Trace level detection and identification of chemicals related to the chemical weapons convention from complex organic samples

Reddy, T. Jagadeshwar; Saradhi, U.V.R. Vijaya; Prabhakar, S.; Vairamani, M.

doi:10.1016/j.chroma.2004.03.028

Cited by 20 publications

(18 citation statements)

References 25 publications

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“…In such a case, the presence of the [M-OR] + ion is expected in the EI spectra of dialkyl phosphonothiolates in addition to the expected [M-SR] + ion. Among the studied dialkyl alkylphosphonothiolates (1)(2)(3)(4)(5)(6)(7)(8)(9)(10)(11)(12)(13)(14)(15)(16)(17)(18), the [M-OR] + ion appeared only in compounds where a propyl or a butyl group was attached to sulfur (3-4, 8-10, 13-14). This reveals that the dialkyl phosphonothiolates undergo a 'thiolo-thiono' rearrangement, especially when a higher alkyl group is attached to sulfur.…”

Section: Thiono-thiolo Rearrangementmentioning

confidence: 99%

“…Over the past two decades, a great deal of attention has been focused on the development of analytical techniques for the rapid identification and analysis of CWAs, their precursors, degradation products and reaction products. Most CWAs are volatile and relatively non‐polar and, hence, gas chromatography (GC) coupled with various selective and sensitive detectors such as flame ionization detector (FID), nitrogen phosphorus detector (NPD), flame photometric detector (FPD), Fourier transform infrared (FTIR) spectroscopy, and mass spectrometry (MS) is widely used for the analysis of non‐polar CWAs . Of these, the MS detector has been extensively used because of its high sensitivity and versatility.…”

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confidence: 99%

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Mass spectral characterization of the CWC‐related isomeric dialkyl alkylphosphonothiolates/alkylphosphonothionates under gas chromatography/mass spectrometry conditions

Karthikraj

Sridhar

Prabhakar

et al. 2013

Rapid Comm Mass Spectrometry

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The present study highlights the structural characterization of the isomeric phosphonothiolates and phosphonothionates based on their selective EI fragmentation. The assigned fragmentation pathway helps in the assignment of P-S and P-alkyl connectivity in phosphonothiolates and phosphonothionates, consequently the structure of the unknown compounds. The EI mass spectra (27 compounds) of isomeric compounds are immensely useful in the OPCW official proficiency tests and for off-site analysis.

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Section: Thiono-thiolo Rearrangementmentioning

confidence: 99%

mentioning

confidence: 99%

Mass spectral characterization of the CWC‐related isomeric dialkyl alkylphosphonothiolates/alkylphosphonothionates under gas chromatography/mass spectrometry conditions

Karthikraj

Sridhar

Prabhakar

et al. 2013

Rapid Comm Mass Spectrometry

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“…The SPE method involves selective elution of the compounds of interest from the cartridge. The recovery was found to be 70 -85% at the 10 ppm level and the limits of detection were about 1 ppm [21].…”

Section: Gas Chromatographymentioning

confidence: 97%

“…The detection limit for ethyl methylphosphonic acid was higher (0.5 ng/mL) due to a lower recovery [20]. [21]. Generally it is difficult to analyse the compounds from the Schedule by direct GC/EI-MS analysis in the presence of dominant masking/background components, especially in a complex hydrocarbon matrix.…”

Section: Gas Chromatographymentioning

confidence: 98%

Utilisation of separation methods in the analysis of chemical warfare agents

et al. 2006

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Chemical warfare agents and their degradation products represent a broad group of compounds with different chemical properties (polarity, volatility, thermostability, etc.). These chemicals often have to be detected and determined in complex matrices and therefore highly efficient separation techniques hyphenated to selective and sensitive detectors play an indispensable role. This review offers an overview of selected papers devoted to the title subject. It cannot be considered as a comprehensive literature compilation but should allow the reader to obtain an insight into the application of separation techniques in the important area of human protection and control of chemical weapons.

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“…Therefore, a pre-treatment of CWAs from the complex environmental samples is very important for analyzing its trace. The pre-treatment techniques for analyzing CWAs include liquid-liquid extraction, 2 solid-phase extraction, 3 and solid-phase microextraction. 4 These extraction techniques were adopted when preparing samples of different sample matrices.…”

Section: Introductionmentioning

confidence: 99%

Analysis of Chemical Warfare Agents in Water Using Single-Drop Microextraction

2009

Bulletin of the Korean Chemical Society

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Single-drop microextraction (SDME) is an extraction methodology where the drop plays an essential role as extracts. It was evaluated for the GC-MS determination of nerve agents, one class of the chemical warfare agents (CWAs). Since these nerve agents are highly toxic, it is important to detect the nerve agents in the environmental samples. Several affecting factors including extraction solvents, stirring rate, extraction time, and amounts of salt were optimized. The limit of detections (LODs) were 0.1 -10 ng/mL and the relative standard deviations (RSDs%, n=5) were in the range of 6.3% to 9.0% for four nerve agents. Without pretreatment of the environmental samples, 5-103 fold enrichments and 48-100% recovery were accomplished. These results demonstrated the feasibility of this method for on-site and off-site analysis of water sample collected from suspicious CWAs site.Key Words: Single-drop microextraction, Chemical warfare agents, Nerve agents IntroductionThe Organization for Prohibition of Chemical Weapons (OPCW) inspects relevant industrial or military sites to implement Chemical Weapons Convention (CWC) which bans the development, production, stockpiling, and transferring of these dreadful weapons in various countries.1 This inspection includes various verification activities (on-site analysis by OPCW inspectors in alleged point and off-site analysis designated by OPCW laboratories). A key point of verification activities is to analyze chemical warfare agents (CWAs) regardless of sample types. Therefore, a pre-treatment of CWAs from the complex environmental samples is very important for analyzing its trace. The pre-treatment techniques for analyzing CWAs include liquid-liquid extraction, 2 solid-phase extraction, 3 and solid-phase microextraction. 4 These extraction techniques were adopted when preparing samples of different sample matrices. Each extraction technique has their strengths and weaknesses and can be used according to the properties of sample and matrix.Recently a fast, simple, inexpensive and solvent free sample preparation technique has been used for extracting CWAs from water. This technique, so called liquid-phase microextraction (LPME) can be performed as a pre-treatment which makes extraction and pre-concentration occur simultaneously. This technique involves hollow fiber protected liquid-phase microextraction 5,6 and single-drop microextraction. 7,8 In case of hollow fiber liquid-phase microextraction, a hollow fiber containing organic solvent is attached into the tip of the syringe needle, and the analytes of interesting are extracted into the organic solvent through a thin layer of a hollow fiber and then detected by GC or GC-MS, 9 typically. After the organic solvent is retracted into the syringe, the hollow fiber is discarded. Therefore, a carry-over effect can be removed. The extraction of CWAs and convention related compounds (CRCs) has been carried out using this technique. 5 The CWAs were directly extracted into organic solvent through hollow fiber and the CRCs having low vola...

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Trace level detection and identification of chemicals related to the chemical weapons convention from complex organic samples

Cited by 20 publications

References 25 publications

Mass spectral characterization of the CWC‐related isomeric dialkyl alkylphosphonothiolates/alkylphosphonothionates under gas chromatography/mass spectrometry conditions

Mass spectral characterization of the CWC‐related isomeric dialkyl alkylphosphonothiolates/alkylphosphonothionates under gas chromatography/mass spectrometry conditions

Utilisation of separation methods in the analysis of chemical warfare agents

Analysis of Chemical Warfare Agents in Water Using Single-Drop Microextraction

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