scholarly journals Development of a method for derivatization of ethanolamines and its application to sand samples

2021 ◽  
pp. 47-47
Author(s):  
Tomas Rozsypal
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Room Temperature ◽  
Degradation Products ◽  
Chemical Warfare Agents ◽  
Rapid Identification ◽  
Chemical Warfare ◽  
Temperature Calibration ◽  
Nitrogen Mustards ◽  
Warfare Agents

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.

Analysis of chemical warfare agents by gas chromatography-mass spectrometry: methods for their direct detection and derivatization approaches for the analysis of their degradation products

2017 ◽  
Vol 37 (1) ◽  
Author(s):  
Carlos A. Valdez ◽  
Roald N. Leif ◽  
Saphon Hok ◽  
Bradley R. Hart
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Direct Detection ◽  
Degradation Products ◽  
Chemical Warfare Agents ◽  
Chemical Warfare ◽  
Gas Chromatography Mass Spectrometry ◽  
Science Center ◽  
Chromatography Mass Spectrometry ◽  
Warfare Agents

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.

scholarly journals ANALYSIS AND IDENTIFICATION SPIKING CHEMICAL COMPOUNDS RELATED TO CHEMICAL WEAPON CONVENTION IN UNKNOWN WATER SAMPLES USING GAS CHROMATOGRAPHY AND GAS CHROMATOGRAPHY ELECTRON IONIZATION MASS SPECTROMETRY

2010 ◽  
Vol 7 (3) ◽  
pp. 297-302 ◽  
Author(s):  
Harry Budiman
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Degradation Products ◽  
Chemical Warfare Agents ◽  
Retention Indices ◽  
Chemical Warfare ◽  
Ionization Mass ◽  
Chemical Weapon ◽  
Chemical Weapon Convention ◽  
Warfare Agents

The identification and analysis of chemical warfare agents and their degradation products is one of important component for the implementation of the convention. Nowadays, the analytical method for determination chemical warfare agent and their degradation products has been developing and improving. In order to get the sufficient analytical data as recommended by OPCW especially in Proficiency Testing, the spiking chemical compounds related to Chemical Weapon Convention in unknown water sample were determined using two different techniques such as gas chromatography and gas chromatography electron-impact ionization mass spectrometry. Neutral organic extraction, pH 11 organic extraction, cation exchanged-methylation, triethylamine/methanol-silylation were performed to extract the chemical warfare agents from the sample, before analyzing with gas chromatography. The identification of chemical warfare agents was carried out by comparing the mass spectrum of chemicals with mass spectrum reference from the OPCW Central Analytical Database (OCAD) library while the retention indices calculation obtained from gas chromatography analysis was used to get the confirmation and supported data of  the chemical warfare agents. Diisopropyl methylphosphonate, 2,2-diphenyl-2-hydroacetic acid and 3-quinuclidinol were found in unknown water sample. Those chemicals were classified in schedule 2 as precursor or reactant of chemical weapons compound in schedule list of Chemical Weapon Convention.   Keywords: gas chromatography, mass spectrometry, retention indices, OCAD library, chemical warfare agents

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