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Forensic Sci Int. 2020 Feb;307:110102. doi: 10.1016/j.forsciint.2019.110102. Epub 2019 Dec 19.

Chemical attribution of the home-made explosive ETN - Part I: Liquid chromatography-mass spectrometry analysis of partially nitrated erythritol impurities.

Forensic science international

Karlijn Bezemer, Lindsay McLennan, Lara van Duin, Chris-Jan Kuijpers, Mattijs Koeberg, Jos van den Elshout, Antoine van der Heijden, Taylor Busby, Alexander Yevdokimov, Peter Schoenmakers, James Smith, Jimmie Oxley, Arian van Asten

Affiliations

  1. Van 't Hoff Institute for Molecular Sciences, Faculty of Science, Amsterdam University of Amsterdam, the Netherlands; Netherlands Forensic Institute, The Hague, the Netherlands. Electronic address: [email protected].
  2. University of Rhode Island, Department of Chemistry, Kingston, RI, USA.
  3. Van 't Hoff Institute for Molecular Sciences, Faculty of Science, Amsterdam University of Amsterdam, the Netherlands.
  4. Netherlands Forensic Institute, The Hague, the Netherlands.
  5. Dept. Energetic Materials, TNO Technical Sciences, Den Haag, the Netherlands.
  6. Van 't Hoff Institute for Molecular Sciences, Faculty of Science, Amsterdam University of Amsterdam, the Netherlands; CLHC, Amsterdam Center for Forensic Science and Medicine, University of Amsterdam, P.O. Box 94157, 1090 GD Amsterdam, the Netherlands.

PMID: 31884003 DOI: 10.1016/j.forsciint.2019.110102

Abstract

Erythritol tetranitrate (ETN) was prepared independently by two research groups from the USA and the Netherlands. The partially nitrated impurities present in ETN were studied using liquid chromatography-mass spectrometry to address the ultimate challenge in forensic explosives investigations, i.e., providing chemical and tactical information on the production and origin of the explosive material found at a crime scene. Accurate quantification of the tri-nitrated byproduct erythritol trinitrate (ETriN) was achieved by in-lab production of an ETriN standard and using custom-made standards of the two isomers of ETriN (1,2,3-ETriN and 1,2,4-ETriN). Large differences in levels of ETriN were observed between the two sample sets showing that, even when similar synthesis routes are employed, batches from different production locations can contain different impurity profiles. In one of the sample sets the ratios of the lesser partially nitrated impurities, EDiN and EMN, in the ETN samples could be determined. The impurity profiles enable prediction of post-synthesis work-up steps by reduction of the level of partially nitrated products upon recrystallization. However, impurity analysis does not enable predictions with respect to raw material or synthesis route used. Nonetheless, characteristic impurity profiles obtained can be used in forensic casework to differentiate or link ETN samples. However, forensic interpretation can be complicated by acid catalyzed degradation which can cause changes in impurity levels over time. The high food-grade quality of the erythritol precursor materials did not provide other impurity markers using the LC-MS methods in this study. To expand our framework of chemical attribution a follow-up study will be reported that focuses on stable isotope analysis of ETN and its precursor materials that potentially allow predictions for forensic explosives intelligence.

Copyright © 2019 Elsevier B.V. All rights reserved.

Keywords: Attribution; Chemical profiling; Erythritol tetranitrate (ETN); Explosives; Forensic science; Liquid chromatography-mass spectrometry (LC–MS)

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