An electrochemical hydride generation (ECHG) technique was developed to improve the determination of thallium by atomic spectrometry. The technique is based on the catholyte variation system for production of thallium hydride. Using Pb-Sn alloy as cathode, a transient peak shaped signal was achieved and its height, the maximum absorbance value, was taken as an analytical parameter. Parameters that might affect the hydride generation efficiency were investigated and the analytical performance of the method under the optimized experimental conditions was assessed. The linear range was 1-250 ng mL(-1) for thallium and the relative standard deviation of the method was 4.2% (RSD, n=7). The LOD for thallium was found to be 0.8 ng mL(-1), showing a significant improvement relative to conventional chemical hydride generation techniques. The proposed method was applied to the determination of thallium in unalloyed zinc standard reference material. This method offers high sensitivity, simplicity, rapidness, freeness from reagent and low acid consumption.