After triturating the residue, easily accomplished in a porcelain
mortar, an excess of the strongest hydrochloric acid is added to the
dry salt, preferably in a tall beaker where there is less surface for
the escape of hydrochloric acid and from which the acid can be decanted
without disturbing the precipitated chlorid. If the salt has been
reduced to a very fine powder, by stirring energetically for a minute,
the hydrochloric acid will set free the perchloric acid and precipitate
the sodium as chlorid, which in a few minutes settles, leaving a clear
solution of the perchloric acid with the excess of hydrochloric acid.
The clear supernatant liquid is then decanted upon a gooch, through
which it may be rapidly drawn with the aid of suction, and the residue
retreated with the strongest hydrochloric acid, settled, and again
decanted, the salt being finally brought upon the filter where it is
washed with a little strong hydrochloric acid. A large platinum cone
will be found more convenient than the crucible, because of its greater
capacity and filtering surface. When the filter will not hold all the
sodium chlorid, the latter, after washing, may be removed by water or
by mechanical means, with precautions not to disturb the felt, which
is then ready for the remainder. Of course, if water is used, the felt
had better be washed with a little strong hydrochloric acid before
receiving another portion of the salt. This residue will be found to
contain only an inconsiderable amount of perchlorate, when tested by
first heating to expel the free acid and then treating the dry and
powdered residue with ninety-seven per cent alcohol, which dissolves
the perchlorate of sodium but has little soluble effect on the chlorid.
The filtrate, containing the perchloric acid with the excess of
hydrochloric acid and the small per cent of sodium chlorid which is
soluble in the latter, is then evaporated over the steam-bath till all
hydrochloric acid is expelled and the heavy white fumes of perchloric
acid appear, when it is ready for use in potassium determinations.
Evidently the acid will not be chemically pure because the sodium
chlorid is not absolutely insoluble in hydrochloric acid; but a portion
tested with silver nitrate will prove that the sodium, together with
any other bases which may have gone through the filter, has been
completely converted into perchlorate, and unless the original chlorate
contained some potassium or on evaporation the acid was exposed to
the fumes of ammonia, the residue of the evaporation of a portion is
easily and completely soluble in ninety-seven per cent alcohol and its
presence is therefore unobjectionable. One cubic centimeter of the acid
thus obtained gives on evaporation a residue of only 0.036 gram, which
is completely soluble in ninety-seven per cent alcohol.
Public-domain text, read in full here on John Shaqi.
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