Carbonate clumped isotope analyses with the long‐integration dual‐inlet (LIDI) workflow: scratching at the lower sample weight boundaries

Müller, Inigo A.; Fernández, Álvaro; Radke, Jens; Dijk, Joep van; Bowen, Devon; Schwieters, Johannes; Bernasconi, Stefano M.

doi:10.1002/rcm.7878

Cited by 105 publications

(139 citation statements)

References 43 publications

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“…These results demonstrate the homogeneity of these materials, whereby the reproducibility for ETH‐2 and ETH‐4 is slightly poorer compared to the other two, and they seem to have slightly less negative δ 18 O values on the GB compared to the Kiel devices. The homogeneity of the four ETH standards with respect to Δ 47 was demonstrated by the long‐term reproducibility obtained over 15 months as reported in Meckler et al (2014) and by the results presented in Müller, Fernandez, et al (2017). …”

Section: Carbonate Standards For Optimized Data Correction and Linkagsupporting

confidence: 64%

“…The advantage of this approach is that short‐term fluctuations caused by the mass spectrometer in both slope and intercept of the ETF can be readily observed and corrected for. We demonstrate this in Figure 4, which shows the evolution of the slope and intercept of the ThermoFisher 253Plus instrument during approximately 5 weeks corresponding to the measurement period of the data discussed in Müller, Fernandez, et al (2017). In contrast, typical measurement windows for laboratories using heated and equilibrated gases are on the order of a few weeks to months.…”

Section: Carbonate Standards For Optimized Data Correction and Linkagsupporting

confidence: 52%

“…With typical reproducibilities of 0.02–0.030‰ these systems may require more replicates than what can be achieved in the best laboratories analyzing large samples of 3–10 mg with custom built lines (0.014–0.020‰; Fernandez et al, 2017). However, the speed of analysis and the small sample sizes used for each analysis allow precise and accurate measurements on total sample sizes of 1 to 2 mg (Müller, Fernandez, et al, 2017) as opposed to 10–15 mg or more for large‐sample systems. The ability of analyzing small samples opens new avenues of research that cannot be approached with the conventional large‐sample systems (e.g., analysis of foraminifera by Rodriguez‐Sanz et al, 2017).…”

Section: Discussionmentioning

confidence: 99%

“…This is the origin of the slope of the heated gas line, and heated gases have been used to demonstrate that negative BGs can be properly corrected after independent determination of the background in the presence of gas (Bernasconi et al, 2013; He et al, 2012). The characterization of negative background, their effect on Δ 47 and correction procedures, has been described in detail in Bernasconi et al (2013), He et al (2012), and Müller, Fernandez, et al (2017). …”

Section: Nomenclature and Isotopic Scales For Clumped Isotopes In Carmentioning

confidence: 99%

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Reducing Uncertainties in Carbonate Clumped Isotope Analysis Through Consistent Carbonate‐Based Standardization

Bernasconi

Müller

Bergmann

et al. 2018

Geochem Geophys Geosyst

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229

380

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About a decade after its introduction, the field of carbonate clumped isotope thermometry is rapidly expanding because of the large number of possible applications and its potential to solve long‐standing questions in Earth Sciences. Major factors limiting the application of this method are the very high analytical precision required for meaningful interpretations, the relatively complex sample preparation procedures, and the mass spectrometric corrections needed. In this paper we first briefly review the evolution of the analytical and standardization procedures and discuss the major remaining sources of uncertainty. We propose that the use of carbonate standards to project the results to the carbon dioxide equilibrium scale can improve interlaboratory data comparability and help to solve long‐standing discrepancies between laboratories and temperature calibrations. The use of carbonates reduces uncertainties related to gas preparation and cleaning procedures and ensures equal treatment of samples and standards. We present a set of carbonate standards of diverse composition, discuss how they can be used to correct for mass spectrometric biases, and demonstrate that their use significantly improves the comparability among four laboratories. We propose that the use of these standards or of a similar set of carbonate standards will improve the comparability of data across laboratories.

