X射线荧光光谱法测定FeCuNbSiB纳米晶合金炉渣中9种组分

Determination of nine components in slag of FeCuNbSiB nanocrystal alloy by X-ray fluorescence spectrometry

提出了用熔融制样-X射线荧光光谱法测定FeCuNbSiB纳米晶合金炉渣中TFe,CaO,MgO,SiO2,Al2O3,MnO,CuO,Nb2O5和TiO2的方法。讨论了玻璃熔片的制备、混合熔剂和脱模剂的用量、基体的吸收和增强效应校正,以及用人工配制的标准样品绘制校准曲线等问题。在最佳的分析条件下,测定了人工配制的标准样品中TFe,CaO,MgO,SiO2,Al2O3,MnO,CuO,Nb2O5和TiO2的含量,11次测定结果的相对标准偏差小于0.7%,所得的分析结果与标准样品的标准值相符合。用此方法分析了FeCuNbSiB纳米晶合金炉渣试样,用同一样品在完全相同条件下制备了11个熔片进行测量,其测定结果的相对标准偏差小于3.0%,所得分析结果与其他方法的测定值相一致。

A method for the determination of 9 components,i.e.TFe,CaO,MgO,SiO2,Al2O3,MnO,CuO,Nb2O5 and TiO2 in slag of FeCuNbSiB nanocrystal alloy by X-ray fluorescence spectrometry with the fusion sample preparation method was proposed.The problems about preparation of glass bead,the usage of mixed flux and mold release agent,matrix correction of absorption and enhancement effects,calibration curves with synthetic standard samples,were discussed.Under the analytical optimum condition,TFe,CaO,MgO,SiO2,Al2O3,MnO,CuO,Nb2O5 and TiO2 in synthetic standard sample were determined.Values of RSDs（n=11） were less than 0.7% and the analytical results obtained were consistent with the certified values.Chemical components in real nanocrystal alloy slag sample were determined.Eleven glass beads which were prepared under the same condition by the same sample were measured.Values of RSDs（n=11） were less than 3.0% and the analytical results obtained by the proposed method were in good accordance with those by chemical analysis method and ICP-AES method.