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NASA NTRS2004

Pancam multispectral imaging results from the Opportunity Rover at Meridiani Planum

Panoramic Camera (Pancam) images from Meridiani Planum reveal a low-albedo, generally flat, and relatively rock-free surface. Within and around impact craters and fractures, laminated outcrop rocks with higher albedo are observed. Fine-grained materials include dark sand, bright ferric iron-rich dust, angular rock clasts, and millimeter-size spheroidal granules that are eroding out of the laminated rocks. Spectra of sand, clasts, and one dark plains rock are consistent with mafic silicates such as pyroxene and olivine. Spectra of both the spherules and the laminated outcrop materials indicate the presence of crystalline ferric oxides or oxyhydroxides. Atmospheric observations show a steady decline in dust opacity during the mission. Astronomical observations captured solar transits by Phobos and Deimos and time-lapse observations of sunsets.

Mars↗

NASA NTRS2004

The Opportunity Rover's Athena science investigation at Meridiani Planum, Mars

The Mars Exploration Rover Opportunity has investigated the landing site in Eagle crater and the nearby plains within Meridiani Planum. The soils consist of fine-grained basaltic sand and a surface lag of hematite-rich spherules, spherule fragments, and other granules. Wind ripples are common. Underlying the thin soil layer, and exposed within small impact craters and troughs, are flat-lying sedimentary rocks. These rocks are finely laminated, are rich in sulfur, and contain abundant sulfate salts. Small-scale cross-lamination in some locations provides evidence for deposition in flowing liquid water. We interpret the rocks to be a mixture of chemical and siliciclastic sediments formed by episodic inundation by shallow surface water, followed by evaporation, exposure, and desiccation. Hematite-rich spherules are embedded in the rock and eroding from them. We interpret these spherules to be concretions formed by postdepositional diagenesis, again involving liquid water.

Mars↗

DOE OSTI2020

A requirement for an active proton delivery network supports a compound I-mediated C–C bond cleavage in CYP51 catalysis

CYP51 enzymes (sterol 14α-demethylases) are cytochromes P450 that catalyze multistep reactions. The CYP51 reaction occurs in all biological kingdoms and is essential in sterol biosynthesis. It removes the 14α-methyl group from cyclized sterol precursors by first forming an alcohol, then an aldehyde, and finally eliminating formic acid with the introduction of a Δ14–15 double bond in the sterol core. The first two steps are typical hydroxylations, mediated by an electrophilic compound I mechanism. The third step, C–C bond cleavage, has been proposed to involve either compound I (i.e. FeO 3+ ) or, alternatively, a proton transfer-independent nucleophilic ferric peroxo anion (compound 0, i.e. Fe 3+ O 2 – ). In this work, using comparative crystallographic and biochemical analyses of WT human CYP51 (CYP51A1) and its D231A/H314A mutant, whose proton delivery network is destroyed (as evidenced in a 1.98-Å X-ray structure in complex with lanosterol), we demonstrate that deformylation of the 14α-carboxaldehyde intermediate requires an active proton relay network to drive the catalysis. These results indicate a unified, compound I-based mechanism for all three steps of the CYP51 reaction, as previously established for CYP11A1 and CYP19A1. We anticipate that our approach can be applied to mechanistic studies of other P450s that catalyze multistep reactions, such as C–C bond cleavage.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Linking the Spin Transition of Ferric Iron in δ‐(Al,Fe)OOH to Water Storage in the Lower Mantle

As the most massive geochemical reservoir, the lower mantle affects the Earth's budget of volatile elements, including hydrogen or H 2 O. The properties of minerals in the lower mantle are further affected by changes in the electronic configurations of iron cations, that is, by spin transitions. The feedback between spin transitions and potential storage of H 2 O in solid hydrous phases in the lower mantle, however, remains unexplored. By combining high‐pressure nuclear resonant inelastic X‐ray scattering and high‐pressure high‐temperature X‐ray diffraction experiments, we constrained the thermal equation of state of δ‐(Al,Fe)OOH, a member of the phase H solid solution. Based on the derived thermal equation of state of δ‐(Al,Fe)OOH and the underlying thermodynamic model, we calculate the excess Gibbs free energy that arises from the spin transition of ferric iron in this compound and evaluate the effect on phase equilibria. The results of our analysis show that the spin transition of ferric iron in phase H may significantly reduce the thermodynamic activity and hence the concentration of H 2 O in a coexisting hydrous melt. As a consequence, nominally anhydrous minerals of the lower mantle may become dehydrated in the presence of phase H. Our analysis further suggests that, under certain conditions, the spin transition may expand the thermal stability of Fe 3+ ‐bearing phase H and create a geochemical link between the storage of H 2 O in phase H and ferric iron in the lower mantle.

