The development of a process for the extraction of antimony from materials produced by Greenbushes Tin Limited has been carried out based on theoretical and laboratory studies. The materials treated have included concentrates of tantalite and cassiterite containing antimony at levels ranging from 0.3% to 2%. Roasting under controlled atmospheres is required to stabilise Sb203 rather than the low vapour pressure metal or higher oxide. Sulphidising additives such as pyrite, pyrrhotite or sulphur give enhanced antimony removal from tantalite and cassiterite at roasting temperatures of 900° to 1100°C. Substantial elimination of antimony to levels of 0.1% or less was Achieved.