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

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

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Complete depolymerization was obtained only in presence of 2 N H 2 S0 4 . These results were attributed to the stability of zirconium sulfate complexes at these acidities and their ability to affect chain cleavage of polymeric zirconium species. It is well known that complexes formed by other anions like chloride, nitrate, and perchlorate are not as stable. Pilkington and Wilson (35) arrived at the following conclusions from their studies. (a) (b) (c) (d) Complete depolymerization of zirconium occurs only in presence of approximately 2 N H 2 S0 4 concentration and above.

Astanina and Ostroumov (133) reported improvement in Kumins' procedure if the precipitate is washed with 95 % ethanol to remove the excess reagent. 1560 g/1. (ii) Washing the precipitate with water only gave low results both for direct weighing and ignition. 34 ANALYTICAL CHEMISTRY OF ZIRCONIUM AND HAFNIUM (iii) Kumins' recommended method for washing gave high results for direct weighing but correct results on ignition. (iv) Washing the precipitate with a saturated solution of zirconium mandelate gave slightly low but consistent results for direct weighing.

Hafnium oxide content in the sample can be calculated by the following: OTHER SEPARATIONS Sulphide precipitation in acidic medium can be utilized to separate members of the hydrogen sulfide group from zirconium. Zirconium can be separated from titanium by precipitating zirconium phosphate in the presence of sulfuric acid and hydrogen peroxide. 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.

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