Part 10, Entire Section, As Amended 2/4/99

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

Rule 1007. (1) The alternate version of procedure L is as follows:

1. Introduction.

1.1 Applicability. This procedure is applicable for determining the input of volatile organic compounds (voc), measured as equivalent propane as measured by a flame ionization instrument. It is intended to be used as a segment in the development of liquid/gas protocols for determining voc capture efficiency (ce) for surface coating and printing operations.

1.2 Principle. The amount of voc introduced to the process (l) is the sum of products of the weight (w) of each voc containing liquid (ink, paint, solvent, or similar material) used and its voc content (v), corrected for a response factor (rf) to allow the input to be calculated in terms of propane, the same calibration gas used in the gaseous voc measurements. A sample of each coating used is distilled to separate the voc fraction. The distillate is used to prepare a known standard for analysis by a flame ionization analyzer (fia), calibrated against propane, to determine its rf.

2. Apparatus and reagents.

2.1 Liquid weight.

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

2.1.2 Volume measurement apparatus (alternative). Volume meters, flow meters, density measurement equipment, or similar material, as needed to achieve the same accuracy as direct weight measurements.

2.2 Response factor (rf) determination (fia technique). The voc distillation and tedlar gas bag generation systems apparatus are shown in figures 1 and 2. The following equipment is required:

2.2.1 Sample collection can. An appropriately sized metal can to collect voc-containing materials. The can shall be constructed in such a way that it can be grounded to the coating container.

2.2.2 Needle valves. To control gas flow.

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

2.2.4 Tubing and fittings. Teflon and stainless steel tubing and fittings with diameters and lengths and sizes determined by connection requirements of the equipment.

2.2.5 Thermometer. Capable of measuring the temperature of the hot water and oil baths to within 1 degree Celsius.

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

2.2.7 Microliter syringe. 10-microliter size.

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

2.2.9 Hot oil bath, with stirring hot plate. Capable of heating and maintaining a distillation vessel at 110 plus or minus 3 degrees Celsius.

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

2.2.11 Rotary evaporator system. Complete with folded inner coil, vertical style condenser, rotary speed control, and teflon sweep gas delivery tube with valved inlet. Buchi rotavapor or equivalent.

2.2.12 Ethylene glycol cooling/circulating bath. Capable of maintaining the condenser coil fluid at minus 10 degrees Celsius.

2.2.13 Dry gas meter. For the precise measurement of dilution gas volume. It shall be calibrated to a primary standard, either spirometer or bubble meter.

2.2.14 Activated charcoal/mole sieve trap. To remove any trace level of organics picked up from the dry gas meter.

2.2.15 Gas coil heater. Sufficient length of 0.125-inch stainless steel tubing to allow heating of the dilution gas to near the water bath temperature before entering the volatilization vessel.

2.2.16 Water bath, with stirring hot plate. Capable of heating and maintaining a volatilization vessel and coil heater at a temperature of 100 plus or minus 5 degrees Celsius.

2.2.17 Volatilization vessel. 50-milliliter midget impinger fitted with a septum top and loosely filled with glass wool to increase volatilization surface.

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

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

2.2.20 Cylinder of compressed thc free n₂. Used as sweep gas in the rotary evaporator system.

2.2.21 Organic concentration analyzer. An fia with a span value of 1.5 times the expected concentration as propane; however, other span values may be used if it can be demonstrated that they would provide more accurate measurements. The fia instrument shall be the same instrument used in the gaseous analyses adjusted with the same fuel, combustion air, and sample backpressure (flowrate) settings. The system shall be capable of meeting or exceeding the following specifications:

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

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

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

2.2.22 Integrator/data acquisition system. An analog or digital device or computerized data acquisition system used to integrate the fia response or compute the average response and record measurement data. The minimum data sampling frequency for computing average or integrated values is 1 measurement value every 5 seconds. The device shall be capable of recording average values at least once per minute.

2.2.23 Chart recorder (optional). A chart recorder or similar device is recommended to provide a continuous analog display of the measurement results during the liquid sample analysis.

2.2.24 Calibration and other gases. For calibration, fuel, and combustion air, if required, contained in compressed gas cylinders. All calibration gases shall be traceable to NIST standards and shall be certified by the manufacturer to plus or minus 1% of the tag value. Additionally, the manufacturer of the cylinder should provide a recommended shelf life for each calibration gas cylinder over which the concentration does not change more than plus or minus 2% from the certified value. For calibration gas values that are not generally available, alternative methods for preparing calibration gas mixtures, such as dilution systems, may be used with prior approval.

2.2.24.1 Fuel. 99.995% hydrogen, 40% hydrogen/60% helium, or 40% hydrogen/ 60% nitrogen. The fia manufacturer's recommended fuel shall be used. An attempt shall be made to avoid fuels with oxygen to avoid an oxygen synergism effect that reportedly occurs when oxygen concentration varies significantly from a mean value.

2.2.24.2 Carrier gas. High purity air with less than 1 ppm of organic material (as propane) or less than 0.1% of the span value, whichever is greater.

2.2.24.3 Fia linearity calibration gases. Low-, mid-, and high-range gas mixture standards with a nominal propane concentration of 20 to 30, 45 to 55, and 70 to 80% of the span value in air, respectively. Other calibration values and other span values may be used if it can be shown that more accurate measurements would be achieved.

2.2.24.4 System calibration gas. Gas mixture standard which contains propane in air and which approximates the voc concentration expected for the tedlar gas bag samples.

3. Determination of liquid input weight. A capture efficiency test shall consist of not less than 3 sampling runs. Each run shall cover at least 1 complete production or processing cycle or shall be at least 1 hour in duration. For automotive surface coating operations, the sampling time per run shall be based on coating a minimum of 3 representative vehicles.

3.1 Weight difference. Determine the amount of material introduced to the process as the weight difference of the feed material before and after each sampling run. In determining the total voc-containing liquid usage, account for all of the following:

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

(b) Any solvent added during the test run.

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

3.1.1 Identify all points where voc-containing liquids are introduced to the process. To obtain an accurate measurement of voc-containing liquids, start with an empty fountain, if applicable. After completing the run, drain the liquid in the fountain back into the liquid drum, if possible, and weigh the drum again. Weigh the voc-containing liquids to plus or minus 0.5% of the total weight (full) or plus or minus 0.1% of the total weight of voc-containing liquid used during the sample run, whichever is less. If the residual liquid cannot be returned to the drum, drain the fountain into a preweighed empty drum to determine the final weight of the liquid.

3.1.2 If it is not possible to measure a single representative mixture, then weigh the various components separately, for example, if solvent is added during the sampling run, weigh the solvent before it is added to the mixture. If a fresh drum of voc-containing liquid is needed during the run, then weigh both the empty drum and the fresh drum.

3.2 Volume measurement (alternative). If direct weight measurements are not feasible, the tester may use volume meters, flow rate meters, and density measurements to determine the weight of liquids that are used if it can be demonstrated that the technique produces results equivalent to the direct weight measurements. If a single representative mixture cannot be measured, measure the components separately.

4. Determination of voc content in input liquids.

4.1 Collection of liquid samples.

4.1.1 Collect a 1-pint or larger sample of the voc-containing liquid mixture at each application location at the beginning and end of each test run. A separate sample shall be taken of each VOC-containing liquid that is added to the application mixture during the test run. If a fresh drum is needed during the sampling run, then obtain a sample from the fresh drum.

4.1.2 When collecting the sample, ground the sample container to the coating drum. Fill the sample container as close to the rim as possible to minimize the amount of headspace.

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

4.1.4 Label the container to identify clearly the contents.

4.2 Distillation of VOC.

4.2.1 Assemble the rotary evaporator as shown in figure 1.

4.2.2 Leak check the rotary evaporation system by aspirating a vacuum of approximately 20 mm hg from absolute. Close up the system and monitor the vacuum for approximately 1 minute. If the vacuum falls more than 125 mm hg in 1 minute, repair leaks and repeat.

4.2.3 Deposit approximately 20 mls of the sample (inks, paints, or similar material) into the rotary evaporation distillation vessel.

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

4.2.5 Begin heating the vessel at a rate of 2 to 3 degrees Centigrade per minute, maintaining the vacuum specified in 4.2.3. Care shall be taken to prevent material bumping from the distillation flask.

4.2.6 Continue heating until a temperature of 110 degrees Centigrade is achieved and maintain this temperature for not less than 10 minutes or until the sample has dried in the distillation flask.

