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
~Determination of Copper in Copper Pyrites.~--Take 2 grams of the dried
and powdered ore and treat in a porcelain dish with 20 c.c. of nitric
acid, and evaporate to dryness. Take up with 30 c.c. of hydrochloric
acid, dilute, and transfer to a pint flask; make up with water to 200
c.c., warm, and pass sulphuretted hydrogen to excess. Filter, and wash
the precipitate with water acidified with sulphuric acid. Wash the
precipitate back into the flask, and dissolve with 15 c.c. of nitric
acid. Evaporate almost to dryness; add 20 c.c. of water, and boil till
free from nitrous fumes; filter off the sulphur and gangue; neutralise
with soda, avoiding excess; add 1 or 2 c.c. of acetic acid, and shake
till clear. Add 5 grams of potassium iodide, dilute to 100 c.c., and
titrate. The following is an example:--
0.5 gram of copper required 50.5 c.c. "hypo."
The assay required 55.6 " "
which is equal to 27.5 per cent. of copper.
COLORIMETRIC PROCESS.
This is based on the blue coloration of ammoniacal copper solutions. The
quantity of copper in 100 c.c. of the assay solution should not be more
than 15 milligrams, or less than half a milligram. It is not so delicate
as most other colorimetric methods, but nevertheless is a very useful
one.
The manner of working is the same as that described under iron.
~Standard Copper Solution.~--Weigh up 0.5 gram of electrotype copper,
dissolve in 10 c.c. of nitric acid, boil off nitrous fumes, and dilute
to 1 litre. 1 c.c. = 0.5 milligram.
In nearly all cases it will be necessary to separate the copper with
sulphuretted hydrogen from a solution of about 5 grams of the material
to be assayed. The filter paper containing the sulphide (and, probably,
much sulphur) is dried and burnt. The ashes are dissolved in 5 c.c. of
dilute nitric acid, 10 c.c. of dilute ammonia added, and the solution
filtered through a coarse filter into a Nessler tube, washing the paper
with a little dilute ammonia.
The estimation of the colour and calculation of the result are made in
the way described on page 44.
The effect of varying conditions on the assay may be seen from the
following experiments.
~Effect of Varying Temperature.~--The effect of increased temperature is
to slightly decrease the colour, but this can only be observed when a
fair quantity of copper is present.
1.0 c.c. at 15° showed the colour of 1.0 c.c. at 70°
2.5 " " " " 2.7 "
5.0 " " " " 5.0 "
10.0 " " " " 9.0 "
~Effect of Varying Ammonia.~--The solution must, of course, contain free
ammonia; about 5 c.c. of dilute ammonia in 50 c.c. bulk is the quantity
to be used in the experiments. A larger quantity affects the results,
giving lower readings and altering the tint. With small quantities of
ammonia the colour approaches a violet; with larger, a sky-blue.
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