波长色散X射线荧光光谱法测定五氧化二钒中主次组分

采用熔融法制备试样,以混合熔剂(mLi2B4O7∶mLiBO2=67∶33)做熔剂,同样品放入铂-黄金坩埚中熔融成玻璃片,其中加入硝酸铵作为氧化剂可避免砷在熔融过程中的损失。通过熔融条件对比试验确定了熔剂稀释比为1∶13,熔融温度为950℃。以五氧化二钒高纯试剂作为基体,加入标准物质,制备标准融片并绘制五氧化二钒、铁、磷、硅、砷、氧化钾、氧化钠主次成分的校准曲线,建立了X射线荧光光谱法(XRF)测定五氧化二钒中主次成分的方法。结果表明,铁、磷、硅、砷、氧化钾、氧化钠次量成分的检出限分别为200、100、100、100、100、100μg/g,相对标准偏差(RSD)均小于0.2%。对五氧化二钒实际样品进行分析,实验方法的测定结果与目前行业标准所用方法的测定结果具有良好的一致性。

Determination of major and minor components in vanadium pentoxide by wavelength dispersive X-ray fluorescence spectrometry

The sample was prepared by the fusion method. The mixed flux (m_Li2B4O7∶m_LiBO2=67∶33) was used to prepare the sample tablet in platinum-gold crucible. The ammonium nitrate was added as the oxidizing agent to avoid the loss of arsenic in fusion process. The results showed that the optimal conditions were as follows: the dilution ratio was 1∶13, and the melting temperature was 950 ℃. The high-purity reagent of vanadium pentoxide was used as matrix. The certified reference material was added to prepare the fusion tablet for the drawing of calibration curves of vanadium pentoxide, iron, phosphorus, silicon, arsenic, potassium oxide and sodium oxide as major and minor components. The determination method of major and minor components in vanadium pentoxide by X-ray fluorescence spectrometry (XRF) was established. The results indicated that the detection limit of minor components including iron, phosphorus, silicon, arsenic, potassium oxide and sodium oxide was 200, 100, 100, 100, 100 and 100 μg/g, respectively. The relative standard deviations (RSD) were less than 0.2%. The actual vanadium pentoxide sample was analyzed, and the found results were in good agreement with those obtained by the industrial standard method at present.