Buchen, Johannes [Univ. of Bayreuth (Germany); Cal↗

NASA NTRS1984

Dynamics of graphite fiber intercalation: In situ resistivity measurements with a four point probe

The dynamics of ferric chloride intercalation of single graphite fibers were studied, in situ, using a four point dc bridge. Measurements before, during and after the intercalation showed that the intercalation occurred within minutes at 200 C. Changes in fiber resistivity after exposure to air suggested hydration of the graphite intercalation compound. Deintercalation of the ferric chloride was initiated at temperatures in excess of 400 C. cycling the intercalant into and out of the graphite fiber gave no improvements in fiber resistivity. The activation energy of the ferric chloride intercalation reaction was found to be 17 + or - 4 kcal/mol 1 consistent with the concept of a preliminary nucleation step in the intercalation reaction.

Jaworske, D. A.↗

NASA NTRS2004

Mineralogy at Gusev Crater from the Mossbauer spectrometer on the Spirit Rover

Mossbauer spectra measured on Mars by the Spirit rover during the primary mission are characterized by two ferrous iron doublets (olivine and probably pyroxene) and a ferric iron doublet (tentatively associated to nanophase ferric iron oxide). Two sextets resulting from nonstoichiometric magnetite are also present, except for a coating on the rock Mazatzal, where a hematite-like sextet is present. Greater proportions of ferric-bearing phases are associated with undisturbed soils and rock surfaces as compared to fresh rock surfaces exposed by grinding. The ubiquitous presence of olivine in soil suggests that physical rather than chemical weathering processes currently dominate at Gusev crater.

Minerals↗

NASA NTRS1995

Ferrix Chloride-Graphite Intercalation Compounds Prepared From Graphite Flouride

The reaction between graphite fluoride and ferric chloride was observed in the temperature range of 300 to 400 C. The graphite fluorides used for this reaction have an sp(sup 3) electronic structure and are electrical insulators. They can be made by fluorinating either carbon fibers or powder having various degrees of graphitization. Reaction is fast and spontaneous and can occur in the presence of air. The ferric chloride does not have to be predried. The products have an sp(sup 2) electronic structure and are electrical conductors. They contain first-stage FeCl3 intercalated graphite. Some of the products contain FeCl2 (center dot) 2H2O, others contain FeF3, in concentrations that depend on the intercalation condition. The graphite intercalated compounds (GIC) deintercalated slowly in air at room temperature, but deintercalated quickly and completely at 370 C. Deintercalation is accompanied by the disappearance of iron halides and the formation of rust (hematite) distributed unevenly on the fiber surface. When heated to 400 C in pure N2 (99.99 vol%), this new GIC deintercalates without losing its molecular structure. However, when the compounds are exposed to 800 C N2, in a quartz tube, they lost most of their halogen atoms and formed iron oxides (other than hematite), distributed evenly in or on the fiber.

Hung, Ching-Cheh↗

NASA NTRS1982

Friction and wear of iron and nickel in sodium hydroxide solutions

A loaded spherical aluminum oxider rider was made to slide, while in various solutions, on a flat iron or nickel surface reciprocate a distance of 1 cm. Time of experiments was 1 hr during which the rider passed over the rider passed over the center section of the track 540 times. Coefficients of friction were measured throughout the experiments. Wear was measured by scanning the track with a profilometer. Analysis of some of the wear tracks included use of the SEM (scanning electron microscrope) and XPS (X-ray photoelectron spectroscopy). Investigated were the effect of various concentractions of NaOH and of water. On iron, increasing NaOH concentration above 0.01 N caused the friction and wear to decrease. This decrease is accompanied by a decrease in surface concentration of ferric oxide (Fe2O3) while more complex iron-oxygen compounds, not clearly identified, also form. At low concentrations of NaOH, such as 0.01 N, where the friction is high, the wear track is badely torn up and the surface is broken. At high concentration, such as 10 N, where the friction is low, the wear track is smooth. The general conclusion is that NaOH forms a protective, low friction film on iron which is destroyed by wear at low concentrations but remains intact at high concentrations of NaOH. Nickel behaves differently than iron in that only a little NaOH gives a low coefficient of friction and a surface which, although roughened in the wear track, remains intact.