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 c_c3 equal the exhaust gas concentration in terms of propane and rf=1.0. Calculate c_voc. Let b_v = 20 liters and calculate m_l, the approximate quantity of liquid to be used to prepare the bag gas sample.

4.3.7 Quickly withdraw an aliquot (approximately 5 microliters) of sample from the distillate vial with the microliter syringe and record its weight from the analytical balance to the nearest 0.01 Mg.

4.3.8 Inject the contents of the syringe through the septum of the volatilization vessel into the glass wool inside the vessel.

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

4.3.10 Record the pressure and temperature of the dilution gas as it is passed through the dry gas meter, as shown in the figure 2 diagram.

4.3.11 After approximately 20 liters of dilution gas have passed into the tedlar bag, close the valve to the dilution air source and record the exact final reading on the dry gas meter.

4.3.12 The gas bag is then analyzed by fia within 1 hour of bag preparation in accordance with the procedures contained in section 4.4.

4.4 Determination of VOC response factor.

4.4.1 Start up the fia instrument using the same settings as used for the gaseous VOC measurements.

4.4.2 Perform the fia analyzer calibration and linearity checks according to the procedure in section 5.1. Record the responses to each of the calibration gases and the back-pressure setting of the fia.

4.4.3 Connect the tedlar bag sample to the fia sample inlet and record the bag concentration in terms of propane. Continue the analysis until a steady reading is obtained for not less than 30 seconds. Record the final reading and proceed with the calculation of the response factor.

4.5 Determination of coating VOC content as VOC (v_u).

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 levels shall 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.

Where:

B_v = Bag sample volume in standard liters.

M_v = Indicated dry gas meter volume, in liters.

T_STD = 293⁰K.

T_M = Meter gas temperature, in ⁰K.

P_M = Meter gas pressure, in mm Hg absolute.

P_STD = 760 mm Hg.

6.2 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.

6.3 Bag sample VOC concentration, as propane, C_c3.

C_c3 = R_c3*K

Where:

C_c3 = Bag sample VOC concentration, as propane, mg C₃/std. liter.

R_c3 = FIA reading for bag gas sample, ppm propane.

6.4 Response factor, RF.

RF = C_voc/C_c3

Where:

RF = Response factor, weight VOC/weight propane.

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

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.

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.

History: 1993 MR 4, Eff. Apr. 28, 1993; 2002 MR 5, Eff. Mar. 19, 2002.

R 336.2011 Reference test method 5B.

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

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

(i) Principle. Particulate matter is withdrawn isokinetically from the source and collected on solid filtering media maintained at stack temperature. The particulate matter mass is determined gravimetrically after removal of uncombined water.

(ii) Applicability. This method is applicable for the determination of particulate emissions from stationary sources as identified in table 31 of R 336.1331. The method is also applicable when specifically provided for in the department’s rules, orders, a permit to install, or a permit to operate.

(iii) Performance test criteria:

(A) A performance test shall consist of a minimum of 3 separate samples of a specific air contaminant conducted within a 36-hour period, unless otherwise authorized by the department. Each of the 3 separate samples shall be obtained while the source is operating at a similar production level. For the purpose of determining compliance with an applicable emission limit, rule, or permit condition, the arithmetic mean of results of the 3 samples shall apply. If a sample is accidentally lost or conditions occur in which 1 of the 3 samples must be discontinued because of forced shutdown, failure of an irreplaceable portion of the sampling train, extreme meteorological conditions, or other circumstances beyond the owner's or operator's control, compliance may, upon the approval of the department, be determined using the arithmetic mean of the results of 2 samples.

(B) For any source that is subject to an emission limitation calculated to 50% excess air, the multipoint, integrated sampling procedure of R 336.2004(1)(c) shall be used for gas analysis. For all other sources that require a determination of the molecular weight of the exhaust, any optional sampling procedure of R 336.2004(1)(c) may be used. Alternatives or modifications to procedures are subject to the approval of the department.

(C) The minimum volume per sample shall be 30 cubic feet of dry gas corrected to standard conditions (70 degrees Fahrenheit, 29.92 inches mercury). Minimum sample time shall be 60 minutes, which may be continuous or a combination of shorter sampling periods for sources that operate in a cyclic manner. Smaller sampling times or sample volumes, if necessitated by process variables or other factors, may be approved by the department.

(D) For any source whose emission control device alters the moisture content of the exhaust gas, a moisture determination shall be performed in a location upstream from the emission control device and in accordance with R 336.2004(1)(d) or an alternative method approved by the department.

(b) The following provisions apply to apparatus:

(i) Sampling train. A schematic of the sampling train used in this method is shown in figure 102. Construction details for many, but not all, of the train components are given in APTD-0581. (See subdivision (g)(ii) of this rule.) For changes from the APTD-0581 document and for allowable modifications to figure 102, the user shall consult with the department.

The operating and maintenance procedures for many, but not all, of the sampling train are described in APTD-0576. (See subdivision (g)(iii) of this rule.) Since correct usage is important in obtaining valid results, all users shall read APTD-0576 and adopt the applicable operating and maintenance procedures outlined in it, unless otherwise specified herein. The sampling train shall consist of the following components:

(A) Probe nozzle. Stainless steel (316) or glass with sharp, tapered leading edge. The angle of taper shall be less than 30 degrees and the taper shall be on the outside to preserve a constant internal diameter. The probe nozzle shall be of the button-hook design, unless otherwise specified by the department. If made of stainless steel, the nozzle shall be constructed from seamless tubing. Other materials of construction may be used, subject to the approval of the department.

A range of nozzle sizes suitable for isokinetic sampling shall be available, for example, 0.32 to 1.27 cm (1/8 to 1/2 in. - or larger if higher volume sampling trains are used - inside diameter (ID) nozzles in increments of 0.16 cm (1/16 in.). Each nozzle shall be calibrated according to the procedures outlined in subdivision (e) of this rule.

(B) Probe liner. Interior surface may be constructed of stainless steel (no specific grade), glass, teflon, or such other material that maintains proper flow at the stack conditions experienced.

(C) Pitot tube. Type S, as described in section 2.1 of method 2, or other device approved by the department. The pitot tube shall be attached to the probe, as shown in figure 102, to allow constant monitoring of the stack gas velocity. The impact (high pressure) opening plane of the pitot tube shall be even with or above the nozzle entry plane (see method 2, figure 2-6b) during sampling. The type S pitot tube assembly shall have a known coefficient, determined as outlined in section 4 of method 2.

(D) Differential pressure gauge. Incline manometer or equivalent devices (2) as described in section 2.2 of method 2. One manometer shall be used for velocity head ( p) readings and the other shall be used for orifice differential pressure readings.

(E) Filter holders. Two separate filter holders in series or 1 filter holder with separate filter supports and seals for 2 filters. One filter holder with 2 filters held in contact with each other is not acceptable. Materials of construction may be stainless steel (316), glass, teflon, or other material approved by the department.

(F) Filter heating system. Auxiliary heating of the filter media is not acceptable. For saturated stack gases, the operator may opt to use filters that do not blind when wet and that do not require heating (see subdivision (c)(i)(A) of this rule).

(G) Condenser. The following system shall be used to determine the stack gas moisture content: Three impingers connected in series with leak-free ground glass fittings or any similar leak-free noncontaminating fittings. All impingers shall be of the Greenburg-Smith design and shall be modified by replacing the tip with a 1.3 cm (1/2 in.) ID glass tube extending to about 1.3 cm (1/2 in.) from the bottom of the flask. Modifications, such as using flexible connections between the impingers or using materials other than glass, are permitted, subject to the approval of the department. The first impinger shall contain a known quantity of water (subdivision (d)(i)(C) of this rule); the second shall be empty; and the third shall contain a known weight of silica gel or equivalent desiccant.

Alternatively, any system that cools the sample gas stream and allows measurement of the water condensed and moisture leaving the condenser, each to within 1 ml or 1 g, may be used, subject to the approval of the department. In any case, the means for measuring the moisture leaving the condenser shall be by passing the sample gas stream through a tared silica gel, or equivalent desiccant, trap with exit gases kept below 20 degrees Centigrade (68 degrees Fahrenheit) and determining the weight gain.

If a determination of the particulate matter collected in the impingers is required by the department’s rules, a permit to install, or a permit to operate, then the impinger system described above shall be used without modification. Contact the department as to the sample recovery and analysis of the impinger contents.

