利用草酸钙逸出气的碳气化反应验证TG/FTIR联用性能  

Performance verification of a TG/FTIR system by carbon gasification reaction of calcium oxalate evolved gas

作　　者：章斐[1] Zhang Fei(Analytical Instrumentation Center,Peking University,Beijing 100871,China)

机构地区：[1]北京大学分析测试中心,北京100871

出　　处：《分析仪器》2021年第3期75-79,共5页Analytical Instrumentation

摘　　要：热重/傅里叶变换红外光谱联用(TG/FTIR)是剖析材料组分和结构、研究材料热稳定性和热分解机理的重要检测技术,但对于其联用性能的验证,国内尚无相应的技术标准、检定规程或校准规范,各仪器公司间也没有统一的方法和明确的性能指标。本文分析了现有TG/FTIR联用仪器验证方法及存在问题,提出以CaC_(2)O_(4)·H_(2) O为标准试样,利用其在惰性气氛下分解逸出气发生碳气化反应所生成的CO峰,作为联用性能是否合格的判断标准,通过一次运行测试即可核查联用系统的检测灵敏度、气体质量流量稳定性及仪器气密性的新方法。此方法操作简便,判断直观准确,适用于各种类型的TG/FTIR联用系统,对于保障未知样测试结果的准确性、促进不同品牌不同型号的仪器间以及不同实验室间测试结果的等效性具有重要意义。TG/FTIR system is an important coupled technology to analyze the structure,composition as well as thermal stability and decomposition mechanism of materials.In the present work,the existing problems in currently used method of TG/FTIR performance verification are analyzed.On this basis,an innovative method is proposed to use CaC_(2)O_(4)·H_(2)O as the standard sample and the CO signal generated by carbon gasification reaction of the evolved gas under inert atmosphere as the standard to judge whether the comprehensive performance is qualified.The detection sensitivity,gas mass flow stability and air tightness of the comprehensive system can be verified through a single operation.This method is easy to apply and accurate to judge.

关 键 词：TG/FTIR 仪器验证 联用性能 灵敏度 气密性 草酸钙 逸出气 碳气化反应 

分 类 号：O657.33[理学—分析化学]