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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 NTRS2012

Investigations Using Laboratory Testbeds to Interpret Flight Instrument Datasets from Mars Robotic Missions

The Astromaterials Research and Exploration Science Directorate at the NASA Johnson Space Center (JSC) has laboratory instrumentation that mimic the capabilities of corresponding flight instruments to enable interpretation of datasets returned from Mars robotic missions. The lab instruments have been and continue to be applied to datasets for the Moessbauer Spectrometer (MB) on the Mars Exploration Rovers (MER), the Thermal & Evolved Gas Analyzer (TEGA) on the Mars Phoenix Scout, the CRISM instrument on the Mars Reconnaissance Orbiter Missions and will be applied to datasets for the Sample Analysis at Mars (SAM), Chemistry and Mineralogy (CheMin) and Chemistry & Camera (ChemCam) instruments onboard the Mars Science Laboratory (MSL). The laboratory instruments can analyze analog samples at costs that are substantially lower than engineering models of flight instruments, but their success to enable interpretation of flight data depends on how closely their capabilities mimic those of the flight instrument. The JSC lab MB instruments are equivalent to the MER instruments except without flight qualified components and no reference channel Co-57 source. Data from analog samples were critical for identification of Mg-Fe carbonate at Gusev crater. Fiber-optic VNIR spectrometers are used to obtain CRISM-like spectral data over the range 350-2500 nm, and data for Fephyllosilicates show irreversible behavior in the electronic transition region upon dessication. The MB and VNIR instruments can be operated within chambers where, for example, the absolute H2O concentration can be measured and controlled. Phoenix's TEGA consisted of a calorimeter coupled to a mass spectrometer (MS). The JSC laboratory testbed instrument consisted of a differential scanning calorimeter (DSC) coupled to a MS configured to operate under total pressure (12 mbar), heating rate (20 C/min), and purge gas composition (N2) analogous to the flight TEGA. TEGA detected CO2 release at both low (400-680 C) and high (725-820 C) temperature and an endothermic reaction in concert with the high temperature release. The high-temperature thermal decomposition is consistent with calcite, dolomite, or ankerite, (3-6 wt.%) or any combination of these phase based upon laboratory testbed experiments. Recent laboratory experiments suggest that the low temperature CO2 release was caused by a reaction between calcium carbonate and hydrated magnesium perchlorate; although, CO2 release by the oxidation of organic materials and Fe-/Mg-rich carbonates cannot be ruled out. MSL landed in Gale crater on August 5, 2012. Although numerous analog samples have been analyzed on the JSC laboratory testbeds, no SAM, CheMin, or ChemCam analyses have been acquired by MSL to date. The JSC SAM laboratory testbed consists of a thermal analyzer coupled with a MS configured to operate under total pressure (30 mbar), heating rate (35 C/min), and purge gas composition (He) analogous to the flight SAM. The CheMin and ChemCam laboratory testbeds were developed and built by inXitu, Inc. and Los Alamos National Laboratory, respectively, to acquire datasets relevant to the MSL CheMin and ChemCam flight instruments.

Ming, D. W.↗

DOE OSTI2024

Geochemical-hydromechanical couplings during water-serpentinized harzburgite interactions at 20° C and 30 bars

