熔融制样-X射线荧光光谱法同时测定金红石中主、次、微量元素含量

Simultaneous Determination of Major,Minor and Trace Elements in Rutile by Melting Sample Preparation-X-ray Fluorescence Spectrometry

采用熔片法制得玻璃片,在标准样品数量少、元素含量不全的条件下,使用标准样品人工配制合成标样及加入多种类标准样品的方法,建立了金红石中Al、Si、Fe、Ca、Mg、P、Ti、Mn、V、Cr、Zr、Nb等12种元素同时测定的X射线荧光光谱分析法。采用熔融制样,以四硼酸锂-偏硼酸锂混合熔剂(67∶33)作为熔样体系,讨论了熔剂选择、熔片温度、稀释比及脱模剂用量等条件对熔片效果的影响。标准曲线使用变化理论α系数校和谱线重叠校正,相对标准偏差为0.21%~4.20%(n=10)。熔融制样-X射线荧光光谱分析法的分析结果与容量法和电感耦合等离子体原子发射光谱法分析结果进行对比,结果令人满意,说明该方法可应用于金红石中主、次、微量成分的快速分析。

Glass flakes were prepared by melting method.Under the condition of small number of standard samples and incomplete element content,X-ray fluorescence spectrometry for simultaneous determination of 12 elements such as Al,Si,Fe,Ca,Mg,P,Ti,Mn,V,Cr,Zr and Nb in rutile was established by using standard samples to artificially prepare synthetic standard samples and adding various standard samples.The lithium tetraborate-lithium metaborate mixed flux(67∶33)was used as the melting sample system.The effects of flux selection,melting temperature,dilution ratio and the amount of release agent on the melting effect were discussed.The standard curve was calibrated by the variation theoryαcoefficient and the spectral line overlap correction,and the relative standard deviation was 0.21%-4.20%(n=10).The results of melting sample preparation-X-ray fluorescence spectrometry were compared with those of volumetric method and inductively coupled plasma atomic emission spectrometry.The results were satisfactory,indicating that this method can be applied to the rapid analysis of major,minor and trace components in rutile.