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Differentiation of Ignitable Liquids in Fire Debris Using Solid-Phase

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Differentiation of Ignitable Liquids in Fire Debris Using Solid-Phase Differentiation of Ignitable Liquids in Fire Debris Using Solid-Phase Microextraction Paired with Gas Chromatography-Mass Spectroscopy and Chemometric Analysis A Thesis Presented to The Honors Tutorial College Ohio University In partial Fulfillment of the Requirements for Graduation from the Honors Tutorial College With the degree of Bachelor of Science in Chemistry By Amanda McKeon May 2019 Abstract: A method for testing fire debris to identify common ignitable liquids present in fire debris samples is proposed. The sampling method used is solid-phase microextraction paired with gas chromatography-mass spectrometry. The data was analyzed using principal component analysis and linear discriminant analysis. This method was successfully implemented to classify burned carpet samples as belonging to one of three classes: carpet samples with no ignitable liquids present, carpet samples with gasoline present, and carpet samples with diesel fuel present. This thesis has been approved by The Honors Tutorial College and the Department of Chemistry and Biochemistry at Ohio University __________________________________________ Dr. Peter de B. Harrington Professor, Chemistry Thesis Advisor __________________________________________ Dr. Lauren McMills Director of Studies, Chemistry __________________________________________ Cary Frith Interim Dean, Honors Tutorial College Table of Contents Introduction 1 Chapter 1: Challenges of Classification 4 Chapter 2: Methods of Extraction and Concentration 10 Chapter 3: Analytical Instruments 16 Chapter 4: Chemometric Analysis 22 Chapter 5: Research Project 28 Conclusion and Acknowledgements 48 Figure Description Example of Random Scission Showing the Breakdown of Polyethylene As Shown in Stauffer’s Paper 1 Concept of Pyrolysis for Fire Debris Analysis Example of Side Group Scission Showing the Breakdown of Polyvinyl Chloride As Shown in Stauffer’s 2 Paper Concept of Pyrolysis for Fire Debris Analysis Example of Monomer Reversion Showing the Breakdown of Polymethacrylate As Shown in Stauffer’s Paper 3 Concept of Pyrolysis for Fire Debris Analysis Diagram of a) A Commercial SPME Syringe Setup b) A Close-Up Cross-Sectional View of the Adjustable 4 Depth Gauge 5 Diagram of a Gas Chromatograph-Mass Spectrometer A Two-Dimensional Data Set, Including Its Two Principal Components, As Seen in Vidal et al.’s 2016 Book 6 Generalized Principal Component Analysis 7 A Score Plot Between Principal Components 1 and 2 From a Set of Data Obtained by Monfreda and Gregori 8 Total Ion Chromatograms of Diesel Samples 9 Total Ion Chromatograms of Gasoline Samples 10 Average Mass Spectra of Diesel Fuel Samples 11 Average Mass Spectra of Gasoline Samples 12 Total Ion Chromatograms of Class A 13 Total Ion Chromatograms of Class B 14 Total Ion Chromatograms of Class C 15 Total Ion Chromatograms of Class D 16 Total Ion Chromatograms of Class E 17 Total Ion Chromatograms of Class F 18 Total Ion Chromatograms of Class G 19 Total Ion Chromatograms of Class H 20 Total Ion Chromatograms of Class I 21 Total Ion Chromatograms of Class J 22 Total Ion Chromatograms of Class K 23 Total Ion Chromatograms of Class L 24 Total Ion Chromatograms of Class M 25 Total Ion Chromatograms of Class N 26 Total Ion Chromatograms of Class O 27 Total Ion Chromatograms of Class P 28 Total Ion Chromatograms of Class Q 29 Total Ion Chromatograms of Class R 30 Total Ion Chromatograms of Class S 31 Total Ion Chromatograms of Class T 32 Total Ion Chromatograms of Class U 33 Total Ion Chromatograms of Class V 34 Total Ion Chromatograms of Class W 35 Two-Way Representation of the Average Diesel Fuel Data 36 Two-Way Representation of the Average Gasoline Data 37 PCA Score Plot of the Three-Way Chromatographic and Spectral Data 38 PCA Score Plot of TIC Data 39 PCA Score Plot of Mass Spectral Data 40 Linear Discriminant Score Plot of the Combined TIC and Mass Spectral Data Table Description 1 Legend of Class Letters 1 Introduction Since at least the nineteen-fifties, it has been accepted that arson is one of the most dangerous and destructive crimes to be committed. As Wakefield pointed out in his 1951 publication, “it is a weapon for murder, robbery, assault, fraud, revenge, spite, and, when completed, has destroyed in many cases the evidence that it was even committed.”1 The history of chemical fire debris analysis is a relatively short one. While there are several papers on arson investigation published in the 1950’s,1–5 the first paper that discussed the detection of trace amounts of fire accelerant was not published until 1960.6 As Burd explains in this paper, “While fire investigators can frequently detect that flammable liquids were used or could have been used at a fire scene, they frequently encounter difficulty in recovering suitable samples of debris from which the laboratory can separate identifiable amounts of the fluid employed.”6 This problem