电感耦合等离子体质谱法测定铀铌混合氧化物中的钐、铕、钆、镝

    Determination of Trace Amounts of Sm, Eu, Gd and Dy in U-Nb Mixed Oxide by Inductively Coupled Plasma Mass Spectrometry

    • 摘要: 建立了应用电感耦合等离子体质谱(ICP-MS)测定铀铌混合氧化物中痕量的稀土元素(Sm、Eu、Gd、Dy)的方法。这四种稀土元素在核燃料中的含量在10-7g/g以下,但热中子截面很大,准确测定其在核燃料中的含量对于核燃料的研究至关重要。样品经HNO3-HF快速溶解后,应用CL-TBP萃淋树脂分离U基体,以115In作为测定内标校正基体干扰和仪器漂移,标准模式下应用ICP-MS定量测定淋洗液中Sm、Eu、Gd和Dy,半定量分析基体U。四种稀土元素的质量浓度为0.01~1.00 μg/L,线性关系良好,线性相关系数(r)均大于0.999,检出限为0.001~0.002 μg/L。对于添加0.2 μg/L的稀土元素,稀土元素的回收率为84.3%~97.3%,相对标准偏差(sr)为5.3%~8.7%(n=6),能够满足实际样品测定需要。

       

      Abstract: A method was developed for determination of trace rare earth elements ( Sm, Eu, Gd and Dy ) in U-Nb mixed oxide using inductively coupled plasma mass spectrometry (ICP-MS). Though the contents of these four rare earth elements in nuclear fuel are below 10-7g/g, the accurate determination of their contents in nuclear fuel is crucially important to the research of nuclear fuel for their thermal neutron-absorption cross-sections are large. After the sample was dissolved fast by HNO3-HF acids, U matrix was separated using CL-TBP extraction resin. 115In was used as internal standard to correct matrix interference and instrument drift for quantitative determination of Sm, Eu, Gd and Dy in eluate, semi-quantitative determination of U in eluate by ICP-MS. The method has a good linear correlation (r>0.999) in the range of 0.01-1.00μg/L and the detection limit is between 0.001-0.002 μg/L. For the add concentrations of rare earth elements is 0.2 μg/L, the recovery is between 84.3%-97.3% and the relative standard deviation (sr) is between 5.3%-8.7% (n=6). The method can be available in practical application.

       

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