tions
serves to oxidize any ferrous hydroxide to ferric hydroxide and to
precipitate manganese as MnO(OH)_{2}. The solution must contain not
more than a bare excess of hydroxyl ions (ammonium hydroxide) when it
is filtered, on account of the tendency of the aluminium hydroxide to
redissolve.
The solution should not be strongly ammoniacal when the bromine is
added, as strong ammonia reacts with the bromine, with the evolution
of nitrogen.]
[Note 2: The precipitate produced by ammonium hydroxide and bromine
should be filtered off promptly, since the alkaline solution absorbs
carbon dioxide from the air, with consequent partial precipitation
of the calcium as carbonate. This is possible even under the most
favorable conditions, and for this reason the iron precipitate is
redissolved and again precipitated to free it from calcium. When the
precipitate is small, this reprecipitation may be omitted.]
[Note 3: In the absence of significant amounts of manganese the iron
and aluminium may be separately determined by fusion of the mixed
ignited precipitate, after weighing, with about ten times its weight
of acid potassium sulphate, solution of the cold fused mass in water,
and volumetric determination of the iron, as described on page 66.
The aluminium is then determined by difference, after subtracting the
weight of ferric oxide corresponding to the amount of iron found.
If a separate determination of the iron, aluminium, and manganese
is desired, the mixed precipitate may be dissolved in acid before
ignition, and the separation effected by special methods (see, for
example, Fay, !Quantitative Analyses!, First Edition, pp. 15-19 and
23-27).]
DETERMINATION OF CALCIUM
PROCEDURE.--To the combined filtrates from the double precipitation of
the hydroxides just described, add 5 cc. of dilute ammonium hydroxide
(sp. gr. 0.96), and transfer the liquid to a 500 cc. graduated flask,
washing out the beaker carefully. Cool to laboratory temperature, and
fill the flask with distilled water until the lowest point of the
meniscus is exactly level with the mark on the neck of the flask.
Carefully remove any drops of water which are on the inside of the
neck of the flask above the graduation by means of a strip of filter
paper, make the solution uniform by pouring it out into a dry beaker
and back into the flask several times. Measure off one fifth of this
solution as follows (Note 1): Pour into a 100 cc. graduated flask
a
|