摘要
用于测定土壤、沉积物样品中无机元素的波长色散X射线荧光光谱法(WD-XRF)基体效应校正经验模型中,通常需要Mg、Al、Si、Ti、K、Fe、Ca等常量元素测定结果。针对能量色散X射线荧光光谱法(ED-XRF)应用方案,如果能将参与基体效应校正的元素个数压缩,不考虑Mg、Al、Si等轻元素,其分析成本和时间将明显得到优化。实验探讨了简化基体效应校正模型的可能性。基于康普顿散射和简化的基体效应校正模型,建立了土壤、沉积物样品中As、Cr、Cu、Ni、Pb、Zn、Mn、V等重金属元素的ED-XRF测定方法。用5个土壤、9个沉积物标样认定值和3个土壤考核样品WD-XRF测定结果为基准,以HJ 780—2015质控要求为依据,评估了方法的准确度和精密度。目标元素分析结果准确度合格率94.1%~100%,精密度合格率100%。基于经典的背景计数法和重复测定法评估了方法检出限。各项实验结果表明,ED-XRF可用于土壤重金属污染状况详查检测实验室质控工作。
During the determination of inorganic elements in soil and sediment samples by wavelength dispersive X-ray fluorescence spectrometry(WD-XRF),the determination results of macro elements such as Mg,Al,Si,Ti,K,Fe and Ca are usually required in empirical model for the correction of matrix effect.According to the application scheme of energy dispersive X-ray fluorescence spectrometry(ED-XRF),if the number of elements which participates in the correction of matrix effect can be reduced,the analysis cost and time can be significantly optimized when the light elements such as Mg,Al and Si are not considered.The feasibility of simplified model for correction of matrix effect was discussed.Based on Compton scattering and simplified model for correction of matrix effect,the determination method of heavy metal elements in soil and sediment samples(As,Cr,Cu,Ni,Pb,Zn,Mn and V)by ED-XRF was established.The accuracy and precision of method was evaluated according to the quality control requirements in HJ 780-2015.The certified values of five soil samples and nine sediment samples and the determination results of three soil examining samples by wavelength dispersion X-ray fluorescence spectrometry(WD-XRF)were used as the benchmarks.The pass rate of accuracy for analysis results of target elements were between 94.1%and 100%,and the pass rate of precision was 100%.The detection limit was evaluated based on classical background counting method and replicate experiments method.The experimental results indicated that ED-XRF could be used for the laboratory quality control of heavy metal pollution in soil samples.
作者
殷惠民
杜祯宇
李玉武
李国会
YIN Hui-min;DU Zhen-yu;LI Yu-wu;LI Guo-hui(National Research Center for Environmental Analysis and Measurements,Beijing 100029,China;Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences,Langfang 065000,China)
出处
《冶金分析》
CAS
CSCD
北大核心
2018年第4期1-10,共10页
Metallurgical Analysis
基金
科技部国家重大科学仪器设备开发专项(No.2011YQ170065)
关键词
土壤
沉积物
重金属
能量色散X射线荧光光谱
测试结果评估
基体效应校正模型
soil
sediment
heavy metal
energy dispersive X-ray fluorescence spectrometer
evaluation of test result
matrix effect correction model
