Determination of basic degradation products of chemical warfare agents in water using hollow fibre-protected liquid-phase microextraction with in-situ derivatisation followed by gas chromatography–mass spectrometry

2008 ◽  
Vol 1196-1197 ◽  
pp. 125-132 ◽  
Author(s):  
Hoi Sim Nancy Lee ◽  
Mui Tiang Sng ◽  
Chanbasha Basheer ◽  
Hian Kee Lee
2017 ◽  
Vol 37 (1) ◽  
Author(s):  
Carlos A. Valdez ◽  
Roald N. Leif ◽  
Saphon Hok ◽  
Bradley R. Hart

AbstractChemical warfare agents (CWAs) are unarguably one of the most feared toxic substances produced by mankind. Their inception in conventional warfare can be traced as far back as the Middle Ages but their full breakthrough as central players in bellic conflicts was not realized until World War I. Since then, more modern CWAs along with efficient methods for their manufacture have emerged and violently shaped the way modern warfare and diplomatic relations are conducted. Owing to their mass destruction ability, counter methods to mitigate their impact appeared almost immediately on par with their development. These efforts have focused on their efficient destruction, development of medical countermeasures and their detection by modern analytical chemistry methods. The following review seeks to provide the reader with a broad introduction on their direct detection by gas chromatography-mass spectrometry (GC-MS) and the various sample derivatization methods available for the analysis of their degradation products. The review concentrates on three of the main CWA classes and includes the nerve agents, the blistering agents and lastly, the incapacitating agents. Each section begins with a brief introduction of the CWA along with discussions of reports dealing with their detection in the intact form by GC-MS. Furthermore, as products arising from their degradation carry as much importance as the agents themselves in the field of forensic analysis, the available derivatization methods of these species are presented for each CWA highlighting some examples from our lab in the Forensic Science Center at the Lawrence Livermore National Laboratory.


Author(s):  
Tomas Rozsypal

Nitrogen mustards are dangerous and available blistering chemical warfare agents. In the presented study, six derivatization methods are compared for the analysis of degradation products of the most important blistering nitrogen mustards (ethyl diethanolamine, methyl diethanolamine and triethanolamine) by gas chromatography coupled with mass spectrometry. Five silylation methods (using BSTFA and BSA) and one trifluoroacetylation method (using TFAA) were tested. The derivatization reactions were performed in acetonitrile. As the method with optimal results, trifluoroacetylation by TFAA was selected. Analytes reacted with the corresponding reagent rapidly, quantitatively, with stable kinetics and at room temperature. Calibration curves for quantitative analysis of ethanolamines after TFAA derivatization were created. Correspond-ing detection limits varied between 9?10-3 and 7?10-5 mmol?dm-3 for the tested analytes. The developed method was applied for the analysis of ethanolamines after extraction from sand using acetonitrile. Limits of detection were 11.4 to 12.3 ?g of the analyte in 1 g of sand. It is encouraged to use the developed method in military deployable laboratories designated for rapid identification of chemical warfare agents and corresponding degradation products.


Sign in / Sign up

Export Citation Format

Share Document