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Abnormal phenomenon of the dependence of the retention factors for uncharged species on applied voltage in capillary electrochromatography

机译:毛细管电色谱中不带电物质的保留因子对施加电压的依赖性异常现象

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Polymethacrylate-based monolithic columns were prepared for capillary electrochromatography (CEC) by in situ copolymerization of butyl methacrylate (BMA), 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS), and ethylene dimethacrylate (EDMA) in the presence of a porogen in fused-silica capillaries of 100 mum I.D. The abnormal phenomenon that retention factors for neutral species decreases with applied voltage in CEC was observed. Capillary electrophoresis (CE) instruments usually require a period of time to increase voltage from 0 kV to desired value, which is called as ramp time. Such ramp time and any error in the determination of dead time should be taken into account during the accurate calculation of retention factors. After the correction of the retention factors, the plots of the corrected factors for alkylbenzene versus applied voltage were made, the absolute value of the plot slopes are less than 1.8 X 10(-4), Which indicates that the corrected retention times for neutral species do not show any dependence on applied voltage. Further, the plots of the corrected retention times for acidic and basic compounds versus the reciprocal of applied voltage were drawn, where the target compounds were eluted in neutral form. The very nice linearity of the plots was obtained. The linear correlation coefficients are over 0.999. Here, the slopes of the plots represent [GRAPHICS] which indicates that retention factors for the test compounds are constants under a given separation condition. [References: 23]
机译:通过在甲基丙烯酸丁酯(BMA),2-丙烯酰胺基-2-甲基-1-丙磺酸(AMPS)和二甲基丙烯酸乙二酯(EDMA)的条件下原位共聚制备用于毛细管电色谱(CEC)的基于聚甲基丙烯酸酯的整体柱。 100毫米ID的熔融石英毛细管中的致孔剂在CEC中观察到中性物质的保留因子随施加电压而降低的异常现象。毛细管电泳(CE)仪器通常需要一段时间才能将电压从0 kV增加到所需值,这称为斜坡时间。在精确计算保留因子时,应考虑到这种斜坡时间和死区时间确定中的任何错误。校正保留因子后,绘制烷基苯校正因子对施加电压的图,该图斜率的绝对值小于1.8 X 10(-4),这表明中性物质的校正保留时间不显示对施加电压的任何依赖性。此外,绘制了酸性和碱性化合物的校正保留时间与施加电压倒数的关系图,其中目标化合物以中性形式洗脱。获得了非常好的线性关系图。线性相关系数超过0.999。在此,曲线的斜率表示[图形],其表示测试化合物的保留因子在给定的分离条件下为常数。 [参考:23]

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