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Effects of Improved 17 O Correction on Interlaboratory Agreement in Clumped Isotope Calibrations, Estimates of Mineral‐Specific Offsets, and Temperature Dependence of Acid Digestion Fractionation
Open accessAbstract
The clumped isotopic composition of carbonate‐derived CO 2 (denoted Δ 47 ) is a function of carbonate formation temperature and in natural samples can act as a recorder of paleoclimate, burial, or diagenetic conditions. The absolute abundance of heavy isotopes in the universal standards VPDB and VSMOW (defined by four parameters: R 13 VPDB , R 17 VSMOW , R 18 VSMOW , and λ ) impact calculated Δ 47 values. Here, we investigate whether use of updated and more accurate values for these parameters can remove observed interlaboratory differences in the measured T‐Δ 47 relationship. Using the updated parameters, we reprocess 14 published calibration data sets measured in 11 different laboratories, representing many mineralogies, bulk compositions, sample types, reaction temperatures, and sample preparation and analysis methods. Exploiting this large composite data set ( n = 1,253 sample replicates), we investigate the possibility for a “universal” clumped isotope calibration. We find that applying updated parameters improves the T‐Δ 47 relationship (reduces residuals) within most labs and improves overall agreement but does not eliminate all interlaboratory differences. We reaffirm earlier findings that different mineralogies do not require different calibration equations and that cleaning procedures, method of pressure baseline correction, and mass spectrometer type do not affect interlaboratory agreement. We also present new estimates of the temperature dependence of the acid digestion fractionation for Δ 47 (Δ* 25‐X ), based on combining reprocessed data from four studies, and new theoretical equilibrium values to be used in calculation of the empirical transfer function. Overall, we have ruled out a number of possible causes of interlaboratory disagreement in the T‐Δ 47 relationship, but many more remain to be investigated.
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“The CDES-referenced calibration of Petersen et al. (2019) is a compilation and recalculation of existing data [n = 132 samples (>1,200 replicate analyses) from 11 laboratories] spanning 4-800°C generated prior to the establishment of I-CDES.”
From Frontiers of Carbonate Clumped Isotope Thermometry (2023) · cites this paper as Petersen et al. 2019
Experimental — accuracy not yet measuredThe source backs part of the claim, not all of it — or backs it for a different population, condition or comparison.
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“The contribution from Ti calibration uncertainty is small compared to the contribution from sample and reference frame measurements (e.g., Petersen et al. 2019, figure 8).”
From Frontiers of Carbonate Clumped Isotope Thermometry (2023) · cites this paper as Petersen et al. 2019
Experimental — accuracy not yet measuredThe source backs part of the claim, not all of it — or backs it for a different population, condition or comparison.
In the citing paper
“Up to 1-2°C external precision (2 standard error of the mean) can be achieved with extensive replication (e.g., Petersen et al. 2019).”
From Frontiers of Carbonate Clumped Isotope Thermometry (2023) · cites this paper as Petersen et al. 2019
Experimental — accuracy not yet measuredThe source backs part of the claim, not all of it — or backs it for a different population, condition or comparison.
In the citing paper
“Theoretical equilibrium i values of clumped molecules increase with decreasing temperature (T ).”
From Frontiers of Carbonate Clumped Isotope Thermometry (2023) · cites this paper as Petersen et al. (2019)
Experimental — accuracy not yet measuredThe source backs part of the claim, not all of it — or backs it for a different population, condition or comparison.
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“These two calibrations are offset from each other by 3°C near 25°C and 7°C near 100°C and show a similar temperature dependence as the 47 theoretical equilibrium calculations of Schauble et al. (2006) and Hill et al. (2014) (difference of ∼2°C at Earth surface temperatures).”
From Frontiers of Carbonate Clumped Isotope Thermometry (2023) · cites this paper as Petersen et al. (2019)
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“However, the results of InterCarb, and the discussions in the literature (e.g., Petersen et al., 2019) show that with the HG/EG approach there are still poorly understood interlaboratory discrepancies (as suggested by Figure 6) which are absent in the carbonate‐based normalization (see Figure 5).”