Rengstorff, G. W. P.↗

NASA NTRS1983

Friction and wear of iron and nickel in sodium hydroxide solutions

A loaded spherical aluminum oxider rider was made to slide, while in various solutions, on a flat iron or nickel surface reciprocate a distance of 1 cm. Time of experiments was 1 hr during which the rider passed over the center section of the track 540 times. Coeficients of friction were measured throughout the experiments. Wear was measured by scanning the track with a profilometer. Analysis of some of the wear tracks included use of the SEM (scanning electron microscope) and XPS (X-ray photoelectron spectroscopy). Investigated were the effect of various concentrations of NaOH and of water. On iron, increasing NaOH concentration above 0.01 N caused the friction and wear to decrease. This decrease is accompanied by a decrease in surface concentration of ferric oxide (Fe2O3) while more complex iron-oxygen compounds, not clearly identified, also form. At low concentrations of NaOH, such as 0.01 N, where the friction is high, the wear track is badly torn up and the surface is broken. At high concentration, such as 10 N, where the friction is low, the wear track is smooth. The general conclusion is that NaOH forms a protective, low friction film on iron which is destroyed by wear at low concentrations but remains intact at high conentrations of NaOH. Nickel behaves differently than iron in that only a little NaOH gives a low coefficient of friction and a surface which, although roughened in the wear track, remains intact. Previously announced in STAR as N83-10171

Rengstorff, G. P.↗

DOE OSTI2021

Iron-activated persulfate oxidation degrades aqueous Perfluorooctanoic acid (PFOA) at ambient temperature

Perfluorooctanoic acid (PFOA, C 8 HF 15 O 2 ) is an industrial surfactant that is highly resistant to natural breakdown processes such as those mediated by heat, hydrolysis, photolysis, and biodegradation. Many efforts have been developed to breakdown PFOA to less harmful species due to its widespread human exposure and potential toxicity. However, these methods require high temperature or specialized equipment with serious disadvantages of high energy cost for long-term use. For this paper, we investigated the effectiveness of PFOA degradation by ferrous iron-activated persulfate oxidation (IAPO) under various aqueous geochemical conditions. Approximately 64% of PFOA (initial concentration = 1.64 μmol L –1 ) was degraded after 4 h under illuminated anoxic conditions at ambient temperature. This degradation rate and magnitude support the potential use of IAPO as a novel inexpensive and environmentally friendly method to remediate PFOA in soil and groundwater.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2006

Effects of gamma-Radiation on Select Lipids and Antioxidants

Radiation encountered on an extended duration space mission (estimates of 3 Sieverts for a mission to Mars) poses a threat not only to human health, but also to the quality, nutritional value, and palatability of the food system. Free radicals generated by radiation interaction with foods may initiate many unwanted reactions including: 1) autoxidation in lipids that alters flavor, odor, and concentrations of essential fatty acids, and 2) depletion of antioxidants food products and dietary supplements. Studies have shown that antioxidants may provide long term health protection from oxidative stress caused by radiation exposure; therefore, consumption of antioxidants will be important. Stability of essential fatty acids is also important for astronauts long-term health status. The objectives of this study were to characterize the effects of low dose gamma-radiation on lipids and antioxidants by monitoring oxidation and reducing power, respectively, in model systems. Select oils and antioxidants were exposed to levels of gamma-radiation ranging from 0 to 1000 Gy (1 Gy = 1 Sv) using a Gammacell 220 and stored at ambient or elevated temperatures (65 C) for up to 3 months prior to analysis. A Fricke dosimeter was used to verify differences between the radiation doses administered. Primary and secondary products of lipid oxidation in soybean and peanut oils were monitored using conjugated diene and 2-thiobarbituric acid (TBARs) assays. Changes in fatty acid composition and formation and vitamin E levels were also measured. The reducing power of antioxidant compounds, including vitamins C and E and beta-carotene, was determined using the ferric reducing antioxidant power (FRAP) assay. Significant differences (alpha =0.05) were present between all radiation doses tested using the Fricke dosimeter. Increasing radiation doses above 3 Sv resulted in significantly (alpha =0.05) elevated levels of oxidation and free fatty acids in soybean and peanut oils. Decreases in concentrations of essential fatty acids upon increasing radiation doses were also observed. Increasing radiation doses caused significant (alpha =0.05) decreases in reducing power and hence the effectiveness of vitamins C and E as well as beta-carotene. This work establishes a need for quantifying the effects of space relevant radiation doses in the development of a food system for an extended duration mission and for identifying threshold radiation levels that will impact the useful shelf-life of the variety of foods that will be sent. Eventual rancidity of lipids and the loss of antioxidant bioprotective effects are major concerns for the acceptability and nutritional profile of a food system.

