浮动液滴固化分散液相微萃取-火焰原子吸收光谱法测定环境样品中的镉  

Determination of trace cadmium by dispersive liquid-liquid microextraction based on solidification of floating organic drop combined with flame atomic absorption spectrometry

作　　者：秦九红 杨君[2] 向国强[2] 

机构地区：[1]河南省有色金属地质勘查总院,河南郑州450052 [2]河南工业大学化学化工学院,河南郑州450002

出　　处：《化学研究》2011年第3期74-78,共5页Chemical Research

基　　金：河南工业大学校科研基金项目(09XJC003)

摘　　要：建立了以十一醇为萃取剂,吡咯烷二硫代甲酸铵（APDC）为螯合剂的浮动液滴固化分散液相微萃取-火焰原子吸收光谱法（DLLME-SFO-FAAS）测定环境样品中痕量镉的分析方法;优化了分散剂、萃取剂的类型和体积,考察了溶液pH值、APDC浓度以及萃取温度和时间对萃取效率的影响.结果表明,该法检出限（3σ）为0.14μg/L,相对标准偏差RSD为2.5%（c=10.0μg/L,n=7）,线性范围为2.0~50.0μg/L,富集倍数18.将其用于水中镉标准物质（GBW（E）080531）和实际环境水样中痕量镉的测定,测定值与标准值吻合良好,实际样品的加标回收率为94%~103%.A new method was established to determine trace cadmium in environmental samples by combining dispersive liquid-liquid microextraction based on solidification of floating organic drop（DLLME-SFO） with flame atomic absorption spectrometry（FAAS）.The main parameters affecting the performance of DLLME-SFO,such as type and volume of extraction solvent,pH,concentration of chelating agent,extraction temperature and time,were investigated.It was found that,under the optimized experimental conditions,the method had a detection limit（3σ） of 0.14 μg/L,linear range of 2.0-50.0 μg/L,relative standard deviation（RSD） of 2.5%（c = 10.0 μg/L,n = 7）,and enrichment factor of 18.The method was successfully applied to determine trace cadmium in the certified reference water sample（GBW（E） 080531） and various to-be-tested water samples.The analytical result for the certified reference water sample was in good agreement with the certified value,and the recoveries for the spiked water samples were in a range of 94%-103%.

关 键 词：分散液相微萃取 浮动液滴固化 原子吸收光谱 环境样品 镉 测定 

分 类 号：O657.3[理学—分析化学]