The hydrochloric acid solution of the phosphate must contain no free
chlorin and is treated with a few drops of a methyl orange solution.
Ammonia is added until nearly neutral, but the acid reaction is
retained as shown by the indicator. A few cubic centimeters of ammonium
acetate are added, which produce a yellow coloration of the liquid and
also a complete precipitation of the iron and aluminum phosphates when
warmed to 70°. At this temperature the precipitation of any calcium
phosphate is avoided. A small quantity of the lime may be carried down
mechanically and therefore the precipitate should be dissolved in
hydrochloric acid and the precipitation again made as above after the
addition of some sodium phosphate. If the original solution contain
any free chlorin, as may be the case when aqua regia is employed as
solvent, before beginning the separation, ammonia should be added in
slight excess and the acidity restored by hydrochloric after adding
the indicator. In washing the precipitates, water of not over 70°
must be used. As has been shown by Hess in the work cited in the
next paragraph, the statement of C. Glaser to the effect that the
precipitates obtained as above are free of lime has not been proved to
be strictly correct. The process, however, is a distinct improvement
over the older methods and forms the basis of the amended process given
below, which appears to be sufficiently accurate to entitle the acetate
method to favorable consideration.
=34. Method of Hess.=—Hess has lately made a thorough investigation of
the standard methods of determining the iron and aluminum oxids in the
presence of phosphoric acid and has shown that the assumption that the
composition of the precipitate is represented by the formula Al₂(PO₄)₂
+ Fe₂(PO₄)₂ is erroneous[24].
In the washing of the precipitated iron and aluminum phosphates there
is a progressive decomposition of the compound with the production
of a basic salt. The composition of the precipitate at the end is
dependent chiefly upon the way in which the washing takes place. It
is quite difficult to always secure a washing in exactly the same way
and the final composition of the precipitate varies with almost every
determination. It is not, therefore, an accurate proceeding to take
half the weight of the precipitate as phosphoric acid or as iron oxid
and alumina. In every case it is necessary to dissolve the precipitate
and determine the phosphoric acid in the regular way. Hess proposes the
following method for carrying out the acetate process of separation:
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