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 mineral is best treated by the method given in the third paragraph
on page 382; but the solution, after being acidified with nitric acid,
should be made exactly neutral with ammonia. A small excess of silver
nitrate should then be added, and since acid is liberated in the
reaction, the liquor must again be neutralised.[19] The precipitate must
then be filtered off, and washed with distilled water. Then dissolve it
in the paper by slowly running over it 20 c.c. of dilute nitric acid.
Wash the filter with distilled water, collecting with the filtrate in a
small flask. Add 2 c.c. of "ferric indicator" and titrate.
If the sulphocyanate solution be made up with 11 or 12 grams of the
potassium salt to the litre, and be then standardised and diluted, so
that for 100 c.c. it shall equal 1.08 gram of silver, (see p. 38), then
it will also equal .25 gram of arsenic (As). Except for ores rich in
arsenic, it will be better to work with a solution one half this
strength. The standard as calculated from an experiment with pure silver
should be checked by another using pure resublimed white arsenic,
As_{2}O_{3}, which contains 75.75 % of the metal. The quantity of white
arsenic taken, .1 or .2 gram, should contain about as much arsenic as
will be present in the assays. It is converted into sodium arsenate by
evaporating to a small bulk with nitric acid and neutralising with soda.
The precipitation and titration of the silver arsenate should be exactly
as in the assays.
The difficulty of the method is in the neutralising; which has to be
very carefully done since silver arsenate is soluble in even faintly
acid solutions; one drop of nitric acid in 100 c.c. of water is enough
to produce an absolutely worthless result; and an excess of acid much
less than this is still very prejudicial. The addition of a little
sodium acetate to the solution after the final neutralising has a good
effect.
~Arsenic in Mispickel.~--Weigh up .250 gram of the finely-powdered ore,
and place in a Berlin crucible about 1-1/4 or 1-1/2 inch in diameter.
Treat with 10 or 12 drops, one drop at a time, of strong nitric acid,
warm very gently, but avoid much heating. Put on a thin layer of nitre,
and rather more than half fill the crucible with a mixture of equal
parts of soda and nitre. Heat quickly in the blow-pipe flame, and when
the mass is fused and effervescing, withdraw and allow to cool. Boil out
with water, filter and wash. Insert a piece of litmus paper and
cautiously neutralise with nitric acid, using ammonia to neutralise any
accidental excess of the acid. Add a gram or so of ammonium nitrate and
silver nitrate in excess, neutralise again with ammonia and add two or
three grams of sodium acetate. Filter off the precipitate, wash and
titrate. In the fusion care should be taken to avoid much effervescence
(an excess of the soda mitigates this) and the operation should be
stopped as soon as the whole has entered into fusion.
COLORIMETRIC DETERMINATION.
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