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 following experiments show the effect of variation in the conditions
of the assay. Use a solution of copper sulphate containing 39.38 grams
of copper sulphate crystals (CuSO_{4}.5H_{2}O) in the litre. 100 c.c.
equal 1.00 gram of copper.
~Effect of Varying Temperature.~--The assay after the addition of the
potassic iodide must be kept cold, else iodine may be volatilised.
~Effect of Varying Potassium Iodide.~--In various descriptions of the
process the amount of iodide required is variously stated at from "a few
crystals" to as much as 10 grams. The proportion required by theory for
1 gram of copper is a little over 5 grams: an excess, however, is
required to keep the liberated iodine in solution. On economic grounds
this excess should not be extravagant; if the student uses 10 parts of
the iodide for each part of copper in the assay he will have sufficient.
In the experiments there were used 20 c.c. of the copper sulphate, with
varying amounts of potassic iodide, and the following results were
got:--
Potassic iodide added 1.5 gram 3 grams 5 grams
"Hypo" required 20.0 c.c. 20.0 c.c. 20.0 c.c.
In these the iodide was added direct to the solution containing the
copper, which was afterwards diluted to 100 c.c. and titrated. In
another series the iodide was added after the dilution to 100 c.c., and
the results were:--
Potassic iodide added 1.5 gram 3 grams 5 grams 10 grams
"Hypo" required 20.0 c.c. 20.1 c.c. 20.0 c.c. 20.0 c.c.
~Effect of Varying Bulk.~--In these experiments, 20 c.c. of copper
sulphate were taken, 3 grams of potassic iodide added, and also water to
the required bulk.
Bulk 20.0 c.c. 100.0 c.c. 200.0 c.c. 500.0 c.c.
"Hypo" required 20.0 " 20.0 " 20.0 " 19.9 "
In the last of these experiments the colour was discharged at 18 c.c.,
but gradually returned until 19.9 c.c. had been run in. It will be seen
that considerable variation in bulk does not interfere.
~Effect of Acetic Acid.~--These experiments were like the last series
mentioned, but the bulk was 100 c.c., and varying amounts of acetic acid
were added.
Acetic acid added 0 c.c. 1.0 c.c. 5.0 c.c. 10.0 c.c. 20.0 c.c.
"Hypo" required 20.0 " 20.1 " 20.1 " 20.0 " 20.2 "
Acetic acid, then, does not interfere to any serious extent.
~Effect of Varying Sodium Acetate.~--These experiments were like those
last mentioned, but without acetic acid, and with varying amounts of
sodium acetate.
Sodium acetate added 0 gram 1 gram 2 grams 5 grams 10 grams
"Hypo" required 20.0 c.c. 20.0 c.c. 20.2 c.c. 19.3 c.c. 18.2 c.c.
In the 5 grams experiment, when the finishing point had been apparently
reached the colour slowly returned; but as the results generally on
titrating were not satisfactory a repetition of the experiment was made
with the addition of 5 c.c. of acetic acid, which gave an equally bad
result.
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