re are to be made. In the absence of such a
solution the liability of passing the end-point is lessened by setting
aside a small fraction of the silver solution, to be added near the
close of the titration.]
DETERMINATION OF SILVER IN COIN
PROCEDURE.-- Weigh out two portions of the coin of about 0.5 gram
each. Dissolve them in 15 cc. of dilute nitric acid (sp. gr. 1.2) and
boil until all the nitrous compounds are expelled (Note 1). Cool the
solution, dilute to 50 cc., and add 5 cc. of the indicator solution,
and titrate with the thiocyanate to the appearance of the faint red
coloration (Note 2).
From the corrected volume of the thiocyanate solution required,
calculate the percentage of silver in the coin.
[Note 1: The reaction with silver may be carried out in nitric acid
solutions and in the presence of copper, if the latter does not exceed
70 per cent. Above that percentage it is necessary to add silver in
known quantity to the solution. The liquid must be cold at the time of
titration and entirely free from nitrous compounds, as these sometimes
cause a reddening of the indicator solution. All utensils, distilled
water, the nitric acid and the beakers must be free from chlorides,
as the presence of these will cause precipitation of silver chloride,
thereby introducing an error.]
[Note 2: The solution containing the silver precipitate, as well as
those from the standardization, should be placed in the receptacle for
"silver residues" as a matter of economy.]
PART III
GRAVIMETRIC ANALYSIS
GENERAL DIRECTIONS
Gravimetric analyses involve the following principal steps: first, the
weighing of the sample; second, the solution of the sample; third, the
separation of some substance from solution containing, or bearing a
definite relation to, the constituent to be measured, under conditions
which render this separation as complete as possible; and finally,
the segregation of that substance, commonly by filtration, and the
determination of its weight, or that of some stable product formed
from it on ignition. For example, the gravimetric determination of
aluminium is accomplished by solution of the sample, by precipitation
in the form of hydroxide, collection of the hydroxide upon a filter,
complete removal by washing of all foreign soluble matter, and the
burning of the filter and ignition of the precipitate to aluminium
oxide, in which condition it is weighed.
Among the operations which
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