The yellow precipitate is washed by decantation in the flask nine times
with twenty cubic centimeters of molybdic solution diluted with one
volume of water and the filter washed out once with the same quantity
of liquid. The funnel, with the filter, is immediately placed upon
the flask and the portion of the precipitate collected in the filter
dissolved in five per cent ammonia, which is easily accomplished by
throwing ammonia upon it from a wash-bottle. Afterwards the filter is
washed with a sufficient quantity of hot water and finally removed. The
contents of the flask are neutralized warm, with hydrochloric acid, the
acid being added until the precipitate first formed, after continued
shaking, is again dissolved in the liquid. The solution is then cooled
and treated, drop by drop, with constant stirring, with twenty cubic
centimeters of magnesia mixture. Finally twenty-five cubic centimeters
of dilute ammonia solution are added, the precipitate is not shaken,
and, after two hours, is filtered through a gooch.
For the filtering of the ammonium magnesium phosphate by the molybdic
method, freshly prepared felts are always employed since the remarkably
fine crystalline precipitates will pass through a filter which has once
been used. It is necessary also that special precautions be taken in
the ignition. The crucible should be heated in a platinum cap, which
has the purpose of protecting the contents of the crucible from the
access of reducing gases during the ignition. After redness has been
reached the cap can be removed and the crucible transferred to a blast
where it is strongly ignited for ten minutes before weighing. The
precipitate should be pure white.
The molybdic solution is prepared as follows: 150 grams of ammonium
molybdate are dissolved in a liter of water, and after the solution is
completely cooled, poured into a liter of nitric acid of 1.2 specific
gravity.
=56. Estimation of Soluble Phosphoric Acid.=—1. The extraction of the
superphosphates is made as follows: Twenty grams of the superphosphates
are placed in a liter flask with 800 cubic centimeters of water and
shaken continuously for thirty minutes. The flask is then filled with
water to the mark and the whole again thoroughly shaken and filtered.
For shaking, a machine is recommended, driven by hand or water power.
The normal rate of the machine is fixed at 150 turns per minute.
2. The solution of the total superphosphates, obtained as above, must
be boiled with nitric acid before the precipitation of the phosphoric
acid in order to convert any phosphoric acid present as pyrophosphoric
into tribasic phosphoric acid. For each twenty-five cubic centimeters
of the superphosphate solution ten cubic centimeters of concentrated
nitric acid are added and the mixture boiled.
3. The precipitation of the phosphoric acid is conducted by the
molybdenum method as usually practiced.
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