化学
质谱法
色谱法
污染
大小排阻色谱法
气相色谱法
解吸
萃取(化学)
检出限
溶剂
蒸发
样品制备
分析化学(期刊)
吸附
有机化学
物理
热力学
酶
生物
生态学
作者
C. Berrueco,Patricia Álvarez,Silvia Venditti,Trevor Morgan,Alan A. Herod,Marcos Millán,Rafael Kandiyoti
出处
期刊:Energy & Fuels
[American Chemical Society]
日期:2009-05-04
卷期号:23 (6): 3008-3015
被引量:46
摘要
1-Methyl-2-pyrrolidinone (NMP) is widely used as a solvent for coal-derived products and as eluent in size exclusion chromatography. It was observed that sample contamination may take place, through reactions of NMP, during extraction under refluxing conditions and during the process of NMP evaporation to concentrate or isolate samples. In this work, product distributions from experiments carried out in contact with air and under a blanket of oxygen-free nitrogen have been compared. Gas chromatography/mass spectrometry (GC-MS) clearly shows that oxidation products form when NMP is heated in the presence of air. Upon further heating, these oxidation products appear to polymerize, forming material with large molecular masses. Potentially severe levels of interference have been encountered in the size exclusion chromatography (SEC) of actual samples. Laser desorption mass spectrometry and SEC agree in showing an upper mass limit of nearly 7000 u for a residue left after distilling "pure" NMP in contact with air. Furthermore, experiments have shown that these effects could be completely avoided by a strict exclusion of air during the refluxing and evaporation of NMP to dryness.
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