Separate the phosphoric acid in the form of the yellow precipitate
and wash this latter in the usual way. Too high a heat should not be
employed, nor should the solutions be allowed to stand too long lest
excess of molybdic acid separate. Dissolve the phosphomolybdate in 100
cubic centimeters of cold two and five-tenths per cent ammonia and add
as many cubic centimeters of the usual magnesia mixture (fifty-five
grams magnesium chlorid and seventy grams ammonium chlorid dissolved
in a liter of two and five-tenths per cent ammonia) as there are
centigrams of phosphorus pentoxid present. Addition should not be
made faster than ten cubic centimeters per minute. Stir during the
addition. After the precipitation, stir briskly once more and then
allow to stand at least three hours. Wash with two and five-tenths per
cent ammonia till the chlorin reaction disappears, dry the filter,
and introduce into a well-cleaned crucible which has been thoroughly
ignited. Place the lid at an angle, carbonize the filter, and
gradually raise the heat, though not higher than a medium red heat,
till the pyrophosphate becomes completely white. When this happens
bring the blast into action and ignite to constant weight. The weight
finally accepted must not change even after half an hour’s ignition.
Upon this requirement especial stress must be laid. Pure magnesium
pyrophosphate does not suffer any loss even after several hours’
ignition nor does a good platinum crucible. To the weighed amount of
pyrophosphate, add the correction given in the table. For example, if
the weight be 250 milligrams, the correction to be added is four and
two-tenths milligrams, and the correct weight is then 254.2 milligrams.
Multiplication of the sum by sixty-four gives the amount of phosphorus
pentoxid in the weight taken for analysis.
CORRECTION FOR PHOSPHORIC ACID DETERMINATION.
Found, Lost, Found, Lost,
Mg₂P₂O₇ milligrams Mg₂P₂O₇ milligrams
in grams. Mg₂P₂O₇. in grams. Mg₂P₂O₇.
0.10 0.6 0.24 4.0
0.12 0.8 0.25 4.2
0.14 1.2 0.26 4.6
0.15 1.4 0.27 5.0
0.16 1.6 0.28 5.5
0.17 2.4 0.29 6.1
0.18 2.6 0.30 6.8
0.19 3.2 0.31 7.6
0.20 3.5 0.32 8.6
0.21 3.6 0.33 9.6
0.22 3.8 0.34 10.6
When phosphoric acid is to be estimated as pyrophosphate it must always
be first separated as molybdate, even when the original solution
contains no bases capable of forming insoluble phosphates, as otherwise
these corrections will not be applicable.
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