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首页> 外文学位 >Retention behavior of poly(methyl methacrylate), poly(ethylene glycol) and poly(tryptophan) in reversed-phase liquid chromatography.
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Retention behavior of poly(methyl methacrylate), poly(ethylene glycol) and poly(tryptophan) in reversed-phase liquid chromatography.

机译：聚（甲基丙烯酸甲酯），聚（乙二醇）和聚（色氨酸）在反相液相色谱中的保留行为。

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摘要

The application of reversed-phase liquid chromatography in separations of macromolecules has been studied for over a decade. There are many reports on the success of this technique. However, the fundamental retention mechanism remains unclear. While some assert that a special retention model is needed for polymers, others contend that polymers just behave like small molecules and conventional chromatographic theory can well explain the retention behavior. The controversy in retention mechanism hinders the full exploitation of the power of reversed-phase liquid chromatography in polymer separations.; In this study, the retention behavior of three model polymers, poly(methyl methacrylate) (PMMA), poly(ethylene glycol) (PEG) and poly(tryptophan) (PTRP) in reversed-phase liquid chromatography is examined. The key to this research is to obtain isocratic retention data under various conditions and to correlate isocratic retention with gradient retention. With various solvent mixtures as mobile phases, isocratic retention is observed for all three polymers and a linear relationship between the logarithm of the capacity factor, k{dollar}spprime{dollar} and the volume fraction of the organic modifier in aqueous binary or ternary solvent mixtures is found. The influence of mobile phase on retention and the interaction of polymers with the stationary phase are studied using the results from the chromatographic experiments. The success in interrelating isocratic elution with gradient elution using the Linear-Solvent-Strength model (LSS) supports that the polymer retention mechanism fundamentally resembles the one for small molecules, though there are some unique characteristics about polymers. The LSS model is found to provide a way of predicting retention and separation of polymers with moderate accuracy (5% to 15% error). As a gateway to the retention mechanism, the temperature effect on retention is investigated. The thermodynamic parameters such as {dollar}Delta{dollar}H and {dollar}Delta{dollar}S of the polymer retention process are obtained from Van't Hoff plots. These parameters are found useful not only for studying retention mechanisms but for obtaining separation and information about polymer molar mass as well. Preliminary study of factor analytical modeling of retention data indicates that factor analysis is a useful technique for study of retention mechanisms. Factor analysis is performed on the retention data under different temperatures. The molar mass is found to be a real factor for the solute space and unknown molar mass can be calculated via the free-floating method. Some interesting topics for future study of polymer chromatography are suggested as the extension of this study.
机译：反相液相色谱在大分子分离中的应用已经研究了十多年。关于此技术成功的报道很多。但是，基本保留机制仍不清楚。尽管有些人断言聚合物需要特殊的保留模型，但另一些人则认为聚合物的行为就像小分子一样，传统的色谱理论可以很好地解释保留行为。保留机制的争议阻碍了反相液相色谱在聚合物分离中的功能的充分利用。在这项研究中，研究了三种模型聚合物，聚甲基丙烯酸甲酯（PMMA），聚乙二醇（PEG）和聚色氨酸（PTRP）在反相液相色谱中的保留行为。这项研究的关键是获得各种条件下的等度保留数据，并将等度保留与梯度保留相关联。在各种溶剂混合物作为流动相的情况下，观察到所有三种聚合物的等度保留，容量因子k {dollar} spprime {dollar}的对数与二元或三元水溶液中有机改性剂的体积分数之间呈线性关系找到混合物。使用色谱实验的结果研究了流动相对保留和聚合物与固定相相互作用的影响。使用线性溶剂强度模型（LSS）成功完成了等度洗脱与梯度洗脱的相互联系，这支持了聚合物保留机理从根本上类似于小分子的保留机理，尽管聚合物具有一些独特的特性。发现LSS模型提供了一种以中等准确度（5％至15％误差）预测聚合物保留和分离的方法。作为保持机制的途径，研究了温度对保持力的影响。聚合物保留过程的热力学参数，例如{Delta} {H}和{Delta} S，是从Van't Hoff图获得的。发现这些参数不仅对于研究保留机理有用，而且对于获得分离和关于聚合物摩尔质量的信息也是有用的。对保留数据进行因子分析建模的初步研究表明，因子分析是研究保留机制的有用技术。在不同温度下对保留数据进行因子分析。发现摩尔质量是溶质空间的真实因素，并且可以通过自由漂浮法计算未知的摩尔质量。作为该研究的扩展，提出了一些未来聚合物色谱研究的有趣话题。

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  • 作者

    Jiang, Chun.;

  • 作者单位

    Duke University.;

  • 授予单位 Duke University.;
  • 学科 Chemistry Analytical.; Chemistry Polymer.
  • 学位 Ph.D.
  • 年度 1994
  • 页码 240 p.
  • 总页数 240
  • 原文格式 PDF
  • 正文语种 eng
  • 中图分类 化学;高分子化学（高聚物）;
  • 关键词

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