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
The separation of traces of lead as chromate is a fairly good one.
Dissolve 5 grams of the copper in 17 c.c. of nitric acid and an equal
volume of water; boil off nitrous fumes, neutralise with soda, and
afterwards acidulate with acetic acid; and dilute to a litre. Add 20
grams of sodium acetate, warm, and precipitate the lead with a dilute
solution of potassium chromate. Copper chromate (yellow) may be at the
same time thrown down, but it is readily soluble on diluting. Filter off
the precipitate; wash it into a beaker and pass sulphuretted hydrogen;
oxidise the sulphide and weigh as lead sulphate. Treated in this way 5
grams of copper yielded sulphate of lead equal to 2.0 milligrams of
lead. Five grams of the same sample to which 10 milligrams of lead were
added gave 11.4 milligrams.
~Nickel and Cobalt.~--Nickel is always present in larger or smaller
quantities in commercial copper, and, perhaps, has an influence on the
properties of the metal. It is determined as follows:--Dissolve 10 grams
of the copper in 35 c.c. of nitric acid and an equal bulk of water, boil
off nitrous fumes and neutralise with soda, add 2 grams of carbonate of
soda dissolved in water, boil, and filter. Acidify the filtrate with 2
or 3 c.c. of dilute nitric acid and dilute to 1 or 1-1/2 litres. Pass
sulphuretted hydrogen through the cold solution till the copper is all
down and the liquid smells of the gas. Filter and evaporate the filtrate
to a small bulk, and determine the nickel by electrolysing the solution
rendered ammoniacal, or by precipitating as sulphide and weighing as
sulphate. (See under _Nickel_.) The precipitate, after weighing, should
be tested for cobalt. If present it is separated with potassium nitrite
as described under _Cobalt_. Ten grams of copper gave 6.0 milligrams of
nickel; and another lot of 10 grams of the same copper, to which 10.0
milligrams of nickel had been added, gave 17.2 milligrams.
~Sulphur.~--The amount of sulphur in refined copper is very small,
seldom exceeding 0.005 per cent. In coarse copper, as might be expected,
it is found in larger quantities.
In determining it, it is first converted into sulphuric acid, and then
precipitated and weighed as barium sulphate. The precipitation cannot be
effected from a nitric acid solution. Ten grams of copper are dissolved
in nitric acid, as for the other determinations, and then boiled with
excess of hydrochloric acid till the nitric acid is completely removed.
There is then added a few drops of a dilute solution of baric chloride,
and the solution is allowed to stand for some hours. The baric sulphate
is filtered off and weighed.
The necessity for precipitating from a hydrochloric acid solution is
seen from the following determinations. In each experiment 10 grams of
copper was used, and a known weight of sulphur, in the form of copper
sulphate, added.
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