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NASA NTRS1993

Utricular otoconia of some amphibians have calcitic morphology

This report concerns the morphological features of otoconia removed from the inner ear of four amphibian species. Results from scanning electron microscopic examination are compared based on the site of origin. These results show that utricular otoconia have a mineral structure that mimics calcite, rather than the widely accepted idea that they are mineralized by calcium carbonate of the aragonite polymorph.

NASA Program Space Physiology and Countermeasures↗

NASA NTRS2001

Potential Evaporite Biomarkers from the Dead Sea

The Dead Sea is located on the northern branch of the African-Levant Rift systems. The rift system, according to one model, was formed by a series of strike slip faults, initially forming approximately two million years ago. The Dead Sea is an evaporite basin that receives freshwater from springs and from the Jordan River. The Dead Sea is different from other evaporite basins, such as the Great Salt Lake, in that it possesses high concentrations of magnesium and has an average pH of 6.1. The dominant cation in the Great Salt Lake is sodium, and the pH is 7.7. Calcium concentrations are also higher in the Dead Sea than in the Great Salt Lake. Both basins are similar in that the dominant anion is chlorine and the salinity levels are approximately 20 %. Other common cations that have been identified from the waters of the Dead Sea and the Great Salt Lake include sodium and potassium. A variety of Archea, Bacteria, and a single genus of a green algal, Dunaliella, has been described from the Dead Sea. Earlier studies concentrated on microbial identification and analysis of their unique physiology that allows them to survive in this type of extreme environment. Potential microbial fossilization processes, microbial fossils, and the metallic ions associated with fossilization have not been studied thoroughly. The present study is restricted to identifying probable microbial morphologies and associated metallic ions. XRD (X Ray Diffraction) analysis indicates the presence of halite, quartz, and orthoclase feldspar. In addition to these minerals, other workers have reported potassium chloride, magnesium bromide, magnesium chloride, calcium chloride, and calcium sulfate. Halite, calcium sulfate, and orthoclase were examined in this report for the presence of microbes, microbially induced deposits or microbial alteration. Neither the gypsum nor the orthoclase surfaces possesses any obvious indications of microbial life or fossilization. The sand-sized orthoclase particles are weathered with 122 extensive fan-shaped mineral deposits. The gypsum deposits are associated with halite minerals and also exhibit extensive weathering. Halite minerals represent the only substrates that have probable rod-shaped microbial structures with long, filamentous, apical extensions. EDS (energy dispersive x-ray) analysis of the putative microbes indicates elevated calcium levels that are enriched with magnesium. The rod-shaped structures exhibit possible fossilization stages. Rhombohedralshaped minerals of magnesium-enriched calcium carbonate are deposited on the microbial surfaces, and eventually coat the entire microbial surface. The sodium chloride continues to crystallize on nearby halite surface and even crystallizes on the fossilized microbial remains. The putative fossils are found exclusively on halite surfaces, and all contained elevated levels of calcium magnesium cations. Both of these metallic cations are associated with microbial activity and fossilization. Their morphological diversity is low in comparison with the reported living Dead Sea microbial population. If we examine the fossil record for multicellular organisms, fossilization rates are lower for soft-bodied organisms than for those possessing hard parts, i.e. shells, bones. For example, smaller, single celled organisms would have a smaller chance of fossilization; their fossilized shapes could be mistaken for abiotic products. Another consideration is that dead organisms in the water column are probably utilized as a food source by other microbes before fossilization processes are completed. This may be an important consideration as we attempt to model and interpret ancient microbial environments either on Earth or on Mars.

Morris, Penny A.↗

DOE OSTI2024

Label-Free In Situ Chemical Characterization of Amyloid Plaques in Human Brain Tissues

