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
~Separation.~--In the usual course of an analytical separation the
hydrate of titanium will be thrown down with ferric hydrate, &c., on the
addition of ammonic chloride and ammonia. It is best separated from this
precipitate by fusion with bisulphate of potash, as already described,
but it must be remembered that the presence of much mineral acid
prevents complete precipitation when the solution is boiled. Further, if
phosphates are present, the precipitate will contain phosphoric oxide;
it may be freed from this by fusion with sodium carbonate. A very good
method of separating titanium from iron is to add tartaric acid and
ammonia to the solution, and then precipitate the iron (as sulphide)
with sulphuretted hydrogen. The filtrate contains the titanium, which is
recovered by evaporating and igniting. It may be separated from zirconia
by the action of sodium carbonate, which precipitates both; but when
concentrated, redissolves the zirconia. The separation from large
quantities of silica is best effected by evaporating with hydrofluoric
acid, which volatilises the silicon; but sulphuric acid must be present,
otherwise some titanium also will be lost, as may be seen from the
following experiments,[77] in which oxide of titanium (pure, ignited)
was evaporated to dryness with a quantity of hydrofluoric acid known by
experiment to be sufficient to volatilise 1 gram of silica.
_Without sulphuric acid_, 0.0466 gram of titanic oxide left 0.0340 gram,
showing a loss of about 25 per cent.
_With sulphuric acid_ the following results were obtained:--
Oxide taken. Left after Evaporation
and Ignition.
0.0340 gram 0.0340 gram
0.0414 " 0.0413 "
0.0520 " 0.0520 "
0.0352 " 0.0352 "
GRAVIMETRIC DETERMINATION.
The titanic hydrate thrown down by ammonia (or on boiling the solution
from the bisulphate) is collected, washed, dried, ignited strongly with
the addition of a little ammonic carbonate, and weighed. The substance
is titanic oxide (TiO_{2}), and is generally reported as such. It
contains 60.98 per cent. of titanium. It should be white, if pure
(Holland), white, yellow, or brown (Fresenius), or black (Tidy).
VOLUMETRIC METHOD.
A method has been proposed based on the reduction of titanic oxide by
zinc in hydrochloric acid solutions to the sesquioxide. The reduction is
marked by the development of a violet or green colour, the former with
chlorides and the latter when fluorides are present. The quantity of
titanium reduced is measured by titrating with permanganate of potassium
solution. The water used must be free from dissolved oxygen.
TUNGSTEN AND TUNGSTATES.
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