The Mg-silicate microballoons containing CYANEX923 were prepared by W/O/W emulsion. The diameter of obtained micro-sphere particles was 10m and shell thickness was 2m. The adsorption of Co(II) and Ni(II) from aqueous solutions using prepared micro-sphere particles was investigated. Experiments were carried out as a function of solute concentration and temperature (25-60C). Several kinetic models were used to test the experimental rate data and to examine the controlling mechanism of the adsorption process. Equilibrium adsorption data were analyzed using Langmuir isotherm model. The results indicated that prepared micro-sphere particles can be used as an efficient adsorbent for the removal of Ni(II) and Co(II) from aqueous solution.