=108. The Process.=—One gram of phosphate rock, or from two to
three grams of phosphatic fertilizer, are dissolved in nitric acid,
and, without evaporation, diluted to 250 cubic centimeters. Without
filtering, twenty-five cubic centimeters are placed in a four-ounce
beaker and ammonia added until a slight precipitate begins to form.
Five cubic centimeters of nitric acid of one and four-tenths specific
gravity are then added, and afterwards ten cubic centimeters of
saturated solution of ammonium nitrate and enough water to make the
volume about sixty-five cubic centimeters. The contents of the beaker
are boiled, and while still hot, five cubic centimeters of the aqueous
solution of ammonium molybdate added. Additional quantities of the
molybdate are added, if necessary, until the whole of the phosphorus
pentoxid is thrown-out.
After allowing to settle for a moment the contents of the beaker are
poured upon a filter seven centimeters in diameter. The precipitate is
thoroughly washed with water, both by decantation and on the filter.
The filter with its precipitate is transferred to a beaker and titrated
with standard alkali, in the presence of phenolphthalein. Each cubic
centimeter of alkali employed should correspond to one milligram of
phosphorus pentoxid, (P₂O₅).
The reagents employed have the composition indicated below:
_Ammonium Molybdate._—Ninety grams of the crystals of ammonium
molybdate are placed in a large beaker and dissolved in a little less
than one liter of water. The beaker is allowed to stand over night
and the clear liquor decanted. Any undissolved acid is brought into
solution in a little ammonia water and added to the clear liquor. If a
trace of phosphoric acid be present a little magnesium sulfate is added
and enough ammonia to produce a slight alkaline reaction. The volume
of the solution is then made up to one liter. Each cubic centimeter
of this solution is capable of precipitating three milligrams of
phosphorus pentoxid.
_Standard Potassium Hydroxid._—This solution is made of such strength
that one cubic centimeter is equivalent to one milligram of phosphorus
pentoxid. Treated with acid of normal strength, 100 cubic centimeters
are required to neutralize 32.37 cubic centimeters thereof.
_Standard Acid._—This should have the same strength, volume for volume,
as the standard alkali solution. It is made by diluting 323.7 cubic
centimeters of normal acid to one liter.
_Indicator._—The indicator to be used is an alcoholic solution of
phenolphthalein, one gram in 100 cubic centimeters of sixty per cent
alcohol, and half a cubic centimeter of this should be used for each
titration.
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