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
_Manganese_ does not directly interfere, but the precipitated hydrate,
which rapidly darkens through atmospheric oxidation, obscures the end
reaction. It may be removed by passing sulphuretted hydrogen through the
filtrate from the acetate separation: sulphides of nickel, cobalt and
zinc will be precipitated, whilst manganese remains in solution: the
addition of more sodium acetate may assist the precipitation. The
precipitate must be filtered off and dissolved in nitric acid: the
solution should be evaporated to dryness. The filtrate may retain a
little nickel; if so, add ammonia till alkaline, then acidify with
acetic acid and again filter; any small precipitate obtained here should
be added to that first obtained.
It is only when _cobalt_ is present that any further separation is
required. Cobalt hydrate takes up oxygen from the air, and on adding
potassium cyanide some may refuse to dissolve; and the solution itself
acquires a brown colour, which becomes deeper on standing. At this stage
the cobalt is easily separated. The solution containing the nickel and
cobalt with no great excess of acid, is made alkaline by adding 20 c.c.
of soda exactly as in preparing for a titration. So, too, the solution
of cyanide is added so as to have an excess of 20 or 30 c.c.; the
solution may have a brown colour, but if it is not quite clear it _must_
be filtered. Then warm (boiling is not needed) and add from 50 to 100
c.c. of bromine water. This throws down all the nickel as black
peroxide in a condition easy to filter. Filter it off and wash with
water. The precipitate can be dissolved off the filter with the greatest
ease by a little warm sulphurous acid. The filtrate and washings, boiled
till free from sulphurous acid, yield the nickel as sulphate in a clean
condition.
~Determination of Nickel in Nickel Sulphate Crystals.~--Take 0.5 gram of
the salt, dissolve in 50 c.c. of water and add 25 c.c. of solution of
soda. Run in from a burette, say, 60 c.c. "cyanide." Add a few drops of
potassium iodide and titrate back with "silver nitrate." Suppose 15.5
c.c. of the latter is required. Then 15.5 c.c. subtracted from 60 c.c.
leaves 44.5 c.c., and since 100 c.c. = 0.25 gram of nickel, 44.5 c.c.
will equal 0.11125 gram of nickel. This in 0.5 gram of the salt equals
22.25 per cent.
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