Ceramic hollow microspheres (CHMSs) were prepared to use as supports for the removal of heavy metal ions from industrial wastewater. A water extraction sol-gel technique was used to prepare porous CHMS by extracting water from an emulsion of LUDOX (silica colloid; SiO2, Aldrich Co.) and 2-ethyl-1-hexanol. Experiments were conducted to control pore size, wall thickness, and separation yield by examining the ratio of precursors (LUDOX and 2-ethyl-1-hexanol), catalyst (NH4OH), sintering temperature, surfactant (SPAN 80), extractant (n-butanol), stirring speed, and concentration of precursor (LUDOX). The results revealed that the optimum conditions were 20 ml of a 10 wt% solution of LUDOX, 10 ml of NH4OH, a sintering temperature of 500 degreesC, 0.4 mi of SPAN 80, 200 ml of n-butanol, and a stirring speed of 730 rpm/100 ml of 2-ethyl-1-hexanol. CHMSs were impregnated in Cyanex 272 and examined for their ability to remove heavy metal ions from a solution. Based on an experiment involving the removal of metal ions using CHMSs that were prepared under optimum conditions, Zn ion was removed at a level of 0.354 mmol/g at pH 4, which was about twice the adsorption capacity of CHMSs prepared by Wilcox (Mater. Res. Sec. Symp. Proc. 346, 201 (1994)).