Non-Contact Detection of Thiodiglycol Vapors and Associated Degradation Products Using Atmospheric Flow Tube Mass Spectrometry

The Analyst ◽  
2021 ◽  
Author(s):  
Kelsey A. Morrison ◽  
Brian Clowers
Keyword(s):  
Mass Spectrometry ◽  
Environmental Degradation ◽  
Degradation Product ◽  
Sulfur Mustard ◽  
Degradation Products ◽  
Chemical Weapons ◽  
Contact Detection ◽  
Flow Tube ◽  
Atmospheric Flow ◽  
Historical Presence

Thiodiglycol (TDG) is a synthetic precursor and an environmental degradation product of sulfur mustard (HD). Consequently, its presence can be indicative of illicit preparation or historical presence of chemical weapons,...

Non-contact vapor detection of illicit drugs via atmospheric flow tube-mass spectrometry

The Analyst ◽  
2020 ◽  
Vol 145 (20) ◽  
pp. 6485-6492
Author(s):  
Kelsey A. Morrison ◽  
Blandina R. Valenzuela ◽  
Elizabeth H. Denis ◽  
Megan K. Nims ◽  
David A. Atkinson ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Real Time ◽  
Illicit Drugs ◽  
Contact Detection ◽  
Flow Tube ◽  
Vapor Detection ◽  
Atmospheric Flow

Atmospheric flow tube-mass spectrometry (AFT-MS) enables real-time, non-contact detection of fentanyl, heroin, and other illicit drugs at parts-per-quadrillion vapor levels or from femtograms of residue.

scholarly journals The limitations and capabilities of wipe samples analysis in control of contamination of facilities with highly toxic organic compounds

2021 ◽  
Author(s):  
MD Shachneva ◽  
MA Leninskii ◽  
EI Savelieva
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Sulfur Mustard ◽  
Degradation Products ◽  
Tandem Mass ◽  
Toxic Substances ◽  
Building Structures ◽  
Engineering Structures ◽  
Ms Analysis ◽  
The Matrix

Wipe sampling is widely used for microbiological control purposes. Sanitary and chemical studies also include analysis of samples wiped from the work surfaces during routine and periodic working conditions safety inspections at chemical facilities. The analysis also allows assessing the toxicity and hazard of items/structures that could be in contact with highly toxic substances. This study aimed to investigate the capabilities and limitations of the surface wipe sample analysis method in control of residual contamination of equipment and building structures of a former chemical weapons destruction facilities (CWDF) with sulfur mustard and O-isobutyl-S(2-diethylaminoethyl) methylphosphonothioate (VR), as well as their degradation products. Gas chromatography with tandem mass spectrometry (GC-MS/MS) enabled identification of the sulfur mustard markers, high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS) allowed identifying VR markers. An assessment of the matrix influence on the results of GC-MS/MS and HPLC-MS/MS analysis was carried out. The matrix effect was established to affect the results the most in case of HPLC-MS/MS analysis: for GC-MS/MS analysis of target substances, the matrix factor averaged at 60–80%, for HPLC-MS/ MS it was less than 40%. The average percent sulfur mustard recoveries from three types of surfaces (PVC tiles, laminate and metal plates) was 9 ± 2%, 0.13 ± 0.02% and 0.10 ± 0.03%; in case of VR, the recoveries was 2.7 ± 0.5%, 11.8 ± 0.3% and 0.8 ± 0.1%, respectively. The limits of detection for sulfur mustard by GC-MS/MS and VR by HPLC-MS/MS were established at 0.001 MPL and 0.02 MPL, respectively. The developed approaches were applied to the analysis of wipe samples from the surfaces of the equipment and engineering structures of the former CWDF.

scholarly journals Organisation for the Prohibition of Chemical Weapons' New Approaches to Laboratory Support for Control over Non-Proliferation

2017 ◽  
Vol 1 (4) ◽  
pp. 24-34
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Sulfur Mustard ◽  
Organic Phosphorus ◽  
Toxic Chemicals ◽  
Phosphorus Compounds ◽  
Gas Chromatography Mass Spectrometry ◽  
Chemical Weapons ◽  
Laboratory Equipment ◽  
Detection And Identification

