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.MethodsWe 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.ResultsThe 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).ConclusionsThe methodological improvements significantly increase sample throughput without compromising analytical precision or accuracy down to 1 nmol of N.
Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Schedule a callDisclaimer: All third-party content on this website/platform is and will remain the property of their respective owners and is provided on "as is" basis without any warranties, express or implied. Use of third-party content does not indicate any affiliation, sponsorship with or endorsement by them. Any references to third-party content is to identify the corresponding services and shall be considered fair use under The CopyrightLaw.
