A sensitive and selective method for the simultaneous determination of copper and bismuth by adsorptive stripping was developed using nuclear fast red (2-anthracenesulfonic acid, 4-amino-9,10-dihydro-1,3-dihydroxy-9,10-dioxo-, monosodium salt) as selective complexing agent onto hanging mercury drop electrode. In a single scan both metals gave peaks that were distinctly separated by 85mV allowing their determination in the presence of each other. Optimal analytical conditions were found to be: nuclear fast red concentration of 80μM, pH of 2.8 and adsorptive potential of −300mV versus Ag/AgCl. With accumulation time of 180s the peaks currents are proportional to concentration of copper and bismuth over the 1–100 and 5–60ngmL −1 range with detection limits of 0.2 and 1.2ngmL −1 , respectively. The procedure was applied to simultaneous determination of copper and bismuth in some real samples.