=81. Wagner’s Shaking Apparatus.=—The latest directions given by
Wagner for determining the phosphoric acid in slags and raw phosphates
soluble in citrate solutions, are the following:[67] Five grams of
the material as it is sent into commerce without grinding or sifting,
are placed in a half liter flask and covered with nearly a quarter
liter of water, and then 200 cubic centimeters of citrate solution
added, prepared as described below. The flask is filled to the mark
with water. The flasks, which are of the shape shown in the figure,
are closed with rubber stoppers, and without delay placed for half an
hour in a rotating apparatus, (Fig. 6) which is turned on its axis from
thirty to forty times a minute. If a shaking apparatus be used instead
of the one mentioned, 200 cubic centimeters of the citrate solution
should be placed in a half liter flask, filled to the mark with water,
and the contents poured into a liter flask containing the phosphate.
This flask should be placed in a nearly horizontal position in the
apparatus and the agitation be continued for half an hour. On removal
from the apparatus the mixture is filtered and fifty cubic centimeters
thereof treated with double the quantity of molybdic solution at
80° and the precipitate separated after cooling. The precipitate is
carefully washed with one per cent nitric acid mixture, after which
the filter is broken and the precipitate washed into a beaker with two
per cent ammonia and the filter washed therewith until about 100 cubic
centimeters have been used. If the solution is turbid from the presence
of silicic acid it should be precipitated a second time by addition of
molybdic solution until the acid reaction is restored. The ammoniacal
solution of the yellow precipitate is treated, drop by drop, with
constant stirring, with fifteen cubic centimeters of magnesia mixture,
and set aside for two hours. The precipitate is collected, washed,
ignited, and weighed in the usual manner. The direct precipitation of
the phosphoric acid by the magnesia solution in presence of citrate is
not advisable because of the almost general presence of silicic acid
which would cause the results to be too high.
[Illustration: FIGURE 6.
WAGNER’S DIGESTION APPARATUS FOR SLAGS.]
The chief objection to this method of Wagner lies in the failure to
control the temperature at which the digestion with citrate solution
is made. Huston has shown, as will be described further on, that the
temperature exercises a great influence in digestion with citrate.
Since the laboratory temperature, especially in this country, may vary
between 10° and 35°, it is evident that on the same sample the Wagner
method would give very discordant results at different seasons of the
year.
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