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
~Solution.~--Ores, &c., containing antimony are best opened up by
boiling with hydrochloric acid or aqua regia; treatment with nitric
acid should be avoided wherever possible, since it forms antimonic acid,
which is subsequently dissolved only with difficulty. Salts of antimony
in solution have a tendency to form insoluble basic salts; so that care
must be exercised in diluting. Compounds such as antimonite which are
soluble in hydrochloric should be dissolved at once in that acid.
~Separation.~--To the solution add potash in excess and a little free
sulphur, and pass a current of sulphuretted hydrogen for some minutes;
allow to digest for an hour or so on a hot plate; filter; and wash the
residue. Acidulate the filtrate with hydrochloric acid: the precipitate
will contain the antimony (as Sb_{2}S_{5}), and possibly arsenic or tin.
The precipitate is transferred to a beaker and boiled with hydrochloric
acid; the solution is filtered off and diluted. Add a few crystals of
tartaric acid, and pass a current of sulphuretted hydrogen for some
time. The first flocculent precipitate will become denser, and render
the filtering more easy. Transfer the precipitate (after washing free
from chlorides) to a Berlin dish, and treat cautiously with fuming
nitric acid. The action of this acid on the sulphide is very violent.
Evaporate and ignite, transfer to a silver dish, and fuse with four or
five times its weight of caustic soda, cool and extract with a little
water, then add an equal volume of alcohol, and allow to stand
overnight. Filter, wash with dilute alcohol. (The filtrate will contain
the tin.) The residue contains the antimony as antimonate of soda, and
is dissolved off the filter with hot dilute hydrochloric, with the help
of a little tartaric, acid. The filtrate is now ready for the
gravimetric determination.
GRAVIMETRIC ASSAY.
Pass a current of sulphuretted hydrogen through the solution containing
the antimony to which a little tartaric acid has been previously added.
Pass the gas till the precipitate becomes dense, and the antimony is all
down. The solution must not be too strongly acid. Filter off the
precipitate, wash with hot water, dry in the water oven, transfer to a
weighed porcelain dish, and cautiously treat with fuming nitric acid.
Continue the action on the water bath till the sulphur and antimony are
completely oxidised. Evaporate; ignite, gently at first, then strongly
over the blast; cool, and weigh. The residue is a white infusible
powder, and consists of antimony tetroxide, Sb_{2}O_{4}, containing
78.94 per cent. of the metal.
~Determination of Antimony as Bigallate.~--What appears to be a very
good method has been worked out by M.A. Guyard, and is described in
Crookes' _Select Methods_, p. 398.
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