Analytical and Bioanalytical Chemistry

, Volume 405, Issue 16, pp 5393–5409 | Cite as

Cross-validation and evaluation of the performance of methods for the elemental analysis of forensic glass by μ-XRF, ICP-MS, and LA-ICP-MS

  • Tatiana Trejos
  • Robert Koons
  • Stefan Becker
  • Ted Berman
  • JoAnn Buscaglia
  • Marc Duecking
  • Tiffany Eckert-Lumsdon
  • Troy Ernst
  • Christopher Hanlon
  • Alex Heydon
  • Kim Mooney
  • Randall Nelson
  • Kristine Olsson
  • Christopher Palenik
  • Edward Chip Pollock
  • David Rudell
  • Scott Ryland
  • Anamary Tarifa
  • Melissa Valadez
  • Peter Weis
  • Jose Almirall
Research Paper


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.


Elemental analysis Forensic Glass X-ray fluorescence ICP-MS Laser ablation ICP-MS 



This project was supported by Award No. 2010-DN-BX-K179 from the National Institute of Justice, Office of Justice Programs, U.S. Department of Justice. The opinions, findings, and conclusions or recommendations expressed in this presentation are those of the authors and do not necessarily reflect those of the Department of Justice, the Department of the Army or the Department of Defense. Thanks to all of the Elemental Analysis Working Group members and their agencies for devoting the time necessary to complete this project. This is publication number 12–14 of the FBI Laboratory Division. Names of commercial manufacturers are provided for identification purposes only, and inclusion does not imply endorsement of the manufacturer, or its products or services by the FBI. The views expressed are those of the authors and do not necessarily reflect the official policy or position of the FBI or the U.S. Government.


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Copyright information

© Springer-Verlag Berlin Heidelberg 2013

Authors and Affiliations

  • Tatiana Trejos
    • 1
  • Robert Koons
    • 2
  • Stefan Becker
    • 3
  • Ted Berman
    • 4
  • JoAnn Buscaglia
    • 2
  • Marc Duecking
    • 3
  • Tiffany Eckert-Lumsdon
    • 5
  • Troy Ernst
    • 6
  • Christopher Hanlon
    • 7
  • Alex Heydon
    • 8
  • Kim Mooney
    • 5
  • Randall Nelson
    • 9
  • Kristine Olsson
    • 10
  • Christopher Palenik
    • 11
  • Edward Chip Pollock
    • 12
  • David Rudell
    • 8
  • Scott Ryland
    • 4
  • Anamary Tarifa
    • 1
  • Melissa Valadez
    • 13
  • Peter Weis
    • 3
  • Jose Almirall
    • 1
    • 14
  1. 1.International Forensic Research InstituteFlorida International UniversityMiamiUSA
  2. 2.Federal Bureau of Investigation, Laboratory DivisionCounterterrorism and Forensic Science Research UnitQuanticoUSA
  3. 3.Bundeskriminalamt (BKA)Forensic Science InstituteWiesbadenGermany
  4. 4.Florida Department of Law EnforcementOrlando Regional Operations CenterOrlandoUSA
  5. 5.US Army Criminal Investigation LaboratoryForest ParkUSA
  6. 6.Michigan State Police-Grand Rapids LaboratoryGrand RapidsUSA
  7. 7.Miami Dade Police DepartmentForensic Science Services BureauMiamiUSA
  8. 8.Center of Forensic SciencesTorontoCanada
  9. 9.Tennessee Bureau of InvestigationForensic Services DivisionNashvilleUSA
  10. 10.Johnson County Sheriff’s Office Crime LaboratorySunset OlatheUSA
  11. 11.Microtrace LLCElginUSA
  12. 12.Sacramento County District Attorney’s OfficeLaboratory of Forensic ServicesSacramentoUSA
  13. 13.Texas Department of Public Safety Crime LaboratoryAustinUSA
  14. 14.Department of Chemistry and BiochemistryFlorida International UniversityMiamiUSA

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