(H) Metering system. Vacuum gauge, leak-free pump, thermometers capable of measuring temperature to within 3 degrees Centigrade (5.4 degrees Fahrenheit), dry-gas meter capable of measuring volume to within 2%, and related equipment as shown in figure 102. Other metering systems capable of maintaining sampling rates within 10% of isokinetic and capable of determining sample volumes to within 2% may be used, subject to the approval of the department. When the metering system is used in conjunction with a pitot tube, the system shall enable checks of isokinetic rates.

Sampling trains utilizing metering systems designed for higher flow rates than those described in APTD-0581 or APTD-0576 may be used if the specifications of this method are met.

(I) Barometer. Mercury, aneroid, or other barometer capable of measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg). In many cases, the barometric reading may be obtained from a nearby national weather service station. In this case, the station value, which is the absolute barometric pressure, shall be requested and an adjustment for elevation differences between the weather station and sampling point shall be applied at a rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 M (100 ft.) elevation increase or vice versa for elevation decrease.

(J) Gas density determination equipment. Temperature sensor and pressure gauge, as described in sections 2.3 and 2.4 of method 2, and gas analyzer, if necessary, as described in method 3. The temperature sensor shall, preferably, be permanently attached to the pitot tube or sampling probe in a fixed configuration such that the tip of the sensor extends beyond the leading edge of the probe sheath and does not touch any metal. Alternatively, the sensor may be attached just before use in the field. If the temperature sensor is attached in the field, then the sensor shall be placed in an interference-free arrangement with respect to the type S pitot tube openings (see method 2, figure 2-7). As a second alternative, if a difference of not more than 1% in the average velocity measurement is to be introduced, then the temperature gauge need not be attached to the probe or pitot tube. This alternative is subject to the approval of the department.

“Construction Details of Isokinetic Source Sampling Equipment,” APTD-0581, April 1971 (PB203-060-LL), and “Maintenance, Calibration, and Operation of Isokinetic Source Sampling Equipment,” APTD-0576, March 1972 (PB209-022-LL), are adopted by reference in this rule. Copies of these documents may be inspected at the Lansing office of the air quality division of the department of environmental quality. Copies of APTD-0581 and APTD-0576 may be obtained from the Department of Environmental Quality, Air Quality Division, P.O. Box 30260, Lansing, Michigan 48909-7760, or from the National Technical Information Service, U.S. Department of Commerce, 5285 Port Royal Road, Springfield, Virginia 22161, at a cost at the time of adoption of these rules of $28.50 each.

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

(A) Probe-liner and probe-nozzle brushes. Nylon bristle brushes with stainless steel wire handles. The probe brush shall have extensions, at least as long as the probe, made of stainless steel, nylon, teflon, or similarly inert material. The brushes shall be properly sized and shaped to brush out the probe liner and nozzle.

(B) Wash bottles -- 2. Glass wash bottles are recommended; the tester may use polyethylene wash bottles, but the acetone should not be stored in polyethylene bottles for longer than 1 month.

(C) Glass sample storage containers. Chemically resistant, borosilicate glass bottles for acetone washes, 500 ml or 1000 ml. Screw cap liners shall either be rubber-backed teflon or shall be constructed so as to be leak-free and resistant to chemical attack by acetone. Narrow-mouth glass bottles are less prone to leakage. Alternatively, polyethylene bottles may be used.

(D) Filter containers. Glass, polyethylene, or aluminum tube containers, unless otherwise specified by the department.

(E) Graduated cylinder or balance. To measure condensed water to within 1 ml or 1 g., graduated cylinders shall have subdivisions of not more than 2 ml. Most laboratory balances are capable of weighing to the nearest 0.5 g or less. Any of these balances may be used here and in paragraph (iii)(D) of this subdivision.

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

(G) Funnel and rubber policeman. To aid in the transfer of silica gel to container; not necessary if silica gel is weighed in the field.

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

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

(A) Glass weighing dishes.

(B) Desiccator.

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

(E) Beakers. 250 ml.

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

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

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

(A) Filters. Two in-stack filters may be any combination of alundum ceramic thimble filters, type RA-98, or glass fiber filters, type A without organic binder. The size of such filters shall allow proper sampling rates to maintain isokinetics using the nozzle sizes specified in subdivision (b)(i)(A) of this rule.

Alternatively, other types of filters may be used, subject to the approval of the department.

(B) Silica gel. Indicating type, 6 to 16 mesh. If previously used, dry at 175 degrees Centigrade (350 degrees Fahrenheit) for 2 hours. New silica gel may be used as received. Alternatively, other types of desiccants that are equivalent or better may be used, subject to the approval of the department.

(C) Water. When analysis of the material caught in the impingers is required, distilled water shall be used. Run blanks before field use to eliminate a high blank of test samples.

(D) Crushed ice.

(E) Stopcock grease. Acetone-insoluble, heat-stable silicone grease. This is not necessary if screw-on connectors with teflon sleeves, or equivalent, are used. Alternatively, other types of stopcock grease may be used, subject to the approval of the department.

If suppliers transfer acetone to glass bottles from metal containers, then acetone blanks shall be run before field use and only acetone with low blank values (less than 0.001%) shall be used. In no case shall a blank value of more than 0.001% of the weight of acetone used be subtracted from the sample weight.

If distilled water is used for washing solvent, use distilled water with less than 0.001% residue. Run blanks before field use to eliminate a high blank on test samples.

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

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

(B) Desiccant. Anhydrous calcium sulfate, indicating type. Alternatively, other types of desiccants may be used, subject to the approval of the department.

(d) The following provisions shall apply to procedure:

(i) Sampling. The complexity of this method is such that, in order to obtain reliable results, testers shall be trained and experienced with the test procedures. Sampling shall comply with the following provisions:

(A) Pretest preparation. All the components shall be maintained and calibrated according to the applicable procedures described in APTD-0576, unless otherwise specified in this rule.

Weigh several 200 to 300 g portions of silica gel in airtight containers to the nearest 0.5 g. Record the total weight of the silica gel plus container on each container. As an alternative, the silica gel need not be preweighed, but may be weighed directly in its impinger or sampling holder just before train assembly.

Check filters visually against light for irregularities, flaws, pinhole leaks, or cracks. Label filters of the proper size on the back side using numbering machine ink. As an alternative, label the shipping containers (subdivision (b)(ii)(D) of this rule) and keep the filters in these containers at all times, except during sampling and weighing.

Dry the filters in an oven at 105 degrees Centigrade (220 degrees Fahrenheit) for a minimum of 2 hours, cool for at least 1 hour in a desiccator containing anhydrous calcium sulfate, and individually weigh and record their weights to the nearest 0.1 mg. During the weighing, the filter shall not be exposed to the laboratory atmosphere for a period of more than 2 minutes and a relative humidity above 50%. Procedures, other than those specified, that account for relative humidity effects may be used, subject to the approval of the department.

(B) Preliminary determinations. Select the sampling site and the minimum number of sampling points according to method 1 or as specified by the department. Determine the stack pressure, temperature, and the range of velocity heads using method 2; it is recommended that a leak check of the pitot lines (see method 2, section 3.1) be performed. Determine the moisture content using approximation method 4, or its alternatives, for the purpose of making isokinetic sampling rate settings. Determine the stack gas dry molecular weight, as described in method 2, section 3.6; if integrated method 3 sampling is used for molecular weight determination, the integrated bag sample shall be taken simultaneously with, and for the same total length of time as, the particulate sample run.

Select a nozzle size based on the range of velocity heads so that it is not necessary to change the nozzle size to maintain isokinetic sampling rates. During the run, do not change the nozzle size. Ensure that the proper differential pressure gauge is chosen for the range of velocity heads encountered (see section 2.2 of method 2).

Select a suitable probe liner and probe length so that all traverse points may be sampled. For large stacks, sampling from opposite sides of the stack may reduce the length of probes.

Select a total sampling time greater than or equal to the minimum total sampling time specified in the department’s rules so that the sampling time per point is not less than 5 minutes, unless approved by the department, or some greater time interval as specified by the department, and so that the sample volume taken, corrected to standard conditions, exceeds the required minimum total gas sample volume. The latter is based on an approximate average sampling rate.

The number of minutes sampled at each point may be an integer or an integer plus 1/2 minute to avoid timekeeping errors.

