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All sourcesNASA NTRSDOE OSTI
NASA NTRS2014

Mineralogy of Fluvio-Lacustrine Sediments Investigated by Curiosity During the Prime Mission: Implications for Diagenesis

The Mars Science Laboratory rover Curiosity investigated sedimentary rocks that were deposited in a diversity of fluvio-lacustrine settings. The entire science payload was employed to characterize the mineralogy and chemistry of the Sheepbed mudstone at Yellowknife Bay and the Windjana sandstone at the Kimberley. Data from the CheMin instrument, a transmission Xray diffractometer, were used to determine the quantitative mineralogy of both samples. The Sheepbed mudstone contains detrital basaltic minerals, calcium sulfates, iron oxides or hydroxides, iron sulfides, trioctahedral smectite, and amorphous material. The mineral assemblage and chemical data from APXS suggest that the trioctahedral smectite and magnetite formed authigenically as a result of alteration of olivine. The apparent lack of higher-grade phyllosilicates (e.g., illite and chlorite) and the presence of anhydrite indicate diagenesis at ~50- 80 ºC. The mineralogy of the Windjana sandstone is different than the Sheepbed mudstone. Windjana contains significant abundances of K-feldspar, low- and high-Ca pyroxenes, magnetite, phyllosilicates, and amorphous material. At least two distinct phyllosilicate phases exist: a 10 Å phase and a component that is expanded with a peak at ~11.8 Å. The identity of the expanded phase is currently unknown, but could be a smectite with interlayer H2O, and the 10 Å phase could be illite or collapsed smectite. Further work is necessary to characterize the phyllosilicates, but the presence of illite could suggest that Windjana experienced burial diagenesis. Candidates for the cementing agents include fine-grained phyllosilicates, Fe-oxides, and/or amorphous material. Interpretations of CheMin data from the Windjana sandstone are ongoing at the time of writing, but we will present an estimate of the composition of the amorphous material from mass balance calculations using the APXS bulk chemistry and quantitative mineralogy from CheMin.

Rampe, Elizabeth B.↗
NASA NTRS2015

Transmission X-ray Diffraction (XRD) Patterns Relevant to the MSL Chemin Amorphous Component: Sulfates And Silicates

The Mars Science Laboratory (MSL) CheMin instrument on the Curiosity rover is a transmission X-ray diffractometer (Co-Kalpha radiation source and a approx.5deg to approx.52deg 2theta range) where the analyzed powder samples are constrained to have discrete particle diameters <150 microns by a sieve. To date, diffraction patterns have been obtained for one basaltic soil (Rocknest (RN)) and four drill fines of coherent rock (John Klein (JK), Cumberland (CB), Windjana (WJ), and Confidence Hills (CH)). The CheMin instrument has detected and quantified the abundance of both primary igneous (e.g., feldspar, olivine, and pyroxene) and secondary (e.g., Ca-sulfates, hematite, akaganeite, and Fe-saponite) minerals. The diffraction patterns of all CheMin samples are also characterized by a broad diffraction band centered near 30deg 2theta and by increasing diffraction intensity (scattering continuum) from approx.15deg to approx.5deg, the 2theta minimum. Both the broad band and the scattering continuum are attributed to the presence of an XRD amorphous component. Estimates of amorphous component abundance, based on the XRD data itself and on mass-balance calculations using APXS data crystalline component chemistry derived from XRD data, martian meteorites, and/or stoichiometry [e.g., 6-9], range from approx.20 wt.% to approx.50 wt.% of bulk sample. The APXSbased calculations show that the amorphous component is rich in volatile elements (esp. SO3) and is not simply primary basaltic glass, which was used as a surrogate to model the broad band in the RN CheMin pattern. For RN, the entire volatile inventory (except minor anhydrite) is assigned to the amorphous component because no volatile-bearing crystalline phases were reported within detection limits [2]. For JK and CB, Fesaponite, basanite, and akaganeite are volatile-bearing crystalline components. Here we report transmission XRD patterns for sulfate and silicate phases relevant to interpretation of MSL-CheMin XRD amorphous components.

