measuring flask
(Note 2). Fill the flask to the mark with water and shake thoroughly.
Measure off 25 cc. of this semi-solution in a measuring flask, or
pipette, observing the precaution that the liquid removed shall
contain approximately its proportion of suspended matter.
Empty the flask or pipette into a beaker and wash it out. Run in the
arsenite solution from a burette until no further reaction takes place
on the starch-iodide paper when touched by a drop of the solution of
bleaching powder. Repeat the titration, using a second 25 cc. portion.
From the volume of solution required to react with the bleaching
powder, calculate the percentage of available chlorine in the latter,
assuming the titration reaction to be that between chlorine and
arsenious oxide:
As_{4}O_{6} + 4Cl_{2} + 4H_{2}O --> 2As_{2}O_{5} + 8HCl
Note that only one twentieth of the original weight of bleaching
powder enters into the reaction.
[Note 1: The powder must be triturated until it is fine, otherwise the
lumps will inclose calcium hypochlorite, which will fail to react with
the arsenious acid. The clear supernatant liquid gives percentages
which are below, and the sediment percentages which are above, the
average. The liquid measured off should, therefore, carry with it its
proper proportion of the sediment, so far as that can be brought about
by shaking the solution just before removal of the aliquot part for
titration.]
[Note 2: Bleaching powder is easily acted upon by the carbonic acid in
the air, which liberates the weak hypochlorous acid. This, of course,
results in a loss of available chlorine. The original material for
analysis should be kept in a closed container and protected form the
air as far as possible. It is difficult to obtain analytical samples
which are accurately representative of a large quantity of the
bleaching powder. The procedure, as outlined, will yield results which
are sufficiently exact for technical purposes.]
III. PRECIPITATION METHODS
DETERMINATION OF SILVER BY THE THIOCYANATE PROCESS
The addition of a solution of potassium or ammonium thiocyanate to one
of silver in nitric acid causes a deposition of silver thiocyanate as
a white, curdy precipitate. If ferric nitrate is also present, the
slightest excess of the thiocyanate over that required to combine with
the silver is indicated by the deep red which is characteristic of the
thiocyanate test for iron.
The reactions involve
|