Holleman[68] proposes to estimate the lime in basic slag by a
modification of the methods of Classen and Jones. The manipulation is
as follows: Fifty cubic centimeters of the solution of slag, equivalent
to one gram of substance, are evaporated to a small volume, twenty
cubic centimeters of neutral ammonium oxalate solution (one to three)
added to the residue and heated on a water-bath with frequent stirring,
until the precipitate is pure white and free from lumps. The time
required is usually about ten minutes. The precipitate is collected
on a filter and washed with hot water until the filtrate contains no
oxalic acid. The precipitated calcium oxalate must be snow-white. The
filter is broken and the calcium oxalate washed through, first with
water and finally with warm, dilute hydrochloric acid (one to one).
The calcium oxalate is dissolved by adding fifteen cubic centimeters
of concentrated hydrochloric acid, the solution evaporated to a volume
of about twenty-five cubic centimeters and ten cubic centimeters of
dilute sulfuric acid (one to five), and 150 cubic centimeters of
ninety-six per cent alcohol added. After standing three hours or more
the precipitate is separated by filtration and washed with ninety-six
per cent alcohol until the washings show no acid reaction with methyl
orange. The calcium sulfate precipitated is dried to constant weight.
This method gives a pure precipitate of calcium sulfate, containing
only traces of manganese.
=84. Estimation of Caustic Lime.=—The lime mechanically present in
basic slags is likely to be found as oxid or hydroxid, especially when
the sample is of recent manufacture. In the form of oxid the lime may
be determined by solution in sugar. In this process one gram of the
fine slag meal is shaken for some time with a solution of sugar, as
suggested by Stone and Scheuch.[69] The dissolved lime is separated
as oxalate by treatment of the solution with the ammonium salt. The
calcium oxalate may be determined by ignition in the usual way or
volumetrically by solution in sulfuric acid and titration of the
free oxalic acid with potassium permanganate solutions. The standard
solution of permanganate should be of such a strength as to have one
cubic centimeter equivalent to about 0.01 gram of iron. The iron value
of the permanganate used multiplied by 0.5 will give the quantity of
calcium oxid found.
=85. Detection of Adulteration of Phosphatic Slags.=—The high
agricultural value of phosphatic slags has led to their adulteration
and even to the substitution of other bodies. Several patents have also
been granted for the manufacture of artificial slags of a value said to
be an approximation to that of the by-products of the basic pig iron
process.
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