Determination of mono- to tri-chlorinated dibenzo-p-dioxins and dibenzofurans in stack gas using isotope dilution high resolution gas chromatography- high resolution mass spectrometry

doi:10.3724/SP.J.1123.2014.05030

Abstract

Abstract:

A method for the determination of mono- to tri- chlorinated dibenzo-p-dioxins and dibenzofurans (mono- to tri-CDD/Fs) in stack gas using isotope dilution high resolution gas chromatography-high resolution mass spectrometry (HRGC-HRMS) was developed. The samples were extracted by Soxhlet extraction, and then the extracts were concentrated and purified using a multilayer silica gel column and a basic alumina column. The analytes were separated by HRGC on a DB-5MS column (30 m×0.25 mm×0.25 μm) and determined by HRMS. The identification of mono- to tri-CDD/Fs was based on the retention times of ¹³C-labelled standard and the abundance ratios of the two exacted mass-to-charge ratios. The quantitative analysis was performed using the ratios of the integrated areas of the ¹³C-labelled standards. This method had the recoveries ranging from 66.6% to 112.5% and the relative standard deviations (RSD) ranging from 19.9% to 40.5% (n=5). The limits of detection (LODs) of this method for the mono- to tri-CDD/Fs were ranging from 0.027 to 0.485 μg/L. Three stack gas samples from waste incinerators were measured using this method, with the recoveries ranging from 85.7% to 137.0% and the concentrations ranging from 11.4 to 9183 pg/Nm³. The results indicated that the method can be applied to the precise determination of mono- to tri-CDD/Fs at trace level in stack gas.

Key words: high resolution gas chromatography-high resolution mass spectrometry (HRGC-HRMS), isotope dilution, mono- to tri-chlorinated dibenzo-p-dioxins and dibenzofurans (mono- to tri-CDD/Fs), stack gas

CLC Number:

O658

TANG Chen, LIU Qipeng, TIAN Zhenyu, XIE Huiting, WANG Mengjing, LIU Wenbin. Determination of mono- to tri-chlorinated dibenzo-p-dioxins and dibenzofurans in stack gas using isotope dilution high resolution gas chromatography- high resolution mass spectrometry[J]. Chinese Journal of Chromatography, 2014, 32(9): 955-959.

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