By Anil K. Mukherji, R. Belcher and M. Frieser (Auth.)

ISBN-10: 0080068863

ISBN-13: 9780080068862

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Extra info for Analytical Chemistry of Zirconium and Hafnium

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Dry at 125-140°C for 10-12 hr. 5 g of the dried precipitate into a tared porcelain crucible. Heat slowly tp 40 ANALYTICAL CHEMISTRY OF ZIRCONIUM AND HAFNIUM drive off the selenium dioxide and ignite at 800-1000°C to the oxide. Cool and weigh the mixed oxides. The hafnium content may be calculated from the following: Note: (1) All foreign metal ions should be absent and the sample should contain only zirconium and hafnium. (2) Only chloride solutions should be used. 5 % when the mixture contains approximately 25 % HfOa.

5 N HC1 or H 2 S0 4 . Composition of the precipitate according to both is Zr(C13H10O2N)4. According to Ryan, the precipitate has a variable composition when obtained from hydrochloric acid solutions, and must be ignited to the oxide. Precipitate obtained from sulfuric acid solutions can be weighed directly. 5 Nacidity. Add dropwisewith stirring, a slight excess of the reagent (4 % in 95 % ethanol) and digest over a steam bath for about 1 hr. Cool, filter through a porcelain filter crucible, and wash with cold water.

Separation from niobium and tantalum can be achieved by precipitating zirconium either by salicylhydroxamic acid or 7V-benzoyl-7V-phenylhydroxylamine. Thorium and the rare earth ions may be precipitated by excess oxalic acid, leaving zirconium in the filtrate. For complete separation the precipitated oxalates should be boiled with cone, sulfuric acid until decomposed, then diluted, nearly neutralized with ammonium hydroxide, and reprecipitated with excess oxalic acid. Combined filtrates contain all the zirconium.

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Analytical Chemistry of Zirconium and Hafnium by Anil K. Mukherji, R. Belcher and M. Frieser (Auth.)

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