Section 336.2011. Reference test method 5B.

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 Particulate matter is withdrawn isokinetically from the source and collected on solid filtering media maintained  at  stack temperature.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.

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

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

(E)    Beakers. 250 ml.

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

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

(c)      The following provisions shall apply to reagents:

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

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

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

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

(D)    Crushed ice.

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

(ii)       Sample recovery. Washing solvent. Either acetone or distilled water may be used for sample recovery. If acetone is used for washing  solvent, then reagent grade, less than 0.001% residue, in glass bottles is required. Acetone from metal containers generally has a high residue blank and shall not be used. If suppliers transfer acetone to glass bottles from metal containers, then acetone blanks shall be run before field use and only acetone with low blank values (less than 0.001%) shall be used. In no case shall a blank value of more than 0.001% of the weight of acetone used be subtracted from the sample weight.  If distilled water is used for washing solvent, use  distilled  water   with

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 Cp and Md are outside the above stated ranges, do not use the nomographs  unless  appropriate   steps (subdivision (g)(iv) of this rule) are taken to compensate for the deviations. When the stack is under significant negative

pressure (height of impinger stem), take care to pull lowflow when inserting the probe into the stack to prevent water from backing into the sample tubing and to avoid pulsation through the filter and possible loss of materials. When the probe is in position, block off the openings around the probe and porthole to   prevent  unrepresentative dilution of the gas stream. Traverse the stack cross section, as required by method 1 or as specified by the department, being careful not to bump the probe nozzle into the stack walls when sampling near the walls or when removing or inserting the probe through the portholes; this minimizes the chance of  extracting   deposited material. During the test run, add more ice and, if necessary, salt to maintain a temperature of less than 20 degrees Centigrade (68 degrees Fahrenheit) at the condenser/silica gel outlet. Also, periodically check the level and zero of the manometer. If the pressure drop across the filter becomes too high and  makes isokinetic sampling difficult to maintain, the filter may be replaced in the midst of a sample run. It is recommended that another complete  filter assembly be used rather than attempting to change the filter itself. Before a new filter assembly is installed, conduct a leak check (paragraph (i)(D)(2) of this subdivision). The total particulate weight shall include the summation of all filter assembly catches. A single train shall be used for the entire sample run, except in cases where simultaneous sampling is required in 2 or more separate ducts, at 2 or more different locations within the same duct, or where equipment failure necessitates a change of trains. In all other situations, the use of 2  or more trains shall be subject to the approval of the department. When 2 or more trains are used, separate analyses of the front-half and, if applicable, impinger catches from each train shall be performed, unless identical nozzle sizes were used on all trains. If identical nozzle sizes were used, the front-half catches from the individual trains may be combined, as may the impinger catches, and 1 analysis of front-half catch and 1 analysis of impinger catch may be performed. Consult with the department for details concerning the calculation of results when 2 or more trains are used. At the end of the sample run, turn off the coarse adjust valve, remove the probe and nozzle from the stack, turn off the pump, record the final dry-gas meter reading, and conduct a post-test leak check, as outlined in paragraph (i)(D)(3) of this subdivision. Leak-check the pitot lines as described in method 2, section 3.1; the lines shall pass this leak check to validate the velocity head data.

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

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

(ii)       Sample recovery. Proper cleanup procedure begins as soon as the probe is removed from the stack at the end of the sampling period. Allow the probe to cool. When the probe can be safely handled, wipe off all  external  particulate matter near the tip of the probe nozzle and place a cap over it to prevent losing or gaining particulate matter. Do not cap off the probe tip tightly while the sampling train is cooling down as this creates a vacuum in the filter holder and draws water from the impingers into the sample tube. Before moving the sampling train to the cleanup site, make sure all condensed water in the probe and flexible sample lines are drained into the first impinger. Disconnect all sample lines and remove the nozzle-filter set assembly from the probe. Cap all openings  to  prevent  contamination  or accidental loss of sample. Remove all excess particulate from  the  exterior of the nozzle-filter assembly to prevent

