The goal of present study is preparation, characterization of magnetic alginate/perlite composite microspheres and to investigate the usability of produced microspheres for the removal of lead and nickel ions from aqueous solution. The effect of perlite concentration, initial metal ion level and the pH of the solution on the heavy metal adsorption capacity of microspheres were investigated. Iron oxide particles were prepared by simple precipitation method. Ionic gelation method was utilized to synthesize the microspheres. Swelling studies showed that addition of perlite to iron oxide-containing micropsheres decreased the swelling degree of the microspheres. SEM analysis indicated that microspheres were almost spherical with rough surface. SEM-EDX showed that alginate/perlite microspheres composed of C, O, Na, Al, Si, K, Cl and Fe. TGA analysis indicated that incorporation of perlite improved the thermal properties of microspheres. Adsorption capacity of microspheres reached the maximum value when the perlite/alginate ratio=2 (wt./wt.), but then adding more than this value significantly decreased the adsorption capacity of microspheres. [ABSTRACT FROM AUTHOR]