A low temperature oxidation process has been developed to separate Pb from Zn in a complexly contaminated scrubber dust. The material consists of approx. 50% galena (PbS) and sphalerite/wurtzite (ZnS), and also an amorphous component, a variety of different silicate and carbonate phases as well as naturally-occurring radionuclides and oil and grease. The two-stage process consists of a grinding stage followed by placing this material into a hydrogen peroxide solution. The resultant oxidation reaction is violently exothermic — the temperature rises spontaneously to approx. 96°C. The amount of solid phases remaining after completion of the reaction was reduced by approx. 40% and consisted largely of insoluble lead sulphate which retained the bulk of the radionuclides. Almost all of the zinc was placed into solution by this process as was the Cd, Re and Cu. The total PAH content of the original Theisenschlamm (468 ppm) was reduced to 11.25 ppm in the residual sediment and the PCDD/PCDF concentrations were reduced by approx. 40%. The radionuclides are almost totally concentrated in the solid phase. The method shows considerable promise as a separation technique for very fine-grained sulphide-bearing residues.