Gas chromatographic determination of methylphosphonic acids by methylation with trimethylphenylammonium hydroxide

Tørnes, John Aa; Johnsen, Bjørn A.

doi:10.1016/s0021-9673(01)93957-3

Cited by 72 publications

(16 citation statements)

References 12 publications

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“…It is clear that with TMPAH, less polar solvent such as Hexane and THF produce methyl derivatives in higher yield than the polar solvents such as MeOH or iPrOH. This result is in agreement with the observations of Tornes and Johnsen [29]. The increase in the injection port temperature does not have an effect on the methylation yield in the THF-Hex solvent and hence for TAM with TMPAH can be achieved with the OPCW normal chromatographic condition.…”

Section: Evaluation Of Injection Port Temperaturesupporting

confidence: 92%

“…Sega et al [33] reported the extraction of methylphosphonic acid and alkyl methylphosphonic acid from 50 mL groundwater using a solid-phase extraction column packed with 500 mg of silica with a bonded quaternary amine phase, and are eluted and derivatised with methanolic trimethylphenylammonium hydroxide and analysed by GC-FPD {P}. Sutherland [34] used 1:1 mixture of benzene and methanolic TMPAH for the analysis of samples from artworks followed by the analysis by GC-MS. TMPAH at 0.03 mM (300 L of 0.1 M TMPAH in MeOH) was used with 1000 g/mL of alkyl phosphonic acid by Tornes and Johnson [29]. Amijee et al [35] had reported methylation with the higher concentrations of a wide variety of analytes at 70-100 mg/kg with 10 mM of TMPAH.…”

Section: Thermally Assisted Methylation By Trimethylphenylammonium Hymentioning

confidence: 99%

“…TMSD has been suggested as an efficient alternative to diazomethane [23][24][25]. Similarly thermally assisted or pyrolytic alkylation reactions are also well documented in the literature for various kinds of organic chemicals and have been reviewed in some recent reviews [26][27][28][29][30]. The pyrolytic alkylation reactions are generally conducted with tetra-alkylammonium salts.…”

Section: Introductionmentioning

confidence: 99%

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Thermally assisted methylation and subsequent silylation of scheduled acids of chemical weapon convention for on-site analysis and its comparison with the other methods of methylation

Amphaisri

Palit

Mallard

2011

Journal of Chromatography A

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Section: Evaluation Of Injection Port Temperaturesupporting

confidence: 92%

Section: Thermally Assisted Methylation By Trimethylphenylammonium Hymentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Thermally assisted methylation and subsequent silylation of scheduled acids of chemical weapon convention for on-site analysis and its comparison with the other methods of methylation

Amphaisri

Palit

Mallard

2011

Journal of Chromatography A

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“…Moreover, some neutral compounds, such as carbohydrates, which contain hydroxide groups competed against the phosphonates in the silylation reaction and suppressed the TBDMS derivatization. 28,31) Several investigations on cleanup of nerve gas hydrolysis products using solid phase extraction (SPE) have been reported, 23,25,[32][33][34] and some drawbacks were found such as low recoveries of RMPAs and MPA and insufficient information about SPE procedures. We attempted some types of SPE including strong cation-exchanger, 28) anionexchanger and reversed-phase 31,35) followed by TBDMS derivatization.…”

Section: Fig 4 Effects Of Alkaline Earth Metals On the Detection Yimentioning

confidence: 99%

Laboratory Identification of the Nerve Gas Hydrolysis Products Alkyl Methylphosphonic Acids and Methylphosphonic Acid, by Gas Chromatography-mass Spectrometry after <i>tert</i>-Butyldimethylsilylation

