Enmienda las Reglas 102 y 405 del Reglamento para el Control de la Contaminación Atmosférica

5.2.16 Container No. 11 (8 N HCI Blank). At least once during each field test, place 200 ml of water Into a sample container labeled No. 11. Then carefully add with stirring 25 ml of 8 N HCI. Mix well and seal the container. 5.2.17 Container No. 12 (Sample Filter Blank). Once during each field test, place into a petri dish labeled No. 12 three unused blank filters from the same lot as the sampling filters. Seal the petri dish. 5.3 Sample Preparation. Note the level of the liquid in each of the containers and determine if any sample was lost during shipment. If a noticeable amount of leakage has occurred, either void the sample or use methods, subject to the approval of the Administrator, to correct the final results. A diagram illustrating sample preparation and analysis procedures for each of the sample train components is shown in Figure 29-3. 5.3.1 Container No. 1 (Sample Filter). 5.3.1.1 If particulate emissions are being determined. first desiccate the filter and filter catch without added heat (do not heat the filters to speed the drying) and weigh to a constant weight as described in Section 4.3 of Method 5. 5.3.1.2 Following this procedure, or initially, if particulate emissions are not being determined in addition to metals analysis, divide the filter with its filter catch into portions containing approximately 0.5 B Pt. 60, App. A, Meth. 29 each. Place the pieces in the analyst's choice of either Individual microwave pressure relief vessels or Parr Bombs. Add 6 ml of concentrated HNO3 and 4 ml of concentrated HF to each vessel. For microwave heating. microwave the samples for approximately 12 to 15 minutes total heating time as follows: heat for 2 to 3 minutes, then turn off the microwave for 2 to 3 minutes, then heat for 2 to 3 minutes. etc.. continue this alternation until the 12 to 15 minutes total heating time are completed (this procedure should comprise approximately 24 to 30 minutes at 600 watts). Microwave heating times are approximate and are dependent upon the number of samples being digested simultaneously. Sufficient heating is evidenced by sorbent reflux within the vessel. For conventional heating, heat the Parr R Bombs at 140 °C (285 °F) for 6 hours. Then cool the samples to room temperature. and combine with the acid digested probe rinse as required in Section 5.3.3. 5.3.1.3 If the sampling train Includes an optional glass cyclone in front of the filter, prepare and digest the cyclone catch by the procedures described in section 5.3.1.2 and then combine the digestate with the digested filter sample. 5.3.2 Container No. 2 (Acetone Rinse). Note the level of liquid in the container and confirm on the analysis sheet whether or not leakage occurred during transport. If a noticeable amount of leakage has occurred, either void the sample or use methods, subject to the approval of the Administrator, to correct the final results. Measure the liquid in this container either volumetrically within 1 ml or gravimetrically within 0.5 g. Transfer the contents to an acid-cleaned, tared 250-ml beaker and evaporate to dryness at ambient temperature and pressure. If particulate emissions are being determined, desiccate for 24 hours without added heat, weigh to a constant weight according to the procedures described in Section 4.3 of Method 5, and report the results to the nearest 0.1 mg. Redissolve the residue with 10 ml of concentrated HNO3. ER25AP96.003 Quantitatively combine the resultant sample, including all liquid and any particulate matter, with Container No. 3 before beginning Section 5.3.3. 5.3.3 Container No. 3 (Probe Rinse). Verify that the pH of this sample is 2 or lower. If it is not, acidify the sample by careful addition with stirring of concentrated HNO 3 to pH 2. Use water to rinse the sample into a beaker, and cover the beaker with a ribbed watch glass. Reduce the sample volume to approximately 20 ml by heating on a hot plate at a temperature just below boiling. Digest the sample in microwave vessels or Parr* Bombs by quantitatively transferring the sample to the vessel or bomb, carefully adding the 6 ml of concentrated HNO 3. 