Fluid bed sulphation roasting followed by leaching at low pH was developed as a means of separating copper and bismuth from a mix- ture of flotation concentrates and flash fur- nace flue dust. A 65 tonne/day plant was established and typically achieves 89 percent copper extraction with negligible bismuth and iron extraction. Acid-chloride leaching of bismuth from copper leach residue was then established, with bismuth oxychloride being precipitated from solution by dilution with water. A small scale batch plant presently in operation typic- ally achieves 80 percent recovery of bismuth to bismuth oxychloride.