X射线荧光光谱法测定转炉渣中8种成分

Determination of eight components in converter slag by X-ray fluorescence spectrometry

探讨了利用压片法制样X射线荧光光谱法测定转炉渣中CaO等8种成分的分析方法。重点对制样条件、仪器参数、基体干扰、曲线拟合等方面进行了研究,确定了合适的研磨时间、样品粒度、压片时间、压片时所需的压力;试验了各成分的通道类型、晶体类型、探测器类型、管压、管流等分析条件,确定了最佳分析参数;选择了与试样基体相匹配的样品,定值后建立校准曲线,消除了基体干扰;对FeO的测定采用经验系数法消除了共存元素的干扰。本法测定范围宽,精密度高,稳定性好,测得各成分的相对标准偏差均小于2%。经对标准样品的测定,各成分测定值的误差符合国家标准允许差。本方法与化学分析法、ICP-AES法比较,操作简单,易于掌握,成本低,适合生产需要,结果吻合较好。

The determination of eight components including CaO in converter slag by X-ray fluorescence spectrometry combined with pressing method was studied. The effects of sample preparation conditions, instrument parameters, matrix interference and curve fitting were investigated. Proper grinding time, sample granularity, pressing time and pressure were obtained. The analytical conditions such as channel type, crystal type, detector type, tube voltage and tube current were investlgated to find the optimal analytical parameters. The calibration curve was established by characterisation of the samples matrix-matched with determined samples to eliminate matrix interference. The interference of coexisting elements with the determination of FeO was eliminated by empirical coefficient method. This method had wide determination range, high precision and good stability. The relative standard deviations were all less than 2 %. The measuring errors of standard sample accorded with the allowable value of GB method. Compared with chemical analysis and ICP-AES, this method had many merits such as simple operation, easy to learn and low cost. This method was satisfatory for the demands of actual production.