4 ml of concentrated HF, and then continuing to follow the procedures described in Section 5.3.1.2. Then combine the resultant sample directly with the acid digested portions of the filter prepared previously in Section 5.3.1.2. The resultant combined sample is referred to as "Sample Fraction 1". Filter the combined sample using Whatman 541 filter paper. Dilute to 300 ml (or the appropriate volume for the expected metals concentration) with water. This diluted sample is "Analytical Fraction 1". Measure and record the volume of Analytical Fraction 1 to within 0.1 ml. Quantitatively remove a 50-ml aliquot and label as "Analytical Fraction 1B". Label the remaining 250-ml portion as "Analytical Fraction 1A". Analytical Fraction IA is used for ICAP or AAS analysis for all desired metals except Hg. Analytical Fraction 1B is used for the determination of front-half Hg. 5.3.4 Container No. 4 (Impingers 1-3). Measure and record the total volume of this sample to within 0.5 ml and label it "Sample Fraction 2". Remove a 75- to 100-ml aliquot for Hg analysis and label the aliquot "Analytical Fraction 2B". Label the remaining portion of Container No. 4 as "Sample Fraction 2A". Sample Fraction 2A defines the volume of Analytical Fraction 2A prior to digestion. All of Sample Fraction 2A is digested to produce "Analytical Fraction 2A". Analytical Fraction 2A defines the volume of Sample Fraction 2A after its digestion and the volume of Analytical Fraction 2A is normally 150 ml. Analytical Fraction 2A is analyzed for all metals except Hg. Verify that the pH of Sample Fraction 2A is 2 or lower. If necessary, use concentrated HNO3 by careful addition and stirring to lower Sample Fraction 2A to pH 2. Use water to rinse Sample Fraction 2A into a beaker and then cover the beaker with a ribbed watch glass. Reduce Sample Fraction 2A to approximately 20 ml by heating on a hot plate at a temperature Just below bolling. Then follow either of the digestion procedures described in Sections 5.3.4.1 or 5.3.4.2. 5.3.4.1 Conventional Digestion Procedure. Add 30 ml of 50 percent HNO₃ and heat for 30 minutes on a hot plate to just below boiling. Add 10 ml of 3 percent H₂O₂ and heat for 10 more minutes. Add 50 ml of hot water, and heat the sample for an additional 20 minutes. Cool. filter the sample. and dilute to 150 ml (or the appropriate volume for the expected metals concentrations) with water. This dilution produces Analytical Fraction 2A. Measure and record the volume to within 0.1 ml. 5.3.4.2 Microwave Digestion Procedure. Add 10 ml of 50 percent HNO₃ and heat for 6 minutes total heating time in alternations of 1 to 2 minutes at 600 Watts followed by 1 to 2 minutes with no power, etc., similar to the procedure described in Section 5.3.1. Allow the sample to cool. Add 10 ml of 3 percent H₂O₂ and heat for 2 more minutes. Add 50 ml of hot water, and heat for an additional 5 minutes. Cool, filter the sample, and dilute to 150 ml (or the appropriate volume for the expected metals concentrations) with water. This dilution produces Analytical Fraction 2A. Measure and record the volume to within 0.1 ml. (NOTE: All microwave heating times given are approximate and are dependent upon the number of samples being digested at a time. Heating times as given above have been found acceptable for simultaneous digestion of up to 12 individual samples. Sufficient heating is evidenced by solvent reflux within the vessel.) 5.3.5 Container No. 5A (Impinger 4), Container Nos. 5B and 5C (Impingers 5 and 6). Keep the samples in Containers Nos. 5A, 5B, and 5C separate from each other. Measure and record the volume of 5A to within 0.5 ml. Label the contents of Container No. 5A to be Analytical Fraction 3A. To remove any brown MnO2 precipitate from the contents of Container No. 5B, filter its contents through Whatman 40 filter paper into a 500 ml volumetric flask and dilute to volume with water. Save the filter for digestion of the brown MnO₂ precipitate. Label the 500 ml flltrate from Container No. 5B to be Analytical Fraction 3B. Analyze Analytical Fraction 3B for Hg within 48 hours of the filtration step. Place the saved filter, which was used to remove the brown MnO₂ precipitate, into an appropriately sized vented container, which will allow release of any gases including chlorine formed when the filter is digested. In a laboratory hood which will remove any gas produced by the digestion of the MnO₂, add 25 ml of 8 N HCI to the filter and allow to digest for a minimum of 24 hours at room temperature. Filter the contents of Container No. 5C through a Whatman 40 filter into a 500-ml volumetric flask. Then filter the result of the digestion of the brown MnO₂ from Container No. 5B through a Whatman 40 filter into the same 500-ml volumetric flask, and dilute and mix well to volume with water. Discard the Whatman 40 filter. Mark this combined 500-ml dilute HCI solution as Analytical Fraction 3C. 5.3.6 Container No. 6 (Silica Gel). Weigh the spent silica gel (or silica gel plus impinger) to the nearest 0.5 g using a balance. 