1, except that. unless particulate

emissions are to be determined, the filter need not be desiccated or weighed. First. rinse all sampling train glassware with hot tap water and then wash in hot soapy water. Next, rinse glassware three times with tap water. followed by three additional rinses with water. Then soak all glassware in a 10 percent (V/V) nitric acid solution for a minimum of 4 hours, rinse three times with water, rinse a final time with acetone, and allow to air dry. Cover all glassware openings where contamination can occur until the sampling train is assembled for sampling. 5.1.2 Preliminary Determinations. Same as Method 5. Section 4.1.2. 5.1.3 Preparation of Sampling Train. 5.1.3.1 Set up the sampling train as shown in Figure 29-1. Follow the same general procedures given in Method 5, Section 4.1.3, except place 100 ml of the HNO₃/H₂ O₂ solution (Section 4.3.1. of this method) in each of the second and third impingers as shown in Figure 29-1. Placee 100 ml of the acidic KMnO4 absorbing solution (Section 4.3.2 of this method) in each of the fifth and sixth impingers as shown in Figure 29-1. and transfer approximately 200 to 300 g of pre-weighed silica gel from its container to the last impinger. Alternatively. the silica gel may be weighed directly in the Impinger just prior to final train assembly. 5.1.3.2 Based on the specific source sampling conditions, the use of an empty first impinger can be eliminated if the moisture to be collected in the Impingers will be less than approximately 100 ml. 5.1.3.3 If Hg analysis will not be performed, the fourth, fifth, and sixth impingers as shown in Figure 29-1 are not required. 5.1.3.4 To Insure leak-free sampling train connections and to prevent possible sample contamination problems. use Teflon tape or other non-contaminating material instead of silicone grease. Precaution: Exercise extreme care to prevent contamination within the train. Prevent the acidic KMnO4 from contacting any glassware that contains sample material to be analyzed for Mn. Prevent acidic H₂O₂ from mixing with the acidic KMnO4. 5.1.4 Leak-Check Procedures. Follow the leak-check procedures given in Method 5, Section 4.1.4.1 (Pretest Leak-Check), Section 4.1.4.2 (Leak-Checks During the Sample Run), and Section 4.1.4.3 (Post-Test Leak- Checks). 5.1.5 Sampling Train Operation. Follow the procedures given In Method 5. Section 4.1.5. When sampling for Hg. use a procedure analagous to that described in Section 7.1.1 of Method 101A, 40 CFR Part 61, Appendix B. if necessary to maintain the desired color in the last acidified permanganate impinger. For each run. record the data required on a data sheet such as the one shown in Figure 5-2 of Method 5. 5.1.6 Calculation of Percent Isokinetic. Same as Method 5. Section 4.1.6. 5.2 Sample Recovery. 5.2.1 Begin cleanup procedures as soon as the probe is removed from the stack at the end of a sampling period. The probe should be allowed to cool prior to sample recovery. When It can be safely handled. wipe off all external particulate matter near the tip of the probe nozzle and place a rinsed, non-contaminating cap over the probe nozzle to prevent losing or gaining particulate matter. Do not cap the probe tip tightly while the sampling train is cooling: a vacuum can form in the filter holder with the undesired result of drawing liquid from the impingers onto the filter. 5.2.2 Before moving the sampling train to the cleanup site, remove the probe from the sampling train and cap the open outlet. Be careful not to lose any condensate that might be present. Cap the filter inlet where the probe was fastened. Remove the umbil- Ical cord from the last impinger and cap the Impinger. Cap the filter holder outlet and Impinger inlet. Use non-contaminating caps, whether ground-glass stoppers, plastic caps, serum caps, or Teflon tape to close these openings. Environmental Protection Agency, EPA 5.2.3 Alternatively. the following procedure may be used to disassemble the train before the probe and filter holder/oven are completely cooled: Initially disconnect the filter holder outlet/Impinger inlet and loosely cap the open ends. Then disconnect the probe from the filter holder or cyclone inlet and loosely cap the open ends. Cap the probe tip and remove the umbilical cord as previously described. 