the acid obtained depends chiefly on the purity of the hydrofluosilicic
acid at first used. Hence to get good results this acid must be free
from foreign bodies. If an absolutely pure product be desired the acid
above obtained must be distilled in a vacuum.
=272. Method of Kreider.=—Kreider has worked out a simpler method of
preparing perchloric acid which will make it easy for every analyst to
make and keep a supply of this admirable yet unappreciated reagent.
This method is conducted as follows:[227]
A convenient quantity of sodium chlorate, from 100 to 300 grains,
is melted in a glass retort or round-bottomed flask and gradually
raised to a temperature at which oxygen is freely, but not too rapidly
evolved, and kept at this temperature till the fused mass thickens
throughout, indicating the complete conversion of the chlorate to the
chlorid and perchlorate, which requires from one and one-half to two
hours: or the retort may be connected with a gasometer and the end of
the reaction determined by the volume of oxygen expelled, according to
the equation
2NAClO₃ = NACl + NAClO₄ + O₂.
The product thus obtained is washed from the retort to a capacious
evaporating dish where it is treated with sufficient hydrochloric acid
to effect the complete reduction of the residual chlorate, which, if
the ignition has been carefully conducted with well distributed heat,
will be present in but small amount. It is then evaporated to dryness
on the steam-bath, or more quickly over a direct flame, and with but
little attention until a point near to dryness has been reached,
when stirring will be found of great advantage in facilitating the
volatilization of the remaining liquid and in breaking up the mass
of salt. Otherwise the perchlorate seems to solidify with a certain
amount of water and its removal from the dish, without moistening and
reheating, is impossible.
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