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Title: Preliminary assessment of stable nitrogen and oxygen isotopic composition of USGS51 and USGS52 nitrous oxide reference gases and perspectives on calibration needs

Abstract

Rationale: Despite a long history and growing interest in isotopic analyses of N 2O, there is a lack of isotopically characterized N 2O isotopic reference materials (standards) to enable normalization and reporting of isotope-delta values. Here, in this paper we report the isotopic characterization of two pure N 2O gas reference materials, USGS51 and USGS52, which are now available for laboratory calibration (https://isotopes.usgs.gov/lab/referencematerials.html). Methods: A total of 400 sealed borosilicate glass tubes of each N 2O reference gas were prepared from a single gas filling of a high vacuum line. We demonstrated isotopic homogeneity via dual-inlet isotope-ratio mass spectrometry. Isotopic analyses of these reference materials were obtained from eight laboratories to evaluate interlaboratory variation and provide preliminary isotopic characterization of their δ 15N, δ 18O, δ 15N α, δ 15N β and site preference (S P) values. Results: The isotopic homogeneity of both USGS51 and USGS52 was demonstrated by one-sigma standard deviations associated with the determinations of their δ 15N, δ 18O, δ 15N α, δ 15N β and S P values of 0.12 mUr or better. The one-sigma standard deviations of SP measurements of USGS51 and USGS52 reported by eight laboratories participating in the interlaboratory comparison were 1.27 andmore » 1.78 mUr, respectively. Conclusions: The agreement of isotope-delta values obtained in the interlaboratory comparison was not sufficient to provide reliable accurate isotope measurement values for USGS51 and USGS52. Lastly, we propose that provisional values for the isotopic composition of USGS51 and USGS52 determined at the Tokyo Institute of Technology can be adopted for normalizing and reporting sample data until further refinements are achieved through additional calibration efforts.« less

Authors:
ORCiD logo [1];  [1];  [2];  [3];  [2];  [4];  [5]; ORCiD logo [6];  [7];  [8];  [7];  [8];  [9]
  1. Michigan State Univ., East Lansing, MI (United States)
  2. U.S. Geological Survey, Reston VA (United States)
  3. Tokyo Institute of Technology, Yokohama (Japan)
  4. Max-Planck-Institute for Biogeochemistry, Jena (Germany)
  5. Stanford Univ., CA (United States)
  6. Centre for Stable Isotope Research and Analysis (Germany)
  7. University Göttingen (Germany); Thünen Institut of Climate‐Smart Agriculture, Braunschweig (Germany)
  8. Laboratory for Air Pollution & Environmental Technology, Empa, Dubendorf (Switzerland)
  9. Tokyo Institute of Technology (Japan)
Publication Date:
Research Org.:
Great Lakes Bioenergy Research Center, Madison, WI (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Biological and Environmental Research (BER) (SC-23)
Contributing Org.:
European Metrology Programme for Innovation and Research (EMPIR)
OSTI Identifier:
1506057
Grant/Contract Number:  
SC0018409; FC02‐07ER64494
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
Rapid Communications in Mass Spectrometry
Additional Journal Information:
Journal Volume: 32; Journal Issue: 15; Journal ID: ISSN 0951-4198
Publisher:
Wiley
Country of Publication:
United States
Language:
English
Subject:
59 BASIC BIOLOGICAL SCIENCES; 54 ENVIRONMENTAL SCIENCES

Citation Formats

Ostrom, Nathaniel E., Gandhi, Hasand, Coplen, Tyler B., Toyoda, Sakae, Böhlke, J. K., Brand, Willi A., Casciotti, Karen L., Dyckmans, Jens, Giesemann, Anette, Mohn, Joachim, Well, Reinhard, Yu, Longfei, and Yoshida, Naohiro. Preliminary assessment of stable nitrogen and oxygen isotopic composition of USGS51 and USGS52 nitrous oxide reference gases and perspectives on calibration needs. United States: N. p., 2018. Web. doi:10.1002/rcm.8157.
Ostrom, Nathaniel E., Gandhi, Hasand, Coplen, Tyler B., Toyoda, Sakae, Böhlke, J. K., Brand, Willi A., Casciotti, Karen L., Dyckmans, Jens, Giesemann, Anette, Mohn, Joachim, Well, Reinhard, Yu, Longfei, & Yoshida, Naohiro. Preliminary assessment of stable nitrogen and oxygen isotopic composition of USGS51 and USGS52 nitrous oxide reference gases and perspectives on calibration needs. United States. doi:10.1002/rcm.8157.
Ostrom, Nathaniel E., Gandhi, Hasand, Coplen, Tyler B., Toyoda, Sakae, Böhlke, J. K., Brand, Willi A., Casciotti, Karen L., Dyckmans, Jens, Giesemann, Anette, Mohn, Joachim, Well, Reinhard, Yu, Longfei, and Yoshida, Naohiro. Fri . "Preliminary assessment of stable nitrogen and oxygen isotopic composition of USGS51 and USGS52 nitrous oxide reference gases and perspectives on calibration needs". United States. doi:10.1002/rcm.8157. https://www.osti.gov/servlets/purl/1506057.
@article{osti_1506057,
title = {Preliminary assessment of stable nitrogen and oxygen isotopic composition of USGS51 and USGS52 nitrous oxide reference gases and perspectives on calibration needs},
author = {Ostrom, Nathaniel E. and Gandhi, Hasand and Coplen, Tyler B. and Toyoda, Sakae and Böhlke, J. K. and Brand, Willi A. and Casciotti, Karen L. and Dyckmans, Jens and Giesemann, Anette and Mohn, Joachim and Well, Reinhard and Yu, Longfei and Yoshida, Naohiro},
abstractNote = {Rationale: Despite a long history and growing interest in isotopic analyses of N2O, there is a lack of isotopically characterized N2O isotopic reference materials (standards) to enable normalization and reporting of isotope-delta values. Here, in this paper we report the isotopic characterization of two pure N2O gas reference materials, USGS51 and USGS52, which are now available for laboratory calibration (https://isotopes.usgs.gov/lab/referencematerials.html). Methods: A total of 400 sealed borosilicate glass tubes of each N2O reference gas were prepared from a single gas filling of a high vacuum line. We demonstrated isotopic homogeneity via dual-inlet isotope-ratio mass spectrometry. Isotopic analyses of these reference materials were obtained from eight laboratories to evaluate interlaboratory variation and provide preliminary isotopic characterization of their δ15N, δ18O, δ15Nα, δ15Nβ and site preference (SP) values. Results: The isotopic homogeneity of both USGS51 and USGS52 was demonstrated by one-sigma standard deviations associated with the determinations of their δ15N, δ18O, δ15Nα, δ15Nβ and SP values of 0.12 mUr or better. The one-sigma standard deviations of SP measurements of USGS51 and USGS52 reported by eight laboratories participating in the interlaboratory comparison were 1.27 and 1.78 mUr, respectively. Conclusions: The agreement of isotope-delta values obtained in the interlaboratory comparison was not sufficient to provide reliable accurate isotope measurement values for USGS51 and USGS52. Lastly, we propose that provisional values for the isotopic composition of USGS51 and USGS52 determined at the Tokyo Institute of Technology can be adopted for normalizing and reporting sample data until further refinements are achieved through additional calibration efforts.},
doi = {10.1002/rcm.8157},
journal = {Rapid Communications in Mass Spectrometry},
issn = {0951-4198},
number = 15,
volume = 32,
place = {United States},
year = {2018},
month = {5}
}

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