高分辨电感耦合等离子体质谱法测定地球化学样品中钪钇和稀土元素
Determination of Sc, Y and Rare Earth Elements in Geochemical Samples by High Resolution Inductively Coupled Plasma-Mass Spectrometry
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摘要: 建立了高分辨电感耦合等离子体质谱法(HR-ICP-MS)测定地球化学样品中钪、钇、镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱和镥的分析方法。样品经氢氟酸-硝酸-硫酸-王水消解,试液直接用HR-ICP-MS测定钪、钇和14种稀土元素。用高分辨模式有效地避免了多原子离子及难熔氧化物离子对待测元素测定的干扰,为钪、钇和14种稀土元素选择了最佳的测定同位素和合适的分辨率;用地球化学标准物质制备的溶液优化仪器工作参数,确定了最佳的仪器测定条件。方法检出限(6σ)为0.003~0.013 μg/g(稀释因子为1000),相对标准偏差(RSD,n=12)小于6%。方法经国家一级地球化学标准物质验证,测定值与标准值吻合。
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关键词:
- 钪 /
- 钇 /
- 稀土元素 /
- 地球化学样品 /
- 高分辨电感耦合等离子体质谱法
Abstract: An analytical method for the determination of Sc, Y and 14 rare earth elements (La, Ce, P, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) by high resolution inductively coupled plasma-mass spectrometry (HR-ICP-MS) has been developed. Samples were decomposed by HF-HNO3-H2SO4-aqua regia, then 16 elements above in the solution were directly analyzed by HR-ICP-MS. The spectra interferences from polyatomic ions and oxide ions (MO+) could be avoided by measuring at high resolution mode. The optimal determination isotopes and appropriate resolution for rare earth elements (REEs) were selected. The operating parameters of HR-ICP-MS were optimized by testing geochemical standard materials with plenty of matrix. The detection limits (6σ) of the method for REEs were 0.003~0.013 μg/g (DF=1000). The relative standard deviation (RSD) was less than 6% (n=12). The method has been applied to determination of Sc, Y and REEs in geochemical national standard reference materials and the analytical results were in agreement with the certified values. -
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