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Selectivity enhancement for the separation of shape-constrained isomers by particle size-derived molecular ordering and density in reversed-phase liquid chromatography

机译:分离的选择性增强由粒子shape-constrained同分异构体size-derived分子分类和密度反相液相色谱

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摘要

The purpose of this study is to describe the enhancement of molecular-shape selectivity and grafted polymer characteristics by altering the particle size, pore size, and polymer chains of polymer-silica hybrid materials used in reversed-phase liquid chromatography. The poly(octadecyl acrylate-alt-N-octadecylmaleimide)-grafted silica hybrid materials were prepared with 3 and 5 mu m particle size silica, respectively. The alternating copolymerisations were conducted with 3-mercaptopropyltrimethoxysilane-modified silica via surface-initiated radical chain transfer reactions. The polymer-silica hybrid materials were characterised by elemental analyses, diffuse reflectance FTIR spectroscopy, solid-state C-13 and Si-29 cross-polarisation-magic-angle spinning and suspended-state H-1 NMR spectroscopy. The NMR spectroscopy results revealed that the alkyl chains of 3 mu m particle size phase are more ordered than those of 5 mu m particle size phase at lower temperatures and vice versa at higher temperatures. After detailed characterisation, the hybrid materials were packed into a stainless-steel column, and their chromatographic performance with polycyclic aromatic hydrocarbons was compared. Regardless of the grafting-density, ordering of the alkyl chains, and column temperature, differences in molecular-planarity selectivity molecular-linearity were observed. Aspects of molecular-shape selectivity were also evaluated using the standard reference material for priority pollutant polycyclic aromatic hydrocarbons.
机译:本研究的目的是描述增强的分子形状选择性和接枝聚合物通过改变特征粒度、孔隙大小和聚合物链polymer-silica混合使用的材料反相液相色谱法。聚十八基acrylate-alt-N-octadecylmaleimide)接枝硅混合材料准备和3和5μm分别粒径硅。copolymerisations交替进行3-mercaptopropyltrimethoxysilane-modified硅通过表面自由基链转移反应。特征是元素分析、扩散固态c13反射红外光谱和Si-29 cross-polarisation-magic-angle旋转和挂起状态h - NMR光谱。光谱分析结果表明,烷基链3μm粒度相比较比5μm命令粒度的阶段在较低的温度和更高亦然温度。挤在一个混合材料不锈钢列,和它们的色谱性能与多环芳烃进行了比较。烷基链的顺序,列温度,molecular-planarity差异选择性molecular-linearity被观察到。方面的分子形状选择性也评估使用标准的参考资料优先污染物多环芳香碳氢化合物。

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