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

Ostrom, Nathaniel E. (Department of Integrative Biology and DOE Great Lakes Bioenergy Research Institute, Michigan State University, East Lansing, MI, USA ) ; Gandhi, Hasand (Department of Integrative Biology and DOE Great Lakes Bioenergy Research Institute, Michigan State University, East Lansing, MI, USA ) ; Coplen, Tyler B. (U.S. Geological Survey, 431 National Center, Reston, VA, USA ) ; Toyoda, Sakae (Department of Chemical Science and Engineering, School of Materials and Chemical Technology, Tokyo Institute of Technology, Yokohama, 226‐8502, Japan ) ; Böhlke, J.K. (U.S. Geological Survey, 431 National Center, Reston, VA, USA ) ; Brand, Willi A. (Beutenberg Campus, Max‐Planck‐Institute for Biogeochemistry, P.O. Box 100164, 07701, Jena, Germany ) ; Casciotti, Karen L. (Department of Earth System Science, Stanford University, Stanford, CA, USA ) ; Dyckmans, Jens ; Giesemann, Anette ; Mohn, Joachim ; Well, Reinhard ; Yu, Longfei ; Yoshida, Naohiro ;
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    Rationale Despite a long history and growing interest in isotopic analyses of N 2 O, there is a lack of isotopically characterized N 2 O isotopic reference materials (standards) to enable normalization and reporting of isotope‐delta values. Here we report the isotopic characterization of two pure N 2 O 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 2 O 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 15 N, δ 18 O, δ 15 N α , δ 15 N 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 15 N, δ 18 O, δ 15 N α , δ 15 N β and S P values of 0.12 mUr or better. The one‐sigma standard deviations of S P 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. 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.


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