5.4 Sample Analysis. For each sampling train sample run, seven individual analytical samples are generated; two for all desired Environmental Protection Agency, EPA metals except Hg. and five for Hg. A schematic identifying each sample container and the prescribed analytical preparation and analysis scheme is shown in Figure 29-3. The first two analytical samples, labeled Analytical Fractions 1A and 1B, consist of the digested samples from the front-half of the train. Analytical Fraction 1A is for ICAP, ICP-MS or AAS analysis as described in Sections 5.4.1 and 5.4.2. respectively. Analytical Fraction 1B is for front-half Hg analysis as described in Section 5.4.3. The contents of the back-half of the train are used to prepare the third through seventh analytical samples. The third and fourth analytical samples, labeled Analytical Fractions 2A and 2B, contain the samples from the moisture removal impinger No. 1. If used, and HNO3 H2O₂ impingers Nos. 2 and 3. Analytical Fraction 2A is for ICAP, ICP-MS or AAS analysis for target metals, except Hg. Analytical Fraction 2B is for analysis for Hg. The fifth through seventh analytical samples, labeled Analytical Fractions 3A, 3B, and 3C, consist of the impinger contents and rinses from the empty impinger No. 4 and the H 2SO/KMnO4 Impingers Nos. 5 and 6. These analytical samples are for analysis for Hg as described in Section 5.4.3. The total back-half Hg catch is determined from the sum of Analytical Fractions 2B, 3A, 3B, and 3C. Analytical Fractions 1A and 2A can be combined proportionally prior to analysis. 5.4.1 ICAP and ICP-MS Analysis. Analyze Analytical Fractions 1A and 2A by ICAP using Method 6010 or Method 200.7 (40 CFR part 136, appendix C). Calibrate the ICAP. and set up an analysis program as described in Method 6010 or Method 200.7. Follow the quality control procedures described in Section 7.3.1. Recommended wavelengths for analysis are as follows: Pt. 60, App. A, Meth. 29 Wave- Element length (nm) Aluminum 308.215 Antimony 206.833 Arsenic 193.696 Barlum 455.403 Beryllium 313.042 Wave- Element length (nm) Cadmium 226.502 Chromium 267.716 Cobalt 228.616 Copper 324.754 Iron 259.940 Lead 220.353 Manganese 257.610 Nickel 231.604 Phosphorous 214.914 Selenium 196.026 Silver 328.068 Thailium 190.864 Zinc 213.858 These wavelengths represent the best combination of specificity and potential detection limit. Other wavelengths may be substituted if they can provide the needed specificity and detection limit. and are treated with the same corrective techniques for spectral Interference. Initially, analyze all samples for the target metals (except Hg) plus Fe and Al. If Fe and Al are present. the sample might have to be diluted so that each of these elements is at a concentration of less than 50 ppm so as to reduce their spectral interferences on As. Cd. Cr. and Pb. Perform ICP-MS analysis by following Method 6020 in EPA Publication SW-846 Third Edition (November 1986) including updates I, II. IIA. and пв. as incorporated by reference in $60.17(i). (NOTE: When analyzing samples In a HF matrix, an alumina torch should be used; since all front-half samples will contain HF, use an alumina torch.) 5.4.2. AAS by Direct Aspiration and/or GFAAS. If analysis of metals in Analytical Fractions 1A and 2A by using GFAAS or direct aspiration AAS is needed, use Table 29- 2 to determine which techniques and procedures to apply for each target metal. Use Table 29-2. if necessary. to determine techniques for minimization of Interferences. Calibrate the Instrument according to Section 6.3 and follow the quality control procedures specified in Section 7.3.2. TABLE 29-2.-APPLICABLE TECHNIQUES, METHODS AND MINIMIZATION OF INTERFERENCE FOR AAS ANALYSIS Metal SW-8461 Technique Wavelength Interferences method No. (nm) Cause Minimization Fe Aspiration 7380 248.3 Contamination Great care taken to avoid contamination. Pb Aspiration 7420 283.3 217.0 nm alternate Background correction required. Pb Furnace 7421 283.3 Poor recoveries Matrix modifier, add 10 of of phosphorus acid to 1 ml of prepared sample in sampler cup. Mn Aspiration 7460 279.5 403.1 nm alternate Background correction required. TABLE 29-2.