=118. Determination of Phosphoric Acid in Superphosphates.=—(1)
_Citrate-Soluble Phosphoric Acid._—Five grams of the superphosphate are
rubbed with 100 cubic centimeters of Wagner’s acid citrate solution in
a mortar and washed into a flask of 500 cubic centimeters content and
diluted to 500 cubic centimeters with water. With frequent shaking the
flask is allowed to stand for twelve hours, after which its contents
are filtered. Fifty cubic centimeters of the filtrate are treated
with ten cubic centimeters of the Joulie solution and fifteen cubic
centimeters of the magnesia mixture and, if necessary, made distinctly
alkaline with ammonia, vigorously stirred, and, after two hours,
filtered. The precipitate is washed, ignited, and weighed as described,
or titrated, after solution in nitric acid and the addition of sodium
acetate, with uranium solution.
Example:
The weighed precipitate has 0.1272 gram Mg₂P₂O₇ then the phosphate
contains 12.72 × 2 × 0.64 = 16.28 per cent of citrate-soluble P₂O₅.
(2) _Water-Soluble Phosphoric Acid._—Twenty grams of superphosphate
are rubbed in a mortar and washed into a flask of one liter content
and made up to the mark with water. After two hours’ digestion with
frequent shaking, the contents of the flask are filtered through a
folded filter. Twenty-five cubic centimeters of the filtrate equivalent
to five-tenths gram of the substance are precipitated with magnesia
mixture, the precipitate filtered, washed, ignited, and weighed, or the
moist filtrate may be dissolved upon the filter with a little nitric
acid, treated with sodium acetate, and titrated, as described, with
uranium solution.
Example: 14.5 cubic centimeters of the uranium solution are required
for the precipitate from twenty-five cubic centimeters of the original
solution = 0.5 gram superphosphate; it contains then 14.5 × 0.00445 =
0.0645 gram P₂O₅. Consequently the superphosphate contains 12.90 per
cent of water-soluble P₂O₅.
_Total Phosphoric Add._—Twenty grams of the superphosphate are boiled
with fifty cubic centimeters of hydrochloric acid of from 16° to 18°
Beaumé for about ten minutes and, after cooling, made up to one liter
with water and filtered. Twenty-five cubic centimeters of the filtrate
are treated with ten cubic centimeters of Joulie’s citrate solution,
a few pieces of filter-paper thrown in, fifteen cubic centimeters
of magnesia mixture added, and the whole thoroughly stirred. After
standing two hours the contents of the flask are filtered and the
precipitate is washed with dilute ammonia and the filter and the
precipitate are placed in a platinum crucible. The crucible is heated
slowly until the moisture is driven off and the filter burned. Then the
temperature is gradually raised to a white heat. The residue is cooled
and weighed. Example:
The precipitate weighs, after the subtraction of the filter ash, 0.1390
gram; then the superphosphate contains 13.90 × 2 × 0.64 = 17.79 per
cent phosphoric acid.
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