Oxidation rates and redox stabilization of ferrous iron in trioctahedral smectites

Kupper, Robert J.; Zhou, Nanqing; Chan, Clara S.; Thompson, Aaron; Catalano, Jeffrey G.

doi:10.1016/j.gca.2023.06.029

Oxidation rates and redox stabilization of ferrous iron in trioctahedral smectites

Journal Article · Fri Jun 30 00:00:00 EDT 2023 · Geochimica et Cosmochimica Acta

DOI:https://doi.org/10.1016/j.gca.2023.06.029· OSTI ID:2423550

Kupper, Robert J. ^[1]; Zhou, Nanqing ^[2]; ^[2]; ^[3]; Catalano, Jeffrey G. ^[1]

Washington University, Saint Louis, MO (United States)
University of Delaware, Newark, DE (United States)
University of Georgia, Athens, GA (United States)

Iron(II)-bearing trioctahedral smectites (saponites) form during anoxic alteration of basaltic rock. They are predicted to have been widespread on the early Earth and are observed in the oceanic subsurface today. Smectite structures, including the occupancy of sites in the octahedral sheet, affect iron redox behavior but the rates and products of trioctahedral smectite oxidation have been largely unexplored to date. In this study we synthesized two Fe(II)-bearing trioctahedral smectites, one moderate (22 wt% Fe) and one high (27 wt% Fe) in iron content. We then examined the rate, extent, and products of their oxidation by dissolved oxygen, nitrite, and hydrogen peroxide. Dissolved oxygen caused partial oxidation of Fe(II) in the smectites with 14 to 43% of Fe(II) unoxidized after 20 to 30 days of exposure. The rate and extent of oxidation correlated with the dissolved oxygen concentration and the Fe(II) content of the clay. The incomplete oxidation in these experiments is consistent with the mixed-valent trioctahedral smectites observed in oxidized natural samples but contrasts with the complete reoxidation by oxygen shown by chemically- or microbially-reduced dioctahedral smectites. Oxidation of structural Fe(II) by 5 mmol L^-1 nitrite was negligible for the moderate-iron smectite and yielded only ~17% oxidation after 54 days of reaction for the high-iron smectite. Hydrogen peroxide caused rapid and near-complete oxidation of both clays. Powder X-ray diffraction, variable-temperature Mössbauer spectroscopy, and extended X-ray absorption fine structure spectroscopy together detected no crystalline or short-range-ordered secondary phases and show that oxidized iron remained in the trioctahedral smectite structure. The recalcitrant Fe(II) pool in oxidized trioctahedral smectites exists in less distorted sites than Fe(II) in the initial clays. Its unreactive nature at prolonged reaction times indicates an elevated redox potential generated by the local coordination environment. Slower oxidation rates create a larger recalcitrant Fe(II) pool, suggesting kinetic competition between oxidation and a process involved in redox stabilization, such as electron exchange between octahedral iron sites or deprotonation of hydroxyl groups in the structure. The resistance to complete oxidation of trioctahedral ferrous smectites and their full retention of iron demonstrates that transitions from anoxic to oxic conditions generate mixed-valence smectites rather than a mixture of new phases. Identifying the diagenetic products of mixed-valent trioctahedral smectites may provide an indicator in the rock record of past redox cycling. In conclusion, substantial portions of structural Fe(II) in trioctahedral smectites display slow abiotic oxidation kinetics and represent potential electron donors for both microaerophilic iron oxidizing and nitrate-reducing, iron-oxidizing microorganisms in altered mafic rocks and related settings.

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Research Organization:: Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF); U.S. National Aeronautics and Space Administration (NASA); McDonnell Center for the Space Sciences at Washington University; USDOE

Grant/Contract Number:: AC02-06CH11357; 80NSSC18K129; 80NSSC19M0069

OSTI ID:: 2423550

Alternate ID(s):: OSTI ID: 1992564

Journal Information:: Geochimica et Cosmochimica Acta, Vol. 355; ISSN 0016-7037

Publisher:: Elsevier; The Geochemical Society; The Meteoritical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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58 GEOSCIENCES
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
Geochemistry
Geophysics
Iron redox
Oxidation rate
Trioctahedral smectite
Mössbauer spectroscopy

Oxidation rates and redox stabilization of ferrous iron in trioctahedral smectites

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