=20. Direct Estimation of the Phosphoric Acid.=—It often happens, in
the case of a mineral phosphate, that the only determination desired
is of the phosphoric acid. In this instance the analyst may proceed as
follows: If the qualitative test shows the usual amount of phosphoric
acid, two grams of the sample passed through a sieve, with a millimeter
mesh, are placed in a beaker and thoroughly moistened with water. The
addition of water is to secure an even action of the hydrochloric acid
on the carbonates present. The beaker is covered with a watch-glass
and a little hydrochloric acid is added from time to time until all
effervescence has ceased. There are then added about thirty cubic
centimeters of aqua regia and the mixture raised to the boiling-point
on a sand-bath or over a lamp. The heating is continued until chlorin
is no longer given off and solution is complete. The volume of the
solution is then made up to 200 cubic centimeters without filtering,
filtered, and an aliquot part of the filtrate, usually fifty cubic
centimeters, representing half a gram of the original sample, taken
for the determination of the phosphoric acid according to the method
of the Official Agricultural Chemists. The small quantity of insoluble
material does not introduce any appreciable error into the process when
the volume is made up to 200 or 250 cubic centimeters.
=21. Method of the Official Agricultural Chemists for Total Phosphoric
Acid.=—To the hot solution, for every decigram of phosphorus pentoxid
which may be present, add fifty cubic centimeters of the molybdic
solution. Digest at 65° for an hour, filter, and wash with water or
ammonium nitrate solution[11]. Test the filtrate by renewed digestion
with additional molybdate reagent. Dissolve the precipitate on the
filter with ammonia in hot water and wash into a beaker, making the
volume of filtrate and washings not more than 100 cubic centimeters.
Nearly neutralize with hydrochloric acid, cool, and add magnesia
mixture from a burette at the rate of about one drop a second, stirring
vigorously, meanwhile. The quantity of magnesia mixture to be added is
not prescribed in the official method but it should always be in excess
of the amount necessary for complete precipitation. For each decigram
of phosphorus pentoxid, from eight to ten cubic centimeters should
be used. Fifteen minutes after the last of the magnesia mixture has
been stirred in, thirty cubic centimeters of ammonia of 0.95 specific
gravity are added and the beaker set aside for two hours or longer. The
ammonium magnesium phosphate is separated by filtration, dried, ignited
gently at first, and finally over a blast-lamp and weighed as magnesium
pyrophosphate. The factors for calculating the phosphorus pentoxid and
tricalcium phosphate from the weight of pyrophosphate are given below
on the two bases; _viz._, hydrogen equals 1, and oxygen equals 16.
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