Scientific American Supplement, No. 299, September 24, 1881Various
Science
Scientific American Supplement, No. 299, September 24, 1881
Various
Science -- Periodicals
To a liquid, which may contain free hydrochloric acid, hydrogen sulphide
is added, then neutralized with ammonium hydrate, and saturated with
ammonium sulphide in excess. The reduction may be accelerated by the
addition of some ammonium sulphate. The antimony separates out as a
fine, light gray precipitate on the electrode, and which adheres very
firmly, provided the precipitation has not been carried on too rapidly,
_i. e._, if the current employed for the reduction was not too strong.
When the reduction has been completed, the supernatant liquid is poured
off, and the residue washed in the ordinary manner.
DETERMINATION OF ARSENIC.
Arsenic cannot be completely separated from either its aqueous
hydrochloric acid, or from a solution to which ammonium oxalate has been
added in excess. From its aqueous as well as from its oxalate solution,
a portion of the metal may be separated, but if the current is passed
through its hydrochloric acid solution for a sufficient length of time,
all the arsenic will be volatilized as arsenious hydride (AsH_3).
SEPARATION OF IRON FROM MANGANESE.
If a solution of ferric oxide and manganese ammonium oxalate is
submitted to electrolysis, without the previous addition of ammonium
oxalate, the characteristic color of permanganic acid immediately makes
its appearance, and the peroxide gradually precipitates itself on the
positive, while the iron is deposited on the negative electrode. When
the examination is made in the above manner, it is impossible to
separate the two metals, for the peroxide will bring down with it a
considerable quantity of ferric hydrate. The separation of the two
metals is only possible when the precipitation of the manganese peroxide
is prevented, until the greater portion of the iron has been deposited.
This result may be attained by adding sodium phosphate, or, better
still, by the addition of ammonium oxalate in great excess. In both
cases the characteristic coloration from permanganic acid is developed
by the action of the current at the positive pole; this, however,
disappears in the direction of the negative electrode. After the greater
portion of the ammonium oxalate has been converted into carbonate, the
coloration and necessarily the formation of manganese peroxide begins.
Ammonium oxalate is added to the solution, and heat applied; then three
or four grammes more of ammonium oxalate are dissolved in the liquid,
which is then immediately submitted to electrolysis. When the amount of
manganese is small, the separation of the two elements takes place very
rapidly, and the results are accurate. If the amount of manganese is
more than double that of iron, the separation of the latter will take a
much longer time. Then, in order to effect a complete separation of the
two elements, it is necessary to redissolve the deposited manganese in
oxalic acid (the acid is added, without interrupting the current, until
the liquid becomes red), and the current is allowed to continue its
action.
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