The accumulation of amyloid plaques and increased brain redox burdens are neuropathological hallmarks of Alzheimer’s disease. Altered metabolism of essential biometals is another feature of Alzheimer’s, with amyloid plaques representing sites of disturbed metal homeostasis. Despite these observations, metal-targeting disease treatments have not been therapeutically effective to date. A better understanding of amyloid plaque composition and the role of the metals associated with them is critical. To establish this knowledge, the ability to resolve chemical variations at nanometer length scales relevant to biology is essential. Here, we present a methodology for the label-free, nanoscale chemical characterization of amyloid plaques within human Alzheimer’s disease tissue using synchrotron X-ray spectromicroscopy. Our approach exploits a C–H carbon absorption feature, consistent with the presence of lipids, to visualize amyloid plaques selectively against the tissue background, allowing chemical analysis to be performed without the addition of amyloid dyes that alter the native sample chemistry. Using this approach, we show that amyloid plaques contain elevated levels of calcium, carbonates, and iron compared to the surrounding brain tissue. Chemical analysis of iron within plaques revealed the presence of chemically reduced, low-oxidation-state phases, including ferromagnetic metallic iron. The zero-oxidation state of ferromagnetic iron determines its high chemical reactivity and so may contribute to the redox burden in the Alzheimer’s brain and thus drive neurodegeneration. Ferromagnetic metallic iron has no established physiological function in the brain and may represent a target for therapies designed to lower redox burdens in Alzheimer’s disease. Additionally, ferromagnetic metallic iron has magnetic properties that are distinct from the iron oxide forms predominant in tissue, which might be exploitable for the in vivo detection of amyloid pathologies using magnetically sensitive imaging. We anticipate that this label-free X-ray imaging approach will provide further insights into the chemical composition of amyloid plaques, facilitating better understanding of how plaques influence the course of Alzheimer’s disease.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1995

Atomic force microscope observations of otoconia in the newt

Calcitic and aragonitic otoconia from the Japanese red-bellied newt, Cynops pyrrhogaster, were examined using an atomic force microscope. The surface structure of both otoconial polymorphs consisted of arrays of elements approximately 50 nm in diameter. Elements were generally round and were separated by shallow depressions of no more than 20 nm. The elements are suggested to be single crystals of calcium carbonate. The relationship of these observations to theories of otoconial genesis is discussed.

NASA Discipline Developmental Biology↗

NASA NTRS1996

Regulation of statoconia mineralization in Aplysia californica in vitro

Statoconia are calcium carbonate inclusions in the lumen of the gravity-sensing organ, the statocyst, of Aplysia californica. The aim of the present study was to examine the role of carbonic anhydrase and urease in statoconia mineralization in vitro. The experiments were performed using a previously described culture system (Pedrozo et al., J. Comp. Physiol. (A) 177:415-425). Inhibition of carbonic anhydrase by acetazolamide decreased statoconia production and volume, while inhibition of urease by acetohydroxamic acid reduced total statoconia number, but had no affect on statoconia volume. Inhibition of carbonic anhydrase initially increased and then decreased the statocyst pH, whereas inhibition of urease decreased statocyst pH at all times examined; simultaneous addition of both inhibitors also decreased pH. These effects were dose and time dependent. The results show that carbonic anhydrase and urease are required for statoconia formation and homeostasis, and for regulation of statocyst pH. This suggests that these two enzymes regulate mineralization at least partially through regulation of statocyst pH.

NASA Discipline Neuroscience↗

DOE OSTI2021

Wellbore Leakage Mitigation Using Advanced Mineral Precipitation Strategies (Final Scientific/Technical Report)

This research project, entitled Wellbore Leakage Mitigation using Advanced Mineral Precipitation Strategies, was directed toward advancing mineral precipitation technologies to seal wellbore leaks and other potential carbon dioxide (CO 2 ) leakage pathways, including compromised wellbore cement and fracture networks of varying geometries throughout the wellbore and surrounding formation. The advanced mineral sealing techniques were evaluated in the laboratory and the field to expand the range of temperature, pressure, and chemical conditions where mineral precipitation could be used. Rates of enzymatically or thermally induced calcium carbonate precipitation (EICP, TICP) were determined as well as rates of enzyme inactivation at elevated temperatures (>60 °C). Immobilization was shown to enhance the thermal stability of urease enzyme and provide protection from inhibition in low pH conditions. Mineral seals promoted by EICP and TICP were used to seal fractured composite (cement/sandstone) and shale cores in high pressure reactors operated at temperatures greater than 55 °C and 130 °C, respectively. A computational model was updated to model processes of EICP and TICP. The work resulted in a successful field test, which showed that EICP in the presence of low pH fluids (CO 2 -impacted brine) could promote permeability reduction and seal a channel in the near-wellbore environment.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Polymer Composites Reinforced by Carbon-Allotrope Fillers for Selective Laser Sintering (SLS) - A Review

