(3) _Citrate-Soluble Acid._—Two grams of the sample are digested with
100 cubic centimeters of citrate solution, 1.09 specific gravity, for
half an hour at 50° in a beaker. Afterwards the soluble matter is
separated by filtration with the aid of a filter-pump and the residue
washed with a solution of one part water and one part citrate solution
until all the dissolved phosphoric acid is removed from the filter.
Generally three or four washings are sufficient. The residue on the
filter is dried, ignited, and dissolved in a mixture of two cubic
centimeters of nitric and twenty cubic centimeters of sulfuric acid,
the solution made up to a volume of 200 cubic centimeters, filtered,
and 100 cubic centimeters of the filtrate taken for the determination.
The acid in the filtrate is nearly neutralized and fifty cubic
centimeters of citrate solution are added, and afterwards twenty-five
cubic centimeters of magnesia mixture and twenty cubic centimeters of
twenty-four per cent ammonia. After standing for forty-eight hours, the
precipitate is separated by filtration, ignited, and weighed in the
usual way. The difference between the total phosphoric acid and that in
the insoluble residue, after treatment with ammonium citrate, as above,
gives the quantity of phosphoric acid soluble in the citrate solution.
The difference between the total citrate-soluble and the water-soluble
gives the quantity of the reverted phosphoric acid.
The ammonium citrate solution used for the digestion is made as
follows: Two hundred and fifty grams of crystallized citric acid
are dissolved in half a liter of hot water, diluted with 550 cubic
centimeters of water, 276 cubic centimeters of twenty-four per cent
ammonia added, and finally, exactly neutralized by adding, little by
little, fifty per cent citric acid solution.
The Halle methods of separating the water and citrate-soluble acids
appear to be less complete and reliable than those in use by the
Official Agricultural Chemists of this country. The precipitation of
basic phosphates, when large quantities of water are used at once in
separating soluble acid, must tend to diminish the quantity obtained,
while the lack of care in assuring the neutrality of the citrate
solution might lead to varying results.
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