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Item Advances in Solid Phase Microextraction for the Analysis of Volatile Compounds in Explosives, Tire Treatments, and Entomological Specimens(2016-05) Kranz, William D.; Goodpaster, John V.; Manicke, Nick; Sardar, Rajesh; Picard, Christine Johanna; Long, Eric C.Solid phase micro-extraction is a powerful and versatile technique, well-suited to the analysis of numerous samples of forensic interest. The exceptional sensitivity of the SPME platform, combined with its adaptability to traditional GC-MS systems and its ability to extract samples with minimal work-up, make it appropriate to applications in forensic laboratories. In a series of research projects, solid phase micro-extraction was employed for the analysis of explosives, commercial tire treatments, and entomological specimens. In the first project, the volatile organic compounds emanating from two brands of pseudo-explosive training aids for use in detector dog imprinting were determined by SPME-GC-MS, and the efficacy of these training materials was tested in live canine trials. In the second project, the headspace above various plasticizers was analyzed comparative to that of Composition C-4 in order to draw conclusions about the odor compound, 2- ethyl-1-hexnaol, with an eye toward the design of future training aids. In the third, automobile tires which had participated in professional race events were analyzed for the presence of illicit tire treatments, and in the fourth, a novel SPME-GC-MS method was developed for the analysis of blowfly (Diptera) liquid extracts. In the fifth and final project, the new method was put to the task of performing a chemotaxonomic analysis on pupa specimens, seeking to chemically characterize them according to their age, generation, and species.Item Daily Situational Brief, January 26, 2015(MESH Coalition, 1/26/2015) MESH CoalitionItem Development of Total Vaporization Solid Phase Microextraction and Its Application to Explosives and Automotive Racing(2015) Bors, Dana E.; Goodpaster, John V.; Picard, Christine Johanna; Shepson, Paul; Cooks, Graham; Long, Eric C.Pipe bombs are a common form of improvised explosive device, due in part to their ease of construction. Despite their simplistic nature, the lethality of pipe bombs should not be dismissed. Due to the risk of harm and their commonality, research into the pipe bomb deflagration process and subsequent chemical analysis is necessary. The laboratory examination of pipe bomb fragments begins with a visual examination. While this is presumptive in nature, hypotheses formed here can lead to subsequent confirmatory exams. The purpose of this study was to measure the mass and velocity of pipe bomb fragments using high speed video. These values were used to discern any trends in container type (PVC or black/galvanized steel), energetic filler (Pyrodex or double base smokeless powder), and ambient temperature (13°C and -8°C). The results show patterns based on container type, energetic filler, and temperature. The second stage of a laboratory exam is chemical analysis to identify any explosive that may be present. Legality calls for identification only, not quantitation. The purpose of this study is to quantitate the amount of explosive residue on post-blast pipe bomb fragments. By doing so, the instrumental sensitivities required for this type of analysis will be known. Additionally, a distribution of the residue will be mapped to provide insight into the deflagration process of a device. This project used a novel sampling technique called total vaporization solid phase microextraction. The method was optimized for nitroglycerin, the main energetic in double base smokeless powder. Detection limits are in the part per billion range. Results show that the concentration of residue is not uniform, and the highest concentration is located on the endcaps regardless of container type. Total vaporization solid phase microextraction was also applied to automotive racing samples of interest to the National Hot Rod Association. The purpose of this project is two-fold; safety of the race teams in the form of dragstrip adhesive consistency and monitoring in the form of fuel testing for illegal adulteration. A suite of analyses, including gas chromatography mass spectrometry, infrared spectroscopy, and evaporation rate, were developed for the testing of dragstrip adhesives. Gas chromatography mass spectrometry methods were developed for both nitromethane based fuel as well as racing gasolines. Analyses of fuel from post-race cars were able to detect evidence of adulteration. Not only was a novel technique developed and optimized, but it was successfully implemented in the analysis of two different analytes, explosive residue and racing gasoline. TV-SPME shows tremendous promise for the future in its ability to analyze a broad spectrum of analytes.Item Electroanalytical Paper-Based Sensors for In-Field Detection of Chlorate-Based Explosives and Quantification of Oxyanions(2023-05) Guimarães Vega, Carolina; Deiss, Frédérique; Manicke, Nicholas; Goodpaster, John; Long, EricImprovised explosive devices (IEDs) are a global threat due to their destructive potential, the easy access to raw materials, and online instructions to manufacture them. These circumstances have led to an increase in the number of IEDs using potassium chlorate as an oxidizer. The standard methods to detect chlorate are mainly designed for laboratory-only testing. Thus, field instrumentation capable of detecting oxidizers from explosives fuel-oxidizers is critical for crime scene investigation and counterterrorism efforts (described in Chapter 1). We developed a paper-based sensor for the in-field detection of chlorate (described in Chapter 2). The sensor is low-cost, disposable, portable, and inexpensive to fabricate, and its flexibility features allow for surface sampling without sample destruction. The sensor has an electrodeposited molybdate sensing layer, as chlorate was reported to have a catalytic effect on the molybdate reduction. The chlorate detection relies on monitoring the change in redox activity of the molybdate sensing layer using different electroanalytical techniques. We effectively demonstrated the analytical performance of the sensor (Chapter 3), obtaining a limit of detection of 1.2 mM and a limit of quantification of 4.10 mM. We evaluated the selectivity of the sensor by testing other oxidizers, such as perchlorate and nitrate, which did not present any electrochemical activity with the molybdate sensing layer. Additionally, we performed an interferent study with sugar, commonly used as fuel in IEDs, and other common white household powders such as baking soda, flour, and corn starch and neither a false positive nor a false negative result was observed (Chapter 3). As bromate has been reported to have a stronger catalytic effect than chlorate on the redox activity of molybdate, the quantification of bromate was also explored, and a bromate sensor was developed using the findings of the chlorate sensor (Chapter 4). The reaction mechanism involved in the molybdate reduction was explored and discussed in Chapter 5. The capability of the sensor in detecting chlorate from combusted samples and post-blast samples was successfully demonstrated in Chapter 6, as well as the design of encased prototypes to allow for an in-field presumptive test, storage, and transport for in-laboratory confirmatory tests and compared the performance of the sensor to the available commercial tests.Item Mapping smokeless powder residue on PVC pipe bomb fragments using total vaporization solid phase microextraction(Elsevier, 2017-07) Bors, Dana; Goodpaster, John V.; Department of Chemistry & Chemical Biology, School of ScienceQuantitating post-blast explosive residue is not a common practice in crime labs as it is typically not legally relevant. There is value in quantitation, however, if the distribution of residues on Improvised Explosive Devices (IEDs) can help guide future sample collection and/or method development. Total vaporization solid phase microextraction gas chromatography mass spectrometry (TV-SPME/GC/MS) was used to quantify residues of double-base smokeless powder (DBSP), which includes nitroglycerin (NG), diphenylamine (DPA), and ethyl centralite (EC) on post-blast PVC pipe bomb fragments. The analytical method could separate the three constituents in under 5 min with a detection limit under 1 ppb, which demonstrates high throughput while maintaining high sensitivity. The method was optimized for nitroglycerin, as it is the most indicative of DBSP. The average mass of nitroglycerin recovered from an entire PVC device was 1.0 mg. The average mass of diphenylamine recovered was much lower (24 μg) and only one device had detectable levels of EC. The typical concentration of NG on any given fragment was approximately 15–30 ppm (μg NG/g fragment). However, there was no correlation between the mass of a fragment and the mass of residue upon it. Instead, the residue was distributed such that the highest concentration of residues was found on end cap fragments.