From InterCarb: A Community Effort to Improve Interlaboratory Standardization of the Carbonate Clumped Isotope Thermometer Using Carbonate Standards (2021) · cites this paper as Petersen et al., 2019
Experimental — accuracy not yet measuredThe source backs part of the claim, not all of it — or backs it for a different population, condition or comparison.
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“The comparison of calibrations established in different laboratories, however, remains challenging, because of many factors: the lack of carbonate standards to compare across laboratories, the fact that clumped isotope data pre-2016 are not calculated using the”
From Calibration of the oxygen and clumped isotope thermometers for (proto-)dolomite based on synthetic and natural carbonates (2019) · cites this paper as Petersen et al., 2019
Experimental — accuracy not yet measuredThe source backs part of the claim, not all of it — or backs it for a different population, condition or comparison.
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“the statistical evaluation of the Winkelstern et al. (2016) dataset reevaluated in Petersen et al. (2019) for 75 °C acid digestion is significantly different in slope (p value of 0.0395) and intercept to the re-evaluated ETH calcite calibration dataset.”
From Calibration of the oxygen and clumped isotope thermometers for (proto-)dolomite based on synthetic and natural carbonates (2019) · cites this paper as Petersen et al., 2019
Experimental — accuracy not yet measuredThe cited source says what the claim attributes to it.
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“Numerous studies have produced empirical T-47 calibrations that relate i values measured in natural, synthetic, biogenic, and abiogenic carbonates of different mineralogies to their known growth temperatures (e.g., Petersen et al. 2019, and references therein) (Figure 3).”
From Frontiers of Carbonate Clumped Isotope Thermometry (2023) · cites this paper as Petersen et al. 2019
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“The result of this study was that differences among calibrations were reduced but not eliminated by the recalculation, implying that other factors must be responsible for the remaining discrepancies.”
From InterCarb: A Community Effort to Improve Interlaboratory Standardization of the Carbonate Clumped Isotope Thermometer Using Carbonate Standards (2021) · cites this paper as Petersen et al. (2019)
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“The theoretical values linking measurements to theory were calculated by Wang et al. (2004) and revised by Petersen et al. (2019).”
From InterCarb: A Community Effort to Improve Interlaboratory Standardization of the Carbonate Clumped Isotope Thermometer Using Carbonate Standards (2021) · cites this paper as Petersen et al. (2019)
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“Among the factors responsible for discrepant calibrations and laboratory comparability, two important ones cannot be tested with a gas‐based standardization: (1) the absolute value and temperature dependence of the phosphoric acid fractionation factor (see Petersen et al., 2019 for a recent compilation) and (2) possible CO2 equilibration effects during acid digestion of the sample.”
From InterCarb: A Community Effort to Improve Interlaboratory Standardization of the Carbonate Clumped Isotope Thermometer Using Carbonate Standards (2021) · cites this paper as Petersen et al., 2019
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“The weighted averages of the four standards (projected to 90 °C for the reactions at 25 and 70 °C using the acid temperature correction suggested by Petersen et al., 2019), comprising 873 analyses of the carbonate standards and 946 heated and equilibrated gases from 10 different laboratories, are reported in Table 1 and Figure 2.”
From InterCarb: A Community Effort to Improve Interlaboratory Standardization of the Carbonate Clumped Isotope Thermometer Using Carbonate Standards (2021) · cites this paper as Petersen et al., 2019
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“The phosphoric acid reaction of the carbonate to CO 2 produces a temperature-dependent isotopic fractionation whose temperature dependence is relatively well constrained for calcite (e.g.Defliese et al., 2015;Murray et al., 2016;Petersen et al., 2019) but not for dolomite.”
From Calibration of the oxygen and clumped isotope thermometers for (proto-)dolomite based on synthetic and natural carbonates (2019) · cites this paper as Petersen et al., 2019
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“The effect on the recalculated temperatures in older publications is difficult to predict without a full recalculation that includes all heated and equilibrated gases measured with the samples (Petersen et al., 2019).”
From Calibration of the oxygen and clumped isotope thermometers for (proto-)dolomite based on synthetic and natural carbonates (2019) · cites this paper as Petersen et al., 2019
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“Δ47 values require correction to account for the effects of the removal of one oxygen atom during acid digestion (conversion of CaCO3 to CO2), which cause an increase in Δ47 values relative to corresponding Δ63 values in the carbonate phase (Bonifacie et al., 2017; Guo et al., 2009; Schauble et al., 2006).”
