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
good one, and differences in the results of an assay will be due to
error in the separation. Ferric hydrate precipitated in a fairly strong
solution of zinc will carry with it perceptible quantities of that
metal. Similarly, large quantities of copper precipitated as sulphide by
means of sulphuretted hydrogen will carry zinc with it, except under
certain nicely drawn conditions. When much copper is present it is best
separated in a nitric acid solution by electrolysis. The titration of
the zinc takes less time, and, with ordinary working, is more
trustworthy than the gravimetric method.
_The standard ferrocyanide solution_ is made by dissolving 43.2 grams of
potassium ferrocyanide (K_{4}FeCy_{6}.3H_{2}O) in water, and diluting to
a litre. One hundred c.c. are equal to 1 gram of zinc.
_The standard zinc solution_ is made by dissolving 10 grams of pure zinc
in 50 c.c. of hydrochloric acid and 100 or 200 c.c. of water, and
diluting to 1 litre, or by dissolving 44.15 grams of zinc sulphate
(ZnSO_{4}.7H_{2}O) in water with 30 c.c. of hydrochloric acid, and
diluting to 1 litre. One hundred c.c. will contain 1 gram of zinc.
_The uranium acetate solution_ is made by dissolving 0.2 gram of the
salt in 100 c.c. of water.
To standardise the "ferrocyanide" measure off 50 c.c. of the standard
zinc solution into a 10 oz. beaker, dilute to 100 c.c., and heat to
about 50° C. (not to boiling). Run in 47 or 48 c.c. of the
"ferrocyanide" solution from an ordinary burette, and finish off
cautiously. Fifty divided by the quantity of "ferrocyanide" solution
required gives the standard.
In assaying ores, &c., take such quantity as shall contain from 0.1 to 1
gram of zinc, separate the zinc as sulphide, as already directed.
Dissolve the sulphide off the filter with hot dilute hydrochloric acid,
which is best done by a stream from a wash bottle. Evaporate the
filtrate to a paste, add 5 c.c. of dilute hydrochloric acid, dilute to
100 c.c. or 150 c.c., heat to about 50° C., and titrate. Manganese, if
present, counts as so much zinc, and must be specially separated, since
it is not removed by the method already given. The following method will
effect its removal. To the hydrochloric acid solution of the zinc and
manganese add sodium acetate in large excess and pass sulphuretted
hydrogen freely. Allow to settle, filter off the zinc sulphide and wash
with sulphuretted hydrogen water. The precipitate, freed from manganese,
is then dissolved in hydrochloric acid and titrated.
The following experiments show the effect of variation in the conditions
of the assay:--
~Effect of Varying Temperature.~--Using 20 c.c. of the standard zinc
solution, 5 c.c. of dilute hydrochloric acid, and diluting to 100 c.c.
Temperature 15° C. 30° C. 70° C. 100° C.
"Ferrocyanide" required 20.6 c.c. 20.3 c.c. 20.3 c.c. 20.3 c.c.
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