Five grams of the finely ground phosphate are fused in a platinum dish
with fifteen grams of the mixed carbonates of sodium and potassium and
three grams of fine sand. After fusing very thoroughly with a strong
heat for a quarter of an hour, the dish is removed from the fire and
cooled. Its contents, dissolved in hot water, are then put into a half
liter flask, and a considerable excess of ammonium carbonate is added
to the liquid. All the soluble silica falls out of solution, and the
flask, after cooling, is made up to the mark with distilled water, well
shaken, and then set aside for twenty-four hours to settle. At the
end of this time 200 cubic centimeters are carefully decanted through
a filter; the filter is well washed, and the filtrate, after being
nearly neutralized with hydrochloric acid, is treated with an excess of
calcium chlorid solution.
The precipitate, consisting of phosphate, fluorid, and some calcium
carbonate, is allowed to settle, and is then carefully washed with
boiling water, first by decantation several times, and finally on
the filter. After being properly dried in the gas-oven, calcined,
and cooled, the residue is treated with acetic acid, placed upon the
water-bath, and evaporated to complete dryness.
The calcium acetate is now well washed out by several treatments
with boiling water, and the residue is brought upon a filter, dried,
calcined, and weighed. The weight represents the calcium phosphate
and fluorid contained in two grams of the original sample; and if
the calcium phosphate in the residue be determined, according to the
usual methods, the difference will be calcium fluorid and may be thus
estimated.
_Example._—Assuming the calcined residue of calcium phosphate and
fluorid in two grains of the original sample to have amounted to one
and six-tenths gram and the calcium phosphate in this quantity to have
been determined as 1.540 gram, the calcium fluorid is thus proved to
be 0.060 gram, and, therefore, 2: 0.60::100: x = 3 per cent calcium
fluorid which, multiplied by 0.4897, gives 1.46 per cent of fluorin.
The above method, while shorter, is not to be preferred to the Chatard
process when great accuracy is desired. All the soluble silica may
not fall out of the solution as Wyatt says. Finally the fluorin
is calculated from small differences in the weight of very heavy
precipitates and all the error of the process may be found affecting
the numbers for fluorin. For commercial purposes, however, the method
is to be recommended for its comparative brevity.
GENERAL METHODS FOR ESTIMATING PHOSPHORIC ACID IN FERTILIZERS.
Public-domain text, read in full here on John Shaqi.
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