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Investigations in secondary reactions of evolved gases by TG-MS with a Skimmer integrated coupling system

机译:TG-MS和Skimmer集成耦合系统对逸出气体的二次反应的研究

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As the knowledge of all evolved gas in TG-MS system can give more detail feature of various reactions, the precise measuring methods must be developed. However some highly reactive gas or higher boiling volatiles are hardly detectable due to polycondensation reaction or recrystallization at low temperature stage. Since the temperature of sampling interface is often lower than the reaction zone of sample, unknown secondary reactions of evolved gases in TG-MS system, which often occur before the sampling of all gases, resulted in misunderstanding of reaction characteristic. Therefore, it is crucial to seek out rational qualitative-quantitative analysis method and evolved gas measuring instruments which can effectively eliminate the secondary reactions. Actually a skimmer sampling interface between reaction sample and mass spectrometer [2] can guarantee that all evolved gas species keep the same temperature in the transferring process. Meanwhile a novel method of equivalent characteristic spectrum analysis (ECSA) [3] was applied to quantitatively analyze the mass spectrum of TG-MS system in order to know whether the secondary reactions occur or not. With this skimmer interface coupling system, the recrystallization of melamine and CxNy was clearly observed in the exhaust port after sampling interface and the decomposition reaction of melamine at 140oC was investigated to give all information about its evolved gases in the pyrolysis process. Also another typical compared experiments for the slag of coal gas after coal gasification were carried out by two different TG-MS systems using skimmer and capillary sampling interface. MS signals from the test by means of the capillary sampling drifted to higher temperature, when these were compared with TG/DTG signals. On the contrary, the MS signals by means of the skimmer sampling were in great agreement with the TG/DTG signals. This skimmer coupling system and ECSA method together can analyze all components of evolved gases, quantitatively research and effectively avoid the secondary reactions. This method will promote the innovation and development of more field, such as energy, geology, materials, pharmaceuticals and so on.
机译:由于对TG-MS系统中所有逸出气体的了解可以提供各种反应的更多详细信息,因此必须开发精确的测量方法。然而,由于在低温阶段的缩聚反应或重结晶,几乎不能检测到一些高反应性气体或较高沸点的挥发物。由于采样界面的温度通常低于样品的反应区,因此在TG-MS系统中发生的未知气体二次反应通常发生在所有气体采样之前,从而导致对反应特性的误解。因此,寻找能够有效消除副反应的合理的定性-定量分析方法和演化的气体测量仪器至关重要。实际上,反应样品和质谱仪之间的撇渣器采样接口[2]可以确保在转移过程中所有逸出的气体物种保持相同的温度。同时,采用一种新的等效特征谱分析方法(ECSA)[3]对TG-MS系统的质谱进行定量分析,以了解是否发生了副反应。使用这种撇渣器界面耦合系统,采样界面后在排气口中清楚地观察到三聚氰胺和CxNy的重结晶,并研究了三聚氰胺在140oC时的分解反应,以提供有关其在热解过程中释放出的气体的所有信息。另一个典型的对比实验是在两个不同的TG-MS系统中使用撇渣器和毛细管采样接口对煤气化后的煤气炉渣进行了比较。通过将毛细管采样从测试中获得的MS信号与TG / DTG信号进行比较后,漂移至更高的温度。相反,通过撇渣器采样获得的MS信号与TG / DTG信号高度吻合。该分离器耦合系统和ECSA方法一起可以分析逸出气体的所有成分,进行定量研究并有效避免副反应。这种方法将促进更多领域的创新和发展,例如能源,地质,材料,制药等。

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