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

引用本文: 唐琛, 刘启鹏, 田振宇, 解惠婷, 王梦京, 刘文彬. 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[J]. 色谱, 2014, 32(9): 955-959. doi: 10.3724/SP.J.1123.2014.05030 shu

Citation: 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. doi: 10.3724/SP.J.1123.2014.05030 shu

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,
,}

通讯作者: 刘文彬

基金项目:
国家重点基础研究发展计划项目(2011CB201500) (2011CB201500)

中国科学院战略性先导科技专项(XDB14000000) (XDB14000000)

国家自然科学基金项目(21321004). (21321004)

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:

English

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

1.
1. Department of Environmental Engineering, School of Civil and Environmental Engineering, University of Science and Technology Beijing, Beijing 100083, China;

Corresponding author: 刘文彬

Received Date: 22 May 2014
Fund Project:
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).

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:

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

通讯作者: 刘文彬

English

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

Corresponding author: 刘文彬

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

通讯作者: 刘文彬

English

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

Corresponding author: 刘文彬

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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