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Validation of methane measurement using headspace‐GC–MS and quantification by a stable isotope‐labeled internal standard generated in situ
Author(s) -
Varlet Vincent,
Smith Fiona,
Augsburger Marc
Publication year - 2013
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201300080
Subject(s) - chemistry , calibration , chromatography , gas chromatography , methane , gas chromatography–mass spectrometry , analytical chemistry (journal) , deuterium , detection limit , mass spectrometry , accuracy and precision , sample preparation , isotope , analyte , reagent , organic chemistry , statistics , physics , mathematics , quantum mechanics
A previous study has shown the possibility to identify methane ( CH 4 ) 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 CH 4 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 CH 4 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 CH 4 by the reaction of G rignard reagent methylmagnesium chloride with deuterated water. This method allows precise measurement of CH 4 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.