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Ground Organic Particles of ca. 3 μm Size as Chromatographic Separation Media in High Performance Liquid Chromatography
Chromatographia ( IF 1.7 ) Pub Date : 2020-04-21 , DOI: 10.1007/s10337-020-03894-z
Yune Sung Kim , Jeong Soo Kim , Genlin Sun , Hyun Joo An , Won Jo Cheong

A new chromatographic stationary phase was prepared by making a soft organic monolith based on thermal polymerization of methyl methacrylate and ethylene glycol di-methacrylate with an aid of gas evolution via decomposition of urea, and by crushing the monolith into particles. The original purpose of urea incorporation was formation of monolith particles with affluent mesopores, but the actual effect was reduction of the particle size to a proper range (mostly in the range of 1–5 μm with an average of ca. 3 μm), which was very crucial for improvement of separation efficiency. A series of washing processes (including common washing and reflux washing) were carried out to remove un-reacted materials and free oligomers. The columns were made by packing the organic monolith particles in glass-lined stainless-steel tubing and evaluated for their performance with the mixture of six aromatic compounds (3-phenyl-1-propanol, acetophenone, methyl benzoate, 2-nitroaniline, ethylbenzene, cumene). The overall number of theoretical plates ( N ) over 6 analytes based on 6 columns was 32,000 plates/column (107,000 plates/m, 9.4 µm plate height).

中文翻译:

约的地面有机颗粒。3 μm 尺寸作为高效液相色谱中的色谱分离介质

基于甲基丙烯酸甲酯和乙二醇二甲基丙烯酸酯的热聚合,借助尿素分解放出气体,制备软有机整料,然后将整料粉碎成颗粒,制备了一种新型色谱固定相。尿素掺入的最初目的是形成具有丰富中孔的整体颗粒,但实际效果是将粒径减小到合适的范围(主要在 1-5 μm 的范围内,平均约为 3 μm),即对提高分离效率至关重要。进行一系列洗涤过程(包括普通洗涤和回流洗涤)以去除未反应的物质和游离的低聚物。这些色谱柱是通过将有机整体颗粒填充在搪玻璃不锈钢管中制成的,并用六种芳香族化合物(3-苯基-1-丙醇、苯乙酮、苯甲酸甲酯、2-硝基苯胺、乙苯、异丙苯)。基于 6 根色谱柱的 6 种分析物的理论塔板总数 (N) 为 32,000 塔板/列(107,000 塔板/m,9.4 µm 塔板高度)。
更新日期:2020-04-21
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