Dissolve the fused mass, after cooling, in a little water and
filter. Add to the filtrate, ammonium chlorid in excess, from three to
five grams for each 100 cubic centimeters of the solution, and allow
to stand, with occasional stirring, for some time. Ammonium vanadate,
insoluble in a saturated solution of ammonium chlorid, separates as
a white powder. It is necessary to keep the solution alkaline, and a
drop of ammonia should be added from time to time for this purpose. The
appearance of a yellowish tint at any time indicates that the solution
has become acid, and this acidity must be corrected, or else the
results will be too low. Separate the ammonium vanadate by filtration;
wash first with a saturated solution of ammonium chlorid containing a
little free ammonia, and then with alcohol. Dry, ignite, and moisten
with a few drops of nitric acid; again ignite to obtain the compound as
vanadium pentoxid. This compound contains 56.22 per cent of vanadium.
The method of Rosenheim and Holversheet may also be used.[105] It is
based on the preliminary precipitation of the vanadic acid as a barium
or lead salt. The substance supposed to contain vanadium is first
brought into solution in such a manner as to secure it as vanadic acid,
which is then precipitated with barium chlorid or lead acetate. The
precipitate is boiled with hydrochloric acid and potassium bromid, and
the liberated bromin determined by the quantity of iodin set free from
potassium iodid. In the absence of bodies, such as molybdic acid, which
are reduced by sulfurous acid or hydrogen sulfid, the vanadic acid
may also be determined by reducing it with one of these reagents and,
after removing the excess by boiling, titrating the vanadium tetroxid
with potassium permanganate. When vanadic and phosphoric acids occur
together the former may be first reduced to tetroxid with sulfurous
acid, and after expelling excess of this reagent, the phosphoric acid
may be separated with molybdate solution and removed by filtration.
When the amount of vanadic acid is large the phosphoric acid should
be separated rapidly at 55°-60°, using a considerable excess of the
molybdate; or the vanadic acid may first be determined in the solution
volumetrically by the bromin process above described, and afterwards
the phosphoric acid obtained by evaporating to dryness with a little
sulfuric acid, taking the residue up with water, reducing the vanadic
with sulfurous acid and precipitating the phosphoric acid with
molybdate solution as described above.
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