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
The separation of manganese from other metals is thus effected: Ignite,
in order to destroy any organic matter which may be present; dissolve in
hydrochloric acid, and evaporate to dryness, to separate silica. Take up
with hydrochloric acid, dilute, pass sulphuretted hydrogen, and filter.
Boil off the excess of gas, peroxidise the iron with a drop or two of
nitric acid, and separate the iron as basic acetate (as described under
_Iron_).[81] If the iron precipitate is bulky, it is dissolved in a
little hydrochloric acid, reprecipitated, and the filtrate added to the
original one. Neutralise with soda, and add bromine in excess; heat
gradually to boiling, allow to settle, and filter. The precipitate is
impure dioxide of manganese (containing alkalies and, possibly, cobalt
or nickel).
GRAVIMETRIC DETERMINATION.
Dissolve the precipitate in hydrochloric acid, and boil; add a slight
excess of carbonate of soda, warm, and filter. Wash with hot water, dry,
carefully ignite in an open Berlin crucible, and weigh. The substance is
the brown oxide (Mn_{3}O_{4}), and contains 72.05 per cent. of
manganese. If the percentage of dioxide is required it may be calculated
by multiplying the percentage of manganese by 1.582. It must be borne in
mind that the manganese should never be calculated to dioxide except
when it is known to exist in the ore only in that form.
VOLUMETRIC METHODS.
The two methods are based on the oxidising effect of manganese dioxide;
and if the metal does not already exist in this form it will require a
preliminary treatment to convert it. The following method due to Mr. J.
Pattinson[82] effects this: A quantity of the ore containing not more
than .25 grams of the metal (Mn), is dissolved in hydrochloric acid in a
pint beaker, and, if necessary, 3 or 4 c.c. of nitric acid are added to
peroxidise the iron, and ferric chloride is added if required, so that
there may be at least as much iron as manganese. Calcium carbonate is
added till the solution is slightly red; and next the redness is removed
by the cautious addition of acid; 30 c.c. of zinc chloride solution
(containing 15 grams of zinc per litre) are added, the liquid is brought
to boil and diluted to about 300 c.c. with boiling water; 60 c.c. of a
solution of bleaching powder (33 grams to the litre and filtered),
rendered slightly greenish by acid, are then run in and are followed by
3 grams of calcium carbonate suspended in 15 c.c. of boiling water.
During effervescence the beaker is covered, the precipitate is stirred,
and 2 c.c. of methylated spirit are mixed in. The precipitate is
collected on a large filter, washed with cold water, and then with hot,
till free from chlorine, which is tested for with starch and potassium
iodide. The acid ferrous sulphate solution (presently described) is then
measured into the beaker, and the precipitate, still in the paper,
added; more acid is added (if necessary), and the solution is diluted
and titrated.
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