Katsuo Shigeharu, Langel Christian, Schanen Patrick, Mazzotti Marco
Institute of Process Engineering, ETH Zurich, Sonneggstrasse 3, CH-8092 Zurich, Switzerland.
J Chromatogr A. 2009 Feb 13;1216(7):1084-93. doi: 10.1016/j.chroma.2008.12.031. Epub 2008 Dec 24.
In small-scale SMB units typically set up by a number of HPLC columns connected in series, the volume of the connecting tubing parts and valves may become comparable to the column volume. Therefore, to guarantee proper and satisfying separation results, the introduced extra-column dead volume needs to be considered in the calculations of the operating parameters. In this work, the impact of extra-column dead volume on the separation performance is studied, with the objective to introduce guidelines and rather simple rules to account for it. It is shown, how these results can be used in the frame of the triangle theory to determine operating conditions that allow to achieve the desired separation performance. For the experiments the separation of a racemic mixture of (+/-)-3,5-bis[1-(4-methoxyphenyl)-1-methyl]hepta-3,4-diene-1,6-diyne was carried out. The numerical model used for the simulation describes explicitly the geometric configuration of the HPLC-SMB laboratory unit to take into account the effect of extra-column dead volume.
在通常由多个串联的高效液相色谱（HPLC）柱组成的小规模模拟移动床（SMB）单元中，连接管部件和阀门的体积可能与柱体积相当。因此，为了保证获得合适且令人满意的分离结果，在操作参数计算中需要考虑引入的柱外死体积。在这项工作中，研究了柱外死体积对分离性能的影响，目的是引入相关指导方针和相当简单的规则来对其进行考量。结果表明，这些结果如何能在三角形理论框架内用于确定能够实现所需分离性能的操作条件。对于实验，进行了（±）-3,5-双[1-（4-甲氧基苯基）-1-甲基]庚-3,4-二烯-1,6-二炔外消旋混合物的分离。用于模拟的数值模型明确描述了HPLC-SMB实验室单元的几何构型，以考虑柱外死体积的影响。
