Standard methods for the examination of water and sewageAmerican Public Health Association. Laboratory Section
Science
Standard methods for the examination of water and sewage
American Public Health Association. Laboratory Section
Sewage -- Analysis; Water -- Analysis
_Acid digestion._—Place in a flask 100 cc. of the water, or, if the
water is of high organic content, a smaller portion diluted to 100 cc.
Add 10 cc. of sulfuric acid solution and 10 cc. of standard potassium
permanganate and digest the liquid exactly 30 minutes in a bath of
boiling water the level of which is kept above the level of the contents
of the flask.[70][71a] If the quantity of permanganate is insufficient
for complete oxidation repeat the digestion with a larger quantity; at
least 5 cc. excess of the standard permanganate should be present when
the ammonium oxalate solution is added. Remove the flask, add 10 cc. of
the ammonium oxalate solution, and titrate with the standard
permanganate until a faint but distinct color is obtained. If 100 cc. of
water is used the number of cubic centimeters of potassium permanganate
solution in excess of the number of cubic centimeters of ammonium
oxalate solution is equal to parts per million of oxygen consumed.
If oxidizable mineral substances, such as ferrous iron, sulfide, or
nitrite, are present in the sample corrections should be applied as
accurately as possible by suitable procedures. Direct titration of the
acidified sample in the cold, using a three-minute period of digestion,
serves this purpose quite well for polluted surface waters and fairly
well for purified sewage effluents. Few raw sewages containing no trade
wastes need such a correction, but raw sewages containing “pickling”
liquors do need it. If the sample contains both oxidizable mineral
compounds and gaseous organic substances the latter should be driven off
by heat and the sample allowed to cool before applying this test for the
correction factor. If such corrections are made the fact should be
stated with the amount of correction.
_Period and temperature of digestion._—As the practice in regard to the
period and temperature of digestion has varied widely it is difficult to
compare the results obtained at one laboratory with those obtained at
another. None of the methods gives absolute results. They are all
relative[26][29][57] at best. Digesting 30 minutes at the boiling
temperature is herein designated the recommended method. If samples are
analyzed by any other method the method should be noted, and,
representative results by the standard method should be placed on record
for purposes of comparison.
OTHER METHODS.
_Additional reagents._—1. Potassium iodide solution. Ten per cent
solution, free from iodate.
2. Standard sodium thiosulfate. Dissolve 1.0 gram of the pure
crystallized salt in 1 liter of distilled water. Standardize this
solution against the standard potassium permanganate. As the thiosulfate
solution does not keep well determine its actual strength at frequent
intervals.
3. Starch indicator. Prepare as directed in the section on dissolved
oxygen (pp. 65–66).
4. Sodium hydroxide solution. Dissolve 1 part of pure sodium hydroxide
in 2 parts of distilled water.
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