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
The bismuth having been separated and dissolved in nitric acid[62] is
precipitated (after dilution) by the addition of carbonate of ammonium
in slight excess, and boiling. The precipitate is filtered off, washed
with hot water, dried, ignited, and weighed. The ignition should be
performed carefully at not above a low red heat. The oxide which is
formed has, at this temperature, a dark yellow or brown colour, and
becomes yellow on cooling. It is bismuthic oxide (Bi_{2}O_{3}) and
contains 89.65 per cent. of bismuth. Fusion with potassium cyanide at a
temperature just sufficient to melt the salt reduces it to the metal
which falls to the bottom and runs into a globule. The button of metal
may be weighed, but it often sticks tenaciously to the bottom of the
crucible. The precipitation with ammonic carbonate must not be made in a
sulphate or chloride solution; since basic compounds would then be
thrown down, and the result on weighing would either be too low (because
of the volatilisation of the chloride), or too high (because of the
retention of sulphuric acid).
Bismuth compounds in a nitric acid solution are readily decomposed by
the electric current, but the deposited bismuth is not coherent. It
comes down in shaggy tufts which are difficult to wash and easy to
oxidise.
VOLUMETRIC ASSAY.
There are two methods which have been proposed; one based on the
precipitation as chromate and the estimation of the chromic acid; and
the other on the precipitation as oxalate and subsequent titration with
permanganate of potash. These offer little advantage over the easy
gravimetric determination.
COLORIMETRIC METHOD.
Bismuth iodide dissolves in excess of potassium iodide, forming a
yellow-coloured solution, indistinguishable in colour from that given by
iodine. The colour, however, is not removed by boiling or by sulphurous
acid. Since none of the commoner metals give such a colour, and free
iodine is easily separated by boiling, this method is specially suited
for small determinations of bismuth.
It requires a _solution of bismuth_, made by dissolving 0.1 gram of
bismuth in a drop or so of nitric acid, evaporating with a little
sulphuric acid and diluting with water to 1 litre. 1 c.c. will contain
0.1 milligram of bismuth. And a _solution of sulphurous acid_, made by
diluting 10 c.c. of the commercial acid to 1 litre with water.
The determination is made in the usual way: 50 c.c. of the prepared
solution, which should not carry more than 0.75 milligram nor less than
0.01 milligram of bismuth, are placed in a Nessler tube and the colour
compared with that observed in a similar tube containing water and
potassium iodide on adding the standard solution of bismuth.
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