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NASA NTRS2006

Formation of "Chemically Pure" Magnetite from Mg-Fe-Carbonates Implications for the Exclusively Inorganic Origin of Magnetite and Sulfides in Martian Meteorite ALH84001

Magnetite and sulfides in the black rims of carbonate globules in Martian meteorite ALH84001 have been studied extensively because of the claim by McKay et al. that they are biogenic in origin. However, exclusively inorganic (abiotic) processes are able to account for the occurrence of carbonate-sulfide-magnetite assemblages in the meteorite. We have previously precipitated chemically zoned and sulfide-bearing carbonate globules analogous to those in ALH84001 (at less than or equal to 150 C) from multiple fluxes of variable-composition Ca-Mg-Fe-CO2-S-H2O solutions. Brief heating of precipitated globules to approx. 470 C produced magnetite and pyrrhotite within the globules by thermal decomposition of siderite and pyrite, respectively. We have also shown that morphology of magnetite formed by inorganic thermal decomposition of Fe-rich carbonate is similar to the morphology of so-called biogenic magnetite in the carbonate globules of ALH84001. Magnetite crystals in the rims of carbonate globules in ALH84001 are chemically pure [Note: "Chemically pure" is defined here as magnetite with Mg at levels comparable or lower than Mg detected by [8] in ALH84001 magnetite]. A debate continues on whether or not chemically pure magnetite can form by the thermal decomposition of mixed Mg-Fe-carbonates that have formed under abiotic conditions. Thomas-Keprta et al. argue that it is not possible to form Mg-free magnetite from Mg-Fe-carbonate based on thermodynamic data. We previously suggested that chemically pure magnetite could form by the thermal decomposition of relatively pure siderite in the outer rims of the globules. Mg-Fe-carbonates may also thermally decompose under conditions conducive for formation of chemically pure magnetite. In this paper we show through laboratory experiments that chemically pure magnetite can form by an inorganic process from mixed Mg-Fe-carbonates.

Golden, D. C.↗
NASA NTRS2004

Process for Making Single-Domain Magnetite Crystals

A process for making chemically pure, single-domain magnetite crystals substantially free of structural defects has been invented as a byproduct of research into the origin of globules in a meteorite found in Antarctica and believed to have originated on Mars. The globules in the meteorite comprise layers of mixed (Mg, Fe, and Ca) carbonates, magnetite, and iron sulfides. Since the discovery of the meteorite was announced in August 1996, scientists have debated whether the globules are of biological origin or were formed from inorganic materials by processes that could have taken place on Mars. While the research that led to the present invention has not provided a definitive conclusion concerning the origin of the globules, it has shown that globules of a different but related chemically layered structure can be grown from inorganic ingredients in a multistep precipitation process. As described in more detail below, the present invention comprises the multistep precipitation process plus a subsequent heat treatment. The multistep precipitation process was demonstrated in a laboratory experiment on the growth of submicron ankerite crystals, overgrown by submicron siderite and pyrite crystals, overgrown by submicron magnesite crystals, overgrown by submicron siderite and pyrite. In each step, chloride salts of appropriate cations (Ca, Fe, and Mg) were dissolved in deoxygenated, CO2- saturated water. NaHCO3 was added as a pH buffer while CO2 was passed continuously through the solution. A 15-mL aliquot of the resulting solution was transferred into each of several 20 mL, poly(tetrafluoroethylene)-lined hydrothermal pressure vessels. The vessels were closed in a CO2 atmosphere, then transferred into an oven at a temperature of 150 C. After a predetermined time, the hydrothermal vessels were removed from the oven and quenched in a freezer. Supernatant solutions were decanted, and carbonate precipitates were washed free of soluble salts by repeated decantations with deionized water.

