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1.
J Am Soc Mass Spectrom ; 34(7): 1349-1358, 2023 Jul 05.
Article in English | MEDLINE | ID: mdl-37291864

ABSTRACT

Improvised explosive devices pose a threat to the public by way of terrorism and criminal activities. In the United States a commonly used low explosive in improvised explosive devices is smokeless powder (SP), due to its ease of access. Traditionally, forensic examinations are often sufficient in determining the physical and chemical characteristics of SPs. However, these exams are limited in differentiating or associating SPs when comparing two materials which are physically and/or chemically consistent. Stable isotope analysis of carbon and nitrogen has been used for explosives to further forensic chemical comparisons and aid in sample differentiation. In this manuscript we explore the utility of stable isotope analysis of SPs to differentiate manufacturer and geographic origin. Both bulk isotope analysis and component isotope analysis of carbon and nitrogen via an extraction method using dichloromethane were evaluated to compare the overall isotope signature of individual SPs. Through the combination of bulk and component isotope measurements of SPs, we were able to identify geographic relationships; however, the manufacturer origins were not as clearly discriminated. This technique demonstrates a potential improvement to traditional forensic examinations of smokeless powder by adding additional information when explosives are chemically and/or physically consistent.

2.
J Sep Sci ; 44(4): 860-869, 2021 Feb.
Article in English | MEDLINE | ID: mdl-33326145

ABSTRACT

In this study, we developed an analytical method for the determination of 1,4-dioxane in aqueous solutions using freeze-assisted liquid-liquid extraction, also known as frozen microextraction, and gas chromatography with triple quadrupole mass spectrometry with select reaction monitoring. The method is capable of quantifying 1,4-dioxane across a broad range of concentrations (1-10 000 µg/L) relevant to contaminated sites, with an instrument detection limit and method detection limit experimentally verified as 2.1 and 2.2 µg/L, respectively. In contrast to methods with similar detection limits that require 50 to 500 mL volume of sample, our method uses only 200 µL of sample. The method presented here facilitates field and laboratory applications where small sample volumes and high precision are required and could be extended to other strongly water-soluble GC-amenable analytes.

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