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Section: Carbonate Standards For Optimized Data Correction and Linkagsupporting

confidence: 64%

Section: Carbonate Standards For Optimized Data Correction and Linkagsupporting

confidence: 52%

Section: Discussionmentioning

confidence: 99%

Section: Nomenclature and Isotopic Scales For Clumped Isotopes In Carmentioning

confidence: 99%

See 2 more Smart Citations

Reducing Uncertainties in Carbonate Clumped Isotope Analysis Through Consistent Carbonate‐Based Standardization

Bernasconi

Müller

Bergmann

et al. 2018

Geochem Geophys Geosyst

Self Cite

229

380

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“… Note: These data are based on the measurements originally reported in Defliese et al recalculated using the Brand et al isotopic parameters. The number of replicates measured on each instrument is reported.…”

Section: Methodsmentioning

confidence: 99%

Analytical effects on clumped isotope thermometry: Comparison of a common sample set analyzed using multiple instruments, types of standards, and standardization windows

Defliese

Tripati

2020

Rapid Comm Mass Spectrometry

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Rationale Carbonate clumped isotope geothermometry is being increasingly used in multiple disciplines in the geosciences. However, potential interlaboratory issues are arising from different standardization procedures that may contribute to the multiple Δ47‐temperature calibrations reported in the literature. We investigate this issue by comparing a common temperature calibration sample set across three different mass spectrometers, using multiple standardization methods. Methods The same temperature calibration sample set was analyzed on three different mass spectrometers. Several standardization methods were utilized, including the use of carbonate versus gas standards, and different types of background correction were applied to the raw data. Results All standardization types applied resulted in statistically indistinguishable Δ47‐temperature slopes, with the exception of standardization calculations that did not correct for background effects. Some instruments and standardizations showed different intercepts relative to each other. The use of carbonate standards improved comparability between different instruments relative to gas standards. Conclusions Our results show that background effects are the largest factor potentially affecting Δ47 results, and there may be an improvement in interlaboratory precision using carbonate standards. Critically, all techniques used for standardizing Δ47 results converge on a common slope as long as background effects are properly corrected. The use of carbonate standards is recommended as a component of standardization procedures.

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A Reassessment of the Precision of Carbonate Clumped Isotope Measurements: Implications for Calibrations and Paleoclimate Reconstructions

Fernández

Müller

Rodríguez‐Sanz

et al. 2017

Geochem Geophys Geosyst

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Carbonate clumped isotopes offer a potentially transformational tool to interpret Earth's history, but the proxy is still limited by poor interlaboratory reproducibility. Here, we focus on the uncertainties that result from the analysis of only a few replicate measurements to understand the extent to which unconstrained errors affect calibration relationships and paleoclimate reconstructions. We find that highly precise data can be routinely obtained with multiple replicate analyses, but this is not always done in many laboratories. For instance, using published estimates of external reproducibilities we find that typical clumped isotope measurements (three replicate analyses) have margins of error at the 95% confidence level (CL) that are too large for many applications. These errors, however, can be systematically reduced with more replicate measurements. Second, using a Monte Carlo‐type simulation we demonstrate that the degree of disagreement on published calibration slopes is about what we should expect considering the precision of Δ47 data, the number of samples and replicate analyses, and the temperature range covered in published calibrations. Finally, we show that the way errors are typically reported in clumped isotope data can be problematic and lead to the impression that data are more precise than warranted. We recommend that uncertainties in Δ47 data should no longer be reported as the standard error of a few replicate measurements. Instead, uncertainties should be reported as margins of error at a specified confidence level (e.g., 68% or 95% CL). These error bars are a more realistic indication of the reliability of a measurement.

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Carbonate clumped isotope analyses with the long‐integration dual‐inlet (LIDI) workflow: scratching at the lower sample weight boundaries

Cited by 105 publications

References 43 publications

Reducing Uncertainties in Carbonate Clumped Isotope Analysis Through Consistent Carbonate‐Based Standardization

Reducing Uncertainties in Carbonate Clumped Isotope Analysis Through Consistent Carbonate‐Based Standardization

Analytical effects on clumped isotope thermometry: Comparison of a common sample set analyzed using multiple instruments, types of standards, and standardization windows

A Reassessment of the Precision of Carbonate Clumped Isotope Measurements: Implications for Calibrations and Paleoclimate Reconstructions

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