NR 440.684(9)(c)1.1. Iodine stock solution, 0.1N. Weigh out 12.7 g of iodine and 20 to 25 g cp potassium iodide for each liter of solution. Dissolve the KI in as little water as necessary and then dissolve the iodine in the concentrated KI solution, make up to proper volume, and store in a glass-stoppered brown glass bottle. NR 440.684(9)(c)2.2. Standard iodine solution, 1 ml ± 0.001771 g I. Transfer 33.7 ml of the 0.1N stock solution into a 250 ml volumetric flask, add water to the mark and mix well. Then, for a 100 ml sample of gas, 1 ml of standard iodine solution is equivalent to 100 grains of H2S per cubic foot of gas. Starch solution. Rub into a thin paste about one teaspoonful of wheat starch with a little water, pour it into about a pint of boiling water and stir. After it has cooled, decant off the clear solution. Make fresh solution every few days.
NR 440.684(9)(d)(d) Procedure. Fill the leveling bulb with starch solution. Raise (L), open cock (G), open (F) to (A), and close (F) when the solution starts to run out of the gas inlet. Close (G). Purge the gas sampling line and connect it with (A). Lower (L) and open (F) and (G). When the liquid level is several ml past the 100 ml mark, close (G) and (F), and disconnect the sampling tube. Open (G) and bring the starch solution to the 100 ml mark by raising (L), then close (G). Open (F) momentarily, to bring the gas in the burette to atmospheric pressure, and close (F). Open (G) and bring the liquid level down to the 10 ml mark by lowering (L). Close (G), clamp the rubber tubing near (E) and disconnect it from the burette. Rinse the graduated cylinder with a standard iodine solution (0.00171 g I per ml), fill the cylinder and record the reading. Introduce successive small amounts of iodine thru (F), shaking well after each addition, and continue until a faint permanent blue color is obtained. Record the reading, subtract it from the previous reading and call the difference D. NR 440.684(9)(e)(e) Reagent test. With every fresh stock of starch solution, perform a blank test as follows: introduce fresh starch solution into the burette up to the 100 ml mark. Close (F) and (G). Lower (L) and open (G). When the liquid level reaches the 10 ml mark, close (G). With air in the burette titrate as during a test and up to the same end point. Call the ml of iodine used C. Then, NR 440.684(9)(f)(f) Sensitivity enhancement. Greater sensitivity can be attained if a 500 ml capacity Tutwiler burette is used with a more dilute (0.001N) iodine solution. Concentrations less than 1.0 grains per 100 cubic foot can be determined in this way. Usually the starch-iodine end point is much less distinct and a blank determination of end point, with H2S-free gas or air, is required.
Figure 1. Tutwiler burette (lettered items mentioned in text).
NR 440.684 HistoryHistory: Cr. Register, September, 1990, No. 417, eff. 10-1-90; am. (2) (a) 4., (4) (b), (7) (a) 2. and 4., (b) 3., (c), (d) (intro.), (e) and (8) (a), renum. (2) (b) 4. to 6. to be (2) (b) 5. to 7., cr. (2) (b) 4., r. and recr. (5), r. (6), Register, July, 1993, No. 451, eff. 8-1-93; am. (5) (c) 3., Register, December, 1995, No. 480, eff. 1-1-96; CR 06-109: am. (2) (a) 8. and (b) 1. to 3., (4) (b), (5) (b) 1. to 3., (c) 2. and 4. and (7) (b) 1. and (c), r. (2) (b) 4., renum. (2) (b) 5. to 7. to be (2) (b) 4. to 5. and am., r. and recr. (5) (c) 3. and (7) (e) Register May 2008 No. 629, eff. 6-1-08. NR 440.686NR 440.686 Volatile organic compound (VOC) emissions from synthetic organic chemical manufacturing industry (SOCMI) distillation operations. NR 440.686(1)(1) Applicability and designation of affected facility. NR 440.686(1)(a)(a) The provisions of this section apply to each affected facility designated in par. (b) that is part of a process unit that produces any of the chemicals listed in sub. (8) as a product, co-product, by-product or intermediate, except as provided in par. (c). NR 440.686(1)(b)(b) The affected facility is any of the following for which construction, modification or reconstruction commenced after December 30, 1983: NR 440.686(1)(b)1.1. Each distillation unit not discharging its vent stream into a recovery system. NR 440.686(1)(b)2.2. Each combination of a distillation unit and the common recovery system into which its vent stream is discharged. NR 440.686(1)(b)3.3. Each combination of 2 or more distillation units and the common recovery system into which their vent streams are discharged. NR 440.686(1)(c)1.1. Any distillation unit operating a part of a process unit which produces coal tar or beverage alcohols or which uses, contains and produces no VOC is not an affected facility. NR 440.686(1)(c)3.3. Any distillation unit that is designed and operates as a batch operation is not an affected facility. NR 440.686(1)(c)4.4. Each affected facility that has a total resource effectiveness (TRE) index value greater than 8.0 is exempt from all provisions of this section except for subs. (3), (5) (d), (e) and (f) and (6) (h) and (L). NR 440.686(1)(c)5.5. Each affected facility in a process unit with a total design capacity for all chemicals produced within that unit of less than one gigagram per year is exempt from all provisions of this section except for the recordkeeping and reporting requirements in sub. (6) (j), (L) 6. and (n). NR 440.686(1)(c)6.6. Each affected facility operated with a vent stream flow rate less than 0.008 scm/min is exempt from all provisions of this section except for the test method and procedure and the recordkeeping and reporting requirements in subs. (5) (g) and (6) (i), (L) 5. and (o). NR 440.686 NoteNote: The intent of these standards is to minimize the emissions of VOC through the application of best demonstrated technology (BDT). The numerical emission limits in these standards are expressed in terms of total organic compounds (TOC), measured as TOC less methane and ethane. This emission limit reflects the performance of BDT.
NR 440.686(1)(d)1.1. Owners or operators of process vents that are subject to this section may choose to comply with the provisions of 40 CFR part 65, subpart D, as in effect on December 14, 2000, to satisfy the requirements of subs. (3) to (6). The provisions of 40 CFR part 65, subpart D, as in effect on December 14, 2000, also satisfy the criteria of par. (c) 4. and 6. Other provisions applying to an owner or operator who chooses to comply with 40 CFR part 65, subpart D, as in effect on December 14, 2000, are provided in 40 CFR 65.1. NR 440.686(1)(d)2.2. Owners or operators who choose to comply with 40 CFR part 65, subpart D, as in effect on December 14, 2000, shall also comply with ss. NR 440.01, 440.02, 440.05, 440.06, 440.07 (1) (a) and (d), 440.14 and 440.15 for those process vents. All sections or subsections from ss. NR 440.01 to 440.19 not specified in this subdivision do not apply to owners or operators of process vents complying with 40 CFR part 65, subpart D, as in effect on December 14, 2000, except that provisions required to be met prior to implementing 40 CFR part 65 still apply. Owners or operators who choose to comply with 40 CFR part 65, subpart D, as in effect on December 14, 2000, shall comply with 40 CFR part 65, subpart A. NR 440.686(1)(d)3.3. Owners or operators who choose to comply with 40 CFR part 65, subpart D, as in effect on December 14, 2000, at initial startup shall comply with subds. 1. and 2. for each vent stream on and after the date on which the initial performance test is completed, but not later than 60 days after achieving the maximum production rate at which the affected facility will be operated, or 180 days after the initial startup, whichever date comes first.