=32. Estimation of Iron and Alumina in Mineral Phosphates.=—When
mineral phosphates are to be used for the manufacture of
superphosphates by treatment with sulfuric acid their content of
iron and alumina becomes a matter of importance. By reason of the
poor drying qualities of the sulfates of these bases their presence
in any considerable excess of a few per cent becomes exceedingly
objectionable. The accurate estimation of these ingredients is not
only then a matter of scientific interest but one of great commercial
significance to the manufacturer.
The conventional methods so long in use depending on the precipitation
of the iron and alumina as phosphates in the presence of acetic acid
have been proved to be somewhat unreliable. Not only does the acetic
acid fail to prevent the precipitation of some of the lime, but it
also dissolves more or less of the iron and aluminum phosphates. The
solution of the precipitate and its reprecipitation by the addition of
ammonia, may free the second precipitate from lime, but it increases
the error due to the solubility of the aluminum salt. The methods
recently introduced for the estimation of iron and alumina in presence
of excess of lime and phosphoric acid are not entirely satisfactory,
but are the best which can now be offered.
=33. The Acetate Method.=—The principle of this process is based on the
fact that in a solution containing iron, alumina, lime, and phosphoric
acid the iron and aluminum phosphates can be thrown down in a slightly
acid solution by ammonium acetate while the calcium phosphate remains
in solution. The acidity in the older methods is due to acetic and can
be secured by making the solution slightly alkaline with ammonia and
adding acetic to slight acidity. One of the best methods of conducting
the operation is that of C. Glaser[23]. Glaser’s modification of the
older processes is based on the assumption that at 70° the aluminum
phosphate is quantitatively precipitated by ammonium acetate in a
dilute hydrochloric acid solution and that the mixed precipitates of
iron and aluminum phosphates obtained at this temperature are free of
lime. The operation is conducted in the following manner:
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