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A pressurized continuous annular chromatograph (CAC) has been developed for truly continuous ion exchange preparative separations. This device utilizes a slowly rotating annular bed of sorbent material, fixed multiple feed points, and fixed withdrawal locations. Most of our investigations have been performed with a 28-cm-diam by 60-cm-long CAC, but a larger model has recently been designed and constructed. A detailed study has been made of the separation of copper, nickel, and cobalt components from a simulated carbonate leach liquor of the Caron process for recovering nickel and cobalt from laterite ores. Recent studies have investigated the ion exchange separation of zirconium and hafnium from a sulfate feed solution. Nuclear reactor-grade zirconium, containing
In the course of a rather cursory examination of the elution of tetra-positive ions from the cation exchange resin Dowex 50 with hydrochloric acid solutions, the authors have discovered a very effective method of separating zirconium from hafnimu. In view of the great labor involved in preparing even reasonably pure hafnium compounds by existing methods, they feel that this procedure will prove very valuable to those interested in obtaining hafnium compounds free of zirconium. Although the conditions which give satisfactory separation were first worked out using microgram amounts of material and the radioactive tracer technique, the run described here, involving milligrams of material, illustrates the applicability of the method to the production of significant amounts of pure hafnium and zirconium.
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.
High-resolution pressurized ion exchange has been used successfully to study and separate hafnium and zirconium sulfate complexes by chromatographic elution from Dowex 50W-X8 (15 to 25 .mu.m) resin with sulfuric acid solutions. Techniques were developed to continuously monitor the column effluents for zirconium and hafnium by reaction with fluorometric and colorimetric reagents. Since neither reagent was specific for either metal ion, peak patterns were initially identified by using the stable isotopes 9°Zr and 18°Hf as fingerprints of their elution position. Distribution ratios for both zirconium and hafnium decrease as the inverse fourth power of the sulfuric acid concentration below 2N and as the inverse second power at higher acid concentration. The hafnium-to-zirconium separation factor is approximately constant (approx. 8) over the 0.5 to 3N range. Under certain conditions, an unseparated fraction was observed that was not retained by the resin. The amount of this fraction which is thought to be a polymeric hydrolysis product appears to be a function of metal and sulfuric acid concentrations. Conditions are being sought to give the highest zirconium concentration and the lowest acid concentration that can be used as a feed material for commercial scale-up in the continuous annular chromatographic (CAC) unit without formation of the polymer.
In the course of a rather cursory examination of the elution of tetra-positive ions from the cation exchange resin Dowex 50 with hydrochloric acid solutions, the authors have discovered a very effective method of separating zirconium from hafnimu. In view of the great labor involved in preparing even reasonably pure hafnium compounds by existing methods, they feel that this procedure will prove very valuable to those interested in obtaining hafnium compounds free of zirconium. Although the conditions which give satisfactory separation were first worked out using microgram amounts of material and the radioactive tracer technique, the run described here, involving milligrams of material, illustrates the applicability of the method to the production of significant amounts of pure hafnium and zirconium.