By Anil K. Mukherji, R. Belcher and M. Frieser (Auth.)
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Extra info for Analytical Chemistry of Zirconium and Hafnium
Cool, filter through a porcelain filter crucible, and wash with cold water. Wash with two or three 5 ml portions of hot water (80°C) and dry at 110°C. 0970 = mg Zr The precipitate must be ignited to the oxide if hydrochloric acid solutions are used. Aluminum, bismuth, cadmium, chromium (III), copper, lead, magnesium, manganese, nickel, thorium, zinc, and the rare earths do not interfere. Ferric, cerium(IV), tin, titanium, and vanadium(V) give precipitates. Cerium (IV), tin(IV), and vanadium (V) interference can be prevented by the addition of hydrogen peroxide.
Cool below 20°C. Add enough EDTA to complex all the titanium. Add 5 ml of 10 % H 2 0 2 . Neutralize with aqueous ammonia (1:1) to the red-violet colour of xylenol orange. Acidify with nitric acid to pH 1-2. 05 M bismuth nitrate to an intense red color. Note. The highest permissible concentration is 35 mg Zr and 40 mg Ti in 150-300 ml. Hydrogen peroxide must be added to the solution after cooling because a small amount of EDTA is otherwise oxidized. Analysis of Zirconium, Thorium, and Titanium Mixtures After the titration of zirconium, it is not possible to determine thorium and titanium if both are present, for the following reasons : (1) Hydrogen peroxide must be added as a stabilizer for titanium and ammonium sulfate as a screening agent for thorium.
5 with chloroacetic acid buffer and titrate once more to yellow. Only thorium is titrated in the second titration. Successive Determination of Zirconium and Titanium(29) After the determination of zirconium, titanium was determined in the same solution by the addition of hydrogen peroxide and excess EDTA and back-titration with bismuth nitrate. 6 N) solution as described. Cool below 20°C. Add enough EDTA to complex all the titanium. Add 5 ml of 10 % H 2 0 2 . Neutralize with aqueous ammonia (1:1) to the red-violet colour of xylenol orange.
Analytical Chemistry of Zirconium and Hafnium by Anil K. Mukherji, R. Belcher and M. Frieser (Auth.)