nt bumping. The ferric
sulphate usually has a silky appearance and is easily distinguished
from the flocculent silica which often remains undissolved.]
!Zimmermann-Reinhardt Procedure!
!Method (B)!
PROCEDURE.--Grind the mineral to a fine powder. Weigh out two portions
of about 0.5 gram each into small porcelain crucibles. Proceed with
the solution of the ore, treat the residue, if necessary, and reduce
the iron by the addition of stannous chloride, followed by mercuric
chloride, as described for the bichromate process on page 56. Dilute
the solution to about 400 cc. with cold water, add 10 cc. of the
manganous sulphate titrating solution (Note 1, page 68) and titrate
with the standard potassium permanganate solution to a faint pink
(Note 1).
From the standardization data already obtained calculate the
percentage of iron (Fe) in the limonite.
[Note 1: It has already been noted that hydrochloric acid reacts
slowly in cold solutions with potassium permanganate. It is, however,
possible to obtain a satisfactory, although somewhat fugitive
end-point in the presence of manganous sulphate and phosphoric acid.
The explanation of the part played by these reagents is somewhat
obscure as yet. It is possible that an intermediate manganic compound
is formed which reacts rapidly with the ferrous compounds--thus in
effect catalyzing the oxidizing process.
While an excess of hydrochloric acid is necessary for the successful
reduction of the iron by stannous chloride, too large an amount
should be avoided in order to lessen the chance of reduction of the
permanganate by the acid during titration.]
DETERMINATION OF THE OXIDIZING POWER OF PYROLUSITE
INDIRECT OXIDATION
Pyrolusite, when pure, consists of manganese dioxide. Its value as an
oxidizing agent, and for the production of chlorine, depends upon the
percentage of MnO_{2} in the sample. This percentage is determined
by an indirect method, in which the manganese dioxide is reduced and
dissolved by an excess of ferrous sulphate or oxalic acid in the
presence of sulphuric acid, and the unused excess determined by
titration with standard permanganate solution.
PROCEDURE.--Grind the mineral in an agate mortar until no grit
whatever can be detected under the pestle (Note 1). Transfer it to a
stoppered weighing-tube, and weigh out two portions of about 0.5 gram
into beakers (400-500 cc.) Read Note 2, and then calculate in each
case the weight of oxalic ac
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