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
~Separation of Nickel and Cobalt.~--Dissolve the sulphides separated as
above in nitric acid; render alkaline with a solution of potash, then
acidify with acetic acid; add a concentrated solution of _nitrite_ of
potash. The liquid after this addition must have an acid reaction. Allow
to stand for 24 hours in a warm place. Filter off the yellow precipitate
of nitrite of potash and cobalt, and wash with a 10 per cent. solution
of acetate of potash. The cobalt is determined in the precipitate in the
way described under _Cobalt_. The nickel is separated from the solution
by boiling with sodic hydrate, filtering, and dissolving the precipitate
in nitric acid. The solution will contain the nickel.
GRAVIMETRIC DETERMINATION.
The solution, which contains the nickel free from other metals, is
heated, and a solution of sodic hydrate added in slight excess. The
precipitate is filtered off, washed with boiling water, dried, ignited
at a red heat, and weighed when cold. The ignited substance is nickel
oxide (NiO), and contains 78.67 per cent. of nickel. The oxide is a
green powder, readily and completely soluble in hydrochloric acid, and
without action on litmus paper. It is very easily reduced by ignition in
hydrogen to metallic nickel.
[Illustration: FIG. 56.]
Nickel is also determined by electrolysis, as follows:--The nitric acid
solution is rendered strongly ammoniacal, and placed under the
electrolytic apparatus used for the copper assay. Three cells (fig. 56),
however, must be used, coupled up for intensity, that is, with the zinc
of one connected with the copper of the next. The electrolysis is
allowed to go on overnight, and in the morning the nickel will be
deposited as a bright and coherent film. A portion of the solution is
drawn off with a pipette; if it smells of ammonia, has no blue colour,
and gives no precipitate with ammonic sulphide, the separation is
complete. Wash the cylinder containing the deposited metal, first with
water and then with alcohol, as in the copper assay. Dry in the water
oven, and weigh. The increase in weight is metallic nickel.
As an example:--There was taken 1 gram of a nickel alloy used for
coinage. It was dissolved in 10 c.c. of nitric acid, and diluted to 100
c.c. with water. The copper was then precipitated by electrolysis. It
weighed 0.734 gram. The solution, after electrolysis, was treated with
sulphuretted hydrogen, and the remaining copper was thrown down as
sulphide, and estimated colorimetrically. This amounted to 3-1/2
milligrams. The filtrate was evaporated, treated with ammonia, warmed,
and filtered. The ferric hydrate was dissolved in dilute acid, and
reprecipitated, dried, ignited, and weighed. Its weight was 0.0310 gram.
The two filtrates were mixed, and reduced in bulk to about 50 c.c.; a
considerable excess of ammonia was added, and the nickel precipitated by
electrolysis. It weighed 0.2434 gram. These quantities are equivalent
to:
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