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NASA NTRS1992

Lunar resources: Oxygen from rocks and soil

The first set of hydrogen reduction experiments to use actual lunar material was recently completed. The sample, 70035, is a coarse-grained vesicular basalt containing 18.46 wt. percent FeO and 12.97 wt. percent TiO2. The mineralogy includes pyroxene, ilmenite, plagioclase, and minor olivine. The sample was crushed to a grain size of less than 500 microns. The crushed basalt was reduced with hydrogen in seven tests at temperatures of 900-1050 C and pressures of 1-10 atm for 30-60 minutes. A capacitance probe, measuring the dew point of the gas stream, was used to follow reaction progress. Experiments were also conducted using a terrestrial basalt similar to some lunar mare samples. Minnesota Lunar Simulant (MLS-1) contains 13.29 wt. percent FeO, 2.96 wt. percent Fe2O3, and 6.56 wt. percent TiO2. The major minerals include plagioclase, pyroxene, olivine, ilmenite, and magnetite. The rock was ground and seived, and experiments were run on the less than 74- and 500-1168-micron fractions. Experiments were also conducted on less than 74-micron powders of olivine, pyroxene, synthetic ilmenite, and TiO2. The terrestrial rock and mineral samples were reduced with flowing hydrogen at 1100 C in a microbalance furnace, with reaction progress monitored by weight loss. Experiments were run at atmospheric pressure for durations of 3-4 hr. Solid samples from both sets of experiments were analyzed by Mossbauer spectroscopy, petrographic microscopy, scanning electron microscopy, tunneling electron microscopy, and x-ray diffraction. Apollo 17 soil 78221 was examined for evidence of natural reduction in the lunar environment. This sample was chosen based on its high maturity level (I sub s/FeO = 93.0). The FeO content is 11.68 wt. percent and the TiO2 content is 3.84 wt. percent. A polished thin section of the 90-150 micron size fraction was analyzed by petrographic microscopy and scanning electron microscopy.

Allen, C. C.↗

NASA NTRS1993

First oxygen from lunar basalt

The Carbotek/Shimizu process to produce oxygen from lunar soils has been successfully demonstrated on actual lunar samples in laboratory facilities at Carbotek with Shimizu funding and support. Apollo sample 70035 containing approximately 25 percent ilmenite (FeTiO3) was used in seven separate reactions with hydrogen varying temperature and pressure: FeTiO3 + H2 yields Fe + TiO2 + H2O. The experiments gave extremely encouraging results as all ilmenite was reduced in every experiment. The lunar ilmenite was found to be about twice as reactive as terrestrial ilmenite samples. Analytical techniques of the lunar and terrestrial ilmenite experiments performed by NASA Johnson Space Center include iron Mossbauer spectroscopy (FeMS), optical microscopy, SEM, TEM, and XRD. The Energy and Environmental Research Center at the University of North Dakota performed three SEM techniques (point count method, morphology determination, elemental mapping), XRD, and optical microscopy.

Gibson, M. A.↗

NASA NTRS1993

The dregs of crystallization in Zagami

The Zagami shergottite is a basaltic meteorite which formed when a phenocryst-bearing lava flow was emplaced at or near the surface of Mars. Recently, a cm-sized olivine-rich lithology has been identified in Zagami by Mossbauer spectroscopy. Olivine is extremely rare in shergottites, particularly in Zagami and Shergotty, where it occurs only as minute grains. We report petrologic and microprobe studies of this olivine-rich lithology. This material represents the last few percent of melt and is highly enriched in phosphates, opaques and mesostases, all of which are late-stage crystallization products. Phosphates replaced augite as a phenocryst phase when the magma became saturated in P. This late stage melt also includes a fayalite-bearing, multi-phase intergrowth which crystallized after the melt became too rich in iron to crystallize pigeonite. We can now reconstruct the entire crystallization history of the Zagami shergottite from a deep-seated magma chamber to crystallization of the final few percent of melt in a near-surface dike or thick flow. Small pockets (tens of microns) of late-stage melt pockets are ubiquitous but volumetrically minor in Zagami. We do not know the physical relationship between these areas and the cm-sized olivine-rich material described here. It is possible that these small pockets were mobile, forming larger areas. Perhaps inspection of the entire hand specimen of Zagami would clarify this relationship.