Golden, D. C.↗
NASA NTRS2015

Carbon and Oxygen Isotope Measurements of Ordinary Chondrite (OC) Meteorites from Antarctica Indicate Distinct Carbonate Species Using a Stepped Acid Extraction Procedure

The purpose of this study is to characterize the stable isotope values of terrestrial, secondary carbonate minerals from five Ordinary Chondrite (OC) meteorites collected in Antarctica. These samples were identified and requested from NASA based upon their size, alteration history, and collection proximity to known Martian meteorites. They are also assumed to be carbonate-free before falling to Earth. This research addresses two questions involving Mars carbonates: 1) characterize terrestrial, secondary carbonate isotope values to apply to Martian meteorites for isolating in-situ carbonates, and 2) increase understanding of carbonates formed in cold and arid environments with Antarctica as an analog for Mars. Two samples from each meteorite, each approximately 0.5 grams, were crushed and dissolved in pure phosphoric acid for 3 sequential reactions: a) R times 0 for 1 hour at 30 degrees Centigrade (fine calcite extraction), b) R times 1 for 18 hours at 30 degrees Centigrade (course calcite extraction), and c) R times 2 for 3 hours at 150 degrees Centigrade (siderite and/or magnesite extraction). CO (sub 2) was distilled by freezing with liquid nitrogen from each sample tube, then separated from organics and sulfides with a TRACE GC using a Restek HayeSep Q 80/100 6 foot 2 millimeter stainless column, and then analyzed on a Thermo MAT 253 Isotope Ratio Mass Spectrometer (IRMS) in Dual Inlet mode. This system was built at NASA/JSC over the past 3 years and proof-tested with known carbonate standards to develop procedures, assess yield, and quantify expected error bands. Two distinct species of carbonates are found: 1) calcite, and 2) non-calcite carbonate (future testing will attempt to differentiate siderite from magnesite). Preliminary results indicate the terrestrial carbonates are formed at approximately sigma (sup 13) C equal to plus 5 per mille, which is consistent with atmospheric CO (sub 2) sigma (sup 13) C equal to minus 7 per mille and fractionation of plus12 per mille based upon polar temperature of -20 degrees Centigrade. The oxygen values fractionate sigma (sup 18) O equal to minus 10-20 per mille lighter between the R times 0 and R times 1 reactions at 30 degrees Centigrade. The carbonate oxygen isotope measurements are consistently heavier than expected with meteoric water and temperatures from Antarctica, perhaps due to secondary carbonate formation during curation in Houston, TX.

Evans, Michael E.↗
NASA NTRS2017

Effects of Martian Surface Materials on the Thermal Decomposition of Hydrogen Peroxide

While hydrogen peroxide (H2O2) has been detected in the martian atmosphere, it has not been detected in surface materials. Since the Viking lander mission, we have sent instruments to Mars with the capability to detect H2O2. The Sample Analysis at Mars (SAM) instrument onboard the Curiosity Rover and Thermal and Evolved Gas Analyzer (TEGA) instrument on the Phoenix lander both detected water and oxygen releases from analyzed sediments but whether or not peroxide could be the source of these gases has not been investigated. We are investigating the possible presence of H2O2 in martian materials by analyzing Mars-relevant minerals that have been mixed with hydrogen peroxide using lab instruments configured as analogs to Mars mission instruments. The object of this research is to use lab instruments to find the effects of Mars analog minerals on hydrogen peroxide gas release temperatures, specifically gas releases of water and oxygen and also determine the effect of the peroxide on the minerals. Data that we get from the lab can then be compared to the data collected from Mars. The minerals hematite, siderite, San Carlos olivine, magnetite and nontronite were chosen as our Mars analog minerals. ~20 mg of analog Mars minerals with 5μl of 50% H2O2, and were either run immediately or placed in a sealed tube for 2, 4, or 9 days to look for changes over time with two reps being done at each time step to determine repeatability. Each sample was heated from -60 degC to 500 degC at 20 degC/min and the evolved gases were monitored with a mass spectrometer. Each sample was also analyzed with an X-ray diffraction instrument to look for changes in mineralogy. Preliminary results show three potential outcomes: 1) peroxide has no effect on the sample (e.g., hematite), 2) the mineral is unaffected but catalyzes peroxide decomposition (magnetite, siderite), or 3) peroxide alters the mineral (pyrrhotite, San Carlos olivine).

