A simple and rapid method for spectrophotometric determination of palladium from highly acidic and highly radioactive nuclear waste using -benzoin oxime (ABO) as extractant and isobutyl methyl ketone (hexone) as diluent has been developed. The method can be employed over a wide range of nitric acid concentrations and for palladium concentrations in the range of 1·10–5M to 4·10–4M in the organic phase. The molar absorptivity was found to be 4·103l·mol–1·cm–1. Influence of various heavy metal ions, fission products and corrosion products was studied. The method was found to give a precision and accuracy better than 4% at 100 g of palladium.