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
The weight of sodium chloride is found by subtracting the combined
weights of lithium chloride and potassium chloride (corrected) from the
total weight of the three chlorides. Calculate sodium chloride to
sodium.
BROMINE, IODINE, ARSENIC, AND BORIC ACID.
Evaporate to dryness a large quantity of the sample to which a small
amount of sodium carbonate has been added. Boil the residue with
distilled water, transfer it to a filter, and thoroughly wash it with
hot water. Dilute the alkaline filtrate to a definite volume, and
determine bromine and iodine, arsenic, and boric acid in aliquot
portions of it.
BROMINE AND IODINE.[10]
_Reagents._—1. Sulfuric acid. 1 to 5.
2. Potassium nitrite or sodium nitrite. Two per cent solution.
3. Carbon bisulfide. Freshly purified by distillation.
4. Iodine standards. Acidify with dilute sulfuric acid measured
quantities of a standard solution of potassium iodide in small tubes.
Add 3 or 4 drops of the potassium nitrite solution and extract with
carbon bisulfide as in the actual determination. Transfer to small
flasks the standards from which the iodine has been removed.
5. Chlorine water. Saturated solution.
6. Bromine standards. Add measured quantities of a standard solution of
a bromide to the liquid in each of the small flasks from which the
iodine has been removed. Add to each 5 cc. of purified carbon bisulfide,
and proceed exactly as with the sample.
_Procedure._—Evaporate to dryness an aliquot portion of the alkaline
filtrate. Dissolve the residue in 2 or 3 cc. of water, and add enough
absolute alcohol to make the percentage of alcohol about 90. Boil and
filter and repeat the extraction of the residue with alcohol once or
twice. Add 2 or 3 drops of sodium hydroxide to the combined alcoholic
filtrates and evaporate to dryness. Dissolve the residue in 2 or 3 cc.
of water and repeat the extraction with alcohol and the filtration. Add
a drop of sodium hydroxide to the filtrate and evaporate it to dryness.
Dissolve the residue in a little water. Acidify this solution with
dilute sulfuric acid, adding 3 or 4 drops excess, and transfer it to a
small flask. Add 4 drops of the solution of potassium nitrite or sodium
nitrite and about 5 cc. of carbon bisulfide. Shake the mixture until all
the iodine is extracted. Separate the acid solution from the carbon
bisulfide by filtration. Wash the flask, filter, and contents with cold
distilled water, and transfer the carbon bisulfide containing the iodine
in solution to Nessler tubes by means of about 5 cc. of pure carbon
bisulfide. In washing the filter, dilute the contents of the tube to a
definite volume, usually 12 or 15 cc., and compare the color with that
of known amounts of iodine dissolved in carbon bisulfide in other tubes.
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