be kept covered as much as possible and the lid carefully
cleaned.]
[Note 5: A gritty residue remaining after the disintegration of
the fused mass by acid indicates that the substance has been but
imperfectly decomposed. Such a residue should be filtered, washed,
dried, ignited, and again fused with the alkaline flux; or, if the
quantity of material at hand will permit, it is better to reject the
analysis, and to use increased care in grinding the mineral and in
mixing it with the flux.]
DEHYDRATION AND FILTRATION
PROCEDURE.--Evaporate the solution of the fusion to dryness, stirring
frequently until the residue is a dry powder. Moisten the residue with
5 cc. of strong hydrochloric acid (sp. gr. 1.20) and evaporate again
to dryness. Heat the residue for at least one hour at a temperature
of 110 deg.C. (Note 1). Again moisten the residue with concentrated
hydrochloric acid, warm gently, making sure that the acid comes into
contact with the whole of the residue, dilute to about 200 cc. and
bring to boiling. Filter off the silica without much delay (Note 2),
and wash five times with warm dilute hydrochloric acid (one part
dilute acid (1.12 sp. gr.) to three parts of water). Allow the filter
to drain for a few moments, then place a clean beaker below the funnel
and wash with water until free from chlorides, discarding these
washings. Evaporate the original filtrate to dryness, dehydrate at
110 deg.C. for one hour (Note 3), and proceed as before, using a second
filter to collect the silica after the second dehydration. Wash this
filter with warm, dilute hydrochloric acid (Note 4), and finally with
hot water until free from chlorides.
[Note 1: The silicic acid must be freed from its combination with
a base (sodium, in this instance) before it can be dehydrated.
The excess of hydrochloric acid accomplishes this liberation. By
disintegrating the fused mass with a considerable volume of dilute
acid the silicic acid is at first held in solution to a large extent.
Immediate treatment of the fused mass with strong acid is likely
to cause a semi-gelatinous silicic acid to separate at once and to
inclose alkali salts or alumina.
A flocculent residue will often remain after the decomposition of the
fused mass is effected. This is usually partially dehydrated silicic
acid and does not require further treatment at this point. The
progress of the dehydration is indicated by the behavior of the
solution, which as evaporation
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