5.2.4 Transfer the probe and filter-impinger assembly to a cleanup area that is clean and protected from the wind and other potential causes of contamination or loss of sample. Inspect the train before and during disassembly and note any abnormal conditions. Take special precautions to assure that all the Items necessary for recovery do not contaminate the samples. The sample is recovered and treated as follows (see schematic in Figures 29-2a and 29-2b): Pt. 60, App. A, Meth. 29 ER25AP96.001 ER25AP86.002 5.2.5 Container No. 1 (Sample Filter). Carefully remove the filter from the filter holder and place it in its labeled petri dish container. To handle the filter. use either acid-washed polypropylene or Teflon coated tweezers or clean, disposable surgical gloves rinsed with water and dried. If it is necessary Pt. 60, App. A, Meth. 29 to fold the filter. make certain the particulate cake is Inside the fold. Carefully transfer the filter and any particulate matter or filter fibers that adhere to the filter holder gasket to the petri dish by using a dry (acidcleaned) nylon bristle brush. Do not use any metal-containing materials when recovering this train. Seal the labeled petri dish. 5.2.6 Container No. 2. (Acetone Rinse). Perform this procedure only if a determination of particulate emissions is to be made. Quantitatively recover particulate matter and any condensate from the probe nozzle, probe fitting, probe liner, and front half of the filter holder by washing these components with a total of 100 ml of acetone, while simultaneously taking great care to see that no dust on the outside of the probe or other surfaces gets In the sample. The use of exactly 100 ml is necessary for the subsequent blank correction procedures. Distilled water may be used Instead of acetone when approved by the Administrator and shall be used when specified by the Administrator: in these cases, save a water blank and follow the Administrator's directions on analysis. 5.2.6.1 Carefully remove the probe nozzle, and clean the inside surface by rinsing with acetone from a wash bottle while brushing with a non-metallic brush. Brush until the acetone rinse shows no visible particles, then make a final rinse of the inside surface with acetone. 5.2.6.2 Brush and rinse the sample exposed inside parts of the probe fitting with acetone in a similar way until no visible particles remain. Rinse the probe liner with acetone by tilting and rotating the probe while squirting acetone Into its upper end SO that all inside surfaces will be wetted with acetone. Allow the acetone to drain from the lower end into the sample container. A funnel may be used to aid in transferring liquid washings to the container. Follow the acetone rinse with a non-metallic probe brush. Hold the probe in an Inclined position. squirt acetone into the upper end as the probe brush is being pushed with a twisting action three times through the probe. Hold a sample container underneath the lower end of the probe, and catch any acetone and particulate matter which is brushed through the probe until no visible particulate matter is carried out with the acetone or until none remains In the probe liner on visual inspection. Rinse the brush with acetone, and quantitatively collect these washings in the sample container. After the brushing, make a final acetone rinse of the probe as described above. 5.2.6.3 It is recommended that two people clean the probe to minimize sample losses. Between sampling runs, keep brushes clean and protected from contamination. Clean the inside of the front-half of the filter holder by rubbing the surfaces with a non-metallic brush and rinsing with acetone. Rinse each surface three times or more if needed to remove visible particulate. Make a final rinse of the brush and filter holder. After all acetone washings and particulate matter have been collected in the sample container, tighten the lid so that acetone will not leak out when shipped to the laboratory. Mark the height of the fluid level to determine whether or not leakage occurred during transport. Clearly label the container to identify its contents. 5.2.7 Container No. 3 (Probe Rinse). Keep the probe assembly clean and free from contamination during the probe rinse. Rinse the probe nozzle and fitting. probe liner. and front-half of the filter holder thoroughly with a total of 100 ml of 0.1 N HNO 3, and place the wash into a sample storage container. (NOTE: The use of a total of exactly 100 ml is necessary for the subsequent blank correction procedures.) Perform the rinses as applicable and generally as described in Method 12, Section 5.2.2. Record the volume of the rinses. Mark the height of the fluid level on the outside of the storage container and use this mark to determine If leakage occurs during transport. Seal the container, and clearly label the contents. Finally, rinse the nozzle, probe liner, and front-half of the filter holder with water followed by acetone, and discard these rinses. 5.2.8 Container No. 4 (Impingers 1 through 3. Moisture Knockout Impinger. when used, HNO₃/H₂O₂ Impingers Contents and Rinses). Due to the potentially large quantity of liquld involved, the tester may place the impinger solutions from Impingers 1 through 3 in more than one container, if necessary. Measure the liquid in the first three impingers to within 0.5 ml using a graduated cylinder. Record the volume. This Information is required to calculate the moisture content of the sampled flue gas. Clean each of the first three Impingers, the filter support. the back half of the filter housing. and connecting glassware by thoroughly rinsing with 100 ml of 0.1 N HNO 3 using the procedure as applicable in Method 12, Section 5.2.4. (NOTE: The use of exactly 100 ml of 0.1 N HNO3 rinse is necessary for the subsequent blank correction procedures. Combine the rinses and impinger solutions, measure and record the final total volume. Mark the height of the fluid level. seal the container, and clearly label the contents.) 