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
For example, 0.7560 gram of pyrolusite and 1.000 gram of iron were taken
and treated as above; 13.9 c.c. of "permanganate" (standard 100 c.c. =
0.4920 gram iron) were required; this indicates that 0.0684 gram of iron
was left unoxidised by the ore. The iron oxidised, then, was 0.9316 gram
(1.000 - 0.0684); multiplying this by 0.7768, we find that 0.7237 gram
is the quantity of manganese dioxide which was present. This is
equivalent to 95.77 per cent.;
0.7560 : 0.7237 :: 100 : 95.77.
IODINE METHOD.
It has been already stated that when dioxide of manganese is boiled with
strong hydrochloric acid chlorine is given off, and that the amount of
chlorine so liberated is a measure of the dioxide present. If the
chlorine is passed into a solution of potassium iodide, an equivalent of
iodine will be set free.[85] This is apparently a very indirect way of
determining how much of the dioxide is present; but the reactions are
very sharp, and the final determination of the iodine is an easy one.
[Illustration: FIG. 60.]
The finely-powdered sample of dioxide is placed in a small flask
provided with an exit tube leading into a solution of potassic iodide
(fig. 60). On adding hydrochloric acid and boiling, the chlorine evolved
is driven into the iodide solution and there absorbed; the boiling is
continued till the steam and hydrochloric acid fumes have driven the
last portions of the chlorine out of the flask and into the solution. In
this experiment there is a strong tendency for the iodide solution to
rush back into the flask. This tendency is overcome by avoiding draughts
and regulating the heat; or by placing a lump of magnesite in the flask,
which acts by evolving carbonic acid and so producing a steady outward
pressure. When the distillation is finished the tube containing the
iodine is detached and washed out into a beaker. If the solution is
strongly acid it should be almost neutralised by the cautious addition
of dilute ammonia. If crystals of iodine have separated, potassium
iodide must be added in quantity sufficient to dissolve them. The
condenser must be kept cool whilst the chlorine is passing into it.
The solution, transferred to a beaker, is titrated with a standard
solution of sodic hyposulphite (100 c.c. = 1.27 gram iodine or 0.435
gram of dioxide of manganese). In titrating, the solution should be
cold, or not warmer than 30° C. The bulk may vary from 100 to 200 c.c.;
but it is best always to work with the same volume. The "hypo" is run in
with constant agitation until the brown colour has been reduced to a
light yellow; 5 c.c. of starch solution are then added and the titration
cautiously continued until the end is reached; the finish is indicated
by a change from blue to colourless.
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