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
When nitric acid, or the fusion method, has been used, the metal will be
in solution in the ferric state, no matter in what condition it existed
in the ore. But with dilute hydrochloric or sulphuric acid it will
retain its former degree of oxidation. Hydrochloric acid, for example,
with chalybite (ferrous carbonate) will give a solution of _ferrous_
chloride; with hæmatite (ferric oxide) it will yield _ferric_ chloride;
and with magnetite (ferrous and ferric oxides) a mixture of ferrous and
ferric chlorides. Metallic iron yields solutions of _ferrous_ salts. It
is convenient to speak of the iron in a ferrous salt as ferrous iron,
and when in the ferric state as ferric iron. Frequently it is required
to determine how much of the iron exists in an ore in each condition. In
such cases it is necessary to keep off the air whilst dissolving; the
operation should, therefore, be performed in an atmosphere of carbonic
acid.
~Separation.~--The separation of the iron from the other substances is
as follows:--Silica is removed by evaporating the acid solution, and
taking up with acid, as described under _Silica_; the whole of the iron
will be in solution. The metals of Groups I. and II. are removed by
passing sulphuretted hydrogen, and at the same time the iron will be
reduced to the ferrous state. The solution should be filtered into a 16
oz. flask, boiled to get rid of the gas, and treated (whilst boiling)
with a few drops of nitric acid, in order to convert the whole of the
iron into the ferric state. When this condition is arrived at, an
additional drop of nitric acid causes no dark coloration. The boiling
must be continued to remove nitrous fumes. Next add caustic soda
solution until the colour of the solution changes from yellow to red.
The solution must be free from a precipitate; if the soda be
incautiously added a permanent precipitate will be formed, in which case
it must be redissolved with hydrochloric acid, and soda again, but more
cautiously, added. After cooling, a solution of sodium acetate is added
until the colour of the solution is no longer darkened. The solution,
diluted to two-thirds of the flaskful with water, is heated to boiling.
Long-continued boiling must be avoided. The precipitate is filtered
quickly through a large filter, and washed with hot water containing a
little acetate of soda.
The precipitate will contain all the iron and may also contain alumina,
chromium, titanium, as well as phosphoric, and, perhaps, arsenic
acids.[64]
Dissolve the precipitate off the filter with dilute sulphuric acid,
avoiding excess, add tartaric acid and then ammonia in excess. Pass
sulphuretted hydrogen, warm, and allow the precipitate to settle. Filter
and wash with water containing a little ammonic sulphide.
GRAVIMETRIC METHOD.
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