熔融制样-X射线荧光光谱法测定硅铁合金中主次元素

X-ray fluorescence spectrometry for the determination of major and minor elements in ferro-silicon alloy with fusion sample preparation

采用四硼酸锂挂壁制备熔剂坩埚,分散剂溶解并分散硅铁合金样品,蒸干过量水分后加混合熔剂[m(Li2B4O7)∶m(LiBO2)=67∶33]熔融制样,用X射线荧光光谱仪对硅铁合金中Si、Fe、Mn、Al、Ca等元素同时进行测定。本法有效避免了硅铁合金熔融过程中铂金坩埚腐蚀问题,且能够制得适合荧光分析硅铁合金玻璃片,实现了快速而准确地分析硅铁合金中主元素和微量元素。采用本方法分析硅铁合金标准样品,测定值与认定值相符,且主次元素相对标准偏差均能满足硅铁合金测定需要。

The fused glass bead of ferro-silicon sample was prepared with ferro-silicon alloy that was dissolved and dispersed with dispersant agent through adding a mixed flux of Li2B4O7 and LiBO2 [m（Li2B4O7）∶m（LiBO2） =67∶33] after evaporating the excessive water in a flux crucible whose wall was attached with lithium tetraborate.Then,Si,Fe,Mn,Al,and Ca in the sample were simultaneously determined with X-ray fluorescence spectrometer.By the proposed method,the ferro-silicon alloy glass bead that was suitable for X-ray fluorescence spectrometer could be prepared while the corrosion of Pt-Au crucible during the fusing process of ferro-silicon alloy was effectively avoided,so that a rapid and accurate determination of major and micro elements in ferro-silicon alloy was realized.The found value of the ferro-silicon alloy standard sample prepared by this method was consistent with the certified value.And the RSD of both major and minor elements could satisfy the requirement of determination.