溶液制样-偏振能量色散X射线荧光光谱法分析石煤钒矿中五氧化二钒

以硝酸、次氯酸溶解样品，溶液制样法，采用偏振能量色散X射线荧光光谱法(EDXRF)对石煤钒中五氧化二钒含量进行了定量分析。采用盐酸溶解高纯五氧化二钒配制校准溶液并绘制校准曲线，线性相关系数为0.999 7，方法检出限为1.99 mg/L。试样中其他元素Si、Ca、Fe、Al、Mg对钒的测定无显著影响；XRF能谱图考察发现：Si、Ca、Fe、Al、Mg的Kα线与V的Kα线均无重叠，并且这些元素的Kβ线及次级线对V的Kα线也无重叠。精密度试验表明，10次测量结果的相对标准偏差为1.5%。方法用于石煤钒矿中钒元素的分析，与滴定法测定结果一致性较好。

Determination of vanadium pentoxide in stone coal vanadium ore by polarized energy dispersive X ray fluorescence spectrometry with sample solution preparation

After dissolved with nitric acid and hypochloric acid and prepared by solution method, the content of vanadium pentoxide in stone coal vanadium ore was quantitatively determined by polarized energy dispersion X ray fluorescence spectrometry (EDXRF).The high purity vanadium pentoxid was dissolved with hydrochloric acid to prepare calibration solution, and calibration curve was plotted with linear correlation coefficient of 0.999 7 and detection limit of 1.99 mg/L. The elements in the sample including Si, Ca, Fe, Al and Mg had no significant influence on the determination of vanadium. The XRF spectra indicated that the Kα lines of Si, Ca, Fe, Al and Mg were not overlapped with the Kα line of V. Moreover, the Kβ lines and secondary lines of these elements also had no overlapping with the Kα line of V. The precision test showed that the relative standard deviation (RSD, n=10) was 1.5%. The proposed method was applied to the analysis of vanadium in stone coal vanadium ore. The results were consistent with those obtained by titration.