This paper presented the synthesis of a novel composite adsorbent silica gel microspheres encapsulated with 5-sulfosalicylic acid functionalized polystyrene (SC-PS-azo-SSA). It was characterized by titration method, FT-IR (Fourier transform infrared spectrometer), SEM (scanning electron microscope), EDXAS (energy dispersive X-ray analysis system), etc. SG-PS-azo-SSA has been used to investigate the adsorption of Mn(II), Fe(III), Co(II), Ni(II), Zn(II), Cd(II), Hg(II), Pd(II), Cu(II), Ag(I) and Au(III) from aqueous solutions. The research results revealed that SG-PS-azo-SSA has the better adsorption capacity for Cu(II), Ag(I) and Au(III). Langmuir and Freundlich isotherm models were applied to analyze the experimental data and the adsorption of Cu(II), Ag(I) and Au(III) on SG-PS-azo-SSA fitted well to the Langmuir isotherm equation. The obtained maximum adsorption capacity for Cu(II), Ag(I), and Au(III) is 0.472 mmol/g, 0.822 mmol/g and 0.810 mmol/g, respectively. Thus, silica gel encapsulated by 5-sulfosalicyclic acid functionalized polystyrene (SC-PS-azo-SSA) is favorable and useful for the removal of Cu(II), Ag(I) and Au(III) metal ions. (C) 2009 Elsevier B.V. All rights reserved.