=51. Total Phosphoric Acid.=—In case of ignition the residual material
is to be dissolved in hydrochloric acid. The following methods of
treating the raw material, using two grams in each case, may be
employed: (1) Evaporate with five cubic centimeters of magnesium
nitrate, ignite, and dissolve in hydrochloric acid. (2) Boil in a
Kjeldahl flask graduated to 250 cubic centimeters, with from twenty
to thirty cubic centimeters of strong sulfuric acid, adding from two
to four grams of sodium or potassium nitrate at the beginning of the
digestion and a small quantity after the solution has become nearly
colorless; or adding the nitrate in small portions from time to time.
After the solution is colorless, add 150 cubic centimeters of water and
boil for a few minutes, cool, and make up to volume. (3) Digest with
strong sulfuric acid and such other reagents as are used in either the
plain or modified Kjeldahl or Gunning methods for estimating nitrogen.
Do not add any potassium permanganate, but after the solution has
become colorless add about 100 cubic centimeters of water and boil
for a few minutes, cool, and make up to a convenient volume; two
and five-tenths grams of substance and a digestion flask graduated
to 250 cubic centimeters are recommended. This method will be found
convenient when both the nitrogen and the total phosphoric acid are to
be determined in a fertilizer. In this case, after diluting the volume
and mixing, a part for the estimation of nitrogen, may be removed with
a pipette and the remainder then filtered through a dry filter and a
portion taken for the determination of the total phosphoric acid. (4)
Dissolve in thirty cubic centimeters of concentrated nitric acid and a
small quantity of hydrochloric acid. (5) Add thirty cubic centimeters
of concentrated hydrochloric acid, heat, and add cautiously, in small
quantities at a time, about five-tenths gram of finely-pulverized
potassium chlorate. (6) Dissolve in from fifteen to thirty cubic
centimeters of strong hydrochloric and from three to ten cubic
centimeters of nitric acid. This method is recommended for fertilizers
containing much iron or aluminum phosphate. Boil until all phosphates
are dissolved and all organic matter is destroyed; cool and dilute
to 200 or 250 cubic centimeters; mix and pass through a dry filter;
take an aliquot part of the filtrate corresponding to a quarter, half,
or one gram, neutralize with ammonia, and clear with a few drops of
nitric acid. In case hydrochloric or sulfuric acid have been used as a
solvent, add about fifteen grams of dry ammonium nitrate.
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