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
Without further addition 21.0 c.c.
With 100 c.c. of dilute sulphuric acid 22.0 "
" 10 grams ammonic sulphate 20.5 "
" 10 " sodic sulphate 20.0 "
" 10 " magnesium sulphate 20.4 "
" 10 " manganese sulphate 20.2 "
The results with these salts, in counteracting the interference of the
acid, however, were not a complete success, since the end-reactions were
all indistinct, with the exception, perhaps, of that with the manganese
sulphate.
~Effect of Varying Amounts of Iron.~--In these experiments the bulk of
the assay was 100 c.c., and 10 c.c. of acid were present.
Ferrous chloride used 1 c.c. 10 c.c. 20 c.c. 50 c.c. 100 c.c.
Permanganate required 1.1 " 10.3 " 20.3 " 50.4 " 100.1 "
In making himself familiar with the permanganate of potassium titration,
the student should practise by working out a series of experiments
similar to the above, varying his conditions one at a time so as to be
certain of the cause of any variation in his results. He may then
proceed to experiment on the various methods of reduction.
_A solution of ferric chloride_ is made by dissolving 5.01 grams of iron
wire in 50 c.c. of hydrochloric acid (sp. g. 1.16), and running from a
burette nitric acid diluted with an equal volume of water into the
boiling iron solution, until the liquid changes from a black to a
reddish-yellow. About 4.5 c.c. of the nitric acid will be required, and
the finishing point is marked by a brisk effervescence. The solution of
iron should be contained in an evaporating dish, and boiled briskly,
with constant stirring. There should be no excess of nitric acid. Boil
down to about half its bulk; then cool, and dilute to one litre with
water. Twenty c.c. of this solution diluted to 100 c.c. with water, and
acidified with 10 c.c. of dilute hydrochloric acid, should not
decolorise any of the permanganate of potassium solution; this shows the
absence of ferrous salts. And 20 c.c. of the same solution, boiled with
20 c.c. of the ferrous sulphate solution, should not decrease the
quantity of "permanganate" required for the titration of the ferrous
sulphate added. In a series of experiments on the various methods of
reduction, the following results were got. The modes of working were
those already described.
(1) _With Stannous Chloride._--Twenty c.c. of the ferric chloride
solution required, after reduction with stannous chloride, 20 c.c. of
"permanganate." Fifty c.c. of a solution of ferrous chloride, which
required on titration 49.8 c.c. of "permanganate," required for
re-titration (after subsequent reduction with stannous chloride) 50 c.c.
of the permanganate solution.
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