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作为层析填充材料的精细核壳颗粒的物理性质和结构。颗粒特性与柱效之间的关系。

Physical properties and structure of fine core-shell particles used as packing materials for chromatography Relationships between particle characteristics and column performance.

机构信息

Department of Chemistry, University of Tennessee, Knoxville, TN 37996-1600, USA.

出版信息

J Chromatogr A. 2010 Jun 11;1217(24):3819-43. doi: 10.1016/j.chroma.2010.04.026. Epub 2010 Apr 20.

DOI:10.1016/j.chroma.2010.04.026
PMID:20447642
Abstract

The recent development of new brands of packing materials made of fine porous-shell particles, e.g., Halo and Kinetex, has brought great improvements in potential column efficiency, demanding considerable progress in the design of chromatographic instruments. Columns packed with Halo and Kinetex particles provide minimum values of their reduced plate heights of nearly 1.5 and 1.2, respectively. These packing materials have physical properties that set them apart from conventional porous particles. The kinetic performance of 4.6mm I.D. columns packed with these two new materials is analyzed based on the results of a series of nine independent and complementary experiments: low-temperature nitrogen adsorption (LTNA), scanning electron microscopy (SEM), inverse size-exclusion chromatography (ISEC), Coulter counter particle size distributions, pycnometry, height equivalent to a theoretical plate (HETP), peak parking method (PP), total pore blocking method (TPB), and local electrochemical detection across the column exit section (LED). The results of this work establish links between the physical properties of these superficially porous particles and the excellent kinetic performance of columns packed with them. It clarifies the fundamental origin of the difference in the chromatographic performances of the Halo and the Kinetex columns.

摘要

新型精细多孔壳颗粒包装材料(如 Halo 和 Kinetex)的发展带来了潜在柱效率的巨大提高,这对色谱仪器的设计提出了更高的要求。填充 Halo 和 Kinetex 颗粒的色谱柱的塔板高度分别接近 1.5 和 1.2,达到了最小化。这些包装材料具有独特的物理性质,与传统多孔颗粒不同。基于一系列 9 个独立且互补的实验结果,分析了填充这两种新型材料的 4.6mm ID 色谱柱的动力学性能:低温氮气吸附(LTNA)、扫描电子显微镜(SEM)、反尺寸排除色谱(ISEC)、库尔特计数器粒度分布、比重瓶法、理论塔板高度(HETP)、峰停泊法(PP)、总孔阻塞法(TPB)和柱出口部分的局部电化学检测(LED)。这项工作的结果将这些表面多孔颗粒的物理性质与填充它们的色谱柱的优异动力学性能联系起来。它阐明了 Halo 和 Kinetex 柱之间色谱性能差异的根本原因。

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