-APPLICABLE TECHNIQUES, METHODS AND MINIMIZATION OF INTERFERENCE FOR AAS ANALYSIS-Continued Technique SW-8461 Interferences Metal Wavelength method No. (nm) Cause Minimization NI Aspiration 7520 232.0 352.4 nm alternate Fe, Background correction re- Co, and Cr. quired. Matrix matching or nitrousoxide/acetylene flame. Nonlinear response sample dilution or use 352.3 nm line. Se Furnace 7740 196.0 Volatility Spike samples and reference materials and add nickel nitrate to minimize volatilization. Adsorption & scatter Background correction is required and Zeeman background correction can be useful. Ag Aspiration 7760 328.1 Adsorption & Scatter AgCl Background correction is insoluble. required. Avoid Hydrochioric acid unless silver is in solution as a chioride complex Sample and standards montored for aspiration rate. TI Aspiration 7840 276.8 Background correction is required. Hydrochloric acid should not be used. TI Furnace 7841 276.8 Hydrochloric acid or chio- Background correction is ride. required. Verify that losses are not occurring for volatization by spiked samples or standard addition; Palladium is B suitable matrix modifier. Zn Aspiration 7950 213.9 High Si, Cu, & P Contami- Strontium removes Cu and nation. phosphate, Great care taken to avoid contamination. Sb Aspiration 7040 217.6 1000 mg/ml Pb NI, Cu, or Use secondary waveacid. lengths of 231.1.nm; match sample & standands acid concentration or use nitrous oxidefacetylene flame. Sb Furnace 7041 217.6 High Pb Secondary Wavelength or Zeeman correction. As Furnace 7060 193.7 Arsenic volatilization Spiked samples and add Aluminum nickel nitrate solution to digestates prior to anaiysis. Use Zeeman background correction. Ba Aspiration 7080 7080 553.6 Calcium High hollow cathode our- Barium ionization rent and narrow band sel. 2 ml of KCI per 100 ml of sample. Be Aspiration 7090 234.9 500 ppm AI High Mg and Add 0.1% fluoride. Si. Use method of standard additions. Be Furnace 7091 234.9 Be in optical path Optimize parameters to minimize effects. Cd Aspiration 7130 228.8 Absorption and light scat- Background correction is tering. required. Cd Furnace 7131 228.8 As above As above. Excess Chloride Ammonium phosphate Pipet tips used as 8 matrix modifier. Use cadmiun-free tips. Environmental Protection Agency, EPA TABLE 29-2.-APPLICABLE TECHNIQUES, METHODS AND MINIMIZATION OF INTERFERENCE FOR AAS ANALYSIS-Continued Metal Technique SW-8461 Wavelength Interferences method No. (nm) Cause Minimization Cr Aspiration 7190 357.9 Akali metal KCI ionization suppressant in samples and standards-Consult mfgs literature. Co Furnace 7201 240.7 Excess chloride Use Method of Standard Additions. Cr Furnace 7191 357.9 200 mg/L Ca and P All calcium nitrate for a known constant effect and to eliminate effect of phosphate. Cu Aspiration 7210 324.7 Absorption & scatter Consult manufacturer's manual. 1 Refer to EPA publication SW-846 Third Edition (November 1986) including updates I, II, IIA, and IIB, as incorporated by reference in $60.17(i). 5.4.3 CVAAS Hg analysis. Analyze Analytical Fractions 1B, 2B, 3A, 3B. and 3C separately for Hg using CVAAS following the method outlined in Method 7470 in EPA Publication SW-846 Third Edition (November 1986) including updates I. II, IIA and UB, as Incorporated by reference in $60.17(i) or in Standard Methods for the Examination of Water and Wastewater, 16th Edition, (1985). Method 303F, as incorporated by reference in $60.17. or, optionally using NOTE No. 2 in this section. Set up the calibration curve (zero to 1000 ng) as described in Method 7470 or similar to Method 303F using 300-ml BOD bottles instead of Erlenmeyers. Perform the following for each Hg analysis. From each original sample, select and record an aliquot in the size range from 1 ml to 10 ml. If no prior knowledge of the expected amount of Hg in the sample exists. a 5 ml aliquot Is suggested for the first dilution to 100 ml (see NOTE No. 1 in this Section). The total amount of Hg in the aliquot shall be less than I µ g and within the range (zero to 1000 ng) of the callbration curve. Place the sample aliquot into a separate 300-ml BOD bottle, and add enough water to make a total volume of 100 ml. Next add to it sequentially the sample digestion solutions and perform the sample preparation described In the procedures of Method 7470 or Method 303F. (See NOTE No. 2 in this Section). If the maximum readings are off-scale (because Hg in the allquot exceeded the calibration range; Including the situation where only a 1-ml aliquot of the original sample was digested). then dilute the original sample (or a portion of it) with 0.15 percent HNO (1.5 ml concentrated HNO3 per liter aqueous