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
Transfer to a small flask the sample from which the iodine has been
removed. Add saturated chlorine water, 1 cc. at a time, shaking after
each addition until all the bromine is freed. Care must be taken not to
add much more chlorine than that necessary to free the bromine, since an
excess of reagent may form a bromochloride that spoils the color
reaction. Separate the water solution from the carbon bisulfide by
filtration through a moistened filter, wash the contents of the filter
two or three times with water, and then transfer them to a Nessler tube
by means of about 1 cc. of carbon bisulfide. Repeat this extraction of
the filtrate twice, using 3 cc. of carbon bisulfide each time. The
combined carbon bisulfide extracts usually amount to 11.5 to 12 cc. Add
enough carbon bisulfide to the tubes to bring them to a definite volume,
usually 12 to 15 cc., and compare the sample with the standards. If much
bromine is present it is not always completely extracted by the amounts
of carbon bisulfide recommended. If the extraction is incomplete,
therefore, make one or two extra extractions with carbon bisulfide,
transfer the extracts to another tube, and compare the color with that
of the standards.
ARSENIC.[31]
Evaporate to dryness an aliquot portion of the alkaline filtrate (p.
61). Acidify the residue with arsenic-free sulfuric acid, and subject it
to the action of arsenic-free zinc and sulfuric acid in a
Marsh-Berzelius apparatus. Compare the mirror obtained with a mirror
obtained from an arsenious oxide solution of known strength.
BORIC ACID.
Evaporate to dryness an aliquot portion of the alkaline filtrate (p.
61), treat the residue with 1 or 2 cc. of water, and slightly acidify
the solution with hydrochloric acid. Add about 25 cc. of absolute
alcohol, boil, filter, and repeat the extraction of the residue. Make
the filtrate slightly alkaline with sodium hydroxide, and evaporate it
to dryness. Add a little water, slightly acidify with hydrochloric acid,
and place a strip of turmeric paper in the liquid. Evaporate to dryness
on the steam bath, and continue the heating until the turmeric paper is
dry. If boric acid is present the turmeric paper becomes cherry red. It
is not usually necessary to determine quantitatively boric acid; the
quantitative method devised by Gooch[33] is recommended.
HYDROGEN SULFIDE.[103]
Hydrogen sulfide should be determined preferably in the field; the
procedure as far as the final titration with sodium thiosulfate must be
carried out in the field.
_Reagents._—1. N/100 sodium thiosulfate.
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