Abstract: Ionic alkyl-lead compounds were determined using a FIA system having an Ar flow rate of 75 ml/min, 2.5% tartaric acid for HG, 4% H2O2 for mobilization of the hydride products and 0.5% NaBH4 reducing agent. The furnace temperature was 350°C for injection, 600°C for pre-treatment, 1600°C for atomization and 2400°C for glow-out and AAS peak heights were measured at 283.3 nm using a Perkin-Elmer Model 4100 ZL spectrometer. For di- and trimethyl-lead and di- and triethyl-lead in the concentration range 0.1-5 µg/l (as Pb), a sample loop of 1.5 mL gave linear calibration graphs except for trimethyl-lead which showed linearity from 0.1-2 µg/l. The detection limits of the four compounds were 19, 7, 25 and 21 ng/l, respectively, with RSD of 2.6-5.8%. Increasing the sample volume to 6 mL gave a detection limit of 1.5 ng/l for trimethyl-lead; use of a continuous-flow system with enrichment of a 50 mL sample gave detection limits 1 ng/l.