If, during the evaporation of the filtrate, any flocculent matter
separate, it should be removed by filtration and examined before
precipitating the magnesia.
=39. Variation of Marioni and Fasselli.=—Glaser’s method has been shown
to be subject to errors by Marioni and Fasselli[29] in the following
respects:
1. The precipitation of a small quantity of calcium phosphate with the
ferric and aluminum phosphates.
2. The possible precipitation of basic phosphates if all the iron and
alumina are not combined with phosphoric acid in the mineral.
3. The partial solubility of ferric and aluminum phosphates in dilute
acetic acid.
4. The decomposition of ferric orthophosphate into soluble acid
phosphate and insoluble basic salt by boiling.
To avoid these errors the following procedure is proposed: From one to
five grams of the phosphate are boiled in a flask for ten minutes with
fifteen cubic centimeters of strong hydrochloric acid, and afterwards
diluted with a double volume of water. A few crystals of potassium
chlorate are added, and several drops of nitric acid, and the liquid
boiled to expel chlorin. It is then filtered and washed until the
volume of the filtered liquid amounts to 150 cubic centimeters. After
cooling, a half gram of ammonium phosphate in solution is added, and
two cubic centimeters of glacial acetic acid, followed by dilute
ammonia, drop by drop, until a slight precipitate persists on stirring.
Again the same quantity of acetic acid is added as above, well shaken,
and left for two hours. The precipitate is collected on a filter and
washed with a one per cent ammonium phosphate solution. The precipitate
is dissolved by a minimum quantity of hydrochloric acid and the
solution collected in the same vessel in which the precipitation took
place. A second precipitation is conducted just as described above.
The precipitate is washed as above described and ignited at a dull red
heat. Half the weight obtained represents the ferric oxid and alumina.
=40. Method of Ogilvie.=—For the separation of alumina from phosphoric
acid Ogilvie recommends that the filtrate from the phosphomolybdate
precipitate be neutralized with ammonia, the precipitate thus formed
redissolved in nitric acid, again precipitated with ammonia, filtered,
ignited, and weighed as aluminum oxid.[30] If iron be present it will,
of course, appear in the product. For use in the examination of mineral
phosphates the method can not have a wide application without amendment.
=41. Method of Krug and McElroy.=—Krug and McElroy show that when
sufficient alcohol is added to precipitate all of the calcium sulfate
in the Glaser method, it will also cause a precipitation of a
considerable quantity of iron, by means of which the calcium sulfate
will be colored.[31] The presence of potassium and ammonium salts also
affects very notably the precipitation of calcium. The method employed
by them, in order to avoid these sources of error, is as follows:
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