Gallium, which is extensively used in the production of semiconductor materials, is present at the parts per million level in Bayer's liquor. The low concentration of gallium in the liquor, along with the high concentration of aluminum, prompted the use of chelating ion exchangers as an alternative separation process. A chelating ion exchange resin with hydroxamic groups attached to the copolymer of acrylonitrile-divinylbenzene has been prepared by suspension polymerization followed by hydrolysis and chelation with hydroxylamine hydrochloride. Adsorption studies of gallium, using the above hydroxamic acid resin, were carried out. Adsorption was dependent on particle size of the resin and optimum conditions are determined for obtaining 0.3- to 0.5-mm particles by varying the composition of the emulsion, using a secondary polymerization technique, and adding of diluents. Acrylic acid, as a diluent in the copolymer matrix, was found to increase the particle size and stability of the resin. IR studies, carried out for the products obtained at various stages, confirmed the conversion of polymer to resin with a hydroxamic acid group and its complex formation with gallium. Both batch and column studies were carried out for the determination of the capacity of the resin with synthetic Bayer's liquor containing gallium and commercial Bayer's liquor. Scaled-up column studies were carried out with commercial Bayer's liquor to test the cyclability and stability of the resin. It was observed that chelated ion exchange resin could be recycled up to 30 times. The optimal liquid to solid phase ratio was found to be 1:12. (C) 2004 Wiley Periodicals, Inc.