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Comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-TOFMS) was applied to the quick qualitative analysis of 17 types of polychlorinated dibenzo-p-dioxins and furans (PCDD/Fs) from the iron ore sintering process.The GC×GC-TOFMS parameters were evaluated and optimized to yield a complete separation for the 17 types of PCCD/Fs from interference and to the attainment of high sensitivity.After optimization,all the 17 types of PCCD/Fs were separated within 42.5 min.The critical and most toxic tetrachlorodibenzop-dioxin (TCDD) detection can be up to 0.5 μg/L.The method was used to analyze real fly ash samples.Accurate identification and determination of all the analyses were by GC×GC,mass spectrum library and ion ratio.The technique is thought to be a substitute for and a supplement to high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS) in the field of dioxin analysis.