电镀污泥成分X荧光检测水分影响机制及校正方法研究  

The Mechanism of Moisture Influence and Correction of Electroplating Sludges Testing With EDXRF

作　　者：滕婧 石垚 李会泉[2,3] 刘作华 李志宏[2] 何明星 张晨牧 TENG Jing;SHI Yao;LI Hui-quan;LIU Zuo-hua;LI Zhi-hong;HE Ming-xing;ZHANG Chen-mu(School of Chemistry and Chemical Engineering,Chongqing University,Chongqing 401331,China;CAS Key Laboratory of Green Process and Engineering,Innovation Academy for Green Manufacture,Chinese Academy of Sciences,National Engineering Research Center of Green Recycling for Strategic Metal Resources,Institute of Process Engineering,Chinese Academy of Sciences,Beijing 100190,China;School of Chemistry and Chemical Engineering,University of Chinese Academy of Sciences,Beijing 100049,China;School of Information and Electrical Engineering,Hebei University of Engineering,Handan 056038,China)

机构地区：[1]重庆大学化学化工学院,重庆401331 [2]中国科学院过程工程研究所,中国科学院绿色过程与工程重点实验室,中国科学院绿色过程制造创新研究院,战略金属资源绿色循环利用国家工程研究中心,北京100190 [3]中国科学院大学化学工程学院,北京100049 [4]河北工程大学信息与电气工程学院,河北邯郸056038

出　　处：《光谱学与光谱分析》2024年第2期419-425,共7页Spectroscopy and Spectral Analysis

基　　金：中国科学院美丽中国生态文明建设科技工程专项(XDA23030303);国家重点研发计划项目(2018YFC1903300)资助。

摘　　要：电镀污泥是金属加工、电子元器件制造等行业在废水处理过程中所产生含重金属危险废物。我国每年产生大量电镀污泥约1000万吨,因含有Zn、Cu、Fe、Ni、Cr等多种有价金属元素其资源化利用潜力巨大,同时大量污泥处置不当也会危害人体健康和污染环境。传统化学分析测试过程复杂周期长,不利于电镀污泥实时污染防控。能量色散X射线荧光(EDXRF)光谱法分析快速简便、费用低廉、可实现原位检测,然而电镀污泥样品含水率高、成分含量不稳定,影响测试结果的及时性和准确度,导致关键元素的资源转化效率难以保证、环境污染管控难度高。因此需要分析X荧光检测水分影响机制并探究水分校正方法,以提高EDXRF测试结果准确度。以不同含水率电镀污泥为对象,研究了水分对电镀污泥EDXRF测试过程中光谱本底、散射峰、目标元素特征峰的影响机制,通过目标元素特征峰与瑞利散射峰强度的比值、样品含水率ω0 wt%和目标元素含量Ci%建立水分校正模型,探究了Ca、Cr、Fe、Ni、Cu、Zn目标元素的水分校正方程中的实验修正因子。结果表明,水分抬高了光谱本底改变谱峰轮廓,对低能段、计数小的谱峰测试结果影响较大。含水率越高,散射峰净强度越大,瑞利散射线更能准确描述散射峰净强度和含水率的关系,目标元素特征峰与瑞利散射峰强度比值与含水率、目标元素含量能够准确符合线性关系。水分校正模型对Cr、Fe、Ni、Cu、Zn五种重金属校正结果准确度较高,校正值与基准值相关系数R2均大于0.95,RMSE均小于0.05,对Ca元素校正准确度较低R2为0.93,RMSE为1.046需增加相关校正因子进一步优化。该研究有望应用于再生铜行业电镀污泥处置现场测量的水分校正方法中,在提高电镀污泥资源利用效率的同时降低环境污染风险。Electroplating sludges are produced in wastewater treatment in metal processing,electronic component manufacturing and other industries with hazardous waste containing heavy metals.Many electroplating sludges about 10 million tons every year,have been produced in China.It contains various valuable metal elements such as Zn,Cu,Fe,Ni,Cr,its resource utilization potential is huge.The improper disposal of a large amount of sludges will also endanger human health and pollute the environment.The traditional chemical analysis testing process is complex,but energy-dispersive X-ray fluorescence(EDXRF)spectroscopy analysis is fast,simple,cost-effective,and can achieve in-situ detection.However,the high moisture content and unstable component content of electroplating sludge samples affect the accuracy of test results.It is a difficult to ensure the resource conversion efficiency of key elements and difficult to control environmental pollution.Therefore,it is necessary to analyze the mechanism of water influence in EDXRF detection and explore moisture correction methods to improve the accuracy of test results.The mechanism of the influence of moisture on the spectral background,scattering peak,and target element characteristic peak during the EDXRF testing process of electroplating sludge was studied.By the ratio of target element characteristic peak to Rayleigh scattering peak intensity,and the sample moisture contentω0(wt%)and target element content Ci%,a moisture correction model was established.The experimental correction factors in the moisture correction equation for Ca,Cr,Fe,Ni,Cu,Zn target elements were explored.The results show that the moisture correction model has high accuracy in correcting the five heavy metals Cr,Fe,Ni,Cu,and Zn,and the correlation coefficient R2 between the corrected value and the reference value is high,R2 are higher than 0.95,and RMSE are lesser than 0.05,indicating a low accuracy in correcting Ca elements R2 is 0.93.RMSE is 1.046 require further optimization by adding relevant correction

关 键 词：X射线荧光光谱 电镀污泥 水分影响 基体效应 散射校正 

分 类 号：O657.3[理学—分析化学]