For the best results the substance to be examined should be placed
in the flask in a dry state and then 800 cubic centimeters of water
added and shaken by means of the machine indicated for half an
hour. Afterwards the flasks are filled up to the mark, well shaken,
and filtered through double folded filters into ordinary flasks of
about 400 cubic centimeters capacity. Before any of the filtrate is
collected, the first that runs through should be well shaken in the
receiving flasks and rejected. Fifty cubic centimeters of the filtrate
thus collected, corresponding to one gram of the substance, should be
used for the determination.
(2) _Total Acid._—For total phosphoric acid, including the insoluble
portions, the material is treated as follows: Five grams of the
substance are placed in a 500 cubic centimeter flask with twenty cubic
centimeters of nitric acid of 1.42 specific gravity, and fifty cubic
centimeters of pure concentrated sulfuric acid, and boiled briskly for
half an hour. With substances which contain much organic material,
a little paraffin is added to avoid frothing. Such substances also
require a larger quantity of nitric acid than that above specified. The
flasks are allowed to cool, water added, again allowed to cool, and
filled up to the mark at 17°.5. If hydrochloric instead of sulfuric
acid be used in making the above solution, when the citrate method
is employed, the results are always too high because the precipitate
contains lime and alumina in such quantities as to render any
compensation for them inaccurate. In addition to this the sulfuric
has this great advantage over the hydrochloric acid; _viz._, in not
separating silicic acid, inasmuch as the silicic acid is insoluble in
boiling sulfuric acid.
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