contamination during disassembly. Transfer the nozzle-filter set assembly and impinger set to  the   cleanup area.  The cleanup area shall be clean and protected from the  wind so that the chances of contaminating or losing the sample are minimized.  Save a portion of the solvent used for cleanup as a blank. Take 200 ml of this solvent directly from the wash bottle being used and place it in a glass sample container labeled "solvent blank". Inspect the train before and during disassembly and note any abnormal conditions. Treat the samples in the following manner: Container Nos. 1, 1A. Carefully remove the filters from the filter holders and place in their identified containers. Use a pair of tweezers or clean disposable surgical gloves, or both, to  handle  the  filters. Carefully transfer to the container any particulate matter or filter fibers, or both, that adhere to the filter holder gasket by using a dry nylon bristle brush or sharp-edged blade, or both. Seal the containers. Container No. 2. Taking care to see that particulate on the outside of the nozzle and filter holders does not get into the sample, the testor shall carefully remove the nozzle and clean the  inside  surface  by  rinsing  with solvent from a wash bottle and brushing with a nylon bristle brush. Brush until the solvent rinse shows no visible particles and then make a final rinse of the inside surface with solvent. After ensuring that all  joints   have  been  cleaned   of  all  extraneous material, the testor shall quantitatively remove particulate from the filter holders by rubbing the surfaces with a nylon bristle brush and rinsing with solvent. Rinse each surface 3 times, or more if needed, to remove visible particulate. Make a final rinse of the brush and filter holder set. After all solvent washings and particulate matter have been collected in the sample container, tighten the lid on the sample container so that solvent will not leak out when it is shipped to the laboratory.   Mark the height of the  fluid level to determine if leakage occurred during transport. Label the container to clearly identify its contents. Container No. 3. Note the color of the indicating silica gel to determine if it has been completely spent and make a notation of its condition. Transfer the silica gel from the third impinger to its original container and seal. A funnel may make it easier to pour the silica gel without spilling it.  A rubber policeman may be used as an aid in removing the silica gel from the impinger. It is not necessary to remove  the  small  amount  of dust particles that adhere to the impinger wall and are difficult to remove. Since the gain in weight will be used for moisture calculations, do not use any water or other liquids to transfer the silica gel. If a balance is available in the field, follow the procedure for container No. 3 in paragraph (iii) of this subdivision. Impinger water. Treat the impingers in the  following  manner:  Make  a notation of any color or film in the liquid catch. Measure the liquid that is in the first 2 impingers to within ±1 ml by using a graduated cylinder or by weighing it to within ±1.0 g by using a balance  if   one is available. Record the volume or weight of liquid present. This information is required to calculate the moisture content of the effluent gas. Discard the liquid after measuring and recording the volume or weight, unless analysis of the impinger catch is required (subdivision (b)(i)(G) of this rule). If a different type of condenser is used, measure the amount of moisture condensed either volumetrically or gravimetrically. If possible, containers shall be shipped in a manner that keeps them upright at all times.

(iii)       Analysis. Record the data required on a sheet such as the sheet in figure 106. Handle each sample container in the following manner: Container Nos. 1, 1A. Analyze and report each filter separately. Transfer the filter and any loose particulate from the sample  container  to   a tared-glass weighing dish.    Dry  the  filter  in  an   oven  at  105

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.

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, mg/g.

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, 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.

gas.

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

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.

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.

P bar = 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).

T m = 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). V a  = Volume of solvent blank, ml.

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

ml.

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

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

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

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

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

Wa  = Weight of residue in solvent wash, mg. Y = Dry-gas meter calibration factor.

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

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

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

p a   = Density of solvent, mg/ml.

p s(std)  = Density of all sampled gas at standard conditions, lb/ft.³ pw  = Density of water, 0.9982 g/ml (0.002201 lb/ml).

θ  = Total sample time, min.

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

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

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

13.6 = Specific gravity of mercury.

60 = Sec/min.

100 = Conversion to percent.

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

453.6 = Conversion of pounds to grams. 3600 = Conversion of hours to sec.

1000 = Conversion of 1000 lb units to lb units.

