scholarly journals Nitrogen isotope analysis of aqueous ammonium and nitrate by membrane inlet isotope ratio mass spectrometry (MIRMS) at natural abundance levels

Author(s):  
Jens Dyckmans ◽  
Wolfram Eschenbach ◽  
Reinhard Langel ◽  
Lars Szwec ◽  
Reinhard Well
Author(s):  
Xing Wang ◽  
Henk G. Jansen ◽  
Haico Duin ◽  
Harro A. J. Meijer

AbstractThere are two officially approved methods for stable isotope analysis for wine authentication. One describes δ18O measurements of the wine water using Isotope Ratio Mass Spectrometry (IRMS), and the other one uses Deuterium-Nuclear Magnetic Resonance (2H-NMR) to measure the deuterium of the wine ethanol. Recently, off-axis integrated cavity output (laser) spectroscopy (OA-ICOS) has become an easier alternative to quantify wine water isotopes, thanks to the spectral contaminant identifier (SCI). We utilized an OA-ICOS analyser with SCI to measure the δ18O and δ2H of water in 27 wine samples without any pre-treatment. The OA-ICOS results reveal a wealth of information about the growth conditions of the wines, which shows the advantages to extend the official δ18O wine water method by δ2H that is obtained easily from OA-ICOS. We also performed high-temperature pyrolysis and chromium reduction combined with IRMS measurements to illustrate the “whole wine” isotope ratios. The δ18O results of OA-ICOS and IRMS show non-significant differences, but the δ2H results of both methods differ much more. As the δ2H difference between these two methods is mainly caused by ethanol, we investigated the possibility to deduce deuterium of wine ethanol from this difference. The results present large uncertainties and deviate from the obtained 2H-NMR results. The deviation is caused by the other constituents in the wine, and the uncertainty is due to the limited precision of the SCI-based correction, which need to improve to obtain the 2H values of ethanol as alternative for the 2H-NMR method.


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.


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