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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 source backs part of the claim, not all of it — or backs it for a different population, condition or comparison.
In the citing paper
“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.
In the citing paper
“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.
In the citing paper
“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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In the citing paper
“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.
In the citing paper
“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.
In the citing paper
“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.
In the citing paper
“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
The cited source says what the claim attributes to it.
In the citing paper
“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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In the citing paper
“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)
The cited source says what the claim attributes to it.
In the citing paper
“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
The cited source says what the claim attributes to it.
In the citing paper
“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
The cited source says what the claim attributes to it.
In the citing paper
“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
The cited source says what the claim attributes to it.
In the citing paper
“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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Citations
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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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Winkelstern, I. Z., Passey, B. H., Rey, K., Huth, T., McGee, D., & QUADE, J. (2026) · Geology · doi:10.1130/g54289.1
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Δ47-Δ48 systematics of speleothem carbonate
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Are Time and Temperature the Simple Answer to the Dolomite Problem?
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“…in dolomites at all, which is not the case for the commonly used Mg/Ca paleothermometer, for example, Dolomite is well understood to follow similar relationships between isotopic “clumping” and temperature as for more commonly studied calcite and aragonite clumped isotopes (Petersen et al., 2019).”
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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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