Abstract: The concentrations of fluorine and chlorine in flue gas of a glass furnace in Wuhan were determined by using experimental comparative method. The result shows that the sampling error of EPA Method 26A is lower. Through one sampling it can obtain multiple parameter data such as gaseous fluorine, gaseous chlorine, hydrogen chloride, halogen, etc. with the advantages of saving time and human resources. The chromatographic conditions for analyzing flue gas absorption are optimized. The KOH concentration of EG40 eluent automatic generator is set at 30 mmol/L, with the eluent flow rate of 1.2 mL/min and the injection volume of 25 μL. The method could fully meet the testing requirements of F ^-, Cl ^- for flue gas absorbent for its high precision with the relative standard deviation RSD less than 3.0% and good accuracy with sample average recovery rate of 96.7%-104.3%.