The following special monitoring and reporting
requirements apply to all facilities regulated by this
Periodic analyses for cyanide are not required when both of the
following conditions are met:
The first wastewater sample of each calendar year has been analyzed
and found to contain less than 0.07 mg/l cyanide, and
The owner or operator of the
coil coating facility certifies in writing that cyanide is not used
in the coil coating process.
the facility is a direct discharger, certification shall be made to
2. If the
facility discharges to a POTW, certification shall be made to the
(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.
OIL AND GREASE ANALYSIS. Follow
the approved methods listed in ch. NR 219.
Note: Pursuant to s.
(c), Stats., sub. (4) is shown as
repealed and recreated eff. 6-29-21 by CR 17-046. Prior to 6-29-21 it
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.
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.
Apparatus. The following apparatus is required
for the oil and grease analysis:
Separatory funnel, 1
liter, with TFE (Teflon or equivalent) stopcock.
Glass stoppered flask, 125
Distilling flask, 125 ml.
Filter paper, 11 cm. diameter, Whatman No. 40 or
Magnetic stirrer and
Teflon coated stir bar.
Reagents. The oil and grease analysis requires
the following reagents:
Hydrochloric acid, HCl, 1+1.
(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.
Sodium sulfate, Na2SO4,
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.
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
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:
Click to view
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.
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.
February 2021 No. 782, eff.