When the mixture submitted for examination consists of bodies perfectly
soluble and perfectly insoluble, simple filtration may suffice to secure
their separation; but this is rarely the case, some colloidal material
being ordinarily mixed with the crystalloid, and the plan of separating
them by _dialysis_, as proposed by Graham, not being altogether
successful. When the substances looked for are volatile, distillation
may be employed to secure them in a state of purity; in this way
prussic acid is separated; but in the case of the poisonous alkaloids
other means must be adopted.
I. In the separation of such an alkaloid as strychnia, for example, the
suspected material is first of all acidulated by one of the weaker
mineral or stronger vegetable acids (hydrochloric acid is best), and the
whole carefully heated over a water bath. After a time this mixture is
to be filtered, and the filtrate well washed with boiling distilled
water, and the filtered fluid subjected to evaporation. When dry the
substance is to be rubbed up with distilled water, and again filtered;
this process to be repeated until a tolerably pure product be obtained.
This is next to be neutralized by hydrogen sodium carbonate, or
bicarbonate of soda, and the freed alkaloid taken up by rubbing or
shaking it with chloroform or ether, and the whole set aside in a
well-corked tall test tube. Finally, the ether or chloroform containing
the alkaloid is to be removed by a pipette and allowed to evaporate
spontaneously, when the alkaloid will probably be left behind in a state
fit for testing. This process is a modification of that invented by
Stas, in following out the case of the Count Bocarmé.
II. For the destruction of organic matter in the search for an inorganic
poison, such as arsenic, a process introduced by Fresenius and Von Babo
is commonly employed. Its essentials are as follows: The organic matter
is to be reduced to as fine shreds as possible, and mixed with about
one-eighth of its bulk of pure hydrochloric acid. This is to be heated,
and, as it boils, from time to time crystals of potassic chlorate are
added, until the solids are reduced to a straw-yellow fluid. This is
next treated with hydrogen sodium sulphite, or bisulphate of soda,
until a distinct smell of sulphurous acid is given off, after which
sulphuretted hydrogen is to be passed through the fluid, concentrated if
necessary, for some hours, thus throwing down most metallic poisons in
the form of sulphide. This precipitate is to be collected and further
tested.
When exceedingly small quantities are dealt with the microscope is of
use, and the plan of subliming alkaloids and examining their crystals
under the microscope, introduced by Guy and Helwig, will be found very
useful. The shape of crystalline poisons is a valuable means of
determining their identity; arsenic and antimony may thus be readily
distinguished, as may other well known substances.
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