粉末压片-能量色散X射线荧光光谱法测定高钛渣中6种组分

高钛渣中TiO2、SiO2、CaO、MnO、MgO、TFe含量采用滴定法、光度法等分析方法测定时,耗时相对较长,化学试剂使用量多,工作量大,开发一种简便、快速、多元素同时分析、准确度高的检测方法十分必要.实验采用粉末压片制样,以能量色散X射线荧光光谱法(EDXRF)测定高钛渣中TiO2、SiO2、CaO、MnO、MgO...

Determination of six components in high titanium slag by energy dispersive X-ray fluorescence spectrometry with pressed powder pellet

The contents of TiO₂, SiO₂, CaO, MnO, MgO and TFe in high titanium slag are usually determined by titrimetric methods or photometric methods. However, these methods are relatively time-consuming, the consumption of chemical reagents is large, and the workload is heavy. Therefore, it is necessary to develop a simple and rapid analysis method with high accuracy for the simultaneous determination of multi-elements. The sample was prepared by powder pressing method. The six components including TiO₂, SiO₂, CaO, MnO, MgO and TFe in high titanium slag were determined by energy dispersive X-ray fluorescence spectrometry (EDXRF). High titanium slag with particle size of 20 μm was selected, and boric acid was used as binder to edge the bottom. The samples prepared under the experimental conditions (pressure of 25 MPa and holding time of 5 min) were smooth and crack-free, and could be stored for a long time. Due to the shortage of high titanium slag standard sample, according to the content range of each component in the high titanium slag sample, the calibration curve was established using self-made reference standard samples with certain concentration gradient, which were prepared by certified reference materials of high titanium slag and high-purity reagents. Meanwhile, the matrix effect was corrected by fundamental parameter method. The correlation coefficients of calibration curves for testing components were not less than 0.998 0. The limits of detection (LOD) were between 0.002 5% and 0.037%. The relative standard deviations (RSD, n=8) of determination results were between 0.10% and 1.5%. The proposed method was applied for the analysis of actual high titanium slag samples, and the found results were in good agreement with those obtained by chemical wet method in industrial standard YS/T 514 series.