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“Since these early studies, the clumped isotope proxy has been applied to various geological archives and there have been significant advances in calibrations, analytical developments, standardization, and data reduction efforts (Bernasconi et al., 2021; Daëron, 2021; Daëron et al., 2016; Dennis et al., 2011; Fernandez…”
BackgroundMethodResultInfluentialSelf-citationCalibration of the carbonate clumped isotope thermometer of land snail shells
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Experimental Constraints on Clumped Isotope Fractionation During BaCO3 Precipitation
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“Applied Chemistry recommended parameters for 17O correction (Brand et al., 2010; Daëron et al., 2016; Petersen et al., 2019).”
MethodComparative clumped isotope temperature relationships in freshwater carbonates
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“For samples at 90°C, an acid fractionation factor of 0.088‰ was used to project into the CDES reference frame at 25°C (Petersen et al., 2019).”
InfluentialSelf-citationHABITAT OF THE NASCENT CHICXULUB CRATER
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“All data were collected prior to the establishment of current background and 17O correction procedures (Bernasconi et al., 2018; Peterson et al., 2019), which can result in higher analytical uncertainties than present.”
BackgroundTraditional Stable Isotope Geochemistry
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Clumped isotope analysis of (bio)apatite using a Kiel IV device in long‐integration dual‐inlet mode
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Self-citationRecent Efforts to Improve the Accuracy and Precision of Carbonate Clumped‐Isotope Analysis
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“Petersen et al. (2019) confirmed that recalculating 14 calibration data points measured in 11 different laboratories using IUPAC parameters reduced the errors in clumped isotope thermometry.”
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Self-citationThe Quaternary landscapes, chronostratigraphy, and paleoenvironments of the Chalbi Desert, Kenya
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“Clumped isotope temperatures ( T (Δ 47 )) are calculated using the temperature calibration of Petersen et al. (2019).”
Self-citationShallow-water temperature seasonality in the middle Cretaceous mid-latitude northwestern Pacific
Ichimura, S., Takayanagi, H., Iryu, Y., Takahashi, S., & Oji, T. (2024) · Frontiers in Marine Science · doi:10.3389/fmars.2024.1324436 · Cited by 2
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Self-citationHollis, S., Dennis, P., Menuge, J., Doran, A., Marca, A., Davidheiser-Kroll, B., Wilkinson, J. J., Snell, K., Turner, O., Güven, J. F., et al. (2024) · Economic Geology · doi:10.5382/econgeo.5100 · Cited by 1
Jon, J., Sierra, V., & Matthew, M. (2025) · Palaeogeography, Palaeoclimatology, Palaeoecology · doi:10.1016/j.palaeo.2025.112778 · Cited by 2
Self-citationA Terrestrial Thermometer Using Carbonate Clumped Isotopes From Gar Scales
Gray, K. E., & Brandon, M. T. (2025) · Geochemistry Geophysics Geosystems · doi:10.1029/2024gc011714 · Cited by 2
“We were initially surprised to find that our gar scale data have a T –Δ 47 relationship three times steeper than other published T –Δ 47 calibrations (Anderson et al., 2021; compilation by Petersen et al., 2019).”
InfluentialD4Xgui: A tool for baseline correction and standardization of carbonate clumped isotope raw data
Bernecker, M., Daëron, M., Staudigel, P. T., Hofmann, S., & Fiebig, J. (2026) · SoftwareX · doi:10.1016/j.softx.2025.102492 · Cited by 3
Self-citationKatz, S., Levin, N., Rodbell, D., Abbott, M., Passey, B., & Katz, S. A. (2025) · Geophysical Research Letters · doi:10.1029/2025gl116249 · Cited by 1
Self-citationRinyu, L., Czébely, A., Kiss, D., Kele, S., Czellár, S., Molnár, J., & Túri, M. (2026) · International Journal of Mass Spectrometry · doi:10.1016/j.ijms.2025.117565
Self-citationChang, B., Zeng, Z., Cheng, X., Zhang, W., Xu, Z., Pu, T., Lu, C., Defliese, W. F., Wang, R., Dai, X., et al. (2026) · Geochimica et Cosmochimica Acta · doi:10.1016/j.gca.2026.01.008 · Cited by 1
Self-citationSchoenemann, S. W., Wolhowe, M. D., Maloney, A. E., Sletten, R. S., Huntington, K. W., Schauer, A. J., & Sachs, J. P. (2026) · Paleoceanography and Paleoclimatology · doi:10.1029/2025pa005339 · Cited by 1
“According to Schauer et al. (2016), data were processed using MATLAB software with updated parameters as per Petersen et al. (2019).”
