Lead and nickel were concentrated and separated after sorbing on Chromosorb-107 filled in a syringe prior to their determination by electrothermal atomic absorption spectrometry. To retain the analytes, the sample solution treated with or without ammonium pyrolidine dithiocarbamate (APDQ was drawn into the syringe filled with Chromosorb-107 and discharged back manually. Then the analyte elements were eluted by drawing and discharging the suitable eluent. The optimum experimental conditions for quantitative recoveries of analytes (amount of sorbent, pH of sample, concentration and kind of eluent, flow rates of sample and eluent and adding of the effect of complexing agent) were investigated. Nickel was quantitatively retained at pH greater than or equal to 6 irrespective of whether it was complexed with APDC while the quantitative sorption of lead was achieved at pH greater than or equal to 8 only if it was treated with APDC prior to passing through the sorbent. The lead and nickel retained on the sorbent were eluted drawing and discharging 4.5 M HNO3, respectively. If the concentration of analyte elements in the sample were too low to be detected, then they were concentrated by increasing the ratio of sample value to eluent volume as needed. The lead and nickel in spiked sea-water samples and in certified reference Apple-Leaves (NIST SRM 1515) standards were quantitatively (greater than or equal to 95%) recovered with R.S.D. of around +/-2%. (C) 2003 Elsevier Science B.V. All rights reserved.