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
~Effect of Foreign Metals.~--Lead, mercury, cadmium, bismuth, arsenic,
tin, antimony, nickel, cobalt, manganese, aluminium, zinc, strontium,
barium, calcium, magnesium, sodium, or potassium, when separately
present in quantities of from 100 to 200 times the weight of iron
present, do not interfere if they have previously been brought to their
highest oxidised condition by boiling with nitric acid or by treating
with permanganate. Arsenic and phosphoric acids interfere unless an
excess of free hydrochloric or other acid is present. Oxalic acid (but
not tartaric acid) in minute quantities destroys the colour. Nitrous
acid strikes a red colour with the sulphocyanate of potassium;
consequently, when nitric acid has been used in excess, high results may
be obtained. Copper and some other metals interfere, so that in most
cases it is advisable to concentrate the iron before estimating it. A
blank experiment should always be made with the reagents used in order
to determine the iron, if any, introduced during the solution, &c., of
the substance assayed.
~Determination of Iron in Metallic Copper.~--This may be most
conveniently done during the estimation of the arsenic. The small
quantity of white flocculent precipitate which may be observed in the
acetic acid solution before titrating, contains the whole of the iron as
ferric arsenate. It should be filtered off, dissolved in 10 c.c. of
dilute hydrochloric acid, and diluted to 100 c.c.; 10 c.c. of this may
be taken for the estimation. For example: 10 grams of copper were taken,
and the iron estimated; 3.0 c.c. of standard ferric chloride solution
were used, equivalent to 0.03 milligram of iron; this multiplied by 10
(because only 1/10th of the sample was taken) gives 0.3 milligram as the
iron in 10 grams of copper. This equals 0.003 per cent.
In a series of experiments with this method working on 10-gram lots of
copper, to which known quantities of iron had been added, the following
were the results:--
Iron present 0.015% 0.070% 0.100% 0.495%
Iron found 0.015" 0.061" 0.087" 0.522"
When no arsenic is present in the copper, the iron can be separated by
fractionally precipitating with sodic carbonate, dissolving in ammonia,
and filtering off the ferric hydrate. Coppers generally carry more iron
the less arsenic they contain.
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