solution) so that when a 1- to 10-ml aliquot of the "0.15 HNO3 percent dilution of the original sample" is digested and analyzed by the procedures described above, it will yield an analysis within the range of the calibration curve. NOTE No. 1 TO SECTION 5.4.3. When Hg levels in the sample fractions are below the instack detection limit given in Table 29-1. select a 10 ml aliquot for digestion and analysis as described. NOTE No. 2 TO SECTION 5.4.3. Optionally. Hg can be analyzed by using the CVAAS analyt- Ical procedures given by some instrument manufacturer's directions. These include callbration and quality control procedures for the Leeman Model PS200, the Perkin Elmer FIAS systems, and similar models, if available. of other instrument manufacturers. For digestion and analyses by these instruments, perform the following two steps: (1) Digest the sample aliquot through the addition of the aqueous hydroxylamine hydrochloride/sodium chloride solution the same as described in this Section 5.4.3.: (The Leeman, Perkin Elmer, and similar instruments described in this note add automatically the necessary stannous chloride solution during the automated analysis of Hg.) and (2) Upon completion of the digestion described in paragraph (I), of this note, analyze the sample according to the instrument manufacturer's directions. This approach allows multiple (Including duplicate) automated analyses of a digested sample aliquot. 6. Calibration Maintain a laboratory log of all calibrations. 6.1 Sampling Train Calibration. Calibrate the sampling train components according to the Indicated sections of Method 5: Probe Nozzle (Section 5.1); Pitot Tube (Section 5.2): Metering System (Section 5.3): Probe Heater (Section 5.4): Temperature Gauges (Section 5.5); Leake-Check of the Metering System (Section 5.6): and Barometer (Section 5.7). 6.2 Industively Coupled Argon Plasma Spectrometer Calibration. Prepare standards as outlined In Section 4.5. Profile and calibrate the instrument according to the manufacturer's recommended procedures using those standards. Check the calibration once per hour. If the Instrument does not reproduce the standard concentrations within 10 percent, perform the complete calibration procedures. Perform ICP-MS analysis by following Method 6020 in EPA Publication SW- 846 Third Edition (November 1986) including updates I, II, ПА and IIB, as incorporated by reference in § 60.17(i). 6.3 Atomic Absorption Spectrometer-Direct Aspiration AAS, GFAAS, and CVAAS analyses. Prepare the standards as outlined in Section 4.5 and use them to calibrate the spectrometer. Calibration procedures are also outlined in the EPA methods referred to in Table 29-2 and in Method 7470 in EPA Publication SW-846 Third Edition (November 1986) including updates I. II. IIA and IIB. as incorporated by reference in $60.17(i) or in Standard Methods for the Examination of Water and Wastewater, 16th Edition, (1985). Method 303F (for Hg) as incorporated by reference in $60.17. Run each standard curve in duplicate and use the mean values to calculate the calibration line. Recalibrate the instrument approximately once every 10 to 12 samples. 7. Quality Control 7.1 Field Reagent Blanks, If analyzed. Perform the digestion and analysis of the blanks in Container Nos. 7 through 12 that were produced in Sections 5.2.11 through 5.2.17, respectively. For Hg field reagent blanks. use a 10 ml aliquot for digestion and analysis. 7.1.1 Digest and analyze one of the filters from Container No. 12 per Section 5.3.1. 100 ml from Container No. 7 per Section 5.3.2. and 100 ml from Container No. 8A per Section 5.3.3. This step produces blanks for Analytical Fractions 1A and 1B. 7.1.2 Combine 100 ml of Container No. 8A with 200 ml from Container No. 9, and digest and analyze the resultant volume per Section 5.3.4. This step produces blanks for Analytical Fractions 2A and 2B. 7.1.3 Digest and analyze a 100-ml portion of Container No. 8A to produce a blank for Analytical Fraction 3A. 7.1.4 Combine 100 ml from Container No. 10 with 33 ml from Container No. 8B to produce a blank for Analytical Fraction 3B. Filter the resultant 133 ml as described for Container No. 5B in Section 5.3.5, except do not dilute the 133ml. Analyze this blank for Hg within 48 hrs. of the filtration step. and use 400 ml as the blank volume when calculating the blank mass value. Use the actual volumes of the other analytical blanks when calculating their mass values. 