预浓缩-微板流控制双柱气相色谱-质谱/氢火焰双检测器法测定环境空气中挥发性有机物  

Determination of volatile organic compounds in ambient air by double column dean switching gas chromatography-mass spectrometry/flame ionization detector coupled with preconcentration system

作　　者：朱小亮 吴到懋 孙步旭 陈树军 王辉 樊冬玲 ZHU Xiaoliang;WU Daomao;SUN Buxu;Chen Shujun;Wang Hui;FAN Dongling(Suqian Environmental Monitoring Center of Jiangsu Province,Suqian 223800)

机构地区：[1]江苏省宿迁环境监测中心,宿迁223800

出　　处：《分析试验室》2020年第11期1334-1339,共6页Chinese Journal of Analysis Laboratory

摘　　要：建立了预浓缩-微板流控制双柱气相色谱-质谱/氢火焰离子化检测器同时测定环境空气中57种挥发性有机物(VOCS)的方法。将采集于苏玛罐中的环境空气样品通过预浓缩系统富集、脱附、除水、除二氧化碳和浓缩,然后通过GC-MS/FID的微板流控制将C2~C3和C4~C12目标物分别引入HP-PLOT柱和DB-1柱进行分离。C2~C3目标物通过FID检测分离,以保留时间定性、外标法定量;C4~C12通过M S检测,采用全扫描模式,以保留时间和特征离子定性、内标法定量。结果表明:在0. 5~20 nmol/mol范围内,57种化合物呈现良好的线性关系,相关系数均大于0. 999,方法检出限范围为0. 015~0. 085μg/m3。低、中、高3种浓度水平的加标回收率范围分别为81. 2%~95. 3%,85. 4%~109. 3%和86. 3%~108. 9%,相对标准偏差范围分别为1. 2%~7. 1%,1. 2%~6. 2%和1. 0%~4. 6%。采用该方法对真实环境空气样品进行检测,检测出包括苯系物、烷烃、烯烃在内的18种目标化合物,质量浓度范围为0. 21~18. 3μg/m3。方法可实现对环境空气中57种目标污染物准确测定。A method for the determination of 57 volatile organic compounds( VOCS) in ambient air based on double column dean switching gas chromatography-mass spectrometry/flame ionization detector( GC-MS/FID)coupled with preconcentration system was established. The ambient air samples collected in the summa canister were enriched,desorbed,dehydrated,decarbonized and concentrated by the preconcentration system,and then C2-C3 and C4-C12 targets were introduced into HP-PLOT and DB-1 columns respectively by the dean switching of GC-MS/FID. The C2-C3 targets were analyzed by FID,qualitative by retention time,and quantified by external standard method,while the C4-C12 targets were detected by MS in full scan mode,qualitative by retention time and characteristic ion,and quantified by internal standard method. The results indicated that the 57 compounds showed good linear relationships in the range of 0. 5-20 nmol/mol,with the correlation coefficients( R2) of more than 0. 999,and the detection limits of the method were 0. 015-0. 085 μg/m3. The ranges of the spiked recoveries for the low,medium and high concentration levels were 81. 2%-95. 3%,85. 4%-109. 3% and86. 3%-108. 9%,respectively,with the relative standard deviations of 1. 2%-7. 1%,1. 2%-6. 2% and1. 0%-4. 6%. The 18 target compounds including benzenes,alkanes and olefins were detected by the method in real ambient air samples. The concentration range was 0. 21-18. 3 μg/m3. The method can achieve accurate determination of 57 target pollutants in ambient air.

关 键 词：挥发性有机物 预浓缩系统 双柱气相色谱-质谱/氢火焰检测器 环境空气 苏码罐 

分 类 号：O657.63[理学—分析化学] X831[理学—化学]