1. Analytical improvements and assessment of long-term performance of the oxidation-denitrifier method
- Author
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Moretti, S., Duprey, N., Foreman, A., Arns, A., Brömme, S., Jung, J., Ai, X., Auderset, A., Bieler, A., Eck, C., Farmer, J., Hinnenberg, B., Lacerra, M., Leichliter, J., Lüdecke, T., Oleynik, S., Rubach, F., Schmitt, M., Vink, M., Wald, T., Yehudai, M., Sigman , D., and Martinez-Garcia, A.
- Abstract
RATIONALE The analysis of the nitrogen (N) isotopic composition of organic matter bound to30fossil biomineral structures (BB-δ 15 N) using the oxidation-denitrifier (O-D) method provides anovel tool to study past changes in N cycling processes.METHODS We report a set of methodological improvements to the O-D method, including: (i) amethod for sealing the reaction vials in which oxidation of organic N to NO3- takes place; (ii) arecipe for bypassing the pH adjustment step before the bacterial conversion of NO3- to N2 O; and35(iii) a storage method of recrystallized dipotassium peroxodisulphate (K2 S 2 O8 ) under Aratmosphere.RESULTS The new method eliminates the occasional contamination and vial breakage, andincreases sample throughput. The protocol for bypassing of pH adjustment does not affect BB-δ 15 N, and it significantly reduces processing time. Storage of K2 S2 O8 reagent under Ar atmosphere40produces stable oxidation blanks over more than two years. We report analytical blanks, accuracyand precision for this methodology from eight users over the course of ~ 3.5 years of analyses atthe Max Planck Institute for Chemistry. Our method produces analytical blanks characterized bylow N content (0.30 ± 0.13 nmol N, 1σ, n=204) and stable δ 15 N (– 2.45 ± 3.50 ‰, n=204). Theanalysis of reference amino acid standards USGS40 and USGS65 indicates an overall accuracy of45– 0.23 ± 0.35 ‰ (1σ, n=891). The analysis of in-house fossil standards gives similar analyticalprecision (1σ) across a range of BB-δ 15 N values and biominerals: zooxanthellate coral standardPO-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).50CONCLUSIONS The proposed analytical improvements significantly increase samplethroughput without compromising analytical precision or accuracy down to 1 nmol of N. Submitted to Rapid Communications in Mass Spectrometry
- Published
- 2023