Ionic alkyllead compounds are extracted from water into carbon tetrachloride by complexation with sodium diethyldithiocarbamate while inorganic lead is effectively removed through the application of EDTA. Evaporation of the organic solvent followed by digestion of the organolead complexes with nitric acid allows the determination of the sum of the ionic alkyllead compounds by graphite furnace atomic absorption spectrometry with an over-all recovery of 85 ± 6% and a detection limit of a few ng l–1.