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

Moretti, Simone; Duprey, Nicolas N.; Foreman, Alan D.; Arns, Anthea; Brömme, Sven; Jung, Jonathan; Ai, Xuyuan E.; Auderset, Alexandra; Bieler, Aaron L.; Eck, Camino; Farmer, Jesse; Hinnenberg, Barbara; Lacerra, Matthew; Leichliter, Jennifer; Lüdecke, Tina; Oleynik , Sergey; Rubach, Florian; Schmitt, Mareike; Vink, Marissa; Wald, Tanja; Yehudai, Maayan; Sigman , Daniel M.; Martinez-Garcia, Alfredo

doi:10.1002/rcm.9650

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

MPS-Authors

/persons/resource/persons246381

Moretti, Simone
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons209287

Duprey, Nicolas N.
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons280805

Foreman, Alan D.
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons273227

Arns, Anthea
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons290266

Brömme, Sven
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons280803

Jung, Jonathan
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons290269

Ai, Xuyuan E.
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons231504

Auderset, Alexandra
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons290271

Bieler, Aaron L.
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons290273

Eck, Camino
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons252335

Farmer, Jesse
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons290275

Hinnenberg, Barbara
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons290277

Lacerra, Matthew
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons273240

Leichliter, Jennifer
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons258064

Lüdecke, Tina
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons192183

Rubach, Florian
Particle Chemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons252051

Schmitt, Mareike
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons280807

Wald, Tanja
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons290281

Yehudai, Maayan
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

/persons/resource/persons192213

Martinez-Garcia, Alfredo
Climate Geochemistry, Max Planck Institute for Chemistry, Max Planck Society;

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https://onlinelibrary.wiley.com/doi/pdfdirect/10.1002/rcm.9650
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Citation

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.

Cite as: https://hdl.handle.net/21.11116/0000-000E-51B8-7

Abstract

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.