A new chelating resin, 2-mercaptobenzothiazole loaded Amberlite XAD-1180 was prepared and used for separation and preconcentration of Cd(II) and Pb(II) ions prior to their determinations by flame atomic absorption spectrometry. The optimum pH for simultaneous retention of the elements and the best elution means for their simultaneous elution were 9.5 and 2 mol L-1 HNO3, respectively. The detection limits for Cd(II) and Pb(II) were 0.35 and 5.0 mu g L-1, respectively. The accuracy of the method was confirmed both by analyzing the certified reference material (RM 8704 Buffalo river sediment) and performing recovery studies. (C) 2013 Production and hosting by Elsevier B.V. on behalf of King Saud University.