Ultrasonically-assisted cathodic stripping voltammetry at a boron-doped diamond electrode, has been developed for the detection of lead. At concentrations above 3 mM, linear sweep voltammetry was used to give the analytical signal from a cathodic strip of electrodeposited PbO 2 ; linearity was observed from 3±100 mM, with 3 mM being the lower detection limit. Square-wave voltammetry was then employed for the cathodic stripping step, to lower the detection limits of the technique while retaining linearity to the order of 10 À8 M. The procedure involves ultrasonic electrode cleaning, cathodic preconditioning and sono-anodic deposition of PbO 2 . This novel analytical tool is mercuryfree, oxygen insensitive and highly speci®c towards lead, yet still offers scope for further elemental diversity, particularly for the detection of copper and iron. The square-wave sono-cathodic stripping voltammetry technique was combined with an ultrasonically assisted acid digestion protocol to successfully determine the lead content of a contaminated sample of river sediment, offering signi®cant time saving over the currently used analytical procedure.