Kanamori-Kataoka

Seto

2008

JOURNAL OF HEALTH SCIENCE

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Alkyl methylphosphonic acids (RMPAs) and methylphosphonic acid (MPA), both nerve gas hydrolysis products, can be identified by gas chromatography-mass spectrometry (GC-MS). We adopted tertbutyldimethylsilylation (TBDMS) as a derivatization technique for the identification of these products by GC-MS. We found that it was difficult to detect RMPAs and MPA from evidence specimens such as soils and body fluids, and ascertained several causes for this. The first is the interference from the TBDMS derivatization. It was determined that the TBDMS derivatization of RMPAs and MPA was suppressed in the presence of divalent metal cations such as calcium and magnesium ions, as well as some neutral compounds like carbohydrates. A cleanup procedure using a strong anion-exchanger (SAX)-solid phase extraction (SPE) method was optimized to remove the interfering compounds. The second reason that detection was difficult was because of strong matrix adsorption. We elucidated that the aqueous extraction recoveries for all phosphonates were inversely correlated with the phosphate adsorption coefficient in the soil samples. To diminish the adsorption of phosphonates to soils, a method of alkali extraction was adopted. For human serum samples, we adopted acetonitrile or trichloroacetic acid deproteinization which worked to break the binding between the proteins and the phosphonates. The detection yields of RMPAs and MPA from soils and human serum were dramatically increased using these pretreatment procedures combined with extraction and/or SAX-SPE. The method of SAX-SPE was applied to various types of samples, such as seawater, drinks and human urine, and good detection yields of RMPAs and MPA were provided by GC-MS.

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“…Gas chromatography/atomic emission detection (GC/AED) was used to quantify volatile compounds (1), including derivatized arsenic compounds related to lewisite (L). Chemical derivatization with GC/MS was used to identify polar and nonvolatile decontamination products (2)(3)(4)(5)(6). Capillary electrophoresis (CE) with indirect UV detection was used to quantify the alkyl methylphosphonic acids from nerve agent (GB and VX) decontamination (7).…”

Section: Introductionmentioning

confidence: 99%

Analysis of Chemical Weapons Decontamination Waste from Old Ton Containers from Johnston Atoll Using Multiple Analytical Methods

Creasy¹,

Brickhouse²,

Morrissey³

et al. 1999

Environ. Sci. Technol.

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Decontamination waste from chemical weapons (CW) agents has been stored in ton containers on Johnston Atoll since 1971. The waste was recently sampled and analyzed to determine its chemical composition in preparation for disposal. Due to the range of products and analytical requirements, multiple chromatographic and spectroscopic methods were necessary, including gas chromatography/ mass spectrometry (GC/MS), gas chromatography/ atomic emission detection (GC/AED), liquid chromatography/ mass spectrometry (LC/MS), capillary electrophoresis (CE), and nuclear magnetic resonance spectroscopy (NMR). The samples were screened for residual agents. No residual sarin (GB) or VX was found to detection limits of 20 ng/mL, but 3% of the samples contained residual sulfur mustard (HD) at <140 ng/mL. Decontamination products of agents were identified. The majority (74%) of the ton containers were documented correctly, in that the observed decontamination products were in agreement with the labeled agent type, but for a number of the containers, the contents were not in agreement with the labels. In addition, arsenic compounds that are decontamination products of the agent lewisite (L) were observed in a few ton containers, suggesting that lewisite was originally present but not documented. This study was a prototype to demonstrate the level of effort required to characterize old bulk CW-related waste.

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Gas chromatographic determination of methylphosphonic acids by methylation with trimethylphenylammonium hydroxide

Cited by 72 publications

References 12 publications

Thermally assisted methylation and subsequent silylation of scheduled acids of chemical weapon convention for on-site analysis and its comparison with the other methods of methylation

Thermally assisted methylation and subsequent silylation of scheduled acids of chemical weapon convention for on-site analysis and its comparison with the other methods of methylation

Laboratory Identification of the Nerve Gas Hydrolysis Products Alkyl Methylphosphonic Acids and Methylphosphonic Acid, by Gas Chromatography-mass Spectrometry after <i>tert</i>-Butyldimethylsilylation

Analysis of Chemical Weapons Decontamination Waste from Old Ton Containers from Johnston Atoll Using Multiple Analytical Methods

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