自动富集-单光子电离质谱在线测量氯酚的研究  

Online Determination of Chlorophenols Using Photon Ionization Time-of-Flight Mass Spectrometry with Full-Automatic Enrichment Inlet System

作　　者：蒋蕾[1,2] 刘巍[2,3] 窦健[1,2] 花磊[2] 侯可勇[2] 谢园园[2,3] 陈平[2,3] 王卫国[2] 田地[1] 李海洋[1,2] 

机构地区：[1]吉林大学仪器科学与电气工程学院,吉林长春130021 [2]中国科学院大连化学物理研究所,辽宁大连116023 [3]中国科学院大学,北京100049

出　　处：《质谱学报》2014年第6期488-494,共7页Journal of Chinese Mass Spectrometry Society

摘　　要：氯酚类化合物是垃圾焚烧所产生的二噁英前生体之一,对二噁英的浓度有很好的指示作用。针对气相中氯酚类二噁英前生体的在线连续监测,自行研制了全自动富集进样-单光子电离-反射式飞行时间质谱仪。为实现低浓度氯酚的检测,设计了全自动的富集进样系统,利用3根阵列式Tenax TA吸附管,结合全自动控制的高温电磁阀,实现了气体样品连续自动的"富集-热解析-质谱进样"。研制的反射式单光子电离-飞行时间质谱仪采用10.6eV真空紫外灯作为光电离源,对气体样品分子进行软电离,避免了碎片离子的产生,所获得的样品分子离子经反射式飞行时间质量分析器完成检测,仪器分辨率达到3 000(m/z 78)。以3种典型的二噁英前生体氯酚类化合物(邻氯苯酚、2,4-二氯苯酚、2,4,6-三氯苯酚)为检测对象,对该仪器性能进行考察。富集进样系统对3种氯酚类化合物的富集倍数分别达到60、249、503,检测限分别达到66、120、125pg/L,动态线性范围分别为166pg/L^16.6ng/L、210pg/L^21ng/L、255pg/L^25.5ng/L。这些研究结果为今后开展垃圾焚烧烟气中二噁英的现场连续监测工作奠定了基础。As typical precursors of dioxin,chlorophenols （CPs） are considered as excellent indicators for the concentration of dioxin.A homemade single photon ionization time-of-flight mass spectrometer （SPI-TOF MS） combined with full-automatic enrichment-inlet system was developed for the online determination of CPs.Three Tenax TA adsorption tubes and four solenoid valves were used to accomplish continuous and automatic sampling-enrichment-thermal desorption-inlet.A vacuum ultraviolet （VUV） lamp with photon energy of 10.6 eV was used as the photon ionization source for soft ionization of sample molecules.The molecular ions of the samples generated by SPI were detected by the reflectron TOF MS,and the achieved resolution of the TOF MS was 3 000 （m/z 78）.The performance of the instrument was investigated by detecting three CPs （o-chlorophenol,2,4-dichlorophenol and 2,4,6-trichlorophenol）.As a result,the enrichment factors of o-chlorophenol,2,4-dichlorophenol and 2,4,6-trichlorophenol by using the enrichment inlet system are 60,249,503,respectively,and the LODs （limit of detection） are 66 pg/L for o-chlorophenol,120 pg/L for 2,4-dichlorophenol,125 pg/L for 2,4,6-trichlorophenol.The instrument shows wide dynamic linear range and excellent stability for continuous operation,the dynamic linear ranges are 166 pg/L-16.6 ng/L,210 pg/L-21 ng/L,255 pg/L-25.5 ng/L for three CPs respectively.These results show the potential applications for on-site detection of CPs in incineration plants.

关 键 词：飞行时间质谱 全自动富集进样 单光子电离 氯酚类有机物 在线测量 二噁英前生体 

分 类 号：O657.63[理学—分析化学]