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
Heat to boiling the filtrate from the insoluble residue, oxidize with
concentrated nitric acid or bromine, and concentrate to about 25 cc. Add
ammonium hydroxide in slight excess, boil one minute, and filter.
Dissolve the precipitate on the filter in a small amount of hot dilute
hydrochloric acid. Reprecipitate with ammonium hydroxide, filter, and
wash. Unless very accurate results are necessary this solution and
reprecipitation may be omitted. Unite the two filtrates for
determination of calcium. Ignite and weigh the precipitate. It will
comprise oxides of iron and aluminium and phosphate. If much phosphate
is present it should be determined in a separate sample and a correction
for the amount applied; otherwise it may be neglected. Determine the
iron in the ignited precipitate by fusion with sodium or potassium
pyrosulfate, reduction with zinc, and titration with potassium
permanganate. Aluminium (Al) is calculated as follows:
Al = 0.53[(Fe_{2}O_{3} + Al_{2}O_{3}) − 1.43 Fe]
CALCIUM.
Concentrate the filtrate from the separation of iron and aluminium to
about 100 cc., and add an excess of concentrated solution of ammonium
oxalate, little by little, to the hot ammoniacal solution. Keep the
solution warm and stir at intervals till the precipitate settles readily
and leaves a clear supernatant liquid. Filter, dissolve the precipitate
in a little hot dilute hydrochloric acid, and reprecipitate with
ammonium hydroxide and ammonium oxalate. If great accuracy is not
required this solution and reprecipitation may be omitted, and the first
precipitate may be washed clean with hot water[64a]. Save the filtrate
for determination of magnesium. Ignite the precipitate and weigh it as
calcium oxide, 71.5 per cent of which is the equivalent of calcium (Ca);
or dissolve the precipitate in hot 2 per cent sulfuric acid and titrate
with a standard solution of potassium permanganate.
MAGNESIUM.
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