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亚临界水-火焰离子化检测-柱后分流色谱分离某些醇、酚和羧酸类化合物

Separation of Some Alcohols, Phenols and Caboxylic Acids by Coupling of Subcritical Water Chromatography and Flame Ionization Detection with Post-column Splitting

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【作者】 富玉宋瑞娟姚娜龙远德黄天宝

【Author】 Fu Yu1, 2, Song Rui-Juan1, 2, Yao Na1,2, Long Yuan-De1, Huang Tian-Bao11(Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences, Chengdu 610041)2(Graduate School of the Chinese Academy of Sciences, Beijing 100049)

【机构】 中国科学院成都有机化学研究所中国科学院成都有机化学研究所 成都610041中国科学院研究生院北京100049成都610041

【摘要】 采用柱前预热和柱后分流技术,构建了亚临界水-氢火焰离子化检测器色谱系统(SubWC-FID)。采用Polymerx RP-1聚合物色谱柱和纯水流动相,在亚临界状态下(柱温160~210℃),分离了某些醇、酚和羧酸类化合物,优化了FID稳定工作条件,考察了柱温、流动相流速和分流比对样品分离的影响。结果表明:在不高于1.48mL/min的流动相流速下,柱后分流模式的FID系统能稳定工作,方法的线性动力学范围在2~3个数量级之间,在分流比为1∶20时,乙醇、苯酚和乙酸的检出限分别为17、54和68ng。

【Abstract】 A coupling system of subcritical water chromatography and flame ionization detection (SubWC-FID) with pre-column heating and post-column splitting mode has been established. Separations of some alcohols, phenols and carboxylic acids have been performed on a Polymerx RP-1 (PS-DVB) column with the column temperature ranging from 160℃ to 210℃ by using the SubWC-FID system and pure water as mobile phase. The stable working conditions of FID have been optimized and the effects of column temperature, flow rate of mobile phase and splitting ratio on the sample separations have been examined. The results indicate that the FID system with post-column splitting is stable even at flow-rate of mobile phase as high as 1.48 mL/min. The linear dynamic ranges are between two and three orders of magnitude and the limits of detection of ethanol, phenol and acetic acid at splitting ratio of 1∶20 are 17 ng, 54 ng and 68 ng, respectively.

  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2007年09期
  • 【分类号】O657.3
  • 【被引频次】5
  • 【下载频次】110
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