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
Dissolve the precipitate of lead sulfate by boiling the filter
containing it in ammonium acetate solution in a porcelain dish. (4).
Filter into a 50 cc. Nessler tube and wash the filter with boiling water
containing a little ammonium acetate. Divide this filtrate in halves and
treat one-half with saturated hydrogen sulfide water in order to get an
approximation of the amount of lead present. To the other half, or an
aliquot portion, if a large amount of lead is present, add a few drops
of acetic acid, then an excess of saturated hydrogen sulfide solution,
and compare the color with that of standards made by treating known
amounts of the standard lead solution with a little acetic acid,
ammonium acetate, and hydrogen sulfide.
ZINC.
If zinc is present and copper is absent concentrate the filtrate from
the lead sulfate to expel the alcohol, and remove the iron by adding an
excess of ammonium hydroxide. Filter, wash, and acidify the filtrate
with sulfuric acid. Concentrate the filtrate to about 150 cc. and
transfer to a weighed platinum dish. Add 2 grams of potassium oxalate
and 1.5 grams of potassium sulfate. Deposit the zinc electrolytically by
means of a current of about 0.3 ampere for three hours. After deposition
is complete and while the current is on, siphon off the solution and at
the same time run into the dish a stream of distilled water in order to
expel the free sulfuric acid, which might dissolve some of the zinc if
the circuit were broken. After the acid has been removed break the
circuit, wash the dish with water, then with 95 per cent alcohol, dry at
70° C., cool, and weigh it. The difference between this weight (10) and
the weight of the platinum dish equals the amount of metallic zinc. Some
difficulty has been experienced in this determination in obtaining pure
reagents. It is therefore advisable to make blank determinations with
each new lot of reagents and to correct the results if necessary.
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