By H SCHÆPPI.
Ten grms. of sulphur, pulverized as finely as possible, are covered
with hot water and a few drops of nitric acid digested for some time,
filtered, and washed till the washings have no longer an acid reaction.
Thus calcium chloride and sulphate are removed, and calcium sulphide, if
present, is destroyed. The sulphur thus prepared is covered with water
at 70° to 80°, a few drops of ammonia are added, and the mixture is
digested for a quarter of an hour. All the arsenic present as sulphide
is dissolved, and the ammoniacal liquid is variously treated
according to the degree of accuracy required. For perfectly accurate
determinations the ammoniacal solution is mixed with silver nitrate, and
all the sulphur present in the state of arsenic sulphide is thrown down
as silver sulphide, acidified with nitric acid, filtered, and washed.
The precipitate of silver sulphide is dissolved in hot nitric acid and
determined as silver chloride. From the weight of the latter the arsenic
sulphide is calculated. As a less accurate but more rapid method, the
ammoniacal solution of arsenic sulphide is cautiously neutralized with
pure dilute nitric acid and considerably diluted. It is then titrated
with decinormal silver nitrate till a drop of the solution is turned
brown with neutral chromate. The arsenic is easily calculated from the
quantity of silver nitrate consumed. For very rough determinations it is
sufficient to treat ten grms. of finely-ground sulphur with nitric acid,
to extract with ammonia, and to add silver nitrate. From the intensity
of the color, or the quantity of the precipitate of silver sulphide,
it may be judged if the sulphur is approximately free from arsenic or
strongly contaminated. The author states that, contrary to the general
belief, reddish yellow sulphur is more free from arsenic than such as is
of a full yellow color.
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