焦化废水中痕量苯并(a)芘的固相萃取和GC-MS检测方法  

A DETECTION METHOD FOR TRACE BENZO(a)PYRENE IN COKING WASTEWATER BY SOLID-PHASE EXTRACTION AND GC-MS ANALYSIS

作　　者：侯嫔[1] 张瑜[1] 彭莲 赵俊慧 卜庆伟[1] 王建兵[1] 贲伟伟[2] 强志民[2] HOU Pin;ZHANG Yu;PENG Lian;ZHAO Junhui;BU Qingwei;WANG Jianbing;BEN Weiwei;QIANG Zhimin(School of Chemical&Environmental Engineering,China University of Mining and Technology-Beijing,Beijing 100083,China;Key Laboratory of Drinking Water Science and Technology,Research Center for Eco-Environmental Sciences,Chinese Academy of Sciences,Beijing 100085,China)

机构地区：[1]中国矿业大学(北京)化学与环境工程学院,北京100083 [2]中国科学院生态环境研究中心饮用水科学与技术重点实验室,北京100085

出　　处：《环境工程》2022年第7期159-164,共6页Environmental Engineering

基　　金：国家重点研发计划(2018YFC0406404);中央高校越崎青年学者“资助计划”(2020QN09);中科院开放基金(18K05KLDWST)。

摘　　要：基于固相萃取(SPE)和气相色谱/质谱联用技术(GC-MS),建立了一种焦化废水中痕量苯并(a)芘(BaP)的定量分析方法。BaP水样添加甲醇改性后经SPE富集净化、二氯甲烷洗脱、氮吹浓缩、二氯甲烷或乙腈定容后采用GC-MS进行定量分析。结果表明:在优化的样品前处理和分析条件下,BaP标准曲线的线性相关系数R2>0.99,方法回收率为79.6%~85.5%,方法检出限和定量限分别为4.33 ng/L和14.45 ng/L。该方法应用于内蒙古某焦化厂二级生化出水加标样品中BaP的测定,得到BaP的回收率为83.3%~89.3%,表明其灵敏度高、选择性好,适用于焦化废水中痕量BaP的定量检测。Based on solid phase extraction(SPE)and gas chromatography/mass spectrometry(GC-MS),the study herein established a quantitative analysis method for trace benzo(a)pyrene(BaP)in coking wastewater.The BaP-containing water samples were enriched and purified by SPE after being modified by methanol,then eluted by dichloromethane,concentrated by nitrogen blowing,and quantified by GC-MS after constant volume of dichloromethane or acetonitrile.The results showed that,after the optimization of sample pretreatment and under the analysis conditions,the linear correlation coefficient(R2)of BaP standard curve was greater than 0.99,the recovery rate was in the range of 79.6%~85.5%,the detection limit and quantitative limit were 4.33 ng/L and 14.45 ng/L,respectively.This method was then applied to the determination of BaP in the secondary effluent of a coking plant in Inner Mongolia.The recoveries of spiked BaP samples were in the range of 83.3%~89.3%,indicating that this method presented high sensitivity and good selectivity.It is suitable for the quantitative determination of trace BaP in coking wastewater.

关 键 词：苯并(A)芘 固相萃取 气相色谱-质谱 焦化废水 定量检测 

分 类 号：O658.2[理学—分析化学] O657.63[理学—化学] X832[环境科学与工程—环境工程]