A new organo-mineral composite material has been synthesized by in situ immobilization of poly[(4-methacroyloxy-(4 '-carboxy-2 '-nitro)azobenzene on the silicagel surface. As a result of thermogravimetric analysis and DSC-MS analysis it has been found that the composition of synthesized composite includes 10,1 wt. % of polymer. It has been found that the synthesized composite exhibits the sorption ability in terms of microquantities of Cu (II), Cd (II), Pb (II) and Fe (III) ions in a neutral aqueous medium. The maximum degree of sorption of ions Cu (II), Pb (II) and Fe (III) is achieved during the first minutes of contact, and for Cd (II) ions the equilibrium is established within a day. The sorption capacity of silica gel as a result of modification by this polymer increases with respect to Cu (II) ions more than 14 times, with respect to Pb (II) ions - 5 times.