7.1.5 Digest the filter that was used to remove any brown MnO₂ precipitate from the blank for Analytical Fraction 3B by the same procedure as described in Section 5.3.5 for the similar sample filter. Filter the digestate and the contents of Container No. 11 through Whatman 40 paper into a 500-ml volumetric flask, and dilute to volume with water. These steps produce a blank for Analytical Fraction 3C. 7.1.6 Analyze the blanks for Analytical Fraction Blanks 1A and 2A per Section 5.4.1 and/or Section 5.4.2. Analyze the blanks for Analytical Fractions 1B. 2B, 3A. 3B. and 3C per Section 5.4.3. Analysis of the blank for Analytical Fraction 1A produces the fronthalf reagent blank correction values for the desired metals except for Hg; Analysis of the blank for Analytical Fraction IB produces the front-half reagent blank correction value for Hg. Analysis of the blank for Analytical Fraction 2A produces the back-half reagent blank correction values for all of the desired metals except for Hg. while separate analyses of the blanks for Analytical Fractions 2B. 3A, 3B, and 3C produce the back-half reagent blank correction value for Hg. 7.2 Quality Control Samples. Analyze the following quality control samples. 7.2.1 ICAP and ICP-MS Analysis. Follow the respective quality control descriptions inalyze each sample by the Method of Standard Additions. Analyze a quality control sample to check the accuracy of the calibration standards. If the results are not within 20 percent. repeat the calibration. 7.2.3 CVAAS Analysis for Hg. Analyze all samples in duplicate. Analyze a quality control sample to check the accuracy of the calibration standards (if not within 15 percent, repeat calibration). Perform a matrix spike on one sample (if not within 25 percent, analyze all samples by the Method of Standard Additions). Additional Information on quality control can be obtained from Method Environmental Protection Agency, EPA 7470 of EPA Publication SW-846 Third Edition (November 1986) Including updates I. II, IIA and IIB, as incorporated by reference in $60.17(i) or in Standard Methods for the Examination of Water and Wastewater, 16th Edition, (1985). Method 303F as incorporated by reference in $60.17. 8. Calculations 8.1 Dry Gas Volume. Using the data from this test, calculate Vₘₓ std). the dry gas sample volume at standard conditions as outlined in Section 6.3 of Method 5. 8.2 Volume of Water Vapor and Moisture Content. Using the total volume of condensate collected during the source sampling, calculate the volume of water vapor Vw (atd) and the moisture content Bws of the stack gas. Use Equations 5-2 and 5-3 of Method 5. 8.3 Stack Gas Velocity. Using the data from this test and Equation 2-9 of Method 2. calculate the average stack gas velocity. 8.4 Metals (Except Hg) in Source Sample. 8.4.1 Analytical Fraction 1A, Front-Half, Metals (except Hg). Calculate separately the amount of each metal collected in Sample Fraction 1 of the sampling train using the following equation: Ma=Cal Fd Vaoin,1 Eq. 29-1 where: Ma=Total mass of each metal (except Hg) collected in the front half of the sampling train (Sample Fraction 1), µ g. C₁=Concentration of metal in Analytical Fraction 1A as read from the standard curve. µg/ml. F&=Dilution factor (F d = the inverse of the fractional portion of the concentrated sample in the solution actually used in the instrument to produce the reading Cal. For example, If a 2 ml aliquot of Analytical Fraction 1A is diluted to 10 ml to place it in the calibration range, Fd - 5). Vaoin,1=Total volume of digested sample solution (Analytical Fraction 1). ml. 8.4.1.1 If Analytical Fractions 1A and 2A are combined, use proportional aliquots. Then make appropriate changes in Equations 29-1 through 29-3 to reflect this approach. 8.4.2 Analytical Fraction 2A, Back-Half. Metals (except Hg). Calculate separately the amount of each metal collected in Fraction 2 of the sampling train using the following equation. where: Mes-Total mass of each metal (except Hg) collected in the back-half of the sampling train (Sample Fraction 2), H g. C,-Concentration of metal in Analytical Fraction 2A as read from the standard curve. (µg/ml). Fr=Aliquot factor, volume of Sample Fraction 2 divided by volume of Sample Fraction 2A (see Section 5.3.4.) M6h=Ca F, V. Eq. 29-2 Va=Total volume of digested sample solution (Analytical Fraction 2A), ml (see Section 5.3.4.1 or 5.3.4.2, as applicable). 