Australian Centre for Research on Separation Science (ACROSS), School of Chemistry, University of Tasmania, Private Bag 75, Hobart 7050, Tasmania, Australia.
J Chromatogr A. 2010 Jul 30;1217(31):5057-62. doi: 10.1016/j.chroma.2010.05.066. Epub 2010 Jun 8.
The first use of the kinetic plot method to characterise the performance of ion-exchange columns for separations of small inorganic anions is reported. The influence of analyte type (mono- and divalent), particle size (5 and 9microm), temperature (30 and 60 degrees C) and maximum pressure drop upon theoretical extrapolations was investigated using data collected from anion-exchange polymeric particulate columns. The quality of extrapolations was found to depend upon the choice of analyte, but could be verified by coupling a series of columns to demonstrate some practical solutions for ion chromatography separations requiring relatively high efficiency. Separations of small anions yielding 25-40,000 theoretical plates using five serially connected columns (9microm particles) were obtained and yielded deviations of <15% from the kinetic plot predictions. While this approach for achieving high efficiencies results in a very long analysis time (t(0)=21min), separations yielding approximately 10,000 theoretical plates using two serially connected columns (t(0)<5min) were shown to be more practically useful for isocratic separations when compared to use of a single column operated at optimum linear velocity (t(0)>10min).
首次报道了利用动力学谱图法来描述用于分离无机小分子阴离子的离子交换柱性能的方法。使用从阴离子交换聚合物颗粒柱上收集的数据,研究了分析物类型(单价和二价)、粒径(5μm 和 9μm)、温度(30℃和 60℃)和最大压降对理论外推的影响。发现外推的质量取决于分析物的选择,但可以通过耦合一系列柱子来验证,为需要相对高效率的离子色谱分离提供一些实际的解决方案。使用五根串联柱(9μm 颗粒)进行的小阴离子分离,得到了 25-40,000 理论板的分离,并且与动力学谱图预测值的偏差小于 15%。虽然这种实现高效率的方法导致分析时间非常长(t(0)=21min),但是与在最佳线性速度下操作单个柱子(t(0)>10min)相比,使用两根串联柱子进行的大约 10,000 理论板的分离对于等度分离更实用。