中国神华煤制油化工有限公司上海研究院煤直接液化国家工程实验室
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李群花, 高山松, 舒歌平. 全二维气相色谱-飞行时间质谱/氢火焰离子化检测器对煤直接液化循环溶剂的定性与定量分析[J]. 分析测试学报, 2019,38(12):1430-1437.
Analysis of Liquefaction Cycled Solvent by Comprehensive Two-dimensional Gas Chromatography-Time-of-flight Mass Spectrometry with Flame Ionization Detector[J]. 2019,38(12):1430-1437.
建立了全二维气相色谱-飞行时间质谱/氢火焰离子化检测器(GC×GC-TOF MS/FID)对煤直接液化循环溶剂(CDLRS)定性定量的分析方法。采用TOF MS和FID两种检测器同时采集数据,并结合谱库检索、标准物质保留值对照、谱图解析、标准质谱图对照、全二维谱图特征以及提取化合物分子离子等定性方法,将TOF MS检测数据定性,然后将定性的烃类化合物以z值分类法分为18类;应用Chroma TOF数据处理软件将TOF MS数据的定性分类结果应用到FID的检测数据中,对TOF MS和FID采集的数据色谱峰面积归一化处理,实现CDLRS的半定量分析。GC×GC/FID定量结果显示:煤直接液化循环溶剂中饱和烃和芳烃分别占45.805%、53.938%,其中饱和烃主要为二环烷烃及三环烷烃,含量依次为14.644%、18.021%;芳烃主要为一环烷苯和二环烷苯,含量依次为19.759%、16.528%。该方法为CDLRS的定性定量提供了一种有效的分析方法。
A method was established for qualitative and quantitative analysis on direct coal liquefaction cycled solvent(CDLRS) by comprehensive two dimensional gas chromatography time of flight mass spectrometry with hydrogen flame ionization detector(GC×GC-TOF MS/FID).The data was acquired simultaneously by TOF MS and FID detector.The acquired data by GC×GC-TOF MS were qualified based on NIST library search,standard material retention value comparison,spectral analysis,standard mass spectrum comparison,two dimensional spectral features and extracting compound molecular ions,and then divided into 18 categories based on z value.Afterwards,the Chroma TOF 47 was used to apply the qualitative classification results of TOF MS to the FID detection data,and the data collected by TOF MS and FID were normalized by the chromatographic peak area to realize semi quantitative analysis of CDLRS.The quantitative results of GC×GC/FID showed that saturated hydrocarbons and aromatic hydrocarbons in the CDLRS accounted for 45.805% and 53.938%,respectively.The saturated hydrocarbons were mainly dicycloalkanes and tricycloalkanes,which contents were 14.644% and 18.021%,respectively.The aromatic hydrocarbons were mainly cycloalkylbenzenes and dinaphthenebenzenes,which accounted for 19.759% and 16.528%,respectively.This method provided an effective analytical means for the qualitative and quantitative analyses of CDLRS.
煤直接液化循环溶剂全二维气相色谱-飞行时间质谱/氢火焰离子化检测器定性与定量分析
coal direct liquefaction cycle solventcomprehensive two dimensional gas chromatography-time-of-flight mass spectrometry with hydrogen flame ionization detectorqualitative and quantitative analysis
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