To the hot solutions, for every decigram of phosphorus pentoxid that is
present, add fifty cubic centimeters of molybdic solution. Digest at
about 65° for an hour, filter, and wash with water or ammonium nitrate
solution. Test the filtrate by renewed digestion and the addition of
more molybdic solution. Dissolve the precipitate on the filter with
ammonia and hot water and wash into a beaker to a bulk of not more than
100 cubic centimeters. Nearly neutralize with hydrochloric acid, cool,
and add magnesia mixture from a burette; add slowly (about one drop per
second), stirring vigorously. After fifteen minutes add thirty cubic
centimeters of ammonia solution of 0.95 density. Let stand for some
time; two hours are usually enough. Filter, wash with dilute ammonia,
ignite gently at first and then at white heat for ten minutes, and
weigh. For the quantity of magnesia mixture to be added see paragraph
=21=.
=52. Citrate-Soluble Phosphoric Acid.=—The sum of the water-soluble and
citrate-insoluble subtracted from the total gives the citrate-soluble
phosphoric acid.
=53. Preparation of Reagents.=—(1) _Ammonium Citrate Solution._—(_a_)
Mix 370 grams of commercial citric acid with 1,500 cubic centimeters
of water, nearly neutralize with commercial ammonia, cool, add ammonia
until exactly neutral (testing with saturated alcoholic solution of
corallin) and bring to a volume of two liters. Test the specific
gravity, which should be 1.09 at 20°, before using.
(_b_) _Alternate Method._—To 370 grams of commercial citric acid add
commercial ammonia, of 0.96 specific gravity, until nearly neutral;
reduce the specific gravity to nearly 1.09 and proceed as follows:
Prepare a solution of fused calcium chlorid 200 grams to the liter,
and add four volumes of strong alcohol. Make the mixture exactly
neutral, using a small amount of freshly prepared corallin solution as
a preliminary indicator, and test finally by withdrawing a portion,
diluting with an equal volume of water, and testing with cochineal
solution. Fifty cubic centimeters of this solution will precipitate
the citric acid from ten cubic centimeters of the citrate solution. To
ten cubic centimeters of the nearly neutral citrate solution add fifty
cubic centimeters of the alcoholic calcium chlorid solution, stir well,
filter at once through a folded filter, dilute with an equal volume
of water, and test the reaction with neutral solution of cochineal.
If acid or alkaline, add ammonia or citric acid, as the case may be,
to the citrate solution, mix, and test again as before. Repeat this
process until a neutral reaction of the citrate solution is obtained.
At the end the specific gravity must be 1.09 at 20°.
(2) _Molybdic Solution._—See paragraph =22=.
(3) _Ammonium Nitrate Solution._—Dissolve 200 grams of commercial
ammonium nitrate in water and bring to a volume of two liters.
(4) _Magnesia Mixture._—See paragraph =22=.
(5) _Dilute Ammonia for Washing._—See paragraph =22=.
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