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毛细管气相色谱切割反吹技术归一化法定量分析航空煤油中的芳烃

Capillary Gas Chromatographic Column Switching-Backflushing Technique for the Analysis of Aromatics in Aviation Kerosene by Normalization Method

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【作者】 沈伟健王涵文赵景红王正萍王风云关亚风

【Author】 Shen Weijian 1,2 ,Wang Hanwen 1,Zhao Jinghong 1,Wang Zhengping 2,Wang Fengyun 2,Guan Yafeng *1 1(Dalian Institute of Chemical Physics,Chinese Academy of Sciences,Dalian 116012) 2(School of Chemistry Engineering ,Nanjing University of Science & Technology,Nanjing 210094)

【机构】 中国科学院大连化学物理研究所南京理工大学化工学院中国科学院大连化学物理研究所 大连116012南京210094大连116012大连116012

【摘要】 用气相毛细管色谱切割反吹技术 ,和在FFAP毛细管预柱上芳烃比高它 3个碳数的烷烃之后出峰的特点 ,通过阀切换把芳烃反吹入非极性OV 1分析柱中 ,按照沸点进行分离。从预柱上先流出的组分和从分析柱上后流出的组分先后通过微型三通进入同一个FID检测器 ,因此可用校正响应因子归一化法进行定量分析。从预柱出口到检测器之间的阻尼柱阻力 6倍于分析柱阻力 ,反吹后因载气流速提高 5 .4倍而有效地压缩了谱带 ,提高芳烃等目标组分的检出灵敏度 2倍。通过切割反吹操作能很好地完成航空煤油中从苯到C11芳烃的检测 ,阀切换的可允许时间窗口达± 18s,且分析结果的重现性误差RSD≤ 4 .0 %。

【Abstract】 The aromatics in aviation kerosene was separated and analyzed by capillary gas chromatography using column switching-backflushing technique. The aromatics having carbon number of n are retained after n -C_ n +3 on the FFAP pre-column,and were cut and back flushed after the elution of n -C_ n +3 ,onto a nonpolar analytical column and were separated according to their boiling points. Since the early eluting components from the pre-column,and the aromatics and heavier saturates from the analytical column are all directed to the same flame ionization detector through a “T” piece,a factor corrected normalization method can be applied for quantitation. The resistance of the resistor after the pre-column is designed 6 times higher than that of analytical column,resulting in 5.4 times higher carrier gas flow rate after backflushing. The chromatographic bands are compressed,enhancing the sensitivity 2 times more for aromatics and heavier saturates. Two aviation kerosene samples were analyzed and the switching time window is more than ±18 s. The error of reproducibility of the analysis is ≤4.0%.

  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2004年07期
  • 【分类号】O657.7;TE622
  • 【被引频次】12
  • 【下载频次】309
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