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离子色谱-质谱联用技术测定污泥样品中的痕量高氯酸盐
  • 期刊名称:分析化学, 2007, 35(1):131-134
  • 时间:0
  • 分类:O614.33[理学—无机化学;理学—化学]
  • 作者机构:[1]中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室,北京100085
  • 相关基金:本文系国家自然科学基金(No.20475060,20577058)、国家重点基础研究计划(973项目)(No.2003CB415001)、中国科学院重要方向性项目(No.KZCX3-SW-432)
  • 相关项目:基于金属氧化物纳米颗粒的半胶束/吸附胶束行为研究及其在环境污染物固相萃取和固相微萃取中的应用
中文摘要:

建立了离子色谱-质谱联用技术测定活性污泥样品中高氯酸盐的分析方法。以高容量、强亲水性的IonPae AS20(2mm)阴离子交换柱为分析柱,EGC在线产生等浓度KOH为淋洗液,淋洗液经抑制成水后将样品带入质谱检测。ESI-MS-MS以多元反应监测模式监控100.8/84.9、98.8/66.9、100.8/68.9和98.8/82.9离子对。以98.8/82.9离子对的峰面积进行定量。该方法对高氯酸盐的检出限(S/N=3)为0.01μg/L,高氯酸盐在0.05—100μg/L浓度范围内具有良好的线性,线性相关系数r=0.9988。0.2μg/L的标准溶液重复进样9次,高氯酸盐峰面积的相对标准偏差(RSD)为2.3%。运用该方法测定采自不同地区的活性污泥样品中的高氯酸盐,并对样品加标回收,得回收率在88.5%-102.2%之间。

英文摘要:

A rapid method for the highly sensitive determination of perchlorate was set up by ion chromatography/electrospray ionization tandem mass spectrometry (IC/ESI-MS/MS) in the negative ESI and multiple reaction monitoring (MRM) mode. Using high capacity and hydroxide selective column IonPac AS20, perchlorate was separated by KOH eluent generated form EGC. The transition 100.8/84.9, 98.8/66.9 and 100.8/68.9 ion pairs were monitored for confirming the target analyte and 98.8/82.9 ion pair for quantifying. The detection limit of quantitation of the method ( S/N= 3 ) was as good as 0.01 g/L for perchlorate. A linear calibration was obtained over the range of 0.05 to 100 g/L with a correlation coefficient of 0. 9988. The relative standard deviation for nine successive injection of 0.2 μg/L perchlorate was 2.3%. The method was applied to the detection of perchlorate in sludge samples, which were obtained from different areas in China. The recoveries of spiked standard were 88.5% -102.2%.

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