Y. S. Fung, H. S. Tung
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引用次数: 15
Abstract
Solving the problem due to transition metals' comigration during electrokinetic injection, the transient isotachophoresis (ITP) procedure was developed to preconcentrate and focus transition metals during electrokinetic injection. It was found to provide a suitable method for trace metals' preconcentration from rainwater at sub-μg/L level from buffer system consisting of 30 mM hydroxylamine hydrochloride, 0.1 mM 1,10-phenanthroline, 1% methanol, 15 mM ammonium chloride, and 0.08 M urea at pH=3.7. Trace metals as Cd2+, Zn2+, Cu2+, Co2+, and Fe2+ (total Fe determined as Fe2+) are determined with working range from 0.5–80 μg/L, repeatability less than 7%, and detection limits from 0.1 to 0.5 μg/L under optimized operation conditions as follows: Injection at 3 kV for 40 s prior to CE run at +15 kV in buffer system developed and with 0.4 mM tetrabutyl ammonium bromide added to rain sample as terminating ion. Leading and terminating ion effect, buffer additive, and operation conditions on performance of ITP procedure were investigated. Procedure developed was applied for trace metals' determination in rain water collected in Hong Kong. It provides fast, efficient, and economic method determining transition metals in rain sample down to sub-μg/L level, reducing sample pretreatment time and eliminating off-column preconcentration steps often leading to contamination problems for transition metals determination at μg/L level. © 2000 John Wiley & Sons, Inc. J Micro Sep 12: 337–344, 2000
毛细管电泳在雨水中痕量离子分析中的应用
为解决电动注射过程中过渡金属的迁移问题,提出了一种用于电动注射过程中过渡金属预富集和聚焦的瞬态等速电泳(ITP)方法。以盐酸羟胺30 mM、1,10-菲罗啉0.1 mM、甲醇1%、氯化铵15 mM、尿素0.08 M为缓冲体系,pH=3.7,对雨水中痕量金属进行亚μg/L浓度的预富集。在优化的操作条件下,Cd2+、Zn2+、Cu2+、Co2+、Fe2+(总Fe以Fe2+计)的工作范围为0.5 ~ 80 μg/L,重复性小于7%,检出限为0.1 ~ 0.5 μg/L,优化的操作条件为:在开发的缓冲系统中,在+15 kV电压下进行CE前,在3 kV电压下注入40 s,在雨样中加入0.4 mM的四丁基溴化铵作为终止离子。考察了起始和终止离子效应、缓冲剂添加剂和操作条件对ITP工艺性能的影响。所制订的方法已应用于香港雨水中痕量金属的测定。为亚μg/L水平的雨样中过渡金属的测定提供了快速、高效、经济的方法,减少了样品前处理时间,消除了常导致污染的柱外预富集步骤,可用于μg/L水平的过渡金属测定。©2000 John Wiley &[J] .中国科技大学学报(自然科学版),2000
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