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 and Separation.~--The decomposition and solution of natural
tungstates is difficult to effect owing to the separation of tungstic
acid; the method of treatment is as follows:--Boil the finely-powdered
substance with hydrochloric acid or aqua regia till it apparently ceases
to be attacked; dilute, filter, and wash with dilute hydrochloric acid.
Cover with dilute ammonia, and filter the solution, which contains
ammonic tungstate, into an evaporating dish. Treat the residue again
with acid, and again dissolve out the separated tungstic acid with
ammonia, and repeat this operation until decomposition is complete. By
this means there will be obtained--(1) a solution containing tungstate
of ammonia; (2) an insoluble residue with silicates, and oxides of tin,
niobium, tantalum, &c.; and (3) an acid solution containing the soluble
bases. The tungstate of ammonia requires simple evaporation on the
water-bath and gentle ignition in order to cause the tungstic acid to be
left in an almost pure state; possibly, it may carry a little silica.
GRAVIMETRIC DETERMINATION.
The tungstic acid is dissolved, and separated as ammonic tungstate, and,
after evaporation, is gently ignited, the heat being increased towards
the end. The residual tungstic acid is fixed, so that when the ammonia
has been driven off it may be strongly heated without loss. It is a dark
yellow or brown powder whilst hot, which becomes a light yellow on
cooling. If any reduction has taken place it will be more or less
greenish. It is weighed when cold, and is the trioxide or "tungstic
acid" (WO_{3}), which contains 79.31 per cent. of tungsten. After its
weight has been taken its purity is checked by fusing with hydric
potassic sulphate, extracting with water, and treating the residue with
ammonic carbonate. Any silica present will be left undissolved; it
should be separated and weighed, and its weight deducted from that of
the tungstic acid found.
~Determination of Tungstic Acid in Wolfram.~--Take 2 grams of the
finely-powdered sample and boil with 50 c.c. of hydrochloric acid for
half an hour, adding 5 c.c. of nitric acid towards the end. Allow to
stand overnight and boil again for 15 or 20 minutes; dilute with an
equal volume of water, and filter. Wash with dilute hydrochloric acid,
dissolve in a few c.c. of warm dilute ammonia, and dilute to 200 c.c.
with distilled water; allow to settle, and filter. Evaporate in a
weighed dish, ignite, and weigh.
The following analysis will illustrate the composition of a sample of
Cornish wolfram as brought into the market:--
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