Gandolph, Jacob↗

NASA NTRS2002

The Speciation of Sulfur in an Ocean on Europa

Stability of native sulfur, iron sulfides, and aqueous sulfur compounds is evaluated at assumed P-T conditions of the Europa's ocean floor. Pyrite, gypsum, and ferric hydroxides can coexist in contact with sulfate-rich oceanic water. Additional information is contained in the original extended abstract.

Zolotov, M. Yu.↗

NASA NTRS1972

Venus clouds - A dirty hydrochloric acid model.

The spectral and polarization data for Venus are consistent with micrometer-sized aerosol cloud particles of hydrochloric acid with soluble and insoluble iron compounds, whose source could be volcanic or crustal dust. The yellow color of the clouds could be due to absorption bands in the near UV involving ferric iron and chlorine complexes. It is pointed out that the UV features could arise from variations in the concentrations of iron and hydrochloric acid in the cloud particles.

Hapke, B.↗

DOE OSTI2020

Chemical-Biological Cyclic Process for Hexavalent Chromium Reduction to Trivalent Chromium in Aqueous Medium - 20224

Conventional treatment of chromium contamination focuses on immobilization of the highly toxic and water-soluble form Cr(VI), by reducing it to the relatively less toxic and less mobile trivalent form, Cr(III), using reducing compounds like ferrous sulfate or ferrous iron, Fe(II). The Cr(VI) also respond to biodegradation and subsequent reduction. During the reduction reaction, Fe(II) is oxidized to ferric, Fe(III), which, being at the highest oxidation state, has no ability to reduce Cr(VI), and therefore remediation process terminates. The good news is that metal-reducing bacteria, S. oneidensis MR-1, can regenerate Fe(II) from Fe(III) with the help of an organic electron donor in an appropriate bacterial media. Thus, in the Cr(VI) chemical remediation process, Fe(II) to Fe(III) conversion is reversed by the biological process, regenerating Fe(II) and the Cr(VI) chemical reduction process continues in a cyclic fashion. This study presents the results of regeneration of Fe(II) from fresh Fe(III) as well as from the reaction products of Cr(VI) and Fe(II). Both fresh Fe(III) and reaction product Fe(III) exhibited the same reduction behavior. Fe(II) production increased with the increase of initial concentration of Fe(III), resulting in 87.5% Fe(II) regeneration. The extent of Fe(III) reduction (Fe(II)t/Fe(III)0.hour) was 21 times higher than the extent of Cr(VI) reduction (Cr(VI)t/Cr(VI)0.hour) by S. oneidensis MR-1. In a cyclic process of sequential Cr(VI) addition, the amount of Fe(II) regeneration decreased with the increase in cycle number, a fixed quantity of starting S. oneidensis MR-1 could regenerate Fe(II) at least five times in a ten-hour period. More importantly, regenerated Fe(II) instantly reduced Cr(VI) to Cr(III). So, Fe(II) regeneration with metal-reducing bacteria has a good potential for application in groundwater and wastewater remediation in reducing Cr(VI) to Cr(III). As a comparison of chemical to biological transformation, chemical transformation of Cr(VI) by Fe(II) was almost 600 times greater than that of biological transformation. Therefore a chemical-biological cyclic process offers potential applications for remediation of groundwater and hexavalent chromium contaminated waste sites. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2026

Can ferric-oxyl excited states explain elongated iron-oxygen bonds in heme peroxidase catalytic intermediates?

The use of X-ray structures to determine and interpret the ferryl iron-oxygen bond order in molecular oxygen-activating heme enzymes has, in the past, been controversial. This has mainly stemmed from the susceptibility of ferryl species to X-ray-induced electronic state changes. In this work we establishe using time-resolved serial femtosecond X-ray crystallography (tr-SFX) on a dye-decolourising peroxidase that the ferryl intermediate species (Compounds I and II) captured following in situ mixing of microcrystals with H 2 O 2 have single, rather than the double bond character expected. X-ray emission validated tr-SFX data with quantum refinement, time-dependent-DFT calculations and QM/MM geometry optimizations together support the concept that the single iron-oxygen bond character is not an indication of ferryl reduction or a protonated form (Fe IV -OH) but is instead attributed to the existence of accessible excited states possessing ferric-oxyl (Fe III –O •– ) character. Such states offer insight into the nature of ferryl heme.

