Legal Chemistry: A Guide to the Detection of Poisons, Examination of Tea, Stains, Etc., as Applied to Chemical JurisprudenceNaquet, Alfred
Science
Legal Chemistry: A Guide to the Detection of Poisons, Examination of Tea, Stains, Etc., as Applied to Chemical Jurisprudence
Naquet, Alfred
Chemistry, Forensic; Poisons
_Remark._--In the operations described above, as well as in those
following, the difficulty in separating minute precipitates from the
filter is often experienced. When the precipitate is to be dissolved in
reagents that do not affect the paper, such as ammonia, tartrate of
ammonia, and dilute acids, it can be brought in solution directly on the
filter. In cases, however, where reagents which attack the paper are
employed, the precipitate should be separated. This is accomplished by
mixing a small quantity of pure silica, obtained by the decomposition of
fluoride of silicium by water, with the solution, before filtering. The
precipitate becomes intimately mixed with the silica, and can then be
readily removed from the paper. The presence of silica does not
interfere, it being insoluble in the reagents commonly made use of.
TREATMENT OF FILTRATE B.
A current of sulphuretted hydrogen is conducted for twelve hours through
the solution, which is kept at a temperature of 70°. by means of a
water-bath. The flask containing the liquid is then closed with a piece
of paper, and allowed to remain in a moderately warm place until the
odor of the gas is no longer perceptible. The solution is next filtered
with the precaution mentioned in the preceding remark, and the
precipitate (_a_) thoroughly washed. The water used in this operation is
united to the filtrate, and the fluid (_b_) examined as directed further
on.
TREATMENT OF PRECIPITATE _a_.
In order to free the precipitate from the organic substances possibly
present, at the same time avoiding a loss of any metal, it is dried,
moistened with nitric acid, and the mass heated on a water-bath. Some
Swedish filtering paper is next added, the mixture well impregnated with
sulphuric acid, and then maintained for several hours at a temperature
of about 170°. until a small portion (afterwards returned) gives a
colorless solution when treated with water. The residue is now heated
with a mixture of one part of hydrochloric acid and eight parts of
water, the liquid filtered, the matter remaining undissolved washed with
dilute hydrochloric acid, and the washings united with the filtrate.
The residue I. and the solution II. are separately examined as directed
below.
RESIDUE I.
This may contain lead, mercury, tin, bismuth and antimony. It is heated
for a considerable time with _aqua regia_, the solution filtered, and
the second residue, should one remain, washed with dilute hydrochloric
acid. If the second residue is fused with cyanide of potassium, the
compounds present are reduced to the metallic state. The liberated
metals are treated with nitric acid, which dissolves _lead_, but leaves
_tin_ as insoluble metastannic acid. The nitrate of lead is then
filtered from the metastannic acid, and both metals are identified as
described in the treatment of residue A.
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