R 336.2011 Reference test method 5B.

Rule 1011. Reference test method 5B, in-stack filtration method, reads as follows: (a) The principle, applicability, and performance test criteria are as follows: (i) Principle. Particulate matter is withdrawn isokinetically from the source and collected on solid filtering media maintained at stack temperature. The particulate matter mass is determined gravimetrically after removal of uncombined water. (ii) Applicability. This method is applicable for the determination of particulate emissions from stationary sources as identified in table 31 of R 336.1331. The method is also applicable when specifically provided for in the department’s rules, orders, a permit to install, or a permit to operate. (iii) Performance test criteria as follows: (A) A performance test must meet the requirements under R 336.2003(2). (B) For sources that are subject to an emission limitation calculated to 50% excess air, the multipoint, integrated sampling procedure of R 336.2004(1)(c) must be used for gas analysis. For all other sources that require a determination of the molecular weight of the exhaust, an optional sampling procedure of R 336.2004(1)(c) may be used. Alternatives or modifications to procedures are subject to the approval of the department. (C) The minimum volume per sample must be 30 cubic feet of dry gas corrected to standard conditions, 68 degrees Fahrenheit and 29.92 inches mercury. Minimum sample time must be 60 minutes, which may be continuous or a combination of shorter sampling periods for sources that operate in a cyclic manner. Smaller sampling times or sample volumes, if necessitated by process variables or other factors, may be approved by the department. (D) For a source whose emission control device alters the moisture content of the exhaust gas, a moisture determination must be performed in a location upstream from the emission control device and in accordance with R 336.2004(1)(d) or an alternative method approved by the department. (b) The following provisions apply to apparatus: (i) Sampling train. A schematic of the sampling train used in this method is shown in figure 102 under R 336.2021. Construction details for many, but not all, of the train components are given in APTD-0581, adopted by reference in R 336.1902. See subdivision (g)(ii) of this rule. For changes from the APTD-0581 document and for allowable modifications to figure 102, the user shall consult with the department. The operating and maintenance procedures for many, but not all, of the sampling train are described in APTD- 0576, adopted by reference in R 336.1902. See subdivision (g)(iii) of this rule. Since correct usage is important in obtaining valid results, all users shall read APTD-0576 and adopt the applicable operating and maintenance procedures outlined in it, unless otherwise specified. The sampling train must consist of the following components: (A) Probe nozzle. Stainless steel 316 or glass with sharp, tapered leading edge. The angle of taper must be less than 30 degrees and the taper must be on the outside to preserve a constant internal diameter. The probe nozzle must be of the button-hook design, unless otherwise specified by the department. If made of stainless steel, the nozzle must be constructed from seamless tubing. Other materials of construction may be used, subject to the approval of the department. A range of nozzle sizes suitable for isokinetic sampling must be available, for example, 0.32 to 1.27 centimeters, 1/8 to 1/2 inch, or larger if higher volume sampling trains are used inside diameter nozzles in increments of 0.16 centimeters, 1/16 inches. Each nozzle must be calibrated according to the procedures outlined in subdivision (e) of this rule. (B) Probe liner. Interior surface may be constructed of stainless steel, no specific grade, glass, Teflon, or other material that maintains proper flow at the stack conditions experienced. (C) Pitot tube. Type S, as described in method 2, or other device approved by the department. The pitot tube must be attached to the probe, as shown in figure 102 under R 336.2021, to allow constant monitoring of the stack gas velocity. The impact, high pressure, opening plane of the pitot tube must be even with or above the nozzle entry plane, see method 2, figure 2-6b, during sampling. The type S pitot tube assembly must have a known coefficient, determined as outlined in method 2. (D) Differential pressure gauge. Two incline manometer or equivalent devices as described in method 2. One manometer must be used for velocity head (p) readings and the other must be used for orifice differential pressure readings. (E) Filter holders. Two separate filter holders in series or 1 filter holder with separate filter supports and seals for 2 filters. One filter holder with 2 filters held in contact with each other is not acceptable. Materials of construction may be stainless steel 316, glass, Teflon, or other material approved by the department. (F) Filter heating system. Auxiliary heating of the filter media is not acceptable. For saturated stack gases, the operator may opt to use filters that do not blind when wet and that do not require heating, see subdivision (c)(i)(A) of this rule. (G) Condenser. The following system must be used to determine the stack gas moisture content: Three impingers connected in series with leak-free ground glass fittings or similar leak-free noncontaminating fittings. All impingers must be of the Greenburg-Smith design and must be modified by replacing the tip with a 1.3 centimeters, 1/2 inch, inside diameter glass tube extending to about 1.3 centimeters, 1/2 inch, from the bottom of the flask. Modifications, such as using flexible connections between the impingers or using materials other than glass, are allowed, subject to the approval of the department. The first impinger must contain a known quantity of water, as described in subdivision (d)(i)(C) of this rule. The second impinger must be empty, and the third must contain a known weight of silica gel or equivalent desiccant. Alternatively, a