Wyatt recommends that two grams of the fine material be heated in
ground watch-glasses, the edges of which are separated so as to allow
the escape of the moisture.[14] The heating is continued for three
hours at 110°, the watch-glasses then closed and held by the clip,
cooled in a desiccator, and weighed. This method is excellent for very
hygroscopic bodies, but where quick-acting balances are used, scarcely
necessary for a powdered mineral.
The residue from the moisture determination is gradually heated to
full redness over a bunsen, and then ignited over the blast-lamp.
This operation is repeated after weighing until a constant weight is
obtained. The loss (after deducting the percentage of carbon dioxid as
found in another portion) may be taken as water and organic matter.
This method is sufficient for all practical purposes; but when minerals
containing fluorin are strongly ignited, a part of the fluorin is
expelled; hence, if more accurate determinations are required, the loss
of fluorin must be taken into account. In this laboratory it has been
proved that a pure calcium fluorid undergoes progressive decomposition
at a bright red heat with formation of lime.
Wyatt directs that the combined water and organic matters be determined
in the residue from the moisture estimation as follows: The residue is
brushed into a weighed platinum crucible, which is heated over a small
bunsen for ten minutes and then brought to full heat of a blast-lamp
for five minutes. After cooling, the total loss is determined by
weighing. After deducting the carbon dioxid determined in a separate
portion, the residual loss is regarded as due to combined moisture and
organic matter.
=25. Carbon Dioxid.=—Many forms of compact apparatus have been devised
for this estimation, but none of them is satisfactory if accurate
results are desired.[15] Not to mention other objections, many
phosphates must be heated nearly to the boiling-point with dilute acid
to effect complete decomposition of the carbonates. The distillation
method described by Gooch[16] is excellent, and when once the apparatus
is set up, its work will be found to be rapid and satisfactory.
Wyatt regards the estimation of carbon dioxid as one of the most
important for factory use. The carbonates present in a sample indicate
the loss of an equivalent amount of acid in the process of conversion
into superphosphate.[17]
The apparatus employed for estimating carbon dioxid may be any one of
those in ordinary use for this purpose. The principle of the process
depends on the liberation of the gas with a mineral acid, its proper
desiccation, and subsequent absorption by a caustic alkali, best in
solution.
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