压片制样-波长色散X射线荧光光谱法测定土壤和沉积物中主、次及微量元素  

Determination of Major,Minor and Micro Elements in Soils and Sediments by Wavelength Dispersive X-ray Fluorescence Spectrometry with Pressed Powder Pellet

作　　者：钟坚海 叶华欣 李泳涛 郑伟强[3] 赵振[3] 郑瑞娟[4] 董清木 张瑞振 冯均利 ZHONG Jianhai;YE Huaxin;LI Yongtao;ZHENG Weiqiang;ZHAO Zhen;ZHENG Ruijuan;DONG Qingmu;ZHANG Ruizhen;FENG Junli(Technology Center,Xiamen Customs,Xiamen,Fujian 361026,China;The Testing and Technology Center for Industrial Products,Shenzhen Customs,Shenzhen,Guangdong 518067,China;Fujian Province 121 Geological Brigade,Longyan,Fujian 364000,China;College of Chemistry and Materials Science,Longyan University,Longyan,Fujian 364000,China)

机构地区：[1]厦门海关技术中心,福建厦门361026 [2]深圳海关工业品检测技术中心,广东深圳518067 [3]福建省121地质大队,福建龙岩364000 [4]龙岩学院化学与材料学院,福建龙岩364000

出　　处：《中国无机分析化学》2022年第6期34-39,共6页Chinese Journal of Inorganic Analytical Chemistry

基　　金：福建省科技计划项目(2021I0032);厦门海关科研项目(2020XK14)。

摘　　要：针对土壤和沉积物中主、次及微量元素的准确、高效检测要求,基于压片制样-波长色散X射线荧光光谱测定技术,采用42种土壤和沉积物标准物质作为校准标样,建立了土壤和沉积物中22种元素成分的同时测定方法。重点研究了压片制样技术存在的矿物效应和粒度效应,考察了测定次数对氯含量检测结果的影响,优化了各元素成分的测试条件,探讨了基体效应及谱线重叠干扰校正等问题。采用软件提供的多元线性回归分析模型建立了各元素分析的校准曲线,基于3倍背景信号波动的标准偏差计算出各元素的检出限范围为0.3~433.4 mg/kg。准确度实验结果表明,土壤(GBW07403a、GBW07450)和水系沉积物(GBW07384)的测试结果与标示值基本一致。针对三个不同含量水平土壤样品的精密度实验(RSD,n=12)结果表明,各元素测定结果相对标准偏差分别在0.13%~9.1%、0~9.3%和0.18%~8.3%。因此,进一步明确了土壤和沉积物X射线荧光光谱测定的关键条件,方法的检出限、准确度及重复性等满足日常分析检测要求,对实验室土壤检测工作具有指导意义。In order to meet the requirements of accurate and efficient detection of primary,secondary and trace elements in soil and sediment,a simultaneous determination method of 22 elements in soil and sediment was developed based on pressed powder pellet-wavelength dispersive X-ray fluorescence spectrometry,using 42 soil and sediment certified reference materials as calibration standards.This paper focuses on the mineral effect and particle size effect of tablet sample preparation technology,investigates the influence of determination times on the detection results of chlorine content,optimizes the test conditions of each element composition,and discusses the matrix correction and spectral line overlap interference correction.The calibration curve of each element was established by using the multiple linear regression analysis model provided by the instrument software.Based on the standard deviation of three times the background signal fluctuation,the detection limit range of each element was calculated to be 0.3—433.4 mg/kg.The accuracy test results showed that the test results of soil(GBW07403a and GBW07450)and stream sediment(GBW07384)were basically consistent with the certified values.The precision test(RSD,n=12)for three soil samples with different content levels showed that the relative standard deviations of each element were 0.13%—9.1%,0—9.3%and 0.18%—8.3%,respectively.Therefore,the key conditions for the determination of soil and sediment by X-ray fluorescence spectrometry were further clarified in this study.The detection limit,accuracy and repeatability of the method met the requirements of daily analysis and detection well,which has guiding significance for laboratory soil testing.

关 键 词：粉末压片制样 X射线荧光光谱法(XRF) 土壤 沉积物 微量元素 

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