system that cools the sample gas stream and allows measurement of the water condensed and moisture leaving the condenser, each to within 1 milliliter or 1 gram, may be used, subject to the approval of the department. In any case, the means for measuring the moisture leaving the condenser must be by passing the sample gas stream through a tared silica gel, or equivalent desiccant, trap with exit gases kept below 20 degrees Centigrade, 68 degrees Fahrenheit, and determining the weight gain. If a determination of the particulate matter collected in the impingers is required by the department’s rules, a permit to install, or a permit to operate, then the impinger system described above must be used without modification. Contact the department as to the sample recovery and analysis of the impinger contents. (H) Metering system. Vacuum gauge, leak-free pump, thermometers capable of measuring temperature to within 3 degrees Centigrade, 5.4 degrees Fahrenheit, dry-gas meter capable of measuring volume to within 2%, and related equipment as shown in figure 102 under R 336.2021. Other metering systems capable of maintaining sampling rates within 10% of isokinetic and capable of determining sample volumes to within 2% may be used, subject to the approval of the department. When the metering system is used in conjunction with a pitot tube, the system must enable checks of isokinetic rates. Sampling trains utilizing metering systems designed for higher flow rates than those described in APTD-0581 or APTD-0576, both adopted by reference in R 336.1902, may be used if the specifications of this method are met. (I) Barometer. Mercury, aneroid, or other barometer capable of measuring atmospheric pressure to within 2.5 millimeters mercury, 0.1 inch mercury. In many cases, the barometric reading may be obtained from a nearby national weather service station. In this case, the station value, which is the absolute barometric pressure, must be requested and an adjustment for elevation differences between the weather station and sampling point must be applied at a rate of minus 2.5 millimeters mercury, 0.1 inch mercury, per 30 meters, 100 feet, elevation increase or vice versa for elevation decrease. (J) Gas density determination equipment. Temperature sensor and pressure gauge, as described in method 2, and gas analyzer, if necessary, as described in method 3. The temperature sensor must, preferably, be permanently attached to the pitot tube or sampling probe in a fixed configuration so that the tip of the sensor extends beyond the leading edge of the probe sheath and does not touch any metal. Alternatively, the sensor may be attached just before use in the field. If the temperature sensor is attached in the field, then the sensor must be placed in an interference-free arrangement with respect to the type S pitot tube openings, see method 2, figure 2-6 Velocity Traverse Data. As a second alternative, if a difference of not more than 1% in the average velocity measurement is to be introduced, then the temperature gauge need not be attached to the probe or pitot tube. This alternative is subject to the approval of the department. “Construction Details of Isokinetic Source Sampling Equipment,” APTD-0581, April 1971, PB203-060-LL, and “Maintenance, Calibration, and Operation of Isokinetic Source Sampling Equipment,” APTD-0576, March 1972, PB209-022-LL, are adopted by reference in R 336.1902. (ii) Sample recovery. The following items are required: (A) Probe-liner and probe-nozzle brushes. Nylon bristle brushes with stainless steel wire handles. The probe brush must have extensions, at least as long as the probe, made of stainless steel, nylon, Teflon, or similarly inert material. The brushes must be properly sized and shaped to brush out the probe liner and nozzle. (B) Wash bottles. Two glass wash bottles are recommended. The tester may use polyethylene wash bottles, but the acetone should not be stored in polyethylene bottles for longer than 1 month. (C) Glass sample storage containers. Chemically resistant, borosilicate glass bottles for acetone washes. Screw cap liners must either be rubber-backed Teflon or must be constructed to be leak-free and resistant to chemical attack by acetone. Narrow-mouth glass bottles are less prone to leakage. Alternatively, polyethylene bottles may be used. (D) Filter containers. Glass, polyethylene, or aluminum tube containers, unless otherwise specified by the department. (E) Graduated cylinder or balance. To measure condensed water to within 1 milliliter or 1 gram, graduated cylinders must have subdivisions of not more than 2 milliliters. Most laboratory balances are capable of weighing to the nearest 0.5 gram or less. Any of these balances may be used here and in paragraph (iii)(D) of this subdivision. (F) Plastic storage containers. Airtight containers to store silica gel. (G) Funnel and rubber policeman. To aid in the transfer of silica gel to container, but not necessary if silica gel is weighed in the field. (H) Funnel. Glass or polyethylene, to aid in sample recovery. (iii) Analysis. The following equipment is required for analysis: (A) Glass weighing dishes. (B) Desiccator. (C) Analytical balance. To measure to within 0.1 milligram. (D) Balance. To measure to within 0.5 milligram. (E) Beakers. 