Archer, P. D., Jr.↗
NASA NTRS1974

Composition of the gases associated with the magmas that produced rocks 15016 and 15065

Gases may be trapped in crystallizing minerals in many different ways but gas analyses can provide geologically meaningful information only if the gases can be related to their specific locations in the host mineral. The gases trapped in glass inclusions can be representative samples of the gases associated with the magma adjacent to the mineral at the time it crystallized. Analyses of the gases in glass inclusions in gabbro 15065,44 and basalt 15016,48 show that in both cases the gases in the parent magma started with a composition close to 46% oxygen, 42% carbon and 12% hydrogen and became more water-rich as crystallization progressed. This enrichment is probably due to a selective removal of the less soluble carbon compounds into the vapor phase. Some of the volatile components may react with the rock as temperature falls to give siderite and possibly hydrous phases.

Barker, C.↗
NASA NTRS1977

Geochemical and mineralogical interpretation of the Viking inorganic chemical results

The current status of geochemical, mineralogical, petrological interpretation of refined Viking Lander data is reviewed, and inferences that can be drawn from data on the composition of Martian surface materials are presented. The materials are dominantly fine silicate particles admixed with, or including, iron oxide particles. Both major element and trace element abundances in all samples are indicative of mafic source rocks (rather than more highly differentiated salic materials). The surface fines are nearly identical in composition at the two widely separated Lander sites, except for some lithologic diversity at the 100-m scale. This implies that some agency (presumably aeolian processes) has thoroughly homogenized them on a planetary scale. The most plausible model for the mineralogical constitution of the fine-grained surface materials at the two Lander sites is a fine-grained mixture dominated by iron-rich smectites, or their degradation products, with ferric oxides, probably including maghemite and carbonates (such as calcite), but not such less stable phases as magnesite or siderite.

Toulmin, P., III↗
NASA NTRS1986

A model for the biological precipitation of Precambrian iron-formation

A biological model for the precipitation of Precambrian iron formations is presented. Assuming an oxygen deficient atmosphere and water column to allow sufficient Fe solubility, it is proposed that local oxidizing environments, produced biologically, led to precipitation of iron formations. It is further suggested that spheroidal structures about 30 mm in diameter, which are widespread in low grade cherty rion formations, are relict forms of the organic walled microfossil Eosphaera tylerii. The presence of these structures suggests that the organism may have had a siliceous test, which allowed sufficient rigidity for accumulation and preservation. The model involves precipitation of ferric hydrates by oxidation of iron in the photic zone by a variety of photosynthetic organisms. Silica may have formed in the frustules of silica secreting organisms, including Eosphaera tylerii. Iron formates formed, therefore, by a sediment rain of biologically produced ferric hydrates and silica and other organic material. Siderite and hematite formed diagenetically on basin floors, and subsequent metamorphism produced magnetite and iron silicates.

Laberge, G. L.↗
NASA NTRS1986

A carbonate-rich, hydrated, interplanetary dust particle Possible residue from protostellar clouds

Transmission electron microscopy of a hydrated interplanetary dust particle (IDP) indicates that it contains abundant magnesium-iron carbonates, primarily breunnerite and magnesian siderite. This IDP displays a strong absorption band at 6.8 micrometers in its infrared spectrum, similar to that in certain protostellar spectra. The carbonates probably account for the 6.8-micrometer band in the IDP spectrum, suggesting that carbonate also may occur in interstellar dust and be the source of the controversial 6.8-micrometer feature from the protostellar spectra.

Tomeoka, K.↗
NASA NTRS1993

Derivation of the midinfrared (5.0-25.0 micron) optical constants of hydrous carbonate and sulfate

