An Introductory Course of Quantitative Chemical Analysis: With Explanatory NotesTalbot, Henry Paul
Science
An Introductory Course of Quantitative Chemical Analysis: With Explanatory Notes
Talbot, Henry Paul
Chemistry, Analytic -- Quantitative
PROCEDURE.--Weigh out, into platinum crucibles, two portions of about
0.5 gram of the sulphate. Mix each in the crucible with five to six
times its weight of anhydrous sodium carbonate. This can best be done
by placing the crucible on a piece of glazed paper and stirring the
mixture with a clean, dry stirring-rod, which may finally be wiped off
with a small fragment of filter paper, the latter being placed in the
crucible. Cover the crucible and heat until a quiet, liquid fusion
ensues. Remove the burner, and tip the crucible until the fused mass
flows nearly to its mouth. Hold it in that position until the mass has
solidified. When cold, the material may usually be detached in a lump
by tapping the crucible or gently pressing it near its upper edge. If
it still adheres, a cubic centimeter or so of water may be placed in
the cold crucible and cautiously brought to boiling, when the cake
will become loosened and may be removed and placed in about 250 cc.
of hot, distilled water to dissolve. Clean the crucible completely,
rubbing the sides with a rubber-covered stirring-rod, if need be.
When the fused mass has completely disintegrated and nothing further
will dissolve, decant the solution from the residue of barium
carbonate (Note 1). Pour over the residue 20 cc. of a solution of
sodium carbonate and 10 cc. of water and heat to gentle boiling for
about three minutes (Note 2). Filter off the carbonate and wash it
with hot water, testing the slightly acidified washings for sulphate
and preserving any precipitates which appear in these tests. Acidify
the filtrate with hydrochloric acid until just acid, bring to boiling,
and slowly add hot barium chloride solution, as in the preceding
determination. Add also any tests from the washings in which
precipitates have appeared. Filter, wash, ignite, and weigh.
From the weight of barium sulphate, calculate the percentage of
sulphur (S) in the sample.
[Note 1: This alkaline fusion is much employed to disintegrate
substances ordinarily insoluble in acids into two components, one
of which is water soluble and the other acid soluble. The reaction
involved is:
BaSO_{4} + Na_{2}CO_{3}, --> BaCO_{3}, + Na_{2}SO_{4}.
As the sodium sulphate is soluble in water, and the barium carbonate
insoluble, a separation between them is possible and the sulphur can
be determined in the water-soluble portion.
It should be noted that this method can be applied to the purification
of a precipitate of barium sulphate if contaminated by most of the
substances mentioned in Note 3 on page 114. The impurities pass into
the water solution together with the sodium sulphate, but, being
present in such minute amounts, do not again precipitate with the
barium sulphate.]
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