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Huygens, D.; Boeckx, P.; Vermeulen, J.; Paepe, X. De; Park, A.; Barker, S.; Pullan, C.; Cleemput, O. Van

Advances in coupling a commercial total organic carbon analyser with an isotope ratio mass spectrometer to determine the isotopic signal of the total dissolved nitrogen pool

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  • Medientyp: E-Artikel
  • Titel: Advances in coupling a commercial total organic carbon analyser with an isotope ratio mass spectrometer to determine the isotopic signal of the total dissolved nitrogen pool
  • Beteiligte: Huygens, D.; Boeckx, P.; Vermeulen, J.; Paepe, X. De; Park, A.; Barker, S.; Pullan, C.; Cleemput, O. Van
  • Erschienen: Wiley, 2005
  • Erschienen in: Rapid Communications in Mass Spectrometry
  • Sprache: Englisch
  • DOI: 10.1002/rcm.2178
  • ISSN: 0951-4198; 1097-0231
  • Schlagwörter: Organic Chemistry ; Spectroscopy ; Analytical Chemistry
  • Entstehung:
  • Anmerkungen:
  • Beschreibung: <jats:title>Abstract</jats:title><jats:p>A new method has been developed to analyse <jats:sup>15</jats:sup>N of the total dissolved nitrogen (TDN) pool. The method operates on a commercial total organic carbon (TOC) analyser coupled to an elemental analyser/isotope ratio mass spectrometer (EA‐IRMS). Nitrogen compounds are combusted to nitric oxide (NO) and nitrogen dioxide (NO<jats:sub>2</jats:sub>) by high‐temperature catalytic oxidation (HTCO), after which the NO<jats:sub>x</jats:sub> gas is transferred to an EA‐IRMS for isotopic nitrogen analysis. The system is described, including five modifications of the system in order to overcome analytical problems. First, flow paths were modified to run both systems on helium as carrier gas, while complete sample oxidation was maintained. Secondly, the catalyst structure was adapted to allow high injection volumes at the given backpressures delivered by the EA system. Thirdly, we installed a Permapure® dehumidification system as the standard Peltier element did not satisfy dehumidification requirements. Finally, we prevented the inflow of atmospheric nitrogen into the system. In a final stage, we are planning to automate the coupled system in order to run a continuous batch of up to 60 samples. We have obtained satisfactory results on the accuracy and precision of 180 ± 1‰ potassium nitrate samples (IAEA, USGS‐32). Running a batch of five samples resulted in a mean isotopic value of 178.8‰ with a standard deviation of 2.8‰. Some important issues could not yet be addressed here, and will have to be evaluated once the system is running on a continuous base. However, the results appear promising and this system has the potential to become a method for TD<jats:sup>15</jats:sup>N analysis. An appropriate TD<jats:sup>15</jats:sup>N analysis method might open new challenges in aquatic and terrestrial ecosystem nitrogen studies, including a more comprehensive study of the dissolved organic nitrogen pool. Copyright © 2005 John Wiley &amp; Sons, Ltd.</jats:p>