In some circumstances, such as in batch cycles, it may be necessary to sample for shorter times at the traverse points and to obtain smaller gas sample volumes. In these cases, the department’s approval shall first be obtained.

(C) Preparation of collection train. During preparation and assembly of the sampling train, keep all openings where contamination can occur covered until just before assembly or until sampling is about to begin.

Place 100 ml of water in the first impinger, leave the second impinger empty, and transfer approximately 200 to 300 g of preweighed silica gel from its container to the third impinger. More silica gel may be used, but care shall be taken to ensure that it is not entrained and carried out from the impinger during sampling. Place the container in a clean place for later use in the sample recovery. Alternatively, the weight of the silica gel plus impinger may be determined to the nearest 0.5 g and recorded.

Using tweezers or clean disposable surgical gloves, place a labeled (identified) and weighed filter in each filter holder. Be sure that the filter is properly centered and the gasket properly placed so as to prevent the sample gas stream from circumventing the filter.

Install the selected nozzle using a Viton A 0-ring when stack temperatures are less than 260 degrees Centigrade (500 degrees Fahrenheit) and an asbestos string gasket when temperatures are higher. See APTD-0576 for requirements. Other connecting systems using either 310 stainless steel or teflon ferrules may be used to form a leak-free direct mechanical connection. Mark the probe with heat-resistant tape or by some other method to denote the proper distance into the stack or duct for each sampling point.

Set up the train as in figure 102. If necessary, use a very light coat of silicone grease on all ground glass joints. Grease only the outer portion (see APTD-0576) to avoid the possibility of contamination by the silicone grease.

Place crushed ice around the impingers.

(D) Leak check procedures:

(1) Pretest leak check. A pretest leak check is strongly recommended, but not required, to prevent invalid sampling and wasted time. If the tester opts to conduct the pretest leak check, the following procedure shall be used:

Perform the leak check on the entire system, including filter housings and nozzle, by plugging the nozzle and pulling a 380 mm Hg (15 in. Hg) vacuum. Alternatively, a lower vacuum may be used if it is not exceeded during the test. Leakage rates in excess of 4% of the average sampling rate or 0.00057 m³/min (0.02 cfm), whichever is less, are unacceptable.

The following leak check instructions for the sampling train described in APTD-0576 and APTD-0581 may be helpful. Start the pump with the bypass valve fully open and the coarse adjust valve completely closed. Partially open the coarse adjust valve and slowly close the bypass valve until the desired vacuum is reached. Do not reverse the direction of the bypass valve; this will cause water to back up into the flexible sample tube and the probe. If the desired vacuum is exceeded, either leak-check at this higher vacuum or end the leak check and start over.

When the leak check is completed, first slowly remove the plug from the inlet to the nozzle and immediately turn off the vacuum pump. This prevents the water in the first impinger from being forced backward into the sample tube and prevents silica gel from being entrained backward into the second impinger.

(2) Leak checks during sample run. If, during the sampling run, a component (such as a filter assembly or impinger) change becomes necessary, a leak check shall be conducted immediately before the change is made. The leak check shall be done according to the procedure outlined in paragraph (i)(D)(1) of this subdivision, except that it shall be done at a vacuum equal to or greater than the maximum value recorded up to that point in the test. If the leakage rate is not more than 0.00057 m³/min (0.02 cfm) or 4% of the average sampling rate, whichever is less, then the results are acceptable and no correction need be applied to the total volume of dry gas metered. If a higher leakage rate is obtained, then the tester shall either record the leakage rate and plan to correct the sample volume, as shown in subdivision (f)(iii) of this rule, or shall void the sampling run.

Immediately after component changes, leak checks may be performed. If leak checks are done, then the procedure outlined in paragraph (i)(D)(1) of this subdivision shall be used.

(3) Post-test leak check. A leak check is required at the conclusion of each sampling run. The leak check shall be performed in accordance with the procedures in paragraph (i)(D)(1) of this subdivision, except that it shall be conducted at a vacuum equal to or greater than the maximum value reached during the sampling run. If the leakage rate is not more than 0.00057 m³/min (0.02 cfm) or 4% of the average sampling rate, whichever is less, then the results are acceptable and no correction need be applied to the total volume of dry gas metered. If a higher leakage rate is obtained, then the tester shall either record the leakage rate and correct the sample volume, as shown in subdivision (f)(iii) of this rule, or shall void the sampling run.

(E) Particulate train operation. During the sampling run, maintain an isokinetic sampling rate that is within 10% of true isokinetic, unless otherwise specified by the department.

For each run, record the data required on a data sheet such as the data sheet in figure 104. Record the initial dry-gas meter reading. Record the dry-gas meter readings at the beginning and end of each sampling time increment, when changes in flow rates are made, before and after each leak check, and when sampling is halted. Take other readings required by figure 104 at least once at each sample point during each time increment, and take additional readings when significant changes (20% variation in velocity head readings) necessitate additional adjustments in flow rate. Level and zero the manometer. Because the manometer level and zero may drift due to vibrations and temperature changes, make periodic checks during the traverse.

Clean the portholes before the test run to minimize the chance of sampling deposited material. To begin sampling, remove the nozzle cap and verify that the pitot tube and probe are properly positioned. Position the nozzle at the first traverse point with the tip pointing directly into the gas stream. Immediately start the pump and adjust the flow to isokinetic conditions. Nomographs that aid in the rapid adjustment of the isokinetic sampling rate without excessive computations are available. These nomographs are designed for use when the type S pitot tube coefficient is 0.85 ±0.02 and the stack gas equivalent density (dry molecular weight) is equal to 29 ±4. APTD-0576 details the procedure for using the nomographs. If C_p and M_d are outside the above stated ranges, do not use the nomographs unless appropriate steps (subdivision (g)(iv) of this rule) are taken to compensate for the deviations.

When the stack is under significant negative 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 (paragraph (i)(D)(2) of this subdivision). The total particulate weight shall include the summation of all filter assembly catches.

A single train shall be used for the entire sample run, except in cases where simultaneous sampling is required in 2 or more separate ducts, at 2 or more different locations within the same duct, or where equipment failure necessitates a change of trains. In all other situations, the use of 2 or more trains shall be subject to the approval of the department.

When 2 or more trains are used, separate analyses of the front-half and, if applicable, impinger catches from each train shall be performed, unless identical nozzle sizes were used on all trains. If identical nozzle sizes were used, the front-half catches from the individual trains may be combined, as may the impinger catches, and 1 analysis of front-half catch and 1 analysis of impinger catch may be performed. Consult with the department for details concerning the calculation of results when 2 or more trains are used.

At the end of the sample run, turn off the coarse adjust valve, remove the probe and nozzle from the stack, turn off the pump, record the final dry-gas meter reading, and conduct a post-test leak check, as outlined in paragraph (i)(D)(3) of this subdivision. Leak-check the pitot lines as described in method 2, section 3.1; the lines shall pass this leak check to validate the velocity head data.

(F) Calculation of percent isokinetic. Calculate percent isokinetic (see subdivision (f) of this rule) to determine if the run was valid or if another test run should be made. If there was difficulty in maintaining isokinetic rates due to source conditions, consult with the department for possible variance on the isokinetic rates.

(ii) Sample recovery. Proper cleanup procedure begins as soon as the probe is removed from the stack at the end of the sampling period. Allow the probe to cool.

When the probe can be safely handled, wipe off all external particulate matter near the tip of the probe nozzle and place a cap over it to prevent losing or gaining particulate matter. Do not cap off the probe tip tightly while the sampling train is cooling down as this creates a vacuum in the filter holder and draws water from the impingers into the sample tube.

Before moving the sampling train to the cleanup site, make sure all condensed water in the probe and flexible sample lines are drained into the first impinger. Disconnect all sample lines and remove the nozzle-filter set assembly from the probe. Cap all openings to prevent contamination or accidental loss of sample. Remove all excess particulate from the exterior of the nozzle-filter assembly to prevent contamination during disassembly.

Transfer the nozzle-filter set assembly and impinger set to the cleanup area. The cleanup area shall be clean and protected from the wind so that the chances of contaminating or losing the sample are minimized.

Save a portion of the solvent used for cleanup as a blank. Take 200 ml of this solvent directly from the wash bottle being used and place it in a glass sample container labeled "solvent blank".

