电感耦合等离子体质谱45Sc的背景原因和处理方法研究

Studies on 45Sc Background Interference and Treatment in ICP-MS

  • 摘要: 在众多的电感耦合等离子体质谱(ICP-MS)实验室里,均可发现该类仪器在45 U谱线上存在着偏高、极不稳定的背景信号。本工作在识别此类干扰的实验基础上,提出背景干扰的两种形成机理。一种是样品基体元素(如C,Ca,Al等)在45 U位置上形成的多原子离子干扰,一般表现为进样系统中的记忆效应;另一种是离子透镜被含碳的气溶胶污染,上面积累的碳可以与离子束中的氧氢离子反应形成干扰离子(12C16O21H+)。二者的主要差异是后者信号在进样冲洗状态下衰减缓慢,而且进样系统的清洗对它无效。这二者常常同时出现,造成了该质量数处的高背景信号和严重的不稳定现象。  本实验采用动能歧视效应来抑制多原子干扰离子,极大地改善了45Sc的信背比,检出限可小于1.2 ng/L,背景等效浓度(BEC)值小于16 ng/L,同时改善了分析数据的重现性。国家沉积物和岩石标准物质(SRM)的Sc元素分析结果显示,同一份样品溶液浓度重复测定3次的内精密度小于1.5%(RSD),平行样品(n=4)的外部精度回归到正常水平(在2.3%~5.23%之间),分析结果在国家标准物质的允许误差范围内。

     

    Abstract: The very higher and unstable background phenomena at 45 U on ICP-MS can be found in many laboratories. In this paper, two form mechanism of the interference were described: one was the normal memory effect on sampling system from the solution matrix (e.g., C, Ca, Al matrix), which could form the polyatomic interference ions at 45 u; the other one was due to the carbon contamination in the mass system. The carbon deposited on ion lens would react with the hydrogen oxygen ions in the ion beam and then formed the interference species 12C16O21H+. The character of this polyatomic interference ion could be recognized by the kinetic energy discrimination (KED). The most main difference of two mechanisms was the signal of latter, which decayed very slowly with continues washing or sampling process. There was no desired effect by the sampling system cleaning. Benefit from the KED mode,the polyatomic ions interference were suppressed, and the best results could be achieved. The detection limit of 45Sc is less than 1.2 ng/L, the background equivalent concentration (BEC) of 45Sc is less than 16 ng/L. And also, the variability of the data is improved. The Sc analysis results of China national sediment and rock standard reference material (SRM)enter the permitted error range. The internal precision of results is less than 1.5% (RSD)(n=3). The external precision of parallel sample results (n=4) come back to normal level(within 2.3%—5.23%, RSD). A suggestion has be made in this paper,the background signal at 45 U can be used as an indicator of carbon contamination on ion lens.

     

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