Use of Solid-Phase Extraction in Determination of Chemical Warfare Agents

T⊘rnes, John Aasulf; Opstad, Aase Mari; Johnsen, Bj⊘rn Arne

doi:10.1080/03067319108027555

Cited by 23 publications

(4 citation statements)

References 9 publications

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“…Importantly the pH of the soil buffer solution should be quite close to the p K a value of VX and quite low to avoid basic hydrolysis. Other reports as well describe the extraction of nerve agents from soils with spiking levels of 0.1–10 mg/g, 0.4% extraction with dichloromethane, spiking level of 0.5 mg/g with 8% ± 6% of recovery, and a spiking level of 20 μg/g with 16.2% ± 1.3% of recovery . A hexane–benzene mixture was used for extraction of sarin from soils; and gas-chromatographic separation and flame ionization detector helped in the analysis of a trace amount of nerve agent at a level of 10 –4 mg/kg .…”

Section: Sensing and Detectionmentioning

confidence: 99%

Destruction and Detection of Chemical Warfare Agents

et al. 2011

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Section: Sensing and Detectionmentioning

confidence: 99%

Destruction and Detection of Chemical Warfare Agents

et al. 2011

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“…Verweij & Boter, (1976), investigated the degradation product of CWA's phosphorus containing products, while Kuitunen et al, (1991), studied the extraction of CWA's in soil samples by offline supercritical fluid extraction and capillary gas chromatography. Other studies in relation to the extraction of CWA's by solid phase extraction using different solvent have also been performed by Tornes et al, (1991a), andTornes et al, (1991b). However, the results of these studies in less satisfactory yields mainly for soil contaminated with O-ethyl S-2-(diisopropylamino)ethyl methylphosphonothiolate (VX).…”

Section: Introductionmentioning

confidence: 99%

Extraction of Chemical Warfare Agents from Soils: Case Study on O-ethyl S-2-(diisopropylamino)ethyl methylphosphonothiolate (VX)

Zuas

2012

J.Nat.Indones

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Extraction of chemical warfare agents, O-ethyl S-2-(diisopropylamino)ethyl methylphosphonothiolate (VX) in soilsample has been carried out. The extraction was performed using six different solvents including 1% TEA/MeOH, 1% NH 4 OH/MeOH, water pH 2 at the ambient temperature , water pH 2 at temperature 4 0 C, water pH 7 at ambient temperature, and water pH 7 at temperature 4 0 C. Percent recovery of VX in soil samples was quantitatively determined by mean LC-MS using selected reaction monitoring (SRM). Among the solvents used, water pH 2 at temperature 4 0 C gave the best extraction capability that was indicated by the highest percent recovery of VX obtained. Storing effect of spiked samples was also investigated by extracting the samples containing VX using water at pH 2/4 0 C and the degradation product was then identified using multiple reaction monitoring (MRM). From the study, two degradation products were identified as Bis[2-(diisopropylamino)ethyl]disulphide and ethyl methylphosphonate.

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“…Further attempts eventually used technological advances such as automated extraction methods: Kutuinen and co-workers reported that supercritical carbon dioxide extraction of soil spiked with VX was completely ineffective, whereas ultrasound-assisted extraction with dichloromethane led to a recovery of 0.4% in one out of three experiments, VX remaining undetected in the two other cases . A Norwegian team reported that VX can only be detected in soil samples spiked at very high levels (0.5 mg·g -1 ), with poor recovery yields (8 ± 6%) . A more recent and extensive study by the same team, involving eight types of soils spiked with 20 μg·g -1 agent and dichloromethane as extraction solvent, indicates that VX can be correctly extracted from sandy loam (16.2 ± 1.3%) and turf (34.2 ± 3.7%), the latter being a very particular case.…”

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Extraction of Nerve Agent VX from Soils

2004

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The development and optimization of a method allowing the extraction of intact organophosphorus chemical warfare agent O-ethyl S-(2-diisopropylaminoethyl) methylphosphonothiolate (VX) from several types of soils are presented here. This involved the selection of an appropriate buffer to bring the sample to a pH close to the pK(a) of VX but sufficiently low to avoid its basic hydrolysis. Buffering with Tris (pH 9) and subsequent extraction of the aqueous layer by a 85:15 (v/v) hexane/dichloromethane mixture allows rapid and sensitive flame photometric detection of VX at spiking levels lower than 10 microg x g(-1), even after 3 months of aging. Extraction yields were close to 60% in complex matrixes. This method also allows recovery and identification of a characteristic degradation product of VX, bis(2-diisopropylaminoethyl) disulfide, which appears to be formed during the aging process. The performance of this method is far better than that of OPCW reference operating procedure, which does not allow extraction of detectable amounts of VX (spiked at 10 microg x g(-1)) in one of the soils used for this study.

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Use of Solid-Phase Extraction in Determination of Chemical Warfare Agents

Cited by 23 publications

References 9 publications

Destruction and Detection of Chemical Warfare Agents

Destruction and Detection of Chemical Warfare Agents

Extraction of Chemical Warfare Agents from Soils: Case Study on O-ethyl S-2-(diisopropylamino)ethyl methylphosphonothiolate (VX)

Extraction of Nerve Agent VX from Soils

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