Analysis of chemical warfare agents in soil samples by off‐line supercritical fluid extraction and capillary gas chromatography

Kuitunen, Marja‐Leena; Hartonen, Kari; Riekkola, Marja‐Liisa

doi:10.1002/mcs.1220030605

Cited by 24 publications

(9 citation statements)

References 13 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…6 The success of this type of analysis depends on the efficacy of the extraction step, but this can be difficult; for example, a recent application of supercritical fluid extraction to the separation of VX was unsuccessful. 7 Other more conventional extraction approaches have been developed and combined with GC and or MS detection. 2,8,9 An additional mass spectrometry approach that has been suc- cessfully utilized for VX detection employed thermospray MS with a HPLC.…”

Section: The Direct Detection Of the Nerve Agent Vx (Methylphosphonot...mentioning

confidence: 99%

“…When the compound can be appropriately separated from its environmental matrix, it can be readily analyzed using GC/MS; in particular, ammonia chemical ionization has been shown to be effective for VX and many of its neutral degradation products . The success of this type of analysis depends on the efficacy of the extraction step, but this can be difficult; for example, a recent application of supercritical fluid extraction to the separation of VX was unsuccessful . Other more conventional extraction approaches have been developed and combined with GC and or MS detection. ,, An additional mass spectrometry approach that has been successfully utilized for VX detection employed thermospray MS with a HPLC .…”

mentioning

confidence: 99%

See 1 more Smart Citation

Analysis of VX on Soil Particles Using Ion Trap Secondary Ion Mass Spectrometry

et al. 1999

View full text Add to dashboard Cite

The direct detection of the nerve agent VX (methylphosphonothioic acid, S-[2-[bis(1-methylethyl)amino]ethyl] O-ethyl ester) on milligram quantities of soil particles has been achieved using ion trap secondary ion mass spectrometry (IT-SIMS). VX is highly adsorptive toward a wide variety of surfaces; this attribute makes detection using gas-phase approaches difficult but renders the compound very amenable to surface detection. An ion trap mass spectrometer, modified to perform SIMS, was employed in the present study. A primary ion beam (ReO4-) was fired on axis through the ion trap, where it impacted the soil particle samples. [VX + H]+, [VX + H]+ fragment ions, and ions from the chemical background were sputtered into the gas-phase environment of the ion trap, where they were either scanned out or isolated and fragmented (MS2). At a surface concentration of 0.4 monolayer, intact [VX + H]+, and its fragment ions, were readily observable above background. However, at lower concentrations, the secondary ion signal from VX became obscured by ions derived from the chemical background on the surface of the soil particles. MS2 analysis using the ion trap was employed to improve detection of lower concentrations of VX: detection of the 34S isotopic ion of [VX + H]+, present at a surface concentration of approximately 0.002 monolayer, was accomplished. The study afforded the opportunity to investigate the fragmentation chemistry of VX. Semiempirical calculations suggest strongly that the molecule is protonated at the N atom. Deuterium labeling showed that formation of the base peak ion (C2H4)N(i-C3H7)2+ involves transfer of the amino proton to the phosphonothioate moiety prior to, or concurrent with, C-S bond cleavage. To manage the risk associated with working with the compound, the vacuum unit of the IT-SIMS was located in a hood, connected by cables to the externally located electronics and computer.

show abstract

Section: The Direct Detection Of the Nerve Agent Vx (Methylphosphonot...mentioning

confidence: 99%

mentioning

confidence: 99%

Analysis of VX on Soil Particles Using Ion Trap Secondary Ion Mass Spectrometry

et al. 1999

View full text Add to dashboard Cite

show abstract

“…The nonpolymeric components of aged single-base propellants were extracted with supercritical CO2 and analyzed with open-tubular GC (523). Kuitunen et al studied the analysis of chemical warfare agents in soil by SFE and open-tubular GC with flame ionization or nitrogen/phosphorus detection (524). SFE was also used to compare chemithermomechanical wood pulps and Kraft pulps (525).…”

Section: Sfe Applicationsmentioning

confidence: 99%

Supercritical Fluid Chromatography and Extraction

Chester¹,

Pinkston²,

Raynie³

1994

Anal. Chem.

163

View full text Add to dashboard Cite

“…A number of works related to the extraction of CW agents from soil have been reported previously. 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).…”

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

View full text Add to dashboard Cite

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.

show abstract

Analysis of chemical warfare agents in soil samples by off‐line supercritical fluid extraction and capillary gas chromatography

Cited by 24 publications

References 13 publications

Analysis of VX on Soil Particles Using Ion Trap Secondary Ion Mass Spectrometry

Analysis of VX on Soil Particles Using Ion Trap Secondary Ion Mass Spectrometry

Supercritical Fluid Chromatography and Extraction

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

Contact Info

Product

Resources

About