The development of scientific research methods and dual-use production technologies, the widening of the range of new toxic chemicals, as well as technical possibilities for the development of a new generation of poisonous substances, formally not forbidden by the acting Convention on the Prohibition of the Development, Production, Stockpiling and Use of Chemical Weapons and on their Destruction, pose a new level of threats to nonproliferation of chemical weapons. Under these circumstances, it is necessary to possess not only legal possibility, but also appropriate laboratory equipment and services for the effective non-proliferation control. Considerable attention in this sphere has been paid earlier to environmental samples for toxic chemicals analysis, including samples of air, soil, vegetation and water. But at the present time the Organisation for the Prohibition of Chemical Weapons (OPCW) gives special emphasis to analysis of biomedical samples (blood, urine) in the context of non-proliferation and investigations of alleged use of chemical weapons and toxic chemicals. The proper sensitivity during the detection and identification of biomarkers of exposure to chemical agents and toxic chemicals can be achieved by gas chromatography- mass spectrometry (GC/MS) and gas chromatography-tandem mass spectrometry (GC/MS/MS) methods. Efforts in this sphere are now focused on three main tasks – sample preparation, the optimization of the conditions of chromatographic separation of samples, storage and interpretation of mass-spectra characteristics. The article provides examples of how the above mentioned techniques are used in the detection of signs and evidence of exposure to organic phosphorus compounds and sulfur mustard

scholarly journals Column Liquid Chromatography-Ultraviolet and Column Liquid Chromatography/Mass Spectrometry Evaluation of Stress Degradation Behavior of Escitalopram Oxalate

2009 ◽  
Vol 92 (1) ◽  
pp. 138-147 ◽  
Author(s):  
Sunil R Dhaneshwar ◽  
Mahadeo V Mahadik ◽  
Mahesh J Kulkarni
Keyword(s):  
Mass Spectrometry ◽  
Column Liquid Chromatography ◽  
Liquid Chromatography ◽  
Degradation Product ◽  
Degradation Products ◽  
Oxidative Degradation ◽  
Stress Conditions ◽  
Assay Method ◽  
Infrared Spectrometry ◽  
Degradation Behavior

Abstract The objective of this work was to study the degradation behavior of escitalopram oxalate under different International Conference on Harmonization (ICH)-recommended stress conditions by column liquid chromatography (LC)-UV and LC/mass spectrometry (LC/MS) and to establish a validated stability-indicating LC assay method. Escitalopram oxalate was subjected to stress conditions of hydrolysis, oxidation, photolysis, and thermal decomposition. Extensive degradation was found to occur in alkaline medium. Mild degradation was observed in acidic and oxidative conditions. Escitalopram oxalate was stable to neutral, photolytic, and thermal stress. Successful separation of the drug from degradation products formed under stress conditions was achieved on a PerfectSil-100 ODS-3 column [C18 (5 m, 25 cm 4.6 mm id)] using methanol0.01 M acetate buffer pH 3.8 adjusted with acetic acid (45 + 55) as the mobile phase. The flow rate was 1 mL/min, and the detection wavelength was 239 nm. The method was validated according to ICH guidelines. Major degradation products formed in hydrolysis and oxidative conditions were isolated, and structural elucidation of degradation products was done by LC/MS and infrared spectrometry studies. The major hydrolysis degradation product was confirmed as 1-(3-dimethylaminopropyl)-1-(4-fluoro- phenyl)-1,3dihydroisobenzofuran-5-carboxylic acid, and the major oxidative degradation product was confirmed as 1-{[3-dimethylamino(oxide)- propyl]-1-(4-fluro-phenyl)}-1,3-dihydro-isobenzofuran- 5-carbonitrile.

scholarly journals Novel analytical approaches to determination of chemical warfare agents and related compounds for verification of nonproliferation of chemical weapons

2017 ◽  
Vol 89 (10) ◽  
pp. 1491-1503 ◽  
Author(s):  
Igor V. Rybalchenko ◽  
Igor A. Rodin ◽  
Timur M. Baygildiev ◽  
Andrey N. Stavrianidi ◽  
Arcady V. Braun ◽  
...  
Keyword(s):  
Analytical Methods ◽  
Sulfur Mustard ◽  
Degradation Products ◽  
Chemical Warfare Agents ◽  
Chemical Warfare ◽  
Chemical Weapons ◽  
Mass Spectral ◽  
Fast Screening ◽  
Warfare Agents ◽  
Analytical Approaches

