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
_Procedure._—Use an amount of the sample that contains not more than 0.2
mg. of manganese. Add 0.5 cc. of sulfuric acid and evaporate to dryness.
Heat until the sulfuric acid is volatilized and ignite the residue.
Dissolve in 40 cc. of nitric acid, add about 0.5 gram of sodium
bismuthate, and heat until the permanganate color disappears. Add a few
drops of a solution of ammonium or sodium bisulfate to clear the
solution and again boil to expel oxides of nitrogen. Remove from the
source of heat, cool to 20° C., again add 0.5 gram of sodium bismuthate,
and stir. When the maximum permanganate color has developed, filter
through an alundum or Gooch crucible containing an asbestos mat ignited
and washed with potassium permanganate. Wash the precipitate with dilute
sulfuric acid until the washings are colorless. Transfer the filtrate to
a 50 cc. Nessler tube and compare the color of it with that of standards
prepared from the potassium permanganate solution. To prepare the
standards, dilute portions of 0.2, 0.4, 0.6 cc., etc. of the
permanganate solution to 50 cc. with dilute sulfuric acid. The content
of manganese is calculated as described under persulfate method (p. 49).
LEAD, ZINC, COPPER, AND TIN.[7][60]
Determinations of lead, zinc, copper, and tin are important in certain
mining regions and in places where the water has a solvent action on
pipes and other containers. The use of certain “germicides” also makes
it necessary to test for some of these metals.
Lead, zinc, and copper may be determined colorimetrically or
electrolytically. The colorimetric methods are not so accurate as a
combination of both, and are chiefly of value as qualitative tests.
It is possible to make a rough estimation of the amount of lead in clear
waters by acidifying with acetic acid, saturating with hydrogen sulfide,
and comparing the color produced with that produced by standard lead
solutions in Nessler tubes, treated in similar manner. This method,
however, is not applicable if the water is colored or contains iron.
_Reagents._—1. Standard lead solution. Dissolve 1.60 grams of lead
nitrate (Pb(NO_{3})_{2}) in 1 liter of distilled water. One cc. of this
solution contains 1 mg. of lead (Pb). As a check it is desirable to
determine lead as sulfate in a measured portion of this solution.
2. Standard copper solution. Dissolve about 0.8 gram of copper sulfate
crystals (CuSO_{4}.5H_{2}O) in water and, after the addition of 1 cc. of
concentrated sulfuric acid, dilute the solution to 1 liter. Determine
the copper in 100 cc. of this solution in the usual way by electrolytic
deposition. Dilute the solution so that 1 cc. contains 0.2 milligram
copper (Cu). This solution is permanent.
3. Ammonium chloride. Twenty-five per cent solution.
4. Ammonium acetate. Fifty per cent solution.
5. Ammonium hydroxide. (Sp. gr. 0.96.)
6. Hydrogen sulfide. Saturated solution.
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