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<p>Validating thermodynamic models is essential in experimental geosciences for exploring increasingly complex systems and developing analytical protocols. However, investigating solid–fluid equilibria in mm<sup>3</sup>-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 (H<sub>2</sub>S and SO<sub>2</sub>) generated during experimental runs at high pressure and temperature conditions of 3 GPa and 700 °C. Using solid sulfides (FeS + FeS<sub>2</sub>) 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 <i>P</i>–<i>T</i> conditions characteristic of the Earth’s interior.</p>

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

  • 期刊论文

  • 出版模式：

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  • 发表日期：

    2025年1月23日

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  • Arianna Secchiari,
  • Luca Toffolo,
  • Sandro Recchia,
  • Simone Tumiati

摘要

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.