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
All zinc compounds are either soluble in, or are decomposed by, boiling
with acids, the zinc going into solution. Zinc forms only one series of
salts, and these are colourless. Their chief characteristic is
solubility in an alkaline solution, from which sulphuretted hydrogen
produces a white precipitate of zinc sulphide. Zinc is detected by
dissolving the substance in hydrochloric or nitric acid, boiling, and
adding sodic hydrate in excess, filtering, and adding ammonic sulphide
to the filtrate. The precipitate contains the zinc, which can be
dissolved out by boiling with dilute sulphuric acid, and detected by the
formation of a white precipitate on the addition of potassic
ferrocyanide.
The dry assay of zinc can only be made indirectly, and is
unsatisfactory. Zinc is volatile, and at the temperature of its
reduction is a gas. It is impracticable to condense the vapour so as to
weigh the metal, consequently its amount is determined by loss. The
following method gives approximate results: Take 10 grams of the dried
and powdered ore and roast, first at a low temperature and afterwards at
a higher one, with the help of carbonate of ammonia to decompose the
sulphates formed; cool and weigh. The metals will be present as oxides.
Mix with 2 grams of powdered charcoal and charge into a black-lead
crucible heated to whiteness, cover loosely, and leave in the furnace
for about a quarter of an hour. Uncover and calcine the residue, cool
and weigh. The loss in weight multiplied by 8.03 gives the percentage of
zinc in the ore.
WET METHODS.
Solution and separation may be effected as follows: Treat 1 or 3 grams
of the substance with 10 or 30 c.c. of hydrochloric acid or aqua regia;
evaporate to dryness; take up with 10 c.c. of hydrochloric acid and
dilute to 100 c.c.; heat nearly to boiling; saturate with sulphuretted
hydrogen; filter, and wash with water acidulated with hydrochloric acid.
Boil off the sulphuretted hydrogen and peroxidise with a few drops of
nitric acid. Cool; add caustic soda till nearly, but not quite,
neutralised, and separate the iron as basic acetate by the method
described under _Iron_. To the filtrate add ammonia till alkaline, and
pass sulphuretted hydrogen. Allow to settle and decant on to a filter.
Dissolve off the precipitate from the filter with hot dilute
hydrochloric acid. The solution will contain the zinc, together with any
manganese the ore contained, and, perhaps, traces of nickel and cobalt.
If the zinc is to be determined volumetrically, and manganese is
present, this latter is separated with carbonate of ammonia, as
described further on; but if a gravimetric method is used, and only
small quantities of manganese are present, it is better to proceed as if
it were absent, and to subsequently determine its amount, which should
be deducted.
GRAVIMETRIC DETERMINATION.
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