Identification of Sulfur and Nitrogen Mustards by GC/FPD/NPD-MS

Abstract

Gas chromatography simultaneously coupled to flame photometric detector, nitrogen phosphorus detector and mass spectrometer (GC/FPD/NPD-MS) was used to identify nitrogen and sulfur mustards, their precursors and degradation products in samples of water, soil, organic solvent and a PVC floor. Extraction techniques and derivatization with BSTFA were employed during sample preparation. Fast screening of the samples was possible due the high sensibility and selectivity of FPD and NPD for sulfur and nitrogen compounds. Mass spectra of the identified chemicals presented match factors equal or bigger than 90% when compared to OPCW databases.Keywords: Mustard gas; gas chromatography; mass spectrometry; chemical weapons. ResumoCromatografia gasosa acoplada simultaneamente a detectores fotométricos de chama, de nitrogênio e fósforo e espectrômetro de massas (CG/DFC/DNP-EM) foi utilizada na identificação de mostardas de enxofre e de nitrogênio, seus precursores e produtos de degradação em amostras de água, solo, solvente orgânico e um piso de PVC preparadas de forma controlada. Técnicas de extração e derivatização com BSTFA foram utilizadas para possibilitar as análises das substâncias por cromatografia gasosa. O uso simultâneo de vários detectores em um só equipamento possibilitou rapidez nas análises. DFC e DNF apresentam boa seletividade e sensibilidade para compostos contendo enxofre e nitrogênio, permitindo a seleção inicial dos picos cromatográficos de possíveis compostos de interesse. Todos os espectros de massa das substâncias identificadas apresentaram índices de similaridades iguais ou superiores a 90% quando comparados aos existentes nas bases de dados da OPAQ.Palavras-chave: Gás mostarda; cromatografia gasosa; espectrometria de massas; armas químicas.

Ethanolysis of nitrogen mustards: A novel strategy for nitrogen mustard identification in environmental matrices by liquid chromatography–electrospray ionization–tandem mass spectrometry

“…Gas chromatography (GC) coupled with nitrogen-phosphorus detectors (NPDs) and GC-mass spectrometry methods have been reported mainly for the determination of intact NMs but also for the corresponding degradation products with and without derivatization in clinical and environmental matrices, organic solvents, vapor forms and hydrophobic matrices. [9][10][11][12][13][14][15][16][17][18][19] Reepmeyer et al derivatized HN2 with thiophenol to form a stable disubstituted derivative with a substantial UV chromophore. 20 Recently, a method was developed for the detection of half NM as a specific biomarker in plasma after NM exposure for verification by the CWC.…”

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

“…A GC/FPD-NPD (flame photometric detection and nitrogen phosphorus detection) method was developed for the determination of nitrogen mustards and ethanolamines in water, soil, organic solvents and PVC. 19 Nerve agent degradation products in soil are derivatized using methylation by trimethyloxonium tetrafluoroborate. 20 Arsenic CWAs in sand samples are identified after thermal desorption.…”