土壤中铁对砷的便携式X射线荧光光谱仪分析基体效应研究与校正  

Study on matrix effect of iron in soil on arsenic by portable X-ray fluorescence spectrometer and its correction

作　　者：唐晓勇 倪晓芳 商照聪 周庆云 张苏伟[5] 刘亮 TANG Xiaoyong;NI Xiaofang;SHANG Zhaocong;ZHOU Qingyun;ZHANG Suwei;LIU Liang(Shanghai Research Institute of Chemical Industry Co.,LTD.,Shanghai 200062,China;Quality Control and Technology Assessment Laboratory of Industrial(Soil Remediation)Product,Shanghai 200062,China;Shanghai Research Institute of Chemical Industry Environmental Engineering Co.,LTD.,Shanghai 200062,China;Shanghai TECH Chemical Industry Testing CO.,LTD.,Shanghai 200062,China;Jiangsu Skyray Instrument Co.,LTD.,Kunshan 215316,China;Shanghai YuanHao Testing Technology Co.,Ltd.,Shanghai 201600,China)

机构地区：[1]上海化工研究院有限公司,上海200062 [2]工业(土壤污染修复)产品质量控制与技术评价实验室,上海200062 [3]上海化工院环境工程有限公司,上海200062 [4]上海化工院检测有限公司,上海200062 [5]江苏天瑞仪器股份有限公司,江苏昆山215316 [6]上海源豪检测技术有限公司,上海201600

出　　处：《冶金分析》2021年第1期69-74,共6页Metallurgical Analysis

基　　金：国家重点研发计划(2020YFC1807304)。

摘　　要：便携式X射线荧光光谱仪(PXRF)能够以低成本快速检测土壤中类重金属砷。但是,土壤中铁元素含量复杂多变,严重影响了PXRF对类重金属元素砷的检测准确度。实验选择硅藻土为基体,人工添加砷、铁元素探究砷元素的特征荧光强度与本身含量和土壤中铁元素含量之间的关系,并根据研究结果设立校正公式,该公式包含铁元素影响扣除项、砷-铁元素相互影响扣除项和常数修正项,以提高土壤中砷元素的PXRF分析准确度。研究结果表明,当土壤中铁元素含量固定不变时,砷元素的荧光强度与其本身含量呈线性变化,相关系数均在0.9950以上;当砷元素含量不变时,砷元素的荧光强度会随着铁元素含量的增大而减小。采用设立的经验校正公式,以电感耦合等离子体原子发射光谱法(ICP-OES)分析值作为参照值,对5个不同类型土壤样品进行检测,结果显示砷元素测定结果的相对标准偏差(RSD)为1.15%~11.92%,相对误差(RE)为5.32%~11.18%,相对于一维线性回归的相对误差(RE)13.18%~72.53%,实验方法提高了PXRF对土壤中砷元素的检测准确度。Portable X-ray fluorescence spectrometer(PXRF)enables the low-cost and rapid detection of metalloid arsenic.However,the iron content in soil is complex and changeable,which seriously affects the detection accuracy of arsenic by PXRF.Diatomite was selected as the matrix.The elements of arsenic and iron were added artificially to explore the relationship between the characteristic fluorescence intensity of arsenic and its own content and iron content in the soil.According to the research results,a correction formula was established,which included the deduction item of iron influence,the deduction item of arseniciron interaction,and the constant correction item,so as to improve the analysis accuracy of arsenic in soil by PXRF.The results showed that the fluorescence intensity of arsenic was linear to its content when the iron content in the soil was fixed,and the correlation coefficients were above 0.9950.When the content of iron was constant,the fluorescence intensity of arsenic decreased with the increase of iron content.Five different types of soil samples were detected according to the established empirical correction formula.The analysis values of inductively coupled plasma atomic emission spectrometry(ICP-OES)were used as reference.The results showed that the relative standard deviations(RSDs)of determination results were between 1.15%and 11.92%.The relative errors(REs)were between 5.32%and 11.18%,the relative errors(REs)relative to one-dimensional linear regression were between 13.18%and 72.53%.The proposed method improved the detection accuracy of arsenic in soil by PXRF.

关 键 词：便携式X射线荧光光谱仪(PXRF) 土壤 砷 铁 基体效应 

分 类 号：O657.34[理学—分析化学]