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

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

V m(std)    =

V m   Y T std   ( Pbar    + DH / 13.6)

=  K1

V m  Y

equation 5-1

( Pbar    + DH / 13.6)

Where:

Tm    Pstd                                                                                                                   Tm

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 shall be modified in the following manner:

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

Vm - (Lp - La)q

(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:

n

Vm - (L1 - La)q 1 - å

i =2

(Li  - La)qi  - (Lp  - La)qp

and  substitute only for those leakage rates (Li or Lp) that exceed La.

(iv)      Volume of water vapor.

equation 5-2

Where:

V w(std)

=   V 1c

( pw / Mw ) (R Tstd  / Pstd ) =  K2

V 1c

K2 = 0.001338 m³/ml for metric units.

(v)      Moisture content.

equation 5-3

Bws

=   V w(std) / (V  m(std)

+   vw(std) )

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 Bws 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.

Ca

(vii)    Solvent wash blank.

=   ma / (V  a

Pa )

equation 5-4

equation 5-5

Wa    =  Ca

V aw    Pa

(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).

Ps(std)

= ( Md

(1 - Bws  ) +  Mw

Bws  ) / 386.9

equation 5-6

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

equation 5-7

mg    =  (V  m(std)

+  V w(std) )  ps(std)

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

equation 5-8

Cs    =   mn / (453.6 mg )

(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.

F 50    =

equation 5-9

                           M d    + 18 Bwo / (100 - Bwo  )                           

0.1826 % N 2

- 2.0592 % 02

+  Md

+ 18 Bwo / (100 - Bwo  )

(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.

F 50D    =

equation 5-10

                           M d    + 18 Bwo / (100 - Bwo )                          

0.1826 % N 2

- 2.0592 % 02

+  Md

+ 18 Bwi / (100 - Bwi )

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

FD    =

  M d    + 18 Bwo  / (100 - Bwo  ) Md

equation 5-11

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

Cs50

Cs50D

CsD

=   Cs

=   Cs

=   Cs

F 50

F 50D

FD

equation 5-12

equation 5-13

equation 5-14

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

3600 A V    C    P    T      P

equation 5-15

E =                                      s           s           s          std            s(std)

=  K3  A V s   Cs    Ps    Ps(std) / Ts

Where:

1000 Ts

Pstd

K3           = 63.77 for English units.

(xv)       Isokinetic variation:

(A)    Calculation from raw data.

I =  100 T s   ( K 4   V lc   + (V  m / T m )( Pbar    + DH / 13.6))

equation 5-16

Where:

60  q V s    Ps    An

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.

5

 

equation 5-17

I =           Ts

V m(std)

Pstd

100

=  K              T s   V m(std)                  

T std

V s  q An

Ps  60(1 - Bws  )

Ps   V s

An  q (1 - Bws  )

Where:

K5 = 4.307 for metric units.

= 0.09409 for English units.

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

If the results are low in comparison to the standard and I is beyond the acceptable range, or if I is less than 90%, then the department may opt to accept the results. Otherwise, reject the results and repeat the test.

(g)      Bibliography:

(i)     Federal Register, Volume 42, No. 160, Part 160, Chapter 1,  Title  40, Appendix A, Method 5, August 18, 1977.

(ii)      Martin, Robert M. Construction Details of Isokinetic Source Sampling Equipment. Environmental Protection Agency. Research Triangle Park, N.C.APTD- 0581. April, 1971.

(iii)    Rom, Jerome J. Maintenance, Calibration, and Operation of Isokinetic Source Sampling  Equipment.   Environmental   Protection  Agency.     Research Triangle Park,

N.C. APTD-0576.  March, 1972.

(iv)      Shigehara, R. T. "Adjustments in the EPA Nomograph for Different Pitot Tube Coefficients and Dry Molecular Weights." Stack Sampling News, 2:4 -  11. October, 1974.

(v)      Guidelines for Source Testing of Particulate. Michigan Department of Natural Resources, Air Quality Division. June 1, 1977.

History: 1985 AACS; 1992 AACS; 2002 AACS; 2005 AACS.