熔融制样-X射线荧光光谱法测定硅锰合金和锰铁合金中硅锰磷铁

Determination of silicon,manganese,phosphorus and iron in silicomanganese and ferromanganese alloys by X-ray fluorescence spectrometry with fusion sample preparation

熔融制样-X射线荧光光谱法测定铁合金化学成分,关键技术是样品预氧化,以有效避免铂金坩埚受到侵蚀。试验以专用氧化剂预处理硅锰合金和锰铁合金样品,以四硼酸锂-混合熔剂(m(Li_2B_4O_7)∶m(LiBO_2)=67∶33)为熔剂熔融制备玻璃片,建立X射线荧光光谱法(XRF)测定硅锰合金和锰铁合金中硅、锰、磷、铁含量的方法。以碳含量校正烧失量对检测结果的影响,进一步探讨了氧化剂加入量、稀释比、熔融温度、熔融时间等条件对硅锰合金和锰铁合金中锰、硅、磷、铁含量的影响,得出最佳熔融条件。熔融制得的玻璃片均匀、光洁,满足XRF测定要求。各元素测定结果的相对标准偏差(RSD,n=12)在0.25%～4.3%之间;测定结果与硅锰、锰铁标准物质认定值相符。

During the determination of chemical composition in iron alloys by X-ray fluorescence spectrometry(XRF)with fusion sample preparation,the key step is the pre-oxidization of sample,which can effectively avoid the erosion of platinum-gold crucible.The silicomanganese and ferromanganese alloy samples were pretreated with special oxidants.The glass beads were prepared using the mixed flux(m(Li2B4O7)∶m(LiBO2)=67∶33).The determination method of silicon,manganese,phosphorus and iron in silicomanganese and ferromanganese alloys by XRF was established.The influence of loss on ignition(LOI)on determination results was corrected using the carbon content.The effects of the oxidant dosage,dilution ratio,melting temperature and melting time on the determination of manganese,silicon,phosphorus and iron in silicomanganese and ferromanganese alloys were further discussed.The optimal melting conditions were obtained.The prepared glass beads were uniform with smooth surface,which could meet the measurement requirements of XRF.The relative standard deviations(RSD,n=12)of measurement results were between 0.25%and 4.3%.The found results were consistent with the certified values of standard substances of silicomanganese and ferromanganese alloys.