=123. Estimation of Vanadium.=—In the complete analysis of basic slags
it becomes necessary to determine the presence of vanadium and its
quantity. The method used in this laboratory for the purpose is the
volumetric process of Lindemann.[103] It is conducted as follows:
Dissolve four grams of the finely powdered slag in sixty cubic
centimeters of dilute sulfuric acid (1: 4), boil for a few minutes,
cool, make the volume up to 100 cubic centimeters, filter, and take
an aliquot part for the determination. Add decinormal potassium
permanganate solution in slight excess to secure the oxidation of the
vanadium to vanadium pentoxid. Add, drop by drop, a weak solution of
ferrous sulfate until the pink color just disappears. Prepare a ferrous
sulfate solution by dissolving 2.183 grams of piano wire in sulfuric
acid and making the volume to one liter. Titrate the vanadic mixture
with this solution until a drop of the clear liquor removed and brought
in contact with potassium ferricyanid shows a distinctive blue-green
color.
One cubic centimeter of the ferrous sulfate solution is equivalent to
0.002 gram of vanadium, 0.002888 gram of vanadium dioxid, and 0.003648
gram of vanadium pentoxid. The ferrous sulfate solution may also be
made and standardized by any of the approved methods in common use.
The method described by Blair, designed especially for the estimation
of vanadium in iron and steel, is conducted in the following
manner:[104] Five grams of the drillings are dissolved in fifty cubic
centimeters of nitric acid of 1.24 specific gravity. The solution is
evaporated to dryness in a porcelain dish and heated thereafter until
the nitrates are nearly decomposed. After cooling, the dried mass is
transferred to a mortar and finely ground with thirty grams of dry
sodium carbonate and three grams of sodium nitrate. The finely ground
materials are placed in a platinum dish and fused for an hour at a
high temperature. Spread the fused mass over the sides of the dish
while cooling, and afterwards dissolve in hot water, filter, and wash
until the volume is a little over half a liter. Add nitric acid to
decompose carbonates, but not completely, and boil to get rid of carbon
dioxid, being careful to keep the mass always slightly alkaline. Add
nitric acid, drop by drop, until slightly in excess, and then sodium
carbonate to marked alkalinity, boil, and filter. Add a slight excess
of nitric acid to the filtrate, and the development of a yellow color
will indicate the presence of vanadic acid. Add to the solution a
small quantity of mercurous nitrate and then an excess of mercuric
oxid, suspended in water to render the solution neutral and insure the
complete precipitation of mercurous vanadate. The mercurous salt also
precipitates phosphoric, chromic, tungstic, and molybdic acids which
may be present. Boil, filter, and wash the precipitate with hot water,
dry, and ignite. Fuse the residue with sodium carbonate and a little
nitrate.
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