New adsorption materials for the metal ions were synthesized with β-diketones retained on the octadecyl-group bonded to silica gel (C18) to capture the metal ions. The β-diketones such as TTA and BFA were used as reagents for separation of the metal ions. The reaction ability of materials (Silica gel, C-18, TTA-C18 and BFA-C18) was evaluated by solid-liquid distribution behavior. It was found that these materials have adsorption ability with metal ions at pH 2-6. On the other hand, silica gel and C-18 could not react with metal ion at pH 2-5.5. It was confirmed that these metal ions were adsorbed on these materials by an ion-exchange reaction, and their selectivity series was Cu
2++>Ni
2+>Co
2+=Zn
2+>Mn
2+. The mutual separation ability was found to be better than that of reported inorganic ion-exchangers such as dihydrogen tetratitanate hydrate fibers. BFA-C18 had an especially high selectivity for Cu
2+.
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