The kinetic plot method applied to gradient chromatography: Theoretical framework and experimental validation

The kinetic plot method applied to gradient chromatography: Theoretical framework and experimental validation
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DOI:
10.1016/j.chroma.2010.02.023
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发表时间:
2010-04-23
影响因子:
4.1
通讯作者:
Desmet, G.
Desmet, G.
中科院分区:
化学2区
文献类型:
--
作者:
Broeckhoven, K.;Cabooter, D.;Desmet, G.

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动力学图法,最初开发的等度分离,扩展到实际上更相关的梯度洗脱分离的情况下。已经建立了一组显式和隐式数据转换表达式。这些表达式可以容易地在任何计算电子表格程序中实现,并且允许将表示在单个柱上测量的分离效率和流速之间的关系的任何实验数据集直接转换为测试的分离介质的动力学性能极限曲线。由于动力学性能限度曲线基于外推至不同长度的色谱柱,因此应认识到,该曲线仅在以下假设下有效:梯度时间和延迟时间(如有)经过调整,使得当色谱柱长度改变时,分析物经历相同的相对移动的相历史。实验和数值数据都证实了这样一个事实,即使用所提出的表达式获得的动力学性能极限曲线确实是独立的柱长度的实验数据收集。如果在具有明显的非绝热热行为的柱中发生过度的粘性加热,则可能出现偏差。(C)2010爱思唯尔有限公司版权所有。
The kinetic plot method, originally developed for isocratic separations, was extended to the practically much more relevant case of gradient elution separations. A set of explicit as well as implicit data transformation expressions has been established. These expressions can readily be implemented in any calculation spread-sheet program, and allow to directly turn any experimental data set representing the relation between the separation efficiency and the flow rate measured on a single column into the kinetic performance limit curve of the tested separation medium. Since the kinetic performance limit curve is based on an extrapolation to columns with a different length, it should be realized that the curve is only valid under the assumption that the gradient time and the delay time (if any) are adapted such that the analytes are subjected to the same relative mobile phase history when the column length is changed. Both experimental and numerical data are presented to corroborate the fact that the kinetic performance limit curves that are obtained using the proposed expressions are indeed independent of the column length the experimental data were collected in. Deviations might arise if excessive viscous heating occurs in columns with a pronounced non-adiabatic thermal behaviour. (C) 2010 Elsevier B.V. All rights reserved.