ece of glazed paper and brushing the precipitate from the
smaller piece into it, sweeping off all particles belonging to the
determination.
Moisten the precipitate with two drops of concentrated nitric acid and
one drop of concentrated hydrochloric acid, and again heat with great
caution until the acids are expelled and the precipitate is white,
when the temperature is slowly raised until the silver chloride just
begins to fuse at the edges (Note 3). The crucible is then cooled in a
desiccator and weighed, after which the heating (without the addition
of acids) is repeated, and it is again weighed. This must be continued
until the weight is constant within 0.0003 gram in two consecutive
weighings. Deduct the weight of the crucible, and calculate the
percentage of chlorine in the sample of sodium chloride taken for
analysis.
[Note 1: The separation of the silver chloride from the filter is
essential, since the burning carbon of the paper would reduce a
considerable quantity of the precipitate to metallic silver, and its
complete reconversion to the chloride within the crucible, by means of
acids, would be accompanied by some difficulty. The small amount of
silver reduced from the chloride adhering to the filter paper after
separating the bulk of the precipitate, and igniting the paper
as prescribed, can be dissolved in nitric acid, and completely
reconverted to chloride by hydrochloric acid. The subsequent addition
of the two acids to the main portion of the precipitate restores the
chlorine to any chloride which may have been partially reduced by the
sunlight. The excess of the acids is volatilized by heating.]
[Note 2: The platinum wire is wrapped around the top of the filter
during its incineration to avoid contact with any reduced silver from
the reduction of the precipitate. If the wire were placed nearer the
apex, such contact could hardly be avoided.]
[Note 3: Silver chloride should not be heated to complete fusion,
since a slight loss by volatilization is possible at high
temperatures. The temperature of fusion is not always sufficient
to destroy filter shreds; hence these should not be allowed to
contaminate the precipitate.]
DETERMINATION OF IRON AND OF SULPHUR IN FERROUS AMMONIUM SULPHATE,
FESO_{4}.(NH_{4})_{2}SO_{4}.6H_{2}O
DETERMINATION OF IRON
PROCEDURE.--Weigh out into beakers (200-250 cc.) two portions of the
sample (Note 1) of about 1 gram each and dissolve these in 50 cc. of
w
|