The investigation reports preparation of two new adsorbent materials, SiPOLHET and SiPOLHOM, by attachment of linear poly(amido amine) (PAA) to silica surface by adopting heterogeneous and homogeneous modification procedures, respectively. Their structures were characterized by FTIR, C-13 and Si-29 NMR spectroscopy. Surface morphologies and corresponding elemental composition were determined by using SEM and EDS techniques. The metal binding characteristics of the adsorbents towards Cu2+ and Ni2+ were studied in dilute aqueous solution which presents an interesting aspect of increasing trend. (C) 2009 Elsevier B.V. All rights reserved.