Morris, R. V.↗
NASA NTRS2015

Diagenetic Mineralogy at Gale Crater, Mars

Three years into exploration of sediments in Gale crater on Mars, the Mars Science Laboratory rover Curiosity has provided data on several modes and episodes of diagenetic mineral formation. Curiosity determines mineralogy principally by X-ray diffraction (XRD), but with supporting data from thermal-release profiles of volatiles, bulk chemistry, passive spectroscopy, and laser-induced breakdown spectra of targeted spots. Mudstones at Yellowknife Bay, within the landing ellipse, contain approximately 20% phyllosilicate that we interpret as authigenic smectite formed by basalt weathering in relatively dilute water, with associated formation of authigenic magnetite as in experiments by Tosca and Hurowitz [Goldschmidt 2014]. Varied interlayer spacing of the smectite, collapsed at approximately 10 A or expanded at approximately 13.2 A, is evidence of localized diagenesis that may include partial intercalation of metal-hydroxyl groups in the approximately 13.2 A material. Subsequent sampling of stratigraphically higher Windjana sandstone revealed sediment with multiple sources, possible concentration of detrital magnetite, and minimal abundance of diagenetic minerals. Most recent sampling has been of lower strata at Mount Sharp, where diagenesis is widespread and varied. Here XRD shows that hematite first becomes abundant and products of diagenesis include jarosite and cristobalite. In addition, bulk chemistry identifies Mg-sulfate concretions that may be amorphous or crystalline. Throughout Curiosity's traverse, later diagenetic fractures (and rarer nodules) of mm to dm scale are common and surprisingly constant and simple in Ca-sulfate composition. Other sulfates (Mg,Fe) appear to be absent in this later diagenetic cycle, and circumneutral solutions are indicated. Equally surprising is the rarity of gypsum and common occurrence of bassanite and anhydrite. Bassanite, rare on Earth, plays a major role at this location on Mars. Dehydration of gypsum to bassanite in the dry atmosphere of Mars has been proposed but considered unlikely based on lab studies of dehydration kinetics in powdered samples. Dehydration is even less likely for bulk vein samples, as lab data show dehydration rates one to two orders of magnitude slower in bulk samples than in powders. On Mars, exposure ages of 100 Ma or more may be a significant factor in dehydration of hydrous phases.

Vaniman, David↗
NASA NTRS2016

Synthesis of Akaganeite in the Presence of Sulfate: Implications for Akaganeite Formation in Yellowknife Bay, Gale Crater, Mars

Akaganeite (beta-FeOOH) is an Fe(III) (hydr)oxide with a tunnel structure usually occupied by chloride. Akaganeite has been recently discovered in a mudstone on the surface of Mars by the Chemistry and Mineralogy (CheMin) and Sample Analysis at Mars (SAM) instruments onboard the Mars Science Laboratory (MSL) Curiosity Rover in Gale crater [1, 2]. Akaganeite was detected together with sulfate minerals [anhydrite (CaSO4) and basanite (2CaSO4·2H2O)] in the drilled Cumberland and John Clein mudstone samples at Yellowknife Bay [2]. Discovery of akaganeite and sulfates in the same samples suggests that sulfate ions could be present in aqueous solution during akaganeite formation. However, mechanism and aqueous environmental conditions of akaganeite formation (e.g., pH and range of sulfate concentration) in Yellowknife Bay remain unknown. The objective of our work was to perform synthesis of akaganeite without or with sulfate addition at variable pHs in order to constrain formation conditions of akaganeite in Yellowknife Bay, Gale crater on Mars.