There is ample theoretical and observational evidence suggesting liquid water was once stable at the surface of Mars. Because water is essential to the evolution of life, it is important to understand the types of environments in which the liquid water was present. For example, if water were present early in Mars' history, then this raises the possibility that biological activity may have evolved only to eventually become extinct as liquid water became scarce. Alternatively, if liquid water were stable only later in Mars' history, then it becomes problematic to envision mechanisms by which biological activity evolved and remained viable without water until more favorable conditions existed. Even without biological activity, atmospheric carbon dioxide dissolved in water can assist the chemical weathering of primary igneous minerals producing common secondary phases such as hydartes, carbonates, and sulfates. While the identification of hydrates, carbonates, and sulfates on Mars cannot provide direct evidence of biological activity, it can provide significant information regarding the presence and duration of an environment that would support the presence of liquid water at the surface. The specific mineralogy of these secondary phases can provide insight into the environments of their formation. For example, the slow precipitation that occurs in large standing bodies of water, e.g. oceans or lakes, commonly results in the formation of calcite, magnesite, dolomite, siderite, and rhodochrosite. Rapid precipitation that occurs in ephemeral bodies of water, e.g. hypersaline lakes or playas, can result in the formation of all of the above phases as well as aragonite, vaterite, hydrated carbonates, alkali carbonates, bicarbonates, and other poorly ordered phases. Absorption features identified in recent near-infrared spectra of Mars have been interpreted as being due to bicarbonate and bisulfate located in the mineral scaplite. Spectral data returned by the Mariner 6 and 7 spacecraft have been inerpreted as remaining consistent with the presence of hydrated carbonates. Additional, airborne thermal infrared spectra of Mars have been interpreted as implying the presence of carbonates, sulfates, and hydrates. Modeling of the thermal infrared data relied upon the optical constants of calcite anhydrite and a mixture of water in basalt because of their availability. The derived abundances of carbonate and sulfate were 1-3 percent and 10-15 percent by volume. However, the observed complexity and positions of the bands suggested other carbonate-, and sulfate-bearing species. We have already derived optical constants for hydrous and anhydrous silicates, and we are now applying these techniques to the derivation of the optical constants of hydrous carbonate and sulfate.

Roush, Ted L.↗
NASA NTRS1994

Volatiles in the deep Earth: An experimental study using the laser-heated diamond cell

Experiments with the laser-heated diamond cell show that H2O and CO2 can be stabilized within crystalline mineral structures of the lower-mantle, and hence can be present at relatively non-volatile components of the Earth's deep interior. Samples quenched from high pressures and temperatures document that the MgCO3-FeCO3 magnesite-siderite solid-solution is stable and coexists with (Mg,Fe)SiO3 perovskite at 30-40 GPa and approximately 1500-2000 K. In contrast, H2O combines with the silicate to form (Mg,Fe)SiH2O4 phase D, coexisting with (Mg,Fe)SiO3 perovskite at these conditions. If enough water is present, phase D can become the predominant phase in the MgSiO3-H2O system at lower-mantle conditions. Our work extends previous studies to Fe-bearing compositions and to the pressures of the mid-lower mantle. Thus, the results of high-pressure experiments suggest that both H2O and CO2 can be abundant in the Earth's lower mantle, being present in stable hydroxisilicate and carbonate phases.

Li, Xiaoyuan↗
NASA NTRS1994

Ammonia on the prebiotic Earth: Iron(II) reduction of nitrite

Theories for the origin of life require the availability of reduced nitrogen. In the non-reducing atmosphere suggested by geochemical evidence, production in the atmosphere and survival of NH3 against photochemical destruction are problematic. Electric discharges and impact shocks would produce NO rather than HCN or NH3. Conversion of NO to nitrous and nitric acid (by way of HNO) and precipitation in acid rain would provide a source of fixed nitrogen to the early ocean. One solution to the NH3 problem may have been the reduction of nitrite/nitrate in the ocean with aqueous ferrous iron, Fe(2+): 6Fe(+2) + 7 H2O + NO2(-) yields 3Fe2O3 + 11 H(+) + NH3. We have measured the kinetics of this reaction as a function of temperature, pH, and concentrations of salts, Fe(+2), and NO2(-). Cations (Na(+), Mg(2+), K(+)) and anions (Cl(-), Br(-), SO4(2-)) increase the rate by factors of 4 to 8. Although a competing pathway yields N2, the efficiency of the conversion of nitrite to ammonia ranges from 25% to 85%. Nitrate reduction was not consistently reproducible; however, when it was observed, its rate was slower by at least 8X than that of nitrite reduction. If the prebiotic atmosphere contained 0.2 to 10 atmospheres CO2 as suggested by Walker (1985), the Fe(+2) concentration and the rate would have been limited by siderite (FeCO3) solubility.

