Thermoanalytical characterization of polymers: A comparative study between thermogravimetry and evolved gas analysis using a temperature-programmable pyrolyzer
Thermoanalytical characterization of polymers: A comparative study between thermogravimetry and evolved gas analysis using a temperature-programmable pyrolyzer
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DOI：
10.1016/j.polymertesting.2014.12.011
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发表时间：
2015-04
期刊：
影响因子：
5.1
通讯作者：
Ai Shiono;A. Hosaka;C. Watanabe;N. Teramae;N. Nemoto;H. Ohtani
中科院分区：
文献类型：
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作者：
Ai Shiono;A. Hosaka;C. Watanabe;N. Teramae;N. Nemoto;H. Ohtani
采用可编程温度裂解器作为加热单元，与MS检测器在线耦合，对15个合成聚合物样品进行了逸出气体分析（EGA）。使用去活化的不锈钢管和无排气口适配器将热解器与MS检测器连接，并将它们置于300°C的GC烘箱中以避免具有高沸点的放出气体的冷凝。通过该系统（Py-EGA-MS）测量的聚苯乙烯的热谱图显示，随着样品质量的增加，峰值温度向较高温度区域移动。结果发现，对于0.20 mg的相同样品质量，EGA热谱图的S/N比比差示热重（DTG）热谱图的S/N比高出420倍上级。由于Py-EGA-MS得到的峰温度与DTG得到的峰温度之间具有良好的线性关系，因此可以得出结论，Py-EGA-MS可以以高灵敏度和使用较少的样品获得可靠的样品热性质数据。
Evolved gas analysis (EGA) was carried out on 15 synthetic polymer samples using a temperature programmable pyrolyzer as a heating unit which was on-line coupled with a MS detector. A deactivated stainless steel tube and a vent free adapter were used to couple the pyrolyzer with the MS detector, and they were placed in a GC oven at 300°C to avoid condensation of evolved gases with high boiling point. Thermograms of polystyrene measured by this system (Py-EGA-MS) showed shifts of the peak temperature to the higher temperature region as the sample mass increased. It was found that the S/N ratios of EGA thermograms were 420-fold superior to those of differential thermogravimetry (DTG) thermograms for the same sample mass of 0.20 mg. Since a good linear relationship was obtained between peak temperatures obtained by Py-EGA-MS and DTG, it can be concluded that Py-EGA-MS can be used to obtain reliable data on thermal properties of samples with high sensitivity and using less sample.