摘要:
采用戴安公司谱睿(Pre)在线样品前处理技术,使用高容量在线Ag柱和Na柱,开发出了一种柱前去除高氯基体中氯离子的在线分析方法。操作简便,且适用样品范围广;不更换Ag柱可耐受10 g/L NaCl基体,25 μL连续进样400针,氯离子去除效率可保持在99%以上。系统选用高容量IonPac AS11-HC氢氧根体系阴离子交换色谱柱,在线淋洗液自动发生装置进行梯度淋洗,用抑制型电导检测。对食盐、分析纯氯化钠等不同基体进行检测,可实现样品在线除氯,并可检测其中不高于10 μg/L的溴酸根、氯酸根、亚硝酸根、硝酸根和硫酸根等离子。不同离子校准曲线相关系数均在99.8%以上,加标回收率为80%~110%。该技术具有操作简单、可重复性强、方法新颖等特点,解决了以往高氯基体检测成本过高、适用范围有限、前处理操作复杂等问题。
Abstract:
We developed a method in which Dionex "Pre" online sample preparation technique was used to remove chloride by Ag cartridge and Na cartridge. This method is applicable to a wide range of samples and is simpler than off-line approach. Each Ag cartridge carries on 400 consecutive injections (25 microlitre each) of 1% NaCl solution, and the removal efficiency is still above 99%. The separation of anions was carried out by high capacity hydroxide selectivity IonPac AS11-HC gradient separation column while Eluent Generator was employed to generate gradient KOH eluent online automatically. Two valves were switched to finish the injection. The system removes chloride well online for different matrix as analysis grade salt and sodium chloride. The detection limits of bromate, chlorate, chlorite, nitrite, nitrate and sulfate are less than 10 μg/L, and the recoveries are between 80% and 110%. This method holds the advantages of easy-operation, good reproducibility, lower operation cost etc and is more convenient than off-line approach.
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