便携式气相色谱质谱联用仪关键技术的研究
发布时间：2018-12-10 13:18
【摘要】：气相色谱质谱联用仪是实验室常用分析仪器之一,具有良好的定性定量能力,在环境监测、石油化工和食品安全等方面广泛应用。传统气相色谱质谱仪体积大、能耗高、对操作环境要求严格,无法满足现场分析的需求。便携式气相色谱质谱联用仪具有体积小、功耗低、分析速度快的优点,在环境监测、应急响应、火灾事故调查、化学战剂及有毒工业化学品快速检测等方面应用广泛。由于国内相关研究起步较晚,技术相对薄弱,目前国内便携式气相色谱质谱联用仪市场几乎都被HAPSITE、TRIDION等国外仪器垄断。为了满足日益增长的市场需求,提高我国质谱仪器开发水平,研制便携式气相色谱质谱联用仪具有重要意义。本文对便携式气相色谱质谱联用技术进行研究,研制了一种体积小、功耗低、适用于现场分析的便携式气相色谱质谱联用仪。首先对便携式气相色谱质谱联用仪的色谱部分进行模块化设计,将气化室、色谱柱和质谱真空腔在结构上实现了一体化,同时设计了联用接口及其加热控温装置;软件方面,对温控系统进行整合,使其作为便携式气相色谱质谱联用仪软件系统的一部分,实现对气化室、色谱柱的精确控温,并重新校正了其测温曲线;最后对色谱模块分离能力和定量稳定性进行了测试。其次是质谱部分关键技术的研究,选择自行设计的混合离子阱作为质量分析器,依据离子阱仿真结果进行加工测试,优化了电极间绝缘材料,防止电极间放电,设计了RF信号功率放大器模块,包括射频功率放大器和射频升压模块;设计了微弱信号放大及检测模块用于对检测器电流进行高增益低噪声放大;搭建了小型真空系统,包括真空腔设计和真空计、真空泵选型,并对该小型真空系统进行测试,能在开机10 min内达到离子阱所需真空度。最后,对便携式气相色谱质谱联用仪进行整机搭建,采用Solidworks对各模块结构图进行模拟装配,确定各模块相对位置,采取层叠式结构对电路系统进行安装。完成搭建后对仪器性能进行了测试,得到了样机的初步测试结果。
[Abstract]:Gas chromatography-mass spectrometry (GC-MS) is one of the commonly used analytical instruments in laboratory. It has good qualitative and quantitative capability and is widely used in environmental monitoring, petrochemical industry and food safety. The traditional gas chromatographic mass spectrometer is large in volume, high in energy consumption and strict in operation environment, so it can not meet the needs of field analysis. Portable gas chromatography-mass spectrometry (GC-MS) has the advantages of small size, low power consumption and fast analytical speed. It is widely used in environmental monitoring, emergency response, fire accident investigation, rapid detection of chemical warfare agents and toxic industrial chemicals, and so on. Due to the late start of domestic related research and relatively weak technology, the domestic market of portable gas chromatography-mass spectrometry is almost monopolized by HAPSITE,TRIDION and other foreign instruments. In order to meet the increasing market demand and improve the development level of mass spectrometer in China, it is of great significance to develop portable gas chromatography-mass spectrometer. In this paper, the portable gas chromatography-mass spectrometry (GC / MS) technique is studied. A portable gas chromatography-mass spectrometer with small volume and low power consumption is developed, which is suitable for field analysis. Firstly, the chromatographic part of the portable gas chromatography-mass spectrometer is modular designed, the gasification chamber, chromatographic column and mass spectrum vacuum cavity are integrated in structure, and the joint interface and the heating and temperature control device are designed at the same time. In the aspect of software, the temperature control system is integrated as a part of the portable gas chromatography-mass spectrometry software system to realize the accurate temperature control of the gasification chamber and the chromatographic column, and the temperature measurement curve is recorrected. Finally, the separation ability and quantitative stability of chromatographic module were tested. Secondly, some key techniques of mass spectrometry are studied. The self-designed mixed ion trap is selected as mass analyzer. The interelectrode insulation material is optimized according to the simulation results of the ion trap to prevent inter-electrode discharge. The module of RF signal power amplifier is designed, including RF power amplifier and RF boost module. The weak signal amplification and detection module is designed to amplify the detector current with high gain and low noise. A small vacuum system, including vacuum chamber design, vacuum gauge, vacuum pump type selection, was built, and the vacuum degree needed by ion trap could be achieved within 10 min. At last, the portable gas chromatography-mass spectrometer is built, and each module structure diagram is simulated and assembled by Solidworks. The relative position of each module is determined, and the circuit system is installed with stacked structure. The performance of the instrument was tested and the preliminary test results of the prototype were obtained.
