The need for highly reliable methods for the determination of trace elements has been recognised in analytical chemistry and environmental science. A method for the trace analysis of Pb and Cd in natural waters is described. In a preconcentration step, 500 ml of an aqueous sample containing lead and cadmium were extracted into 3.5 ml of a solution containing a complexing agent (dithizone) in xylene. Subsequently, the dithizonate complexes were back-extracted into 600 mul of nitric acid solution for direct determination by flame atomic absorption spectrometry. Important microextraction parameters were optimised using spiked deionised water. The 3sigma detection limits, relative standard deviations and linear calibration graphs were, respectively, 0.39 mugl(-1), 6.3% and 1.0-20.0 mugl(-1) for lead and 8.2 ngl(-1), 4.0% and 0.05-1.0 mugl(-1) for cadmium for solvent microextraction times of 4 min and microvolume back-extraction times of 1 min. The preconcentration factors were 543- and 331-fold for lead and cadmium, respectively.