A simple, sensitive and rapid method using differential-pulse polarography is described for the determination of organolead compounds (alkyl, aryl and mixed organolead chlorides) in dimethyl sulphoxide. The lowest experimental detection limit of most of these compounds was found to be 2 × 10^–7M with a relative standard deviation of 2–3%. The method can also be applied to the analysis of a mixture of some organolead compounds.