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 solution containing the zinc is contained in an evaporating dish,
and freed from sulphuretted hydrogen by boiling, and, if necessary, from
an excess of acid by evaporation. The evaporating dish must be a large
one. Cautiously add sodium carbonate to the hot, moderately dilute
solution, until the liquid is distinctly alkaline, and boil. Allow the
precipitate to settle, decant on to a filter, and wash with hot water.
Dry, transfer to a porcelain crucible (cleaning the paper as much as
possible), add the ash, ignite, and weigh. The substance weighed is
oxide of zinc, which contains 80.26 per cent. of the metal. It is a
white powder, becoming yellow when heated. It must not show an alkaline
reaction when moistened. If it contains manganese this metal will be
present as sesquioxide (Mn_{2}O_{3}). Its amount can be determined by
dissolving in dilute acid and boiling with an excess of sodic hydrate.
The oxide of manganese will be precipitated, and can be ignited and
weighed. Its weight multiplied by 1.035 must be deducted from the weight
of oxide of zinc previously obtained. The results yielded by the
gravimetric determination are likely to be high, since the basic
carbonate of zinc frequently carries down with it more or less soda
which is difficult to wash off.
VOLUMETRIC DETERMINATION
This method is based on the facts that zinc salts in an acid solution
decompose potassium ferrocyanide, forming a white insoluble zinc
compound; and that an excess of the ferrocyanide can be detected by the
brown coloration it strikes with uranium acetate. The method resembles
in its working the bichromate iron assay. The standard solution of
potassium ferrocyanide is run into a hot hydrochloric acid solution of
the zinc until a drop of the latter brought in contact with a drop of
the indicator (uranium acetate) on a white plate strikes a brown colour.
The quantity of zinc in the solution must be approximately known; run in
a little less of the ferrocyanide than is expected will be necessary;
test a drop or two of the assay, and then run in, one or two c.c. at a
time, until the brown colour is obtained. Add 5 c.c. of a standard zinc
solution, equivalent in strength to the standard "ferrocyanide,"
re-titrate, and finish off cautiously. Of course 5 c.c. must be deducted
from the reading on the burette. The precipitate of zinc ferrocyanide
formed in the assay solution is white; but if traces of iron are
present, it becomes bluish. If the quantity of ferrocyanide required is
known within a few c.c., the finishing point is exactly determined in
the first titration without any addition of the standard zinc solution.
Unfortunately this titration serves simply to replace the gravimetric
determination, and does not, as many volumetric processes do, lessen the
necessity for a complete separation of any other metals which are
present. Most metals give precipitates with ferrocyanide of potassium in
acid solutions. If the conditions are held to, the titration is a fairly
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