_Manipulation._—Twenty-five or fifty cubic centimeters of a solution
of the phosphate which has been made up to a standard volume and
containing about one-tenth gram of phosphorus pentoxid, are placed
in a beaker together with 100 cubic centimeters of the molybdate
solution and treated with as much ammonium nitrate solution as will be
sufficient to give the liquid a content of fifteen per cent of ammonium
nitrate. The contents of the beaker are well mixed and warmed for about
twenty minutes at from 60° to 80°. After cooling, they are filtered and
the precipitate washed on the filter with cold water until a drop of
the filtrate saturated with ammonia does not become opaque on treatment
with ammonium oxalate. The filtrate is then washed from the filter with
two and one-half per cent ammonia solution and precipitated slowly and
with constant stirring by the magnesia mixture. After standing for two
hours the ammonium magnesium phosphate is separated by filtration,
washed with two and one-half per cent ammonia until the filtrate
contains no more chlorin, and ignited.
_Conduct of the Citrate Method._—The principle of this method depends
upon the fact that when a sufficient quantity of ammonium citrate is
added to phosphate solutions, iron, alumina, and lime are retained in
solution when, on the addition of the magnesia mixture in the presence
of free ammonia, the phosphoric acid is completely precipitated as
ammonium magnesium phosphate.
_Manipulation._—From ten to fifty cubic centimeters of the solution
of the phosphate to be determined are treated with fifteen cubic
centimeters of the Joulie citrate solution avoiding warming. A few
pieces of filter-paper, the ash content of which is known, are thrown
in and, with stirring, fifteen cubic centimeters of magnesia mixture
slowly added and if necessary also some free ammonia. By the small
pieces of filter-paper the collection of the precipitate against
the sides of the vessel and on the stirring rod is prevented and in
this way the production of the precipitate hastened. After standing
from one-half an hour to two hours the mixture is filtered, ignited,
and weighed. If it be preferred to estimate the phosphoric acid by
titration, the precipitate is dissolved in a little nitric acid, made
slightly alkaline with ammonia, and then acid with acetic and then
afterwards titrated with the standard uranium solution.
_Conduct of the Uranium Method._—The principle upon which this
method rests depends upon the fact that uranium nitrate or acetate
precipitates uranium phosphate from solutions containing phosphoric
acid and which contain no other free acid except acetic. In the
presence of ammonium salts the precipitate is uranium ammonium
phosphate having the formula PO₄NH₄UrO₂. The smallest excess of soluble
uranium salt is at once detected by the ordinary treatment with
potassium ferrocyanid.
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