The limited commercial availability of applicable polymer powders has hindered the widespread implementation of SLS as a legitimate manufacturing method. This is partly due to the mechanism of SLS, which requires powders to meet rigid specifications if processing is to be successful. Furthermore, powders that do meet requirements are often incapable of producing quality, high-performance parts. Academic and industrial research has focused on composite development to overcome this problem. The incorporation of fillers including calcium carbonate, molybdenum disulfide, and aluminum have all been found to influence the processing behavior of PA12 powder and ultimately, the properties of the final part.3-5 Here, the thermal and mechanical properties of sintered composite parts produced using polymer powders reinforced by various carbon-based fillers is discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Real Time 3D Observations of Portland Cement Carbonation at CO2 Storage Conditions

Depleted oil reservoirs are considered a viable solution to the global challenge of CO 2 storage. A key concern is whether the wells can be suitably sealed with cement to hinder the escape of CO 2 . Under reservoir conditions, CO 2 is in its supercritical state, and the high pressures and temperatures involved make real-time microscopic observations of cement degradation experimentally challenging. Here, we present an in situ 3D dynamic X-ray micro computed tomography (μ-CT) study of well cement carbonation at realistic reservoir stress, pore-pressure, and temperature conditions. The high-resolution time-lapse 3D images allow monitoring the progress of reaction fronts in Portland cement, including density changes, sample deformation, and mineral precipitation and dissolution. By switching between flow and nonflow conditions of CO 2 -saturated water through cement, we were able to delineate regimes dominated by calcium carbonate precipitation and dissolution. For the first time, we demonstrate experimentally the impact of the flow history on CO 2 leakage risk for cement plugging. In-situ μ-CT experiments combined with geochemical modeling provide unique insight into the interactions between CO 2 and cement, potentially helping in assessing the risks of CO 2 storage in geological reservoirs.

58 GEOSCIENCES↗

DOE OSTI2024

Carbon sequestration into lime-stabilized soils: Engineering and mineralogical characterization

Stabilizing weak clayey soils with lime is an effective method for improving the mechanical properties of soil. However, lime production is an energy-intensive process producing significant CO 2 emissions in lime-stabilized soils, which can be counteracted through accelerated carbonation that enhances its engineering performance. The present study evaluates accelerated carbonation of lime-treated soils by adding gaseous (CO 2 -rich gas), liquid (water-CO 2 mixture), and solid (sodium bicarbonate) CO 2 sources. Results indicated that samples carbonated with gaseous CO 2 exhibited 100% lime carbonation, while samples treated with solid and aqueous sources of CO 2 had a mean lime carbonation of 60% and 40%, respectively. Further, all lime-treated-carbonated samples exhibited a mean 50% increase in unconfined compressive strength compared to the untreated samples after a 7-day curing period. Durability evaluation through cyclic wetting and drying indicated that the carbonated samples had higher durability than the untreated samples. X-ray computed tomography showed that adding solid and liquid sources of CO 2 facilitated the flocculation of montmorillonite, reducing the porosity. However, a higher dosage of solid CO 2 induced clay dispersion, increasing the porosity. X-ray diffraction and thermogravimetric analysis verified CO 2 sequestration through the formation of calcite, a thermodynamically stable polymorph of calcium carbonate.

58 GEOSCIENCES↗

DOE OSTI2020

Fractal breakage of porous carbonate sand particles: Microstructures and mechanisms

In situ, three-dimensional (3D) characterizations of particle breakage in porous carbonate sands are presented, for the first time, with synchrotron-based micro computed tomography. Evolution of grain-scale characteristics are identified and quantified via elaborate image processing and topology analyses. The sequential 3D images reveal distinctly different fracture mechanisms for carbonate sands from silica sands. The angular shape of carbonate sand particles facilitates bending fracture, and particles with a lower sphericity and a higher porosity are more prone to break. 3D crack networks extracted from fractured particles imply considerable cleavage along initial pores. The fractal dimension of crack networks increases with external loading due to crack branching via cleavage. The resultant fragment size distribution also appears fractal and the fractal feature is valid down to the breakage limit of calcium carbonate. Crack propagation along the initial pores reduces the energy barrier for particle breakage and thus fracture strength of particles

Carbonate sands↗

NASA NTRS1988

Response of marine and freshwater algae to nitric acid and elevated carbon dioxide levels simulating environmental effects of bolide impact

