The determination of trace amounts of Cd, Cu and Pb in riverine, estuarine, sea water and in urine samples, using a flow injection on-line preconcentration procedure coupled with electrothermal atomic absorption spectrometry, was investigated, The sorption material used consists of macrocyclic ligand immobilised on a silica gel support. The sample at pH 1.6 is loaded onto a 50 mu l column for a specific time interval. The column is then washed with a dilute nitric acid solution (pH 3) and emptied by pumping air through the column. The column is eluted with 40 mu l of 2.5 mol l(-1) nitric acid solution and the eluate introduced into the electrothermal atomiser. Detection limits (3 sigma) of 0.8, 46 and 20 ng l(-1) were obtained for Cd, Cu and Pb, respectively. The accuracy of the procedure was tested with water and urine certified reference materials. (C) 1999 Elsevier Science B.V. All rights reserved.