Homeland security relies heavily on analytical chemistry to identify suspicious materials and persons. Traditionally this role has focused on attribution, determining the type and origin of an explosive, for example. But as technology advances, analytical chemistry can and will play an important role in the prevention and preemption of terrorist attacks. More sensitive and selective detection techniques can allow suspicious materials and persons to be identified even before a final destructive product is made. The work presented herein focuses on the use of commercial and novel detection techniques for application to the prevention of terrorist activities. Although drugs are not commonly thought of when discussing terrorism, narcoterrorism has become a significant threat in the 21st century. The role of the drug trade in the funding of terrorist groups is prevalent; thus, reducing the trafficking of illegal drugs can play a role in the prevention of terrorism by cutting off much needed funding. To do so, sensitive, specific, and robust analytical equipment is needed to quickly identify a suspected drug sample no matter what matrix it is in. Single Particle Aerosol Mass Spectrometry (SPAMS) is a novel technique that has previously been applied to biological and chemical detection. The current work applies SPAMS to drug analysis, identifying the active ingredients in single component, multi-component, and multi-tablet drug samples in a relatively non-destructive manner. In order to do so, a sampling apparatus was created to allow particle generation from drug tablets with on-line introduction to the SPAMS instrument. Rules trees were developed to automate the identification of drug samples on a single particle basis. A novel analytical scheme was also developed to identify suspect individuals based on chemical signatures in human breath. Human breath was sampled using an RTube{trademark} and the trace volatile organic compounds (VOCs) were preconcentrated using solid phase microextraction (SPME) and identified using gas chromatography - mass spectrometry (GC-MS). Modifications to the sampling apparatus allowed for increased VOC collection efficiency, and reduced the time of sampling and analysis by over 25%. The VOCs are present in breath due to either endogenous production, or exposure to an external source through absorption, inhalation, or ingestion. Detection of these exogenous chemicals can provide information on the prior location and activities of the subject. Breath samples collected before and after exposure in a hardware store and nail salon were analyzed to investigate the prior location of a subject; breath samples collected before and after oral exposure to terpenes and terpenoid compounds, pseudoephedrine, and inhalation exposure to hexamine and other explosive related compounds were analyzed to investigate the prior activity of a subject. The elimination of such compounds from the body was also monitored. In application, this technique may provide an early warning system to identify persons of interest in the prevention and preemption stages of homeland security.
