Mesoporous aluminosilicates, have been prepared with various mole ratios of Si/Al and Cethyltrimethylammonium bromide (CTAB). They have been characterized by XRD, nitrogen adsorption/desorption measurements, FT-IR and thermogravimetry. Adsorption behavior of heavy metal ions on this adsorbent have been studied and discussed. The results show that incorporation of aluminum ions in the framework of the mesoporous MCM-41 has transformed it into an effective cation exchanger. The K-d values of several metal ions have been increased. Separation of Sr(II)-Ce(III), Sr(II)-U(VI) and Cd(II)-Ce(III) has been developed on columns of this novel mesoporous cation exchanger. (C) 2009 Elsevier B.V. All rights reserved.