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本文首次提出用三正辛基氧膦为固定相,反相萃取柱色层法将十五个稀土杂质与基体钪分离,然后用ICP发射光谱法测定高纯氧化钪中十五个稀土杂质的方法。本法具有使用酸度低,分离完全、迅速,基体负载量较大,ICP光谱测定灵敏度高等优点。通过试样分析与加入实验各八次的测定结果表明,试样分析和加入实验的RSD分别为5-15.4％和0.63-6.3％,平均回收率在99-112％之间。试样含0.00095％的稀土杂质,钪纯度相当于99.999％,则可分离分析。若相应增加柱径以提高基体的负载量及柱效,分析纯度更高的试样应当是可以达到的。
In this paper, we first proposed the use of tri-n-octylphosphine oxide as the stationary phase, reversed-phase extraction column chromatography fifteen rare earth impurities and the matrix scandium separation, and then ICP emission spectrometry determination of high-purity scandium oxide fifteen rare earth impurities method. This method has the advantages of low acidity, complete and rapid separation, large substrate load and high sensitivity of ICP spectrometry. Through the analysis of the sample and the addition of eight times each, the results showed that the RSD of the sample analysis and the addition experiment were 5-15.4% and 0.63-6.3%, respectively. The average recovery was between 99-112%. The sample contains 0.00095% of rare earth impurities, scandium purity equivalent to 99.999%, you can separate analysis. If a corresponding increase in diameter to increase the load capacity and efficiency of the matrix, the analysis of samples with higher purity should be achievable.