A method is proposed for the determination of antimony in ores. Antimony is volatilized as antimony iodide by heating with ammonium iodide at a controlled temperature.The fusion mixture is extracted with hydrochloric acid and the antimony content is measured by atomic absorption spectrophotometry using an air/ acetylene flame. The time taken for analysis when comparedwith existing fusion and separation procedures is considerably reduced. Cations and anions likely to be present in antimony ores were also studied for possible interference effects but were not found to interfere.