a porcelain basin of about 200 c.c. capacity, and
removing the loosened foil and broken composition by
means of a pointed wooden chip. Composition adhering
to the shell or foil is loosened by alcohol, and washed
into the dish by means of alcohol in a small wash
bottle. The shell and foil are put to one side
and subsequently weighed when dry. The composition
in the dish is broken down quite fine with a flat-headed
glass rod, and the alcohol evaporated on the water
bath till the residue is moist, but not quite dry,
25 c.c. of water are then added, and the composition
well stirred from the bottom. After the addition
of 0.5 grm. of pure sodium, thiosulphate, the contents
of the dish, is well stirred for two and a half minutes.
One drop of methyl orange is then added, and the solution
titrated with N/20 sulphuric acid, which has been
standardised against weighings of 0.05-0.1 grm. fulminate
to which 25 c.c. of water is added in a porcelain
dish, then 0.5 grm. of thiosulphate, and after stirring
for two and a half minutes, titrated with N/20 sulphuric
acid. The small amount of antimony sulphide present
does not interfere with the recognition of the end
point. After titration, the solution is filtered
through a small 5-1/2 cm. filter paper, which retains
the antimony sulphide. The filter paper containing
the Sb_{2}S_{3} is well washed and then transferred
to a large 6 by 1 test tube. Five c.c. of strong
hydrochloric acid are added, and the contents of the
tube boiled gently for a few seconds until the sulphide
is dissolved and all the H_{2}S driven off or decomposed:
2-3 c.c. of a saturated solution of tartaric acid
are added, and the contents of the tube washed into
a 250 c.c. Erlenmeyer flask. The solution
is then nearly neutralised with sodium carbonate,
excess of bi-carbonate added, and after the addition
of some starch solution titrated with N/20 iodine
solution. This method for small quantities of
stibnite is both quick and accurate, the error being
about +-0.0003 grm. Sb_{2}S_{3} at the outside.
The tendency of this method is to give slightly low figures for the fulminate, but since these are uniform within a negligible error, it does not affect the value of the results as a criterion of uniformity. The following test results were obtained by Dr Brownsdon:—
_______________________________________________________
_____ | | | | | Fulminate Taken. | Fulminate Found. | Error. | | Grm. | Grm. | Grm. | | | | | | 0.0086 | 0.0083 | -0.0003 | | 0.0082 | 0.0081 | -0.0001 | | 0.0074 | 0.0071 | -0.0003 | | 0.0068 | 0.0066 | -0.0002 | |____________________|___________________|__________________
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