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Abstract: A metal ion-imprinted microsphere was prepared by surface molecular template polymerization. Trimethylolpropane trimethacrylate (TRIM), zinc ions, 1,12-dodecanediol-O, O'-diphenyl phosphonic acid (DDDPA) were used as a crosslinking agent, an imprint molecule, and a functional host molecule. The Zn(II)-imprinted microspheres, which are spherically well-defined particles, were prepared by using water- in-oil-in-water (W/O/W) multiple emulsions. The combination of TRIM and DDDPA serves to align the recognition sites resulting in better template sites produced on the polymer surface. We firstly conducted diagnostic zinc- and copper-ion adsorption tests with the Zn(II)- imprinted and unimprinted microspheres in order to make an assessment on the effectiveness of the molecular imprinting technique. Further, the metal-imprinted microspheres were applied to the column operation. The separation and recovery of metals were carried out by an adsorption column packed with the Zn(II)-imprinted microspheres. This performance was compared to that of commercial chelating resins that possess similar phosphoric functional groups. The Zn(II)- imprinted polymer shows an extremely high selectivity to the imprinted zinc ions compared to that of the commercial chelating resin. (C) 2000 John Wiley & Sons, Inc