Williams, Lewis J. [University of Essex, Colcheste↗

NASA NTRS1961

Kinetics of the Reaction Between Alcohols and Isocyanates Catalyzed by Ferric Acetylacetonate

The rate and temperature dependence of reaction for the ferric acetylacetonate catalyzed reaction between a-naphthyl, ortho-tolyl, and para-tolyl isocyanates and n-butyl alcohol are investigated. The effect of substituents on the reactivity of isocyanate and hydroxyl group are reported and for substituted isocyanates are correlated by means of the Hammett equation. Several metal chelates were studied and their catalytic activity was compared to that of ferric acetylacetonate. All rate data are interpreted in terms of a mechanism involving simultaneous second-order uncatalyzed and catalyzed reactions between alcohol and isocyanate.

ACETONE↗

NASA NTRS1998

The role of biomineralization in microbiologically influenced corrosion

Synthetic iron oxides (goethite, alpha-FeO.OH; hematite, Fe2O3; and ferrihydrite, Fe(OH)3) were used as model compounds to simulate the mineralogy of surface films on carbon steel. Dissolution of these oxides exposed to pure cultures of the metal-reducing bacterium, Shewanella putrefaciens, was followed by direct atomic absorption spectroscopy measurement of ferrous iron coupled with microscopic analyses using confocal laser scanning and environmental scanning electron microscopies. During an 8-day exposure the organism colonized mineral surfaces and reduced solid ferric oxides to soluble ferrous ions. Elemental composition, as monitored by energy dispersive x-ray spectroscopy, indicated mineral replacement reactions with both ferrihydrite and goethite as iron reduction occurred. When carbon steel electrodes were exposed to S. putrefaciens, microbiologically influenced corrosion was demonstrated electrochemically and microscopically.

Non-programmatic↗

NASA NTRS2015

Aram Chaos: a Long Lived Subsurface Aqueous Environment with Strong Water Resources Potential for Human Missions on Mars

Aram Chaos, Mars is a crater 280 kilometers in diameter with elevations circa. minus 2 to minus 3 kilometers below datum that provides a compelling landing site for future human explorers as it features multiple scientific regions of interest (ROI) paired with a rich extensible Resource ROI that features poly-hydrated sulfates [1]. The geologic history of Aram Chaos suggests several past episodes of groundwater recharge and infilling by liquid water, ice, and other materials [1-3]. The creation of the fractured region with no known terrestrial equivalent may have been caused by melting of deep ice reservoirs that triggered the collapse of terrain followed by catastrophic water outflows over the region. Aram Chaos is of particular scientific interest because it is hypothesized that the chaotic terrain may be the source of water that contributed to the creation of nearby valleys such as Ares Vallis flowing toward Chryse Planitia. The liquid water was likely sourced as groundwater and therefore represents water derived from a protected subsurface environment making it a compelling astrobiological site [2]. The past history of water is also represented by high concentrations of hematite, Fe-oxyhydroxides, mono-hydrated and poly-hydrated sulfates [1, 2]. Poly-hydrated sulfates are likely to contain abundant water that evolves at temperatures below 500 degrees Centigrade thus conferring Aram Chaos a potentially high value for early in-situ resource utilization (ISRU) [4]. The geologic history also calls for future prospecting of deep ice deposits and possibly liquid water via deep drilling. The most recent stratigraphic units in the central part of Aram Chaos are not fractured, and are part of a dome-shaped formation that features bright, poorly-consolidated material that contains both hydrated sulfates and ferric oxides according to OMEGA (Observatoire pour la Minéralogie, l'Eau, les Glaces et l'Activité) data [5]. These surface material characteristics are preliminary indications of their potential use in civil engineering activities that involve regolith moving and hauling, while further study is needed to assess traverse-ability challenges. The widespread distribution of sulfates is also of interest as a resource for the use of sulfur as a binding compound in regolith-based concrete for constructions. The terrain depressions caused by the rock fracturing events may challenge surface mobility but also suggest the possibility of using such natural features for additional shielding from space radiation and as emplacement of nuclear surface power reactors for the same reason. The high concentration of hematite (up to 16 percent) in some of the smoother recent terrains of the central part of Aram Chaos [2] is a favorable attribute for metal extraction ISRU to create iron-based feedstock for in-situ fabrication of replacement parts or their repairs. Preliminary data on Aram Chaos indicate that it offers a combination of many critical criteria for human missions to the surface of Mars: equatorial region at low Mars Orbiter Laser Altimeter (MOLA), evidence of hydrated minerals over large areas and at high concentrations tied to historic evidence of liquid water over long periods.

Sibille, L.↗