熔融制样-X射线荧光光谱法测定氯化炉渣中12种组分含量

Determination of 12 components in chlorinated furnace slag by fusion sample preparation and X-ray fluorescence spectrometry

本文采用钒钛高炉渣、钒渣、高钛渣、高炉渣等标准样品建立含量范围梯度大的标准曲线,同时测定氯化炉渣中Al、Si、Fe、Ca、Mg、P、Ti、Mn、K、Na、V、Cr。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,讨论了熔融制样熔剂选择、熔片温度、稀释比及脱模剂用量等条件对熔片效果的影响。使用变化理论α系数校正,谱线重叠校正对标准曲线进行校正,对方法的精密度进行了考察,其中相对标准偏差为0.21%~4.20%(n=10)。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,本方法可适用于氯化炉渣样品成分的快速分析。

The standard curves with large gradient in content range are established with standard samples such as vanadium-titanium blast furnace slag,vanadium slag,high-titanium slag,and blast furnace slag.And Al,Si,Fe,Ca,Mg,P,Ti,Mn,K,Na,V and Cr in slag are determined at the same time.The sample was prepared by melting,and the mixed flux of lithium tetraborate and lithium metaborate(67:33)was used as the melting system.The effects of the selection of melting flux,melting temperature,dilution ratio and the amount of release agent on the melting effect were discussed.The standard curve was corrected by usingαcoefficient correction of change theory and spectral line overlap correction,and the precision of the method was investigated,among which the relative standard deviation was 0.21%~4.20%(n=10).The analysis results are compared with those of volumetric method and inductively coupled plasma atomic emission spectrometry,and the results are satisfactory,which can be applied to the rapid analysis of various types of vanadium slag samples.