Inspect the train before and during disassembly and note any abnormal conditions. Treat the samples in the following manner:

Container Nos. 1, 1A. Carefully remove the filters from the filter holders and place in their identified containers. Use a pair of tweezers or clean disposable surgical gloves, or both, to handle the filters. Carefully transfer to the container any particulate matter or filter fibers, or both, that adhere to the filter holder gasket by using a dry nylon bristle brush or sharp-edged blade, or both. Seal the containers.

Container No. 2. Taking care to see that particulate on the outside of the nozzle and filter holders does not get into the sample, the 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 No. 3. Note the color of the indicating silica gel to determine if it has been completely spent and make a notation of its condition. Transfer the silica gel from the third impinger to its original container and seal. A funnel may make it easier to pour the silica gel without spilling it. A rubber policeman may be used as an aid in removing the silica gel from the impinger. It is not necessary to remove the small amount of dust particles that adhere to the impinger wall and are difficult to remove. Since the gain in weight will be used for moisture calculations, do not use any water or other liquids to transfer the silica gel. If a balance is available in the field, follow the procedure for container No. 3 in paragraph (iii) of this subdivision.

Impinger water. Treat the impingers in the following manner: Make a notation of any color or film in the liquid catch. Measure the liquid that is in the first 2 impingers to within ±1 ml by using a graduated cylinder or by weighing it to within ±1.0 g by using a balance if one is available. Record the volume or weight of liquid present. This information is required to calculate the moisture content of the effluent gas.

Discard the liquid after measuring and recording the volume or weight, unless analysis of the impinger catch is required (subdivision (b)(i)(G) of this rule).

If a different type of condenser is used, measure the amount of moisture condensed either volumetrically or gravimetrically.

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

(iii) Analysis. Record the data required on a sheet such as the sheet in figure 106. Handle each sample container in the following manner:

Container Nos. 1, 1A. Analyze and report each filter separately. Transfer the filter and any loose particulate from the sample container to a tared-glass weighing dish. Dry the filter in an oven at 105 degrees Centigrade (220 degrees Fahrenheit) for a minimum of 2 hours, cool for at least 1 hour in a desiccator containing anhydrous calcium sulfate and weigh and record its weight to the nearest 0.1 mg. During the weighing the filter shall not be exposed to the laboratory atmosphere for a period greater than 2 minutes or a relative humidity above 50%. Procedures, other than those specified, that account for relative humidity effects may be used, subject to the approval of the department. The method used for drying and weighing of filters shall be consistent before and after the test.

Container No. 2. Note the level of liquid in the container and confirm on the analysis sheet if leakage occurred during transport. If a noticeable amount of leakage has occurred, then either void the sample or use methods, subject to the approval of the department, to correct the final results. Measure the liquid in this container either volumetrically to ±1 ml or gravimetrically to ±1.0 g. Transfer the contents to a tared 250 ml beaker and evaporate to dryness either at ambient temperature and pressure for acetone or at 95 degrees Centigrade (203 degrees Fahrenheit) in an oven for distilled water. Then subject the sample to 250 degrees Centigrade (482 degrees Fahrenheit) in an oven for 2 to 3 hours. Desiccate 24 hours and weigh to a constant weight. Report the results to the nearest 0.1 mg.

Container No. 3. Weigh the spent silica gel, or silica gel plus impinger, to the nearest 0.5 g using a balance. This step may be conducted in the field.

"Solvent blank" container. Measure solvent in this container either volumetrically or gravimetrically. Transfer the contents to a tared 250 ml beaker and evaporate to dryness either at ambient temperature and pressure for acetone or at 95 degrees Centigrade (203 degrees Fahrenheit) in an oven for distilled water. Then subject the sample to 250 degrees Centigrade (482 degrees Fahrenheit) in an oven for 2 to 3 hours. Desiccate for 24 hours and weigh to a constant weight. Report the results to the nearest 0.1 mg.

If acetone is used, the contents of Container No. 2, as well as the acetone blank container, may be evaporated at temperatures higher than ambient. If evaporation is done at an elevated temperature, then the temperature shall be closely supervised, and the contents of the beaker shall be swirled occasionally to maintain an even temperature. Use extreme care, as acetone is highly flammable and has a low flash point.

(e) Calibration. Maintain a laboratory log of all calibrations. Calibrations shall comply with the following provisions:

(i) Probe nozzle. Probe nozzles shall be calibrated before their initial use in the field. Using a micrometer, measure the inside diameter of the nozzle to the nearest 0.025 mm (0.001 in.). Make 3 separate measurements using different diameters each time and obtain the average of the measurements. The difference between the high and low numbers shall not exceed 0.1 mm (0.004 in.). When nozzles become nicked, dented, or corroded, they shall be reshaped, sharpened, and recalibrated before use. Each nozzle shall be permanently and uniquely identified.

(ii) Pitot tube. The type S pitot tube assembly shall be calibrated according to the procedures in section 4 of method 2.

(iii) Metering system. Before its initial use in the field, the metering system shall be calibrated according to the procedure in APTD-0576. Instead of physically adjusting the dry-gas meter dial readings to correspond to the wet-test meter readings, calibration factors may be used to mathematically correct the gas meter dial readings to the proper values. Before calibrating the metering system, a leak check may be conducted. For metering systems having diaphragm or rotary pumps, the normal leak check procedure will not detect leakages within the pump. For these cases, the following leak check procedure may be used: Make a 10-minute calibration run at 0.00057 m³/min (0.02 cfm); at the end of the run, take the difference of the measured wet-test meter and dry-gas meter volumes; divide the difference by 10 to get the leak rate. The leak rate shall not exceed 0.00057 m³/min (0.02 cfm).

After each field use, the calibration of the metering system shall be checked by performing 3 calibration runs at a single, intermediate orifice setting, based on the previous field test, with the vacuum set at the maximum value reached during the test series. To adjust the vacuum, insert a valve between the wet-test meter and the inlet of the metering system. Calculate the average value of the calibration factor. If the calibration has changed by more than 5%, then recalibrate the meter over the full range of orifice settings, as outlined in APTD‑0576.

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

Alternative procedures, such as using the orifice meter coefficients, may be used, subject to the approval of the department. If the dry-gas meter coefficient values obtained before and after a test series differ by more than 5%, then the test series shall be performed using whichever meter coefficient value (before or after) gives the lower value of total sample volume.

(iv) Temperature gauges. Use the procedure in section 4.3 of method 2 to calibrate in-stack temperature gauges. Dial thermometers, such as those used for the dry-gas meter and condenser outlet, shall be calibrated against mercury-in-glass thermometers.

(v) Leak check of metering system shown in figure 102. That portion of the sampling train from the pump to the orifice meter shall be leak-checked before initial use and after each shipment. Leakage after the pump will result in less volume being recorded than is actually sampled. The following procedure is suggested (see figure 107): Close the main valve on the meter box. Insert a 1-hole rubber stopper with rubber tubing attached into the orifice exhaust pipe. Disconnect and vent the low side of the orifice manometer. Close off the low side orifice tap. Pressurize the system to 13 to 18 cm (5 to 7 in.) water column by blowing into the rubber tubing. Pinch off the tubing and observe the manometer for 1 minute. A loss of pressure on the manometer indicates a leak in the meter box; leaks, if present, shall be corrected.

(vi) Barometer. Calibrate against a mercury barometer.

(f) Calculations. When carrying out calculations, retain at least 1 extra decimal figure beyond that of the acquired data. Round off figures after the final calculation. Other forms of the equations may be used if they give equivalent results. The following provisions apply to calculations:

(i) Nomenclature:

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

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

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

Bwi = Percent water vapor in gas entering source particulate control device determined by method 4.

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

Ca = Wash blank residue concentration, mg/g.

Cs = Concentration of particulate matter in stack gas, pounds per 1,000 pounds of actual stack gas.

CsD = Concentration of particulate matter in stack gas, moisture excluded, pounds per 1000 pounds of dry stack gas.

Cs50 = Concentration of particulate matter corrected to 50% excess air, pounds per 1000 pounds of stack gas.

Cs50D = Concentration of particulate matter corrected to 50% excess air, excluding any water addition from a collector, pounds per 1000 pounds of stack gas.

E = Mass emission rate of particulate, lb/hr.

F50 = Concentration conversion factor to 50% excess air with no moisture alterations in exhaust.

F50D = Concentration conversion factor to 50% excess air, excluding any moisture added to exhaust gas by pollution collection system.

FD = Concentration conversion factor to dry basis, excluding any water in the stack gas.

I = Percent of isokinetic sampling.

