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无外接电源富集装置-手持式XRF现场分析水体中重金属 被引量:7

On-Site Analysis of Heavy Metals in Water with Handheld X-Ray Fluorescence and Pre-Concentration Device without External Power Supply
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摘要 水体中重金属污染越来越受到人们的关注与重视,急需开发高效低耗、利于推广的便携式的水质检测技术,帮助地质及环境领域的工作者现场获取实验数据,对污染区域及时做出准确的水体环境评价,有助于水体污染的预防与治理工作。采用无外接电源的富集装置,在pH 4的条件下以S-930螯合树脂捕集水体中的重金属,经抽滤制得均匀薄膜样,再使用手持式XRF现场分析水体中Mn,Fe,Ni,Cu,Zn和Pb等6种重金属元素。各元素标准曲线的相关性r>0.992,方法检出限为5.8~18.6μg·L-1,精确度基本控制在15%RSD以内。方法应用于我国东北某矿区周边采集的20余个地表/下水样品的现场分析,检测结果与实验室ICP-MS结果进行了对比:两种方法的Pb,Ni和Cu一致性良好;Zn和Mn含量高的样品,ICP-MS结果高于现场XRF结果,可能因溶液中存在细微悬浮颗粒引起,但总体趋势一致;两种方法对水质类型的总体判断结果一致。本法使用的富集和测量装置体积小、重量轻、便于携带,不使用外接电源,可在12h内现场完成10个水体样品的采集、前处理操作、结果获取及数据处理等工作,避免实验室分析方法检测工作中存在的交通运输、测试周期长、测试成本高等问题,基本具备了在偏远地区现场分析水体中六种重金属元素、评定水质的能力,具有较好的推广应用前景。 Currently,increasing importance has been attached to heavy metal pollution of water environment.In order to help geologist and environmentalist to obtain on-site experimental data,there is an urgent need to develop portable analysis techniques of water quality,which can be used to give an timely and accurate assessment of water quality of the contaminated area with low cost and to monitor water environment conveniently in daily preventing and controlling work of water pollution.Based on adsorption with Purolite S930 chelating resin at pH 4and thin-film sample preparation technique,a rapid and simple on-site-oriented analysis method of heavy metal ions,namely Mn,Fe,Ni,Cu,Zn and Pb in aqueous solutions,was developed utilizing a handheld energy-dispersive X-ray fluorescence in this paper.The correlation coefficients of the calibration curves were greater than0.992 for all six metal ions,the lower limits of detection were between 5.8and 18.6μg·L-1.Precision tests carried out on multi-element mixed solutions showed that the relative standard deviations(RSD,n=10)were better than 15%.The method has been used on-site to analysis 21 water samples collected from different river or well sites near a mining area northeast China.Out of the five underground water samples,one was found contaminated by Cu and Zn(ClassⅢ),one by Zn and Fe(ClassⅡ),and one by Fe(in between ClassⅡtoⅢ).Surface water samples showed better qualities.But two out of the sixteen were found to be contaminated by Mn heavily(ClassⅣ).Laboratory ICPMS was used to analyze the same samples.The results for Cu,Ni and Pb were coincident with the on-site data in general.But for Zn and Mn with higher concentrations,on-site data were lower than that by ICPMS.The reason for that might be the inclusion of the fine suspending particles in the samples by ICPMS.We conclude that the on-site data were effective.With the described method,an overall data acquisition time,including sampling,processing and measuring,can be within 12 hours for a bat
作者 焦距 詹秀春 翟磊 樊兴涛 温宏利 袁继海 刘晓 郭澍 JIAO Ju ZHAN Xiu-chun ZHAI Lei FAN Xing-tao WEN Hong-li YUAN Ji-hai LIU Xiao GUO Shu(National Research Center for Geoanalysis, Beijing 100037, China Faculty of Material Science and Chemistry, China University of Geosciences (Wuhan), Wuhan 430074, China)
出处 《光谱学与光谱分析》 SCIE EI CAS CSCD 北大核心 2017年第1期267-272,共6页 Spectroscopy and Spectral Analysis
基金 国土资源公益性行业科研专项经费项目(201311013) 中国地质大调查项目(12120113091000)资助
关键词 手持式XRF 无外接电源 化学富集 薄膜法 现场分析 水体样品 重金属 Handheld XRF Without external power Chemical pre-concentration Thin-layer sample On-site analysis Water sample Heavy metal
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