250 milliliters. (F) Hygrometer. To measure the relative humidity of the laboratory environment. (G) Temperature gauge. To measure the temperature of the laboratory environment. (c) The following provisions must apply to reagents: (i) Sampling. The reagents used in sampling are as follows: (A) Filters. Two in-stack filters may be any combination of alundum ceramic thimble filters, type RA-98, or glass fiber filters, type A without organic binder. The size of the filters must allow proper sampling rates to maintain iso-kinetics using the nozzle sizes specified in subdivision (b)(i)(A) of this rule. Alternatively, other types of filters may be used, subject to the approval of the department. (B) Silica gel. Indicating type, 6 to 16 mesh. If previously used, dry at 175 degrees Centigrade, 350 degrees Fahrenheit, for 2 hours. New silica gel may be used as received. Alternatively, other types of desiccants that are equivalent or better may be used, subject to the approval of the department. (C) Water. When analysis of the material caught in the impingers is required, distilled water must be used. Run blanks before field use to eliminate a high blank of test samples. (D) Crushed ice. (E) Stopcock grease. Acetone-insoluble, heat-stable silicone grease. This is not necessary if screw-on connectors with Teflon sleeves, or equivalent, are used. Alternatively, other types of stopcock grease may be used, subject to the approval of the department. (ii) Sample recovery. Washing solvent. Either acetone or distilled water may be used for sample recovery. If acetone is used for washing solvent, then reagent grade, less than 0.001% residue, in glass bottles is required. Acetone from metal containers generally has a high residue blank and must not be used. If suppliers transfer acetone to glass bottles from metal containers, then acetone blanks must be run before field use and only acetone with low blank values, less than 0.001%, must be used. In no case must a blank value of more than 0.001% of the weight of acetone used be subtracted from the sample weight. If distilled water is used for washing solvent, use distilled water with less than 0.001% residue. Run blanks before field use to eliminate a high blank on test samples. (iii) Analysis. Two reagents are required for the analysis: (A) Solvent. Same as paragraph (ii) of this subdivision for quantitative transfer. (B) Desiccant. Anhydrous calcium sulfate, indicating type. Alternatively, other types of desiccants may be used, subject to the approval of the department. (d) The following provisions must apply to procedure: (i) Sampling. The complexity of this method is such that, in order to obtain reliable results, testers shall be trained and experienced with the test procedures. Sampling must comply with the following provisions: (A) Pretest preparation provisions are as follows: (I). All the components must be maintained and calibrated according to the applicable procedures described in APTD-0576, adopted by reference in R 336.1902, unless otherwise specified in this rule. (II) Weigh several 200 to 300 gram portions of silica gel in airtight containers to the nearest 0.5 gram. Record the total weight of the silica gel plus container on each container. As an alternative, the silica gel need not be preweighed, but may be weighed directly in its impinger or sampling holder just before train assembly. (III) Check filters visually against light for irregularities, flaws, pinhole leaks, or cracks. Label filters of the proper size on the back side using numbering machine ink. As an alternative, label the shipping containers, as described under subdivision (b)(ii)(D) of this rule, and keep the filters in these containers at all times, except during sampling and weighing. (IV) Dry the filters in an oven at 105 degrees Centigrade, 220 degrees Fahrenheit, for a minimum of 2 hours, cool for at least 1 hour in a desiccator containing anhydrous calcium sulfate, and individually weigh and record each weight to the nearest 0.1 milligram. During the weighing, the filter must not be exposed to the laboratory atmosphere for a period of more than 2 minutes and a relative humidity above 50%. (V) Procedures, other than those specified, that account for relative humidity effects may be used, subject to the approval of the department. (B) Preliminary determinations provisions are as follows: (I) Select the sampling site and the minimum number by the department. (II) Determine the stack pressure, temperature, and the range of velocity heads using method 2. It is recommended that a leak check of the pitot lines, see method 2, be performed. (III) Determine the moisture content using approximation method 4, or its alternatives, for the purpose of making isokinetic sampling rate settings. (IV) Determine the stack gas dry molecular weight, as described in method 2, if integrated method 3 sampling is used for molecular weight determination, the integrated bag sample must be taken simultaneously with, and for the same total length of time as, the particulate sample run. (V) Select a nozzle size based on the range of velocity heads so that it is not necessary to change the nozzle size to maintain isokinetic sampling rates. During the run, do not change the nozzle size. Ensure that the proper differential pressure gauge is chosen for the range of velocity heads encountered, see method 2. (VI) Select a suitable probe liner and probe length so that all traverse points may be sampled. For large stacks, sampling from opposite sides of the stack may reduce the length of probes. (VII) Select a total sampling time greater than or equal to the minimum total sampling time specified in the department’s rules so that the sampling time per point is not less than 5 minutes, unless approved by the department, or some greater time interval as specified by the department, and so that the sample volume taken, corrected to standard conditions, exceeds the required minimum total gas sample volume. The latter is based on an approximate average sampling rate. The number of minutes sampled at each point may be an integer or an integer plus 1/2 minute to avoid timekeeping errors. In some circumstances, such as in batch cycles, it may be necessary to sample for shorter times at the traverse points and to obtain smaller gas sample volumes. In these cases, the department’s approval must first be obtained. (C) Preparation of collection train provisions are as follows: (I) During preparation and assembly of the sampling train, keep all openings where contamination can occur covered until just before assembly or until sampling is about to begin. (II) Place 100 milliliters of water in the first impinger, leave the second impinger empty, and transfer approximately 200 to 300 grams of preweighed silica gel from its container to the third impinger. More silica gel may be used, but