A novel, efficient, highly stable, and reusable organic inorganic hybrid material was synthesized via silanization of silica gel with (3-aminopropyl)trimethoxysilane followed by covalent immobilization with diacetylmonoxime. The grafting was confirmed by FTIR, elemental analysis, C-13 CPMAS NMR spectroscopy, SEM, TGA, and BET surface area analysis. The modified solid phase was found to be highly selective for Cu(II) ions under near neutral conditions with a high sorption capacity of 0.93mmolg(-1) and a preconcentration factor of 250. Isotherm and kinetic parameters correlated well with the Langmuir and pseudo-second-order model. The recovery of analyte was efficiently performed for ten consecutive adsorption-desorption cycles. The present environmentally benign and economical procedure was successfully applied for the separation and preconcentration of copper from fly ash ameliorated soil samples.