Abstract: Aiming at the shortage of current separation and purification technique of Al2O3 column for polychlorinated dibenzo-p-dioxins and dibenzofurans(PCDD/Fs),the application of the newest purifying technique for PCDD/Fs,porous graphitic carbon(PGC) column-high performance liquid chromatography (HPLC) method,was introduced.Through the study on the actual separation conditions and analysis process of (()13C)-PCDD/Fs,the automation of final purifying technique was obtained.The method was applied in the analysis of PCDD/Fs in the soil and it was shown that the technique had good separation effect for PCDD/Fs and the recovery rate was stable at over 99%,being more automatic and safer and with less solvent used.The technique could eliminate man-induced disturbance and reduce failures in the operation.