Thermal Analysis Instrument coupled to a Mass Spectrometer

采购由耦合到质谱仪（MS）的同步热分析（STA）组成的设置允许采集质量变化信号以及有关废气成分的定量信息。从这个意义上说，在高达1600 °C的温度下工作并进行氧敏测量的可能性对于以下研究特别必要：材料特性的推导;合成步骤的研究，如热解，选择性解吸，碳活化，还原或氧化;洞察非催化和催化过程中的变化。尽管达姆施塔特工业大学的不同研究小组已经使用了这种技术，但目前还没有一种装置可以覆盖高达1600 °C的温度范围，同时满足无氧操作和长期稳定定量质谱测量逸出气体的特殊要求。特别是对于在高达1600 °C的温度下热解聚合物，最少量的残留氧是至关重要的。当研究表面官能团的脱附行为时，也可以获得失真的图像，特别是对于仅表现出小程度官能化的材料。同样，残留的氧可以伪造在惰性气体下的离子液体的长期稳定性的研究。到目前为止，热重装置固有的大死体积和由此产生的未知的长吹扫时间一直是主要问题。然而，通过在设备的吹扫步骤期间监测氧含量，确保了随后的无氧操作，而没有质谱仪的污染，例如水的污染。此外，自动进样器的使用不仅是有效使用仪器和最大吞吐量所必需的，而且还允许在测量活动期间自动分析校准物质。由于计划应用复杂的温度和气体程序，一个良好的软件耦合热重和质谱分析是必要的。

The procurement of a setup consisting of a Simultaneous Thermal Analysis (STA) coupled to a Mass Spectrometer (MS) allows the acquisition of a mass change signal in combination with quantitative information about the exhaust gas composition. In this sense, the possibility to work at temperatures up to 1600 °C and to perform oxygen-sensitive measurements is especially necessary for the following studies: Derivation of material properties; studies of synthesis steps such as pyrolysis, selective desorption, carbon activation, reduction or oxidation; insights into changes during non-catalytic and catalytic processes. Although different groups at the TU Darmstadt already use this technique, there is currently no setup that can cover the temperature range up to 1600 °C while meeting the special requirements of an oxygen-free operation and long-term stable quantitative mass spectrometry measurements of the evolved gas. Especially for the pyrolysis of polymers at temperatures up to 1600 °C, the smallest amounts of residual oxygen are critical. A distorted picture can also be obtained when investigating the desorption behavior of surface functional groups, particularly for materials exhibiting only a small degree of functionalization. Likewise, residual oxygen can falsify investigations on the long-term stability of ionic liquids under inert gas. Until now, the inherently large dead volume of the thermogravimetric apparatus and the resulting unknown long purging time has been the major problem. However, by monitoring the oxygen content during the purging step of the apparatus ensures the subsequent oxygen-free operation without the contamination of the mass spectrometer, e.g. with water. The use of an automatic sample changer is furthermore not only necessary for an efficient use of the instrument and maximum throughput, but also allows the automated analysis of calibration substances during the measurement campaign. Due to the planned application of complex temperature and gas programs, a good software coupling of thermogravimetric and mass spectrometry analysis is necessary.