Mccoy, T. J.↗

NASA NTRS1995

The effects of ion implantation on the tribology of perfluoropolyether-lubricated 440C stainless steel couples

The lubricating lifetime of thin films of a perfluoropolyether (PFPE) based on hexafluoropropene oxide in the presence of ion implanted 440C stainless steel is presented. Stainless steel discs, either unimplanted or implanted with N2, C, Ti, Ti + N2, or Ti + C had a thin film of PFPE (60-400 A) applied to them reproducibly (+/- 20 percent) and uniformly (+/- 15 percent) using a device developed for this study. The lifetimes of these films were quantified by measuring the number of sliding-wear cycles required to induce an increase in the friction coefficient from an initial value characteristic of the lubricated wear couple to a final, or failure value, characteristic of an unlubricated, unimplanted couple. The tests were performed in a dry nitrogen atmosphere (less than 1 percent RH) at room temperature using a 3 N normal load with a relative sliding speed of 0.05 m/s. The lubricated lifetime of the 440C couple was increased by an order of magnitude by implanting the disc with Ti. Ranked from most to least effective, the implanted species were: Ti; Ti+C; unimplanted; N2; C approximately equals Ti+N2. The mechanism postulated to explain these results involves the formation of a passivating or reactive layer which inhibits or facilitates the production of active sites. The corresponding surface microstructures induced by ion implantation, obtained using x-ray diffraction and conversion electron Mossbauer spectroscopy, ranked from most to least effective in enhancing lubricant lifetime were: amorphous Fe-Cr-Ti; amorphous Fe-Cr-Ti-C + TiC; unimplanted; epsilon-(Fe,Cr)(sub x)N, x = 2 or 3; amorphous Fe-Cr-C approximately equals amorphous Fe-Cr-Ti-N.

Shogrin, Bradley↗

NASA NTRS1994

The oxidation state of the surface of Venus

We present experimental results showing that basalt is oxidized in CO-CO2 gas mixtures having CO number densities close to those (approximately 2 times higher) at the surface of Venus. The results suggest that the red color observed by Pieters et al at the Venera 9 and 10 landing sites is due to subaerial oxidation of Fe(2+)-bearing basalt on the surface of Venus, and that hematite, instead of magnetite, is present on the surface of Venus. Well-characterized basalt powder was iosthermally heated in 1000 ppm CO-CO2 gas mixtures at atmospheric pressure for several days. The starting material and reacted samples were analyzed by Mossbauer spectroscopy to determine the amount of Fe(2+) and Fe(3+) in the samples. X-ray diffraction and optical microscopy were also used to characterize samples. The basalt oxidation occurs because the CO and CO2 do not equilibrate in the gas mixture at the low temperatures used. Thus, the basalt reacts with the more abundant CO2 and is oxidized. We propose that the red color of the surface of Venus is due to failure of CO and CO2 to equilibrate with one another in the near-surface atmosphere of Venus, leading to subaerial oxidation of erupted Fe(2+)-bearing basalts. Our interpretation is supported by our studies of magnetite oxidation, which show that synthetic magnetite powders are oxidized to hematite in CO-CO2 gas mixtures inside the magnetite stability field, by our studies of pyrite decomposition, and by independent work on CO-CO2 equilibration in furnace gases.

