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有机悬浮固化分散液-液微萃取测定水样中痕量铅

Dispersive liquid-liquid microextraction based on solidification of floating organic drop for the determination of trace lead in water samples

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【作者】 杨丽李超王雨堃张婧雯李敬慈马晶军

【Author】 YANG Li,LI Chao,WANG Yu-kun,ZHANG Jing-wen,LI Jing-ci,MA Jing-jun*(Key Laboratory of Bioinorganic Chemistry,College of Science,Agricultural University of Hebei,Baoding 071001,China)

【机构】 河北农业大学理学院河北省生物无机化学重点实验室

【摘要】 建立了以二乙基二硫代氨基甲酸钠为配位剂,十二醇为萃取剂,乙醇为分散剂的悬浮固化分散液-液微萃取—火焰原子吸收光谱法测定水样中痕量铅的方法。详细探讨了影响萃取效率的因素。优化条件为:二乙基二硫代氨基甲酸钠的用量为10-6 mol,十二醇体积为90.00μL,乙醇体积为1.00 mL,pH为7.00。在最佳条件下,铅的检出限为1.12μg/L,富集倍率为16.00,线性范围5.00~600.00μg/L,对含有20.00μg/L和600.00μg/L Pb的标准溶液平行萃取测定11次,测定结果的RSD分别为3.73%和2.62%。本方法应用于自来水、河水及海水中痕量铅的分析,加标回收率为90.10%~100.70%。

【Abstract】 The process of dispersive liquid-liquid microextraction based on solidification of floating organic droplet(DLLME-SFO)was successfully applied for the extraction and preconcentration of trace lead from water samples,prior to flame atomic absorption spectrometry(FAAS).In the proposed approach,diethyldithiocarbamate was used as a chelating agent,1-dodecanol as extraction solvent and ethanol as dispersive solvent.Under the optimized experimental conditions(diethyldithiocarbamate amount:10-6 mol;1-dodecanol solvent volume:90.00 μL;ethanol volume:1.00 mL;pH:7.00),an enrichment factor of 16.00 was obtained from only 5.00 mL of water sample.The calibration graph was linear in the range of 5.00~600.00 μg/L with a detection limit of 1.12 μg/L.The relative standard deviation(RSD)for eleven replicate measurements of 20.00 and 600.00 μg/L of lead were 3.73 and 2.62%.The method was applied to the analysis of tap,river,and sea water samples and good spiked recoveries over the range of 90.10~100.70%were obtained.

【基金】 河北省教育厅科研发展基金(2007121)资助项目;河北农业大学非生命学科资助项目新兴学科科研发展基金资助项目
  • 【文献出处】 化学研究与应用 ,Chemical Research and Application , 编辑部邮箱 ,2012年01期
  • 【分类号】O657.31
  • 【被引频次】6
  • 【下载频次】237
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