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«While we have taken steps to ensure the accuracy of this Internet version of the document, it is not the official version. Please refer to the ...»

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While we have taken steps to ensure the accuracy of this Internet version of the document, it is not the official

version. Please refer to the official version in the FR publication, which appears on the Government Printing

Office's eCFR website:

http://www.ecfr.gov/cgi-bin/text-

idx?SID=c7836e6ff67e5ad001bcb19ccfd99c1a&node=40:8.0.1.1.1&rgn=div5#40:8.0.1.1.1.0.1.1.4

METHOD 8—DETERMINATION OF SULFURIC ACID AND SULFUR DIOXIDE EMISSIONS FROM

STATIONARY SOURCES

NOTE: This method does not include all of the specifications (e.g., equipment and supplies) and procedures (e.g., sampling and analytical) essential to its performance. Some material is incorporated by reference from other methods in this part. Therefore, to obtain reliable results, persons using this method should have a thorough knowledge of at least the following additional test methods: Method 1, Method 2, Method 3, Method 5, and Method 6.

1.0 Scope and Application

1.1 Analytes.

Analyte CAS No. Sensitivity

0.05 mg/m3 (0.03 × Sulfuric acid, including: Sulfuric acid (H2SO4) mist, 7664-93-9, 10−7lb/ft3).

Sulfur trioxide (SO3) 7449-11-9

1.2 mg/m3 (3 × Sulfur dioxide (SO2) 7449-09-5 10−9 lb/ft3).

1.2 Applicability. This method is applicable for the determination of H2SO4 (including H2SO4 mist and SO3) and gaseous SO2 emissions from stationary sources.

NOTE: Filterable particulate matter may be determined along with H2SO4 and SO2 (subject to the approval of the Administrator) by inserting a heated glass fiber filter between the probe and isopropanol impinger (see section 6.1.1 of Method 6). If this option is chosen, particulate analysis is gravimetric only; sulfuric acid is not determined separately.

1.3 Data Quality Objectives. Adherence to the requirements of this method will enhance the quality of the data obtained from air pollutant sampling methods.

2.0 Summary of Method A gas sample is extracted isokinetically from the stack. The H2SO4 and the SO2 are separated, and both fractions are measured separately by the barium-thorin titration method.

3.0 Definitions [Reserved]

4.0 Interferences

4.1 Possible interfering agents of this method are fluorides, free ammonia, and dimethyl aniline.

If any of these interfering agents is present (this can be determined by knowledge of the process), alternative methods, subject to the approval of the Administrator, are required.

5.0 Safety

5.1 Disclaimer. This method may involve hazardous materials, operations, and equipment. This testmethod may not address all of the safety problems associated with its use. It is the responsibility of the user of this test method to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to performing this test method.

5.2 Corrosive reagents. Same as Method 6, section 5.2.

6.0 Equipment and Supplies

6.1 Sample Collection. Same as Method 5, section 6.1, with the following additions and

exceptions:

6.1.1 Sampling Train. A schematic of the sampling train used in this method is shown in Figure 8-1; it is similar to the Method 5 sampling train, except that the filter position is different, and the filter holder does not have to be heated. See Method 5, section 6.1.1, for details and guidelines on operation and maintenance.

6.1.1.1 Probe Liner. Borosilicate or quartz glass, with a heating system to prevent visible condensation during sampling. Do not use metal probe liners.

6.1.1.2 Filter Holder. Borosilicate glass, with a glass frit filter support and a silicone rubber gasket. Other gasket materials (e.g., Teflon or Viton) may be used, subject to the approval of the Administrator. The holder design shall provide a positive seal against leakage from the outside or around the filter. The filter holder shall be placed between the first and second impingers. Do not heat the filter holder.

6.1.1.3 Impingers. Four, of the Greenburg-Smith design, as shown in Figure 8-1. The first and third impingers must have standard tips. The second and fourth impingers must be modified by replacing the insert with an approximately 13-mm (1⁄2 -in.) ID glass tube, having an unconstricted tip located 13 mm (1⁄2 in.) from the bottom of the impinger. Similar collection systems, subject to the approval of the Administrator, may be used.

6.1.1.4 Temperature Sensor. Thermometer, or equivalent, to measure the temperature of the gas leaving the impinger train to within 1 °C (2 °F).

