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The results of preliminary tests showed that it is possible to separate zirconium and hafnium in sulphate solution using high molecular weight liquid amines. Tertiary amines are considered to be the most promising extractants because of their high capacities. A separation factor of the order of 10 was obtained from an aqueous solution containing 10 g/l zirconium oxide and 0.2 g/l hafnium oxide at a pH value of 0.5 units using tertiary amines. 0.2 M organic solutions of tertiary amines have a capacity of approximately 6 g/l zirconium oxide. Alamine 336 has been selected for more detailed study. Substantially, complete separation of zirconium and hafnium was obtained in a five stage countercurrent experiment using alamine 336. Hafnium was not detected by spectrographic means in the organic phase of the final stage. The results of preliminary tests with fluoride solutions were inconclusive, revealing a lack of fundamental knowledge of the chemistry of zirconium and hafnium fluoride complexes in solution. However, these tests are to be repeated with modifications. The extraction isotherm of zirconium in sulphate solution extracted by tri-iso-octylamine was shown to correspond to the theory developed by Dr PJ Lloyd. A general theory of separation using liquid amines was developed and tests designed to prove its applicability are in progress.
Analytical Chemistry of Zirconium and Hafnium compiles literature on the characterization and analysis of zirconium and hafnium. Various methods in studying the properties of the featured elements are presented in this book. This book also discusses the aqueous solutions of zirconium and hafnium. It then explains the methods such as dissolution of ores and alloys, detection and identification, and gravimetric determinations. This text further examines the titrimetric, electrometric, and absorptiometric methods, as well as methods of separations using ion-exchange and using solvent extraction, along with separation of hafnium from zirconium. The latter part of this text presents methods such as spectrographic analyses, X-ray analyses, and neutron activation analysis and separation of tracers. This book will come in handy for chemists and chemistry students, as well as for others interested in studying zirconium and hafnium.
The theoretical aspects of solvent extraction using amine extractants were considered. In particular the extraction of the disulphato-zirconic and disulphato-hafnyl complexes by tri-n-octylamine was studied. The elementary theory was found to be valid in the case of zirconium and hafnium, whose association numbers are equal. Equations describing the equilibrium curves were verified to be of form:- y1/x1 = E1 [M - n (y1 + y2)] y2/x2 = E2 [M - n (y1 + y2)]. A graphical procedure for the determination of ideal stage requirements in the case of the separation of zirconium and hafnium was postulated for the limited experiments performed. A process for the production of nuclear grade zirconium was designed. The zirconium-hafnium separation step was designed on the basis of the developed theory. The cost of nuclear grade zirconium oxide so produced was found to be comparable with that produced by existing processes.