X射线荧光光谱法测定高铬型钒渣中主次组分

Determination of Major and Minor Components in High Chromium Type Vanadium Slag by X-Ray Fluorescence Spectrometry

称取于750~800℃灼烧2h后的试样0.300 0g,置于盛有4.000 0g四硼酸锂、3.000 0g偏硼酸锂、0.500 0g碳酸锂的铂黄坩埚中,搅匀,加入300g·L-1溴化锂溶液0.5mL,在(1 050±20)℃熔融制片,采用X射线荧光光谱法测定高铬型钒渣中主次组分含量。采用钒渣标准样品和由标准样品加基准物质配制成的系列校准样品绘制校准曲线以消除基体效应,选择分析谱线并进行谱线重叠干扰校正。各组分的质量分数在一定范围内与荧光强度呈线性关系。方法用于分析高铬型钒渣样品,所得结果与滴定法、电感耦合等离子体原子发射光谱法的结果一致,测定值的相对标准偏差(n=10)在0.030%~7.3%之间。

After ignition at 750-800 ℃for 2 h,0.300 0 g of the sample was mixed well with 4.000 0 g of lithium tetraborate,3.000 0 g of lithium metaborate,and 0.500 0 g of lithium carbonate in a platinum yellow crucible.Then 0.5 mL of 300 g·L-1 lithium bromide solution was added into the crucible and the mixture was melted at（1 050±20）℃ to prepare sample sheets.The contents of major and minor components in the high chromium type vanadium slag were determined by X-ray fluorescence spectrometry.Vanadium slag standard samples and a series of calibration samples prepared with the standard samples and the reference substance were used to draw calibration curves to eliminate the matrix effect.The analysis lines were selected and spectral line overlap interference correction was performed.Linear relationships were found between values of the fluorescence intensity and the mass fractions of each component within definite ranges.The method was applied to analysis of high chromium type vanadium slag samples,giving results in consistency with those obtained by titration and inductively coupled plasma atomic emission spectrometry,and RSDs（n=10）were between 0.030% and 7.3%.