6.2 Sample Recovery. The following items are required for sample recovery:

6.2.1 Wash Bottles. Two polyethylene or glass bottles, 500-ml.

6.2.2 Graduated Cylinders. Two graduated cylinders (volumetric flasks may be used), 250-ml, 1liter.

6.2.3 Storage Bottles. Leak-free polyethylene bottles, 1-liter size (two for each sampling run).

6.2.4 Trip Balance. 500-g capacity, to measure to ±0.5 g (necessary only if a moisture content analysis is to be done).

6.3 Analysis. The following items are required for sample analysis:

6.3.1 Pipettes. Volumetric 10-ml, 100-ml.

6.3.2 Burette. 50-ml.

6.3.3 Erlenmeyer Flask. 250-ml (one for each sample, blank, and standard).





6.3.4 Graduated Cylinder. 100-ml.

6.3.5 Dropping Bottle. To add indicator solution, 125-ml size.

7.0 Reagents and Standards NOTE: Unless otherwise indicated, all reagents are to conform to the specifications established by the Committee on Analytical Reagents of the American Chemical Society, where such specifications are available. Otherwise, use the best available grade.

7.1 Sample Collection. The following reagents are required for sample collection:

7.1.1 Filters and Silica Gel. Same as in Method 5, sections 7.1.1 and 7.1.2, respectively.

7.1.2 Water. Same as in Method 6, section 7.1.1.

7.1.3 Isopropanol, 80 Percent by Volume. Mix 800 ml of isopropanol with 200 ml of water.

NOTE: Check for peroxide impurities using the procedure outlined in Method 6, section 7.1.2.1.

7.1.4 Hydrogen Peroxide (H2O2), 3 Percent by Volume. Dilute 100 ml of 30 percent H2O2) to 1 liter with water. Prepare fresh daily.

7.1.5 Crushed Ice.

7.2 Sample Recovery. The reagents and standards required for sample recovery are:

7.2.1 Water. Same as in section 7.1.2.

7.2.2 Isopropanol, 80 Percent. Same as in section 7.1.3.

7.3 Sample Analysis. Same as Method 6, section 7.3.

8.0 Sample Collection, Preservation, Storage, and Transport

8.1 Pretest Preparation. Same as Method 5, section 8.1, except that filters should be inspected but need not be desiccated, weighed, or identified. If the effluent gas can be considered dry (i.e., moisture-free), the silica gel need not be weighed.

8.2 Preliminary Determinations. Same as Method 5, section 8.2.

8.3 Preparation of Sampling Train. Same as Method 5, section 8.3, with the following

exceptions:

8.3.1 Use Figure 8-1 instead of Figure 5-1.

8.3.2 Replace the second sentence of Method 5, section 8.3.1 with: Place 100 ml of 80 percent isopropanol in the first impinger, 100 ml of 3 percent H2O2 in both the second and third impingers; retain a portion of each reagent for use as a blank solution. Place about 200 g of silica gel in the fourth impinger.

8.3.3 Ignore any other statements in section 8.3 of Method 5 that are obviously not applicable to the performance of Method 8.

NOTE: If moisture content is to be determined by impinger analysis, weigh each of the first three impingers (plus absorbing solution) to the nearest 0.5 g, and record these weights. Weigh also the silica gel (or silica gel plus container) to the nearest 0.5 g, and record.)

8.4 Metering System Leak-Check Procedure. Same as Method 5, section 8.4.1.

8.5 Pretest Leak-Check Procedure. Follow the basic procedure in Method 5, section 8.4.2, noting that the probe heater shall be adjusted to the minimum temperature required to prevent condensation, and also that verbage such as “* * * plugging the inlet to the filter holder * * * ” found in section 8.4.2.2 of Method 5 shall be replaced by “ * * * plugging the inlet to the first impinger * * * ”. The pretest leak-check is recommended, but is not required.

8.6 Sampling Train Operation. Follow the basic procedures in Method 5, section 8.5, in

conjunction with the following special instructions:

8.6.1 Record the data on a sheet similar to that shown in Figure 8-2 (alternatively, Figure 5-2 in Method 5 may be used). The sampling rate shall not exceed 0.030 m3/min (1.0 cfm) during the run. Periodically during the test, observe the connecting line between the probe and first impinger for signs of condensation. If condensation does occur, adjust the probe heater setting upward to the minimum temperature required to prevent condensation. If component changes become necessary during a run, a leak-check shall be performed immediately before each change, according to the procedure outlined in section 8.4.3 of Method 5 (with appropriate modifications, as mentioned in section 8.5 of this method); record all leak rates. If the leakage rate(s) exceeds the specified rate, the tester shall either void the run or plan to correct the sample volume as outlined in section 12.3 of Method 5. Leak-checks immediately after component changes are recommended, but not required. If these leak-checks are performed, the procedure in section 8.4.2 of Method 5 (with appropriate modifications) shall be used.

