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-5 MS毛细管色谱柱（30 m×0.25 mm×0.25μm）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0.027-0.485μg/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11.4-9 183 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。
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 sampies 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 ttRGC on a DB-SMS column （30 m×0. 25 mm×0.25 μm） and determined by HRMS. The identi- fication of monoto 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 monoto 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 9 183 pg/Nm3. The results indicated that the method can be applied to the precise determination of monoto tri-CDD/Fs at trace level in stack gas.
出处
《色谱》
CAS
CSCD
北大核心
2014年第9期955-959,共5页
Chinese Journal of Chromatography
基金
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)
关键词
高分辨气相色谱-高分辨质谱
同位素稀释
低氯代二恶英
烟道气
high resolution gas chromatography-high resolution mass spectrometry （HRGC-HRMS）
isotope dilution
monoto tri-chlorinated dibenzo-p-dioxins and dibenzofurans （ mono-to tri-CDD/Fs）
stack gas
