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
The fact that tin forms two well-defined series of compounds is taken
advantage of in assaying (just as in the case of iron), by determining
how much of an oxidising agent is required to convert it from the
stannous into the stannic state. For example, on the addition of a
solution of permanganate of potash to a solution of stannous chloride
the oxidation goes on rapidly, and the finishing point is sharp and
distinct; but acid solutions of stannous chloride quickly take up oxygen
from that dissolved in the water used and from the air. Unfortunately,
there is no obvious sign that such oxidation has taken place, except
that (fatal to the assay) a smaller volume of the permanganate is
required. Great care is required with such solutions, both before and
during titration. The addition of an excess of ferric chloride to the
stannous solution, as soon as the whole of the tin has been dissolved,
will lessen this liability to oxidation.
~Separation.~--If the tin is present in an alloy, the substance is
boiled in an evaporating dish with dilute nitric acid until the whole of
the material is attacked. Evaporate nearly to dryness, dilute, boil for
a few minutes, and filter off the white insoluble residue. Under certain
circumstances this residue will be nearly free from other metals, in
which case it is ignited and weighed. If not known to be pure it must be
ignited, reduced in a current of hydrogen, and treated as subsequently
described.
When the tin is present as insoluble oxide in an ore, the substance is
finely powdered, and from 1 to 5 grams of it (according to its richness)
boiled with 30 c.c. of hydrochloric acid in an evaporating dish till the
oxide of iron is seen to be dissolved. Then add 1 c.c. of nitric acid
(or more if much pyrites, &c., is present) and continue the boiling till
these are decomposed; dilute and filter off, washing first with dilute
acid and afterwards with a little dilute ammonia, dry, ignite, and place
in a combustion tube (together with the filter-ash) and heat to redness
for about thirty minutes in a current of dried hydrogen.
[Illustration: FIG. 58.]
The oxide of tin is placed in a porcelain boat (fig. 58), which is then
introduced into a piece of combustion tube. The latter, wrapped in a
piece of wire gauze, is supported on a couple of iron rings, and heated
by one or two Bunsen burners in a furnace fitted up with loose
fire-brick tiles, as shown in fig. 59.
[Illustration: FIG. 59.]
When the reduction is complete the tube is allowed to cool; the boat is
removed and the tin dissolved. Add a rod of zinc to the freely-acid hot
solution, and in a few minutes decant through a filter and wash with
water, after having removed the zinc. Wash the precipitated metal back
into the beaker, and dissolve in 10 c.c. of dilute nitric acid,
evaporate off the excess of acid; dilute, boil, and filter. Wash, dry,
ignite strongly in a porcelain crucible, and weigh.
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