Summers, David P.↗
NASA NTRS1994

Hydrous carbonates on Mars? Evidence from Mariner 6/7 infrared spectrometer and ground-based telescopic spectra

Absorption features at 2.28 and 5.4 micrometers identified in Mariner 6/7 infrared spectrometer and terrestrial telescopic spectra are consistent with the spectra of hydrous magnesium carbonates such as hydromagnesite and artinite. Spectral characteristics of these hydrous carbonates are different from those of the anhydrous carbonates, as the former do not have the strong spectral features typically associated with anhydrous carbonates such as calcite and siderite. Theoretical mixing indicates that, depending on the type of hydrous carbonate, 10-20 wt % can be incorporated into the regolith without contradicting the spectral observations or the Viking x ray fluorescence chemical analysis. Hydrous carbonates form as weathering products of mafic minerals in the presence of H2O and CO2, even in the Antarctic. Their formation as evaporite minerals from either original magmas or hydrothermally altered rocks is consistent with the Martian environment, provided liquid water is or has been at least transiently present. On Earth, formation of hydrous Mg carbonates is associated with the production of amorphous iron oxides, which is consistent with both the environment and the inferred surface mineralogy of Mars. These minerals are about 60 wt % H2O, CO3, and OH; if they are abundant everywhere at the 10% level, then about 6% of the surface weight could be volatiles bound in this type of mineral. Although the spectroscopic evidence for anhydrous carbonates is scant, the possible presence of hydrous carbonates provides an appealing mechanism for the existence of carbonates on Mars.

Calvin, Wendy M.↗
NASA NTRS2000

Differential Scanning Calorimetry of Volatile-Bearing Iron Minerals Under Mars-Like Pressures: New Insights Into Energetics and Mechanisms of Thermal Decomposition

In this study, we have examined the thermal decomposition of two volatile-bearing iron minerals, in particular, lepidocrocite (gamma-FeOOH) and siderite (FeCO3), under Mars-like pressures. Both minerals exhibit different enthalpic events during their decomposition at reduced atmospheric pressures when compared to those at ambient pressure. These differences in energetics are related to the mechanisms of thermal decomposition at Mars-like pressures. Such knowledge regarding the thermal stability of volatile-bearing minerals on Mars will provide useful information for planetary surface processes.

Lin, I.-C.↗
NASA NTRS1999

Carbon Dioxide Cycling, Climate, Impacts, and the Faint Young Sun

Evidence for relatively mild climates on ancient Earth and Mars has been a puzzle in light of the faint early sun. The geologic evidence, although far from conclusive, would appear to indicate that the surfaces of both planets were, if anything, warmer ca. 3-4 Ga than they are now. The astrophysical argument that the sun ought to have brightened approx. 30% since it reached the main sequence is hard to refute. There results a paradox between the icehouse we expect and the greenhouse we think we see. The usual fix has been to posit massive CO2 atmospheres, although reduced gases (e.g., NH3 or CH4 ) have had their partisans. Evidence against siderite in paleosols dated 2.2-2.75 Ga sets a rough upper limit of 30 PAL (present atmospheric levels) on pCO2 at that time. This is an order of magnitude short of what is needed to defeat the fainter sun. We present here an independent argument against high pCO2 on early Earth that applies not only to the Archean but yet more forcefully to the Hadean era. Additional information is contained in the original extended abstract.