Peretyazhko, T. S.↗
NASA NTRS2016

Diagenesis Along Fractures in an Eolian Sandstone, Gale Crater, Mars

The Mars Science Laboratory rover Curiosity has been exploring sedimentary deposits in Gale crater since August 2012. The rover has traversed up section through approx.100 m of sedimentary rocks deposited in fluvial, deltaic, lacustrine, and eolian environments (Bradbury group and overlying Mount Sharp group). The Stimson formation lies unconformable over a lacustrine mudstone at the base of the Mount Sharp group and has been interpreted to be a cross-bedded sandstone of lithified eolian dunes. Mineralogy of the unaltered Stimson sandstone consists of plagioclase feldspar, pyroxenes, and magnetite with minor abundances of hematite, and Ca-sulfates (anhydrite, bassanite). Unaltered sandstone has a composition similar to the average Mars crustal composition. Alteration "halos" occur adjacent to fractures in the Stimson. Fluids passing through these fractures have altered the chemistry and mineralogy of the sandstone. Silicon and S enrichments and depletions in Al, Fe, Mg, Na, K, Ni and Mn suggest aqueous alteration in an open hydrologic system. Mineralogy of the altered Stimson is dominated by Ca-sulfates, Si-rich X-ray amorphous materials along with plagioclase feldspar, magnetite, and pyroxenes, but less abundant in the altered compared to the unaltered Stimson sandstone and lower pyroxene/plagioclase feldspar. The mineralogy and geochemistry of the altered sandstone suggest a complicated history with several (many?) episodes of aqueous alteration under a variety of environmental conditions (e.g., acidic, alkaline).

Ming, D. W.↗
NASA NTRS2016

Similarities Across Mars: Acidic Fluids at Both Meridiani Planum and Gale Crater in the Formation of Magnesium-Nickel Sulfates

In-situ identification of sulfates at the martian surface by the Mars Exploration Rovers and the Mars Science Laboratory have included calcium sulfates with various states of hydration (gypsum, bassanite, anhydrite), iron sulfates of likely fumarolic origin, massive deposits of iron hydroxysulfates indicative of an acidic history, and minor occurrences of magnesium sulfates. Recent measurements by the Opportunity and Curiosity Alpha Particle X-ray Spectrometers (APXS) have indicated the presence of Ni-substituted Mg-sulfates at the Meridiani Planum and Gale Crater landing sites. The Opportunity rover has traversed nearly 43 km and is currently exploring the impact breccias of the rim of Endeavour crater, near a location where signatures of aqueous alteration have been established from orbit. APXS analyses of subsurface materials excavated by a rover wheel show clear evidence for a Mg(Ni)-sulfate with Mg:Ni (is) approximately 100:1 (molar). On the other side of the planet, Curiosity is continuing its climb up Mount Sharp after driving (is) approximately 13 km since landing. Over the last 4 km of the traverse, there have been multiple chemical analyses of erosionally-resistant nodules and dendritic features in a finely laminated mudstone unit which also indicate Mg(Ni)-sulfate (Mg:Ni (is) approximately 30:1, molar). The geologic settings for the Endeavour rim and the Mount Sharp mudstones are clearly different, but similar formation conditions for these sulfates may be possible. Ni(2+) readily substitutes for Mg(2+) in a variety of geochemical processes due to their comparable ionic radii. The availability of soluble Ni at the time of Mg-sulfate precipitation suggests acidic solutions. The fluids responsible for alteration in the Endeavour rim and for the formation of nodules in Gale mudstones may have had similar chemical characteristics at the time the Mg-sulfates were formed.

Yen, Albert S.↗
NASA NTRS2016

Is Tridymite at Gale Crater Evidence for Silicic Volcanism on Mars?