La = Maximum acceptable leakage rate for either a pretest leak check or for a leak check following a component change; equal to 0.00057 m³/min (0.02 cfm) or 4% of the average sampling rate, whichever is less.

Li = Individual leakage rate observed during the leak check conducted before the "ith" component change (i = 1, 2, 3 . . . . n), m³/min (cfm).

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

Md = Molecular weight of dry stack gas, g/g mole (lb/lb-mole), calculated by method 3, equation 3-2, using data from integrated method 3.

mn = Total amount of particulate matter collected, mg.

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

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

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

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

Ps = Absolute stack gas pressure.

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

R = Ideal gas constant, 0.06236 mm Hg-m³/°K-g-mole (21.85 in. Hg-ft.³/°R‑lb-mole).

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

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

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

Va = Volume of solvent blank, ml.

Vaw = Volume of solvent used in wash, ml.

Vlc = Total volume of liquid collected in impingers and silica gel (see figure 106), ml.

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

Vm(std) = Volume of gas sample measured by the dry-gas meter, corrected to standard conditions, dscm (dscf).

Vw(std) = Volume of water vapor in the gas sample, corrected to standard conditions, scm (scf).

Vs = Stack gas velocity, calculated by method 2, equation 2-9, using data obtained from method 5, m/sec (ft./sec).

Wa = Weight of residue in solvent wash, mg.

Y = Dry-gas meter calibration factor.

DH = Average pressure differential across the orifice meter (see figure 104), mm H20 (in. H20).

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

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

pa = Density of solvent, mg/ml.

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

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

q = Total sample time, min.

q1 = Sample time, interval, from the beginning of a run until the first component change, min.

qi = Sampling time interval, between 2 successive component changes, beginning with the interval between the first and second changes, min.

qp = Sampling time interval, from the final (nth) component change until the end of the sampling run, min.

13.6 = Specific gravity of mercury.

60 = Sec/min.

100 = Conversion to percent.

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

453.6 = Conversion of pounds to grams.

3600 = Conversion of hours to sec.

1000 = Conversion of 1000 lb units to lb units.

(ii) Average the dry-gas meter temperature and average the orifice pressure drop. See data sheet (figure 5-2).

(iii) Dry gas volume. Correct the sample volume measured by the dry-gas meter to standard conditions (21.11 degrees Centigrade, 760 mm Hg or 70 degrees Fahrenheit, 29.92 in. Hg) by using equation 5-1.

equation 5-1

Where:

K₁ = 0.3869 °K/mm Hg for metric units.

= 17.71 °R/in. Hg for English units.

Equation 5-1 may be used as written. However, if the leakage rate observed during any of the mandatory leak checks (for example, the post-test leak check or leak checks conducted before component changes) exceeds L_a, equation 5-1 shall be modified in the following manner:

(A) Case I. No component changes made during sampling run. In this case, replace V_m in equation 5-1 with the following expression:

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

and substitute only for those leakage rates (L_i or L_p) that exceed L_a.

(iv) Volume of water vapor.

equation 5-2

Where:

K₂ = 0.001338 m³/ml for metric units.

(v) Moisture content.

equation 5-3

In saturated or water droplet-laden gas streams, 2 calculations of the moisture content of the stack gas shall be made: 1 from the impinger analysis (equation 5-3), and a second from the assumption of saturated conditions. The lower of the 2 values of B_ws shall be considered correct. The procedure for determining the moisture content based upon assumption of saturated conditions is given in the note of section 1.2 of method 4. For the purpose of this method, the average stack gas temperature from figure 104 may be used to make the determination, if the accuracy of the instack temperature sensor is ±1 degree Centigrade (2 degrees Fahrenheit).

(vi) Solvent blank concentration.

equation 5-4

(vii) Solvent wash blank.

equation 5-5

(viii) Total particulate weight. Determine the total particulate catch from the sum of the weights obtained from containers 1, 1A, and 2 less the wash solvent blank (see figure 106).

Refer to subdivision (d)(i)(E) of this rule to assist in the calculation of results involving 2 or more pairs of filters or 2 or more sampling trains.

(ix) Sampled gas density. Determine the density of the gas sampled from the stack, at standard conditions (lb/ft.³).

equation 5-6

(x) Total weight of gas sampled (lbs).

equation 5-7

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

equation 5-8

(xii) Excess air and moisture correction factors:

(A) Correction factor to 50% excess air for those sources with or without any particulate collector where no increase in moisture content of the exhaust gas occurs after the process and before the point of sampling.

equation 5-9

(B) Correction factor to 50% excess air for those sources with a wet collection device (scrubber) that increases the moisture content of the exhaust gas after the process and before the point of sampling.

equation 5-10

equation 5-11

(xiii) Converted particulate concentrations, where applicable under the department’s rules or permit.

equation 5-12

equation 5-13

equation 5-14

(xiv) Mass emission rate (lb/hr).

equation 5-15

Where:

K₃ = 63.77 for English units.

(xv) Isokinetic variation:

(A) Calculation from raw data.

equation 5-16

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

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 MR 2, Eff. Feb. 22, 1985; 1992 MR 9, Eff. Oct. 31, 1992; 2002 MR 5, Eff. Mar. 19, 2002; 2004 MR 18, Eff. Oct. 15, 2004; 2005 MR 8, Eff. April 29, 2005.

R 336.2012 Reference test method 5C.

Rule 1012. Reference test method 5C, outstack filtration method, reads as follows:

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

(i) Principle. Particulate matter is withdrawn isokinetically from the source and collected on solid filtering media maintained at a temperature in the range of 120 ±14 degrees Centigrade (248 ±25 degrees Fahrenheit) or such other temperature as specified by the department’s rules or a permit condition, or as approved by the department for a particular application. The particulate mass, which includes any material that condenses at or above the filtration temperature, is determined gravimetrically after removal of uncombined water.

(iii) Performance test criteria:

(C) The minimum volume per sample shall be 30 cubic feet of dry gas corrected to standard conditions (70 degrees Fahrenheit, 29.92 inches mercury). Minimum sample time shall be 60 minutes, which may be continuous or a combination of shorter sampling periods for sources that operate in a cyclic manner. Smaller sampling times or sample volumes, when necessitated by process variables or other factors, may be 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. 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, consult with the department.

The operating and maintenance procedures for many, but not all, of the sampling train are described in APTD-0576 (subdivision (g)(iii) of this rule). Since correct usage is important in obtaining valid results, all users shall read APTD-0576 and adopt the applicable operating and maintenance procedures outlined in it, unless otherwise specified herein. The sampling train consists of the following components:

A range of nozzle sizes suitable for isokinetic sampling shall be available, for example, 0.32 to 1.27 cm (1/8 to 1/2 in.) - or larger if higher volume sampling trains are used - inside diameter (ID) nozzles in increments of 0.16 cm (1/16 in.). Each nozzle shall be calibrated according to the procedures outlined in subdivison (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 which utilize the calibration curves of APTD-0576, or calibrated according to the procedure outlined in APTD-0576, 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 shall 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 shall 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 section 2.1 of method 2, or other device approved by the department. The pitot tube shall be attached to the probe, as shown in figure 103, to allow constant monitoring of the stack gas velocity. The impact (high pressure) opening plane of the pitot tube shall be even with or above the nozzle entry plane (see method 2, figure 2-6b) during sampling. The type S pitot tube assembly shall have a known coefficient, determined as outlined in section 4 of method 2.

(D) Differential pressure gauge. Incline manometer or equivalent devices (2), as described in section 2.2 of method 2. One manometer shall be used for velocity head ( p) readings, and the other shall be used for orifice differential pressure readings.

(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) shall 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 shall be used to determine the stack gas moisture content: Three impingers connected in series with leak-free ground glass fittings or any similar leak-free noncontaminating fittings. All impingers shall be of the Greenburg-Smith design and shall be modified by replacing the tip with a 1.3 cm (1/2 in.) ID glass tube extending to about 1.3 cm (1/2 in.) from the bottom of the flask. Modifications, such as using flexible connections between the impingers or using materials other than glass, are permitted subject to the approval of the department’s staff. The first impinger shall contain a known quantity of water (subdivision (d)(i)(C) of this rule), the second shall be empty, and the third shall contain a known weight of silica gel or equivalent desiccant.

