One hundred cubic centimeters, equivalent to one gram of the substance,
in a nitric acid solution, are placed in a half liter flask and a
solution of ammonium molybdate added until all the phosphoric acid
has been precipitated. The addition of ammonium nitrate will hasten
the separation of the ammonium phosphomolybdate. The liquid should be
allowed to stand for twelve hours. The flask is then filled to the
mark, the contents well shaken, filtered through a dry filter, and
duplicate samples of 200 cubic centimeters each of the filtrate taken
for analysis.
A small quantity of ammonium nitrate is dissolved in the liquid, and
ammonia cautiously added, keeping the solution as cool as possible. The
iron and alumina are precipitated as hydroxids. The mixed hydroxids are
collected on a filter, washed with water, the filtrate and washings
being collected in a beaker. The precipitate should be dissolved with a
small quantity of a solution of ammonium nitrate and nitric acid, again
precipitated with ammonia, filtered, washed, ignited, and weighed. This
treatment is for the purpose of excluding all possibility of error from
the presence of molybdic anhydrid. After weighing, the mixed oxids
should be fused with sodium bisulfate, the magma dissolved in water,
and the iron determined volumetrically with potassium permanganate
after reduction to the ferrous state.
McElroy has further shown by experiments in this laboratory that even
the molybdate method of separating the iron and alumina from phosphoric
acid with the improvements as first suggested by Krug and himself, may
not always give reliable results.[32] In a solution containing ferrous
iron equivalent to 56.4 milligrams of ferric oxid, were placed enough
of a solution of sodium phosphate to correspond to 100 milligrams of
phosphorus pentoxid. The precipitate was dissolved by adding nitric
acid, oxidized with bromin water, and the phosphoric acid thrown out
with ammonium molybdate. The precipitate was washed with weak nitric
acid and the combined filtrate and washings neutralized with ammonia.
The resultant precipitate was dissolved in a solution of ammonium
nitrate and nitric acid, filtered, and again precipitated with ammonia.
In two instances the quantities of material recovered after ignition
were 56.9 and 57.3 milligrams, respectively, instead of the theoretical
amount, _viz._, 56.4 milligrams.
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