The X-ray diffraction (XRD) instrument (CheMin) onboard the MSL rover Curiosity detected 17 wt% of the SiO2 polymorph tridymite (relative to bulk sample) for the Buckskin drill sample (73 wt% SiO2) obtained from sedimentary rock in the Murray formation at Gale Crater, Mars. Other detected crystalline materials are plagioclase, sanidine, cristobalite, cation-deficient magnetite, and anhydrite. XRD amorphous material constitutes approx. 60 wt% of bulk sample, and the position of its broad diffraction peak near approx. 26 deg. 2-theta is consistent with opal-A. Tridymite is a lowpressure, high-temperature mineral (approx. 870 to 1670 deg. C) whose XRD-identified occurrence on the Earth is usually associated with silicic (e.g., rhyolitic) volcanism. High SiO2 deposits have been detected at Gale crater by remote sensing from martian orbit and interpreted as opal-A on the basis H2O and Si-OH spectral features. Proposed opal-A formation pathways include precipitation of silica from lake waters and high-SiO2 residues of acid-sulfate leaching. Tridymite is nominally anhydrous and would not exhibit these spectral features. We have chemically and spectrally analyzed rhyolitic samples from New Mexico and Iwodake volcano (Japan). The glassy (by XRD) NM samples have H2O spectral features similar to opal-A. The Iwodake sample, which has been subjected to high-temperature acid sulfate leaching, also has H2O spectral features similar to opal-A. The Iwodake sample has approx. 98 wt% SiO2 and 1% wt% TiO2 (by XRF), tridymite (>80 wt.% of crystalline material without detectable quartz by XRD), and H2O and Si-OH spectral features. These results open the working hypothesis that the opal-A-like high-SiO2 deposits at Gale crater detected from martian orbit are products of alteration associated with silicic volcanism. The presence or absence of tridymite will depend on lava crystallization temperatures (NM) and post crystallization alteration temperatures (Iwodake).

Morris, Richard V.↗
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 NTRS2018

Using Mineralogy of the Bagnold Dune Field in Gale Crater to Interpret Eolian Sediment Sorting on the Martian Surface

The Mars Science Laboratory Curiosity rover landed in Gale crater in August 2012 to characterize modern and ancient surface environments. Curiosity executed a two-phase campaign to study the morphology, activity, physical properties, and chemical and mineralogical composition of the Bagnold Dune Field, an active eolian dune field on the lower slopes of Aeolis Mons (Mount Sharp). Detectable aspects of dune sand mineralogy have been examined from orbit with the visible/short-wave infrared spectrometer CRISMand the thermal-infrared spectrometers THEMIS and TES. CRISM data demonstrate variations in plagioclase, pyroxene, and olivine abundances across the dune field. Curiosity analyzed sediments from two locations in the dune field to evaluate the causes of the mineralogical differences observed from orbit. The Gobabeb sample was collected from Namib Dune, a barchanoidal dune on the upwind margin of the dune field, and the Ogunquit Beach sample was collected from the Mount Desert Island sand patch located downwind from Namib. These samples were sieved to <150 μm and delivered to the CheMin X-ray diffraction instrument for quantitative mineralogical analysis. CRISM-derived mineralogy of the Namib Dune and Mount Desert Island and CheMin-derived mineralogy of the Gobabeb and Ogunquit Beach samples can be used in a value-added manner to interpret grain segregation at the bedform to dune-field scale and evaluate contributions from local sediment sources. Models of CRISM data demonstrate that Mount Desert Island is more enriched in olivine and less enriched in plagioclase than Namib dune, suggesting that fine-grained mafic sediments are preferentially mobilized downwind. Curiosity data indicate olivine also forms a coarse lag on the lee sides of barchanoidal dunes. Minor abundances of hematite, quartz, and anhydrite and small differences in the crystal chemistry of plagioclase and pyroxene derived from CheMin data suggest that sediments from the underlying lacustrine rocks also contribute to the Bagnold sands.

Rampe, E. B.↗
NASA NTRSDate not supplied

Mineralogy of the Greenheugh Pediment and Underlying Murray Formation from the Mars Science Laboratory CheMin Instrument

