Abstract:A method for determination of fluoride and chloride content in Iron-bearing dust and sludge by ion chromatography was established with steam distillation for sample pretreament. The fluoride and chloride were effective vaporized using water vapor distillation. The method was based on ion chromatography separation under the condition eluent with 3.2 mmol/L Na2CO3 plus 1.0 mmol/L NaHCO3, by using of the Metrosep A Supp 5-250 anion –exchange column and suppressed conductivity detector. As a result, the correlation coefficient were fluoride and chloride 0.9996 and 0.9997. The standard addition recoveries were in the range of 93.0%～97.9% and 92.4%～97.1%. the sample detection limit were 0.004% and 0.006%. Values of RSD’s (n=10) found were in the range of 3.17%～5.90% and 0.79%～2.94%. The method has low detection limit, good precusion and high accuracy, which meet the requirement for fast and accurately testing fluoride and chloride content in Iron-bearing dust and sludge.