Ordered mesoporous silica with hexagonal and cubic structure, type MCM-41 and MCM-48 respectively, were synthesized under basic media using pure silica, cetyltrimethylammonium bromide and tetramethylammonium hydroxide, for MCM-41 and tetraethylorthosilica, cetyltrimethylammonium and NaOH for MCM-48. The expanded materials were prepared by post-synthesis method with N-N dimethyldodecylamine (DMDDA) and dodecylamine (DDA). Small angle X-ray diffraction, nitrogen adsorption-desorption measurements, FT-IR and thermogravimetry were used to characterize the samples. The expanded materials were tested for adsorption of Cd2+, Co2+, Cu2+, and Pb2+ in aqueous solution. Aminated materials were found to be fast adsorbents for metallic ions cation with affinity for Cu2+, Pb2+, than for Cd2+ and Co2+ from single solution. In mixed metallic ions cation solutions, competition by the adsorption sites is likely to occur, the adsorption preference is for Cu2+ and Pb2+. The kinetic of the reaction is very rapid and follow pseudo-second order and clearly indicated that Langmuir model describe better the for metal ions adsorption on aminated mesoporous material than Freundlich model. (C) 2009 Elsevier B.V. All rights reserved.