process described.
If, however, the solutions of such ores are treated with sulphureted
hydrogen or sulphurous acid, instead of zinc or stannous chloride to
reduce the iron, and the excess reducing agent removed by boiling, an
accurate determination of the iron can be made.

PROCEDURE.--Grind the mineral to a fine powder. Weigh out two portions
of about 0.5 gram each into small porcelain crucibles. Roast the ore
at dull redness for ten minutes (Note 1), allow the crucibles to cool,
and place them and their contents in casseroles containing 30 cc. of
dilute hydrochloric acid (sp. gr. 1.12).

Proceed with the solution of the ore, and the treatment of the
residue, if necessary, exactly as described for the bichromate process
on page 56. When solution is complete, add 6 cc. of concentrated
sulphuric acid to each casserole, and evaporate on the steam bath
until the solution is nearly colorless (Note 2). Cover the casseroles
and heat over the flame of the burner, holding the casserole in
the hand and rotating it slowly to hasten evaporation and prevent
spattering, until the heavy white fumes of sulphuric anhydride are
freely evolved (Note 3). Cool the casseroles, add 100 cc. of water
(measured), and boil gently until the ferric sulphate is dissolved;
pour the warm solution through the reductor which has been previously
washed; proceed as described under standardization, taking pains
to use the same volume and strength of acid and the same volume of
wash-water as there prescribed, and titrate with the permanganate
solution in the reductor flask, using the ferrous sulphate solution if
the end-point should be overstepped.

From the corrected volume of permanganate solution used, calculate the
percentage of iron (Fe) in the limonite.

[Note 1: The preliminary roasting is usually necessary because, even
though the sulphuric acid would subsequently char the carbonaceous
matter, certain nitrogenous bodies are not thereby rendered insoluble
in the acid, and would be oxidized by the permanganate.]

[Note 2: The temperature of the steam bath is not sufficient to
volatilize sulphuric acid. Solutions may, therefore, be left to
evaporate overnight without danger of evaporation to dryness.]

[Note 3: The hydrochloric acid, both free and combined, is displaced
by the less volatile sulphuric acid at its boiling point. Ferric
sulphate separates at this point, since there is no water to hold
it in solution and care is required to preve