One of the intriguing facets of the Cretaceous-Tertiary extinction is the apparently selective pattern of mortality amongst taxa. Some groups of organisms were severely affected and some remained relatively unscathed as they went through the K/T boundary. While there is argument concerning the exact interpretation of the fossil record, one of the best documented extinctions at the Cretaceous-Tertiary boundary is that of the calcareous nannoplankton. These organisms include coccolithic algae and foraminiferans. Attempts to explain their decline at the K/T boundary center around chemistry which could affect their calcium carbonate shells while leaving their silica-shelled cousins less affected or unaffected. Two environmental consequences of an extraterrestrial body impact which were suggested are the production of large quantities of nitrogen oxides generated by the shock heating of the atmosphere and the possible rise in CO2 from the dissolution of CaCO3 shells. Both of these phenomena would acidify the upper layers of the oceans and bodies of freshwater not otherwise buffered. The effects of nitric acid, carbon dioxide, or both factors on the growth and reproduction of calcareous marine coccoliths and non-calcareous marine and freshwater species of algae were considered. These experiments demonstrate that nitric acid and carbon dioxide have significant effects on important aspects of the physiology and reproduction of modern algae representative of extinct taxa thought to have suffered significant declines at the Cretaceous-Tertiary boundary. Furthermore, calcareous species showed more marked effects than siliceous species and marine species tested were more sensitive than freshwater species.

Boston, P. J.↗

DOE OSTI2023

Gravity-driven controls on fluid and carbonate precipitation distributions in fractures

Abstract Many challenges related to carbon-dioxide ( $$\hbox {CO}_2$$ CO 2 ) sequestration in subsurface rock are linked to the injection of fluids through induced or existing fracture networks and how these fluids are altered through geochemical interactions. Here, we demonstrate that fluid mixing and carbonate mineral distributions in fractures are controlled by gravity-driven chemical dynamics. Using optical imaging and numerical simulations, we show that a density contrast between two miscible fluids causes the formation of a low-density fluid runlet that increases in areal extent as the fracture inclination decreases from 90 $$^\circ$$ ∘ (vertical fracture plane) to 30 $$^\circ$$ ∘ . The runlet is sustained over time and the stability of the runlet is controlled by the gravity-driven formation of 3D vortices that arise in a laminar flow regime. When homogeneous precipitation was induced, calcium carbonate covered the entire surface for horizontal fractures (0 $$^\circ$$ ∘ ). However, for fracture inclinations greater than 10 $$^\circ$$ ∘ , the runlet formation limited the areal extent of the precipitation to less than 15% of the fracture surface. These insights suggest that the ability to sequester $$\hbox {CO}_2$$ CO 2 through mineralization along fractures will depend on the fracture orientation relative to gravity, with horizontal fractures more likely to seal uniformly.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Project Methods to Enhance Wellbore Cement Integrity with Microbially-Induced Calcite Precipitation (MICP) (Final Scientific/Technical Report)

The goal of this project was to develop improved methods for sealing compromised wellbore cement in leaking oil and gas wells, thereby reducing the risk of unwanted upward fluid migration. Novel methods for improving wellbore integrity, such as microbially induced calcite precipitation (MICP), can reduce leakage potential, improve the safety of fossil fuel extraction, improve the public perception of hydraulic fracturing, and promote environmentally-prudent unconventional oil and gas development. Microbes, with the urease enzyme, can catalyze the chemical reaction of urea hydrolysis to induce the precipitation of calcium carbonate which can be used as a cementitious material to seal leakage pathways. In this project, methods to promote robust bio-composite cementitious materials were designed and tested in the laboratory. Scale-up of those methods were tested in meso-scale reactor systems and in field applications. In this report, in Section One, we describe laboratory efforts to develop injection strategies to promote precipitation in wellbore analogs and determine the strength of the bio-composite cements as compared to fine cement. In Section Two, we describe the efforts to scale up the work and study the use of materials that can be used in field application, for example exploring the use of calcium chloride ice melt or urea fertilizer as source chemicals. In Section Three, the three field trials (methods and results) performed as part of the project are described and summarized. At the end of the report is a comprehensive summary and conclusion section which highlights the key findings of the project. The work performed during this project significantly advanced the technology readiness level (TRL) of the MICP wellbore sealing strategy.

