Decant the clear liquid through a filter, and transfer the precipitate to the filter, using as wash-water a mixture of one volume of concentrated ammonia and three volumes of water. It is not necessary to clean the beaker completely or to wash the precipitate thoroughly at this point, as it is necessary to purify it by reprecipitation.
[Note 1: Magnesium ammonium phosphate is not a wholly insoluble substance, even under the most favorable analytical conditions. It is least soluble in a liquid containing one fourth of its volume of concentrated aqueous ammonia (sp. gr. 0.90) and this proportion should be carefully maintained as prescribed in the procedure. On account of this slight solubility the volume of solutions should be kept as small as possible and the amount of wash-water limited to that absolutely required.
A large excess of the magnesium solution tends both to throw out magnesium hydroxide (shown by a persistently flocculent precipitate) and to cause the phosphate to carry down molybdic acid. The tendency of the magnesium precipitate to carry down molybdic acid is also increased if the solution is too concentrated. The volume should not be less than 90 cc., nor more than 125 cc., at the time of the first precipitation with the magnesia mixture.]
[Note 2: The magnesium ammonium phosphate should be perfectly crystalline, and will be so if the directions are followed. The slow addition of the reagent is essential, and the stirring not less so. Stirring promotes the separation of the precipitate and the formation of larger crystals, and may therefore be substituted for digestion in the cold. The stirring-rod must not be allowed to scratch the glass, as the crystals adhere to such scratches and are removed with difficulty.]
REPRECIPITATION AND IGNITION OF MAGNESIUM AMMONIUM PHOSPHATE
A single precipitation of the magnesium compound in the presence of molybdenum compounds rarely yields a pure product. The molybdenum can be removed by solution of the precipitate in acid and precipitation of the molybdenum by sulphureted hydrogen, after which the magnesium precipitate may be again thrown down. It is usually more satisfactory to dissolve the magnesium precipitate and reprecipitate the phosphate as magnesium ammonium phosphate as described below.
Procedure.—Dissolve the precipitate from the filter in a little dilute hydrochloric acid (sp. gr. 1.12), allowing the acid solution to run into the beaker in which the original precipitation was made (Note 1). Wash the filter with water until the wash-water shows no test for chlorides, but avoid an unnecessary amount of wash-water. Add to the solution 2 cc. (not more) of magnesia mixture, and then dilute ammonium hydroxide solution (sp. gr. 0.96), drop by drop, with constant stirring, until the liquid smells distinctly of ammonia. Stir for a few moments and then add a volume of strong ammonia