_Manipulation._—Place twenty grams of substance in a mortar together
with some cold distilled water or pure rain water, stir, and decant
the water and suspended matters into a liter flask. After this has
been repeated several times, rub up the residual mass and wash it all
into the flask. Fill up to about 900 cubic centimeters and allow to
stand two hours (twenty-four hours in the case of double phosphates
with more than twenty-two per cent of soluble phosphoric acid),
shaking repeatedly; or shaking continuously, for half an hour. Fill
up to the liter mark and filter through a dry filter. Take portions
of twenty-five or fifty cubic centimeters for each determination, add
100 cubic centimeters of molybdate solution for each 100 milligrams of
phosphorus pentoxid present, warm to about 80° for an hour, filter, and
wash the precipitate with the ammonium nitrate solution. Add a little
molybdate solution to the filtrate, warm, and, if a fresh precipitate
be observed, it is to be added to the first. The precipitate is to
be dissolved in ammonia, and hydrochloric acid carefully added until
the precipitate caused by it only slowly redissolves on stirring. The
phosphoric acid is precipitated from the clear liquid which is still
ammoniacal with magnesia mixture, using ten cubic centimeters for each
100 milligrams of phosphorus pentoxid present. This is added, drop
by drop, and the liquid kept stirred during the addition. Allow it
to stand at least two hours, filter, wash with dilute ammonia, dry,
and ignite. This last is done at first with a very small flame but is
finished with the blast-lamp or in a Rössler furnace. To insure burning
to whiteness, nitric acid may be used, but not more than one or two
drops.
_B. Total Phosphoric Acid._—(1) For bone and flesh-meal, fish-guano,
and similar fertilizers the reagents necessary are the same as before.
Carefully burn five grams to ash, boil the ash for half an hour with
nitric acid of 1.32 specific gravity, dilute with water, and, after
cooling, dilute to 500 cubic centimeters. Filter through a dry filter
and take fifty cubic centimeters of the filtrate. Add 100 cubic
centimeters of the molybdate solution for each 100 milligrams of
phosphorus pentoxid present. Treat further as before described.
(2) Phosphates, guanos, bone-black, etc.
One gram of substance, after powdering, and, if necessary, igniting,
is covered with four cubic centimeters of hydrochloric acid of 1.13
specific gravity and a little water and heated for an hour and a half.
Evaporate to dryness without filtration, making repeated additions of
nitric acid until no more vapors of hydrochloric acid are evolved. Boil
the residue with nitric acid, cool, make up to 100 cubic centimeters
with water, and shake. Filter and treat fifty cubic centimeters of
the resulting solution by the molybdate method and proceed further as
before described.
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