(4) _Double Superphosphates._—In the case of double superphosphates,
which sometimes contain large quantities of pyrophosphate, the solution
is made in the usual way so that in 100 cubic centimeters there will
be contained two grams of the substance. Usually ten grains are taken
and the volume made up to half a liter. Twenty-five cubic centimeters
of the filtrate are diluted with seventy-five cubic centimeters of
water and the pyro converted to orthophosphoric acid by heating with
ten cubic centimeters of strong nitric acid on a sand-bath. The heating
should be continued until the volume be reduced to twenty-five cubic
centimeters. The strongly acid liquid is made alkaline with ammonia,
and afterwards slightly acid with nitric, and the rest of the process
is carried on in the usual way.
(5) _Phosphoric Acid in the Residue of Superphosphate Manufacture._—In
the mixture of superphosphates and gypsum, the residue of the
manufacture of double superphosphates, the phosphoric acid is estimated
in the following manner: Five grams of the substance are placed in a
dish, rubbed up with absolute alcohol, and washed into a 250 cubic
centimeter flask. The flask is filled with absolute alcohol to the
mark, closed with a stopper, and with frequent shaking, allowed to
stand for two hours; it is thereupon filtered as quickly as possible;
fifty cubic centimeters of the filtrate corresponding to one gram
of the substance, are taken for the estimation. This fifty cubic
centimeters is evaporated on a sand-bath to a sirupy consistence,
diluted with water, and treated, as in the case of the soluble
phosphates above mentioned. In all cases as described above, after
the solutions are obtained they are treated with the ammonium citrate
solution and the phosphoric acid estimated as in the first instance
given.
(6) _Solutions Employed._—
(a) The citrate solution is made as follows: 1,500 grams of
citric acid are dissolved in water, treated with five liters
of twenty-four per cent ammonia, and made up to fifteen liters.
(b) The magnesia mixture is made as follows: 500 grams of
magnesium chlorid, 1,050 grams of ammonium chlorid, three
and five-tenths liters of twenty-four per cent ammonia, and
six and five-tenths liters of distilled water are used.
In the case of the superphosphates fifty cubic centimeters of the
citrate solution are employed and with the basic slags 100 cubic
centimeters; and in both cases twenty-five cubic centimeters of the
magnesia mixture.
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