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
~Examination of Tin Slags.~--In tin smelting works the term "slag" is
applied to the unfused portion of the charge. It is made up of unburnt
anthracite and small lumps of slag proper together with some buttons of
metallic tin. This is rarely, if ever, assayed. The slag proper (or, as
it is generally called, "glass") is a silicate of iron, alumina, and
lime, containing from 3 to 7 per cent. of tin. It is thus examined:--The
sample after bruising on an iron plate, is reduced to a very fine powder
by grinding in an agate mortar. In this state it is in most cases
readily decomposed by hydrochloric acid.
~Determination of Tin.~--Where the percentage of tin only is required,
take 2 grams of the powdered slag and well mix with it 20 c.c. of
hydrochloric acid, and heat to boiling. Add 1 c.c. of nitric acid, allow
to stand for fifteen minutes, dilute with water, and filter. Pass a
rapid current of sulphuretted hydrogen for some time. Allow to settle,
and filter. The precipitate, after washing with hot water, is dried, and
gently calcined until the greater part of the sulphur is burnt off. It
is then strongly ignited in the muffle (or over the blowpipe) with the
addition of a small lump of ammonic carbonate. The residue is weighed as
stannic oxide (SnO_{2}); and is calculated to metallic tin by
multiplying by 0.787. The percentage on the slag is calculated in the
usual way.
The tin is always best determined in the examination of slags by a
separate assay carried out in this way. The determination of the other
constituents is thus made:--
~Silica.~--Take 2 grams of the powdered slag and cover them, in a small
evaporating dish, with 20 c.c. of hydrochloric acid; mix well by
stirring with a glass rod; and evaporate to dryness. If (as is generally
the case) tungsten is present the solution will be blue. Take up with 20
c.c. of hydrochloric acid. Add 1 c.c. of nitric acid; and reduce by
boiling to about half the bulk. Add about 20 c.c. of water, boil, and
filter. Wash the residue with hot dilute hydrochloric acid. It consists
of silica with the tungstic acid. Wash it back into the dish; and digest
with 5 or 10 c.c. of a cold solution of ammonic carbonate. Filter; and
collect the filtrate and washings in a weighed porcelain dish. Dry the
residue, ignite strongly, and weigh as silica, SiO_{2}. In certain
exceptional cases this may contain some unaltered cassiterite, which is
easily recognised by its appearance.
~Tungsten.~--The ammonic carbonate filtrate from the silica is
evaporated to dryness, ignited strongly over the blowpipe, and weighed.
The residue is tungstic acid, WO_{3}. The tungsten may be conveniently
reported in this form, although it is probably present as a lower
oxide.
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