摘要
采用熔融制样-X射线荧光光谱法测定矿物中的Cu、Pb、Zn、Mo、W、Al、Fe、Si、K、Na、Ti、Ca、Sn等13种主次量元素,采用混合均匀的三混熔剂,以硝酸锂为氧化剂、溴化锂为脱膜剂,进行实验条件优化选择。在650℃下对样品进行预氧化,在1100℃下高温熔融,熔融时间为300 s,最后制成均匀透明,表面光滑无气孔的熔片,以部分国家一级标准物质和自制的钨钼锡标准样品,熔融制片进行测定,线性拟合建立标准曲线,并通过测定谱线选择、基体校正,使钨钼锡的测定范围扩宽,从微量到主量均能进行测定,并且适用于多种不同矿石的测定。样品的组成和含量变化会对分析线强度造成吸收、增强以及谱线重叠的影响,采用经验系数和理论α系数结合来校正其产生的基体效应。相同条件下熔融10个标准样品进行测定,其相对标准偏差(RSD)均小于5%,表明方法的准确度、精密度均满足国家相关质量标准的要求。选用一些含量不同的标准样品进行测定,最终的测定结果与标准值相符,表明方法可用于钨钼锡矿的测定。
In this paper,determination method of 13 primary and secondary elements,including Cu,Pb,Zn,Mo,W,Al,Fe,Si,K,Na,Ti,Ca,Sn,by the melting sample preparation-X ray fluorescence spectrometry with mixing 3 solvent,lithium nitric acid as oxidizing agent,lithium bromide as remover was developed.The optimal selection experiment condition is the samples under 650℃to oxidation,and then under the 1100℃high temperature melting,melting time of 300 s,the last made uniform transparent,smooth surface,no stomata fuse link,as part of a national level standard substance and homemade molybdenum tungsten tin standard sample,melting production were determined,linear fitting to establish standard curve,and by measuring the spectral line selection,the matrix correction,expanding the area of the determination of molybdenum tungsten tin,from the trace to the quantity can be measured,and suitable for a variety of different analysis of the ore.Changes on the analysis of the composition and content of the sample line intensity due to absorption,enhance,and the influence of the spectral overlap,by adopting the combination of theory of alpha coefficient and experience coefficient method to correcting the matrix effect.Under the same conditions,10 melt sample are determined,the RSD are less than 5%,it shows that accuracy and precision of the method can meet the requirements of relevant national quality standards.Some different content samples are chosen to determine,the final determination results shows that this method are consistent with the standard values,indicates that this method can be used for the determination of tungsten and molybdenum tin ore.
作者
刘恒杰
贾海峰
谭清月
LIU HengJie;JIA Haifeng;TAN Qingyue(Central South Institute of Metallurgical Geology,Yichang,Hubei 443003,China)
出处
《中国无机分析化学》
CAS
2020年第1期70-75,共6页
Chinese Journal of Inorganic Analytical Chemistry
关键词
X射线荧光光谱法
钨钼锡
熔融制样
校准曲线
基体校正
X-ray fluorescence spectrometry
molybdenum tungsten tin
the molten sample preparation
calibration curve
matrix correction
作者简介
刘恒杰,男,研究实习员,主要从事岩石矿物检测分析研究。E-mail:13163367173@163.com.
