A furnace design for XANES spectroscopy of silicate melts under controlled oxygen fugacities and temperatures to 1773 K

Andrew J. Berry; J. Michael G. Shelley; Garry J. Foran; Hugh St C. O'Neill; Dean R. Scott

doi:10.1107/S0909049503007556

A furnace design for XANES spectroscopy of silicate melts under controlled oxygen fugacities and temperatures to 1773 K

Andrew J. Berry^*, J. Michael G. Shelley, Garry J. Foran, Hugh St C. O'Neill, Dean R. Scott

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

59 Citations (Scopus)

Abstract

A controlled-atmosphere furnace has been constructed for X-ray absorption spectroscopy experiments under imposed oxygen fugacities at temperatures up to 1773 K. The use of the furnace is demonstrated in a study of the oxidation state of Cr in a basaltic silicate melt (mid-ocean ridge basalt) by K-edge XANES spectroscopy. This is the first time the Cr²⁺/Cr³⁺ ratio has been identified directly in an Fe-bearing melt. At typical terrestrial oxygen fugacities around half the Cr is present as Cr²⁺, even though this oxidation state has never been identified in a terrestrial material and only Cr³⁺ is observed after quenching to a glass. Cr²⁺ oxidizes to Cr³⁺ on cooling in the presence of Fe³⁺ according to the electron exchange reaction Cr²⁺ + Fe³⁺ → Cr³⁺ + Fe²⁺. This illustrates the importance of the in situ determination of metal oxidation states in melts.

Original language	English
Pages (from-to)	332-336
Number of pages	5
Journal	Journal of Synchrotron Radiation
Volume	10
Issue number	4
DOIs	https://doi.org/10.1107/S0909049503007556
Publication status	Published - 1 Jul 2003

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title = "A furnace design for XANES spectroscopy of silicate melts under controlled oxygen fugacities and temperatures to 1773 K",

abstract = "A controlled-atmosphere furnace has been constructed for X-ray absorption spectroscopy experiments under imposed oxygen fugacities at temperatures up to 1773 K. The use of the furnace is demonstrated in a study of the oxidation state of Cr in a basaltic silicate melt (mid-ocean ridge basalt) by K-edge XANES spectroscopy. This is the first time the Cr2+/Cr3+ ratio has been identified directly in an Fe-bearing melt. At typical terrestrial oxygen fugacities around half the Cr is present as Cr2+, even though this oxidation state has never been identified in a terrestrial material and only Cr3+ is observed after quenching to a glass. Cr2+ oxidizes to Cr3+ on cooling in the presence of Fe3+ according to the electron exchange reaction Cr2+ + Fe3+ → Cr3+ + Fe2+. This illustrates the importance of the in situ determination of metal oxidation states in melts.",

keywords = "Controlled oxygen fugacity, Mid-ocean ridge basalts, Oxidation states, Silicate melts, Spectroscopy furnaces, XANES",

author = "Berry, {Andrew J.} and Shelley, {J. Michael G.} and Foran, {Garry J.} and O'Neill, {Hugh St C.} and Scott, {Dean R.}",

year = "2003",

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doi = "10.1107/S0909049503007556",

language = "English",

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T1 - A furnace design for XANES spectroscopy of silicate melts under controlled oxygen fugacities and temperatures to 1773 K

AU - Berry, Andrew J.

AU - Shelley, J. Michael G.

AU - Foran, Garry J.

AU - O'Neill, Hugh St C.

AU - Scott, Dean R.

PY - 2003/7/1

Y1 - 2003/7/1

N2 - A controlled-atmosphere furnace has been constructed for X-ray absorption spectroscopy experiments under imposed oxygen fugacities at temperatures up to 1773 K. The use of the furnace is demonstrated in a study of the oxidation state of Cr in a basaltic silicate melt (mid-ocean ridge basalt) by K-edge XANES spectroscopy. This is the first time the Cr2+/Cr3+ ratio has been identified directly in an Fe-bearing melt. At typical terrestrial oxygen fugacities around half the Cr is present as Cr2+, even though this oxidation state has never been identified in a terrestrial material and only Cr3+ is observed after quenching to a glass. Cr2+ oxidizes to Cr3+ on cooling in the presence of Fe3+ according to the electron exchange reaction Cr2+ + Fe3+ → Cr3+ + Fe2+. This illustrates the importance of the in situ determination of metal oxidation states in melts.

AB - A controlled-atmosphere furnace has been constructed for X-ray absorption spectroscopy experiments under imposed oxygen fugacities at temperatures up to 1773 K. The use of the furnace is demonstrated in a study of the oxidation state of Cr in a basaltic silicate melt (mid-ocean ridge basalt) by K-edge XANES spectroscopy. This is the first time the Cr2+/Cr3+ ratio has been identified directly in an Fe-bearing melt. At typical terrestrial oxygen fugacities around half the Cr is present as Cr2+, even though this oxidation state has never been identified in a terrestrial material and only Cr3+ is observed after quenching to a glass. Cr2+ oxidizes to Cr3+ on cooling in the presence of Fe3+ according to the electron exchange reaction Cr2+ + Fe3+ → Cr3+ + Fe2+. This illustrates the importance of the in situ determination of metal oxidation states in melts.

KW - Controlled oxygen fugacity

KW - Mid-ocean ridge basalts

KW - Oxidation states

KW - Silicate melts

KW - Spectroscopy furnaces

KW - XANES

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DO - 10.1107/S0909049503007556

M3 - Article

SN - 0909-0495

VL - 10

SP - 332

EP - 336

JO - Journal of Synchrotron Radiation

JF - Journal of Synchrotron Radiation

IS - 4

ER -

A furnace design for XANES spectroscopy of silicate melts under controlled oxygen fugacities and temperatures to 1773 K

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