The presence of large quantities of iron and alumina also impairs the
accuracy of the molybdate method when the precipitation of the yellow
salt takes place at too high a temperature. When the temperature of
precipitation in the method is above 50° the results are likely to be
too high while a great excess of nitric acid in the reagent may produce
a contrary effect. In the latter case the filtrate from the yellow salt
should be mixed with additional quantities of molybdate solution until
no further precipitate takes place.
Many methods of conducting the citrate method have been proposed but
the best of them are based on the one elaborated at the experiment
station of Halle by Bühring, and which will be given in the next
paragraph, followed by some other methods in use in other localities.
=64. Method of the Halle Agricultural Experiment Station.=[52]—The
citrate method, as described by Morgen, is the one employed.[53] The
principle depends upon the direct precipitation of the phosphoric acid
by magnesia mixture. By the addition of a solution of ammonium-citrate
the precipitation of lime, iron, alumina, and other bases, is
prevented. The precipitate of ammonium magnesium phosphate is converted
by ignition into magnesium pyrophosphate and weighed as such. By the
use of this method a part of the phosphoric acid sometimes escapes
precipitation and a portion of the other bases is sometimes thrown down
with the precipitate. Experience has shown that by adhering to certain
precautions the weight of impurities in the precipitate may be made to
correspond exactly to the weight of the phosphoric acid which escapes
precipitation.
[Illustration: FIGURE 3.
SHAKING APPARATUS FOR SUPERPHOSPHATES.]
(1) _Soluble Acid._—The soluble phosphates are first brought into
solution in such a way that one liter of water contains the soluble
phosphoric acid from twenty grams of the substance. Twenty grams are
rubbed in a porcelain mortar with water and through a wide-necked
funnel washed into a bottle-shaped flask in which a little water has
been previously placed. The flasks employed are made of thick glass
in order to withstand shaking. After the substance is washed, the
flasks are filled to the mark and closed with rubber stoppers. They are
then placed upon a shaking rack as indicated in Fig. 3, which is also
furnished with an apparatus for separating the fine meal from basic
slag.
On a table, as shown in the figure, is fastened a movable horizontal
board by means of hinges. At the left hand of this movable board is
placed an open wooden box in which is a perforated shelf for the
purpose of holding the flasks, so as to prevent their striking together
during the shaking.
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