Fernández Beatriz, Rodríguez-González Pablo, García Alonso J Ignacio, Malherbe Julien, García-Fonseca Sergio, Pereiro Rosario, Sanz-Medel Alfredo
Department of Physical and Analytical Chemistry, Faculty of Chemistry, University of Oviedo, Julian Clavería, 8, Oviedo 33006, Spain.
Department of Physical and Analytical Chemistry, Faculty of Chemistry, University of Oviedo, Julian Clavería, 8, Oviedo 33006, Spain.
Anal Chim Acta. 2014 Dec 3;851:64-71. doi: 10.1016/j.aca.2014.08.017. Epub 2014 Aug 13.
We report on the determination of trace elements in solid samples by the combination of on-line double isotope dilution and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The proposed method requires the sequential analysis of the sample and a certified natural abundance standard by on-line IDMS using the same isotopically-enriched spike solution. In this way, the mass fraction of the analyte in the sample can be directly referred to the certified standard so the previous characterization of the spike solution is not required. To validate the procedure, Sr, Rb and Pb were determined in certified reference materials with different matrices, including silicate glasses (SRM 610, 612 and 614) and powdered samples (PACS-2, SRM 2710a, SRM 1944, SRM 2702 and SRM 2780). The analysis of powdered samples was carried out both by the preparation of pressed pellets and by lithium borate fusion. Experimental results for the analysis of powdered samples were in agreement with the certified values for all materials. Relative standard deviations in the range of 6-21% for pressed pellets and 3-21% for fused solids were obtained from n=3 independent measurements. Minimal sample preparation, data treatment and consumption of the isotopically-enriched isotopes are the main advantages of the method over previously reported approaches.
我们报告了通过在线双同位素稀释与激光烧蚀电感耦合等离子体质谱法(LA-ICP-MS)联用测定固体样品中的微量元素。所提出的方法需要使用相同的同位素富集的标样溶液,通过在线同位素稀释质谱法(IDMS)对样品和有证天然丰度标准物质进行顺序分析。通过这种方式,样品中分析物的质量分数可以直接参照有证标准物质,因此无需对标样溶液进行预先表征。为验证该方法,在具有不同基质的有证标准物质中测定了Sr、Rb和Pb,包括硅酸盐玻璃(SRM 610、612和614)以及粉末样品(PACS-2、SRM 2710a、SRM 1944、SRM 2702和SRM 2780)。粉末样品的分析通过压制片的制备和硼酸锂熔融两种方式进行。粉末样品分析的实验结果与所有物质的有证值一致。通过n = 3次独立测量,压制片的相对标准偏差在6 - 21%范围内,熔融固体的相对标准偏差在3 - 21%范围内。与先前报道的方法相比,该方法的主要优点是样品制备、数据处理简单,且同位素富集同位素的消耗量少。