The precipitate is collected on a filter, washed, and dissolved in
caustic potash. The solution is saturated with hydrogen sulfid, and
on adding acetic acid in slight excess the tin sulfid is separated
and removed by filtration. The whole of the phosphoric acid, supposed
to be almost free of tin, is now found in the filtrate. The filtrate
is concentrated to small bulk and any tin sulfid present separated by
filtering, and the phosphoric acid finally removed from the ammoniacal
filtrate by precipitation with magnesia mixture. The chief difficulties
of this method are to be found, on the one hand, in the retention
of some of the phosphoric acid by the iron and alumina which may be
present, and on the other, in the presence of some tin in the final
magnesium pyrophosphate. If the tin be all removed as sulfid, the
latter source of error will be avoided. It is difficult to secure pure
metallic tin, and this is another disturbing element in the process.
It can not be recommended for the work which agricultural analysts are
usually called on to perform.[38]
=49. Water-Soluble Phosphoric Acid.=—The method of procedure
recommended by the Association of Official Chemists is as follows:[39]
Place two grams of the sample in a nine centimeter filter; wash with
successive small portions of cold water, allowing each portion to pass
through before adding more, until the filtrate measures about 250 cubic
centimeters. If the filtrate be turbid, add a little nitric acid. Make
up to any convenient definite volume; mix well; take any convenient
portion and proceed as under total phosphoric acid.
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