熔融制样—X射线荧光光谱法测定锰矿石中17种主次组分

选用混合熔剂(Li₂B₄O₇-LiBO₂-LiF)熔融制样，用X射线荧光光谱仪对锰矿样品中的Mn、TFe、SiO₂、Al₂O₃、CaO、MgO、K₂O、Na₂O、TiO₂、P、S、BaO、Cu、Co、Ni、V、As等17种主次组分进行测定。以NH₄NO₃为氧化剂、Li₂CO₃为保护剂可使锰矿中的S与As在预氧化时转化为稳定的盐形式，从而防止S、As在熔样过程中的挥发损失。加入Cr₂O₃做Mn的内标可消除基体效应对Mn测定的影响。对锰矿石合成标样进行精密度考察，相对标准偏差(RSD，n=12)均小于10%：对锰矿石标准样品及合成样品进行准确度考察，测定值与认定值或湿法测定值一致。

Determination of seventeen major and minor components in manganese ores by X-ray fluorescence spectrometry with fusion sample preparation

After the sample was melted with mixed flux (Li₂B₄O₇-LiBO₂-LiF), seventeen major and minor components in manganese ore, including Mn, TFe, SiO₂, Al₂O₃, CaO, MgO, K₂O, Na₂O, TiO₂, P, S, BaO, Cu, Co, Ni, V and As, were determined by X-ray fluorescence spectrometry. S and As could be converted to stable salt during pre-oxidation with NH₄NO₃ as oxidizing agent and Li₂CO₃ as protective agent. Consequently, the volatilization loss of S and As in sample preparation by fusion could be prevented. Cr₂O₃ was added and used as internal standard for Mn to eliminate the matrix effect on the determination of Mn. The precision test was performed with manganese ore synthetic reference samples. The relative standard deviation (RSD, n=12) was less than 10%. The accuracy test was conducted with manganese ore reference samples and synthetic samples. The results were consistent with the certified values and those obtained by wet method.