care must be taken to ensure that it is not entrained and carried out from the impinger during sampling. Place the container in a clean place for later use in the sample recovery. Alternatively, the weight of the silica gel plus impinger may be determined to the nearest 0.5 gram and recorded. (III) Using tweezers or clean disposable surgical gloves, place a labeled, identified, and weighed filter in each filter holder. Be sure that the filter is properly centered and the gasket properly placed so as to prevent the sample gas stream from circumventing the filter. (IV) Install the selected nozzle using a Viton A 0-ring when stack temperatures are less than 260 degrees Centigrade, 500 degrees Fahrenheit, and a heat-resistant fiberglass, graphite, or other material string gasket when temperatures are higher. See APTD-0576, adopted by reference in R 336.1902, for requirements. Other connecting systems using either 310 stainless steel or Teflon ferrules may be used to form a leak-free direct mechanical connection. (V) Mark the probe with heat-resistant tape or by some other method to denote the proper distance into the stack or duct for each sampling point. (VI) Set up the train as in figure 102 under R 336.2021. (VII) If necessary, use a very light coat of silicone grease on all ground glass joints. Grease only the outer portion, see APTD-0576, to avoid the possibility of contamination by the silicone grease. (VIII) Place crushed ice around the impingers. (D) Leak check procedures: (I) Pretest leak check. A pretest leak check is strongly recommended, but not required, to prevent invalid sampling and wasted time. If the tester opts to conduct the pretest leak check, the following procedure must be used: Perform the leak check on the entire system, including filter housings and nozzle, by plugging the nozzle and pulling a 380 millimeter mercury, 15 inch mercury, vacuum. Alternatively, a lower vacuum may be used if it is not exceeded during the test. Leakage rates in excess of 4% of the average sampling rate or 0.00057 cubic meters per minute, 0.02 cubic feet per minute, whichever is less, are unacceptable. The following leak check instructions for the sampling train described in APTD-0576 and APTD-0581, adopted by reference in R 336.1902, may be helpful. Start the pump with the bypass valve fully open and the coarse adjust valve completely closed. Partially open the coarse adjust valve and slowly close the bypass valve until the desired vacuum is reached. Do not reverse the direction of the bypass valve, as this will cause water to back up into the flexible sample tube and the probe. If the desired vacuum is exceeded, either leak-check at this higher vacuum or end the leak check and start over. When the leak check is completed, first slowly remove the plug from the inlet to the nozzle and immediately turn off the vacuum pump. This prevents the water in the first impinger from being forced backward into the sample tube and prevents silica gel from being entrained backward into the second impinger. (II) Leak checks during sample run. If, during the sampling run, a component, such as a filter assembly or impinger, change becomes necessary, a leak check must be conducted immediately before the change is made. The leak check must be done according to the procedure outlined in paragraph (i)(D)(I) of this subdivision, except that it must be done at a vacuum equal to or greater than the maximum value recorded up to that point in the test. If the leakage rate is not more than 0.00057 cubic meters per minute, 0.02 cubic feet per minute, or 4% of the average sampling rate, whichever is less, then the results are acceptable and no correction need be applied to the total volume of dry gas metered. If a higher leakage rate is obtained, then the tester shall either record the leakage rate and plan to correct the sample volume, as shown in subdivision (f)(iii) of this rule, or void the sampling run. Immediately after component changes, leak checks may be performed. If leak checks are done, then the procedure outlined in paragraph (i)(D)(I) of this subdivision must be used. (III) Post-test leak check. A leak check is required at the conclusion of each sampling run. The leak check must be performed in accordance with the procedures in paragraph (i)(D)(I) of this subdivision, except that it must be conducted at a vacuum equal to or greater than the maximum value reached during the sampling run. If the leakage rate is not more than 0.00057 cubic meters per minute, 0.02 cubic feet per minute, or 4% of the average sampling rate, whichever is less, then the results are acceptable and no correction need be applied to the total volume of dry gas metered. If a higher leakage rate is obtained, then the tester shall either record the leakage rate and correct the sample volume, as shown in subdivision (f)(iii) of this rule, or void the sampling run. (E) Particulate train operation. During the sampling run, maintain an isokinetic sampling rate that is within 10% of true isokinetic, unless otherwise specified by the department. For each run, record the data required on a data sheet such as the data sheet in figure 104 under R 336.2021. Record the initial dry-gas meter reading. Record the dry-gas meter readings at the beginning and end of each sampling time increment, when changes in flow rates are made, before and after each leak check, and when sampling is halted. Take other readings required by figure 104 under R 336.2021 at least once at each sample point during each time increment, and take additional readings when significant changes, 20% variation in velocity head readings, necessitate additional adjustments in flow rate. Level and zero the manometer. Because the manometer level and zero may drift due to vibrations and temperature changes, make periodic checks during the traverse. Clean the portholes before the test run to minimize the chance of sampling deposited material. To begin sampling, remove the nozzle cap and verify that the pitot tube and probe are properly positioned. Position the nozzle at the first