A text-book of assaying : $b for the use of those connected with mines.Beringer, C. (Cornelius)
Science
A text-book of assaying : $b for the use of those connected with mines.
Beringer, C. (Cornelius)
Assaying
These, of course, preclude a method of the kind aimed at, and at the
same time emphasise the importance of uniformity of work in the ordinary
process. In the determination of chlorides in sea-water, Dittmar used a
combined method: precipitating the bulk of the silver as chloride, and
after filtering, determining the small excess of silver by
sulphocyanate. This modification answers admirably when applied to the
assay of bullion. In the ordinary Gay-Lussac method, the precipitation
of the bulk of the silver by the 100 c.c. of salt solution leaves
nothing to be desired, either as to ease in working or accuracy of
result; the silver precipitate settles quickly, and leaves a clear
liquor admirably fitted for the determination of the few milligrams of
silver remaining in solution. But the method of determining this
residual silver by adding successive small quantities of salt so long as
they continue to give a precipitate is unsatisfactory, and, judged on
its own merits apart from the rest of the process, could hardly escape
condemnation. It is clumsy in practice, for the continued adding of
small portions of salt solution is laborious and becomes impossible with
more than a few milligrams of silver in solution. The proposed
modification is simple; having precipitated the silver with the 100 c.c.
of salt solution, as described under Gay-Lussac's method (page 120),
shake till the liquor clears, and filter into a flask, washing with a
little distilled water. Add 2 c.c. of "ferric indicator" to the filtrate
and titrate with a standard "sulphocyanate solution" made by diluting
the ordinary standard solution to such an extent that 100 c.c. after
diluting shall be equivalent to 0.1 gram of silver.[18] Calculate the
weight of silver found by "sulphocyanate" and add it to the weight which
100 c.c. of the salt solution will precipitate.
An advantage of this modification is that an excess of 15 milligrams may
be determined as easily and exactly as 5. In standardising the salt
solution, then, weigh up, say 1.0150 gram of pure silver, dissolve and
titrate. Suppose 13.5 c.c. of "sulphocyanate" required; then these are
equivalent to .0135 gram of silver, (100 c.c. = .1); the silver
precipitated by the salt is 1.0150-.0135--_i.e._, 1.0015 gram, which is
the standard.
~Application of the Method to Assays for Arsenic.~--If silver nitrate be
added to a neutral solution of an arsenate of one of the alkali metals,
silver arsenate (Ag_{3}AsO_{4}), is thrown down as a dark-red
precipitate. If, after adding excess of silver nitrate to insure a
complete precipitation, the arsenate of silver be filtered off, the
weight of the arsenic could be estimated from the weight of silver
arsenate formed. But this may be done much more conveniently by
dissolving the precipitate in nitric acid, and titrating with
sulphocyanate; the silver found will be to the arsenic present as 324
(108×3) is to 75.
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