Self-citationDual clumped isotopes in foraminiferal calcite reveal kinetic bias in some species
Davies, A., Peral, M., Erez, J., Levi, A., Evans, D., Friedrich, O., Caley, T., Nambiar, R., Coenen, D., Staudigel, P. T., et al. (2026) · Communications Earth & Environment · doi:10.1038/s43247-026-03770-y · Cited by 1
“…using equilibrated gas standards as anchors and a pooled session approach applying drift correction and variance minimization over unknowns and anchors, assigning Δ 47 values of 0.9196 ‰ and 0.0266 ‰ and Δ 48 values of 0.345 ‰ and 0 ‰ for CO 2 equilibrated at 25 ˚ and 1000 °C, respectively 52,110 .”
InfluentialSelf-citationOCEAN TEMPERATURES IN THE LATE ORDOVICIAN: A CLUMPED ISOTOPE STUDY OF BRACHIOPODS AND CEMENTS
Barney, B. B., & Grossman, E. L. (2020) · Abstracts with programs - Geological Society of America · doi:10.1130/abs/2020am-354845 · Cited by 1
Clumped Isotope Analysis of Calcite and Dolomite Mixtures Using Selective Acid Extraction
Li, S., Schauer, A. J., Licht, A., Liang, J., Huntington, K. W., & Peng, K. (2023) · Journal of Earth Science · doi:10.1007/s12583-022-1630-4 · Cited by 1
“In the most recent quantification effort, Petersen et al. (2019) calculated a phosphoric acid correction compared to di‐ gestion at 25 °C of 0.066‰ at 70 °C, 0.088‰ at 90 °C reac‐ tions, respectively.”
MethodInfluentialSelf-citationCarbonate clumped isotopes and blocking temperatures of marbles from the Backbone Range, Taiwan
Laskar, A. H., Yui, T., & Liang, M. (2023) · Journal of Asian Earth Sciences · doi:10.1016/j.jseaes.2023.105975 · Cited by 1
OCEAN—An EXCEL add-in for 17O correction using a novel approximation
Flierl, L., & Rienitz, O. (2023) · MethodsX · doi:10.1016/j.mex.2023.102529 · Cited by 1
Yang, M., Frank, T. D., Fielding, C. R., & Chang, B. (2024) · Earth and Planetary Science Letters · doi:10.1016/j.epsl.2024.118641 · Cited by 1
Cooling climate across last interglacial high stands on San Salvador and Great Inagua, The Bahamas
Winkelstern, I. Z., Petersen, S., Curran, H. A., Phillips, C., Quizon, A. A., Glumac, B., & Griffing, D. H. (2025) · The Depositional Record · doi:10.1002/dep2.70038 · Cited by 1
Self-citationBayClump: Bayesian Calibration and Temperature Reconstructions for Clumped Isotope ThermometryPreprint
Palacios, C. R., Carroll, H. M., Arnold, A. J., Flores, R., Petersen, S., McKinnon, K., & Tripati, A. (2021) · doi:10.1002/essoar.10507995.1 · Cited by 3
Self-citationSupplemental Material: Reassessment of ocean paleotemperatures during the Late Ordovician
Barney, B. B., & Grossman, E. L. (2022) · doi:10.1130/geol.s.18822950.v1 · Cited by 1
BayClump: Bayesian Calibration and Temperature Reconstructions for Clumped Isotope ThermometryPreprint
Román‐Palacios, C., Carroll, H. M., Arnold, A., Gan, Q., & Tripati, A. (2022) · doi:10.1002/essoar.10507995.2 · Cited by 1
Self-citationThe Habitat of the Nascent Chicxulub Crater
Bralower, T. J., Cosmidis, J., Fantle, M. S., Lowery, C. M., Passey, B. H., Gulick, S. P. S., Morgan, J. V., Vajda, V., Whalen, M. T., Wittmann, A., et al. (2020) · AGU Advances · doi:10.1029/2020av000208
Self-citationLinol, B., Montañez, I., Lombardo, A., Kuta, D., Upadhyay, D., Arnold, A. J., Tripati, A., Bauer, A., & Musa, S. (2021) · South African Journal of Geology · doi:10.25131/sajg.124.0045
