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熔融制样-X射线荧光光谱法测定磁铁矿中7种组分

     

摘要

研究了熔融制样-X射线荧光光谱法测定磁铁矿中7种组分的分析方法.考察了稀释比、硝酸锂氧化剂用量、溴化锂脱模剂用量等因素,在优化条件下进一步选择了熔融温度及熔融时间.按试样与熔剂稀释比为1∶20在1 050℃熔融10 min制成玻璃样片,直接用X射线荧光光谱法(XRF)测定磁铁矿中的TFe、CaO、MgO、Al2O3、SiO2、TiO2和S.选择含铁量不同的一组磁铁矿标准样品建立校准曲线,线性相关系数均不小于0.997 4.测定磁铁矿实际样品时,测定结果与化学法一致,相对标准偏差中TFe为0.29%,S为3.4%,其它组分在0.29%~2.5%之间.%A determination method of seven components in magnetite was investigated by X-ray fluorescence spectrometry with fusion sample preparation.Such influence factors,including dilution ratio,the oxidant dosage (lithium nitrate) and the releasing agent (lithium bromide) dosage,were discussed.Under the optimal conditions,melting temperature and melting time was further selected.After glass sample pieces were prepared by fusion at 1 050 ℃ for 10 min with dilution ratio of 1∶ 20,seven components in magnetite,including TFe,CaO,MgO,Al2O3,SiO2,TiO2,were directly determined by X-ray fluorescent spectrometry.Calibration curves were established by magnetite certified reference materials with different iron content,and the linear correlation coefficients were not less than 0.997 4.When this method was applied to the determination of actual magnetite sample,the results were consistent with those obtained by chemical method,and the relative standard deviation (RSD) were as follows:0.29% for TFe,3.4% for S and 0.29%-2.5% for other elements.

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