The Mars Science Laboratory Curiosity rover has been investigating a sequence of ancient fluvio-lacustrine and eolian units in Gale crater. For much of the mission, Curiosity has studied the fluvio-lacustrine deposits of the Murray formation. Curiosity has also studied the ancient eolian Stimson formation in a few locations, which unconformably overlies the Murray fm. The Stimson formation was previously studied at the Naukluft and Emerson Plateaus and recently studied at the Greenheugh pediment capping unit. The Curiosity science team also investigated the Murray formation directly underlying the pediment. Curiosity drilled the “Edinburgh” target within the pediment capping unit and the “Hutton” target in the Murray formation near the contact with the pediment and delivered these materials to the CheMin X-ray diffractometer to characterize bulk mineralogy. Edinburgh contains abundant plagioclase, pyroxene, magnetite, olivine, and X-ray amorphous materials, with 10 wt.% smectite and minor sanidine. The mineralogy of the Stimson at Greenheugh is distinct from the mineralogy of the Stimson at Naukluft and Emerson because previous Stimson targets did not contain olivine or clay minerals. This suggests sediments in the pediment may have a different source and/or different aqueous alteration history than those from Naukluft and Emerson. Hutton contains abundant plagioclase, pyroxene, magnetite, and X-ray amorphous materials, 6 wt.% smectite, and minor cristobalite, opal-CT, sanidine, hematite, fluorapatite, and anhydrite. Other Murray targets in the surrounding Glen Torridon region that are farther from the pediment contact contain ~30 wt.% smectite and lack cristobalite and opal-CT. Cristobalite and/or opal-CT are present in a few other targets elsewhere along the traverse, including the top of the nearby Vera Rubin ridge and the top of the Pahrump Hills outcrop. Stimson overlies the Pahrump Hills, and, based on projections of the pediment slope, the Stimson may have overlain Vera Rubin ridge. The proximity of the low-smectite and cristobalite- and/or opal-CT-bearing outcrops to the contact between the Murray and Stimson suggests the contact provided a conduit for diagenetic fluids that altered clay minerals and formed crystalline and paracrystalline silica.

E. B. Rampe↗
NASA NTRS2021

Near-infrared Reflectance of Rocks at high Temperature: Preliminary Results and Implications for Near-infrared Emissivity of Venus's Surface

Light emitted from Venus’s surface can be viewed through spectral “windows” in its atmosphere, in the nearinfrared (NIR) around 1000 nanometer (nm) wavelengths. The NIR emissivity of Venus’s surface can constrain rock types and their weathering state; emissivities can be measured directly or calculated from reflectances. We measured the reflectances of igneous and sedimentary rocks at Venus’s surface temperature, 400 °C–500 °C at 850 and 950 nm; samples were heated in a box furnace in air, illuminated by light-emitting diodes (LEDs), and imaged with a modified charge-coupled device (CCD) camera. Reflectances were also measured at 25 °C from 350 to 1400 nm. Rock reflectances at 850 and 950 nm and 400 °C–500 °C are nearly identical to those at 25 °C, except for the effects of nanophase hematite forming on some surfaces. Fresh basalts have reflectances (high and low temperatures) near 7.5%; a leucogranite similarly has reflectances near 50%. Pigmentary hematite has nearly identical reflectances at high- and low-temperature at these wavelengths. Pigmentary hematite appears dark brown 400 °C–500 °C because its absorption edge has shifted to beyond the limit of human vision. These rock reflectances imply that basalts should have emissivities near 0.9, and granite (and similar felsic rocks) should have lower emissivities ∼0.5. Thus, basalt and felsic rock should be easily distinguished in NIR emissivity measurements of Venus’s surface, such as are baselined in recent Venus mission proposals. Other sedimentary rocks should have even lower emissivities: quartz sand at around ∼0.3, and anhydrite as low as 0.1.

Allan H Treiman↗
NASA NTRS2021

Evidence for the Protection of N-heterocycles from Gamma Radiation by Mars Analogue Minerals

