The beneficiation of tailings from Kolar Gold Mines involves the flotation of sulphides. Appreciable amounts of arsenic and antimony are expected to accompany gold in this process. The activation analysis of gold in these samples is facilitated by a preseparation of gold from arsenic and antimony. The present paper describes a method for the rapid analysis of gold in the concentration range 0.5 to 50 ppm using a simple pre-irradiation separation, with the recovery of gold being evaluated by an isotope dilution technique using198Au tracer.