粉末压片制样-X射线荧光光谱法测定稀土镁中间合金中镁锰硅钛钙铁

摘要

以粉末压片法制样,采用X射线荧光光谱法(XRF)测定稀土镁中间合金中M g、M n、Si、Ti、Ca、Fe含量.对样品的矿物效应、样品粒度及成型试验进行了分析研究,通过实验发现利用不同产地的标准样品制作校准曲线,矿物效应影响不大;通过将样品粒度研磨至不大于74 μm,能很好的解决粒度效应的影响.精密度实验表明,待测组分的相对标准偏差(RSD, n=10)均不大于2.8%;对来自不同产地的样品进行正确度考察,测定值与国标方法的测定值一致,满足GB/T16477—2010稀土镁中间合金中各组分含量的允许差要求.%The sample was prepared with pressed powder pellet.The contents of Mg,Mn,Si,Ti,Ca and Fe in rare earth-magnesium intermediate alloy were determined by X-ray fluorescence spectrometry (XRF).The mineral effect,sample granularity and forming experiment were analyzed and investigated. The experiments showed that the influence of mineral effect was insignificant when the calibration curve was prepared with certified reference materials from different producing area.The influence of granularity effect could be well solved by grinding the sample to not more than 74μm.The precision tests indicated that the relative standard deviations(RSD,n=10)of tested components were not more than 2.8%.The accuracy was investigated with samples from different producing area.The results were consistent with those obtained by national standard method.The proposed method could meet the requirements of allowed tolerance for each component in rare earth-magnesium intermediate alloy specified in GB/T 16477—2010.