A Kinetic Study on the Mass Transfer Phenomena in Reversed-Phase Liquid Chromatography

反相液相色谱传质现象的动力学研究

基本信息

批准号：
12640581
负责人：
MIYABE Kanji
金额：
$ 2.24万
依托单位：
Nagoya Institute of Technology (2003)University of Toyama (2000-2002)
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 2003
项目状态：
已结题

项目摘要

Kinetic studies on the mass transfer phenomena in columns were studied by means of pulse response experiments and the moment analysis under the conditions of reversed-phase liquid chromatography (RPLC). Various stationary phases having different physical and chemical properties were used, that is, porous silica gel particles bonded with alkyl chains of different carbon numbers, porous silica gel particles bonded with C_<18>-ligands of different surface coverages, porous silica gel particles bonded with phenyl group, porous particles made of styrene-divinylbenzene copolymer, and porous particles made of graphitic carbon. Methanol/water mixtures and standard materials of benzene derivatives and phenol derivatives were mainly used as the mobile phases and sample compounds, respectively. The information about the retention equilibrium and mass transfer kinetics were derived from the first absolute moment and the second central moment of the elution peak profiles. Especially, the characteri … More stics and mechanism of surface diffusion were studied in detail. To the best of the author's knowledge, there is so far no systematic study on surface diffusion. Thermodynamic properties of the retention equilibrium and surface diffusion were derived from the results of the pulse response experiments carried out under different temperature conditions. It was tried to systematically analyze the results in this study from various points of view in order to consistently understand the separation mechanism in RPLC.On the basis of the results about surface diffusion, the surface-restricted molecular diffusion model was proposed for surface diffusion as a first approximation. The new model was formulated according to the absolute rate theory. This model is effective for a comprehensive interpretation of the intrinsic characteristics and mechanism of surface diffusion.New moment equations were derived for monolithic columns packed with continuous porous separation media by solving the basic equations of the general rate model of chromatography in the Laplace domain. They correlate the peak moments and some parameters characterizing the retention equilibrium and the mass transfer kinetics in monolithic columns. Some items of new information on the mass transfer kinetics in C_<18>-silica monolithic columns were derived by applying the new moment equations to a set of experimental data. The validity of the new moment equations was confirmed. Less

通过脉冲反应实验研究了柱中传质现象的动力学研究，以及在反相液相色谱（RPLC）条件下的力矩分析。 Various stationary phases having different physical and chemical properties were used, that is, porous silica gel particles bonded with alcohol chains of different carbon numbers, porous silica gel particles bonded with C_<18>-ligands of different surface Coverages, porous silica gel particles bonded with phenyl group, porous particles made of styrene-divinylbenzene copolymer, and porous particles made of graphical carbon.苯酚/水混合物和苯衍生物和苯酚衍生物的标准材料分别用作移动相和样品化合物。有关保留平衡和质量转移动力学的信息源自第一个绝对力矩和洗脱峰值谱的第二个中央力矩。尤其是，详细研究了表面扩散的更多的特征和表面扩散的机理。据作者所知，到目前为止，还没有关于表面扩散的系统研究。保留平衡和表面扩散的热力学特性是从在不同温度条件下进行的脉冲反应实验的结果得出的。它被尝试从各种角度系统地分析了这项研究的结果，以始终理解RPLC中的分离机制。在有关表面扩散的结果的基础上，提出了表面限制的分子扩散模型，以作为第一个近似的表面扩散模型。新模型是根据绝对速率理论制定的。该模型可有效地对表面扩散的内在特征和机制进行综合解释。通过求解拉普拉斯域中色谱的一般速率模型的基本方程，对整体柱进行了新的矩方程。它们将峰值矩和某些参数相关联，这些参数表征了整体柱中的保留平衡和传质动力学。通过将新的力矩方程应用于一组实验数据，可以得出有关C_ <18> - 硅整体柱中传播动力学的一些新信息。确认了新力矩方程的有效性。较少的