rmanganate solution, adding it directly to the
contents of the vacuum flask. Should the end-point be overstepped, the
ferrous sulphate solution may be added.
From the volume of the solution required to oxidize the iron in
the wire, calculate the relation to the normal of the permanganate
solution. The duplicate results should be concordant within two parts
in one thousand.
[Note 1: The funnel of the reductor must never be allowed to empty.
If it is left partially filled with water the reductor is ready for
subsequent use after a very little washing; but a preliminary test is
always necessary to safeguard against error.
If more than a small drop of permanganate solution is required to
color 100 cc. of the dilute acid after the reductor is well washed, an
allowance must be made for the iron in the zinc. !Great care! must be
used to prevent the access of air to the reductor after it has been
washed out ready for use. If air enters, hydrogen peroxide forms,
which reacts with the permanganate, and the results are worthless.]
[Note 2: The iron is reduced to the ferrous condition by contact with
the zinc. The active agent may be considered to be !nascent! hydrogen,
and it must be borne in mind that the visible bubbles are produced by
molecular hydrogen, which is without appreciable effect upon ferric
iron.
The rate at which the iron solution passes through the zinc should not
exceed that prescribed, but the rate may be increased somewhat when
the wash-water is added. It is well to allow the iron solution to run
nearly, but not entirely, out of the funnel before the wash-water
is added. If it is necessary to interrupt the process, the complete
emptying of the funnel can always be avoided by closing the stopcock.
It is also possible to reduce the iron by treatment with zinc in a
flask from which air is excluded. The zinc must be present in excess
of the quantity necessary to reduce the iron and is finally completely
dissolved. This method is, however, less convenient and more tedious
than the use of the reductor.]
[Note 3: The dilute sulphuric acid for washing must be warmed ready
for use before the reduction of the iron begins, and it is of the
first importance that the volume of acid and of wash-water should
be measured, and the volume used should always be the same in the
standardizations and all subsequent analyses.]
[Note 4: The end-point is more permanent in cold than hot solutions,
possibly because of a
|