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
~Arsenic.~--The proportion of arsenic in copper varies from 0.01 to 0.75
per cent. whilst in coarse copper it may amount to 2 or even 3 per cent.
To determine it, dissolve 5, 10, or 20 grams of the copper (according to
the amount of arsenic present) in 18 c.c., 35 c.c., or 70 c.c. of nitric
acid, and an equal volume of water. Boil off the nitrous fumes, dilute
to 100 c.c. and neutralise with soda; add 1.5 or 2 grams of carbonate of
soda dissolved in a little water, and boil. Filter (washing is
unnecessary) and dissolve back into the flask with a little dilute
hydrochloric acid; add 30 c.c. of dilute ammonia and 25 c.c. of
"magnesia mixture," and allow to stand overnight. The whole of the
arsenic is precipitated as ammonic-magnesic arsenate in one hour, but it
is advisable to leave it longer. The precipitate may be dried and
weighed, or, better, titrated with uranium acetate. (See _Arsenic_.) To
test this method of separation 10 grams of pure copper were taken and
0.200 gram of arsenic dissolved with it. The arsenic was determined by
titration with uranium acetate, and 0.200 gram was found. Two other
similar experiments with 0.080 and 0.010 gram of arsenic added, gave
0.079 and 0.012 gram respectively.
Antimony or bismuth may be present without interfering with the
titration. With 0.100 gram of antimony and 0.100 gram of arsenic, 0.100
gram of arsenic was found; and in another case, with 0.100 gram of
bismuth and 0.060 gram of arsenic, 0.060 gram was found. In these
experiments the antimony and bismuth were present in the assay solution
when titrated. For a gravimetric determination they would require to be
removed before precipitating with "magnesia mixture."
Phosphorus, if present, counts as arsenic in the proportion of 1 to 2.4;
but, except in the case of coarse coppers, it is always absent.
Iron, if present, interferes by forming a white flocculent precipitate
of ferric arsenate after the addition of the sodium acetate and
preliminary to the titration. Each milligram of iron abstracts, in this
way, 1.3 milligrams of arsenic.
~Iron.~--Refined coppers carry traces of iron, varying from 0.001 to
0.01 per cent. It is best determined during the arsenic estimation. The
precipitate of the ammonic-magnesic arsenate will contain the whole of
the iron as ferric hydrate. On dissolving in hydrochloric acid,
neutralising with ammonia, adding 5 c.c. of sodic acetate, diluting, and
boiling, it reappears as a white precipitate of ferric arsenate. It is
filtered off (the arsenic being estimated in the filtrate), dissolved in
warm hydrochloric acid, and determined colorimetrically as described
under _Iron_. A series of experiments testing the separation is there
given.
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