=109. Estimation of Phosphoric Acid as a Lead Compound.=—In the
volumetric lead method, as described by Wavelet, the phosphoric acid
is precipitated by the magnesium citrate solution as in the uranium
method of Joulie, as practiced by the French chemists, and the washing
of the precipitate and its solution in nitric acid are also conducted
as in that method.[89] After solution in nitric acid ammonia is added
to neutrality and the solution is then made acid with acetic. The
phosphoric acid is precipitated in the acid solution by a standard
solution of lead nitrate, the precipitate having the formula P₂O₅3PbO.
The end reaction is determined by placing a drop of the titrated
mixture on a white greased dish in contact with a drop of a five per
cent solution of potassium iodid. When all the phosphoric acid is
precipitated the least excess of the lead salt is revealed by the
characteristic yellow precipitate of lead iodid.
The author of the process claims that the lead phosphate is insoluble
in the excess of acetic acid and that the phosphate itself does not
give any yellow coloration with potassium iodid. The process is quite
as exact as the uranium method and the end reaction is far sharper and
the standard reagents are easily made and preserved.[90] The method
described merits, at least, a comparative trial with the uranium
process, but cannot be recommended as exact until further approved by
experience.
The reagents employed have the following composition:
(1) Disodium phosphate solution containing 10.085 grams per liter
(2) Sodium acetate “ “ 50.000 “ “ “
(3) Lead nitrate “ “ 40.000 “ “ “
(4) Potassium iodid “ “ 50.000 “ “ “
The titrations should be conducted in the cold.
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