8.4.3 Total Train. Metals (except Hg). Calculate the total amount of each of the quantified metals collected in the sampling train as follows: M,=(M₂ - Mas) + (Mah - Monb) Eq. 29-3 where: M,=Total mass of each metal (separately stated for each metal) collected in the sampling train. µg. Mₘ₆=Blank correction value for mass of metal detected in front-half field reagent blank, µg. Math=Blank correction value for mass of metal detected In back-half field reagent blank. µg. 8.4.3.1 If the measured blank value for the front half (M mb) is in the range 0.0 to "A" µg [where "A" µg equals the value determined by multiplying 1.4 µg/in.² times the actual area in in.2 of the sample filter]. use M fhb to correct the emission sample value (Ma ): if Mmb exceeds "A" µg. use the greater of I or II: I. "A" µg. II. the lesser of (a) M thbs or (b) 5 percent of Mm. If the measured blank value for the blackhalf (Mbab) is in the range 0.0 to 1 µg, use Mbhb to correct the emission sample value (M bh): If Mbbb) exceeds 1 µg, use the greater of I or II: I. 1 µg. II. the lesser of (a) Mbhb or (b) 5 percent of Mbh. 8.5 Hg in Source Sample. 8.5.1 Analytical Fraction 1B: Front-Half Hg. Calculate the amount of Hg collected in the front-half, Sample Fraction 1, of the sampling train by using Equation 29-4: ER25AP96.005 where: Hgn=Total mass of Hg collected in the fronthalf of the sampling train (Sample Fraction 1), µg. Qa=Quantity of Hg, µg, TOTAL in the ALI- QUOT of Analytical Fraction 1B selected for digestion and analysis. 8.5.1.1 For example, if a 10 ml aliquot of Analytical Fraction 1B is taken and digested and analyzed (according to Section 5.4.3 and its NOTES Nos. 1 and 2), then calculate and use the total amount of Hg in the 10 ml allquot for Qm. Vacin,1=Total volume of Analytical Fraction 1, ml. VπB=Volume of aliquot of Analytical Fraction IB analyzed, ml. 8.5.1.2 For example, if a 1 ml aliquot of Analytical Fraction IB was diluted to 50 ml Pt. 60, App. A, Meth. 29 with 0.15 percent HNO3 as described in Section 5.4.3 to bring it into the proper analytical range, and then 1 ml of that 50-ml wa digested according to Section 5.4.3 and analyzed, VnB would be 0.02 ml. 8.5.2 Analytical Fractions 2B, 3A, 3B. and 3C: Back Half Hg. 8.5.2.1 Calculate the amount of Hg collected in Sample Fraction 2 by using Equation 29-5: 40 CFR Ch. I (7-1-99 Edition) ER25AP96.006 where: Hgsh=Total mass of Hg collected in Sample Fraction 2, µg. Q of Hg, µg. TOTAL in the ALI- QUOT of Analytical Fraction 2B selected for digestion and analysis. 8.5.2.1.1 For example, if a 10 ml aliquot of Analytical Fraction 2B is taken and digested and analyzed (according to Section 5.4.3 and its NOTES Nos. I and 2), then calculate and use the total amount of Hg in the 10 ml aliquot for Quitz- Vaoin,2=Total volume of Sample Fraction 2, ml. VπB=Volume of Analytical Fraction 2B analyzed, ml. 8.5.2.1.2 For example, If 1 ml of Analytical Fraction 2B was diluted to 10 ml with 0.15 percent HNO3 as described in Section 5.4.3 to bring it into the proper analytical range, and then 5 ml of that 10-ml was analyzed, V C2B would be 0.5 ml. 8.5.2.2 Calculate each of the back-half Hg values for Analytical Fractions 3A, 3B, and 3C by using Equation 29-6: ER25AP96.007 where: mass of Hg collected separately in Fraction 3A, 3B, or 3C, µg. Quantacy=Quantity of Hg, µg. TOTAL. separately, in the ALIQUOT of Analytical Fraction 3A, 3B. and 3C selected for digestion and analysis, (see previous notes in Sections 8.5.1 and 8.5.2 describing the quantity "Q" and calculate similarly). VO(A,B,C)=Volume, separately, of Analytical Fraction 3A. 3B, or 3C analyzed, ml (see previous notes in Sections 8.5.1 and 8.5.2, describing the quantity "V" and calculate similarly). Vaoia,KA,B,C)=Total volume, separately. of Analytical Fraction 3A. 3B. or 3C, ml. 8.5.2.3 Calculate the total amount of Hg collected in the back-half of the sampling train by using Equation 29-7: Eq. 29-7 where: Hgah=Total mass of Hg collected in the backhalf of the sampling train. µg. 8.5.3 Total Train Hg Catch. Calculate the total amount of Hg collected in the sampling train by using Equation 29-8: Eq. 29-8 where: Hg=Total mass of Hg collected In the sampling train, µg. Hgms=Blank correction value for mass of Hg detected in front-half field reagent blank. µg. Hgass-Blank correction value for mass of Hg detected in back-half field reagent blanks, µg. 8.5.4 If the total of the measured blank values (Hgmh+Hghh) is in the range of 0.0 to 0.6 µg. then use the total to correct the sample value (Hga+Hgan): if it exceeds 0.6 µg, use the greater of I. or II: II. the lesser of (a) (Hg mo+Hgbbb). or (b) 5 percent of the sample value (Hge +Hgbb). 