色谱

色谱 ›› 2014, Vol. 32 ›› Issue (9): 955-959.DOI: 10.3724/SP.J.1123.2014.05030

• 特别策划：新型污染物色谱分析专栏 • 上一篇    下一篇

同位素稀释高分辨气相色谱-高分辨质谱法检测烟道气中的低氯代二恶英

唐琛1,2, 刘启鹏1, 田振宇2, 解惠婷2, 王梦京2, 刘文彬2   

  1. 1. 北京科技大学土木与环境工程学院环境工程系, 北京 100083;
    2. 中国科学院生态环境研究中心, 北京 100085
  • 收稿日期:2014-05-22 修回日期:2014-07-10 出版日期:2014-09-08 发布日期:2014-08-30
  • 通讯作者: 刘文彬
  • 作者简介:刘文彬，liuwb@rcees.ac.cn.
  • 基金资助:

    国家重点基础研究发展计划项目（2011CB201500）；中国科学院战略性先导科技专项（XDB14000000）；国家自然科学基金项目（21321004）.

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

TANG Chen1,2, LIU Qipeng1, TIAN Zhenyu2, XIE Huiting2, WANG Mengjing2, LIU Wenbin2   

  1. 1. Department of Environmental Engineering, School of Civil and Environmental Engineering, University of Science and Technology Beijing, Beijing 100083, China;
    2. Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China
  • Received:2014-05-22 Revised:2014-07-10 Online:2014-09-08 Published:2014-08-30

PDF

278

被引次数

16

摘要：

建立了同位素稀释高分辨气相色谱-高分辨质谱检测烟道气中痕量低氯代二恶英的分析方法。采用索氏提取富集烟道气样品中的目标物，提取液经过复合硅胶柱和碱性氧化铝柱净化后，进行高分辨气相色谱-高分辨质谱检测。采用DB-5MS毛细管色谱柱（30 m×0.25 mm×0.25 μm）分离，以保留时间和同位素特征离子丰度比定性，以与同位素的峰面积比值定量。实验结果表明，方法的回收率为66.6%~112.5%，相对标准偏差（RSD）的范围为19.9%~40.5%（n=5），方法的检出限（LOD）为0.027~0.485 μg/L。应用该方法检测了3个焚烧炉烟道气样品，回收率在85.7%~137.0%范围内，样品中目标物含量分布在11.4~9183 pg/Nm3之间。结果表明该方法适合用于烟道气中痕量低氯代二恶英的检测。

关键词: 低氯代二恶英, 高分辨气相色谱-高分辨质谱, 同位素稀释, 烟道气

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

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