traverse point with the tip pointing directly into the gas stream. Immediately start the pump and adjust the flow to isokinetic conditions. Nomographs that aid in the rapid adjustment of the isokinetic sampling rate without excessive computations are available. These nomographs are designed for use when the type S pitot tube coefficient is 0.85 ±0.02 and the stack gas equivalent density, dry molecular weight, is equal to 29 ±4. APTD-0576, adopted by reference in R 336.1902, details the procedure for using the nomographs. If Cp and Md are outside the above stated ranges, do not use the nomographs unless appropriate steps, see subdivision (g)(iv) of this rule, are taken to compensate for the deviations. When the stack is under significant negative pressure, height of impinger stem, take care to pull low-flow when inserting the probe into the stack to prevent water from backing into the sample tubing and to avoid pulsation through the filter and possible loss of materials. When the probe is in position, block off the openings around the probe and porthole to prevent unrepresentative dilution of the gas stream. Traverse the stack cross section, as required by method 1 or as specified by the department, being careful not to bump the probe nozzle into the stack walls when sampling near the walls or when removing or inserting the probe through the portholes; this minimizes the chance of extracting deposited material. During the test run, add more ice and, if necessary, salt to maintain a temperature of less than 20 degrees Centigrade, 68 degrees Fahrenheit, at the condenser/silica gel outlet. Also, periodically check the level and zero of the manometer. If the pressure drop across the filter becomes too high and makes isokinetic sampling difficult to maintain, the filter may be replaced in the midst of a sample run. It is recommended that another complete filter assembly be used rather than attempting to change the filter itself. Before a new filter assembly is installed, conduct a leak check, as described under paragraph (i)(D)(II) of this subdivision. The total particulate weight must include the summation of all filter assembly catches. A single train must be used for the entire sample run, except in cases where simultaneous sampling is required in 2 or more separate ducts, at 2 or more different locations within the same duct, or where equipment failure necessitates a change of trains. In all other situations, the use of 2 or more trains must be subject to the approval of the department. When 2 or more trains are used, separate analyses of the front-half and, if applicable, impinger catches from each train must be performed, unless identical nozzle sizes were used on all trains. If identical nozzle sizes were used, the front-half catches from the individual trains may be combined, as may the impinger catches, and 1 analysis of front-half catch and 1 analysis of impinger catch may be performed. Consult with the department for details concerning the calculation of results when 2 or more trains are used. At the end of the sample run, turn off the coarse adjust valve, remove the probe and nozzle from the stack, turn off the pump, record the final dry- gas meter reading, and conduct a post-test leak check, as outlined in paragraph (i)(D)(III) of this subdivision. Leak-check the pitot lines as described in method 2. The lines must pass this leak check to validate the velocity head data. (F) Calculation of percent isokinetic. Calculate percent isokinetic, see subdivision (f) of this rule, to determine if the run was valid or if another test run should be made. If there was difficulty in maintaining isokinetic rates due to source conditions, consult with the department for possible variance on the isokinetic rates. (ii) Sample recovery. Proper cleanup procedure begins as soon as the probe is removed from the stack at the end of the sampling period. Allow the probe to cool. When the probe can be safely handled, wipe off all external particulate matter near the tip of the probe nozzle and place a cap over it to prevent losing or gaining particulate matter. Do not cap off the probe tip tightly while the sampling train is cooling down as this creates a vacuum in the filter holder and draws water from the impingers into the sample tube. Before moving the sampling train to the cleanup site, make sure all condensed water in the probe and flexible sample lines are drained into the first impinger. Disconnect all sample lines and remove the nozzle-filter set assembly from the probe. Cap all openings to prevent contamination or accidental loss of sample. Remove all excess particulate from the exterior of the nozzle-filter assembly to prevent contamination during disassembly. Transfer the nozzle-filter set assembly and impinger set to the cleanup area. The cleanup area must be clean and protected from the wind so that the chances of contaminating or losing the sample are minimized. Save a portion of the solvent used for cleanup as a blank. Take 200 milliliters of this solvent directly from the wash bottle being used and place it in a glass sample container labeled "solvent blank". Inspect the train before and during disassembly and note any abnormal conditions. Treat the samples in the following manner: Container numbers. 