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Application of solid phase microextraction with gas chromatography-mass spectrometry as a rapid, reliable, and safe method for field sampling and analysis of chemical warfare agent precursors /

by Parrish, Douglas K.

Abstract (Summary)
Title of Dissertation: “Application of Solid Phase Microextraction with Gas Chromatography-Mass Spectrometry as a Rapid, Reliable, and Safe Method for Field Sampling and Analysis of Chemical Warfare Agent Precursors” Author: LT Douglas K. Parrish, MSC USN Doctor of Philosophy in Environmental Health Sciences Dissertation Advisor: CDR Gary L. Hook, PhD, MPH, MSC USN Assistant Professor Department of Preventive Medicine and Biometrics Solid phase microextraction was combined with gas chromatography-mass spectrometry (SPME-GC-MS) for detection of hydrogen cyanide (HCN) in the headspace above deionized (DI) water samples, with linear results that were sensitive to below Department of Defense short-term drinking water standards. HCN and several common volatile organic contaminants were also detected in 3 water types in a laboratory and field setting. The method provides an advantage over the standard drinking water detection methods for HCN as it can also simultaneously detect common low molecular weight hydrocarbons. iii Linear results were achieved for the detection of diisopropylamine (DIPA) by SPME-GC-MS in soil from 0.72 - 3584.5 µg DIPA/g soil and in DI water from 0.018 - 17.9 µg/mL. The methods were successfully field tested with common hydrocarbon contaminants in 3 common agricultural soil types and 3 water types. In particular, this methodology would be useful for investigation of a suspected VX nerve agent production facility. Solid phase dynamic extraction (SPDE) was compared to passive SPME for vapor sampling of DIPA and dimethyl methylphosphonate (DMMP) with analysis by fast GC- MS. Equilibrium sampling by SPDE for DIPA and DMMP vapor provided linear results at lower concentrations and gave larger extracted ion peak areas than comparable SPME sampling. This unique application has shown great potential for further laboratory and field use, both for health risk assessment and initial chemical detection employment. A fast GC capillary column was integrated with a novel low pressure, quadrupole ion trap, time-of-flight photoionization mass spectrometer (Qit Tof PI-MS). The addition of a GC injection port and column allowed the use of SPME to provide headspace extraction of several chemical warfare agent (CWA) precursors for introduction to this GC/PI-MS. This prototype instrumentation was shown to be able to detect CWA precursor vapors in air individually and in mixtures. The central research goal was to develop the ability to rapidly detect CWA precursors in a field setting. The greatest benefit to using these SPME-GC-MS methods is they allow unambiguous detection and identification of CWA precursors as well as common environmental contaminants. These detection methods are applicable to the military environmental scientist as well as homeland defense and hazardous material iv detection personnel. Identification of environmental chemicals is the first step in assessing military deployment exposures and health risks. v
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School:Uniformed Services University of the Health Sciences

School Location:USA - Maryland

Source Type:Master's Thesis

Keywords:polymers phosphorylation hydrolysis chemistry analytical environmental monitoring exposure time factors soil pollutants water supply osmolar concentration sensitivity and specificity occupational health disaster planning risk assessment specimen handling war terrorism national security hydrogen cyanide chemical warfare agents organophosphorus compounds chromatography gas mass fragmentography

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