本文通过离子色谱与柱切换技术联用实现了高浓度样品基体中的痕量阴离子检测。分别研究了不同类型基体的处理方法,使用商品化离子排斥柱和自制的聚合物色谱柱实现多种样品基体中痕量阴离子的检测。同时开发一种简化的单泵柱切换系统,利用抑制器将KOH淋洗液转化为水作为前处理柱的淋洗液,在同一个色谱系统中产生两种淋洗液,实现色谱分离与前处理柱再生同步进行。采用离子排斥柱作为前处理柱分析了有机酸和有机酸盐中的三种常见阴离子,检测限达到0.1~1.7μg/L,方法相对标准偏差小于5%,样品加标回收率在75.2%~114.6%之间;同时采用自制的色谱柱作为前处理柱在同一分析系统中实现多种样品基体中七种常见痕量阴离子的分析,检测限在0.4~2.3,μg/L之间,方法相对标准偏差小于4%,样品加标回收率在88.1%~109.5%之间。该方法使用简便,准确性高,是一种极有利用价值的在线样品前处理技术。
In this study, trace anions in complex matrix of high concentration were determined using ion chromatography with single-pump column-switching technique. Various types of matrix treatments were investigated. Trace ions in multiple sample matrix were analyzed using both commercial ion exclusion columns and home-made polymer-based columns. In the meantime, a simplified single-pump-column-switching system has been developed. In this system, a suppressor is used to convert KOH eluent into water, which is used as the eluent for the pretreatment column. Therefore, in same chromatography system, two kinds of eluents can be produced, which allows chromatographic separation and pretreatment column regeneration processes to proceed simultaneously. In this research, ion exclusion columns were used as the pretreatment columns to analyze three ordinary anions in the organic acids and their salts. The detectionlimits were tested as in the range of 0.1-1.7 μg/L, RSDs were less than 5%, and the recoveries were in the range of 75.2%-114.6% In addition, by using the home-made polymer column in the same chromatography system, seven ordinary trace anions in multiple sample matrix were determined simultaneously. The detection limits were about 0.4-2.3 μg/L, RSDs were less than 4% and the recoveries were about 88.1%-109.5%. In conclusion, this column switching technique is simple to use and with high accuracy, thus,is very useful for on-line sample pretreatment.