多仪器协同-X射线荧光光谱法在区域地球化学调查分析中的应用评价
河北省地矿中心实验室, 河北 保定 071051 |
Evaluation in the Application of Multi-instrument Synergy X-ray Fluorescence Spectrometry in a Regional Geochemical Survey
Hebei Province Geological and Mineral Center Laboratory, Baoding 071051, China |
摘要：在区域地球化学调查样品多元素分析测试中，通常将XRF、ICP-OES、ICP-MS、AFS等仪器相互配套使用，但由于XRF测定20多个元素，与其他仪器测定速度并不同步，影响了项目的整体进度。本方法对配套方案进行了优化，调整了XRF部分测量元素的分析方法，即将基体校正和谱线重叠校正涉及Na2O、MgO、V的数据由ICP-OES法测量；Cu、Pb、Zn、Mn、Th的数据由ICP-MS法测量；As、Bi的数据由AFS法测量。优化后的XRF方法测量元素减少为16个：SiO2、Al2O3、CaO、TFe2O3、K2O、Ti、P、Sr、Ba、Zr、Nb、Y、Rb、Br、Ga、Cl。通过设计的XRF数据处理程序，实现了这些不同方法的测量数据共享，利用ICP-OES、ICP-MS、AFS等测量数据对XRF数据进行基体效应和谱线重叠干扰校正。本方法精密度（RSD，n=12）为0.55%~8.22%，准确度（△logC）为0.000~0.031，用国家标准物质及实际样品验证的结果满足区域地球化学调查样品分析测试质量规范要求。本方案减少了XRF直接测量元素的数量，提高了多种仪器协同的分析效率。
Evaluation in the Application of Multi-instrument Synergy X-ray Fluorescence Spectrometry in a Regional Geochemical Survey
ABSTRACT Multi-element analysis of a regional geochemical survey sample usually involves X-ray Fluorescence Spectrometry (XRF), Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES), Inductively Coupled Plasma-Mass Spectrometry (ICP-MS), Atomic Fluorescence Spectrometry (AFS) and other instruments. Because there are more than 20 elements determined by XRF, the detection speed of XRF is not synchronous with other instruments, which influences the overall progress of the project. The matching scheme is optimized, and the analysis method of XRF for part of the elements is adjusted in this study. The data of Na2O, MgO and V involved in matrix correction and spectral overlap correction are measured by ICP-OES. The data of Cu, Pb, Zn, Mn, and Th were measured by ICP-MS. As and Bi data were measured by AFS. The optimized XRF method reduces the number of elements to 16, namely SiO2, Al2O3, CaO, Fe2O3, K2O, Ti, P, Sr, Ba, Zr, Nb, Y, Rb, Br, Ga and Cl. Through the designed XRF data reduction program, the data sharing of different analysis methods is realized, and the influence of XRF data caused by matrix effects and spectral line overlap is corrected using the data from XRF, ICP-OES, ICP-MS and AFS. The precision of this method (RSD, n=12) is 0.55%-8.22%, and the accuracies (△logC) are 0-.0.031. The method is validated by determination of national standard reference materials and actual samples. The results meet the quality requirements for a regional geochemical survey. This scheme reduces the number of elements directly measured by XRF, and improves the analysis efficiency of various collaborative instruments. 
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