2-乙基己基磷酸单(2-乙基己基)酯萃淋树脂分离-火花源质谱法测定高纯氧化镱中痕量稀土杂质

Extration Chromatographic Separation of Rare Earth Elements Impurities in High Purity Ytterbium Oxide With 2-Ethylhexylhydrogen-2-ethylhexylphosphonate and Their Determination by Spark Source Mass Spectrometry

本文采用萃取色谱法以２－乙基己基膦酸单（２－乙基己基）酯（Ｐ５０７）萃淋树脂为固定相，以ＨＣｌ－ＮＨ４Ｃｌ体系为淋洗液，研究了９９．９９９％￣９９．９９９９％的高纯Ｙｂ２Ｏ３中稀土杂质和Ｙｂ基体的分离条件，将杂质淋洗液富集于复合螯合剂－活性碳上，经灼烧灰化后制成样品电极，进行质谱测定。测定下限达０．０１￣０．０５μｇ／ｇ，可用于高纯Ｙｂ２Ｏ３中杂质的测定。回收率在８０％以上。

An extraction chromatographic method for separating rare earth impurities from high purity Yb203 was studied by using HCl-NH4Cl as eluate and P507 as stationary phase. After enriching the impurities from eluate by activated carbon the ashed product was used to prepare sample electrode for spark source mass spectrometric determination, the impurities in 99. 9999 Yb2O3 can be determined with recovery of over 80% by the proposed mehtod.