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Development of New Separation Analysis and Continuous Flow Analysis Using Supercritical Water or Subcritical Water

使用超临界水或亚临界水的新型分离分析和连续流动分析的开发

基本信息

批准号：
12650795
负责人：
MORISHITA Fujio
金额：
$ 2.18万
依托单位：
KYOTO UNIVERSITY
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2000
资助国家：
日本
起止时间：
2000 至 2001
项目状态：
已结题

来源：
https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-12650795/
关键词：
supercritical and subcritical water chromatography using water as mobile phase retention selectivity retention index retention vector van't Hoff plot continuous flow analysis simultaneous determination 亜臨界水保持ベクトル超臨界水クロマトグラフィー極性

项目摘要

A chromatograph using supercritical water or subcritical water as mobile phase was constructed and its separation characteristics were investigated in order to elucidate its potentiality. One eminent aspect of the separation characteristics is the column efficiency. The HETP was increased slowly with the temperature of water mobile phase : a different behavior from that expected from the physical properties such as diffusivity. The other significant aspect of the separation characteristics is the retention behavior of various solutes. The solvent strength of water mobile phase was increased with the temperature and water mobile phase at 190 ℃ corresponded to the mixture of methanol and water (80/20). A new method describing and evaluating the retention selectivity was proposed, in which the retention indices of a set of standard solutes were measured relatively to linear alkane homologs. Taking into account the facts that alkanes are sparingly soluble in hot water and don't respond to … More UV detector, the homologous series of alkyl acetates were used as the reference for measurement of the retention index of any solutes. The retention indices of the former was determined by the calculation using a monoacetate and a diacetate. Five standard solutes of different types were chosen by reference to McReynolds' method in GC and so on. The retention vector reflecting the retention selectivity had the contributions of five different functional groups as element, which were determined as the difference in retention index between a standard solute and the homomorphic hydrocarbon. Some differences in the contribution of the same functional groups were observed between super-heated water and the mixture of methanol-water with comparable solvent strength. The extent of the variation in the retention selectivity with the water temperature was smaller than that with the composition of methanol-water mixture.Simultaneous determination by using plural reactors in series was also discussed for fundamental investigation of advanced techniques of continuous flow analysis using subcritical water. Less

构建了以超临界水或亚临界水为流动相的色谱仪，并研究了其分离特性，以阐明其潜力。分离特性的一个突出方面是柱效率。 HETP 随着水流动相的温度缓慢增加：与扩散率等物理性质预期的行为不同。分离特性的另一个重要方面是各种溶质的保留行为。水流动相的溶剂强度随着温度的升高而增加，190 ℃的水流动相相当于甲醇和水（80/20）的混合物。提出了一种描述和评估保留选择性的新方法，其中相对于直链烷烃同系物测量一组标准溶质的保留指数。考虑到烷烃难溶于热水且对紫外检测器无响应，因此使用同系的烷基乙酸酯作为测量任何溶质保留指数的参比。前者的保留指数通过使用单乙酸酯和二乙酸酯的计算来确定。参考气相色谱中的麦克雷诺方法等，选择了五种不同类型的标准溶质。反映保留选择性的保留向量有五个不同官能团作为元素的贡献，其被确定为标准溶质与同态烃之间保留指数的差异。在过热水和具有相当溶剂强度的甲醇-水混合物之间观察到相同官能团的贡献存在一些差异。保留选择性随水温变化的程度比随甲醇-水混合物的组成变化的程度要小。还讨论了使用多个串联反应器同时测定的方法，以对使用亚临界水进行连续流动分析的先进技术进行基础研究。较少的