Wis. Admin. Code Department of Natural Resources § NR 263.03 - Monitoring and reporting requirements

The following special monitoring and reporting requirements apply to all facilities regulated by this chapter:

(1) CYANIDE. Periodic analyses for cyanide are not required when both of the following conditions are met:

(a) The first wastewater sample of each calendar year has been analyzed and found to contain less than 0.07 mg/l cyanide, and

(b) The owner or operator of the coil coating facility certifies in writing that cyanide is not used in the coil coating process.

1. If the facility is a direct discharger, certification shall be made to the department.

2. If the facility discharges to a POTW, certification shall be made to the control authority.

(2) MONTHLY DISCHARGE LIMIT. The monthly average regulatory values, listed in the tables within this chapter, shall be the basis for the monthly average discharge limits in direct discharge permits and for pretreatment standards. Compliance with the monthly discharge limits is required regardless of the number of samples analyzed and averaged.

(3) CANMAKING WITH ALUMINUM ALLOY CONTAINING LESS THAN 1.0% MANGANESE. The owner or operator of any canmaking facility subject to the provisions of the canmaking subcategory shall advise the department or control authority and the EPA Office of Water Regulations and Standards, Washington, D.C. 20460, whenever it has been decided that the plant will manufacture cans from an aluminum alloy containing less than 1.0% manganese. Notification shall be made in writing not less than 30 days in advance of the scheduled production and shall provide the chemical analysis of the alloy and the expected period of use.

(4) OIL AND GREASE ANALYSIS. Follow the approved methods listed in ch. NR 219.

Note: Pursuant to s. 299.11(4) (c), Stats., sub. (4) is shown as repealed and recreated eff. 6-29-21 by CR 17-046. Prior to 6-29-21 it reads:

(4) OIL AND GREASE ANALYSIS. The following analytical method, based on Methods 503A and 503E, Standard Methods, 15th Edition, shall be used to determine the oil and grease concentration in wastewater samples from all subcategories in this chapter. The following hydrocarbon oil and grease method screens out fatty material and the more polar hydrocarbon interferences peculiar to wastewaters in this category. The method measures total oil and grease based on the concentration of hydrocarbons of petroleum origin.

(a) Outline of method. This method uses a partition-gravimetric procedure to determine petroleum-based hydrocarbon oil and grease (O & G-E). Samples of the regulated wastewater discharge, preserved according to ch. NR 219, are mixed with trichlorotrifluoroethane, a solvent which extracts dissolved or emulsified oil and grease. Silica gel absorbs the fatty acids and polar hydrocarbons from the extract, distillation removes the solvent, and the resulting hydrocarbon residue is weighed to determine the petroleum-based hydrocarbon oil and grease concentration of the sample.

(b) Apparatus. The following apparatus is required for the oil and grease analysis:

1. Separatory funnel, 1 liter, with TFE (Teflon or equivalent) stopcock.

2. Glass stoppered flask, 125 ml.

3. Distilling flask, 125 ml.

4. Water bath.

5. Filter paper, 11 cm. diameter, Whatman No. 40 or equivalent.

6. Glass funnel.

7. Magnetic stirrer and Teflon coated stir bar.

(c) Reagents. The oil and grease analysis requires the following reagents:

1. Hydrochloric acid, HCl, 1+1.

2. Trichlorotrifluoroethane. (1,1,2-trichloro-1,2,2-trifluoroethane), Freon or equivalent, boiling point 47"'C. The solvent should leave no measurable residue on evaporation; distill if necessary. Do not use plastic tubing to transfer solvent between containers.

3. Sodium sulfate, Na2SO4, anhydrous crystal.

4. Silica gel, 60 to 200 mesh, Davidson Grade 950 or equivalent. Dry at 110'C for 24 hours and store in a tightly sealed container.

(d) Procedure. To determine petroleum-based hydrocarbon oil and grease, collect about one liter of sample and mark sample level on bottle for later determination of sample volume. Acidify to pH 2 or lower; generally, adding 5 ml HCl is sufficient. Transfer to a separatory funnel. Carefully rinse sample bottle with 30 ml trichlorotrifluoroethane and add solvent washings to separatory funnel. Shake vigorously for 2 minutes; however, if formation of a stable emulsion is suspected, shake gently for 5 to 10 minutes. Let layers separate. Drain solvent layer through funnel containing solvent-moistened filter paper into a clean glass stoppered flask. If a clear solvent layer cannot be obtained, add 1.0 g Na₂SO₄ to the filter paper cone and slowly drain emulsified solvent onto the crystals; add more Na2SO4 if necessary. Extract sample in separatory funnel twice more with 30 ml solvent each, but first rinse sample container with each solvent portion. Combine filtered extracts in the glass stoppered flask and wash filter paper with an additional 10 to 20 ml solvent. Add 3.0 g silica gel to solvent extract, add stir bar, stopper flask, and stir on a magnetic stirrer for 5 minutes. Filter solution through clean filter paper into tared distilling flask. Wash silica gel and filter paper with 10 ml solvent and combine with filtrate in distilling flask. Distill solvent from distilling flask in a water bath at 70° C. Place flask on a water bath at 70"'C for 15 minutes and draw air through it with an applied vacuum for the final one minute. Cool flask in desiccator for 30 minutes and weigh.

(e) Calculation of O & G-E. If the organic solvent is free of residue, the total gain in weight, E, of the tared distilling flask is due to the amount (mg) of petroleum-based hydrocarbon oil and grease (O & G-E) in the sample:

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(f) Use of O & G-E. The O & G-E value shall be used as the measure of compliance with the oil and grease limitations and standards set forth in this chapter.

Notes

Wis. Admin. Code Department of Natural Resources § NR 263.03

Cr. Register, April, 1989, No. 400, eff. 5-1-89. Amended by, CR 17-046: r. and recr. (4) Register February 2021 No. 782, eff. 6/29/2021