Fegley, B., Jr.↗

NASA NTRS1993

Assumptions about the presence of natural glasses on Mars

Natural glasses occur not only on Earth but also in lunar rocks and in some meteorites. On geological grounds, natural glasses could be expected on the surface of Mars and their presence would have important implications for the weathering and alteration of the near-surface layer. Ultramafic and mafic magmatism rich in iron and some volatiles appears to have been important on Mars as has been impact cratering, volcanism, and possibly hydrothermal alteration. Available data indicate that we can presume the past or present existence of volcanic basaltic glasses, impact glasses formed by thermal fusion of meteorite-impact targets, and diaplectic (mainly maskelynite) glasses. Conditions appear unsuitable for the formation of tektites on the Martian surface, and the production of measurable amounts of fulgurite or combustion glass seems improbable. Prospects for the remote and in-situ identification of Martian glasses and their subsequent weathering products are discussed and include orbital reflectance and thermal emission spectroscopic measurements and Mossbauer spectroscopy from a surface lander.

Bouska, Vladimir↗

NASA NTRS1993

Assumptions About the Presence of Natural Glasses on Mars

Natural glasses occur not only on Earth but also in lunar rocks and in some meteorites. On geological grounds, natural glasses could be expected on the surface of Mars and their presence would have important implications for the weathering and alteration of the near-surface layer. Ultramafic and mafic magmatism rich in iron and some volatiles appears to have been important on Mars as has been impact cratering, volcanism, and possibly hydrothennal alteration. Available data indicate that we can presume the past or present existence of volcanic basaltic glasses, impact glasses formed by thermal fusion of meteorite-impact targets, and diaplectic (mainly maskelynite) glasses. Conditions appear unsuitable for the formation of tektites on the Martian surface, and the production of measurable amounts of fulgurite or combustion glass seems improbable. Prospects for the remote and in situ identification of Martian glasses and their subsequent weathering products are discussed and include orbital reflectance and thermal emission spectroscopic measurements and Mossbauer spectroscopy from a surface lander.

Bouska, Vladimir↗

NASA NTRS1993

Assumption About the Presence of Natural Glasses on Mars

Natural glasses occur not only on Earth but also in lunar rocks and in some meteorites. On geological grounds, natural glasses could be expected on the surface of Mars and their presence would have important implications for the weathering and alteraton of the near-surface layer. Ultramafic and mafic magmatism rich in iron and some volatiles appears to have been important on Mars as has been impact cratering, volcanism, and possibly hydrothertnal alteration, Available data indicate that we can presume the past or present existence of volcanic basaltic glasses, impact glasses formed by thermal fusion of meteorite-impact targets, and diaplectic (mainly maskelynite) glasses. Conditions appear unsuitable for the formation of tektites on the Martian surface, and the production of measurable amounts of fulgurite or combustion glass seems improbable. Prospects for the remote and in situ identificaton of Martian glasses and their subsequent weathering products are discussed and include orbital reflectance and thermal emission spectroscopic measurements and Mossbauer spectroscopy from a surface lander.

Bouska, Vladimir↗

NASA NTRS2004

Hydrogen and Ferric Iron in Mars Materials

Knowledge of oxygen and hydrogen fugacity is of paramount importance in constraining phase equilibria and crystallization processes of melts, as well as understanding the partitioning of elements between the cope and silicate portions of terrestrial planets. H and Fe(3+) must both be analyzed in order to reconstruct hydrogen and oxygen fugacities on Mars. To date, SIMS data have elucidated D/H and H contents of hydrous phases in SNC meteorites, but until now anhydrous martian minerals have not been systematically examined for trace hydrogen. Ferric iron has been quantified using XANES in many martian phases, but integrated studies of both Fe(3+) and H on the same spots are really needed to address the H budget. Finally, the effects of shock on both Fe(3+) and H in hydrous and anhydrous phases must be quantified. Thus, the overall goal of this research was to understand the oxygen and hydrogen fugacities under which martian samples crystallized. In this research one-year project, we approached this problem by 1) characterizing Fe(3+) and H contents of SNC meteorites using both bulk (Mossbauer spectroscopy and uranium extraction, respectively) and microscale (synchrotron micro-XANES and SIMS) methods; 2) relating Fe(3+) and H contents of martian minerals to their oxygen and hydrogen fugacities through analysis of experimentally equilibrated phases (for pyroxene) and through study of volcanic rocks in which the oxygen and hydrogen fugacities can be independently constrained (for feldspar); and 3) studying the effects of shock processes on Fe(3+) and H contents of the phases of interest. Results have been used to assess quantitatively the distribution of H and Fe(3+) among phases in the martian interior, which will better constrain the geodynamic processes of the interior, as well as the overall hydrogen and water budgets on Mars. There were no inventions funded by this research.

