Coal fly ash is a waste by-product of the coal fire industry, which generates many environmental problems. Alternative uses of this material would provide efficient solutions for this by-product. In this work, nitric acid-etched coal fly ash labelled with 2-mercaptoethanol or thioglycolic acid was assessed for retention of Al(III), As(III), Cu(II), Cd(II), Fe(III), Mn(II), Hg(II), Ni(II), Pb(II) and Zn(II) ions. The bonding characteristics between the organic compounds with the solid support, as well as with the metal ions, were evaluated using various surface analytical techniques. Visualization of the organically-functionalized coal fly ash particle was possible using scanning electron microscopy (SEM), while the elemental composition of the functionalized material, before and after retention of the metal ions, was obtained by energy dispersive (ED)-X ray spectrometry (XRS) and electrothermal atomic absorption spectrometry (ETAAS). Fourier transform infrared (FT-IR) spectrometry and Raman spectrometry were used to obtain information about the functional groups. It was found that some metal(oid) ions (As, Ni, Pb, Zn) were coordinated through the mercaptan group, while other metal(oid)s (Al, Cd, Cu, Fe, Hg, Mn) were apparently bonded to oxygen atoms. A low-cost and effective solid phase retention system for extraction of heavy metals from aqueous solutions was thus developed. (C) 2013 Elsevier B.V. All rights reserved.