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论文编号:HG137 论文字数:10262,页数:35
摘 要:采用二维气相色谱方法分析汽油中氧化物添加剂;采用配有微板流路控制阀(Deans switch)的Agilest 7890N 气相色谱系统,进行动态中心切割,将汽油基体切入到第二根色谱柱,并可快速简便地设定切割时间。这一技术增强了色谱分离度,使得氧化物与烃类基质完全分开;提高了极性低含量添加剂分析结果的可信度;多种常用的氧化物添加剂的测定证实了系统卓越的校正和定量性能;用该方法分析汽油中0%~10%的含氧添加剂,各物质校正曲线的线性相关性良好,相关系数均大于0.999;标准样品5次重复测定的相对标准偏差均小于1.29%;车用汽油实际样品中含氧添加剂的加标回收率在90%~110%之间;采用反吹技术可以大大的减少分析时间,提高了分析效率。该方法是车用汽油中含氧添加剂测定的一种快捷,准确可靠的分析方法。
关键词:二维气相色谱;微板流路控制技术;含氧添加剂;汽油
Abstract: A two-dimensional GC method for the analysis of oxygenated additives in gasline is described .This method employ an Agilent 7890N GC system equipped with a Deans swith device to dynamically heart-cut the analytes from the gasline matrix to a second GC column . The unique design of the heat-cut device allows fast easy method setup when determining cut times .The Agilent 7890N GC electronic pneumatices control (EPC) used for this system provides better retention time precision that allows narrower cut times for better resolution an quantitative precision . Excellent calibration an quantitative performance of this system is demonstrated for several commonly used oxygenated additives .The linearity test showed that the correlation coefficient r2 values for oxygenated additives were all higher than 0.999.The results showed that the relative standard (RSDs) of standard samples in five continued were within 1.29%and the recoveries of added standards tests were from 90%~110%.The EPC of the Agilent 7890N GC is shown to enable greater productivity by decreasing analysis times with a backflushing technique .The method is quick ,sinple an useful for the determination of oxygenated in gasline .
Keywords:two-dimensional gas chromatography ;capillary flow technique (Deans Switch );oxygenated ;gasline
目 录
中文摘要 I
英文摘要 II
目录 III
1 绪论 1
研究背景 1
1.2 目前提高辛烷值的方法 1
1.3 含氧添加剂现状 2
1.4 汽油中含氧物质的测定 3
1.4.1 传统方法 3
1.4.2 二维气相色谱中心切割技术 4
2 实验部分 5
2.1 Deans Switch 工作原理 5
2.2 仪器、试剂及分析条件 7
3 结果与讨论 9
3.1 建立电磁阀切割时间表 9
3.2 校正曲线的测绘 14
3.3 精密度 17
3.4 ASTM D4815专用标准混标的测定 18
3.5 汽油样品的测定和加标回收率 19
4 总结与展望 21
4.1 总结 21
4.2 展望 21
致 谢 23
附录 26