A separation-preconcentration procedure based oil the coprecipitation of lead(II) and chromium(III) ions with copper(II)-5-chloro-2-hydroxyaniline system has been developed. Effects of pH, sample volume and interferences oil the recovery of the metal ions were investigated. The detection limits corresponding to three times the standard deviation of the blank were found to be 2.72 mu g L-1 for lead and 1.20 mu g L-1 for chromium. The preconcentration factor is 50. The effectiveness of the present method was assessed by determining analyte metals in GBW 07309 stream sediment and NIST SRM 1633b coal fly ash certified reference materials. The method was successfully applied to the determination of trace lead and chromium in environmental samples. (C) 2008 Elsevier B.V. All rights reserved.