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  Analytical improvements and assessment of long-term performance of the oxidation-denitrifier method

Moretti, S., Duprey, N. N., Foreman, A. D., Arns, A., Brömme, S., Jung, J., et al. (2024). Analytical improvements and assessment of long-term performance of the oxidation-denitrifier method. Rapid Communications in Mass Spectrometry, 38(1): e9650. doi:10.1002/rcm.9650.

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 Urheber:
Moretti, Simone1, Autor           
Duprey, Nicolas N.1, Autor           
Foreman, Alan D.1, Autor           
Arns, Anthea1, Autor           
Brömme, Sven1, Autor           
Jung, Jonathan1, Autor           
Ai, Xuyuan E.1, Autor           
Auderset, Alexandra1, Autor           
Bieler, Aaron L.1, Autor           
Eck, Camino1, Autor           
Farmer, Jesse1, Autor           
Hinnenberg, Barbara1, Autor           
Lacerra, Matthew1, Autor           
Leichliter, Jennifer1, Autor           
Lüdecke, Tina1, Autor           
Oleynik , Sergey2, Autor
Rubach, Florian3, Autor           
Schmitt, Mareike1, Autor           
Vink, Marissa2, Autor
Wald, Tanja1, Autor           
Yehudai, Maayan1, Autor           Sigman , Daniel M.2, AutorMartinez-Garcia, Alfredo1, Autor            mehr..
Affiliations:
1Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society, ou_2237635              
2external, ou_persistent22              
3Particle Chemistry, Max Planck Institute for Chemistry, Max Planck Society, ou_1826291              

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 Zusammenfassung:

The analysis of the nitrogen (N) isotopic composition of organic matter bound to fossil biomineral structures (BB-δ15N) using the oxidation–denitrifier (O–D) method provides a novel tool to study past changes in N cycling processes.
Methods

We report a set of methodological improvements to the O–D method, including (a) a method for sealing the reaction vials in which the oxidation of organic N to NO3− takes place, (b) a recipe for bypassing the pH adjustment step before the bacterial conversion of NO3− to N2O, and (c) a method for storing recrystallized dipotassium peroxodisulfate (K2S2O8) under Ar atmosphere.
Results

The new sealing method eliminates the occasional contamination and vial breakage that occurred previously while increasing sample throughput. The protocol for bypassing pH adjustment does not affect BB-δ15N, and it significantly reduces the processing time. Storage of K2S2O8 reagent under Ar atmosphere produces stable oxidation blanks over more than 3.5 years. We report analytical blanks, accuracy, and precision for this methodology from eight users over the course of ~3.5 years of analyses at the Max Planck Institute for Chemistry. Our method produces analytical blanks characterized by low N content (0.30 ± 0.13 nmol N, 1σ, n = 195) and stable δ15N (−2.20 ± 3.13‰, n = 195). The analysis of reference amino acid standards USGS 40 and USGS 65 indicates an overall accuracy of −0.23 ± 0.35‰ (1σ, n = 891). The analysis of in-house fossil standards gives similar analytical precision (1σ) across a range of BB-δ15N values and biominerals: zooxanthellate coral standard PO-1 (6.08 ± 0.21‰, n = 267), azooxanthellate coral standard LO-1 (10.20 ± 0.28‰, n = 258), foraminifera standard MF-1 (5.92 ± 0.28‰, n = 243), and tooth enamel AG-Lox (4.06 ± 0.49‰, n = 78).
Conclusions

The methodological improvements significantly increase sample throughput without compromising analytical precision or accuracy down to 1 nmol of N.

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Sprache(n): eng - English
 Datum: 2023-12-062024
 Publikationsstatus: Erschienen
 Seiten: -
 Ort, Verlag, Ausgabe: -
 Inhaltsverzeichnis: -
 Art der Begutachtung: -
 Identifikatoren: ISI: 001121271200001
DOI: 10.1002/rcm.9650
 Art des Abschluß: -

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Titel: Rapid Communications in Mass Spectrometry
  Andere : Rapid Commun. Mass Spectrom.
Genre der Quelle: Zeitschrift
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Ort, Verlag, Ausgabe: New York, NY : John Wiley & Sons
Seiten: 19 Band / Heft: 38 (1) Artikelnummer: e9650 Start- / Endseite: - Identifikator: ISSN: 0951-4198
CoNE: https://pure.mpg.de/cone/journals/resource/954925574961