2. _The Determination._—Take twenty-five cubic centimeters of the
superphosphate solution thus prepared (when a twenty per cent sample
is taken equal to one-tenth gram phosphorus pentoxid); add a quantity
of molybdic solution sufficient for complete precipitation, leave
standing for four hours in a beaker covered with a watch-glass; decant
the solution through a small filter, wash the precipitate first by
decantation, then on filter, with a mixture containing 100 parts
molybdic solution, twenty parts nitric acid of 1.2 specific gravity,
and eighty parts water, until a few drops put into alcohol, to which
some dilute sulfuric acid has been added, does not, any longer, cause
turbidity. The molybdic precipitate is now washed with but little water
from the filter into a beaker, and particles adhering to the filter are
dissolved by a hot mixture of one part ammonia and three parts water,
which is allowed to flow into the beaker till the precipitate is,
finally, completely dissolved in it. To the clear solution, add dilute
hydrochloric acid while stirring, till the yellow precipitate formed
by the acid is no longer immediately dissolved; then add from six to
eight cubic centimeters of ammonia through the filter. The volume of
the solution is not to exceed seventy-five cubic centimeters. It is now
cooled completely and one cubic centimeter of magnesia mixture is added
from a burette for every centigram of phosphorus pentoxid which it is
expected to contain, and finally one-quarter of its volume of ammonia
is added. The precipitate may be filtered after four hours. This is
washed on the filter, preferably by means of suction, with a mixture of
one part ammonia and three parts water till the filtrate is entirely
free from chlorin. After drying, heat the precipitate, first gently,
then stronger, and finally with a blast for a few minutes and then
weigh it.
Treated with hydrochloric acid it must leave no insoluble residue
(SiO₂), nor should hydrogen sulfid cause any precipitation in the
solution thus formed (MoO₃).
(b) _Total Phosphoric Acid._—1. _In Superphosphates._—For the
determination of total phosphoric acid, treat a weighed quantity of the
superphosphate with nitric acid, if necessary to bring a difficultly
soluble residue into solution, with addition of hydrochloric acid, or
of potassium chlorate, to destroy organic matter present. Dilute the
solution to a definite volume, and determine the phosphoric acid in a
measured quantity of the same, as directed under (a) 2; if hydrochloric
acid or potassium chlorate, be applied in the preparation of the
solution, however, not till the measured quantity has been repeatedly
evaporated to dryness with concentrated nitric acid.
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