Self-citationVleeschouwer, D. D., Peral, M., Marchegiano, M., et al. (2021) · Climate of the past · doi:10.5194/cp-2021-151-rc1
O'Hora, H. E., Petersen, S. V., Vellekoop, J., et al. (2021) · Climate of the past · doi:10.5194/cp-2021-104-rc1
O'Hora, H. E., Petersen, S. V., Vellekoop, J., et al. (2022) · Climate of the past · doi:10.5194/cp-2021-104-rc2
Vleeschouwer, D. D. (2022) · Climate of the past · doi:10.5194/cp-2021-151-ac2
Vleeschouwer, D. D. (2022) · Climate of the past · doi:10.5194/cp-2021-151-ac1
Attachement #2 relating to Reply on Comment 1
Petersen, S. (2022) · Climate of the past · doi:10.5194/cp-2021-104-ac3
Self-citationAuthors' reply to Clara Bolton (RC1)
Vleeschouwer, D. D. (2022) · Climate of the past · doi:10.5194/cp-2021-151-ac3
Supplemental Material: A tropically hot mid-Cretaceous North American Western Interior Seaway
Jones, M. M., & al., E. (2022) · doi:10.1130/geol.s.19633128
Supplemental Material: A tropically hot mid-Cretaceous North American Western Interior Seaway
Jones, M. M., & al., E. (2022) · doi:10.1130/geol.s.19633128.v1
(2019) · Geochemistry Geophysics Geosystems · doi:10.1002/ggge.21614
Nehme, C., Todisco, D., Breitenbach, S., Couchoud, I., Marchegiano, M., Peral, M., Vonhof, H., Hellstrom, J., Tjallingi, R., Claeys, P., et al. (2023) · Social Science Research Network · doi:10.2139/ssrn.4172978 · Cited by 13
Self-citationDaëron, M., & Vermeesch, P. (2023) · doi:10.31223/x5k394
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“Data were processed using Easotope software (John & Bowen, 2016), using the Brand et al. (2010) 17 O correction parameters (Daëron et al., 2016; Schauer et al., 2016) and corrected with a 70°C calcite acid fractionation of 0.066 (Petersen et al., 2019).”
MethodInfluentialisogeochem: Tools for Stable Isotope Geochemistry
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Self-citationBARMPy: Bayesian additive regression models Python package
Boxel, D. V. (2024) · Computational Statistics · doi:10.1007/s00180-024-01535-9
“The ecological details are beyond the scope of this paper, but there are various studies on this topic (Eiler and Schauble 2004; Román Palacios et al. 2022; Petersen et al. 2019).”
Braniecki, G. F. N., Surge, D. M., & Hyland, E. G. (2025) · Geosciences · doi:10.3390/geosciences15080295
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“Finally, we used an acid fractionation factor of + 0.088‰ to calibrate our data (Petersen et al., 2019).”
InfluentialSelf-citationHuth, T. E., Cerling, T. E., Marchetti, D. W., Ellwein, A. L., Mahan, S. A., Bowling, D. R., Passey, B. H., Polyak, V. J., & Asmerom, Y. (2026) · Geochemistry Geophysics Geosystems · doi:10.1029/2025gc012660
“Standards included equilibrated (30°C) and heated (1000°C) gases (Petersen et al., 2019) and carbonate standards ETH‐1, ETH‐2, and ETH‐3 (Bernasconi et al., 2021).”
Self-citation
Metadata
- Authors
- Petersen, S. V., Defliese, W. F., Saenger, C., Daëron, M., Huntington, K. W., John, C. M., Kelson, J. R., Bernasconi, S. M., Colman, A. S., Kluge, T., Olack, G. A., Schauer, A. J., Bajnai, D., Bonifacie, M., Breitenbach, S. F. M., Fiebig, J., Fernandez, A. B., Henkes, G. A., Hodell, D., Katz, A., Kele, S., Lohmann, K. C., Passey, B. H., Peral, M. Y., Petrizzo, D. A., Rosenheim, B. E., Tripati, A., Venturelli, R., Young, E. D., & Winkelstern, I. Z.
