Current Approaches to the Derivatization of Chemical Weapon Convention-Related Alcohol for On-Site Gas Chromatographic Analysis †
Nuclear, Biological and Chemical Defence Institute, University of Defence, Vita Nejedleho 1, 68203 Vyskov, Czech Republic
†
Presented at the International Conference EcoBalt 2023 “Chemicals & Environment”, Tallinn, Estonia, 9–11 October 2023.
Proceedings 2023, 92(1), 13; https://doi.org/10.3390/proceedings2023092013
Published: 21 November 2023
(This article belongs to the Proceedings of International Conference EcoBalt 2023 "Chemicals & Environment")
The task of deployable military laboratories is to perform the fast identification of chemical warfare agents (CWAs) and related chemicals in various types of samples in field conditions. Identification is limited by the time and equipment of mobile laboratories. Polar degradation products are commonly derivatized by a procedure using N,O-Bis(trimethylsilyl)trifluoroacetamide (BSTFA) [1,2], which is time-consuming, and the resulting chromatograms often contain a number of artifacts that hinder their identification [3]. This work describes the development and optimization of an alternative trimethylsilylation (TMS) procedure for on-site identification. The goal was to develop a fast and robust method that was efficient without heating, producing clean chromatograms. The analytes were precursors and degradation products of blistering (thiodiglycol, ethyldiethanolamine, methyldiethanolamine, triethanolamine), nerve (N,N-diisopropylamino ethanol), and psychoactive (3-quinuclidinol) CWAs. Ten TMS reagents were compared in terms of their derivatization efficiency. The solvent effect, catalyst addition effect, and the time and temperature of derivatization were studied and optimized. The stability of the derivatives was observed over time, and chromatogram artifacts were monitored. The original recommended and widely used method of derivatizing alcohol for 30 min at 60 °C in acetonitrile using BSTFA was overcome using three optimized procedures with different TMS reagents. They achieved high and stable yields in an acetone environment already at room temperature and a reaction lasting 5 min. Due to the same chemical structure of the resulting compounds (TMS-derivatives), it was possible to use established mass spectral databases. Optimized procedures were applied to environmental (water, sand) and urban (acrylic paint, asphalt-aluminum paint, concrete) samples contaminated with the studied alcohol. The results obtained on a benchtop gas chromatograph were validated afterward on a field device used by the deployable chemical laboratory of the Czech Army following their standard operating procedures for sample preparation. The developed methods are useful for military teams and stationary analytical laboratories whose task is the unambiguous identification of CWAs and related compounds in various samples.
Funding
This research received no external funding.
Institutional Review Board Statement
Not applicable.
Informed Consent Statement
Not applicable.
Data Availability Statement
The data presented in this study are available on request from the corresponding author. The data are not publicly available due to internal military regulations.
Acknowledgments
I would like to express my gratitude to the teams of deployable chemical laboratories of the 31st Chemical, Biological, Radiological and Nuclear Regiment of the Czech Army for the possibility of using their capacities to verify the developed methods in the mobile laboratory as part of their regular internship at our Institute under my leadership.
Conflicts of Interest
The author declares no conflict of interest.
References
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MDPI and ACS Style
Rozsypal, T. Current Approaches to the Derivatization of Chemical Weapon Convention-Related Alcohol for On-Site Gas Chromatographic Analysis. Proceedings 2023, 92, 13. https://doi.org/10.3390/proceedings2023092013
AMA Style
Rozsypal T. Current Approaches to the Derivatization of Chemical Weapon Convention-Related Alcohol for On-Site Gas Chromatographic Analysis. Proceedings. 2023; 92(1):13. https://doi.org/10.3390/proceedings2023092013
Chicago/Turabian StyleRozsypal, Tomas. 2023. "Current Approaches to the Derivatization of Chemical Weapon Convention-Related Alcohol for On-Site Gas Chromatographic Analysis" Proceedings 92, no. 1: 13. https://doi.org/10.3390/proceedings2023092013
