Poisons, Their Effects and Detection: A Manual for the Use of Analytical Chemists and ExpertsBlyth, Alexander Wynter
Science
Poisons, Their Effects and Detection: A Manual for the Use of Analytical Chemists and Experts
Blyth, Alexander Wynter
Poisons
Another method, accurate but only applicable to the fairly pure
substance, is to dissolve 1 to 2 grms. in water, remove any free acid by
baric carbonate, and then treat the liquid thus purified by a known
volume of standard soda. The soda is now titrated back, using litmus as
an indicator, each c.c. of normal alkali neutralised by the sample
corresponds to 0·1655 grm. of chloral hydrate. Small quantities of
chloral hydrate may be conveniently recovered from complex liquids by
shaking them up with ether, and removing the ethereal layer, in the tube
represented in the figure.[182] The ether must be allowed to evaporate
spontaneously; but there is in this way much loss of chloral. The best
method of estimating minute quantities is to alkalise the liquid, and
slowly distil the vapour through a red-hot combustion-tube charged with
pure lime, as in the process described at p. 153. A dilute solution of
chloral may also be treated with a zinc-copper couple, the nascent
hydrogen breaks the molecule up, and the resulting chloride may be
titrated, as in water analyses, by silver nitrate and potassic chromate.
[Illustration]
[182] The figure is from “Foods”; the description may be here
repeated:--A is a tube of any dimensions most convenient to the analyst.
Ordinary burette size will perhaps be the most suitable for routine
work; the tube is furnished with a stopcock and is bent at B, the tube
at K having a very small but not quite capillary bore. The lower end is
attached to a length of pressure-tubing, and is connected with a small
reservoir of mercury, moving up and down by means of a pulley. To use
the apparatus: Fill the tube with mercury by opening the clamp at H, and
the stopcock at B, and raising the reservoir until the mercury, if
allowed, would flow out of the beak. Now, the beak is dipped into the
liquid to be extracted with the solvent, and by lowering the reservoir,
a strong vacuum is created, which draws the liquid into the tube; in the
same way the ether is made to follow. Should the liquid be so thick that
it is not possible to get it in by means of suction, the lower end of
the tube is disconnected, and the syrupy mass worked in through the wide
end. When the ether has been sucked into the apparatus, it is emptied of
mercury by lowering the reservoir, and then firmly clamped at H, and the
stopcock also closed. The tube may now be shaken, and then allowed to
stand for the liquids to separate. When there is a good line of
demarcation, by raising the reservoir after opening the clamp and
stopcock, the whole of the light solvent can be run out of the tube into
a flask or beaker, and recovered by distillation. For heavy solvents
(such as chloroform), which sink to the bottom, a simple burette, with a
fine exit tube is preferable; but for petroleum ether, ordinary ether,
&c., the apparatus figured is extremely useful.
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