lor)
with ferrous compounds as long as there are unoxidized ferrous ions in
the titrated solution. Drops of the indicator solution are placed upon
a glazed porcelain tile, or upon white cardboard which has been coated
with paraffin to render it waterproof, and drops of the titrated
solution are transferred to the indicator on the end of a stirring
rod. When the oxidation is nearly completed only very small amounts
of the ferrous compounds remain unoxidized and the reaction with the
indicator is no longer instantaneous. It is necessary to allow a brief
time to elapse before determining that no blue color is formed. Thirty
seconds is a sufficient interval, and should be adopted throughout the
analytical procedure. If left too long, the combined effect of light
and dust from the air will cause a reduction of the ferric compounds
already formed and a resultant blue will appear which misleads the
observer with respect to the true end-point.
The indicator solution must be highly diluted, otherwise its own color
interferes with accurate observation. Prepare a fresh solution, as
needed each day, by dissolving a crystal of potassium ferricyanide
about the size of a pin's head in 25 cc. of distilled water. The salt
should be carefully tested with ferric chloride for the presence of
ferrocyanides, which give a blue color with ferric salts.
In case of need, the ferricyanide can be purified by adding to its
solution a little bromine water and recrystallizing the compound.
COMPARISON OF OXIDIZING AND REDUCING SOLUTIONS
PROCEDURE.--Fill one burette with each of the solutions, observing
the general procedure with respect to cleaning and rinsing already
prescribed. The bichromate solution is preferably to be placed in a
glass-stoppered burette.
Run out from a burette into a beaker of about 300 cc. capacity nearly
40 cc. of the ferrous solution, add 15 cc. of dilute hydrochloric acid
(sp. gr. 1.12) and 150 cc. of water and run in the bichromate
solution from another burette. Since both solutions are approximately
tenth-normal, 35 cc. of the bichromate solution may be added without
testing. Test at that point by removing a very small drop of the
iron solution on the end of a stirring rod, mixing it with a drop of
indicator on the tile (Note 1). If a blue precipitate appears at once,
0.5 cc. of the bichromate solution may be added before testing again.
The stirring rod which has touched the indicator should be dipped in
distil
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