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Effect of Column Structure on Separation Efficiency in Low-Temperature HPLC Using Pure Liquid Carbon Dioxide as the Mobile Phase

机译:以纯液态二氧化碳为流动相的低温HPLC中色谱柱结构对分离效率的影响

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The effect of column structure and chromatographic conditions (flow rate, inlet pressure, and temperature) on separation behavior in low-temperature HPLC using pure liquid CO_(2) mobile phase was investigated. Three types of packed columns (fully porous, small nonporous, and core-shell particles) and a monolithic column (fully porous) were used. The effect of temperature (-5 to -30°C), inlet pressure (5.3 or 6.3 MPa), and flow rate (1 or 2 mm/s) on chromatographic behavior was evaluated. The retention factors of the analytes (naphthalene, anthracene, and pyrene) were not affected by either inlet pressure or flow rate. Although the column temperature somewhat affected the separation efficiency, the typical relationship between temperature and separation efficiency was not observed. On the other hand, both inlet pressure and flow velocity affected the separation efficiency. In this study, the highest separation efficiency was achieved in the core-shell column with a flow rate of 1 mm/s and inlet pressure of 6.3 MPa. The best separation efficiency under this condition was 12 ?m in theoretical plate height (85 000 N /m) for pyrene at -30°C. In addition, the supplied liquid CO_(2) was found to solidify in the column at low temperatures and its behavior also depends on both the chromatographic conditions (particularly for flow rate) and the column structure. The typical relationship between solidification and chromatographic behavior was not observed clearly.
机译:在纯液相CO_(2)流动相的低温HPLC中,研究了色谱柱结构和色谱条件(流速,入口压力和温度)对分离行为的影响。使用了三种类型的填充柱(完全多孔,小的无孔和核-壳颗粒)和整体柱(完全多孔)。评估了温度(-5至-30°C),入口压力(5.3或6.3 MPa)和流速(1或2 mm / s)对色谱行为的影响。分析物(萘,蒽和race)的保留因子不受入口压力或流速的影响。尽管柱温在某种程度上影响分离效率,但未观察到温度与分离效率之间的典型关系。另一方面,入口压力和流速都影响分离效率。在这项研究中,在芯壳塔中以1 mm / s的流速和6.3 MPa的入口压力实现了最高分离效率。在此条件下,pyr的最佳分离效率是在-30°C下theoretical的理论塔板高度为12 µm(85 000 N / m)。另外,发现所供应的液体CO_(2)在低温下会在色谱柱中凝固,其行为还取决于色谱条件(尤其是流速)和色谱柱结构。没有清楚地观察到固化与色谱行为之间的典型关系。

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