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

作　　者：杨丽[1] 李超[1] 王雨堃[1] 张婧雯[1] 李敬慈[1] 马晶军[1] 

机构地区：[1]河北农业大学理学院,河北省生物无机化学重点实验室,河北保定071001

出　　处：《化学研究与应用》2012年第1期21-25,共5页Chemical Research and Application

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

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%。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-dedecanol as extraction solvent and ethanol as dispersive solvent. Under the optimized experimental conditions（diethyldithiocarbamate amount： 10-6 mol;l- dodecanol solvent volume ：90. 00 μL;ethanol volume：l. 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. （30 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.

关 键 词：悬浮固化 分散液-液微萃取 火焰原子吸收光谱法 铅 

分 类 号：O657.3[理学—分析化学]