is of vital importance because, in terms of criminal justice, the case is not decided because the perpetrator has been identified. It is the job of investigators and forensic experts to provide sufficient evidence to convict the perpetrator in a court of law. Without this evidence, it is very likely that they will continue to commit crimes, thus disrupting society. Stauffer et al. defined fire debris analysis as “the science related to the examination of fire debris samples performed to detect and identify ignitable liquid residues (ILR).”7 In other words, it is the application of analytical chemistry to evidence that has been collected from the scene of a suspected arson or explosion with the intent to determine if an ignitable liquid or accelerant was used to start or increase the rate of a fire. While many people outside of the field believe that the terms “ignitable liquid” and 2 “accelerant” are synonymous, their definitions vary slightly. The main difference is that, while an ignitable liquid can be used as an accelerant, it does not have to be used as an accelerant. For example, gasoline is an ignitable liquid, but in its day-to-day use, it is not an accelerant if used for its intended purpose. An accelerant is anything that serves to increase the rate of a conflagration and can be a liquid, solid, or gas. The publications reviewed in this thesis focus on ignitable liquids that are commonly used as accelerants. Ignitable liquids can be broken down into seven main classes, as defined by the American Society of Materials and Testing (ASTM). These classes are 1) aromatic products such as xylenes and some lamp oils, 2) gasoline, 3) petroleum distillates such as kerosene and diesel fuel, 4) isoparaffinic products such as some paint thinners and mineral spirits, 5) naphthenic-paraffinic products such as industrial solvents, 6) normal alkane products such as pentane and some toners, and 7) oxygenated solvents such as alcohols and some lacquer thinners. If a sample does not meet the criteria for any of the seven categories, it is classified as miscellaneous. Additionally, all categories except gasoline can be further broken down into light, medium, or heavy subclasses, based on the number of carbon atoms per molecule.8 Samples are typically categorized by matching a chromatogram of the sample to a chromatogram of a known standard, as specified in ASTM E1618-01.9 It is important to recognize that different categories of ignitable liquid will behave differently based on their chemical compositions. For example, Fettig et al. used only two different types of ignitable liquids: gasoline and diesel fuel. While the intended uses of these two fluids are very similar, they consist of “different substances with a variety of components and different polarities.”10 Both liquids contain alkanes and alkylbenzenes, but gasoline also contains toluene, indane, and 3 xylene, while diesel fuel contains dodecane, tetradecane, and eicosane, among other compounds. Fettig et al. found that even between these two functionally similar liquids, there were differences in behavior. Because diesel fuel has components with a wider range of boiling points, a higher temperature was determined to be ideal for extraction based on data from several trials with differing extraction temperature, thus highlighting the different behaviors of the two liquids when heated. This thesis proposes and validates a method of testing fire debris analysis in suspected arson cases for the presence of ignitable liquid residues. The background of the field of fire debris analysis was thoroughly researched in order to design a suitable thesting method. This project focuses on the use of solid-phase microextraction paired with gas chromatography-mass spectrometry to collect sample data. The data was then analyzed using principal component analysis and linear discriminant analysis. All methods used are described in detail in the following chapters. 4 Chapter 1: Challenges of Classification One of the main challenges of analyzing fire debris is that, by the nature of fire itself, once the crime is complete, much of the evidence where it took place has been destroyed. In fact, one of the reasons people commit arson, as laid out by Wakefield, is to cover up evidence of another crime.1 There are several reasons that only residues from ignitable fluids would be left on fire debris, the first being the chemical makeup of the fluids. Most ignitable fluids are made up of several components, some of which are highly volatile, meaning they have very low boiling points, and therefore evaporate quickly in the heat of a fire, which is referred to as thermal weathering. Weathering is problematic because a fire debris chromatogram may have missing or attenuated peaks from the volatile compounds that are typically found in the earlier parts of the chromatogram. The fire debris chromatogram often may appear to be very different form the reference chromatogram of the pure ignitable fluid.11 Another problem that arises due to the heat of the conflagration is the phenomenon of pyrolysis.
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