熔融制样—X射线荧光光谱法测定锰矿石中17种主次组分

刘江斌,党亮,和振云

冶金分析 ›› 2013, Vol. 33 ›› Issue (9) : 37-41.

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冶金分析 ›› 2013, Vol. 33 ›› Issue (9) : 37-41.
目次

熔融制样—X射线荧光光谱法测定锰矿石中17种主次组分

  • 刘江斌,党亮,和振云
作者信息 +

Determination of seventeen major and minor components in manganese ores by X-ray fluorescence spectrometry with fusion sample preparation

  • LIU Jiang-bin,DANG Liang, HE Zhen-yun
Author information +
文章历史 +

摘要

选用混合熔剂(Li2B4O7-LiBO2-LiF)熔融制样,用X射线荧光光谱仪对锰矿样品中的Mn、TFe、SiO2、Al2O3、CaO、MgO、K2O、Na2O、TiO2、P、S、BaO、Cu、Co、Ni、V、As等17种主次组分进行测定。以NH4NO3为氧化剂、Li2CO3为保护剂可使锰矿中的S与As在预氧化时转化为稳定的盐形式,从而防止S、As在熔样过程中的挥发损失。加入Cr2O3做Mn的内标可消除基体效应对Mn测定的影响。对锰矿石合成标样进行精密度考察,相对标准偏差(RSD,n=12)均小于10%:对锰矿石标准样品及合成样品进行准确度考察,测定值与认定值或湿法测定值一致。

Abstract

After the sample was melted with mixed flux (Li2B4O7-LiBO2-LiF), seventeen major and minor components in manganese ore, including Mn, TFe, SiO2, Al2O3, CaO, MgO, K2O, Na2O, TiO2, P, S, BaO, Cu, Co, Ni, V and As, were determined by X-ray fluorescence spectrometry. S and As could be converted to stable salt during pre-oxidation with NH4NO3 as oxidizing agent and Li2CO3 as protective agent. Consequently, the volatilization loss of S and As in sample preparation by fusion could be prevented. Cr2O3 was added and used as internal standard for Mn to eliminate the matrix effect on the determination of Mn. The precision test was performed with manganese ore synthetic reference samples. The relative standard deviation (RSD, n=12) was less than 10%. The accuracy test was conducted with manganese ore reference samples and synthetic samples. The results were consistent with the certified values and those obtained by wet method.

关键词

X射线荧光光谱 / 熔融制样 / 锰矿石

Key words

X-ray fluorescence spectrometry / fusion sample preparation / manganese ore

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刘江斌, 党亮, 和振云. 熔融制样—X射线荧光光谱法测定锰矿石中17种主次组分[J]. 冶金分析, 2013, 33(9): 37-41
LIU Jiang-bin, DANG Liang, HE Zhen-yun. Determination of seventeen major and minor components in manganese ores by X-ray fluorescence spectrometry with fusion sample preparation[J]. Metallurgical Analysis, 2013, 33(9): 37-41
中图分类号: O657.34   

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