A novel functionalized silica gel with poly(diethylenetriamine bis(methylene phosphonic acid)) (SH-DETA-PDBMPA) was synthesized in order to improve the adsorption for transition metal ions from aqueous solutions. The material was characterized using infrared spectra (IR), X-ray diffractometry (XRD), scanning electron microscope (SEM), Brunauer-Emmett-Teller (BET) surface area measurement, porous analysis, thermogravimetric analysis (TG) and (29)Si Magic Angle Spinning Nuclear Magnetic Resonance ((29)Si MAS NMR). The application of this material in adsorption of transition metal ions revealed that SH-DETA-PDBMPA had excellent adsorption amount and high selectivity for Au(III), which provided a novel material for adsorbing this specious metal ions from aqueous solutions. (C) 2011 Elsevier B.V. All rights reserved.