熔融制样-波长色散X射线荧光光谱法测定钽铁、铌铁精矿中五氧化二钽、五氧化二铌、二氧化钛  

Determination of tantalum pentoxide,niobium pentoxide and titanium dioxide in tantalum-iron and niobium-iron concentrates by wavelength dispersive X-ray fluorescence spectrometry with fusion sample preparation

作　　者：刘名红 熊定淦 肖娟 袁琦 LIU Minghong;XIONG Dinggan;XIAO Juan;YUAN Qi(Ganzhou Metallurgical Research Institute Testing Technology Service Co.,Ltd.,Ganzhou 341000,China)

机构地区：[1]赣州冶研所检测技术服务有限公司,江西赣州341000

出　　处：《冶金分析》2025年第2期70-75,共6页Metallurgical Analysis

摘　　要：目前钽铁、铌铁精矿中五氧化二钽、五氧化二铌的测定采用重量法,二氧化钛的测定采用双安替吡啉甲烷分光光度法或电感耦合等离子体原子发射光谱法(ICP-AES);这些测定方法操作流程较长,且不能一次制样同时测定,不能够完全满足检测效率的要求。本文建立了熔融制样-波长色散X射线荧光光谱法(WDXRF)测定钽铁、铌铁精矿中五氧化二钽、五氧化二铌、二氧化钛的测定方法。通过实验对仪器工作参数进行了优化;对熔融温度和时间进行了考察,确定了熔融温度1 100℃、熔融时间10 min的最佳条件,此时熔体流动性好,试料片均匀,无不熔物;另外,比较了用内标校正与直接测定对校准曲线线性相关系数的影响,结果显示五氧化二钽用二氧化铪校正后校准曲线线性相关系数得到明显改善,五氧化二铌和二氧化钛使用内标和直接测定两者校准曲线线性相关系数无明显差别。按照实验方法测定3个钽铁、铌铁精矿样品中五氧化二钽、五氧化二铌、二氧化钛,结果的相对标准偏差(RSD,n=9)小于3%;分别采用本法和化学湿法分别对钽铁、铌铁精矿样品中各组分进行测定,结果无明显差异。At present,the determination of tantalum pentoxide and niobium pentoxide in tantalum-iron and niobium-iron concentrate usually adopts gravimetric method,while the determination of titanium dioxide adopts diantipyrylmethane spectrophotometry or inductively coupled plasma atomic emission spectrometry(ICP-AES).However,these determination methods have long operation procedures,and the sample cannot be determined simultaneously in once sample preparation,which hardly meet the requirements of detection efficiency.In this study,the determination method of tantalum pentoxide,niobium pentoxide and titanium dioxide in tantalum-iron and niobium-iron concentrates by wavelength dispersive X-ray fluorescence spectrometry(WDXRF)with fusion sample preparation was established.The working parameters of the instrument were optimized by experiments,and the melting temperature and time were studied.It was found that the optimal melting temperature and time were 1100℃and 10 min,respectively.The fluidity of melt flow good,the test piece was uniform without non-melt.In addition,the effects of internal standard correction and direct determination on the linear correlation coefficient of the calibration curve were compared.The results showed that the linear correlation coefficient of the calibration curve of tantalum pentoxide was significantly improved after correction with hafnium dioxide.There was no significant difference in the linear correlation coefficient of the calibration curve using internal standard and direct determination for niobium pentoxide and titanium dioxide.The contents of tantalum pentoxide,niobium pentoxide and titanium dioxide in three tantalum-iron and niobium-iron concentrate samples were determined according to the experimental method.The relative standard deviations(RSD,n=9)of determination results were less than 3%.The components of tantalum-iron and niobium-iron concentrate samples were determined by this method and the chemical wet method,and there was no significant difference in the results.

关 键 词：熔融制样 波长色散X射线荧光光谱法(WDXRF) 五氧化二钽 五氧化二铌 二氧化钛 钽铁精矿 铌铁精矿 

分 类 号：TF031[冶金工程—冶金物理化学] TF041[理学—分析化学] O657.34[理学—化学]