Zahnle, K. J.↗
NASA NTRS1999

Isotopic Constraints on the Genesis of Carbonates in Martian Meteorite ALH 84001

Oxygen isotopic analyses in approximately 20 micrometer spots in a chemically diverse suite of carbonates from ALH 84001 show highly variable delta(exp 18)O values from +5.4 to +25.3%. The isotopic data are correlated with the major element composition of the carbonate. The earliest forming (Ca-rich) carbonates have the lowest delta(exp 18)O values and the late-forming Mg-rich carbonates have the highest delta(exp 18)O values. Two models that can explain the isotopic variation were investigated. The carbonates could have formed in a water-rich environment at relatively low, but highly variable temperatures. In this open-system case the lower limit to the temperature variation is approximately 125 C, with fluctuations of over 250 C possible within the constraints of the model, depending on fluid composition. Alternatively the data can be explained by a closed-system model in which carbonates precipitated from a limited amount of a CO2-rich fluid. This scenario can reproduce the range of isotopic values observed, even at relatively high temperatures (greater than 500 C). Thus, the oxygen isotopic compositions do not provide unequivocal evidence for formation of the carbonates at low temperature. Neither of these scenarios is consistent with a biological origin of the carbonates and their associated features. Olivine from ALH 84001 occurs as clusters within orthopyroxene adjacent to fractures containing disrupted carbonate globules and feldspathic shock glass. The inclusions are irregular in shape and range in size from approximately 40 micrometers to submicrometer. The olivine exhibits a limited range of chemical composition from Fo(sub 65) to Fo(sub 66). We measured delta(exp 18)O values of the olivine to be +5.1 +/- 1.4%, indistinguishable within uncertainty from the host orthopyroxene. The data suggest that the olivine formed at high temperature (greater than 800 C), and is probably unrelated to carbonate formation. Instead the olivine probably formed by metamorphic reactions involving either dehydration of hydrous silicates or reduction of opx + spinel. If the reactions took place after carbonate formation, they could have caused devolatilization of siderite, producing the magnetite in the ALH carbonate globules. This scenario is also inconsistent with a biological origin for the features in ALH 84001.

Leshin, Laurie A.↗
NASA NTRS2001

Higher Flux from the Young Sun as an Explanation for Warm Temperatures for Early Earth and Mars

Observations indicate that the Earth was at least warm enough for liquid water to exist as far back as 4 Gyr ago, namely, as early as half a billion years after the formation of the Earth; in fact, there is evidence suggesting that Earth may have been even warmer then than it is now. These relatively warm temperatures required on early Earth are in apparent contradiction to the dimness of the early Sun predicted by the standard solar models. This problem has generally been explained by assuming that Earth's early atmosphere contained huge amounts of carbon dioxide (CO2), resulting in a large enough greenhouse effect to counteract the effect of a dimmer Sun. However, recent work places an upper limit of 0.04 bar on the partial pressure of CO2 in the period from 2.75 to 2.2 Gyr ago, based on the absence of siderite in paleosols; this casts doubt on the viability of a strong CO2 greenhouse effect on early Earth. The existence of liquid water on early Mars has been even more of a puzzle; even the maximum possible CO2 greenhouse effect cannot yield warm enough Martian surface temperatures. These problems can be resolved simultaneously for both Earth and Mars, if the early Sun was brighter than predicted by the standard solar models. This could be accomplished if the early Sun was slightly more massive than it is now, i.e., if the solar wind was considerably stronger in the past than at present. A slightly more massive young Sun would have left fingerprints on the internal structure of the present Sun. Today, helioseismic observations exist that can measure the internal structure of the Sun with very high precision. The task undertaken here was to compute solar models with the highest precision possible at this time, starting with slightly greater initial masses. These were evolved to the present solar age, where comparisons with the helioseismic observations could be made. Our computations also yielded the time evolution of the solar flux at the planets - a key input to the climates of early Earth and Mars. Early solar mass loss is not the only influence that can alter the internal structure of the present Sun. There are minor uncertainties in the physics of the solar models and in the key observed solar parameters that also affect the present Sun's internal structure. It was therefore imperative to obtain an understanding of the effects of these other uncertainties, in order to disentangle them from the fingerprints that might be left by early solar mass loss. From these considerations, our work was divided into two parts: (1) We first computed the evolution of standard solar models with input parameters varied within their uncertainties, to determine their effect on the observable helioseismic quantities; (2) We then computed non-standard solar models with higher initial masses to test against the helioseismological observations.

Sackmann, I.-Juliana↗