5.2.9 Container Nos. 5A (0.1 N HNO3). 5B (KMnOJH₂SO₄ absorbing solution). and 5C (8 N HCI rinse and dilution). 5.2.9.1 When sampling for Hg. pour all the liquid from the impinger (normally impinger No. 4) that immediately preceded the two permanganate impingers into a graduated cylinder and measure the volume to within 0.5 ml. This Information is required to calculate the moisture content of the sampled Environmental Protection Agency, EPA flue gas. Place the liquid in Container No. 5A. Rinse the Impinger with exactly 100 ml of 0.1 N HNO3 and place this rinse in Container No. 5A. 5.2.9.2 Pour all the liquid from the two permanganate impingers into a graduated cylinder and measure the volume to within 0.5 ml. This information is required to calculate the moisture content of the sampled flue gas. Place this acidic KMnO4 solution into Container No. 5B. Using a total of exactly 100 ml of fresh acidified KMnO₄ solution for all rinses (approximately 33 ml per rinse), rinse the two permanganate Impingers and connecting glassware a minimum of three times. Pour the rinses into Container No. 5B. carefully assuring transfer of all loose precipitated materials from the two impingers. Similarly, using 100 ml total of water, rinse the permanganate impingers and connecting glass a minimum of three times, and pour the rinses into Container 5B, carefully assuring transfer of any loose precipitated material. Mark the height of the fluid level, and clearly label the contents. Read the Precaution: In Section 4.3.2. NOTE: Due to the potential reaction of KMnO4 with acid, pressure buildup can occur in the sample storage bottles. Do not fill these bottles completely and take precautions to relieve excess pressure. A No. 70-72 hole drilled in the container cap and Teflon liner has been used successfully. 5.2.9.3 If no visible deposits remain after the water rinse, no further rinse is necessary. However, if deposits remain on the impinger surfaces, wash them with 25 ml of 8 N HCI, and place the wash in a separate sample container labeled No. 5C containing 200 ml of water. First. place 200 ml of water in the container. Then wash the impinger walls and stem with the HCI by turning the impinger on its side and rotating it so that the HCI contacts all inside surfaces. Use a total of only 25 ml of 8 N HCI for rinsing both permanganate impingers combined. Rinse the first Impinger, then pour the actual rinse used for the first impinger into the second Impinger for its rinse. Finally, pour the 25 ml of 8 N HCI rinse carefully into the container. Mark the height of the fluid level on the outside of the container to determine if leakage occurs during transport. 5.2.10 Container No. 6 (Silica Gel). Note the color of the Indicating silica gel to determine whether it has been completely spent and make a notation of its condition. Transfer the silica gel from its impinger to its original container and seal it. The tester may use a funnel to pour the silica gel and a rubber policeman to remove the silica gel from the impinger. The small amount of particles that might adhere to the impinger wall need not be removed. Do not use water or other liquids to transfer the silica gel since weight gained in the silica gel impinger is used for moisture calculations. Alternatively, if a balance is available in the field. record the weight of the spent silica gel (or silica gel plus impinger) to the nearest 0.5 g. 5.2.11 Container No. 7 (Acetone Blank). If particulate emissions are to be determined, at least once during each field test, place a 100-ml portion of the acetone used in the sample recovery process into a container labeled No. 7. Seal the container. 5.2.12 Container No. 8A (0.1 N HNO3 Blank). At least once during each field test, place 300 ml of the 0.1 N HNO3 solution used in the sample recovery process into a container labeled No. 8A. Seal the container. 5.2.13 Container No. 8B (Water Blank). At least once during each field test, place 100 ml of the water used in the sample recovery process Into a container labeled No. BB. Seal the container. 5.2.14 Container No. 9 (5 Percent HNO/10 Percent H2O2 Blank). At least once during each field test, place 200 ml of the 5 Percent HNO3/10 Percent H2O2 solution used as the nitric acid impinger reagent into a container labeled No. 9. Seal the container. 5.2.15 Container No. 10 (Acidified KMnO, Blank). At least once during each field test, place 100 ml of the acidified KMnO4 solution used as the Impinger solution and in the sample recovery process into a container labeled No. 10. Prepare the container as described in Section 5.2.9.2. Read the Precaution: in Section 4.3.2. and read the N OTE in