=31. Lime Method of Immendorff.=—The tedious processes required
to determine the lime in the presence of iron, alumina, and large
quantities of phosphoric acid are well known to analysts. Immendorff
has published a method, accompanied by the necessary experimental
data, based on the comparative insolubility of calcium oxalate in very
dilute solution of hydrochloric acid. He has shown in the data given
that the lime is all precipitated in the conditions named and that the
precipitate, when properly prepared, is not contaminated with weighable
amounts of the other substances found in the original solution[22].
The ease with which oxalic acid can be determined volumetrically
with potassium permanganate solution aids greatly in the time-saving
advantages of the process.
In a hydrochloric acid solution of a mineral phosphate an aliquot
part of the filtrate representing about 250 milligrams of calcium
oxid, usually about twenty-five cubic centimeters, should be taken
for the analysis. Ammonia is added in slight excess and then the acid
reaction restored with hydrochloric until shown plainly by litmus. The
solution is then heated and the lime thrown down by adding a solution
of ammonium oxalate in excess. In order to secure a greater dilution
of the hydrochloric acid after the precipitation has been made, water
should be added until the volume is half a liter. Before filtering, the
whole should be cooled to room temperature. The precipitate should be
washed first with cold and afterwards with warm water. The well-washed
precipitate is dissolved in hot dilute sulfuric acid and the solution,
while hot, titrated with a standard solution of potassium permanganate
set by a solution of ammonio-ferrous sulfate.
If one cubic centimeter of the permanganate represent 0.005 gram of
iron it will correspond almost exactly to 0.0035 gram of calcium oxid.
_Example._—Sample of rather poor mineral phosphate, five
grams in half a liter. Strength of potassium permanganate, one
cubic centimeter equivalent to 0.00697 gram of iron and to
0.003484 gram of calcium oxid.
Twenty-five cubic centimeters of the solution, representing one
quarter of a gram, in which the lime was precipitated as above
described, required 9.6 cubic centimeters of the potassium
permanganate to saturate the oxalic acid. Then
9.6 × 0.003484 = 0.0334464 gram,
or 13.38 per cent of calcium oxid. The method is also applicable
to basic slags.
Public-domain text, read in full here on John Shaqi.
Reviews
Reviews
No reviews yet
Be the first to share your thoughts on this work.
Join the Discussion
Join the discussion
Sign in to leave a comment or review.
Sign InorCreate an account