An Introductory Course of Quantitative Chemical Analysis: With Explanatory NotesTalbot, Henry Paul
Science
An Introductory Course of Quantitative Chemical Analysis: With Explanatory Notes
Talbot, Henry Paul
Chemistry, Analytic -- Quantitative
PROCEDURE.--Fill a glass-stoppered burette with the permanganate
solution, observing the usual precautions, and fill a second burette
with the ferrous sulphate solution prepared for use with the potassium
bichromate. The permanganate solution cannot be used in burettes with
rubber tips, as a reduction takes place upon contact with the rubber.
The solution has so deep a color that the lower line of the meniscus
cannot be detected; readings must therefore be made from the upper
edge. Run out into a beaker about 40 cc. of the ferrous solution,
dilute to about 100 cc., add 10 cc. of dilute sulphuric acid, and run
in the permanganate solution to a slight permanent pink. Repeat, until
the ratio of the two solutions is satisfactorily established.
STANDARDIZATION OF A POTASSIUM PERMANGANATE SOLUTION
!Selection of a Standard!
Commercial potassium permanganate is rarely sufficiently pure to admit
of its direct weighing as a standard. On this account, and because
of the uncertainties as to the permanence of its solutions, it is
advisable to standardize them against substances of known value. Those
in 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]
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