Legal Chemistry: A Guide to the Detection of Poisons, Examination of Tea, Stains, Etc., as Applied to Chemical JurisprudenceNaquet, Alfred
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Legal Chemistry: A Guide to the Detection of Poisons, Examination of Tea, Stains, Etc., as Applied to Chemical Jurisprudence
Naquet, Alfred
Chemistry, Forensic; Poisons
Otto also recommends the agitation of the fluid containing the oxalates
or tartrates of the alkaloids with ether, previously to their separation
by means of bicarbonate of soda. By this treatment the elimination of
the coloring matter present--as well as of _colchicine_, _digitaline_,
_picrotoxine_, traces of _atropine_, and various impurities--is
accomplished. As soon as the ether ceases to become colored and to leave
a residue upon evaporation, alkali is added, and the operation concluded
as usual. In this way the alkaloid is obtained, almost directly, in a
pure condition. This last modification appears to us to be a very happy
one, inasmuch as it greatly facilitates the purification of the alkaloid
present.
MODIFICATIONS TO STAS'S METHOD, PROPOSED BY USLAR AND ERDMAN.
1st. The materials to be examined are brought to the consistence of a
thin paste, and digested for about two hours with water, to which some
hydrochloric acid has been added, at a temperature of 60° to 80°. The
mixture is then filtered through a moistened linen cloth, and the
residue washed with warm acidulated water; the washings being added to
the solution.
2nd. Some pure quartz sand--or, preferably, silica prepared by the
decomposition of fluoride of silicium--is added to the filtrate, the
fluid supersaturated with ammonia, and evaporated to dryness over a
water-bath: the addition of silica renders the residue friable.
3rd. The residue is boiled repeatedly with amylic alcohol, which
extracts all the alkaloid present as well as the fatty and coloring
matters, and the extracts filtered through filter paper that has been
moistened with amylic alcohol.
4th. The filtered fluid is thoroughly agitated with ten or twelve times
its volume of almost boiling water acidulated with hydrochloric acid:
the hydrochlorate of the alkaloid present goes into the aqueous
solution, the fatty and coloring substances remaining dissolved in the
oily supernatant layer. The latter is separated by means of a pipette,
and the acid aqueous solution shaken with fresh quantities of amylic
alcohol until completely decolorized.
5th. The aqueous solution is then concentrated, ammonia added, and the
mixture well shaken with warm amylic alcohol, in which the alkaloid
dissolves. As soon as the solution forms a supernatant layer upon the
surface of the fluid, it is drawn off with a pipette and evaporated on a
water-bath. In this manner, the alkaloid is usually obtained in a
sufficient state of purity to admit of its immediate identification; if,
however, a small portion turns brown when treated with concentrated
sulphuric acid, the process of purification must be repeated. Under
these circumstances it is re-dissolved in dilute hydrochloric acid, the
solution repeatedly shaken with amylic alcohol, in order to extract the
impurities present, and the alkaloid then extracted with ammonia and
amylic alcohol, as previously directed.
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