Analytical protocol for measuring micro-molar quantities of sulfur volatile species in experimental high pressure and temperature fluids

Abstract Validating thermodynamic models is essential in experimental geosciences for exploring increasingly complex systems and developing analytical protocols. However, investigating solid–fluid equilibria in mm3-sized experimental capsules poses several challenges, particularly in sulfur-bearing...

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Main Authors: Arianna Secchiari, Luca Toffolo, Sandro Recchia, Simone Tumiati
Format: Article
Language:English
Published: Nature Portfolio 2025-01-01
Series:Communications Chemistry
Online Access:https://doi.org/10.1038/s42004-024-01370-5
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author Arianna Secchiari
Luca Toffolo
Sandro Recchia
Simone Tumiati
author_facet Arianna Secchiari
Luca Toffolo
Sandro Recchia
Simone Tumiati
author_sort Arianna Secchiari
collection DOAJ
description Abstract Validating thermodynamic models is essential in experimental geosciences for exploring increasingly complex systems and developing analytical protocols. However, investigating solid–fluid equilibria in mm3-sized experimental capsules poses several challenges, particularly in sulfur-bearing chemical systems. These include maintaining bulk fluid composition and performing quantitative analysis with extremely low amounts of synthesized fluid. We present an innovative methodology for measuring ultra-low amounts of sulfur volatiles (H2S and SO2) generated during experimental runs at high pressure and temperature conditions of 3 GPa and 700 °C. Using solid sulfides (FeS + FeS2) and water as reactants, we performed redox-controlled syntheses employing a piston cylinder apparatus. We demonstrate that ex-situ measurements of these fluids by quadrupole mass spectrometry ensure accurate and precise analysis, confirming predicted thermodynamic compositions. This methodology allows in-depht investigation of sulfide solid–fluid equilibria, shedding light on sulfur volatiles behavior and geochemical cycles under high P–T conditions characteristic of the Earth’s interior.
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institution Kabale University
issn 2399-3669
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spelling doaj-art-28250cd4340e4136b20afe12520336cf2025-01-26T12:19:12ZengNature PortfolioCommunications Chemistry2399-36692025-01-01811710.1038/s42004-024-01370-5Analytical protocol for measuring micro-molar quantities of sulfur volatile species in experimental high pressure and temperature fluidsArianna Secchiari0Luca Toffolo1Sandro Recchia2Simone Tumiati3Dipartimento di Scienze Della Terra, Università Degli Studi di MilanoDipartimento di Scienze Della Terra, Università Degli Studi di MilanoDipartimento di Scienza e Alta Tecnologia, Università degli Studi dell’InsubriaDipartimento di Scienze Della Terra, Università Degli Studi di MilanoAbstract Validating thermodynamic models is essential in experimental geosciences for exploring increasingly complex systems and developing analytical protocols. However, investigating solid–fluid equilibria in mm3-sized experimental capsules poses several challenges, particularly in sulfur-bearing chemical systems. These include maintaining bulk fluid composition and performing quantitative analysis with extremely low amounts of synthesized fluid. We present an innovative methodology for measuring ultra-low amounts of sulfur volatiles (H2S and SO2) generated during experimental runs at high pressure and temperature conditions of 3 GPa and 700 °C. Using solid sulfides (FeS + FeS2) and water as reactants, we performed redox-controlled syntheses employing a piston cylinder apparatus. We demonstrate that ex-situ measurements of these fluids by quadrupole mass spectrometry ensure accurate and precise analysis, confirming predicted thermodynamic compositions. This methodology allows in-depht investigation of sulfide solid–fluid equilibria, shedding light on sulfur volatiles behavior and geochemical cycles under high P–T conditions characteristic of the Earth’s interior.https://doi.org/10.1038/s42004-024-01370-5
spellingShingle Arianna Secchiari
Luca Toffolo
Sandro Recchia
Simone Tumiati
Analytical protocol for measuring micro-molar quantities of sulfur volatile species in experimental high pressure and temperature fluids
Communications Chemistry
title Analytical protocol for measuring micro-molar quantities of sulfur volatile species in experimental high pressure and temperature fluids
title_full Analytical protocol for measuring micro-molar quantities of sulfur volatile species in experimental high pressure and temperature fluids
title_fullStr Analytical protocol for measuring micro-molar quantities of sulfur volatile species in experimental high pressure and temperature fluids
title_full_unstemmed Analytical protocol for measuring micro-molar quantities of sulfur volatile species in experimental high pressure and temperature fluids
title_short Analytical protocol for measuring micro-molar quantities of sulfur volatile species in experimental high pressure and temperature fluids
title_sort analytical protocol for measuring micro molar quantities of sulfur volatile species in experimental high pressure and temperature fluids
url https://doi.org/10.1038/s42004-024-01370-5
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