【学位授予单位】：哈尔滨工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.63
本文编号：2370638
[Abstract]:Gas chromatography-mass spectrometry (GC-MS) is one of the commonly used analytical instruments in laboratory. It has good qualitative and quantitative capability and is widely used in environmental monitoring, petrochemical industry and food safety. The traditional gas chromatographic mass spectrometer is large in volume, high in energy consumption and strict in operation environment, so it can not meet the needs of field analysis. Portable gas chromatography-mass spectrometry (GC-MS) has the advantages of small size, low power consumption and fast analytical speed. It is widely used in environmental monitoring, emergency response, fire accident investigation, rapid detection of chemical warfare agents and toxic industrial chemicals, and so on. Due to the late start of domestic related research and relatively weak technology, the domestic market of portable gas chromatography-mass spectrometry is almost monopolized by HAPSITE,TRIDION and other foreign instruments. In order to meet the increasing market demand and improve the development level of mass spectrometer in China, it is of great significance to develop portable gas chromatography-mass spectrometer. In this paper, the portable gas chromatography-mass spectrometry (GC / MS) technique is studied. A portable gas chromatography-mass spectrometer with small volume and low power consumption is developed, which is suitable for field analysis. Firstly, the chromatographic part of the portable gas chromatography-mass spectrometer is modular designed, the gasification chamber, chromatographic column and mass spectrum vacuum cavity are integrated in structure, and the joint interface and the heating and temperature control device are designed at the same time. In the aspect of software, the temperature control system is integrated as a part of the portable gas chromatography-mass spectrometry software system to realize the accurate temperature control of the gasification chamber and the chromatographic column, and the temperature measurement curve is recorrected. Finally, the separation ability and quantitative stability of chromatographic module were tested. Secondly, some key techniques of mass spectrometry are studied. The self-designed mixed ion trap is selected as mass analyzer. The interelectrode insulation material is optimized according to the simulation results of the ion trap to prevent inter-electrode discharge. The module of RF signal power amplifier is designed, including RF power amplifier and RF boost module. The weak signal amplification and detection module is designed to amplify the detector current with high gain and low noise. A small vacuum system, including vacuum chamber design, vacuum gauge, vacuum pump type selection, was built, and the vacuum degree needed by ion trap could be achieved within 10 min. At last, the portable gas chromatography-mass spectrometer is built, and each module structure diagram is simulated and assembled by Solidworks. The relative position of each module is determined, and the circuit system is installed with stacked structure. The performance of the instrument was tested and the preliminary test results of the prototype were obtained.
【学位授予单位】：哈尔滨工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.63
【参考文献】
相关期刊论文 前10条
1 刘喜;施玉格;;便携式气相色谱—质谱联用仪应急现场测定空气中54种VOCs[J];干旱环境监测;2016年04期
2 郝峰;李亮;石艳菊;;便携式GC-MS在化学品污染事件中的应用[J];环境与发展;2016年02期
3 曹骁;;HAPSITE便携式气质谱联用仪在环境应急工作中的优越性[J];资源节约与环保;2015年04期
4 李琦;邓一兵;黄刚;;小型离子阱技术及其航天应用进展[J];传感器与微系统;2014年12期
5 张欣;;便携式气相色谱-质谱联用仪的研制及应用[J];药物与人;2014年06期
6 封跃鹏;房丽萍;邱赫男;王伟;;便携式气相色谱质谱测定水中挥发性有机物再现性和准确度研究[J];中国环境监测;2013年06期
7 张华;张小华;肖瑞林;丁传凡;;三维离子阱内空间电荷效应的理论分析[J];质谱学报;2013年03期
8 李晓旭;刘立鹏;马乔;俞建成;郑毅;吴文明;王健;;便携式气相色谱-质谱联用仪的研制及应用[J];分析化学;2011年10期
9 蒋海威;褚春莹;张婷婷;房贤文;谭培功;;便携式GC-MS在环境应急监测中的应用[J];现代仪器;2011年02期
10 邵昶铭;;顶空便携式气相色谱—质谱仪现场测定地表水中苯系物[J];干旱环境监测;2010年01期
相关博士学位论文 前5条
1 肖育;新型离子阱质量分析器的研发[D];复旦大学;2014年
2 王亮;新型离子阱质量分析器和气相离子解离方法的研究[D];复旦大学;2013年
3 欧阳永中;电子轰击和电喷雾电离源有机质谱裂解规律的量子化学解析[D];中南大学;2010年
4 赵占锋;月球资源探测小型质谱仪关键技术研究[D];哈尔滨工业大学;2010年
5 姜杰;矩形离子阱质谱仪和离子淌度谱仪的研制[D];吉林大学;2008年
相关硕士学位论文 前2条
1 张冬冬;混合离子阱质量分析器的研究[D];哈尔滨工业大学;2014年
2 戴辰铖;便携式气相色谱仪控制系统的研究[D];哈尔滨工业大学;2013年
，本文编号：2370638
本文链接：https://www.wllwen.com/kejilunwen/huaxue/2370638.html
教材专著
