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
~Tin.~--The acid filtrate from the silica and tungstic acid is treated
with sulphuretted hydrogen. The sulphide of tin is filtered off. Since
the percentage of tin has been already determined, this precipitate may
be neglected; or may be treated in the same way as the previous one, so
as to check the result. Since some stannic chloride will have been lost
in the evaporation, a low result may be expected. The tin should be
reported as stannous oxide; and is calculated by multiplying the
percentage of tin by 1.136.
The filtrate from the tin is boiled rapidly down to remove sulphuretted
hydrogen; and then peroxidised with 1 or 2 c.c. of nitric acid. It is
cooled, transferred to a graduated flask, and diluted with water to 200
c.c.
~Ferrous Oxide and Alumina.~--Half the filtrate from the tin (that is,
100 c.c.) is taken, nearly neutralised with soda, and treated with
sodium acetate. The basic acetate precipitate obtained on boiling is
filtered off and washed. Reserve the filtrate. The precipitate is
dissolved off the filter with hot dilute hydrochloric acid; and the
solution thus formed is treated with a slight excess of ammonia, and
boiled. The precipitate is filtered off, washed with hot water, dried,
ignited, and weighed as mixed ferric oxide and alumina. The ignited
precipitate is then dissolved with sulphuric and hydrochloric acids; and
the iron determined in the solution by titration with the solution of
stannous chloride. The iron found is calculated to and reported as
ferrous oxide, FeO (factor = 1.286). To find the alumina, which is best
estimated by difference, multiply the iron by 1.428 to get the weight of
ferric oxide, and deduct this from the weight of alumina and ferric
oxide found. This, of course, gives the alumina. A direct determination
may be made by removing the tin from the titrated solution with
sulphuretted hydrogen, filtering, nearly neutralising with ammonia, and
boiling with a few grams of hyposulphite of soda. The precipitate,
filtered, washed, and ignited, is the alumina, which is weighed. The
direct determination gives a slightly low result.
~Oxides of Zinc and Manganese.~--These are determined in the filtrate
from the basic acetate precipitate by rendering alkaline with ammonia,
and passing a current of sulphuretted hydrogen. Generally a small, but
decided, precipitate of alumina comes down, together with sulphides of
any zinc or manganese which is present. The precipitate is allowed to
settle, dried, ignited, and weighed. The metals are separately
determined in it; and the residue is counted as alumina, and added to
that already found. The mixed precipitate amounts to from 1 to 2 per
cent. of the sample.
~Lime.~--The filtrate from the last is treated with ammonic oxalate,
boiled for a few minutes, allowed to settle, and filtered. The
precipitate is washed with hot water; dried; ignited; and weighed as
carbonate, after gentle ignition; or as lime, after strong ignition in
the muffle.
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