Ratification of the Chemical Weapons Convention by more than 165 States Parties has reduced the risk of chemical warfare agent use, but there still remains a concern that other parties may make use of these weapons against civilian or military targets. Concerns within the defense and homeland security communities over possible terrorist use as well as the requirements for a verifiable Chemical Weapons Convention have driven the development of analytical methods such as liquid chromatography-mass spectrometry (LC-MS) for the detection and identification of chemical warfare agents. This paper provides a general overview of chemical warfare agents and analytical methods for their analysis, a focused review of LC-MS applications, a summary of in-house LC-MS methods developed at DRDC Suffield, and a comprehensive bibliography of analytical open literature papers dealing with chemical warfare agent detection and identification. The review sections provide the homeland security and defense communities with an overview of chemical warfare agents and analytical methods for their determination. Researchers interested in developing new methods for chemical warfare agents may use the reviewed material to quickly ascertain the state of development of analytical methods, in particular LC-MS methods, for chemical warfare agents. The reviewed materials will be used for reference purposes during the development of high field asymmetric waveform ion mobility spectrometry (FAIMS) mass spectrometry, a new analytical technique with the potential to rapidly separate and identify chemical warfare agents. The report concludes with 67 references. Appendix A is a 454-item bibliography of open literature analytical methods for the detection and identification of chemical warfare agents, their degradation products, and related compounds. Paper copies of each paper are held at DRDC Suffield and this comprehensive database of methods continues to be updated regularly using Procite software.

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. Linear results were achieved for the detection of diisopropylamine (DIPA) by SPME-GC-MS in soil from 0.72 - 3584.5 micrograms DIPA/g soil and in DI water from 0.018 - 17.9 microgram/milliliter. 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.

The threat of biological and chemical terrorism has driven the demand for timely techniques that can quickly detect the agent or agents used in an attack. The detection and/or prevention of these potential security threats provide significant scientific and technical challenges due to the combination of possible agents and modes of delivery available. This book will present a thorough look at the importance and technological challenges of mass spectrometry (MS) for the detection & identification of biological and chemical threats. This new contribution’s general aims are to draw the attention of recognized practitioners, experts and graduate students trying to grasp the latest MS developments in the cutting-edge fields of MS-biodefense technologies for the rapid/early/specific sensitive threat detection of pathogens, viruses, explosives, mycotoxins, chemical agents, and biological markers of xenobiotic chemicals.

As part of a study on the role of natural organics in determining the physical properties of soils, the use of combined gas chromatographic/mass spectrometric methods for identification of the more volatile organic chemicals in soils were explored. Soil was first treated at 100, 150, and 200C to select the optimum temperature where minimum pyrolysis of soil organic matter occurred. The vapors from three soils heated in a closed system at 150C were then analyzed. Subsequent refinement in technique involved collection of vapor from the three soils maintained at 150C using a constant flow sample holder/inlet system. About 50 organic compounds were identified. While application of this approach is restricted to the volatile compounds in the lower molecular weight range, conditions of analysis are thought to be suitable for identification of compounds originally present as opposed to pyrolysis products of soil organic matter. (Author).