快速气相色谱/电子轰击离子源-飞行时间质谱联用仪的研制
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摘要
基于快速气相色谱分析技术和飞行时间质谱技术,研制了快速气相色谱/电子轰击离子源-飞行时间质谱联用仪。仪器由进样系统、气相色谱分离系统、气质接口、电子轰击离子源、垂直引入反射式飞行时间质量分析器、数据采集系统和硬件控制系统等组成。设计了汽化室、加热膜色谱柱和一种三层套管的传输管用于连接色谱与质谱。以烃类混合标准气体为对象,对载气压力、色谱柱温度和电压参数进行了优化,实现了对各类有机物的快速分离和准确定性。最后,将该方法用于测试苯系物和异丁烷标气,进行了仪器性能测试。结果表明,质量范围是4~502 amu,分辨率优于500,检测限为500 ppb,分析时间小于5 min,重现性RSD小于10%,动态范围达到四个数量级。
Based on fast gas chromatograph and time-of-flight mass spectrum technology,fast gas chromatography/electron impaction source of time-of-flight mass spectrometer(FGC/EI-TOF MS) is developed.The FGC/EI-TOF MS is mainly composed of a sample system,a GC separation system,a GC-MS interface,an electron impaction source,a vertical introduction of reflection time-of-flight mass analyzer,a data acquisition system and hardware control system.A vaporization chamber,heating film of GC and three-wall-tube line are built.After the optimization of EPC,temperature of GC,and important voltage parameters,Alkanes standard gas mixtures are studied,and fast seperation and accurate classification different kinds of organic compounds are eventually realized rapidly and accurately.At last,the FGC-TOF MS is applied to test the characteristics of benzenes and isobutane standard gas mixtures.The results indicate that mass range is 4~502amu,resolution is better than 500,detection limit is 500 ppb,analysis time is less than 5 min,reproducibility RSD is less than 10%,dynamic range is four orders of magnitude.
Based on fast gas chromatograph and time-of-flight mass spectrum technology,fast gas chromatography/electron impaction source of time-of-flight mass spectrometer(FGC/EI-TOF MS) is developed.The FGC/EI-TOF MS is mainly composed of a sample system,a GC separation system,a GC-MS interface,an electron impaction source,a vertical introduction of reflection time-of-flight mass analyzer,a data acquisition system and hardware control system.A vaporization chamber,heating film of GC and three-wall-tube line are built.After the optimization of EPC,temperature of GC,and important voltage parameters,Alkanes standard gas mixtures are studied,and fast seperation and accurate classification different kinds of organic compounds are eventually realized rapidly and accurately.At last,the FGC-TOF MS is applied to test the characteristics of benzenes and isobutane standard gas mixtures.The results indicate that mass range is 4~502amu,resolution is better than 500,detection limit is 500 ppb,analysis time is less than 5 min,reproducibility RSD is less than 10%,dynamic range is four orders of magnitude.
引文
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[2]Chen Jingshi,Zhao Xiaomin.Application of GCMS to pollution accident[J].Environmental Science and Management,2008,33(1):155-158(in Chinese).陈璟士,赵小敏.气质联用在环境突发事件中的应用[J].环境科学与管理,2008,33(1):155-158.
[3]Jiang Haiwei,Chu Chunying,Zhang Tingting,et al.Application for environmental emergency monitoring with portable GC-MS[J].Modern Instruments,2011,17(2):63-65(in Chinese).蒋海威,褚春莹,张婷婷,等.便携式GC-MS在环境应急监测中的应用[J].现代仪器,2011,17(2):63-65.
[4]Hill H H,Jr,Martin S J.Conventional analytical methods for chemical warfare agents[J].J.Pure.Appl.Chem,2002,74(12):2281-2291.
[5]Wang Yujun,Xing Zhixian,Zhang Xiufang,et al.On-site detection of volatile organic compounds during composting treatment of livestock and poultry manure by GC-MS[J].J.Chinese Jouranl of Analytical Chemistry,2012,40(6):899-903(in Chinese).王玉军,邢志贤,张秀芳,等.便携式气相色谱-质谱联用仪现场测定畜禽粪便堆肥中挥发性有机物[J].分析化学,2012,40(6):899-903.
[6]Wu Huiqin,Huang Xiaolan,Chen Jianghan,et al.A novel method for the identification of gutter oils using SPMS/GC-MS[J].Journal of Instrumental Analysis,2012,31(1):l-6(in Chinese).吴惠勤,黄晓兰,陈江韩,等.SPME/GC-MS鉴别地沟油新方法[J].分析测试学报,2012,31(1):1-6.
[7]Liu Lipeng,Zhu Rong,Duan Lian,et aJ.Development and application of portable fast gas chromatograph-mass sepectrometer[J].Modern Scientific Instruments,2014 3:69-72(in Chinese).刘立鹏,朱蓉,段炼,等.便携式快速色谱-质谱联用仪的研制与应用[J].现代科学仪器,20143:66-72.
[8]Li Xiaoxu,Liu Lipeng,Ma Qiao,et al.Development and application of portable gas chromatograph-mass sepectrometer[J].Chinese Jouranl of Analytical Chemistry,2011,39(10):1476-1481(in Chinese).李晓旭,刘立鹏,马乔,等.便携式气相色谱-质谱联用仪的研制及应用[J].分析化学,2011,39(10):1476-1481.
[9]Smith P A,Roe M T A,Sadowski C,et al.Unknown exposures:Gaps in basic characterization addressed with person-portable gas chromatography-mass spectrometry instrumentation[J].J.Occup.Environ.Hyg.,2011,8(3):129-138.
[10]Gao W,Huang Z X,Nian H Q,et al.A novel gas analysis system for metallurgical materials based on time-of-flight mass spectrometry[J].Int.J.Mass Spectrom.,2010,294:77-82.
[11]Dodonow A F,Kozlovsji V I,Soulimenkow I V,et al.High-resolution electrospray ionization orthogonal-injection time-of-flight mass spectrometer[J].Eur.J.Mass Spectrom,2000,6:481-490.
[12]Warren J M,Pawliszyn J.Development and evaluation of needle trap device geometry and packing methods for automated and manual analysis[J].J.Chromatogr.A,2011,1218(50):8982-8988.
[13]Gao Wei,Huang Zhengxu,Guo Ghangjuan,et al.Electron ionization and orthogonal acceleration time-of-flight mass spectrometer[J].Journal of Chinese Mass Spectrometry Society,2008,29(4):209-212(in Chinese).高伟,黄正旭,郭长娟,等.电子轰击源垂直加速式飞行时间质谱仪的研制[J].质谱学报,2008,29(4):209-212.
[14]Tan Guobin,Huang Zhengxu,Gao Wei,et al.Development of orthogonal acceleration time-offlight mass spectrometer for detection of ions with wide energies distribution[J].Chinese Journal of Analytical Chemistry,2013,10(41):1614-1619(in Chinese).谭国斌,黄正旭,高伟,等.宽离子能量检测范围垂直引入反射式飞行时间质谱仪的研制[J].分析化学,2013,41(10):1614-1619.