Alternatively, any system that cools the sample gas stream and allows measurement of the water condensed and moisture leaving the condenser, each to within 1 ml or 1 g, may be used subject to the approval of the department. In any case, the means for measuring the moisture leaving the condenser shall be by passing the sample gas stream through a tared silica gel, or equivalent desiccant, trap with exit gases kept below 20 degrees Centigrade (68 degrees Fahrenheit) and determining the weight gain.

If a determination of the particulate matter collected in the impingers is required by the department’s rules, a permit to install, or a permit to operate, the impinger system described in this subparagraph shall be used, without modification. Contact the department as to the sample recovery and analysis of the impinger contents.

(H) Metering system. Vacuum gauge, leak-free pump, thermometers capable of measuring temperature to within 3 degrees Centigrade (5.4 degrees Fahrenheit), dry-gas meter capable of measuring volume to within 2%, and related equipment as shown in figure 103. Other metering systems capable of maintaining sampling rates within 10% of isokinetic and capable of determining sample volumes to within 2% may be used, subject to the approval of the department. When the metering system is used in conjunction with a pitot tube, the system shall enable checks of isokinetic rates.

Sampling trains utilizing metering systems designed for higher flow rates than those described in APTD-0581 or APTD-0576 may be used if the specifications of this method are met.

(I) Barometer. Mercury, aneroid, or other barometer capable of measuring atmospheric pressure to within 2.5 mm Hg (0.1 in. Hg). In many cases, the barometric reading may be obtained from a nearby national weather service station. When obtained from this source, the station value, which is the absolute barometric pressure, shall be requested and an adjustment for elevation differences between the weather station and sampling point shall be applied at a rate of minus 2.5 mm Hg (0.1 in. Hg) per 30 m (100 ft.) elevation increase or vice versa for elevation decrease.

(J) Gas density determination equipment. Temperature sensor and pressure gauge, as described in sections 2.3 and 2.4 of method 2, and gas analyzer, if necessary, as described in method 3. The temperature sensor shall, preferably, be permanently attached to the pitot tube or sampling probe in a fixed configuration such that the tip of the sensor extends beyond the leading edge of the probe sheath and does not touch any metal. Alternatively, the sensor may be attached just prior to use in the field. Note, however, that if the temperature sensor is attached in the field, the sensor shall be placed in an interference-free arrangement with respect to the type S pitot tube openings (see method 2, figure 2.7). As a second alternative, if a difference of not more than 1% in the average velocity measurement is to be introduced, 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 are needed:

(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, 500 ml or 1000 ml. Screw cap liners shall either be rubber-backed teflon or shall be constructed so as to be leak-free and resistant to chemical attack by acetone. Narrow-mouth glass bottles have been found to be less prone to leakage. Alternatively, polyethylene bottles may be used.

(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 ml or 1 g. Graduated cylinders shall have subdivisions of not more than 2 ml. Most laboratory balances are capable of weighing to the nearest 0.5 g or less. Any of these balances 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. Glass or polyethylene, to aid in sample recovery.

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

(A) Glass weighing dishes.

(B) Desiccator.

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

(E) Beakers. 250 ml.

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

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

(i) Sampling. 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 such filters shall allow proper sampling rates to maintain isokinetics using the nozzle sizes specified in subdivision (b)(i)(A) of this rule.

Alternatively, other types of filters may be used, subject to the approval of the department.

(B) Silica gel. Indicating type, 6 to 16 mesh. If previously used, dry at 175 degrees Centigrade (350 degrees Fahrenheit) for 2 hours. New silica gel may be used as received. Alternatively, other types of desiccants (equivalent or better) may be used, subject to the approval of the department.

(C) Water. When analysis of the material caught in the impingers is required, distilled water shall be used. Run blanks prior to field use to eliminate a high blank on test samples.

(D) Crushed ice.

(ii) Sample recovery. Washing solvent. Either acetone or distilled water may be used for sample recovery. If acetone is used for washing solvent, then reagent grade, less than 0.001% residue, in glass bottles is required. Acetone from metal containers generally has a high residue blank and shall not be used. Suppliers sometimes transfer acetone to glass bottles from metal containers; thus, acetone blanks shall be run prior to field use and only acetone with low blank values (less than 0.001%) shall be used. A blank value of more than 0.001% of the weight of acetone used shall 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) 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 apply to procedure:

(A) Pretest preparation. All the components shall be maintained and calibrated according to the applicable procedures described in APTD-0576, unless otherwise specified in this rule.

Dry the filters in an oven at 105 degrees Centigrade (220 degrees Fahrenheit) for a minimum of 2 hours, cool for at least 1 hour in a desiccator containing anhydrous calcium sulfate, and individually weigh and record their weights to the nearest 0.1 mg. During the weighing, the filters shall not be exposed to the laboratory atmosphere for a period of more than 2 minutes and a relative humidity above 50%. Procedures, other than those specified, that account for relative humidity effects may be used, subject to the approval of the department.

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 section 2.2 of 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.

Place 100 ml of water in the first impinger, leave the second impinger empty, and transfer approximately 200 to 300 g of preweighed silica gel from its container to the third impinger. More silica gel may be used, but care should be taken to ensure that it is not entrained and carried out from the impinger during sampling. Place the container in a clean place for later use in the sample recovery. Alternatively, the weight of the silica gel plus impinger may be determined to the nearest 0.5 g and recorded.

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 0ring when stack temperatures are less than 260 degrees Centigrade (500 degrees Fahrenheit) and an asbestos string gasket when temperatures are higher. See APTD-0576 for 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. If necessary, use a very light coat of silicone grease on all ground glass joints. Grease only the outer portion (see APTD-0576) to avoid the possibility of contamination by the silicone grease.

Place crushed ice around the impingers.

(D) Leak check procedures:

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 0-ring or other leak-free connection is used in assembling the probe nozzle to the probe liner, leakcheck the train at the sampling site by plugging the nozzle and pulling a 380 mm Hg (15 in. Hg) vacuum. A lower vacuum may be used, if it is not exceeded during the test.

If an asbestos string is used, do not connect the probe to the train during the leak check. Instead, leak check the train by first plugging the inlet to the filter holder (cyclone, if applicable) and pulling a 380 mm Hg (15 in. Hg) 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 25 mm Hg (1 in. Hg) vacuum; alternatively, the probe may be leak checked with the rest of the sampling train, in 1 step, at 380 mm Hg (15 in. Hg) vacuum. Leakage rates in excess of 4% of the average sampling rate or 0.00057 m³/min (0.02 cfm), whichever is less, are unacceptable.

The following leak check instructions for the sampling train described in APTD-0576 and APTD-0581 may be helpful. Start the pump with the bypass valve fully open and the coarse adjust valve completely closed. Partially open the coarse adjust valve and slowly close the bypass valve until the desired vacuum is reached. Do not reverse the direction of the bypass valve; this will cause water to back up into the 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.

(2) Leak checks during sample run. If, during the sampling run, a component (such as a filter assembly or impinger) change becomes necessary, a leak check shall be conducted immediately before the change is made. The leak check shall be done according to the procedure outlined in paragraph (i)(D)(1) of this subdivision, except that it shall be done at a vacuum equal to or greater than the maximum value recorded up to that point in the test. If the leakage rate is found to be not more than 0.00057 m³/min (0.02 cfm) 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 this rule, or shall void the sampling run.

Immediately after component changes, leak checks are optional; if such leak checks are done, the procedure outlined in paragraph (i)(D)(1) of this subdivision shall be used.

(3) Post-test leak check. A leak check is mandatory at the conclusion of each sampling run. The leak check shall be done in accordance with the procedures outlined in paragraph (i)(D)(1) of this subdivision, except that it shall be conducted at a vacuum equal to or greater than the maximum value reached during the sampling run. If the leakage rate is found to be not more than 0.00057 m³/min (0.02 cfm) 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 this rule, or shall void the sampling run.

(E) Particulate train operation. During the sampling run, maintain an isokinetic sampling rate that is within 10% of true isokinetic, unless otherwise specified by the department.

For each run, record the data required on a data sheet such as the one shown in figure 104. 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 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 prior to the test run to minimize the chance of sampling deposited material. To begin sampling, remove the nozzle cap and verify that the pitot tube and probe are properly positioned. Position the nozzle at the first traverse point with the tip pointing directly into the gas stream. Immediately start the pump and adjust the flow to isokinetic conditions. Nomographs that aid in the rapid adjustment of the isokinetic sampling rate without excessive computations are available. These nomographs are designed for use when the type S pitot tube coefficient is 0.85 ±0.02 and the stack gas equivalent density (dry molecular weight) is equal to 29 ±4. APTD-0576 details the procedure for using the nomographs. If C_p and M_d are outside the above stated ranges, do not use the nomographs uless appropriate steps (see subdivision (g)(iv) of this rule) are taken to compensate for the deviations.

