1. Institute for Environmental Reference Materials of Ministry of Environmental Protection, Beijing 100029, China; 2. State Environmental Protection Key Laboratory of Environmental Pollutant Metrology and Reference Materials, Beijing 100029, China
Abstract：Heavy metals are important indexes for the environmental monitoring of soil and stream sediment. Since the matrix of soil and stream sediment samples is complex, the reasonable optimization of determination conditions is very import to improve the accuracy of analysis method when the contents of heavy metals are determined by X-ray fluorescence spectrometry (XRF). The analysis method of 13 heavy metal elements (including As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Sb, Sn, V and Zn) in environmental samples such as soil and stream sediment by XRF was established after sample preparation by powder pressed pellet. Total 31 certified reference materials of primary soil, stream sediment and rock were employed to fit the calibration curve. The determination conditions of elements were discussed. The spectral overlapping interference and matrix effect correction were also investigated. The detailed measures to improve the analysis accuracy of trace heavy metals (including As, Cd, Co, Mo, Ni, Sb and Sn) were proposed. The precision of analysis method was investigated using two soil samples with different contents of heavy metals. For the elements with content higher than 10mg/kg, the relative standard deviations (RSD, n=12, within one day) of measurements results were 0.47%-5.3% (within one day) and 0.83%-6.3% (in days), respectively. The detection limits ranged from 0.39mg/kg to 5.1mg/kg. Four certified reference materials of soil and stream sediment were used to evaluate the trueness of method. The found results of heavy metals were consistent with the certified values. The proposed method could meet the technical requirements of environmental monitoring of soil and stream sediment in detection limit, precision and trueness. Compared with the standard methods, the analysis of three heavy metals (Cd, Sb and Sn) was added in the proposed method, which broadened the analysis range of trace elements.
陆安军,苏梦晓.波长色散X射线荧光光谱法测定中低品位铝土矿和高硫铝土矿中主次组分[J].冶金分析,2019,39(4):53-59.LU An-jun,SU Meng-xiao.Determination of major and minor components in medium-low grade bauxite and high-sulfur bauxite by wavelength dispersive X-ray fluorescence spectrometry[J].Metallurgical Analysis,2019,39(4):53-59.
[2]
周伟,曾梦,王健,等.熔融制样-X射线荧光光谱法测定稀土矿石中的主量元素和稀土元素[J].岩矿测试,2018,37(3):298-305.ZHOU Wei,ZENG Meng,WANG Jian,et al.Determination of major and rare earth elements in rare earth ores by X-ray fluorescence spectrometry with fusion sample preparation[J].Rock and Mineral Analysis,2018,37(3):298-305.
[3]
马景治,刘恒杰,王峰.熔融制样-X射线荧光光谱法测定地质样品中的主次成分[J].分析试验室,2016,35(11):1348-1352.MA Jing-zhi,LIU Heng-jie,WANG Feng.Simultaneous determination of major and minor components in geological sample by XRF with fusion sample preparation[J].Chinese Journal of Analysis Laboratory,2016,35(11):1348-1352.
[4]
刘玉纯,林庆文,马玲,等.粉末压片制样-X射线荧光光谱法分析地球化学调查样品测量条件的优化[J].岩矿测试,2018,37(6):671-677.LIU Yu-chun,LIN Qing-wen,MA Ling,et al.Optimization of measurement conditions for geochemical survey sample analysis by X-ray fluorescence spectrometry with pressed powder pellet sample preparation[J].Rock and Mineral Analysis,2018,37(6):671-677.
[5]
陈素兰,胡冠九,周春宏,等.X射线荧光光谱法测定土壤及底泥中多种元素[J].环境监测管理与技术,2006,18(4):15-18.CHEN Su-lan,HU Guan-jiu,ZHOU Chun-hong,et al.To measure variety elements in the soil and mud by X-ray fluorescence spectrometry[J].The Administration and Technique of Environmental Monitoring,2006,18(4):15-18.
[6]
陈静,高志军,陈冲科,等.X射线荧光光谱法分析地质样品的应用技巧[J].岩矿测试,2015,34(1):91-98.CHEN Jing,GAO Zhi-jun,CHEN Chong-ke,et al.Application skills on determination of geological sample by X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2015,34(1):91-98.
[7]
王建其,柳小明.X射线荧光光谱法分析不同类型岩石中10种主量元素的测试能力验证[J].岩矿测试,2016,35(2):145-151.WANG Jian-qi,LIU Xiao-ming.The proficiency testing of XRF method for measuring 10 major elements in different type rocks[J].Rock and Mineral Analysis,2016,35(2):145-151.
[8]
于波,严志远,杨乐山,等.X射线荧光光谱法测定土壤和水系沉积物中碳和氮等36个主次痕量元素[J].岩矿测试,2006,25(1):74-78.YU Bo,YAN Zhi-yuan,YANG Le-shan,et al.Determination of 36 major,minor and trace elements in soil and stream sediment samples by X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2006,25(1):74-78.
[9]
殷惠民,杜祯宇,任立军,等.波长色散X射线荧光光谱谱线重叠和基体效应校正系数有效性判断及在土壤、沉积物重金属测定中的应用[J].冶金分析,2018,38(7):1-11.YIN Hui-min,DU Zhen-yu,REN Li-jun,et al.Coefficient effectiveness judgment of overlapping line and matrix effect correction in wavelength dispersive X-ray fluorescence spectrometry and its application in determination of heavy metal elements in soil and sediment samples[J].Metallurgical Analysis,2018,38(7):1-11.
[10]
孙晓飞,文孟喜,杨丹丹.康普顿散射线结合经验系数法校正在X射线荧光光谱测定石灰石和白云石中的应用[J].冶金分析,2016,36(1):11-17.SUN Xiao-fei,WEN Meng-xi,YANG Dan-dan.Application of compton scatter and empirical coefficient correction in X-ray fluorescence spectrometric determination of limestone and dolomite[J].Metallurgical Analysis,2016,36(1):11-17.
