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粉末压片-X射线荧光光谱法快速分析多金属结核和富钴结壳中22种组分 被引量:10

Rapid determination of twenty-two components in polymetallic nodule and cobalt-rich crusts by X-ray fluorescence spectrometry with pressed powder pellet
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摘要 应用台式X射线荧光光谱仪结合压片法制样现场快速测定太平洋多金属结核和富钴结壳样品中的氧化钠、氧化镁、三氧化二铝、二氧化硅、五氧化二磷、氧化钾、氧化钙、二氧化钛、硫、氯、锰、铁、钴、镍、铜、锌、钒、锶、锆、钡、铈和钇等组分.采用国家标准物质、以国家标准物质为基体制备的校准样品和定值富钴结壳样品绘制校准曲线,解决了相关标准样品不足的问题.对22个组分的测量条件进行优化,并通过经验系数法校正了主要成分二氧化硅、氧化钙、铁和锰的干扰.方法的检出限在10.5~733 μg/g.精密度试验结果表明,各组分测定值的相对标准偏差(RSD,n=7)在0.56%~7.7%之间.方法用于实际样品分析,分析结果与实验室内其他方法的结果吻合,能够满足野外现场多种组分同时快速分析的要求. A method has been introduced for the field determination of Na2O,MgO,Al2O3,SiO2,P2O5,K2O,CaO,TiO2,S,Cl,Mn,Fe,Co,Ni,Cu,Zn,V,Sr,Zr,Ba,Ceand Y of polymetallic nodule and cobalt-rich crusts in the Pacific Ocean by X-ray fluorescence spectrometry (XRF) coupled with directly pressed powder sample preparation technique.The calibration curve was established with national certified reference materials,calibration samples made from national standard sample and calibration samples certified by other methods,adressing the shortage of nodule and crusts standard sample.The measuring conditions of 22 components were optimized,and the interference from major components including SiO2,CaO,Fe and Mn was corrected by the methods of empirical coefficient.The detection limit of the described method was 10.5-733 μg/g.The results of precision test indicated that the relative standard deviations (RSD,n=7) were 0.56%-7.7%.The proposed method has been applied to the determination of actual samples,the results were consistent with those obtained by other methods in laboratory,which is appropriate for rapid determination of multi-components in field.
作者 李强 张学华
出处 《冶金分析》 CAS CSCD 北大核心 2014年第1期28-33,共6页 Metallurgical Analysis
基金 中国地质调查局地质调查项目(1212011120271)
关键词 台式X射线荧光光谱仪 结核结壳 多种组分 现场分析 desktop X-ray fluorescence spectrometry nodule and crusts multi-components on-site analysis
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