This final solution is nearly neutralized, as before; a little sodium
carbonate solution is added; it is heated to boiling and an excess
of solution of calcium chlorid is added. The precipitate of calcium
fluorid and carbonate must be boiled for a few minutes, when it can
be easily filtered and washed with hot water. The precipitate is then
washed from the filter into a small platinum dish and evaporated to
dryness, while the filter, after being partially dried and used to wipe
off any particles of the precipitate adhering to the dish in which it
was formed, is burned, and the ash is added to the main precipitate.
This, when dry, is ignited, and allowed to cool; dilute acetic acid is
added in excess, and the whole is evaporated to dryness, being kept
on the water-bath until all odor of acetic acid has disappeared. The
residue is then treated with hot water, digested, filtered on a small
filter, washed with hot water, partially dried, put into a crucible,
carefully ignited, and weighed as calcium fluorid. The calcium fluorid
is then dissolved in sulfuric acid by gentle heating and agitation,
evaporated to dryness on a radiator, ignited at full red heat, and
weighed as calcium sulfate. From this weight the equivalent weight of
calcium fluorid should be calculated, and this should be very close
to that actually found as above, but should never exceed it. The
difference, which is generally about a milligram (sometimes more), is
due to silica precipitated with the fluorid. The percentage of fluorin
is, therefore, always calculated from the weight of the sulfate, and
not from that of the fluorid obtained.
The main improvements in this method are the use of sodium bicarbonate
to separate the silica, and the keeping of the earlier solutions as
dilute as possible, which can not be done, if ammonium carbonate be
used for the separation of the silica. These changes make the fluorin
estimation, although still tedious, far more rapid than before, and the
results are very satisfactory.
=46. Modification of Wyatt.=—By reason of the tediousness of the method
of Chatard given above, Wyatt has sought to shorten the process by the
following modification:[35]
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