Dyar, Melinda D.↗

NASA NTRS2005

Integrated Spectroscopic Studies of Anhydrous Sulfate Minerals

Sulfates have been identified in Martian soils and bedrock and are emerging as an important indicator for aqueous activity on Mars. Sulfate minerals can form in a variety of low-temperature (evaporitic; chemical-weathering) and high-temperature (volcanic/fumarolic; hydrothermal) environments and their formational environments can range from alkaline to acidic. Although sulfates generally form in the presence of water, not all sulfates are hydrous or contain water in their structures. Many of these anhydrous sulfates (Dana group 28; Strunz class 67A) are minerals that form as accompanying phases to the main minerals in ore deposits or as replacement deposits in sedimentary rocks. However, some form from thermal decomposition of OH or H2O-bearing sulfates, such as from the reaction [1]: jarosite = yavapaiite + Fe2O3 + H2O. Where known, the stability fields of these minerals all suggest that they would be stable under martian surface conditions [2]. Thus, anhydrous sulfate minerals may contribute to martian surface mineralogy, so they must be well-represented in spectral libraries used for interpretation of the Martian surface. We present here the preliminary results of an integrated study of emittance, reflectance, and Mossbauer spectroscopy of a suite of wel-lcharacterized anhydrous sulfates.

Lane, M. D.↗

NASA NTRS2005

Effects of Variable Temperature on Mossbauer Data Acquisition: Laboratory-based and MER A Results

Mossbauer spectrometers on the Spirit and Opportunity rovers have played a valuable role in identifying mineralogy at both the Gusev and Meridiani landing sites. Key to the application of Mossbauer results is the issue of how accurately the peak positions, on which the mineral identifications are based, can be determined. Remote Mossbauer spectroscopy has by necessity some unusual experimental constraints that may influence the confidence with which peak positions can be fit. We present here an analysis of the effects of variable temperature and short duration run times on spectral resolution.

Rothstein, Y.↗

NASA NTRS2006

Understanding Surface Processes on Mars Through Study of Iron Oxides/Oxyhydroxides: Clues to Surface Alteration and Aqueous Processes

We are performing oxidation and reduction reactions on hydrated ferric oxide minerals in order to investigate how these might alter under a variety of conditions on the surface of Mars. Preliminary experiments on ferrihydrite and goethite showed that heating these minerals in a dry oxidizing environment produces fine-grained hematite, while heating these minerals in a reducing environment produces fine-grained magnetite. Under Mars-like oxidation levels this magnetite then oxidizes to maghemite. These reactions are dependent on the presence of water and organic material that can act as a reductant. We are using reflectance and Mossbauer spectroscopy to characterize the reaction products and TEM to analyze the sample texture. Our preliminary results indicate that magnetite and maghemite could be formed in the soil on Mars from ferrihydrite and goethite if organics were present on early Mars.

Bishop, J. L.↗

NASA NTRS2007

Experimental Shock Decomposition of Siderite and the Origin of Magnetite in Martian Meteorite ALH84001

