The exclusive use of carbonate reference materials is a robust method for the standardization of clumped isotope measurements • Measurements using different acid temperatures, designs of preparation lines, and mass spectrometers are statistically indistinguishable • We propose new consensus values for a set of 7 carbonate reference materials and updated guidelines to report clumped isotope measurements
Rationale: Clumped isotope geochemistry examines the pairing or clumping of heavy isotopes in molecules and provides information about the thermodynamic and kinetic controls on their formation. The first clumped isotope measurements of carbonate minerals were first published 15 years ago, and since then, interlaboratory offsets have been observed, and laboratory and community practices for measurement, data analysis, and instrumentation have evolved. Here we briefly review historical and recent developments for measurements, share Tripati Lab practices for four different instrument configurations, test a recently published proposal for carbonate-based standardization on multiple instruments using multi-year data sets, and report values for 21 different carbonate standards that allow for recalculations of previously published data sets.Methods: We examine data from 4628 standard measurements on Thermo MAT 253 and Nu Perspective IS mass spectrometers, using a common acid bath (90 C) and small-sample (70 C) individual reaction vessels. Each configuration was investigated
Estimates of the permafrost-climate feedback vary in magnitude and sign, partly because permafrost carbon stability in warmer-than-present conditions is not well constrained. Here we use a Plio-Pleistocene lacustrine reconstruction of mean annual air temperature (MAAT) from the Tibetan Plateau, the largest alpine permafrost region on the Earth, to constrain past and future changes in permafrost carbon storage. Clumped isotope-temperatures (Δ47-T) indicate warmer MAAT (~1.2 °C) prior to 2.7 Ma, and support a permafrost-free environment on the northern Tibetan Plateau in a warmer-than-present climate. Δ47-T indicate ~8.1 °C cooling from 2.7 Ma, coincident with Northern Hemisphere glacial intensification. Combined with climate models and global permafrost distribution, these results indicate, under conditions similar to mid-Pliocene Warm period (3.3–3.0 Ma), ~60% of alpine permafrost containing ~85 petagrams of carbon may be vulnerable to thawing compared to ~20% of circumarctic permafrost. This estimate highlights ~25% of permafrost carbon and the permafrost-climate feedback could originate in alpine areas.
The Last Glacial Maximum (LGM; ∼23,000-19,000 years ago; ka) is the subject of extensive study and represents a global climate state dramatically different from that of today, characterized by reduced greenhouse gas concentrations and extensive ice sheets (Mix et al., 2001;Raynaud et al., 1993). Proxy records and climate models show that glacial-interglacial cycles are driven by orbital forcing and internal mechanisms such as variations in insolation, greenhouse gas levels, and distribution of ice sheets (
Upper Cretaceous-Cenozoic marine sequences preserved between 30 and 350 masl across southern South Africa record a complex history of climatic and tectonic changes. In this study, we measure the strontium (Sr) isotope composition of fossil shark teeth, echinoderms, corals and oyster shells to chronostratigraphically constrain the ages of these sequences. The method requires careful petrographic screening and micro-drilling of the samples to avoid possible alteration by diagenesis. To assess palaeoenvironmental effects in the shells we measured the Mg/Ca elemental ratios and O isotope values using electron microprobe analysis (EMPA) and secondary ion mass spectrometry (SIMS). In addition, we employed carbonate clumped isotope thermometry to test palaeotemperatures reconstruction. The analysis of recent to modern stromatolites by clumped isotopes yields an average temperature of 20.2°C, in agreement with present day observations. The fossil oyster shells suggest a warmer (23.0°C) seawater palaeotemperature, possibly due to major deglaciation and sea-level rise during the Neogene. We also find that transgressions occurred above 200 to 350 m elevation during: 1) the Campanian-Maastrichian (~75 Ma); 2) the mid-Oligocene (32 to 26 Ma); and 3) the Messinian-Zanclean (6 to 5 Ma). These three episodes are linked to well-known variations in global sea level and regional tectonic processes that could have affected the continental margin differently. The most recent transgression coincides with a maximum global sea-level rise of ~50 m at ca. 5.3 Ma, and a worldwide plate kinematic change around 6 Ma, which in Eurasia led to the closure of the Mediterranean Sea. In the Eastern Cape of South Africa, the new dates of analyzed oyster shells constrain a minimum uplift rate of ca. 150 m/Myr during this tectonic activity. The results have important implications for robust calibration of relative sea level in southern Africa.
Rationale: Clumped isotope geochemistry examines the bond ordering of rare, heavy isotopes in molecules and provides information about the thermodynamic and kinetic controls on their formation. Since the first clumped isotope measurements of carbonate minerals were published 15 years ago, interlaboratory offsets in calibrations have been observed, and laboratory and community practices for measurement, data analysis, and instrumentation have evolved. Here we briefly review historical and recent developments for carbonate clumped isotope measurements, test a recently published proposal for carbonate-based standardization on multiple instruments using multi-year datasets, and report values for 21 different carbonate standards that allows for recalculations of previously published datasets. Methods: We examine data from 4628 standards analyzed over a 4 year interval on Thermo MAT 253 and Nu Perspective IS mass spectrometers, using common acid bath and small sample individual reaction vessels. Each configuration was analyzed by treating some standards as working
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