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A new method for determining delta C-13 and delta D simultaneously for CH4 by gas chromatography continuous-flow isotope-ratio mass spectrometry

, and . RAPID COMMUNICATIONS IN MASS SPECTROMETRY, 18 (2): 175-180 (2004)
DOI: {10.1002/rcm.1311}

Abstract

A continuous-flow technique has been developed to analyse the deltaD and delta(13)C values for CH4 from gas samples, in a single run. This is achieved by splitting the sample gas stream and directing the streams simultaneously through a CuNiPt combustion reactor and an alumina pyrolysis reactor. The CO2 from CH4 combustion is trapped in a liquid nitrogen trap while the H-2 exiting the pyrolysis reactor is directed to the mass spectrometer for deltaD(CH4) determination. The CO2 is then sublimed and directed to the mass spectrometer for delta(13)C(CH4) determination. Sample runs take approximately 10 minutes. This technique gives accurate delta(13)C(CH4) results to within +/-0.3-0.5parts per thousand and deltaD(CH4) results to within +/-2-5parts per thousand. Injection volumes between 0.5 and 2.5 muL of CH4, equivalent to between 20 and 100 nmol CH4, are required for accurate delta(13)C and deltaD analyses, respectively, using sample injection into a split flow with a split ratio of 10. This method provides rapid, accurate and reproducible results on multiple sample runs and is, therefore, an ideal method for analysing natural gas samples from a variety of sources. Copyright (C) 2003 John Wiley Sons, Ltd.

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