Organic compounds have been delivered to the surface of Mars via meteorites, comets and interplanetary dust particles for billions of years. Determining the effects of high energy radiation and galactic cosmic radiation (GCR) on these organic compounds is critical for understanding the potential for the preservation of organic molecules associated with past or present life, and where to look for possible chemical bio- signatures during future Mars missions. Understanding how these effects are attenuated by the mineral matrix and the depth at which they are buried have been challenging to determine in situ on Mars. There have been very few experimental studies on the survival of organic compounds under radiation from a gamma source under realistic conditions, and their interpretation until now has been difficult due to the lack of data for actual radiation levels on Mars. Using the in-situ data obtained by the MSL/RAD instrument to anchor the dose calculations, here we show that the N-heterocycles purine and uracil, crucial components of biochemical processes in extant living systems, mixed with calcite, anhydrite, and kaolinite as Mars analogue minerals can survive the effects of radiation with a dose corresponding to ~500,000 years on the Martian surface. The extent of survival varied not only with the nature of the organic compound, but its depth from the surface. These results provide new experimental data for the degree of protection offered by the regolith, in conjunction with minerals, for organic compounds that may be present on Mars.

mars↗
NASA NTRSDate not supplied

The Chemistry and Mineralogy of Mars Soils: A Tour of Landed Mission Results from the Last 45 years

Eight landed missions demonstrated that martian soils (defined as loose, unconsolidated surface material) consist of basaltic mineralogy, iron (hydr)oxides, amorphous material, sulfate, chloride, (per)chlorate, nitrate, carbonate, and possible organic C. The Viking Lander 1 and 2 (1976), Mars Pathfinder (1997), and Mars Exploration Rover (MER-A,B) (2004) missions determined that martian soil was similar at all landing sites by having mafic chemistry, high S (~ 7 wt.% SO3) and Cl (0.7 wt.%), and spectral detections of poorly crystalline and crystalline Fe-(hydr)oxide phases. The MER Mössbauer spectrometers detected Fe-bearing olivine and pyroxene along with magnetite, nano-phase Fe-oxides (npOx), hematite, and ferric sulfate. The 2008 Phoenix Lander instrumentation measured a soil pH of 7.7 and detected ~0.6 wt.% perchlorate, 3-5 wt.% Ca-rich carbonate and carbon (500 gC/g) consistent with oxidized organics and Fe-rich carbonate. The 2012 Mars Science Laboratory (MSL) rover (Gale Crater) through X-ray diffraction detected plagioclase feldspar, pyroxene, magnetite, hematite, anhydrite, and quartz, with the balance being composed of Si/Fe-containing amorphous (30 to 40 wt.%) material. MSL evolved gas analysis detected (per)chlorate (0.4 wt.% ClO4), nitrate (0.23 wt.%), along with minor Fe/Mg sulfate and oxidized organic C (~2000 gC/g). Limited pedogenesis may have occurred at the 2018 InSight landing site and in one Gusev Crater soil (MER-B) which have 3 to 10 cm-thick duricrust horizons consistent with atmospheric water vapor interactions with soil salts. Martian soil primary mineralogy was derived mostly from local rock (volcanic, sedimentary) that is largely basaltic planet wide. Secondary minerals [e.g., sulfate, chloride, perchlorate, nitrate, carbonate, Fe-(hydr)oxides] in martian soils formed from oxidative aqueous alteration processes and were likely derived from a combination of local sedimentary rock sources and the global bright dust. The Mars 2020 mission will collect soil for Earth return to enable a thorough assessment of the nature and origin of martian soil.

Mars↗
NASA NTRS2024

Basalt Alteration in a CO 2 -SO 2 Atmosphere: Implications for Surface Processes on Venus

