USGS44, a new high purity calcium carbonate reference material for δ13 C measurements

Qi, H., Moossen, H., Meijer, H. A. J., Coplen, T. B., Aerts-Bijma, A. T., Reid, L., Geilmann, H., Richter, J., Rothe, M., Brand, W. A., Toman, B., Benefield, J. & Hélie, J-F., 17-Nov-2020, In : Rapid Communications in Mass Spectrometry. 35, 4, e9006.

Research output: Contribution to journalArticleAcademicpeer-review

  • Haiping Qi
  • Heiko Moossen
  • Harro A J Meijer
  • Tyler B Coplen
  • Anita T Aerts-Bijma
  • Lauren Reid
  • Heike Geilmann
  • Jürgen Richter
  • Michael Rothe
  • Willi A Brand
  • Blaza Toman
  • Jacqueline Benefield
  • Jean-François Hélie

RATIONALE: The stable carbon isotopic (δ13 C) reference material (RM) LSVEC Li2 CO3 has been found to be unsuitable for δ13 C standardization work because its δ13 C value increases with exposure to atmospheric CO2 . A new CaCO3 RM, USGS44, has been prepared to alleviate this situation.

METHODS: USGS44 was prepared from 8 kg of Merck high purity CaCO3 . Two sets of δ13 C values of USGS44 were determined. The first set of values was determined by on-line combustion, continuous-flow (CF) isotope-ratio mass spectrometry (IRMS) of NBS 19 CaCO3 (δ13 CVPDB = +1.95 milliurey (mUr) exactly, where mUr = 0.001 = 1 ‰), and LSVEC Li2 CO3 (δ13 CVPDB = -46.6 mUr exactly), and normalized to the two-anchor δ13 CVPDB-LSVEC isotope-delta scale. The second set of values was obtained by dual-inlet (DI) IRMS of CO2 evolved by reaction of H3 PO4 with carbonates, corrected for cross contamination, and normalized to the single anchor δ13 CVPDB scale.

RESULTS: USGS44 is stable and isotopically homogeneous to within 0.02 mUr in 100-μg amounts. It has a δ13 CVPDB-LSVEC value of -42.21 ± 0.05 mUr. Single-anchor δ13 CVPDB values of -42.08 ± 0.01 and -41.99 ± 0.02 mUr were determined by DI-IRMS with corrections for cross contamination.

CONCLUSIONS: The new high-purity, well homogenized calcium carbonate isotopic reference material USGS44 is stable and has a δ13 CVPDB-LSVEC value of -42.21 ± 0.05 mUr for both EA-IRMS and DI-IRMS measurements. As a carbonate relatively depleted in 13 C, it is intended for daily use as a secondary isotopic reference material to normalize stable carbon isotope-delta measurements to the δ13 CVPDB-LSVEC scale. It is useful in quantifying drift with time, determining mass-dependent isotopic fractionation (linearity correction), and adjusting isotope-ratio-scale contraction. Due to its fine grain size (smaller than 63 μm), it is not suitable as a δ18 O reference material. A δ13 CVPDB-LSVEC value of -29.99 ± 0.05 mUr was determined for NBS 22 oil.

Original languageEnglish
Article numbere9006
JournalRapid Communications in Mass Spectrometry
Issue number4
Publication statusE-pub ahead of print - 17-Nov-2020

ID: 146585487