=50. Citrate-Insoluble Phosphoric Acid.=—Heat 100 cubic centimeters of
strictly neutral ammonium citrate solution of 1.09 specific gravity
to 65° in a flask placed in a bath of warm water, keeping the flask
loosely stoppered to prevent evaporation. When the citrate solution
in the flask has reached 65°, drop into it the filter containing the
washed residue from the water-soluble phosphoric acid determination,
close tightly with a smooth rubber stopper, and shake violently until
the filter paper is reduced to a pulp. Place the flask back into the
bath and maintain the water in the bath at such a temperature that the
contents of the flask will stand at exactly 65°. Shake the flask every
five minutes. At the expiration of exactly thirty minutes from the time
the filter and residue were introduced, remove the flask from the bath
and immediately filter as rapidly as possible. It has been shown by
Sanborn, in this laboratory, that the filtration is greatly facilitated
by adding asbestos pulp. Wash thoroughly with water at 65°. Transfer
the filter and its contents to a crucible, ignite until all organic
matter is destroyed, add from ten to fifteen cubic centimeters of
strong hydrochloric acid, and digest until all phosphate is dissolved;
or return the filter with contents to the digestion flask, add from
thirty to thirty-five cubic centimeters of strong nitric, and from
five to ten cubic centimeters of strong hydrochloric acid, and boil
until all the phosphate is dissolved. Dilute the solution to 200 cubic
centimeters. If desired, the filter and its contents can be treated
according to methods (1), (2), or (3), under total phosphoric acid.
Mix well; filter through a dry filter; take a definite portion of the
filtrate and proceed as under total phosphoric acid.
In case a determination of citrate-insoluble phosphoric acid be
required in non-acidulated goods it is to be made by treating two
grams of the phosphatic material, without previous washing with water,
precisely in the way above described, except that in case the substance
contain much animal matter (bone, fish, etc.), the residue insoluble
in ammonium citrate is to be treated by one of the processes described
below under total phosphoric acid, (1), (2), or (3).
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