- Affiliations
- University of Michigan (US)
- University of California, Los Angeles (US)
- University of Washington (US)
- Laboratoire des Sciences du Climat et de l'Environnement (FR)
- Imperial College London (GB)
- ETH Zurich (CH)
- University of Chicago (US)
- Heidelberg University (DE)
- Goethe University Frankfurt (DE)
- Institut de physique du globe de Paris (FR)
- University of Cambridge (GB)
- Department of Earth Sciences ETH‐Zurich Zurich Switzerland
- Stony Brook University (US)
- Institute for Geological and Geochemical Research (HU)
- Jet Propulsion Laboratory (US)
- University of South Florida St. Petersburg (US)
- Grand Valley State University (US)
- Corresponding author
- Petersen, S. V.
- ORCID
- Petersen, S. V.
- Defliese, W. F.
- Saenger, C.
- Daëron, M.
- Huntington, K. W.
- John, C. M.
- Kelson, J. R.
- Bernasconi, S. M.
- Colman, A. S.
- Kluge, T.
- Olack, G. A.
- Schauer, A. J.
- Bajnai, D.
- Bonifacie, M.
- Breitenbach, S. F. M.
- Fiebig, J.
- Fernandez, A. B.
- Henkes, G. A.
- Hodell, D.
- Katz, A.
- Kele, S.
- Lohmann, K. C.
- Passey, B. H.
- Peral, M. Y.
- Petrizzo, D. A.
- Rosenheim, B. E.
- Tripati, A.
- Venturelli, R.
- Young, E. D.
- Winkelstern, I. Z.
- Venue
- Geochemistry, Geophysics, Geosystems
- Publisher
- American Geophysical Union (AGU)
- Published
- 2019-07
- Volume
- 20
- Issue
- 7
- Pages
- 3495-3519
- ISSN
- 1525-2027 (ISSN-L)
- OpenAlex
- W2947366632
- Semantic Scholar
- ead0cf9b337105657195db631c449c24e051275e
- Cited by
- 209
- References
- 89
- Citations by year
- 2026: 16 · 2025: 14 · 2024: 32 · 2023: 28 · 2022: 35 · 2021: 45 · 2020: 23 · 2019: 16
- FWCI
- 11.89
- Type
- journal article
- Language
- en
- Open access
- hybrid
- doi.org
- Licence
- Locations
- Geochemistry Geophysics Geosystems (publishedVersion, other-oa)
- Northumbria Research Link (Northumbria University) (acceptedVersion, other-oa)
- Repository of the Academy's Library (Library of the Hungarian Academy of Sciences) (acceptedVersion)
- Digital Commons - University of South Florida (University of South Florida) (submittedVersion, other-oa)
- HAL (submittedVersion, other-oa)
- Deep Blue (University of Michigan) (submittedVersion, other-oa)
- OSTI OAI (U.S. Department of Energy Office of Scientific and Technical Information) (submittedVersion, other-oa)
- HAL Portal Artxiker (Hindustan Aeronautics Limited (India)) (submittedVersion)
- OSTI OAI (U.S. Department of Energy Office of Scientific and Technical Information) (submittedVersion)
- VUBIR (Vrije Universiteit Brussel) (submittedVersion)
- Funders
- National Science Foundation (1156134, 1713275, 0923831)
- U.S. Department of Energy (DE‐SC0010288)
- Nemzeti Kutatási Fejlesztési és Innovációs Hivatal (KH 125584)
- Natural Environment Research Council (NE/M003752/1)
- Topics
- Physical Sciences › Earth and Planetary Sciences › Atmospheric Science › Geology and Paleoclimatology Research
- Physical Sciences › Earth and Planetary Sciences › Paleontology › Paleontology and Stratigraphy of Fossils
- Physical Sciences › Earth and Planetary Sciences › Geochemistry and Petrology › Geological and Geochemical Analysis
- Keywords
- clumped isotopes, interlaboratory agreement, empirical transfer functions, carbonate diagenesis
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