MISCELLANEOUS NOTES ON PHOSPHATES AND PHOSPHATIC FERTILIZERS.
=119. Time Required for Precipitation of Phosphoric Acid.=—The length
of time required for the complete precipitation of the phosphoric acid
by molybdate mixture is perhaps much less than generally supposed.
At 65° the precipitation, as shown by de Roode, is complete in five
minutes.[100] In a given case the weight of pyrophosphate obtained
after five minutes was 0.0676 gram, and exactly the same weight was
found after twenty-four hours. In view of these facts analysts would
often be able to save time by omitting the delay usually demanded by
the setting aside of the yellow precipitate for a few hours in order
to secure a complete separation of the phosphoric acid. In the method
of the official chemists it is directed that the digestion at 65° be
continued for one hour, and this time may possibly be shortened with
advantage. In all cases, however, where there is any doubt in regard to
the complete separation, some of the molybdate solution should be added
to the filtrate and, with renewed digestion, it should be noted whether
any additional precipitate be formed.
=120. Examination of the Pyrophosphate.=—In fertilizer control it is
not usually thought necessary to examine the magnesium pyrophosphate
for impurities. Among those most likely to be found is silica. It
is proper, in all cases where accuracy is required, to dissolve the
precipitate in nitric acid, boil for some time to convert the pyro-
into orthophosphate, and reprecipitate with molybdate and magnesia
mixture. This treatment will separate the silica which remains
practically insoluble after the first ignition. It has been observed
by some analysts that the results obtained by the official method are
a trifle too high and also that on re-solution the second precipitate
of pyrophosphate weighs less than the first.[101] The difference in
most cases is very little but it may become a quantity of considerable
magnitude in samples where soluble silica is found in notable
quantities. The danger of contamination with iron, alumina, and arsenic
has already been mentioned but it is not of sufficient importance to
warrant further attention.
=121. Iodin in Phosphates.=—The presence of iodin has been detected in
many natural phosphates and is of interest in the discussion of the
problem of their origin.[102] A qualitative test for the detection
of iodin may be applied in the following manner: Some finely ground
phosphate is mixed with strong sulfuric acid and the gases arising from
the reaction are aspired into some carbon disulfid or chloroform. The
violet coloration arising indicates the presence of iodin. The gases
carrying the iodin may also be brought into contact with starch-paste
producing the well-known blue color.
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