Interaction of groundwater with the serpentinized harzburgites of the upper mantle plays an important role in the geologic carbon cycle and serpentinization processes. Here, in this study, an intact serpentinized harzburgite with more than 60% lizardite from the Semail ophiolite in Oman was reacted with water at near neutral pH and low PCO 2 to observe its dissolution behavior and reaction path within the CaO-MgO-SiO 2 -CO 2 -H 2 O system at 20 °C and 30 bars. In the experiment, mass (i.e. H 2 O, ions) transfer is by diffusion and the selected temperature and pressure conditions mimic water-rock interactions at the shallow portions of most ultramafic rock hosted aquifers. Equilibrium activity-activity diagrams and thermodynamic data were used to compare the experimentally determined reaction path with the theoretical stability boundaries for minerals involved to investigate the evolution of bulk chemical composition, mineralogy, and water composition. The experiments demonstrated that (i) the water-rock interactions increased the pH of the aqueous phase from 5.9 to 7.5 over a period of 18 weeks; (ii) the dissolution of lizardite, orthopyroxene (enstatite), and clinopyroxene (diopside and augite) increased the concentration of Mg, Ca, and Si in the aqueous phase; (iii) the dissolution was incongruent with respect to Mg and Si, favoring Si release at pH > 6 due to (a) breaking of more reactive cation‑oxygen bonds that is consistent with the stoichiometry of magnesium for proton exchange reaction which favors a surface that is enriched in Mg at basic conditions, and (b) preferential dissolution of clinopyroxene Mg 1.30 Ca 0.52 Fe 0.06 Si 2 O 6 ; (iv) the aqueous phase was undersaturated with respect to carbonate (e.g. calcite, magnesite, and hydromagnesite) and hydrous (e.g. lizardite, chrysotile, brucite, and talc) minerals; (v) the bulk chemical composition and mineralogy of the intact serpentinized harzburgite matrix did not change; (vi) the thermodynamic data can successfully predict water-intact serpentinized harzburgite behavior if the water chemical composition can be constrained; and (vii) no detectable macroscopic form of damage (e.g. microcracks forming as a result of differential stress fields due to changes in volume during chemical reaction) was observed.

Carbonation↗

NASA NTRS2014

Properties of Desert Sand and CMAS Glass

As-received desert sand from a Middle East country has been characterized for its phase composition and thermal stability. X-ray diffraction analysis showed the presence of quartz (SiO2), calcite (CaCO3), gypsum (CaSO4.2H2O), and NaAlSi3O8 phases in as-received desert sand and showed weight loss of approx. 35 percent due to decomposition of CaCO3 and CaSO4.2H2O when heated to 1400 C. A batch of as-received desert sand was melted into calcium magnesium aluminosilicate (CMAS) glass at approx. 1500 C. From inductively coupled plasma-atomic emission spectrometry, chemical composition of the CMAS glass was analyzed to be 27.8CaO-4MgO-5Al2O3-61.6SiO2-0.6Fe2O3-1K2O (mole percent). Various physical, thermal and mechanical properties of the glass have been evaluated. Bulk density of CMAS glass was 2.69 g/cc, Young's modulus 92 GPa, Shear modulus 36 GPa, Poisson's ratio 0.28, dilatometric glass transition temperature (T (sub g)) 706 C, softening point (T (sub d)) 764 C, Vickers microhardness 6.3 +/- 0.4 GPa, indentation fracture toughness 0.75 +/- 0.15 MPa.m (sup 1/2), and coefficient of thermal expansion (CTE) 9.8 x 10 (exp -6)/degC in the temperature range 25 to 700 C. Temperature dependence of viscosity has also been estimated from various reference points of the CMAS glass using the Vogel-Fulcher-Tamman (VFT) equation. The glass remained amorphous after heat treating at 850 C for 10 hr but crystallized into CaSiO3 and Ca-Mg-Al silicate phases at 900 C or higher temperatures. Crystallization kinetics of the CMAS glass has also been investigated by differential thermal analysis (DTA). Activation energies for the crystallization of two different phases in the glass were calculated to be 403 and 483 kJ/mol, respectively.

Desert sand↗

NASA NTRS1999

Calcium Solubility and Cation Exchange Properties in Zeoponic Soil

An important aspect of a regenerative life support system at a Lunar or Martian outpost is the ability to produce food. Essential plant nutrients, as well as a solid support substrate, can be provided by: (1) treated Lunar or Martian regolith; (2) a synthetic soil or (3) some combination of both. A synthetic soil composed of ammonium- and potassium-saturated chinoptlolite (a zeolite mineral) and apatite, can provide slow-release fertilization of plants via dissolution and ion-exchange reactions. Previous equilibrium studies (Beiersdorfer, 1997) on mixtures of synthetic hydroxyapatite and saturated-clinoptilolite indicate that the concentrations of macro-nutrients such as ammonium, phosphorous, potassium, magnesium, and calcium are a function of the ratio of chinoptilolite to apatite in the sample and to the ratio of potassium to ammonium on the exchange sites in the clinoptilolite. Potassium, ammonium, phosphorous, and magnesium are available to plants at sufficient levels. However, calcium is deficient, due to the high degree of calcium adsorption by the clinoptilolite. Based on a series of batch-equilibration experiments, this calcium deficiency can be reduced by (1) treating the clinoptilolite with CaNO3 or (2) adding a second Ca-bearing mineral (calcite, dolomite or wollastonite) to the soil. Treating the Cp with CaNO3 results in increased Ca in solution, decreased P in solution and decreased NH4 in solution. Concentrations of K were not effected by the CaNO3 treatment. Additions of Cal, Dol and Wol changed the concentrations of Ca and P in solution in a systematic fashion. Cal has the greatest effect, Dol the least and Wol is intermediate. The changes are consistent with changes expected for a common ion effect with Ca. Higher concentrations of Ca in solution with added Cal, Dol or Wol do not result in changes in K or NH4 concentrations.

