By mean of heterophase polimarzation on the silica gel surface has been made in situ immobilization of poly[4-methacroyloxy-(4'-carboxy-3-Chloro)-azobenzene] and has been received new organic-mineral composit material. The fact of polymer immobilization has been confirmed by IR spectroscopic method and thermogravimetric analysis combined with mass spectrometry. According to the results of thermogravimetric analysis, has been found the mass of the immobilized polymer is 13.33%.The synthesized composite revealed sorption activity to the ions of Cu (II), Pb (II) and Fe (III) micro quantities in a neutral water environment. Maximum sorption ions Cu (II), Pb (II) and Fe (III) degree is reached during first contact hour in static sorption condition. According to the results of isotherms sorption treatment has been determined the silica gel surface poly [4-methacryloxy- (4'-carboxy-3-chloro)-azobenzene] modification led to the sorbtion volum Cu (II) ions more than 1.5 times, for ions Pb (II) - 3.6 times, but for Fe (III) ions - almost 2 times.