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使用动力学图谱优化超高压液相色谱的分离时间。

Use of kinetic plots for the optimization of the separation time in ultra-high-pressure LC.

机构信息

Department of Chemical Engineering, Vrije Universiteit Brussels, Brussels, Belgium.

出版信息

J Sep Sci. 2010 Sep;33(17-18):2629-35. doi: 10.1002/jssc.201000339.

DOI:10.1002/jssc.201000339
PMID:20730838
Abstract

The kinetic-plot approach, in which experimental t(0) and N-values are extrapolated to the performance at maximum system pressure by increasing the column length, was validated by coupling 250×3 mm columns packed with 3 μm particles. The extra-column volume introduced by coupling columns could be neglected with respect to the peak volumes. Plate numbers of up to 132,000 were experimentally achieved by coupling four columns. The maximum deviation between the experimental and predicted plate numbers was 7% for two coupled columns, and decreasing to 0.1% for four coupled columns. Kinetic plots were used to find the conditions to separate a critical pair, with a preset value for the effective plate number, in the shortest possible time. For high-efficiency separations yielding 100,000 effective plates, the optimum critical-pair retention factor was around 4.5. Kinetic plots are presented to find the optimal column length to obtain the fastest possible 100,000 effective-plate separation, taking into account the effect of mobile-phase viscosity on column pressure, and consequently the optimum column length.

摘要

动力学曲线法通过增加柱长将实验的 t(0) 和 N 值外推至最大系统压力下的性能,该方法通过耦合 250×3mm 柱(装填 3μm 颗粒)进行了验证。对于峰体积,柱间体积可以忽略不计。通过耦合四根柱子,实验达到了高达 132000 块理论塔板数。实验和预测的塔板数之间的最大偏差为两个耦合柱的 7%,而四个耦合柱的偏差减小到 0.1%。动力学曲线用于找到在最短时间内分离具有预设有效塔板数的关键对的条件。对于产生 100000 个有效塔板的高效分离,最佳关键对保留因子约为 4.5。动力学曲线用于找到获得最快可能的 100000 个有效塔板分离的最佳柱长,同时考虑到流动相粘度对柱压的影响,以及由此产生的最佳柱长。

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