A rapid method for the preparation of combustion samples for stable carbon isotope analysis by isotope ratio mass spectrometry

1988 ◽  
Vol 16 (1-12) ◽  
pp. 269-273 ◽  
Author(s):  
Brian A. McGaw ◽  
Eric Milne ◽  
Gary J. Duncan
2013 ◽  
Vol 6 (5) ◽  
pp. 1425-1445 ◽  
Author(s):  
J. Schmitt ◽  
B. Seth ◽  
M. Bock ◽  
C. van der Veen ◽  
L. Möller ◽  
...  

Abstract. Stable carbon isotope analysis of methane (δ13C of CH4) on atmospheric samples is one key method to constrain the current and past atmospheric CH4 budget. A frequently applied measurement technique is gas chromatography (GC) isotope ratio mass spectrometry (IRMS) coupled to a combustion-preconcentration unit. This report shows that the atmospheric trace gas krypton (Kr) can severely interfere during the mass spectrometric measurement, leading to significant biases in δ13C of CH4, if krypton is not sufficiently separated during the analysis. According to our experiments, the krypton interference is likely composed of two individual effects, with the lateral tailing of the doubly charged 86Kr peak affecting the neighbouring m/z 44 and partially the m/z 45 Faraday cups. Additionally, a broad signal affecting m/z 45 and especially m/z 46 is assumed to result from scattered ions of singly charged krypton. The introduced bias in the measured isotope ratios is dependent on the chromatographic separation, the krypton-to-CH4 mixing ratio in the sample, the focusing of the mass spectrometer as well as the detector configuration and can amount to up to several per mil in δ13C. Apart from technical solutions to avoid this interference, we present correction routines to a posteriori remove the bias.


2013 ◽  
Vol 6 (1) ◽  
pp. 1409-1460 ◽  
Author(s):  
J. Schmitt ◽  
B. Seth ◽  
M. Bock ◽  
C. van der Veen ◽  
L. Möller ◽  
...  

Abstract. Stable carbon isotope analysis of methane (δ13C of CH4) on atmospheric samples is one key method to constrain the current and past atmospheric CH4 budget. A frequently applied measurement technique is gas chromatography isotope ratio mass spectrometry coupled to a combustion-preconcentration unit. This report shows that the atmospheric trace gas krypton can severely interfere during the mass spectrometric measurement leading to significant biases in δ13C of CH4 if krypton is not sufficiently separated during the analysis. The effect comes about by the lateral tailing of the peak of doubly charged 86Kr in the neighbouring m/z, 44, 45, and 46 Faraday cups. Accordingly, the introduced bias is dependent on the chromatographic separation, the Kr to CH4 mixing ratio in the sample, the mass spectrometer source tuning as well as the detector configuration and can amount to up to several permil in δ13C. Apart from technical solutions to avoid this interference we present correction routines to a posteriori remove the bias.


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