Chemical Sciences Division, Material Measurement Laboratory, National Institute of Standards and Technology, Gaithersburg, MD 20899, USA.
Anal Chim Acta. 2013 Sep 2;793:72-8. doi: 10.1016/j.aca.2013.07.031. Epub 2013 Jul 16.
Quantitative analysis using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) remains challenging primarily due to the lack of appropriate reference materials available for the wide variety of samples of interest and to elemental fractionation effects. Isotopic dilution mass spectrometry (IDMS) is becoming the methodology of choice to address these issues because the different isotopes of an element represent near-perfect internal standards. In this work, we investigated the lithium borate fusion of powdered solid samples, including soils, sediments, rock mine waste and a meteorite, as a strategy to homogenously distribute, i.e. equilibrate the elements and the added isotopically enriched standards. A comparison of this methodology using two pulsed laser ablation systems (ArF* excimer and Nd:YAG) with different wavelengths as well as two ICP-MS instruments (quadrupole and double-focusing sector field) was performed. Emphasis was put on using standard equipment to show the potential of the proposed strategy for its application in routine laboratories. Cr, Zn, Ba, Sr and Pb were successfully determined by LA-ICP-IDMS in six Standard Reference Materials (SRMs) representing different matrices of environmental interest. Experimental results showed the SRM fused glasses exhibited a low level of heterogeneity (intra- and inter-sample) for both natural abundance and isotopically enriched samples (RSD <3%, n=3, 1σ). A good agreement between experimental results and the certified values was also observed.
基于激光烧蚀电感耦合等离子体质谱法(LA-ICP-MS)的定量分析主要面临两个挑战:缺乏适用于各种感兴趣样品的标准物质,以及元素分馏效应。同位素稀释质谱法(IDMS)正成为解决这些问题的首选方法,因为元素的不同同位素代表近乎完美的内标。在这项工作中,我们研究了粉末状固体样品(包括土壤、沉积物、岩石矿渣和陨石)的硼酸锂熔融,作为一种均匀分布的策略,即平衡元素和添加的同位素富集标准品。我们比较了两种具有不同波长的脉冲激光烧蚀系统(ArF*准分子和 Nd:YAG)以及两种 ICP-MS 仪器(四极杆和双聚焦扇形场)的这种方法。我们强调使用标准设备来展示所提出策略的应用潜力,以使其在常规实验室中得到应用。通过 LA-ICP-IDMS,成功地测定了六种代表不同环境基质的标准参考物质(SRMs)中的 Cr、Zn、Ba、Sr 和 Pb。实验结果表明,熔融玻璃对于天然丰度和同位素富集的样品均表现出较低的异质性(内标和样品间)(RSD<3%,n=3,1σ)。实验结果与认证值之间也存在良好的一致性。