When the probe is in position, block off the openings around the probe and porthole to prevent unrepresentative dilution of the gas stream.

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 paragraph (i)(D)(2) of this subdivision). The total particulate weight shall include the summation of all filter assembly catches.

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 paragraph (i)(D)(3). Also, leak check the pitot lines as described in method 2, section 3.1; the lines shall pass this leak check to validate the velocity head data.

(F) Calculation of percent isokinetic. Calculate percent isokinetic (see subdivision (f) of this rule) to determine 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.

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 shall be clean and protected from the wind so that the chances of contaminating or losing the sample are minimized.

Save a portion of the solvent used for cleanup as a blank. Take 200 ml of this solvent directly from the wash bottle being used and place it in a glass sample container labeled "solvent blank."

Inspect the train prior to and during disassembly and note any abnormal conditions. Treat the samples as follows:

Container No. 2. Taking care to see that dust on the outside of the probe or other exterior surfaces does not get into the sample, the testor 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 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 be used to 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.

Container No. 3. Note the color of the indicating silica gel to determine if it has been completely spent and make a notation of its condition. Transfer the silica gel from the third impinger to its original container and seal. A funnel may make it easier to pour the silica gel without spilling it. A rubber policeman may be used as an aid in removing the silica gel from the impinger. It is not necessary to remove the small amount of dust particles that adhere to the impinger wall and are difficult to remove. Since the gain in weight is to be used for moisture calculations, do not use any water or other liquids to transfer the silica gel. If a balance is available in the field, follow the procedure for container No. 3 in paragraph (iii) 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 ml by using a graduated cylinder or by weighing it to within ±1.0 g 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 moisture condensed either volumetrically or gravimetrically.

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

(iii) Analysis. Record the data required on a sheet such as the one shown in figure 106. Handle each sample container as follows:

Container Nos. 1, 1A. Analyze and report each filter separately. Transfer the filter and any loose particulate from the sample container to a tared-glass weighing dish. Dry the filter in an oven at 105 degrees Centigrade (220 degrees Fahrenheit) for a minimum of 2 hours, cool for at least 1 hour in a desiccator containing anhydrous calcium sulfate, and weigh and record its weight to the nearest 0.1 mg. During the weighing, the filter shall not be exposed to the laboratory atmosphere for a period 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 shall be consistent before and after the test.

Container No. 2. Note the level of liquid in the container and confirm on the analysis sheet 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 ml or gravimetrically to ±1.0 g. Transfer the contents to a tared 250-ml beaker and evaporate to dryness either at ambient temperature and pressure for acetone or at 95 degrees Centigrade (203 degrees Fahrenheit) in an oven for distilled water. Then subject the sample to 250 degrees Centigrade (482 degrees Fahrenheit) in an oven for 2 to 3 hours. Desiccate for 24 hours and weigh to a constant weight. Report the results to the nearest 0.1 mg.

Container No. 3. Weigh the spent silica gel, or silica gel plus impinger, to the nearest 0.5 g using a balance. This step may be conducted in the field.

"Solvent blank" container. Measure solvent in this container either volumetrically or gravimetrically. Transfer the contents to a tared 250-ml beaker and evaporate to dryness either at ambient temperature and pressure for acetone or at 95 degrees Centigrade (203 degrees Fahrenheit) in an oven for distilled water. Then subject the sample to 250 degrees Centigrade (482 degrees Fahrenheit) in an oven for 2 to 3 hours. Desiccate for 24 hours and weigh to a constant weight. Report the results to the nearest 0.1 mg.

If acetone is used, the contents of container No. 2, as well as the acetone blank container, may be evaporated at temperatures higher than ambient. If evaporation is done at an elevated temperature, the temperature shall be closely supervised, and the contents of the beaker shall be swirled occasionally to maintain an even temperature. Use extreme care, as acetone is highly flammable and has a low flash point.

(e) Calibration. Maintain a laboratory log of all calibrations. Calibrations shall comply with all of the following provisions:

(ii) Pitot tube. The type S pitot tube assembly shall be calibrated according to the procedure outlined in section 4 of method 2.

(iii) Metering system. Before its initial use in the field, the metering system shall be calibrated according to the procedure outlined in APTD-0576. Instead of physically adjusting the dry-gas meter dial readings to correspond to the wet-test meter readings, calibration factors may be used to mathematically correct the gas meter dial readings to the proper values. Before calibrating the metering system, 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 m³/min (0.02 cfm); at the end of the run, take the difference of the measured wet-test meter and dry-gas meter volumes; divide the difference by 10 to get the leak rate. The leak rate shall not exceed 0.00057 m³/min (0.02 cfm).

After each field use, the calibration of the metering system shall be checked by performing 3 calibration runs at a single, intermediate orifice setting, based on the previous field test, with the vacuum set at the maximum value reached during the test series. To adjust the vacuum, insert a valve between the wet-test meter and the inlet of the metering system. Calculate the average value of the calibration factor. If the calibration has changed by more than 5%, 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 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 shall 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 shall be calibrated before its initial use in the field according to the procedures outlined in APTD-0576. 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 section 4.3 of method 2 to calibrate in-stack temperature gauges. Dial thermometers, such as those used for the dry-gas meter and condenser outlet, shall be calibrated against mercury-in-glass thermometers.

(vi) Leak check of metering system shown in figure 103. That portion of the sampling train from the pump to the orifice meter shall be leak checked before initial use and after each shipment. Leakage after the pump will result in less volume being recorded than is actually sampled. The following procedure is suggested (see figure 107): Close the main valve on the meter box. Insert a 1-hole rubber stopper with rubber tubing attached into the orifice exhaust pipe. Disconnect and vent the low side of the orifice manometer. Close off the low side orifice tap. Pressurize the system to 13 to 18 cm (5 to 7 in.) water column by blowing into the rubber tubing. Pinch off the tubing and observe the manometer for 1 minute. A loss of pressure on the manometer indicates a leak in the meter box; leaks, if present, shall be corrected.

(vii) Barometer. Calibrate against a mercury barometer.

(i) Nomenclature:

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

A = Cross-sectional area of stack or flue at the point of sampling, ft.².

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

B_wi = Percent water vapor in gas entering source particulate control device, determined by method 4.

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

C_a = Wash blank residue concentration, mg/g.

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

C_sD = Concentration of particulate matter in stack gas, moisture excluded, pounds per 1,000 pounds of dry stack gas.

C_s50 = Concentration of particulate matter corrected to 50% excess air, pounds per 1,000 pounds of stack gas.

C_s50D = Concentration of particulate matter corrected to 50% excess air, excluding any water addition from a collector, pounds per 1,000 pounds of stack gas.

E = Mass emission rate of particulate, lb/hr.

F₅₀ = Concentration conversion factor to 50% excess air with no moisture alterations in exhaust.

F_50D = Concentration conversion factor to 50% excess air, excluding any moisture added to exhaust gas by pollution collection system.

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

I = Percent of isokinetic sampling.

L_a = Maximum acceptable leakage rate for either a pretest leak check or for a leak check following a component change; equal to 0.00057 m³/min (0.02 cfm) or 4% of the average sampling rate, whichever is less.

L_i = Individual leakage rate observed during the leak check conducted before the "ith" component change (i = 1, 2, 3 . . . . . n), m³/min (cfm).

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

M_d = Molecular weight of dry stack gas, g/g mole (lb/lb-mole), calculated by method 3, equation 3-2, using data from integrated method 3.

m_n = Total amount of particulate matter collected, mg.

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

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

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

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

P_s = Absolute stack gas pressure.

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

R = Ideal gas constant, 0.06236 mm Hg-m³/°K-g-mole (21.85 in. Hg-ft³/°R-lb-mole).

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

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

T_std = Standard absolute temperature, 294.1 °K (530 °R).

V_a

	Peak Heights					Integrated Values
	THC	NMHC	CH4	CO	CO2	THC	NMHC	CH4	CO	CO2	cal#

SAMPLE
BAG

Range

PURGE
BAG

Range

DIGEST
BAG

Range

PART 10. INTERMITTENT TESTING AND SAMPLING