Duemichen E, Braun U, Senz R, Fabian G, Sturm H
BAM Federal Institute of Material Research and Testing, Unter den Eichen 87, 12205 Berlin, Germany.
BAM Federal Institute of Material Research and Testing, Unter den Eichen 87, 12205 Berlin, Germany.
J Chromatogr A. 2014 Aug 8;1354:117-28. doi: 10.1016/j.chroma.2014.05.057. Epub 2014 May 27.
For analysis of the gaseous thermal decomposition products of polymers, the common techniques are thermogravimetry, combined with Fourier transformed infrared spectroscopy (TGA-FTIR) and mass spectrometry (TGA-MS). These methods offer a simple approach to the decomposition mechanism, especially for small decomposition molecules. Complex spectra of gaseous mixtures are very often hard to identify because of overlapping signals. In this paper a new method is described to adsorb the decomposition products during controlled conditions in TGA on solid-phase extraction (SPE) material: twisters. Subsequently the twisters were analysed with thermal desorption gas chromatography mass spectrometry (TDS-GC-MS), which allows the decomposition products to be separated and identified using an MS library. The thermoplastics polyamide 66 (PA 66) and polybutylene terephthalate (PBT) were used as example polymers. The influence of the sample mass and of the purge gas flow during the decomposition process was investigated in TGA. The advantages and limitations of the method were presented in comparison to the common analysis techniques, TGA-FTIR and TGA-MS.
对于聚合物气态热分解产物的分析，常用技术是热重分析法，并结合傅里叶变换红外光谱法（TGA-FTIR）和质谱分析法（TGA-MS）。这些方法为分解机理提供了一种简单的途径，特别是对于小分子分解产物。由于信号重叠，气态混合物的复杂光谱往往很难识别。本文描述了一种新方法，即在热重分析（TGA）的受控条件下，将分解产物吸附在固相萃取（SPE）材料——搅拌棒上。随后，使用热脱附气相色谱质谱联用仪（TDS-GC-MS）对搅拌棒进行分析，该仪器能够利用质谱库对分解产物进行分离和鉴定。以热塑性塑料聚酰胺66（PA 66）和聚对苯二甲酸丁二醇酯（PBT）作为示例聚合物。在TGA中研究了样品质量和分解过程中吹扫气流的影响。与常用分析技术TGA-FTIR和TGA-MS相比，阐述了该方法的优缺点。
