采用粉末压片法制取试样,波长色散X射线荧光光谱法测定氧化钼中的Mo、Pb、Cu、Fe、SiO_2、CaO、K等7种成分.对仪器参数、基体干扰、曲线拟合进行了研究,试验了各成分的通道类型、晶体类型、探测器类型、管压、管流等分析条件后确定了最佳分析参数.选择了与试样基体相匹配的定值样品建立校准曲线,采取经验系数法对基体效应进行校正.对于主次量组分,相对标准偏差低于1%(n=11).方法用于实际样品的分析,其荧光分析值与湿法分析值相符.方法能够很好满足氧化钼的主次成分分析.
A method for the determination of Mo,Pb,Cu,Fe,SiO_2 ,CaO and K in molybdenum oxide by wave-dispersive X-ray fluorescence spectrometry was established in combination with powder pellet sample preparation. The effects of instrument parameters, matrix interference and curve fitting were investigated. The analytical conditions were investigated such as channel, crystal type, detector, tube voltage and tube current. The calibration curves were drawn by characterization samples that were matched with the determined samples to eliminate matrix interference. The matrix effect was eliminated by using empirical coefficient method. The relative standard deviation for major and minor components were smaller than 1% (n=11). The results in molybdenum oxide were in agreement with those provided by the wet methods. The method has been applied for analysis of major and minor components for molybdenum oxide with satisfactory results.
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