Venus’ surface and interior dynamics remain largely unconstrained, due in great part to the major obstacles to exploration imposed by its 470°C, 90 bar surface conditions and its thick, opaque atmosphere. Orbiter-based thermal emission data provide opportunities to characterize the surface composition of Venus. However, interpretations of such spectra depend on understanding interactions between the planet’s surface basaltic rocks and its caustic, sulfur dioxide (SO 2 )-bearing carbon dioxide (CO 2 ) atmosphere. Several studies, using remote sensing, thermodynamic modeling, and laboratory experiments, have placed constraints on basaltic alteration mineralogies and rates. Yet constraint with respect to SO 2 -mediated reactions with basalts of contrasting compositions remains incomplete. Here, we present new data from a series of gas-solid reaction experiments, in which samples of two basalt compositions were reacted in an SO 2 -bearing CO 2 atmosphere, at relevant Venus temperatures, pressure, and oxygen fugacity. We subjected reacted specimens to scanning electron microscopy (SEM) and scanning transmission electron microscopy (STEM) analyses using sample cross-sections produced with focused ion beam (FIB) milling. Surface alteration products were characterized, and their abundances estimated; subsurface cation concentrations were mapped to show depth of alteration. We demonstrate that the initial rate of reaction in our experiments is very rapid. Alkaline basalt samples are coated by (meta)thenardite (Na 2 SO 4 ) and amorphous calcium carbonate (CaCO 3 ) alteration products, and tholeiitic basalt samples are primarily covered by anhydrite (CaSO 4 ), Fe-oxide (Fe x O y : likely magnetite, Fe 3 O 4 ), and other minor phases.

Venus↗
DOE OSTI2020

Big Sky Regional Carbon Sequestration Partnership (Phase III Final Scientific/Technical Report)

The Big Sky Carbon Sequestration Partnership (BSCSP) pursued a Phase III demonstration project at Kevin Dome in north central Montana. Kevin Dome covers approximately 700 square miles and is a naturally occurring CO 2 reservoir that is flanked by oil and gas fields. The carbon dioxide (CO 2 ) is in the upper Devonian Duperow (carbonate) formation and does not reach the spill point of the dome; therefore, the dome has potential as a CO 2 sequestration reservoir, a CO 2 supply, or as both if anthropogenic sources and enhanced oil recovery (EOR) operations are associated with the dome. Kevin Dome could potentially act as a buffer to continue accepting anthropogenic CO 2 when EOR flooding operations are interrupted or completed. The project objective was to produce one million tonnes of CO 2 from the gas cap of Kevin Dome, pipe it laterally, inject, and re-store it in the brine leg of the same formation to test the hub / buffer storage concept. This was to be accomplished by drilling up to five production wells, building a short pipeline and compression facilities, and drilling an injection well and several monitoring wells. BSCSP commenced outreach and site characterization activities including acquiring baseline data for near-surface insurance monitoring, acquiring 3-dimensional, 9-component surface seismic over the project area, drilling two test wells (one in the production area and one in the injection area), coring key intervals, and performing comprehensive logging. Well tests of those wells revealed two barriers to the project. The production (Danielson 33-17) well was perforated in multiple zones but failed to produce any significant CO 2 . This was despite being drilled in the near vicinity of a historic well that had produced 3700 MCF per day in a drill stem test. Modeling indicated that this was likely due to a phase change during production causing a temperature drop resulting in hydrate and/or water ice formation that clogged the formation. Tests of the injection zone (Wallewein 22-1) well indicated total dissolved solids (TDS) slightly below the EPA required 10,000 parts per million (ppm) for a Class VI underground injection control permit. While the project was initiated before Class VI rules were promulgated, and this was an experimental project (seemingly qualified for a Class V permit), the Environmental Protection Agency (EPA) indicated that injection would require a Class VI permit. The low salinity result was unexpected as contours plotted based on regional formation water quality data indicated an expected TDS above 20,000 ppm, and wells between the recharge zone and the Wallewein well tested above 10,000 ppm. Faced with the inability to obtain an injection permit, the demonstration project could not proceed. However, the project had generated valuable samples and data on a large natural analog including 32 sq. mi. of 3-D, 9-C seismic, 430 ft. of carbonate core covering seven different depositional environments taken from areas with, and without the presence of CO 2 , 30 ft. of core of two caprocks, a tight carbonate and an anhydrite, a full set of modern logs on both wells, and well tests. DOE decided to re-scope the project around completing studies utilizing this data. This report covers both the initial scope and the re-scope (Task / Section numbers preceded with an R). While the report covers a wide range of project activities, highlights of this work include: Development of a geostatic model using neural nets to match well logs to facies and using multi-waveform seismic to inform reservoir heterogeneity; Unique mechanical testing of permeability – stress relationship in two caprock materials; Development of full waveform inversion to generate a high resolution velocity model; Model development for dual permeability (fracture and matrix) systems to better account for matrix-matrix interactions; Joint seismic wave inversion (including the first quadr-joint inversion) exhibiting better imaging of a challenging reservoir zone in stiff rock; Core flow and core flood results on a reactive carbonate; and Innovative laboratory measurements of seismic response of fractured core as a function of fluid fill.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

