Caspari’s acid under similar treatment gave a residue in one case
of 0.024 gram and in another 0.047 gram. If, however, a portion of
pure acid be required, it may be obtained by distilling this product
under diminished pressure and, as Caspari has shown, without great
loss providing the heat is regulated according to the fumes in the
distilling flask.
Some modification of the above treatment will be found necessary in
case the sodium chlorate contains any potassium as an impurity, or if
the latter has been introduced from the vessel in which the fusion was
made. In these circumstances the hydrochloric acid would not suffice
for the removal of potassium, since a trace might also go over with
the sodium and thus on evaporation a residue insoluble in ninety-seven
per cent alcohol be obtained. To avoid this difficulty, the mixture of
sodium perchlorate and chlorid, after treating with hydrochloric acid
for the reduction of the residual chlorate, being reduced to a fine
powder, is well digested with ninety-seven per cent alcohol, which
dissolves the sodium perchlorate but leaves the chlorid, as well as
any potassium salt insoluble. By giving the alcohol time to become
saturated, which was facilitated by stirring, it was found on filtering
and evaporating that an average of about two-tenths of a gram of sodium
perchlorate are obtained for every cubic centimeter of alcohol and that
the product thus obtained is comparatively free of chlorids, until the
perchlorate is nearly all removed, when more of the chlorid seems to
dissolve. This treatment with alcohol is continued until on evaporation
of a small portion of the latest filtrate, only a small residue is
found. The alcoholic solution of the perchlorate is then distilled from
a large flask until the perchlorate begins to crystallize, when the
heat is removed and the contents quickly emptied into an evaporating
dish, the same liquid being used to wash out the remaining portions of
the salt. When the distillation is terminated at the point indicated,
the distillate will contain most of the alcohol employed, but in a
somewhat stronger solution, so that it requires only diluting to
ninety-seven per cent to fit it for use in future preparations. The
salt is then evaporated to dryness on the steam-bath and subsequently
treated with strong hydrochloric acid for the separation of the
perchloric acid.
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