X射线荧光光谱扩展基本参数法解析不锈钢炉渣成分

针对复杂的不锈钢炉渣成分解析问题,实验采用Li₂B₄O₇-LiBO₂(m∶m=67∶33)为混合熔剂,NH₄NO₃做氧化剂,LiBr溶液(500g/L)做脱模剂,制备玻璃熔片;应用X射线荧光光谱(XRF)分析软件UniQuant扩展基本参数法,建立并校正不锈钢炉渣的背景形状、杂质因子,以谱线灵敏度系数和光谱重叠系数校正光谱干扰和基体效应,对不锈钢渣中可能存在的20余种成分进行解析,实现了不锈钢渣系中CaO、MgO、SiO₂、Al₂O₃、TiO₂、MnO、Fe₂O₃、P₂O₅、SO₃、F、Cr₂O₃、NiO、V₂O₅、BaO共14种成分的定量分析及其他成分的定性半定量分析。对不锈钢工艺炉渣进行制样方法精密度考察,各组分测定结果的相对标准偏差(RSD,n=11)为0.15%~11%;对标样JKS11进行精密度测试,各组分测定结果的相对标准偏差(RSD,n=11)为0.030%~12%;对不锈钢炉渣标样和不锈钢工艺炉渣试样进行分析,14种主要组分的测定值与认定值或湿法值比对一致性好。

Composition analysis of stainless steel slag by X-ray fluorescencespectrometry combined with extended fundamental parameter method

For the analysis of complicated composition in stainless steel slag, the sample was prepared by fusion method under the following conditions: Li₂B₄O₇-LiBO₂ (m∶m=67∶33) was used as mixed flux, NH₄NO₃ was used as oxidizing agent, and LiBr solution (500g/L) was used as releasing agent. The extended fundamental parameter method in X-ray fluorescence spectrometry (XRF) analysis software UniQuant was adopted to establish and correct the background shape and impurity factor of stainless steel slag. The spectral interference and matrix effect were corrected using the spectral sensitivity coefficient and spectral overlapping coefficient. More than 20 components which possibly existed in stainless steel slag were analyzed. The quantitative analysis of 14 components (including CaO, MgO, SiO₂, Al₂O₃, TiO₂, MnO, Fe₂O₃, P₂O₅, SO₃, F, Cr₂O₃, NiO, V₂O₅ and BaO) as well as qualitative and semi-quantitative analysis of other components in stainless steel slag were realized. The precision of sample preparation method was investigated, and the relative standard deviations (RSD, n=11) of determination results were between 0.15% and 11%. The precision test of standard sample JKS11 was conducted, and the RSD (n=11) were between 0.030% and 12%. The standard sample and actual sample of stainless steel slag were analyzed according to the experimental method. The found results of 14 main components were consistent with the certified values or those obtained by wet method.