AbstractIn this paper a summary of the author’s approaches for investigation of the mass spectral behavior of some chemical warfare agents (CWAs), their degradation products and metabolites, as well as the results of development of analytical methods for confirmation of nerve and blister agents application are presented. Hydrolysis and oxidation metabolites of nerve agents, sulfur mustard and lewisite were used as biomarkers of the exposure. Sensitive analytical methods have been developed for their detection, based mainly on tandem mass spectrometry coupled with liquid chromatography. Several techniques for fast screening of CWAs degradation products based on capillary electrophoresis were also proposed. Some of developed approaches were successfully applied in the frame of the proficiency testing system of the Organization for the Prohibition of Chemical Weapons.

Oxidative degradation of chemical warfare agents in water by bleaching powder

2012 ◽  
Vol 66 (7) ◽  
pp. 1377-1383 ◽  
Author(s):  
Lihong Qi ◽  
Guomin Zuo ◽  
Zhenxing Cheng ◽  
Haiyan Zhu ◽  
Shanmao Li
Keyword(s):  
Mass Spectrometry ◽  
Sulfur Mustard ◽  
Degradation Products ◽  
Oxidative Degradation ◽  
Chemical Warfare Agents ◽  
Gas Chromatography Mass Spectrometry ◽  
Product Analysis ◽  
Bleaching Powder ◽  
Chromatography Mass Spectrometry ◽  
Warfare Agents

Degradation of sulfur mustard (HD), S-2-(di-isopropylamino)ethyl O-ethyl methylphosphonothioate (VX) and Soman (GD) in water by bleaching powder was investigated. The degradation products were comprehensively analyzed by gas chromatography/mass spectrometry (GC/MS), liquid chromatography/mass spectrometry (LC/MS) and ion chromatography. Degradation pathways were deduced based on the identified products. The product analysis results indicated that HD could be degraded through oxidation and chlorination reactions, and a small portion of sulfur atoms could be mineralized into SO42− ion. Oxidative degradation of VX could finally generate O-ethyl methylphosphonate acid (EMPA), sulfonic acids, SO42− and NO3− ions. GD would be converted into non-toxic pinacolyl methylphosphonate via nucleophilic substitution.

scholarly journals Hygienic assessment of the chemical weapons destruction facilities in the context of relieving the consequences of their operation and subsequent conversion thereof

2021 ◽  
Author(s):  
DV Gulyaev
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Gas Chromatography Mass Spectrometry ◽  
Chemical Weapons ◽  
Tandem Mass ◽  
Toxic Substances ◽  
Building Structures

After elimination of the chemical weapons, it is necessary to relieve the consequences of operation of the chemical weapons destruction facilities (CWDF). This study aimed to assess the results of such relieve activities from the hygienic point of view. The assessment allows considering partial conversion of the CWDFs' infrastructure for civil purposes. At four CWDFs, the sites of contamination of equipment and infrastructural components with degradition products of organophosphorous agents (OPA) and blister agents (BA) were identified. The technologies that enabled analysis of the samples taken were high performance liquid chromatography with tandem mass spectrometry, gas chromatography–mass spectrometry, gas chromatography–tandem mass spectrometry, and atomic absorption spectroscopy with electrothermal atomization. The analysis revealed contamination of building structures, equipment, utility lines, waterproofing, heatinsulating, and other materials inside the CWDF process buildings, regardless of their purpose, with OPA and BA degradation products. In the absence of hygienic standards and information on their toxicity, it was impossible to assess the hazard thereof. In all the samples taken, the residual content of toxic substances was below the limit of detection of the measurement methods applied, i.e., none was found. The article presents a methodology for a stepwise hygienic assessment of the CWDF infrastructure to be converted and develops recommendations for its subsequent safe use. The conclusions state expediency of development of hygienic standards for the OPA and BA degradation products and development and certification of the relevant measurement procedures.

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