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Oxygen isotope analysis for silicate minerals using a high temperature conversion/elemental analyzer-isotope ratio mass spectrometer
  • Ryosuke Kikuchi,
  • Tobimaru Ishiwata,
  • Ichiro Tayasu
Ryosuke Kikuchi
Hokkaido University

Corresponding Author:rkikuchi@eng.hokudai.ac.jp

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Tobimaru Ishiwata
Hokkaido University
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Ichiro Tayasu
Research Institute of Humanity and Nature
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Abstract

RATIONALE: Oxygen isotope composition of silicates is an important indicator of the formation environment and/or subsequent geochemical processes of minerals. Compared to carbonate minerals and organic matter, silicate is a less common target for oxygen isotope measurements because of the need for specialized fluorination instruments to break strong Si-O bonds. METHODS: We introduce a simple method using a high temperature conversion elemental analyzer-isotope ratio mass spectrometer (TC/EA-IRMS), which does not require specialized instrumentation. Silicate powder with various fluorine compounds and ratios of fluorine/oxygen were decomposed at 1450°C, and then, mass spectral characteristics, oxygen yields, and δ 18O values were compared. RESULTS: NaF and KF were the most reactive fluorine sources, followed by polytetrafluoroethylene, LiF, CaF 2, BaF 2, and AlF 3, with decreasing reactivity. The F/O ratio affected the tailing of the CO peaks in the mass spectrum. Higher F/O ratios show a more rapid regression to background, resulting in higher reproducibility of oxygen yield and δ 18O. In addition to simply adding fluorides to the sample, homogenization treatment also improved the reactivity. Activated carbon catalyzed by nickel is a better carbon source than graphite in terms of reactivity. The quartz and smectite with NaF added at an F/O ratio of 6 provided 90.0–99.3% of oxygen yields, δ 18O values that deviated less than 1.2‰ from literature values, and 0.18–0.29 ‰ of precision. CONCLUSIONS: Although further investigation is required to verify its accuracy, the potential of the TC/EA-IRMS method for silicates is demonstrated. Because the hydrogen isotope composition can also be examined using the same instrument, it is expected that this method can be applied to a wider range of earth materials, including hydrous silicates such as clay minerals.
Submitted to Rapid Communications in Mass Spectrometry
07 Feb 2025Review(s) Completed, Editorial Evaluation Pending
07 Feb 2025Editorial Decision: Revise Major
06 Mar 20251st Revision Received
06 Mar 2025Submission Checks Completed
06 Mar 2025Assigned to Editor
06 Mar 2025Review(s) Completed, Editorial Evaluation Pending
06 Mar 2025Reviewer(s) Assigned
12 Mar 2025Editorial Decision: Revise Minor