δ13C and δ15N analyses of solid, liquid and gaseous samples

Elemental Analysis – Isotope Ratio Mass Spectrometry (EA-IRMS)

Bulk material from soils, plants and other sources can be combusted quantitatively to CO2 (and other oxides if applicable). In a second step the produced NOx is reduced to elemental N2. Thus the δ15N and δ13C composition of carbon and nitrogen containing bulk samples can be analysed. Details on the analytical principles can be found in Brooks et al. (2003) and Werner et al. (1999). The BGC-IsoLab uses an EA (NA 1110, CE Instruments, Milan, Italy) coupled to a Delta+XL IRMS (Thermo Finnigan, Bremen, Germany) via a ConFlow III. The autosampler has been modified to allow the analysis of gaseous samples (e.g. CH4 or N2O). A 10-port valve with two 1 ml sample loops can be connected to the autosampler allowing the alternating measurements of gaseous samples with solid samples. In this way such samples can be standardised against solid primary standards (Mohn et al., 2016; Sperlich et al., 2016).

Solid samples and standards are weighed into tin-capsules so that the anticipated signal of each is of similar intensity. We aim for signal intensities around 6000 mV to improve measurement precision. Samples are standardised against in-house standards Acetylanilide (Ali-j3; δ13C: -30.06 ± 0.1 ‰, δ15N: -1.51 ± 0.1 ‰) and Caffeine (Caf-j3 ; δ13C: -40.46 ± 0.1 ‰, δ15N: -15.46 ± 0.1 ‰). See Figure 2 for the long term performance of the quality control measurements of caffeine. The details on the necessary post-measurement corrections and on the structure of a sample sequence can be found in Werner and Brand (2001).

Mohn, J., Gutjahr, W., Toyoda, S., Harris, E., Ibraim, E., Geilmann, H., Schleppi, P., Kuhn, T., Lehmann, M. F., Decock, C., Werner, R. A., Yoshida, N., and Brand, W. A.
Reassessment of the NH4NO3 thermal decomposition technique for calibration of the N2O isotopic composition.
Rapid Communications in Mass Spectrometry, 30, 2487-2496, 2016
Sperlich, P., Uitslag, N. A. M., Richter, J. M., Rothe, M., Geilmann, H., van der Veen, C., Röckmann, T., Blunier, T., and Brand, W. A.
Development and evaluation of a suite of isotope reference gases for methane in air.
Atmos. Meas. Tech., 9, 3717-3737, 2016
Brooks, P. D.; Geilmann, H.; Werner, R. A.; Brand, W. A.: Improved precision of coupled δ13C and δ15N measurements from single samples using an elemental analyzer/isotope ratio mass spectrometer combination with a post-column sixport valve and selective CO2 trapping; improved halide robustness of the combustion reactor using CeO2. Rapid Communications in Mass Spectrometry 17 (16), pp. 1924 - 1926 (2003)
Werner, R. A.; Brand, W. A.: Referencing strategies and techniques in stable isotope ratio analysis. Rapid Communications in Mass Spectrometry 15 (7), pp. 501 - 519 (2001)
Werner, R. A.; Bruch, B. A.; Brand, W. A.: ConFlo III - An interface for high precision δ 13C and δ 15N analysis with an extended dynamic range. Rapid Communications in Mass Spectrometry 13 (13), pp. 1237 - 1241 (1999)
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