8.6 Individual Metal Concentrations in Stack Gas. Calculate the concentration of each metal in the stack gas (dry basis, adjusted to standard conditions) by using Equation 29-9: I. 0.6 µg. ER25AP96.008 C=Concentration of a metal In the stack gas, mg/dscm. K4=10⁻³ mg/µg. M,=Total mass of that metal collected in the sampling train. µg: (substitute Hg, for M, for the Hg calculation). Vm(etd)=Volume of gas sample as measured by the dry gas meter, corrected to dry standard conditions, dscm. 8.7 Isokinetic Variation and Acceptable Results. Same as Method 5, Sections 6.11 and 6.12, respectively. Environmental Protection Agency, EPA 3. Bibliography 1. Method 303F in Standard Methods for the Examination of Water Wastewater, 16th Edition, 1985. Available from the American Public Health Association, 1015 18th Street NW., Washington, DC 20036. 2. EPA Methods 6010, 6020, 7000, 7041, 7060, 7131, 7421, 7470, 7740, and 7841, Test Methods for Evaluating Solid Waste: Physical/Chemical Methods. SW-846, Third Edition, September 1986, with updates I. II, ПА and IIB. Office of Solid Waste and Emergency Response. U.S. Environmental Protection Agency, Washington, DC 20460. 3. EPA Method 200.7. Code of Federal Regulations, Title 40. Part 136, Appendix C. July 1. 1987. Pt. 60, App. A, Meth. 29 4. EPA Methods 1 through 5, Code of Federal Regulations, Title 40, Part 60, Appendix A. July 1, 1991. 5. EPA Method 101A, Code of Federal Regulations, Title 40, Part 61, Appendix B. July 1. 1991. [36 FR 24877. Dec. 23, 1971] EDITORIAL NOTE: For FEDERAL REGISTER cltations affecting part 60, appendix A see the List of CFR Sections in the Finding Aids section of this volume. EFFECTIVE DATE NOTE: At 64 FR 26490. May 14, 1999, Appendix A to part 60 was amended by adding Methods 2F, 2G, and 2H and corrected at 64 FR 37196, July 9, 1999, and 64 FR 38241, July 15, 1999, effective July 13. 1999. 40 CFR PART 60 APPENDIX B APPENDIX B-PERFORMANCE SPECIFICATIONS Performance Specification 1-Specifications and test procedures for opacity continuous emission monitoring systems in stationary sources Performance Specification 2-Specifications and test procedures for SO₂ and NO. continuous emission monitoring systems in stationary sources Performance Specification 3-Specifications and test procedures for O₂ and CO₂ continuous emission monitoring systems in stationary sources Performance Specification 4-Specifications and test procedures for carbon monoxide continuous emission monitoring systems in stationary sources Performance Specification 4A-Specifications and test procedures for carbon monoxide continuous emission monitoring systems in stationary sources Performance Specification 5-Specifications and test procedures for TRS continuous emission monitoring systems in stationary sources Performance Specification 6-Specifications and test procedures for continuous emission rate monitoring systems in stationary sources Performance Specification 7-Specifications and test procedures for hydrogen suifide continuous emission monitoring systems in stationary sources PERFORMANCE SPECIFICATION 1-SPECIFICATIONS AND TEST PROCEDURES FOR OPACITY CONTINUOUS EMIS- SION MONITORING SYSTEMS IN STATIONARY SOURCES 1. Applicability and Principle 1.1 Applicability. This specification contains requirements for the design. performance, and installation of instruments for opacity continuous emission monitoring systerms (CEMS's) and data computation procedures for evaluating the acceptability of a CEMS. Certain design requirements and test procedures established in this specification may not apply to all instrument designs. In such instances, equivalent design requirements and test procedures may be used with prior approval of the Administrator. Performance Specification 1 (PS 1) applies to opacity monitors installed after March 30, 1983. Opacity monitors installed before March 30, 1983, are required to comply with the provisions and requirements of PS 1 except for the following: (a) Section 4. "Installation Specifications." (b) Sections 5.1.4, 5.1.6, 5.1.7, and 5.1.8 of Section 5. "Design and Performance Specifications." (c) Section 6.4 of Section 6 "Design Specifications Verification Procedure." An opacity monitor installed before March 30, 1983, need not be tested to demonstrate compliance with PS 1 unless required by regulatory action other than the promulgation of PS 1. If an existing monitor is replaced with a new monitor, PS I shall apply except that the new monitor may be located at the old measurement location regardless of whether the location meets the requirements of