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
The actual process is as follows:--10 grms. of the sample are
weighed out and run into a litre flask, water added, and the mixture
shaken. The flask being finally filled up to the neck, some of the
solution is now filtered through a dry filter, and 10 c.c. of this
filtrate is placed in a 6 or 8-ounce stoppered bottle, and 30 c.c.
of the alum solution added. In a similar bottle 10 c.c. of the
standard solution of carbolic acid are placed, and a similar
quantity of alum solution is added, as in the first bottle. The
bromine-water is now run into the bottle containing the standard
solution of carbolic acid from a burette until there is no further
precipitate; the bottle is stoppered and shaken after every
addition. Towards the end of the reaction the precipitate forms but
slowly, and when the carbolic acid is saturated, the slight excess
of bromine-water gives the solution a pale yellow tint. The solution
from the sample is treated in the same way, and from the amount of
bromine-water used, the percentage of the sample is obtained by
making the usual calculations. Thus, supposing that 5 c.c. of the
standard required 15 c.c. of the bromine-water for precipitation,
and 10 c.c. of the solution of the sample required 17 c.c., the
calculation would be 15 × 2 : 17 = 100 : _x_ per cent. With most
samples of crude carbolic acid, the precipitate does not readily
separate. It is then best to add a little of the precipitate already
obtained by testing the standard solution, which rapidly clears the
liquid.
=Koppeschaar’s volumetric method= is more exact, but also more
elaborate, than the one just described. Caustic normal soda is
treated with bromine until permanently yellow, and the excess of
bromine is then driven off by boiling. The liquid now contains 5NaBr
+ NaBrO₃, and on adding this to a solution containing carbolic acid,
and a sufficient quantity of hydrochloric acid to combine with the
sodium, the following reactions occur:--
(1.) 5NaBr + NaBrO₃ + 6HCl = 6NaCl + 6Br + 3H₂O;
and
(2.) C₆H₆O + 6Br = C₆H₃Br₃O + 3HBr.
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