热重-质谱联用技术(TG-MS)及系统优化研究  

Research on the Combination and Optimization of TG-MS System

作　　者：李淑娥[1] 王晓东[1] 颜国纲[1] 李恩霞[1] 林云良[1] 祝贺[1] 孙庆雷[1] 

机构地区：[1]山东省分析测试中心,山东济南250014

出　　处：《山东科学》2008年第2期9-14,共6页Shandong Science

基　　金：山东省优秀中青年科学家科研奖励基金资助项目(2005BS09003)

摘　　要：详细考察了热重-质谱联用时遇到的问题及解决的方法,包括热重-质谱联用的可行性和可靠性、连接处加热的影响、热重和质谱检测的同步性以及系统误差等。实验采用ATI-CAHN公司生产的TG-151加压热天平和瑞士Balzers公司生产的Omnistar小型在线质谱分析仪,采用草酸钙为标准物质对系统的可行性和可靠性进行考察。结果表明连接处加热后水的逸出无拖尾现象,基本无冷凝,并可缩短气体到达离子化室所用的时间,说明使用加热带后效果明显,能够满足实验要求,而且热重和质谱检测基本同步。系统误差分析结果表明,热重和质谱检测结果重复性好,系统误差较小,所得结果准确可信,说明热重和质谱联用系统为最优化状态。The combination of thermogravimetry and mass spectrum （TG-MS） was systematically investigated, which included the feasibility and reliability, the effect of heating at the connection, and the system errors. The feasibility and reliability of this system were measured with the standard samples of calcium oxalate, and such instniments as AT1-CAHN made TG-151 pressarized thermogravimetry and Balzers made Omristar on line mass spectrum analyzer. Results show that there are no time delay and steam condensation in the process of heating, and that the flow rate is greatly increased, These demonstrate that the heating is effective and can satisfy the experiment requirements. The results of system error analysis show that the data derived from TG and MS have better repetitions and smaller system errors, and are more precise, These suggest that the combination of TG and MS is optimmn. The combination of thennogravimetry and mass spectrum- a very effective approach, can be applied not only to the substance analysis of its composition and structure characteristics, but also to the research of substance pyrolysis mechanism

关 键 词：热重-质谱联用 优化 

分 类 号：O657.63[理学—分析化学] O655.1[理学—化学]