1, 1A. Carefully remove the filters from the filter holders and place each filter in its identified container. Use a pair of tweezers or clean disposable surgical gloves, or both, to handle the filters. Carefully transfer to the container any particulate matter or filter fibers, or both, that adhere to the filter holder gasket by using a dry nylon bristle brush or sharp- edged blade, or both. Seal the containers. Container number 2. Taking care to see that particulate on the outside of the nozzle and filter holders does not get into the sample, the tester shall carefully remove the nozzle and clean the inside surface by rinsing with solvent from a wash bottle and brushing with a nylon bristle brush. Brush until the solvent rinse shows no visible particles and then make a final rinse of the inside surface with solvent. After ensuring that all joints have been cleaned of all extraneous material, the tester shall quantitatively remove particulate from the filter holders by rubbing the surfaces with a nylon bristle brush and rinsing with solvent. Rinse each surface 3 times, or more if needed, to remove visible particulate. Make a final rinse of the brush and filter holder set. After all solvent washings and particulate matter have been collected in the sample container, tighten the lid on the sample container so that solvent will not leak out when it is shipped to the laboratory. Mark the height of the fluid level to determine if leakage occurred during transport. Label the container to clearly identify its contents. Container number 3. Note the color of the indicating silica gel to determine if it has been completely spent and make a notation of its condition. Transfer the silica gel from the third impinger to its original container and seal. A funnel may make it easier to pour the silica gel without spilling it. A rubber policeman may be used as an aid in removing the silica gel from the impinger. It is not necessary to remove the small amount of dust particles that adhere to the impinger wall and are difficult to remove. Since the gain in weight will be used for moisture calculations, do not use any water or other liquids to transfer the silica gel. If a balance is available in the field, follow the procedure for container number 3 in paragraph (iii) of this subdivision. Impinger water. Treat the impingers in the following manner: Make a notation of any color or film in the liquid catch. Measure the liquid that is in the first 2 impingers to within ±1 milliliter by using a graduated cylinder or by weighing it to within ±1.0 gram by using a balance if one is available. Record the volume or weight of liquid present. This information is required to calculate the moisture content of the effluent gas. Discard the liquid after measuring and recording the volume or weight, unless analysis of the impinger catch is required, see subdivision (b)(i)(G) of this rule. If a different type of condenser is used, measure the amount of moisture condensed either volumetrically or gravimetrically. If possible, containers must be shipped in a manner that keeps them upright at all times. (iii) Analysis. Record the data required on a sheet such as the sheet in figure 106 under R 336.2021. Handle each sample container in the following manner: Container numbers 1, 1A. Analyze and report each filter separately. Transfer the filter and any loose particulate from the sample container to a tared-glass weighing dish. Dry the filter in an oven at 105 degrees Centigrade, 220 degrees Fahrenheit, for a minimum of 2 hours, cool for at least 1 hour in a desiccator containing anhydrous calcium sulfate, and weigh and record its weight to the nearest 0.1 milligram. During the weighing the filter must not be exposed to the laboratory atmosphere for a period greater than 2 minutes or a relative humidity above 50%. Procedures, other than those specified, that account for relative humidity effects may be used, subject to the approval of the department. The method used for drying and weighing of filters must be consistent before and after the test. Container number 2. Note the level of liquid in the container and confirm on the analysis sheet if leakage occurred during transport. If a noticeable amount of leakage has occurred, then either void the sample or use methods, subject to the approval of the department, to correct the final results. Measure the liquid in this container either volumetrically to ±1 milliliter or gravimetrically to ±1.0 gram. Transfer the contents to a tared 250-milliliter beaker and evaporate to dryness either at ambient temperature and pressure for acetone or at 95 degrees Centigrade, 203 degrees Fahrenheit, in an oven for distilled water. Then subject the sample to 250 degrees Centigrade, 482 degrees Fahrenheit, in an oven for 2 to 3 hours. Desiccate 24 hours and weigh to a constant weight. Report the results to the nearest 0.1 milligram. Container number 3. Weigh the spent silica gel, or silica gel plus impinger, to the nearest 0.5 gram using a balance. This step may be conducted in the field. "Solvent blank" container. Measure solvent in this container either volumetrically or gravimetrically. Transfer the contents to a tared 250-milliliters beaker and evaporate to dryness either at ambient temperature and pressure for acetone or at 95 degrees Centigrade, 203 degrees Fahrenheit, in an oven for distilled water. Then subject the sample to 250 degrees Centigrade, 482 degrees Fahrenheit, in an oven for 2 to 3 hours. Desiccate for 24 hours and weigh to a constant weight. Report the results to the nearest 0.1 milligram. If acetone is used, the contents of Container number 2, as well as the acetone blank container, may be evaporated at temperatures higher than ambient. If evaporation is done at an elevated temperature, then the temperature must be closely supervised, and the contents of the beaker must be swirled occasionally to maintain an even temperature. Use extreme care, as acetone is highly flammable and has a low flash point. (e) Calibration. Maintain a laboratory log of all calibrations. Calibrations must comply with the following provisions: (i) Probe nozzle. A probe nozzle must be calibrated before its initial use in the field. Using a micrometer, measure the inside diameter of the nozzle to the nearest 0.025 millimeter, 0.001 inch. Make 3 separate measurements using different diameters each time and obtain the average of the measurements. The difference between the high and low numbers must not exceed 0.1 millimeter, 0.004 inch. When nozzles become nicked, dented, or corroded, the nozzles must be reshaped, sharpened, and recalibrated before use. Each nozzle must be permanently and uniquely identified. (ii) Pitot tube. The type S pitot tube assembly must be calibrated according to the procedures in method 2. (iii) Metering system. Before its initial use in the field, the