Abstract: Fluoride and Cl- ion in sulfide concentrate were separated by steam distillation, and their contents in the distillate were determined by ion chromatography. AG19 protective column and AS19 separation column were used for separation and 25.00 mmol·L-1 NaOH solution was used as eluant. Successive-auto regenerative chemical suppressor was adopted in the determination. Linear relationships between values of peak area and mass concentration of F- and Cl- were kept in the same range within 10.00 mg·L-1, with detection limits (3s) of 0.006 mg·L-1 for F- and 0.003 mg·L-1 for Cl-. The proposed method was used for the analysis of samples of copper sulfide concentrate, zinc concentrate and lead concentrate, giving values of recovery and RSD′s (n=11) in ranges of 94.1%-97.2% and 1.5%-2.3% for F-, 96.4%-101% and 1.1%-1.9% for Cl- respectively.