=77. Alternate Method.=—The following method may also be used: Ten
grams of the substance are heated with fifty cubic centimeters of
concentrated sulfuric acid until white vapors have been evolved for
some time. The operation lasts for about fifteen minutes and can be
carried on in a half liter flask or in a porcelain dish. Without
regarding the undissolved material the volume of the liquid is now
made up to half a liter and filtered. The filtered liquid becomes
turbid after some time through the separation of calcium sulfate, but
this turbidity should not be regarded. To fifty cubic centimeters of
the solution, corresponding to one gram of substance, twenty cubic
centimeters of citric acid solution (500 grams citric acid to the
liter) are added, and it is afterwards nearly neutralized by the
addition of ten per cent ammonia and the liquid, which is warmed
by this operation, cooled. There are now added twenty-five cubic
centimeters of the ordinary magnesium chlorid mixture and the solution
stirred until turbidity is produced, one-third of its volume of ten per
cent ammonia added, and again stirred for about a minute.
Instead of the addition of the citric acid and ammonia the ammonium
citrate prepared as follows, may be added: 1,500 grams of citric acid
are dissolved with water, made up to three liters and five liters of
twenty-four per cent ammonia and seven liters of water added. The rest
of the operation is carried on in the usual manner.
=78. Halle Method for Basic Slag.=—The total phosphoric acid is
estimated at the Halle Station by the following process:[65]
Ten grams of the substance are moistened in a porcelain dish with a
few drops of water and about five cubic centimeters of a one to one
solution of sulfuric acid added, and after the mass has hardened,
which takes place very soon, fifty cubic centimeters of concentrated
sulfuric acid are added and stirred with a glass rod until it is evenly
distributed throughout the whole mass. In stirring this mixture the
greatest care must be taken, otherwise the substance would remain
attached to the sides of the dish, which during later heating would
cause loss through spurting. The complete solution now takes place
after a few hours’ heating on a sand-bath. During the cooling the
jelly-like mass must be stirred with a glass rod, and after it is cool,
by means of a washing-bottle, gently along the sides of the dish,
water is added, and when the mixture becomes hot it is again cooled
and washed into a half liter flask, which is made up to the mark at a
temperature of 17°.5 and filtered. When the acid filtrate stands for
some time there is often a separation of gypsum which, however, does
not in any way influence the subsequent analysis, which is made in the
usual manner.
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