International Forensic Research Institute, Florida International University, OE116 11200 SW 8th St, Miami, FL 33199, USA.
Anal Bioanal Chem. 2013 Jun;405(16):5393-409. doi: 10.1007/s00216-013-6978-y. Epub 2013 May 15.
Elemental analysis of glass was conducted by 16 forensic science laboratories, providing a direct comparison between three analytical methods [micro-x-ray fluorescence spectroscopy (μ-XRF), solution analysis using inductively coupled plasma mass spectrometry (ICP-MS), and laser ablation inductively coupled plasma mass spectrometry]. Interlaboratory studies using glass standard reference materials and other glass samples were designed to (a) evaluate the analytical performance between different laboratories using the same method, (b) evaluate the analytical performance of the different methods, (c) evaluate the capabilities of the methods to correctly associate glass that originated from the same source and to correctly discriminate glass samples that do not share the same source, and (d) standardize the methods of analysis and interpretation of results. Reference materials NIST 612, NIST 1831, FGS 1, and FGS 2 were employed to cross-validate these sensitive techniques and to optimize and standardize the analytical protocols. The resulting figures of merit for the ICP-MS methods include repeatability better than 5% RSD, reproducibility between laboratories better than 10% RSD, bias better than 10%, and limits of detection between 0.03 and 9 μg g(-1) for the majority of the elements monitored. The figures of merit for the μ-XRF methods include repeatability better than 11% RSD, reproducibility between laboratories after normalization of the data better than 16% RSD, and limits of detection between 5.8 and 7,400 μg g(-1). The results from this study also compare the analytical performance of different forensic science laboratories conducting elemental analysis of glass evidence fragments using the three analytical methods.
采用三种分析方法（微束 X 射线荧光光谱法（μ-XRF）、电感耦合等离子体质谱法（ICP-MS）溶液分析和激光烧蚀电感耦合等离子体质谱法）对玻璃进行了元素分析，由 16 个法医学实验室进行，可对这三种方法进行直接比较。使用玻璃标准参考物质和其他玻璃样品设计了实验室间研究，以（a）评估使用相同方法的不同实验室之间的分析性能，（b）评估不同方法的分析性能，（c）评估这些方法正确关联源自同一来源的玻璃以及正确区分不具有相同来源的玻璃样品的能力，以及（d）使分析方法和结果解释标准化。采用 NIST 612、NIST 1831、FGS 1 和 FGS 2 标准参考物质来交叉验证这些灵敏技术，并优化和标准化分析方案。ICP-MS 方法的主要性能指标包括重复性优于 5%RSD、实验室间再现性优于 10%RSD、偏差优于 10%以及大多数监测元素的检出限介于 0.03 和 9μg/g 之间。μ-XRF 方法的主要性能指标包括重复性优于 11%RSD、数据归一化后实验室间再现性优于 16%RSD 以及检出限介于 5.8 和 7400μg/g 之间。该研究的结果还比较了使用三种分析方法对玻璃证据碎片进行元素分析的不同法医学实验室的分析性能。
