Abstract:During the determination of primary and secondary elements in iron ore by melting sample preparation-X-ray fluorescence spectrometry (XRF), if the iron ore samples are directly melted, the measurement results of TFe are instable due to the influence of various matrix effects. In order to obtain stable and reliable TFe contents, the cobalt internal standard method is usually adopted. In other words, quantitative cobalt is added as the internal standard in fusion sample preparation of iron ore. However, Co2O3 is easily converted into CoO at high temperature, which will cause corrosion of platinum-gold crucible. The oxidation environment was continuously provided for Co2O3 before being melted into lithium borate flux,so that Co element did not appear as CoO in the whole melting sample preparation process,which solved the corrosion problem of platinum-gold crucible. The melting conditions were optimized through experiments: swing at 1 050 ℃ for 7 min, dilution ratio of 1∶10, and KBr as release agent. The correlation coefficients of calibration curves for major and minor components in iron ore were all above 0.997. The precision of iron ore certified reference material was investigated. The relative standard deviations (RSD, n=12) of the determination results were not more than 6.7%. The trueness results showed that the measured values of standard samples and actual samples were consistent with the certified values and those obtained by the national standard wet method, respectively.
顾强, 滕广清, 王彬果, 冀丽英, 张建忠, 温静. 钴内标熔融制样-X射线荧光光谱法分析铁矿石中主次成分[J]. 冶金分析, 2021, 41(11): 43-48.
GU Qiang, TENG Guangqing, WANG Binguo, JI Liying, ZHANG Jianzhong, WEN Jing. Analysis of major and minor components in iron ore by cobalt internal standard X-ray fluorescence spectrometry with fusion sample preparation. , 2021, 41(11): 43-48.
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