高压制样X射线荧光光谱法测定铝土矿中的16种主次痕量元素  

High-pressure sample preparation X-ray fluorescence spectrometry for the determination of 16 major,minor,and trace elements in bauxite

作　　者：付利龙 谭靖 刘杰[1] 曹洁[1] 钟奕昕 李华兴 陈美华 FU Li-long;TAN Jing;LIU Jie;CAO Jie;ZHONG Yi-xin;LI Hua-xing;CHEN Mei-hua(Changsha General Survey of Natural Resources Center,China Geological Survey,Changsha 410600,China)

机构地区：[1]中国地质调查局长沙自然资源综合调查中心,湖南长沙410600

出　　处：《化学研究与应用》2025年第4期881-886,共6页Chemical Research and Application

摘　　要：高压制样法波长色散X射线荧光光谱测定了铝土矿中的三氧化二铝、二氧化硅、三氧化二铁、二氧化钛、氧化钾、氧化钙、氧化镁、五氧化二磷、钒、铬、铅、铜、锶、锆、镓和锌16种主次痕量元素的含量。扫面电镜对样片表面形态分析显示,高压制样可以制备出更致密、平整光滑的样片,从而减小了样片表面不平整度引起的测定误差,高压制备的试样片较常规压力元素的灵敏度显著地提高、检出限明显降低、分析结果更接近标准值、精密度和样品制备的重现性均有较大提高。以铑靶康普顿散射线做内标校正痕量重元素(Z>26)铅、铜、锶、锆、镓和锌的基体效应,其余元素采用经验系数法校正谱线重叠及基体效应。各组分校准曲线的相关系数R^(2)≥0.98。经未参加回归的样品验证,样品的分析结果与化学值基本吻合,可满足快速分析的要求。The High-pressure sample preparation method combined with wavelength-dispersive X-ray fluorescence spectrometry has been used to determine the contents of 16 major,minor,and trace elements in bauxite,including aluminum oxide,silicon dioxide,iron oxide,titanium dioxide,potassium oxide,calcium oxide,magnesium oxide,phosphorus pentoxide,vanadium,chromium,lead,copper,strontium,zirconium,gallium,and zinc.Scanning electron microscopy analysis of the sample surface morphology revealed that the high-pressure sample preparation can produce samples that are denser,flatter,and smoother,thereby reducing the determination error caused by surface irregularities.The sensitivity of the high-pressure prepared powder pellet for elemental analysis is significantly improved,the detection limits are significantly lowered,the analysis results are closer to the standard values,and both precision and the reproducibility of sample preparation are greatly enhanced.The internal standard correction of trace heavy elements(Z>26)such as lead,copper,strontium,zirconium,gallium,and zinc is performed using rhodium target Compton scattered radiation,while empirical coefficient methods are used to correct spectral line overlap and matrix effects for the other elements.The correlation coefficients R^(2)of the calibration curves for each component are≥0.98.The analytical results of the samples,verified by samples not involved in the regression,are basically consistent with the chemical values,meeting the requirements for rapid analysis.

关 键 词：铝土矿 高压制样 灵敏度 精密度 

分 类 号：O614.3[理学—无机化学]