metering system must be calibrated according to the procedure in APTD-0576, adopted by reference in R 336.1902. Instead of physically adjusting the dry-gas meter dial readings to correspond to the wet- test meter readings, calibration factors may be used to mathematically correct the gas meter dial readings to the proper values. Before calibrating the metering system, a leak check may be conducted. For metering systems having diaphragm or rotary pumps, the normal leak check procedure will not detect leakages within the pump. For these cases, the following leak check procedure may be used: Make a 10-minute calibration run at 0.00057 cubic meters per minute, 0.02 cubic feet per minute. At the end of the run, take the difference of the measured wet-test meter and dry-gas meter volumes and divide the difference by 10 to get the leak rate. The leak rate must not exceed 0.00057 cubic meters per minute (0.02 cubic feet per minute). After each field use, the calibration of the metering system must be checked by performing 3 calibration runs at a single, intermediate orifice setting, based on the previous field test, with the vacuum set at the maximum value reached during the test series. To adjust the vacuum, insert a valve between the wet-test meter and the inlet of the metering system. Calculate the average value of the calibration factor. If the calibration has changed by more than 5%, then recalibrate the meter over the full range of orifice settings, as outlined in APTD-0576. Alternatively, a spirometer may be substituted for a wet-test meter in the above calibration procedures. Alternative procedures, such as using the orifice meter coefficients, may be used, subject to the approval of the department. If the dry-gas meter coefficient values obtained before and after a test series differ by more than 5%, then the test series must be performed using whichever meter coefficient value, before or after, gives the lower value of total sample volume. (iv) Temperature gauges. Use the procedure in method 2 to calibrate in-stack temperature gauges. Dial thermometers, such as those used for the dry-gas meter and condenser outlet, must be calibrated against mercury-in-glass thermometers or other thermometers that are calibrated using a National Institute of Standards and Technology calibrated reference thermometer. (v) Leak check of metering system shown in figure 102 under R 336.2021. That portion of the sampling train from the pump to the orifice meter must be leak-checked before initial use and after each shipment. Leakage after the pump will result in less volume being recorded than is actually sampled. The following procedure is suggested, also see figure 107 under R 336.2021: Close the main valve on the meter box. Insert a 1-hole rubber stopper with rubber tubing attached into the orifice exhaust pipe. Disconnect and vent the low side of the orifice manometer. Close off the low side orifice tap. Pressurize the system to 13 to 18 centimeters, 5 to 7 inches, water column by blowing into the rubber tubing. Pinch off the tubing and observe the manometer for 1 minute. A loss of pressure on the manometer indicates a leak in the meter box. Leaks, if present, must be corrected. (vi) Barometer. Calibrate against a mercury barometer. (f) Calculations. When carrying out calculations, retain at least 1 extra decimal figure beyond that of the acquired data. Round off figures after the final calculation. Other forms of the equations may be used if the other forms of the equations give equivalent results. The following provisions apply to calculations: (i) Nomenclature: An = Cross-sectional area of nozzle, meters² or the equivalent feet². A = Cross-sectional area of stack or flue at the point of sampling, feet². B ws = Water vapor in the gas stream, proportion by volume, expressed as a fraction. B wi = Percent water vapor in gas entering source particulate control device determined by method 4. B wo = Percent water vapor in gas exiting source particulate control device. Ca = Wash blank residue concentration, milligrams per gram. Cs = Concentration of particulate matter in stack gas, pounds per 1,000 pounds of actual stack gas. C sD = Concentration of particulate matter in stack gas, moisture excluded, pounds per 1000 pounds of dry stack gas. 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, pounds/hour. 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. L a = Maximum acceptable leakage rate for either a pretest leak check or for a leak check following a component change; equal to 0.00057 meters³/minute (0.02 cubic feet per minute) or 4% of the average sampling rate, whichever is less. Li = Individual leakage rate observed during the leak check conducted before the "ith" component change (i = 1, 2, 3 . . . . n), meters³/minute (cubic feet per minute). Lp = Leakage rate observed during the post-test leak check, meters³/minute (cubic feet per minute). Md = Molecular weight of dry stack gas, gram/gram mole (pound/pound-mole), calculated by method 3, equation 3-1, using data from integrated method 3. mn = Total amount of particulate matter collected, milligram. Mw = Molecular weight of water, 18.0 gram/gram-mole (18.0 pound/pound-mole). ma = Mass of residue of solvent after evaporation, milligram. mg = Total weight of gas samples through nozzle, pound. P bar = Barometric pressure at the sampling site, millimeter mercury (inches mercury). Ps = Absolute stack gas pressure. Pstd = Standard absolute pressure, 760 millimeters mercury (29.92 inches mercury). R = Ideal gas constant, 0.06236 millimeters of mercury-cubic meters per kelvin-gram- mole, (21.85 inches of mercury-cubic feet per Rankine-pound-mole). T m = Absolute average dry-gas meter temperature, see figure 104 under R 336.2021, °Kelvin, (°Rankine). Ts = Absolute average stack gas temperature, see figure 104 under R 336.2021, °Kelvin, (°Rankine). Tstd = Standard absolute temperature, 294.I°Kelvin, (530°Rankine). V a = Volume of solvent blank, milliliters. V aw = Volume of solvent used in wash, milliliters. V lc = Total volume of liquid collected