The Separation and Concentration of Acetylacetonato Chelates Using a Benzene Column

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This paper is concerned with the application of the zone-melting technique to metal-chelate compounds. An organic solvent which is liquid at room temperature such as benzene, and several acetylacetonato and thenoyltrifluoroacetonato chelates as solutes were prepared. The effective distribution-coefficient <I>k</I> dependence on the molecular weight was revealed by the normal freezing technique. In the deployment process, the acetylacetonato chelates of Fe and Th were chosen as solutes because their <I>k</I> values were different. The experiment was carried out at 2 cm/hr, the rate of zone travel. When a 30-cm column was used, the "removal percentages" of Fe from Th were 41 and 85% for 3 and 5 zone passes respectively. However there was a 22% loss of Th in the latter case. Furthermore, a remarkable concentration was found, and it was shown that the concentration effect may be useful for micro-analysis. At this stage, a relatively large bubble of benzene was observed at the liquid and solid interface; therefore we can call this "three-phase zone-melting."
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