高分辨气相色谱-高分辨质谱分析2,5-二氯酚工业品中的二GFDA1英及多氯联苯

袁继委, 徐威力, 徐方曦, 张亦弛, 高媛, 陈吉平

现代化工 ›› 2020, Vol. 40 ›› Issue (S1) : 300 -305.

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现代化工 ›› 2020, Vol. 40 ›› Issue (S1) : 300-305. DOI: 10.16606/j.cnki.issn0253-4320.2020.S.068
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高分辨气相色谱-高分辨质谱分析2,5-二氯酚工业品中的二GFDA1英及多氯联苯

    袁继委, 徐威力, 徐方曦, 张亦弛, 高媛, 陈吉平
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Analysis on PCDD/Fs and PCBs in industrial grade 2,5-dichlorophenol by HRGC-HRMS

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摘要

建立了高分辨气相色谱-高分辨质谱方法分析2,5-二氯酚工业品中的二GFDA1英(PCDD/Fs)和多氯联苯(PCBs)。比较了2,5-二氯酚工业品经甲苯直接溶解后净化、溶解于0.15 mol/L NaOH水溶液中再与正己烷液液萃取后净化两种前处理方法对PCDD/Fs及PCBs出峰峰型和回收率的影响。对于空白样品,两种方法PCDD/Fs及PCBs回收率相差不大。对于实际样品,先溶解于碱液再液液萃取的方法明显优于直接溶解后净化,除PCB 169回收率为49%外,其他所有PCDD/Fs和PCBs组分的回收率都大于80%,均满足标准HJ 77.3—2008和EPA1668C (2010)的质控要求;PCDD/Fs和PCBs的检出限分别为0.005 0~0.044和0.016~0.12 ng/kg;将本方法应用于2,5-二氯酚工业品分析,PCDD/Fs毒性当量浓度为100和135 ng TEQ/g,PCBs毒性当量浓度为6.5和21 ng TEQ/g。

Abstract

A method using high resolution gas chromatography-high resolution mass spectrometry method is established for the analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) and polychlorinated biphenyls (PCBs) in industrial grade 2,5-dichlorophenol.The sample is pretreated through direct dissolution in toluene and dissolution in 0.15 mol·L-1 NaOH aqueous solution followed by liquid-liquid extraction with n-hexane,respectively.The chromatographic peaks and recoveries of PCDD/Fs and PCBs are compared.No obvious differences are found in the recoveries of PCDD/Fs and PCBs in the quality blank samples.As for actual samples,the method of dissolution in 0.15 mol/L NaOH aqueous solution followed by liquid-liquid extraction with n-hexane achieves higher recoveries.The recoveries of all PCDD/Fs and PCBs homologous except PCB169 exceed 80%,which meet the quality control requirements of environmental standard methods HJ 77.3—2008 and EPA1668C(2010).The detection limits by this method are 0.005 0-0.044 ng·kg-1 for PCDD/Fs and 0.016-0.12 ng·kg-1 for PCBs.This method is used to detect PCDD/Fs and PCBs in two kinds of industrial grade 2,5-dichlorophenol products,indicating that the toxic equivalent quantity concentrations of PCDD/Fs are 100 g TEQ/g and 135 ng TEQ/g,respectively,and that of PCBs are 6.5 and 21 ng TEQ/g,respectively.

关键词

持久性有机污染物 / 同系物分布 / 工业2,5-二氯酚 / 多氯联苯 / 二 GFDA1 英

Key words

persistent organic pollutants / homologous distribution / industrial grade 2,5-dichlorophenol / polychlorinated biphenyls / polychlorinated dibenzo-p-dioxins and dibenzofurans

Author summay

袁继委(1973-),男,本科,高级工程师,研究方向为环境监测与分析

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高分辨气相色谱-高分辨质谱分析2,5-二氯酚工业品中的二GFDA1英及多氯联苯[J]. 现代化工, 2020, 40(S1): 300-305 DOI:10.16606/j.cnki.issn0253-4320.2020.S.068

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