Validation of methane measurement using headspace‐GC–MS and quantification by a stable isotope‐labeled internal standard generated in situ. Issue 12 (27th May 2013)

• Record Type: Journal Article
• Authors: Varlet, Vincent; Smith, Fiona; Augsburger, Marc
• Is Part Of: Journal of separation science. Volume 36:Issue 12(2013:Jun.)
• Page Start: 1967
• Page End: 1972
• Publication Date: 2013-05-27
• Subjects: Separation (Technology) -- Periodicals; Chromatographic analysis -- Periodicals; 543.089
• DOI: 10.1002/jssc.201300080
• Languages: English
• ISSNs: 1615-9306

Abstract

<abstract abstract-type="main"> <title> <x xml:space="preserve">Abstract</x> </title> <p>A previous study has shown the possibility to identify methane (CH₄) using headspace‐GC–MS and quantify it with a stable isotope as internal standard. The main drawback of the GC–MS methods discussed in literature for CH₄ measurement is the absence of a specific internal standard necessary to perform quantification. However, it becomes essential to develop a safer method to limit the manipulation of gaseous CH₄ and to precisely control the injected amount of gas for spiking and calibration by comparison with external calibration. To avoid the manipulation of a stable isotope‐labeled gas, we have chosen to generate a labeled gas as an internal standard in a vial on the basis of the formation of CH₄ by the reaction of Grignard reagent methylmagnesium chloride with deuterated water. This method allows precise measurement of CH₄ concentrations in gaseous sample as well as in a solid or a liquid sample after a thermodesorption step in a headspace vial. A full accuracy profile validation of this method is then presented.</p> </abstract>