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Hydrogenation Reactions during Pyrolysis-Gas Chromatography/Mass Spectrometry Analysis of Polymer Samples Using Hydrogen Carrier Gas
Analytical Chemistry ( IF 6.7 ) Pub Date : 2016-04-29 00:00:00 , DOI: 10.1021/acs.analchem.6b00892
Atsushi Watanabe 1 , Chuichi Watanabe 1 , Robert R. Freeman 2 , Norio Teramae 1, 3 , Hajime Ohtani 4
Affiliation  

Pyrolysis-gas chromatography/mass spectrometry of polymer samples is studied focusing on the effect of hydrogen (H2) carrier gas on chromatographic and spectral data. The pyrograms and the related mass spectra of high density polyethylene (HDPE), low density polyethylene, and polystyrene (PS) serve to illustrate the differences between the species formed in H2 and the helium environment. Differences in the pyrograms and the spectra are generally thought to be a result of the hydrogenation reaction of the pyrolyzates. From the peak intensity changes in the pyrograms of HDPE and PS, hydrogenation of unsaturated pyrolyzates is concluded to occur when the pyrolysis is done in H2. Moreover, additional hydrogenation of the pyrolyzates occurs in the electron ionization source of a MS detector when H2 is used as a carrier gas. Finally, the applicability of mass spectral libraries to characterize pyrograms obtained in H2 is illustrated using 24 polymers. The effect of the hydrogenation reaction on the library search results is found to be negligible for most polymer samples with polar and nonpolar monomer units.

中文翻译:

载气对聚合物样品进行热解-气相色谱/质谱分析时的加氢反应

研究了聚合物样品的热解-气相色谱/质谱,重点研究了氢气(H 2)载气对色谱和光谱数据的影响。高密度聚乙烯(HDPE),低密度聚乙烯和聚苯乙烯(PS)的热解图和相关质谱图用于说明H 2和氦气环境中形成的物质之间的差异。通常认为热解图和光谱的差异是热解产物的氢化反应的结果。从HDPE和PS的热解图中峰强度的变化,可以得出结论,当在H 2中进行热解时,不饱和热解产物会发生氢化。。此外,当将H 2用作载气时,热解产物的额外氢化发生在MS检测器的电子电离源中。最后,使用24种聚合物说明了质谱库表征H 2中获得的热解图的适用性。对于大多数带有极性和非极性单体单元的聚合物样品,发现氢化反应对谱库搜索结果的影响可忽略不计。
更新日期:2016-04-29
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