预富集单波长激发能量色散X射线荧光光谱法现场测定地表水中10种重金属  

On-site Determination of 10 Heavy Metals in Surface Water by Pre-enriched Single-wavelength Excitation Energy Dispersive X-ray Fluorescence Spectrometry

作　　者：杏艳 杨震 窦蓓蕾 郭峰 陈静 宋硙 张霖琳 XING Yan;YANG Zhen;DOU Beilei;GUO Feng;CHEN Jing;SONG Wei;ZHANG Linlin(Shaanxi Environmental Monitoring Center,Xi′an,Shaanxi 710054,China;Suzhou Jia Pu Technology Co.,Ltd.Suzhou,Jiangsu 215000,China;China National Environmental Monitoring Centre,Beijing 100012,China)

机构地区：[1]陕西省环境监测中心站,西安710054 [2]苏州佳谱科技有限公司,江苏苏州215000 [3]中国环境监测总站,北京100012

出　　处：《中国无机分析化学》2022年第4期18-27,共10页Chinese Journal of Inorganic Analytical Chemistry

基　　金：陕西省地方标准项目(SDBXM 120-2019);湖湘高层次人才聚集工程-创新团队项目(2021RC5030);国家环境保护重金属污染监测重点实验室基金项目(SKLMHM202202)。

摘　　要：为实现现场快速定量分析地表水中的多种重金属元素,建立了一种树脂预富集-单波长激发能量色散X射线荧光光谱法现场准确快速测定地表水中Cr(Ⅵ)、Mn、Fe、Co、Ni、Cu、Zn、As、Cd、Pb 10种元素的分析方法。通过对树脂预富集条件进行了优化,结果表明,最佳预富集条件为:树脂粒径38~75μm,水样体积30 mL,水样流速6 mL/min,样品pH值为5。Cr(Ⅵ)、Cu、Zn、As、Cd、Pb元素的检出限低于地表水环境质量标准GB 3838—2002中规定的限值要求,相对标准偏差为2.1%~10.4%,水样加标回收率为90.0%~114%。方法用于测定实际地表水样品,其测定结果与电感耦合等离子体质谱(ICP-MS)法测定结果基本一致。方法的检出限可以满足地表水中Cr(Ⅵ)、Mn、Fe、Co、Ni、Cu、Zn、As、Cd、Pb的检测要求,精密度和准确性较好。对地表水中无机元素分析方法的拓展进行了有益尝试和积累,并为后续相关标准制订提供有益参考。In order to fulfill the rapid quantitative analysis of multiple elements in surface water on site,in this work an analytical method for the accurate and rapid determination of Cr(VI),Mn,Fe,Co,Ni,Cu,Zn,As,Cd and Pb in surface water by single-wavelength excitation energy dispersive X-ray fluorescence with pre-enrichment resin has been developed.The pre-enrichment parameters of method were optimized and the results showed that the conditions were as follows:the particle size of exchange resin was 38—75μm,the volume of water samplewas 30 mL,the flow rate of water sample was 6 mL/min,the test should be done immediately after enrichment;the optimum pH of water sample was 5.The detection limits,precision and accuracy of the methodology were further investigated.The detection limits of Cr(VI),Cu,Zn,As,Cd and Pb were better than the limit requirements of surface water environmental quality standard GB 3838—2002,the relative standard deviation of precision was within the range of 2.1%—10.4%,the recoveries of sample were between 90.0%—114%.This method was used to determine the actual surface water samples,the results were basically consistent with ICP-MS method.This experiment showed that the detection limit of this method can meet the detection requirements of Cr(VI),Mn,Fe,Co,Ni,Cu,Zn,As,Cd and Pb in surface water,and there was good precision and accuracy.The work is a useful attempt and accumulation of methods for the analysis of inorganic elements in surface water,and provides useful reference for the subsequent development of relevant standards.

关 键 词：地表水 重金属 预富集 单波长激发能量色散X射线荧光 现场 快速测定 

分 类 号：O657.34[理学—分析化学] TH744.15[理学—化学]