1. 华东理工大学上海市功能性材料化学重点实验室
2. 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, 姜元博, 杜一平, 等. 中心切割二维GC-MS法测定煤直接液化加氢改质油组成[J]. 分析测试学报, 2013,32(5):527-534.
Composition Determination of Coal Direct Liquefaction Hydrotreated Oil by Heart-cutting Two-dimensional GC-MS[J]. 2013,32(5):527-534.
采用SYD-6536C石油产品蒸馏试验器取煤直接液化加氢改质全馏分油55.2~138.2 ℃的馏分段,建立了一种运用中心切割二维GC-MS法研究其单体烃组成的分析方法。实验采用PONA毛细管气相色谱柱(50 m×200 μm×0.5 μm)对色谱条件进行优化,找到煤直接液化加氢改质油55.2~138.2 ℃馏分段的最佳分离条件。被测样品首先在第一根色谱柱上进行分离,然后使用Dean Switch微流控制系统把目标化合物切割至第二根色谱柱(DB-35MS 30 m×250 μm×0.25 μm)上,进一步分离。实验将烃类化合物在PONA柱上的色谱保留规律、化合物保留指数、标准化合物保留值及质谱谱库检索等多种方法联合对煤直接液化加氢改质油在55.2~138.2 ℃的馏分段中66种化合物进行定性分析。鉴于被测油样中化合物的结构性质相近,忽略化合物相对校正因子的影响,采用面积归一化法NORM%进行定量分析。该方法方便快捷、精确度高,适用于低馏分段的煤直接液化加氢改质油的分析,同时也为高馏分段煤直接液化加氢改质油和其他种类油样的单体烃组成分析提供了参考。
The 55.2-138.2 ℃fraction of coal direct liquefaction hydrogenation modification oil was cut out by distillation tester of petroleum products SYD-6536C,and a method was developed for the analysis of 55.2-138.2 ℃fraction of coal direct liquefaction hydrotreated oil by heart-cutting two-dimensional GC-MS.A PONA capillary chromatographic column(50 m×200 μm×0.5 μm) was used for chromatographic condition optimization,and the best chromatographic separation condition for 55.2-138.2 ℃ fraction of coal direct liquefaction hydrotreated oil were obtained.The oil sample would be separated on the first capillary chromatographic column in the best experimental conditions.Then the target compounds were cut out to the second chromatographic column(DB-35MS,30 m×250 μm×0.25 μm) by Dean Switch micro flow control system,which would get further separation.The identification was based on hydrocarbon compounds retention rules on PONA,compound retention index,standard compound retention value and mass spectra library searching.With those methods,66 compounds of 55.2-138.2 ℃ fraction of coal direct liquefaction hydrotreated oil were identified.Ignoring the effect of compounds relative correction factor due to the similar compounds structure properties in the oil sample,the area normalization method was used for the quantitative analysis.The proposed method was simple,rapid and accurate,and could be used for composition determination of light petroleum distillate of coal direct liquefaction hydrotreated oil.Also the method provides reference for detailed analysis of high petroleum distillate of coal direct liquefaction hydrotreated oil and other oil sample.
中心切割二维气相色谱保留值定性分析煤直接液化加氢改质油
heart-cuttingtwo-dimensional gas chromatographyidentification by retention timecoal direct liquefaction hydrogenation modification oil
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