X射线荧光光谱法测定电解锰中锰、硅、磷和铁含量

Quantitative Determination of Mn,Si,P and Fe in Electrolytic Manganese by X-ray Fluorescence Spectrometry

熔融制样X射线荧光光谱法测定电解锰中锰、硅、磷和铁含量。用熔融后的四硼酸锂制作铂金坩埚保护层,以BaO2做氧化剂,在马弗炉内通过逐渐升温来氧化电解锰,然后熔融制取玻璃熔片,用X射线荧光(XRF)光谱法分析电解锰中锰、硅、磷和铁含量。锰、硅、磷和铁的相对标准偏差RSD分别为0.23%、2.82%、0.31%和0.53%。与其它分析方法比较,其结果更稳定。有效消除了电解锰熔融制样过程中的坩埚腐蚀问题,分析误差可完全控制在国家相关标准允许的范围内,实现了电解锰中各元素的快速准确测定。

X-ray fluorescence spectrometry with fusion sample preparation method was used to determine the quantity of Mn, Si, P and Fe in electrolytic manganese. APt Au crucible was coated with a protective layer made by melting lithium tetraborate and used as the container for electrolytic manganese. The Pt-Au crucible with electrolytic manganese was placed in a muffle furnace. BaO2 was used as the oxidizing agent and the electrolytic manganese was gradually oxidized with increased temperatures. Afterwards, the glass plate was made by fusion method and then tested by X-ray fluorescence （XRF） spectrometer to determine the content of Mn, Si, P and Fe elements in electrolytic manganese. The precision of the method for Mn, Si, P,Feis 0.23%, 2.82%,0.31% and 0.53%, respectively. Comparing with other analytical methods, XRF method is more stable. Since this method solved the problem caused by corrosion of Pt-Au crucible during sample preparation by fusion method, analytical errors of the method could be controlled completely within the acceptable limits of the national standard. Thus, this method allows to quantitatively determine all elements in electrolytic manganese with fast speed and good reliability.