§ 63.457 Test methods and procedures.

(a) Performance tests. Initial and repeat performance tests are required for the emissions sources specified in paragraphs (a)(1) and (2) of this section, except for emission sources controlled by a combustion device that is designed and operated as specified in § 63.443(d)(3) or (4).

(1) Conduct an initial performance test for all emission sources subject to the limitations in §§ 63.443, 63.444, 63.445, 63.446, and 63.447.

(2) Conduct repeat performance tests at five-year intervals for all emission sources subject to the limitations in §§ 63.443, 63.444, and 63.445. The first of the 5-year repeat tests must be conducted by September 7, 2015, and thereafter within 60 months from the date of the previous performance test. Five-year repeat testing is not required for the following:

(i) Knotter or screen systems with HAP emission rates below the criteria specified in § 63.443(a)(1)(ii).

(ii) Decker systems using fresh water or paper machine white water, or decker systems using process water with a total HAP concentration less than 400 parts per million by weight as specified in § 63.443(a)(1)(iv).

(b) Vent sampling port locations and gas stream properties. For purposes of selecting vent sampling port locations and determining vent gas stream properties, required in §§ 63.443, 63.444, 63.445, and 63.447, each owner or operator shall comply with the applicable procedures in paragraphs (b)(1) through (b)(6) of this section.

(1) Method 1 or 1A of part 60, appendix A-1, as appropriate, shall be used for selection of the sampling site as follows:

(i) To sample for vent gas concentrations and volumetric flow rates, the sampling site shall be located prior to dilution of the vent gas stream and prior to release to the atmosphere;

(ii) For determining compliance with percent reduction requirements, sampling sites shall be located prior to the inlet of the control device and at the outlet of the control device; measurements shall be performed simultaneously at the two sampling sites; and

(iii) For determining compliance with concentration limits or mass emission rate limits, the sampling site shall be located at the outlet of the control device.

(2) No traverse site selection method is needed for vents smaller than 0.10 meter (4.0 inches) in diameter.

(3) The vent gas volumetric flow rate shall be determined using Method 2, 2A, 2C, or 2D of part 60, appendix A-1, as appropriate.

(4) The moisture content of the vent gas shall be measured using Method 4 of part 60, appendix A-3.

(5) To determine vent gas concentrations, the owner or operator shall conduct a minimum of three test runs that are representative of normal conditions and average the resulting pollutant concentrations using the following procedures.

(i) Method 308 in Appendix A of this part; Method 320 in Appendix A of this part; Method 18 in appendix A-6 of part 60; ASTM D6420-99 (Reapproved 2004) (incorporated by reference in § 63.14(b)(28) of subpart A of this part); or ASTM D6348-03 (incorporated by reference in § 63.14(b)(54) of subpart A of this part) shall be used to determine the methanol concentration. If ASTM D6348-03 is used, the conditions specified in paragraphs (b)(5)(i)(A) though (b)(5)(i)(B) must be met.

(A) The test plan preparation and implementation in the Annexes to ASTM D6348-03, sections A1 through A8 are required.

(B) In ASTM D6348-03 Annex A5 (Analyte Spiking Technique), the percent (%) R must be determined for each target analyte (Equation A5.5 of ASTM D6348-03). In order for the test data to be acceptable for a compound, %R must be between 70 and 130 percent. If the %R value does not meet this criterion for a target compound, the test data is not acceptable for that compound and the test must be repeated for that analyte following adjustment of the sampling or analytical procedure before the retest. The %R value for each compound must be reported in the test report, and all field measurements must be corrected with the calculated %R value for that compound using the following equation: Reported Result = Measured Concentration in the Stack × 100)/%R.

(ii) Except for the modifications specified in paragraphs (b)(5)(ii)(A) through (b)(5)(ii)(K) of this section, Method 26A of part 60, appendix A-8 shall be used to determine chlorine concentration in the vent stream.

(A) Probe/sampling line. A separate probe is not required. The sampling line shall be an appropriate length of 0.64 cm (0.25 in) OD Teflon ® tubing. The sample inlet end of the sampling line shall be inserted into the stack in such a way as to not entrain liquid condensation from the vent gases. The other end shall be connected to the impingers. The length of the tubing may vary from one sampling site to another, but shall be as short as possible in each situation. If sampling is conducted in sunlight, opaque tubing shall be used. Alternatively, if transparent tubing is used, it shall be covered with opaque tape.

(B) Impinger train. Three 30 milliliter (ml) capacity midget impingers shall be connected in series to the sampling line. The impingers shall have regular tapered stems. Silica gel shall be placed in the third impinger as a desiccant. All impinger train connectors shall be glass and/or Teflon ®.

(C) Critical orifice. The critical orifice shall have a flow rate of 200 to 250 ml/min and shall be followed by a vacuum pump capable of providing a vacuum of 640 millimeters of mercury (mm Hg). A 45 millimeter diameter in-line Teflon 0.8 micrometer filter shall follow the impingers to protect the critical orifice and vacuum pump.

(D) The following are necessary for the analysis apparatus:

(1) Wash bottle filled with deionized water;

(2) 25 or 50 ml graduated burette and stand;

(3) Magnetic stirring apparatus and stir bar;

(4) Calibrated pH Meter;

(5) 150-250 ml beaker or flask; and

(6) A 5 ml pipette.

(E) The procedures listed in paragraphs (b)(5)(ii)(E)(1) through (b)(5)(ii)(E)(7) of this section shall be used to prepare the reagents.

(1) To prepare the 1 molarity (M) potassium dihydrogen phosphate solution, dissolve 13.61 grams (g) of potassium dihydrogen phosphate in water and dilute to 100 ml.

(2) To prepare the 1 M sodium hydroxide solution (NaOH), dissolve 4.0 g of sodium hydroxide in water and dilute to 100 ml.

(3) To prepare the buffered 2 percent potassium iodide solution, dissolve 20 g of potassium iodide in 900 ml water. Add 50 ml of the 1 M potassium dihydrogen phosphate solution and 30 ml of the 1 M sodium hydroxide solution. While stirring solution, measure the pH of solution electrometrically and add the 1 M sodium hydroxide solution to bring pH to between 6.95 and 7.05.

(4) To prepare the 0.1 normality (N) sodium thiosulfate solution, dissolve 25 g of sodium thiosulfate, pentahydrate, in 800 ml of freshly boiled and cooled distilled water in a 1-liter volumetric flask. Dilute to volume. To prepare the 0.01 N sodium thiosulfate solution, add 10.0 ml standardized 0.1 N sodium thiosulfate solution to a 100 ml volumetric flask, and dilute to volume with water.

(5) To standardize the 0.1 N sodium thiosulfate solution, dissolve 3.249 g of anhydrous potassium bi-iodate, primary standard quality, or 3.567 g potassium iodate dried at 103 =/−2 degrees Centigrade for 1 hour, in distilled water and dilute to 1000 ml to yield a 0.1000 N solution. Store in a glass-stoppered bottle. To 80 ml distilled water, add, with constant stirring, 1 ml concentrated sulfuric acid, 10.00 ml 0.1000 N anhydrous potassium bi-iodate, and 1 g potassium iodide. Titrate immediately with 0.1 n sodium thiosulfate titrant until the yellow color of the liberated iodine is almost discharged. Add 1 ml starch indicator solution and continue titrating until the blue color disappears. The normality of the sodium thiosulfate solution is inversely proportional to the ml of sodium thiosulfate solution consumed: