Samples have been taken from a two-stage industrial gold roaster treating a pyrite/pyrrhotite/arsenopyrite concentrate, in order to describe the mineralogy, composition and surface area of the calcines. Sulphides oxidised to produce a porous magnetite in the first stage and a porous hematite in the second; pyrite predominantly roasted via a pyrrhotite intermediate. Sulphur was eliminated in both the first and second stages whereas arsenic was eliminated in the first but retained in the second, partly as rims on hematite particles. The finer sized particles from the cyclones and electrostatic precipitator, while having the greatest surface area, were the most refractory with respect to gold solubilisation, probably as a result of incomplete decomposition (through short-circuiting) in the first stage, and through a combination of factors such as overheating and entrapment of sub-microscopic gold in the second stage.