Abstract: A method for the mercury thiocyanate spectrophotometric determination of chlorine in ore samples was reported in this paper. The sample was sintered with zinc oxidesodium carbonate and then leached with water. Chlorine in the sample solution was indirectly determined by mercury thiocyanate spectrophotometry. The results are in good agreement with those from other methods with precision of 1.74%RSD (n=6) for the sample with 1.08% chlorine. The method is suitable for the determination of chlorine in the samples with 0.02%～2% of chlorine with the advantage of simplity, rapidity, accuracy and less tedious procedure.