Beiersdorfer, Raymond E.↗

DOE OSTI2020

Shape-preserving amorphous-to-crystalline transformation of CaCO3 revealed by in situ TEM

Organisms use inorganic ions and macromolecules to regulate crystallization from amorphous- precursors, endowing natural biominerals with complex morphologies and enhanced properties. The mechanisms by which modifiers enable these shape preserving transformations are poorly understood. We used in situ liquid-phase transmission electron microscopy to follow the evolution from amorphous calcium carbonate to calcite in the presence of additives. A combination of contrast analysis and infrared spectroscopy shows that Mg ions, which are widely present in seawater and biological fluids, alter the transformation pathway in a concentration-dependent manner. The ions bring excess (structural) water into the amorphous bulk so that a direct transformation is triggered by dehydration in the absence of morphological changes. Molecular dynamics simulations suggest Mg-incorporated water induces structural fluctuations, allowing transformation without the need to nucleate a separate crystal. Thus, the obtained calcite retains the original morphology of the amorphous state, biomimetically achieving the morphological control of crystals seen in biominerals

crystallization, biomineralization, calcium carbon↗

NASA NTRS1989

Venus volcanism: Rate estimates from laboratory studies of sulfur gas-solid reactions

Thermochemical reactions between sulfur-bearing gases in the atmosphere of Venus and calcium-, iron-, magnesium-, and sulfur-bearing minerals on the surface of Venus are an integral part of a hypothesized cycle of thermochemical and photochemical reactions responsible for the maintenance of the global sulfuric acid cloud cover on Venus. SO2 is continually removed from the Venus atmosphere by reaction with calcium bearing minerals on the planet's surface. The rate of volcanism required to balance SO2 depletion by reactions with calcium bearing minerals on the Venus surface can therefore be deduced from a knowledge of the relevant gas-solid reaction rates combined with reasonable assumptions about the sulfur content of the erupted material (gas + magma). A laboratory program was carried out to measure the rates of reaction between SO2 and possible crustal minerals on Venus. The reaction of CaCO3(calcite) + SO2 yields CaSO4 (anhydrite) + CO was studied. Brief results are given.

Ehlers, K.↗

DOE OSTI2026

Alkaline mineral residues from pulp mills as a sustainable and economical alternative to lime fertilizers

Lime is typically comprised of calcium carbonate (CaCO 3 ) or calcium magnesium carbonate (CaMg(CO 3 ) 2 ) and is needed to maintain a proper pH in agriculture and forestry soils, but it represents a major cost to growers and results in significant greenhouse gas emissions due to the mining, crushing, and transport required. There is a need to identify existing sources of alkaline mineral wastes and assess their potential as sustainable and cost-effective alternatives to lime. Dregs and grits (DGs) are highly alkaline mineral residues from biomass pulp mills that form during the recovery of pulping chemicals and are mostly comprised of CaCO 3 . For the first time, we assess the efficacy of industrially sourced DGs on 22 acidic soils across the Southeastern United States that are currently used in either agriculture or forestry operations. The application of DGs was found on average to result in the same soil pH response as calcite over multiple soil incubations (0 day to 120 days). An analysis of the carbon content of the soils after the incubation revealed that soils incubated with DGs experienced a statistically significant increase in soil carbon relative to control soils and those incubated with CaCO 3 . The generation and application of DGs emits 0.35 tonnes of CO 2 for every tonne of DGs, which compares favorably to the 0.86 tonnes of CO 2 for every tonne of agricultural lime generated and $85 per tonne lime reported in the literature. DGs prove to be a sustainable and economical substitute for agricultural lime in the acidic soils of the Southeastern United States.

54 ENVIRONMENTAL SCIENCES↗