8.6.2 After turning off the pump and recording the final readings at the conclusion of each run, remove the probe from the stack. Conduct a post-test (mandatory) leak-check as outlined in section 8.4.4 of Method 5 (with appropriate modifications), and record the leak rate. If the posttest leakage rate exceeds the specified acceptable rate, either correct the sample volume, as outlined in section 12.3 of Method 5, or void the run.

8.6.3 Drain the ice bath and, with the probe disconnected, purge the remaining part of the train by drawing clean ambient air through the system for 15 minutes at the average flow rate used for sampling.

NOTE: Clean ambient air can be provided by passing air through a charcoal filter. Alternatively, ambient air (without cleaning) may be used.

8.7 Calculation of Percent Isokinetic. Same as Method 5, section 8.6.

8.8 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. Treat the samples as follows:

8.8.1 Container No. 1.

8.8.1.1 If a moisture content analysis is to be performed, clean and weigh the first impinger (plus contents) to the nearest 0.5 g, and record this weight.

8.8.1.2 Transfer the contents of the first impinger to a 250-ml graduated cylinder. Rinse the probe, first impinger, all connecting glassware before the filter, and the front half of the filter holder with 80 percent isopropanol. Add the isopropanol rinse solution to the cylinder. Dilute the contents of the cylinder to 225 ml with 80 percent isopropanol, and transfer the cylinder contents to the storage container. Rinse the cylinder with 25 ml of 80 percent isopropanol, and transfer the rinse to the storage container. Add the filter to the solution in the storage container and mix. Seal the container to protect the solution against evaporation. Mark the level of liquid on the container, and identify the sample container.

8.8.2 Container No. 2.

8.8.2.1 If a moisture content analysis is to be performed, clean and weigh the second and third impingers (plus contents) to the nearest 0.5 g, and record the weights. Also, weigh the spent silica gel (or silica gel plus impinger) to the nearest 0.5 g, and record the weight.

8.8.2.2 Transfer the solutions from the second and third impingers to a 1-liter graduated cylinder.

Rinse all connecting glassware (including back half of filter holder) between the filter and silica gel impinger with water, and add this rinse water to the cylinder. Dilute the contents of the cylinder to 950 ml with water. Transfer the solution to a storage container. Rinse the cylinder with 50 ml of water, and transfer the rinse to the storage container. Mark the level of liquid on the container. Seal and identify the sample container.

9.0 Quality Control

9.1 Miscellaneous Quality Control Measures.

–  –  –

9.2 Volume Metering System Checks. Same as Method 5, section 9.2.

10.0 Calibration and Standardization

10.1 Sampling Equipment. Same as Method 5, section 10.0.

10.2 Barium Standard Solution. Same as Method 6, section 10.5.

11.0 Analytical Procedure

11.1. Sample Loss. Same as Method 6, section 11.1.

11.2. Sample Analysis.

11.2.1 Container No. 1. Shake the container holding the isopropanol solution and the filter. If the filter breaks up, allow the fragments to settle for a few minutes before removing a sample aliquot. Pipette a 100-ml aliquot of this solution into a 250-ml Erlenmeyer flask, add 2 to 4 drops of thorin indicator, and titrate to a pink endpoint using 0.0100 N barium standard solution.

Repeat the titration with a second aliquot of sample, and average the titration values. Replicate titrations must agree within 1 percent or 0.2 ml, whichever is greater.

11.2.2 Container No. 2. Thoroughly mix the solution in the container holding the contents of the second and third impingers. Pipette a 10-ml aliquot of sample into a 250-ml Erlenmeyer flask.

Add 40 ml of isopropanol, 2 to 4 drops of thorin indicator, and titrate to a pink endpoint using

0.0100 N barium standard solution. Repeat the titration with a second aliquot of sample, and average the titration values. Replicate titrations must agree within 1 percent or 0.2 ml, whichever is greater.

11.2.3 Blanks. Prepare blanks by adding 2 to 4 drops of thorin indicator to 100 ml of 80 percent isopropanol. Titrate the blanks in the same manner as the samples.

12.0 Data Analysis and Calculations Carry out calculations retaining at least one extra significant figure beyond that of the acquired data. Round off figures after final calculation.



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