n most common use are iron wire, ferrous ammonium sulphate, sodium
oxalate, oxalic acid, and some other derivatives of oxalic acid.
With the exception of sodium oxalate, these all contain water of
crystallization which may be lost on standing. They should, therefore,
be freshly prepared, and with great care. At present, sodium oxalate
is considered to be one of the most satisfactory standards.
!Method A!
!Iron Standards!
The standardization processes employed when iron or its compounds are
selected as standards differ from those applicable in connection with
oxalate standards. The procedure which immediately follows is that in
use with iron standards.
As in the case of the bichromate process, it is necessary to reduce
the iron completely to the ferrous condition before titration. The
reducing agents available are zinc, sulphurous acid, or sulphureted
hydrogen. Stannous chloride may also be used when the titration is
made in the presence of hydrochloric acid. Since the excess of both
the gaseous reducing agents can only be expelled by boiling, with
consequent uncertainty regarding both the removal of the excess and
the reoxidation of the iron, zinc or stannous chlorides are the most
satisfactory agents. For prompt and complete reduction it is essential
that the iron solution should be brought into ultimate contact with
the zinc. This is brought about by the use of a modified Jones
reductor, as shown in Figure 1. This reductor is a standard apparatus
and is used in other quantitative processes.
[Illustration: Fig. 1]
The tube A has an inside diameter of 18 mm. and is 300 mm. long; the
small tube has an inside diameter of 6 mm. and extends 100 mm. below
the stopcock. At the base of the tube A are placed some pieces of
broken glass or porcelain, covered by a plug of glass wool about 8 mm.
thick, and upon this is placed a thin layer of asbestos, such as is
used for Gooch filters, 1 mm. thick. The tube is then filled with the
amalgamated zinc (Note 1) to within 50 mm. of the top, and on the zinc
is placed a plug of glass wool. If the top of the tube is not already
shaped like the mouth of a thistle-tube (B), a 60 mm. funnel is fitted
into the tube with a rubber stopper and the reductor is connected
with a suction bottle, F. The bottle D is a safety bottle to
prevent contamination of the solution by water from the pump. After
preparation for use, or when left standing, the tube A should be
filled with water,
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