Shock recovery experiments to determine whether magnetite could be produced by the decomposition of iron-carbonate were initiated. Naturally occurring siderite was first characterized by electron microprobe (EMP), transmission electron microscopy (TEM), Mossbauer spectroscopy, and magnetic susceptibility measurements to be sure that the starting material did not contain detectable magnetite. Samples were shocked in tungsten-alloy holders (W=90%, Ni=6%, Cu=4%) to further insure that any iron phases in the shock products were contributed by the siderite rather than the sample holder. Each sample was shocked to a specific pressure between 30 to 49 GPa. Previously reported results of TEM analyses on 49 GPa experiments indicated the presence of nano-phase spinel-structured iron oxide. Transformation of siderite to magnetite as characterized by TEM was found in the 49 GPa shock experiment. Compositions of most magnetites are greater than 50% Fe sup(+2) in the octahedral site of the inverse spinel structure. Magnetites produced in shock experiments display the same range of single-domain, superparamagnetic sizes (approx. 50 100 nm), compositions (100% magnetite to 80% magnetite-20% magnesioferrite), and morphologies (equant, elongated, euhedral to subhedral) as magnetites synthesized by Golden et al. (2001) or magnetites grown naturally by MV1 magnetotactic bacteria, and as the magnetites in Martian meteorite ALH84001. Fritz et al. (2005) previously concluded that ALH84001 experienced approx. 32 GPa pressure and a resultant thermal pulse of approx. 100 - 110 C. However, ALH84001 contains evidence of local temperature excursions high enough to 1 melt feldspar, pyroxene, and a silica-rich phase. This 49 GPa experiment demonstrates that magnetite can be produced by the shock decomposition of siderite as a result of local heating to greater than 470 C. Therefore, magnetite in the rims of carbonates in Martian meteorite ALH84001 could be a product of shock devolatilization of siderite as well.

Bell, Mary Sue↗

NASA NTRS2008

Structural, Physical, and Compositional Analysis of Lunar Simulants and Regolith

Relative to the prior manned Apollo and unmanned robotic missions, planned Lunar initiatives are comparatively complex and longer in duration. Individual crew rotations are envisioned to span several months, and various surface systems must function in the Lunar environment for periods of years. As a consequence, an increased understanding of the surface environment is required to engineer and test the associated materials, components, and systems necessary to sustain human habitation and surface operations. The effort described here concerns the analysis of existing simulant materials, with application to Lunar return samples. The interplay between these analyses fulfills the objective of ascertaining the critical properties of regolith itself, and the parallel objective of developing suitable stimulant materials for a variety of engineering applications. Presented here are measurements of the basic physical attributes, i.e. particle size distributions and general shape factors. Also discussed are structural and chemical properties, as determined through a variety of techniques, such as optical microscopy, SEM and TEM microscopy, Mossbauer Spectroscopy, X-ray diffraction, Raman microspectroscopy, inductively coupled argon plasma emission spectroscopy and energy dispersive X-ray fluorescence mapping. A comparative description of currently available stimulant materials is discussed, with implications for more detailed analyses, as well as the requirements for continued refinement of methods for simulant production.

Greenberg, Paul↗

NASA NTRS2017

Examination of Multiple Lithologies Within the Primitive Ordinary Chondrite NWA 5717

Northwest Africa 5717 is a primitive (subtype 3.05) ungrouped ordinary chondrite which contains two apparently distinct lithologies. In large cut meteorite slabs, the darker of these, lithology A, looks to host the second, much lighter in color, lithology B (upper left, Fig. 1). The nature of the boundary between the two is uncertain, ranging from abrupt to gradational and not always following particle boundaries. The distinction between the lithologies, beyond the obvious color differences, has been supported by a discrepancy in oxygen isotopes and an incongruity in the magnesium contents of chondrule olivine. Here, quantitative textural analysis and mineralogical methods have been used to investigate the two apparent lithologies within NWA 5717. Olivine grains contained in a thin section from NWA 7402, thought to be paired to 5717, were also measured to re-examine the distinct compositional range among the light and dark areas. Procedure: Particles from a high-resolution mosaic image of a roughly 13x15cm slice of NWA 5717 were traced in Adobe Photoshop. Due to the large size of the sample, visually representative regions of each lithology were chosen to be analyzed. The resulting layers of digitized particles were imported into ImageJ, which was used to measure their area, along with the axes, the angle from horizontal, and the centroid coordinates of ellipses fitted to each particle following the approach. Resulting 2D pixel areas were converted to spherical diameters employing the unfolding algorithm, which outputs a 3D particle size distribution based on digitized 2D size frequency data. Spatstat was used to create kernel density plots of the centroid coordinates for each region. X-ray compositional maps, microprobe analyses, and Mossbauer spectroscopy was conducted on a thin section of NWA 7402, tentatively paired to NWA 5717.