Raman Microscopy Analysis of Wyoming CarbonSAFE Pilot Well Thin Sections for Mineralogy and Organic Matter Characterization

Scanning confocal Raman microspectroscopy (RMS) was used to analyze thin sections for inorganic mineral content and for evaluation of organic material (OM). Thin sections were selected from a stratigraphic test well core in the Powder River Basin, Wyoming under the Wyoming CarbonSAFE project. The well was analyzed with a variety of rock and fluid characterization techniques to determine the feasibility of a commercial-scale CO2 storage site. RMS complements other analyses, including traditional petrography, SEM, porosity and permeability, and XRD For this aspect of the study, RMS is especially important in the evaluation of OM in sealing lithologies. At prospective geologic CO2 storage sites, it is imperative to assess the unconventional oil and gas potential of seals to ensure that any future development would not compromise the integrity of the seals. Whole-slide mineralogical surveys were performed on thin sections from various shale and sandstone formations. Surveys were analyzed with Direct Classical Least Squares to identify and quantify minerals. The location and concentration of minerals was color-coded and overlaid on optical images for visualization of the distribution of minerals. Dense hyperspectral Raman mapping of OM was performed on five thin sections. Eleven spectral parameters diagnostic of organic type and thermal maturity were used to train a Partial Least Squares (PLS) calibration against a set of artificially matured samples spanning the pre- to mid-oil window. The PLS was applied to the study set and a post-mature set. Additionally, the PLS was applied to each point in hyperspectral maps for visualization of trends in maturity across sample sets and discrimination of organic matter types within a given map. In inorganic surveys on thin sections, a total of 14 unique inorganic minerals were identified in Raman spectra including quartz, dolomite, calcite, hematite and anhydrite. Shale thin sections tended to be dominated by organic material. OM was often observed mixed with inorganic minerals. Sand- and mudstones were dominated by inorganic minerals. The PLS extrapolated the post-mature set to reflectances >1.2%. The study set ranged from very immature to postmature in the median of map fit-peak parameters. However, point maturity maps indicate that matrix OM in all study samples is immature and that discreet organic particles selected for mapping, which may be inertinites, bias medians towards more-mature. The work demonstrates the capabilities of RMS to perform both whole-slide mineralogy and OM analysis with applications to formation evaluation in oil & gas, carbon sequestration and mining. Here, analysis of sealing formations in the well indicates high levels of immature organic matter that would not be a viable target for future oil production that could compromise the CO2 storage site. The work brings together diverse disciplines from geology and petrography to analytical chemistry, big data and microscopy.

Myers, Grant↗
DOE OSTI2021

Prehydration of calcium sulfoaluminate (CSA) clinker at different relative humidities

The use of CSA cement in practice has been hindered by its unstable performance and short shelf-life caused by the prehydration of CSA clinker. In this study, the effect of ambient humidity on the prehydration rate and process of CSA clinker was investigated. The prehydration degree, ageing progress, and the dynamic change of mineral composition of CSA clinker exposed to five different relative humidities (ranging from 23% to 98%) for up to 180 days were studied. Experiments revealed that the ambient humidity of 60% RH can be considered a threshold value for storage of CSA clinker. Exposure of CSA clinker to RH higher than 60% will not only result in a significant decrease of hydraulic reactivity, but also in agglomeration of the clinker. Although the exposure of CSA clinker to RH lower than 60% has little effect on the hydraulic reactivity, the main hydration peak was found to be slightly delayed with the increase of RH.

36 MATERIALS SCIENCE↗