in impingers and silica gel (see figure 106 under R 336.2021), milliliters. Vm = Volume of gas sample as measured by the dry-gas meter, deci-centimeter, (deci- cubic-foot). V m(std) = Volume of gas sample measured by the dry-gas meter, corrected to standard conditions, deci-standard cubic meter, (deci-standard cubic foot). V w(std) = Volume of water vapor in the gas sample, corrected to standard conditions, standard cubic meter, (standard cubic foot). V s = Stack gas velocity, calculated by method 2, using data obtained from method 5, meters/second (feet/second). Wa = Weight of residue in solvent wash, milligram. Y = Dry-gas meter calibration factor. ΔH = Average pressure differential across the orifice meter (see figure 104 under R 336.2021), millimeter water (inches water). %02 = Percent oxygen in stack gas by volume (dry basis). %N2 = Percent nitrogen in stack gas by volume (dry basis). p a = Density of solvent, milligrams/milliliter. p s(std) = Density of all sampled gas at standard conditions, pounds/feet.³ pw = Density of water, 0.9982 grams/milliliter (0.002201 pounds/milliliter). θ = Total sample time, minute. θ1 = Sample time, interval, from the beginning of a run until the first component change, minute. θi = Sampling time interval, between 2 successive component changes, beginning with the interval between the first and second changes, minute. θp = Sampling time interval, from the final (nth) component change until the end of the sampling run, minute. 13.6 = Specific gravity of mercury. 60 = Seconds/minute. 100 = Conversion to percent. 386.9 = Cubic feet per pound-mole of ideal gas at standard conditions. 453.6 = Conversion of pounds to grams. 3600 = Conversion of hours to seconds. 1000 = Conversion of 1000 pound units to pound units. (ii) Average the dry-gas meter temperature and average the orifice pressure drop. See data sheet, figure 104 under R 336.2021. (iii) Dry gas volume. Correct the sample volume measured by the dry-gas meter to standard conditions, 21.11 degrees Centigrade, 760 millimeters mercury or 68 degrees Fahrenheit, 29.92 inches mercury, by using equation 5-1. Equation 5-1: m(std) m std bar m std 1 m bar m V = V Y T ( P + H / 13.6) T P = K V Y ( P + H / 13.6) T   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 La, equation 5-1 must be modified as follows: (A) Case I. No component changes made during sampling run. In this case, replace Vm in equation 5-1 with the following expression:  ) L - (L - V a p m (B) Case II. One or more component changes made during the sampling run. In this case, replace V m in equation 5-1 by the following expression: p i n i    ) L - L ( ) L - (L ) L - (L - V a p a i a 1 m 2 1 − − = and substitute only for those leakage rates (Li or Lp) that exceed La. (iv) Volume of water vapor. Equation 5-2 w(std) 1c w w std std 2 1c V = V ( p / M ) (R T / P ) = K V Where: K2 = 0.001338 m³/ml for metric units. = 0.04733 ft.3/ml for English units. (v) Moisture content. Equation 5-3 ws w(std) m(std) w(std) B = V / (V + v ) In saturated or water droplet-laden gas streams, 2 calculations of the moisture content of the stack gas must be made: 1 from the impinger analysis, equation 5-3, and a second from the assumption of saturated conditions. The lower of the 2 values of Bws must be considered correct. The procedure for determining the moisture content based on the assumption of saturated conditions as described in 40 CFR part 60 appendix A method 4. For the purpose of this method, the average stack gas temperature from figure 104 under R 336.2021 may be used to make the determination, if the accuracy of the in-stack temperature sensor is ±1 degree Centigrade, 2 degrees Fahrenheit. (vi) Solvent blank concentration. Equation 5-4 a a a a C = m / (V P ) (vii) Solvent wash blank. Equation 5-5 a a aw a W = C V P (viii) Total particulate weight. Determine the total particulate catch from the sum of the weights obtained from containers 1, 1A, and 2 less the wash solvent blank, see figure 106 under R 336.2021. Refer to subdivision (d)(i)(E) of this rule to assist in the calculation of results involving 2 or more pairs of filters or 2 or more sampling trains. (ix) Sampled gas density. Determine the density of the gas sampled from the stack, at standard conditions in pounds per cubic foot, lb/ft.³. Equation 5-6 s(std) d ws w ws P = ( M (1- B ) + M B ) / 386.9 (x) Total weight of gas sampled, lbs. Equation 5-7 g m(std) w(std) s(std) m = (V + V ) p (xi) Particulate concentration, lbs/1000 lbs. Equation 5-8 s n g C = m / (453.6 m ) (xii) Excess air and moisture correction factors: (A) Correction factor to 50% excess air for those sources with or without a particulate collector where no increase in moisture content of the exhaust gas occurs after the process and before the point of sampling. Equation 5-9 50 d wo wo 2 2 d wo wo F = M + 18 B / (100 - B ) 0.1826 % N - 2.0592 %0 + M + 18 B / (100 - B ) (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 50D d wo wo 2 2 d wi wi F = M + 18 B / (100 - B ) 0.1826 % N - 2.0592 %0 + M + 18 B / (100 - B ) (C) Correction factor to convert the actual concentration, Cs, to dry conditions. Equation 5-11 D d wo wo d F = M + 18 B / (100 - B ) M (xiii) Converted particulate concentrations, where applicable under the department’s rules or permit. Equation 5-12 s50 s 50 C = C F Equation 5-13 s50D s 50D C = C F Equation 5-14 sD s D C = C F (xiv) Mass emission rate in pounds per hour, lb/hr. Equation 5-15 E = 3600 A V C P T P 1000 T P = K A V C P P / T s s s std s(std) s std 3 s s s s(std) s Where: K3 = 63.77 for English units. (xv) Isokinetic variation using 1 of the following methods: (A) Calculation from raw data. Equation 5-16 I = 100 T ( K V + (V / T )( P + H / 13.6)) 60 V P A s 4 lc m m bar s s n   Where: K4 = 0.003458 mm Hg - m³ml - °K for metric units. = 0.002672 in. Hg - ft.³/ml - °R for English units. (B) Calculation from intermediate values. Equation 5-17 I = T V P 100 T V A P 60(1- B ) = K T V P V A (1- B ) s m(std) std std s n s ws 5 s m(std) s s n ws   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.