离子交换树脂-固相萃取富集-电感耦合等离子体光谱法测定水中重金属元素  

Preconcentration and Determination of Heavy Metals in Water Samples by Ion Exchange Resin Solid Phase Extraction with Inductively Coupled Plasma Atomic Emission Spectrometry

作　　者：刘冰冰[1] 刘佳 张辰凌[1] 韩梅[1] 贾娜[1] 刘圣华[1] LIU Bing-bing;LIU Jia;ZHANG Chen-ling;HAN Mei;JIA Na;LIU Sheng-hua(Institute of Hydrogeology and Environmental Geology,Chinese Academy of Geologica l Sciences,Zhengding 050803,China)

机构地区：[1]中国地质科学院水文地质环境地质研究所,河北正定050803

出　　处：《光谱学与光谱分析》2018年第12期3917-3922,共6页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金项目(41703020);中国地质科学院基本科研业务费项目(YK201504;YK201704和YYWF201622)资助

摘　　要：建立了离子交换树脂-固相萃取富集-电感耦合等离子体光谱(ICP-AES)联用测定水中的重金属元素Zn,Mn,Cu,Co,Ni,Cd,Pb的方法。实验采用Dowex50WX8强酸型阳离子交换树脂,通过优化富集分离条件和排除共存离子的干扰,最终确定最佳的样品pH,样品流速,洗脱液种类和浓度,样品体积分别为3. 0～4. 0,3. 0 m L·min^(-1),3. 0 mol·L^(-1) HNO_3,200 mL。方法中各元素的检出限和定量限范围分别为0. 09～0. 45和0. 31～1. 50μg·L^(-1),加标回收率和相对标准偏差RSD(n=6)分别为95. 3%～104. 2%和1. 25%～4. 12%。采用该方法测定不同地区的样品,并与直接采用ICP-MS法进行对比,其测定结果基本吻合。实验表明该方法的检出限,定量限可以满足水中重金属元素Zn,Mn,Cu,Co,Ni,Cd,Pb的检测要求,准确性和精密度好,结果可靠,适用于测定水中Zn,Mn,Cu,Co,Ni,Cd,Pb。This paper established the method for preconcentration and determination of heav y metals such as Zn,Cu,Co,Mn,Ni Cd,Pb in water samples by solid phase extraction(SPE)with inductively coupled plasma atomic emission spectrometry(ICP-AES).In this experiment,Dowex 50WX8 strong acid cation exchange resin was used and by optimizing the conditions of preconcentration and eliminating the in terference of coexisting ions,the optimum sample pH,sample flow rate,eluent type and concentration,sample volumes were determined with 3.0~4.0,3.0 mL·min^-1,3.0 mol·L^-1 HNO 3 and 200 mL,respectively.For this me thod,the detection limit and quantitation limit of each element were 0.09~0.45 and 0.31~1.50μg·L^-1,respectively.The recoveries and relative standard deviations RSD(n=6)were 95.3%~104.2%and 1.25%~4.12%.The water samples of different parts were determined by this method and compared wit h the direct determination by ICP-MS,the results of the both methods were basi cally identical.All of these indicated that the detection limit and quantitativ e limit in this method could meet the requirements for determination of heavy metals in water samples.The accuracy and precision of the method were high which w ere suitable for the determination of Zn,Mn,Cu,Co,Ni,Cd,Pb in water samples.

关 键 词：离子交换树脂 固相萃取 ICP-AES 富集 重金属元素 

分 类 号：O657.3[理学—分析化学]