Cato, M. J.↗

NASA NTRS2017

Smectite Formation in the Presence of Sulfuric Acid: Implications for Acidic Smectite Formation on Early Mars

The excess of orbital detection of smectite deposits compared to carbonate deposits on the martian surface presents an enigma because smectite and carbonate formations are both favored alteration products of basalt under neutral to alkaline conditions. We propose that Mars experienced acidic events caused by sulfuric acid (H2SO4) that permitted phyllosilicate, but inhibited carbonate, formation. To experimentally verify this hypothesis, we report the first synthesis of smectite from Mars-analogue glass-rich basalt simulant (66 wt% glass, 32 wt% olivine, 2 wt% chromite) in the presence of H2SO4 under hydrothermal conditions (approximately 200 degC). Smectites were analyzed by X-ray diffraction, Mossbauer spectroscopy, visible and near-infrared reflectance spectroscopy and electron microprobe to characterize mineralogy and chemical composition. Solution chemistry was determined by Inductively Coupled Plasma Mass Spectrometry. Basalt simulant suspensions in 11-42 mM H2SO4 were acidic with pH less than or equal to 2 at the beginning of incubation and varied from acidic (pH 1.8) to mildly alkaline (pH 8.4) at the end of incubation. Alteration of glass phase during reaction of the basalt simulant with H2SO4 led to formation of the dioctahedral smectite at final pH approximately 3 and trioctahedral smectite saponite at final pH approximately 4 and higher. Anhydrite and hematite formed in the final pH range from 1.8 to 8.4 while natroalunite was detected at pH 1.8. Hematite was precipitated as a result of oxidative dissolution of olivine present in Adirondack basalt simulant. Formation of secondary phases, including smectite, resulted in release of variable amounts of Si, Mg, Na and Ca while solubilization of Al and Fe was low. Comparison of mineralogical and solution chemistry data indicated that the type of smectite (i.e., dioctahedral vs trioctahedral) was likely controlled by Mg leaching from altering basalt and substantial Mg loss created favorable conditions for formation of dioctahedral smectite. We present a model for global-scale smectite formation on Mars via acid-sulfate conditions created by the volcanic outgassing of SO2 in the Noachian and early Hesperian.

Smectite↗

NASA NTRS1972

Mg/2+/-Fe/2+/ order-disorder in cummingtonite, /Mg, Fe/7Si8O22/OH/2 - A new geothermometer.

Determination of the temperature dependence of the Mg(2+)-Fe(2+) distribution between the M4 site and the M1, M2 and M3 sites in magnesium-rich cummingtonites by Fe-57 Mossbauer resonance spectroscopy. For the basic reversible ion-exchange reaction involved, the Gibbs free energy is estimated to be 3.6 to 4.1 kcal/mole, assuming an ideal solution model at each set of sites. The crystallization temperatures of two cummingtonite-bearing metamorphosed ultrabasic rocks are estimated to be 265 and 290 deg C. The Mossbauer resonance spectra are found to be an effective basis for detecting changes in site occupancies as a function of temperature.

Ghose, S.↗

NASA NTRS2004

Basaltic rocks analyzed by the Spirit Rover in Gusev Crater

The Spirit landing site in Gusev Crater on Mars contains dark, fine-grained, vesicular rocks interpreted as lavas. Pancam and Mini-Thermal Emission Spectrometer (Mini-TES) spectra suggest that all of these rocks are similar but have variable coatings and dust mantles. Magnified images of brushed and abraded rock surfaces show alteration rinds and veins. Rock interiors contain </=25% megacrysts. Chemical analyses of rocks by the Alpha Particle X-ray Spectrometer are consistent with picritic basalts, containing normative olivine, pyroxenes, plagioclase, and accessory FeTi oxides. Mossbauer, Pancam, and Mini-TES spectra confirm the presence of olivine, magnetite, and probably pyroxene. These basalts extend the known range of rock compositions composing the martian crust.

Minerals↗