Removal of toxic arsenite ions from aqueous solutions was investigated using an innovative hybrid nanocrystalline surfactant-modified akaganeite. This sorbent was prepared using ferric chloride as the precursor and a cationic surfactant, hexadecyltrimethylammonium bromide. From the experimental work, the material was found to be an effective adsorbent for the separation of arsenites. The chemical kinetics of the process was studied, described by a pseudo-second-order equation. The Freundlich adsorption isotherm was determined to examine the mechanism of sorption. FTIR measurements and XPS analysis gave useful information both on the sorbent synthesized and on the arsenite removal process. (c) 2006 Elsevier Inc. All rights reserved.