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
Dissolve the precipitate in dilute hydrochloric acid; peroxidise with a
few drops of nitric acid and boil, dilute to about 200 c.c., add ammonia
(with constant stirring) till the liquid smells of it, and heat to
boiling. Wash as much as possible by decantation with hot water.
Transfer to the filter, and wash till the filtrate gives no indication
of soluble salts coming through. The filtrate must be colourless and
clear. The wet precipitate is very bulky, of a dark-brown colour and
readily soluble in dilute acids, but insoluble in ammonia and dilute
alkalies. When thrown down from a solution containing other metals it is
very apt to carry portions of these with it, even when they are by
themselves very soluble in ammoniacal solutions. It must be dried and
ignited, the filter paper being burnt separately and its ash added. When
further ignition ceases to cause a loss of weight, the residue is ferric
oxide (Fe_{2}O_{3}), which contains 70 per cent. of iron. The weight of
iron therefore can be calculated by multiplying the weight of oxide
obtained by 0.7.
The presence of ammonic chloride causes loss of iron during the
ignition, and organic matter causes an apparent loss by reducing the
iron to a lower state of oxidation. When the iron in the solution much
exceeds 0.2 gram the volumetric determination is generally adopted, as
the bulkiness of the precipitate of ferric hydrate makes the gravimetric
method very inconvenient.
VOLUMETRIC METHODS.
As already explained these are based on the measurement of the volume of
a reagent required to bring the whole of the iron from the ferrous to
the ferric state (oxidation), or from the ferric to the ferrous
(reduction). Ferrous compounds are converted into ferric by the action
of an oxidising agent in the presence of an acid. Either permanganate or
bichromate of potash is generally used for this purpose.[65]
Ferric compounds are reduced to ferrous by the action of:--
(1) Stannous chloride;
(2) Sulphuretted hydrogen;
(3) Sodium sulphite; or
(4) Zinc.[66]
The processes, then, may be divided into two kinds, one based on
oxidation and the other on reduction. In each case the titration must be
preceded by an exact preparation of the solution to be assayed in order
that the iron may be in the right state of oxidation.
~PERMANGANATE AND BICHROMATE METHODS.~
These consist of three operations:--
(1) Solution of the ore;
(2) Reduction of the iron to the ferrous state; and
(3) Titration.
~Solution.~--The only point to be noticed concerning the first operation
(in addition to those already mentioned) is that nitric acid must be
absent. If nitric acid has been used, evaporate to dryness, of course
without previous dilution; add hydrochloric or sulphuric acid, and boil
for five or ten minutes. Dilute with water to about 100 c.c., and warm
until solution is complete.
The reduction is performed by either of the following methods:--
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