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
~Determination of Iron in Substances Insoluble in Acids.~--Weigh up 1
gram of the ore, mix with 5 or 6 grams of carbonate of soda and 0.5 gram
of nitre by rubbing in a small mortar, and transfer to a platinum
crucible. Clean out the mortar by rubbing up another gram or so of soda,
and add this to the contents of the crucible as a cover. Fuse till
tranquil. Cool. Extract with water. If the ore carries much silica,
evaporate to dryness with hydrochloric acid to separate it. Re-dissolve
in hydrochloric acid, and separate the iron by precipitating with
ammonia and filtering. If only a small quantity of silica is present,
the aqueous extract of the "melt" must be filtered, and the insoluble
residue washed and dissolved in dilute hydrochloric acid. Reduce and
titrate.
A convenient method of at once separating iron from a solution and
reducing it, is to add ammonia, pass sulphuretted hydrogen through it,
filter, and dissolve the precipitate in dilute sulphuric acid. The
solution, when boiled free from sulphuretted hydrogen, is ready for
titrating.
STANNOUS CHLORIDE PROCESS.
The colour imparted to hot hydrochloric acid solutions by a trace of a
ferric compound is so strong, and the reducing action of stannous
chloride is so rapid, that a method of titration is based upon the
quantity of a standard solution of stannous chloride required to
completely decolorise a solution containing ferric iron. This method is
more especially adapted for the assay of liquors containing much ferric
iron and of those oxidised ores which are completely soluble in
hydrochloric acid. It must be remembered, however, that it only measures
the ferric iron present, and when (as is generally the case) the total
iron is wanted, it is well to calcine the weighed portion of ore
previous to solution in order to get the whole of the iron into the
higher state of oxidation, since many ores which are generally supposed
to contain only ferric iron carry a considerable percentage of ferrous.
_The stannous chloride solution_ is made by dissolving 20 grams of the
commercial salt (SnCl_{2}.2H_{2}O) in 100 c.c. of water with the help of
20 c.c. of dilute hydrochloric acid, and diluting to a litre. The
solution may be slightly opalescent, but should show no signs of a
precipitate. The strength of this is about equivalent to 1 gram of iron
for each 100 c.c. of the solution, but it is apt to lessen on standing,
taking up oxygen from the air, forming stannic chloride. A larger
proportion of hydrochloric acid than is ordered above would remove the
opalescence, but at the same time increase this tendency to atmospheric
oxidation, as the following experiments show. The stannous chloride
solution (20 c.c.) was mixed with varying amounts of strong hydrochloric
acid (sp. g. 1.16), diluted to 100 c.c., and exposed in open beakers for
varying lengths of time; and the residual stannous chloride measured by
titration with permanganate. The quantities required were as follows:--
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