and filter heating system may be heated at 248 ±25 degrees

Fahrenheit.

(i) Electric arc furnace stack test procedures. Emissions from any electric arc

furnace stack shall be tested as follows:

(i) The testing program shall consist of 3 valid sampling runs. A sampling run

is the time beginning when the roof is placed on the furnace, after the first charge, and

ending with the time when the roof is removed, just prior to tapping.

(ii) The particulate emission rate shall be determined as specified in reference

test method 5C, with the following exceptions:

(A) A stainless steel probe liner after the nozzle may be used.

(B) Glass or glass-lined stainless steel tubing and a glass cyclone between the

probe and filter holder may be used.

(C) The probe and filter heating system may be heated to 248 ±25 degrees

Fahrenheit.

(D) The emission rate for any furnace controlled by

a

positive pressure

baghouse, or by a baghouse exhausted by more than 5 stacks, shall be determined

as specified in R 336.2014.

(j) Sinter plant gravel bed filter test procedures. Emissions from any gravel bed

filter emission control equipment controlling emissions from a sinter plant shall be

tested as follows:

(i) The testing program shall consist of 3 valid sampling runs.

(ii) The stack sampling equipment and procedures described in method 5C shall

be used in performing a particulate emission test with the following variations:

(A) A stainless steel probe liner after the nozzle may be used.

(B) Glass or glass-lined stainless steel tubing and a glass cyclone between the

probe and filter holder may be used.

(C) The probe and filter heating system may be heated at 248 ±25 degrees

Fahrenheit.

(k) Miscellaneous. During each stack test performed, the owner or operator

shall provide a representative of the department access to production data and

other parameters that are necessary for determining compliance.

(l) Sample volume. The minimum volume per sample shall be 50 cubic feet of dry

gas corrected to standard conditions, 70 degrees Fahrenheit, 29.92 inches of mercury,

unless specified otherwise in the provisions of this rule.

Page 52

Courtesy of Michigan Administrative Rules

(m) Opacity tests. During each stack test performed,

simultaneous visible

emission evaluations shall be conducted according to the reference test method

specified in R 336.1303 for the process being tested.

(n) Operating conditions. During each run of a stack test, the facility to be tested

shall be operated at a batch or other similar production level which is representative of

the actual level during the preceding 3 months before the first day of the test, unless

the department approves or specifies alternate acceptable operating conditions.

(o) Compliance. Compliance with any mass emission standard shall be

determined by averaging 3 test runs using all test procedures specified for the tested

process in this rule.

History: 1985 AACS; 2002 AACS.

R 336.2014 Reference test method 5E.

Rule 1014. Reference method 5E, determination of particulate matter emissions

from positive pressure fabric filters, 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 a glass fiber filter maintained at a temperature at or above the exhaust gas

temperature up to a nominal 248 ±25 degrees Fahrenheit. The particulate mass, which

includes any material that condenses at or above the filtration temperature, is determined

gravimetrically after the removal of uncombined water.

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

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

is also applicable when specifically provided for in the department's rules, orders, a

permit to install, or a permit to operate.

(iii) Performance test criteria as follows:

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

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

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

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

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

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

(C) The minimum volume per sample must be 30 cubic feet actual gas. Minimum

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

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

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

approved by the department.

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

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

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

method approved by the department.

(b) The following provisions apply to apparatus:

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

in figure 103 under R 336.2021. Construction details for many, but not all, of the train

components are given in APTD-0581, subdivision (g)(ii) of this rule. For changes from

Page 53

Courtesy of Michigan Administrative Rules

the APTD-0581 document and for allowable modifications to figure 103 under

R 336.2021, consult with the department. The operating and maintenance procedures for

many, but not all, of the sampling train are described in APTD-0576, adopted by

reference in R 336.1902 and as referenced under subdivision (g)(iii) of this rule. Since

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

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

otherwise specified in these rules. The sampling train consists of the following