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Forensic Analysis of C-4 and Commercial Blasting Agents for Possible Discrimination

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Forensic Analysis of C-4 and Commercial Blasting Agents for Possible Discrimination University of Central Florida STARS Electronic Theses and Dissertations, 2004-2019 2007 Forensic Analysis Of C-4 And Commercial Blasting Agents For Possible Discrimination Katie Steele University of Central Florida Part of the Chemistry Commons, and the Forensic Science and Technology Commons Find similar works at: https://stars.library.ucf.edu/etd University of Central Florida Libraries http://library.ucf.edu This Masters Thesis (Open Access) is brought to you for free and open access by STARS. It has been accepted for inclusion in Electronic Theses and Dissertations, 2004-2019 by an authorized administrator of STARS. For more information, please contact [email protected]. STARS Citation Steele, Katie, "Forensic Analysis Of C-4 And Commercial Blasting Agents For Possible Discrimination" (2007). Electronic Theses and Dissertations, 2004-2019. 3364. https://stars.library.ucf.edu/etd/3364 FORENSIC ANALYSIS OF C-4 AND COMMERCIAL BLASTING AGENTS FOR POSSIBLE DISCRIMINATION by KATIE L. STEELE B.S. University of Central Florida, 2005 A thesis submitted in partial fulfillment of the requirements for the degree of Master of Science in the Department of Chemistry in the College of Sciences at the University of Central Florida Orlando, Florida Summer Term 2007 © 2007 Katie Steele ii ABSTRACT The criminal use of explosives has increased in recent years. Political instability and the wide spread access to the internet, filled with “homemade recipes,” are two conjectures for the increase. C-4 is a plastic bonded explosive (PBX) comprised of 91% of the high explosive RDX, 1.6% processing oils, 5.3% plasticizer, and 2.1% polyisobutylene (PIB). C-4 is most commonly used for military purposes, but also has found use in commercial industry as well. Current methods for the forensic analysis of C-4 are limited to identification of the explosive; however, recent publications have suggested the plausibility of discrimination between C-4 samples based upon the processing oils and stable isotope ratios. This research focuses on the discrimination of C-4 samples based on ratios of RDX to HMX, a common impurity resulting from RDX synthesis. The relative amounts of HMX are a function of the RDX synthetic route and conditions. RDX was extracted from different C-4 samples and was analyzed by ESI-MS-SIM as the chloride adduct, EI-GC-MS-SIM, and NICI-GC-MS. Ratios (RDX/HMX) were calculated for each method. An analysis of variance (ANOVA) followed by a Tukey HSD allowed for an overall discriminating power to be assessed for each analytical method. The C-4 processing oils were also extracted, and analyzed by direct exposure probe mass spectrometry (DEP-MS) with electron ionization, a technique that requires less than two minutes for analysis. The overall discriminating power of the processing oils was calculated by conducting a series of t tests. Lastly, a set of heterogeneous commercial blasting agents were analyzed by laser induced breakdown spectroscopy (LIBS). The data was analyzed by principal components analysis (PCA), and the possibility of creating a searchable library was explored. iii To my husband, my best friend “It is for your own happiness that you need the person you love and that the greatest compliment, the greatest tribute you can pay to that person.” -Ayn Rand iv ACKNOWLEDGMENTS There are many people to whom I owe a great debt of gratitude. I would first like to thank Candice Bridge, my favorite Jersey girl, for her invaluable help with all of my Excel spreadsheets. Thank you for all of your help, and for keeping me up to date on “current events.” Jen Molina, my “Powerpoint expert,” thank you for always helping me out when I needed it the most! I would be remiss if I did not thank Derek Dorrien for demonstrating “what-not-to-do” when submitting a thesis. It always helps to have someone make your mistakes for you. I want to thank Sara “Blinker” Linker, my 180° counterpart, for always helping me to see the other side, the gray side. Aloha! I want to send a special thank you to Joe Castelbuono for always letting me know when it was 3pm. I shudder to think where I would be without Jessica Frisch the “Paint expert.” I have to say thank you to both Jessica and Erin McIntee for always laughing at my jokes, even when they were underwhelming. A great deal of thanks goes out to the “adults,” Mary Williams and Doug Clark. Mary, thank you for all of you help and support. You are the glue that keeps us all together! Doug, thank you for all of your help, you are going to miss me when I am gone, I am sure of it! Sincere thanks to Major Ron McCardle from the Florida State Fire Marshal’s office in Havana, Fl for donating C-4 samples. Last, and definitely not least, Dr. Sigman, thank you so much for all of your help and support. I appreciate it more than you know! v TABLE OF CONTENTS LIST OF FIGURES ................................................................................................................... xi LIST OF TABLES ................................................................................................................... xiv LIST OF ACRONYMS ........................................................................................................... xvi CHAPTER 1: BACKGROUND ................................................................................................. 1 Introduction ............................................................................................................................. 1 Blackpowder ........................................................................................................................... 2 Military Explosives ................................................................................................................. 3 Plastic Bonded Explosives ...................................................................................................... 3 RDX and HMX Synthesis ................................................................................................... 4 Herz/Hale Method ........................................................................................................... 9 Woolwich Method ........................................................................................................ 10 Bachmann Method ........................................................................................................ 11 Brockman Method ........................................................................................................ 12 Summary of RDX synthesis.......................................................................................... 14 Commercial Explosives ........................................................................................................ 14 Ammonium Nitrate Fuel Oil (ANFO) .............................................................................. 15 Slurry Explosives .............................................................................................................. 16 Emulsion Explosives ......................................................................................................... 17 Forensic Importance.............................................................................................................. 19 CHAPTER 2: PREVIOUS METHODS FOR ANALYSIS OF C-4 ......................................... 22 Identification of C-4 .............................................................................................................. 22 vi Infrared Spectroscopy ....................................................................................................... 22 Direct Exposure Probe Mass Spectrometry ...................................................................... 23 Differentiation of C-4 ........................................................................................................... 23 Processing Oils.................................................................................................................. 23 Stable Isotopes .................................................................................................................. 24 What Makes This Work Different ........................................................................................ 25 Ratios of RDX and HMX ................................................................................................. 25 Processing Oils.................................................................................................................. 26 Statistical Approach .......................................................................................................... 27 One-way ANOVA ........................................................................................................ 27 Principal Component Analysis (PCA) .......................................................................... 29 Comparison of Two Experimental Means by t Test ..................................................... 30 CHAPTER 3: EXTRACTION METHODS ............................................................................. 32 Samples ................................................................................................................................. 32 Extraction Scheme ................................................................................................................ 32 RDX Extraction ................................................................................................................ 34 Process Oils Extraction ....................................................................................................
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