02 PETROLEUM↗

DOE OSTI2020

Methods to Enhance Wellbore Cement Integrity with Microbially-Induced Calcite Precipitation (MICP) (Final Scientific/ Technical Report)

03 NATURAL GAS↗

NASA NTRS1988

Rate of production, dissolution and accumulation of biogenic solids in the ocean

The equatorial current system, by its response to global circulation changes, provides a unique recording mechanism for long range climatic oscillations. A permanent record of the changes in rate of upwelling and organic production is generated in the equatorial deep sea sediments, particularly by such biogenic components which are unaffected by secondary dissolution. In order to determine the rates of accumulation of various sedimentary components, a reliable differential measurement of age of the strata must be obtained. Various approaches to this problem are reviewed, and sources of error discussed. Secondary dissolution of calcium carbonate introduces a substantial and variable difference between the dissolution-modified, and hence a priori unknown, rate of deposition on one hand and the rate of accumulation, derivable from the observed concentration, on the other. The cause and magnitude of these variations are of importance, particularly since some current dating schemes are based on assumed constancy in the rate of accumulation of this and, in some cases, also all other sedimentary components. The concepts used in rate evaluation are discussed with emphasis on the difference between the state of dissolution, an observable property of the sediment, and the rate of dissolution, a parameter that requires deduction of the carbonate fraction dissolved, and of the time differential. As a most likely cause of the enhanced state of dissolution of the interglacial carbonate sediments is proposed the lowered rates of biogenic production and deposition, which cause longer exposure of the carbonate microfossils to corrosion in the bioturbated surface layer of the sediment. Historical perspective is included in the discussion in view of the dedication of the Symposium to Hans Pettersson, the leader of the Swedish Deep Sea Expedition 1947-1948, an undertaking that opened a new era in deep sea research and planetary dynamics.

NASA Discipline Exobiology↗

NASA NTRS1998

"CHON" particles: The interstellar component of cometary dust

Interstellar dust is characterized by strong absorption in the ultraviolet and the mid-IR. Current models of interstellar dust are based on three chemically distinct components: a form of carbon (usually graphite), a silicate, and a blend of polycyclic aromatic hydrocarbons or other carbonaceous material. Previous work using effective medium theories to understand the optical properties of cometary dust suggested that an amalgam of materials could reproduce the observed interstellar and cometary dust features. Recently, Lawler and Brownlee (1992) re-analyzed the PIA and PUMA-1 data sets from the Giotto flyby of P/Halley and discovered that the so-called "CHON" particles were actually composed of a blend of carbon-bearing and silicon-bearing materials. Based on effective medium theories, the absorption spectrum of such a material would display the spectral features of each of the components - strong UV absorption from the carbonaceous component and strong absorption in the IR from the silicate component. To test this idea, vapor-deposited samples were created using two different deposition techniques: sputtering with an argon RF magnetron and deposition from an argon plasma torch. Two different compositions were tested: a blend of graphite and silica in a 7:1 ratio and an amalgam of materials whose approximate composition matches the "CHON"-silicate abundances for the uncompressed PIA data set of Lawler and Brownlee: graphite, iron oxide, magnesium oxide, ammonium sulfate, calcium carbonate, and silica in mass ratios of 6:4.3:4:2.2:1:9. The samples were finely ground and pressed into 2" diameter disks using a 40 ton press. In all, four different experiments were performed: one with each of the compositions (C:SiO and "CHON") in both the RF magnetron and the plasma torch chambers. The RF magnetron created a uniform dark thin film on the substrate surface, and the plasma torch created a coating of small (<100 micron) diameter grey particles. The spectra of all four samples show a strong, broad absorption feature at around 220 nm as well as a strong but narrower absorption peak near 10 microns. The RF magnetron sputtered samples showed some sub-structure in the UV, and the peak of the absorption was shifted toward longer wavelengths. The UV absorption in the plasma torch deposited samples have no sub-structure, and the peak absorption is very near 220 nm. Strong absorption near 9 microns is seen in the spectra from both sample preparation techniques, and is consistent with the IR spectra of some terrestrial silicates. Other features, particularly at 6.2 and 8.6 microns, are seen in the interstellar medium. A strong feature near 2 microns is due to absorbed water in the sample. Based on the results of these experiments, there is evidence that a material with a composition similar to that detected in "CHON" particles in the coma of P/Halley have a spectral signature which reproduces the main absorption features of interstellar dust. This suggests that the "CHON" particles could be the interstellar component of cometary dust.

Lien, David J.↗

NASA NTRS1974

Evaluation of ERTS data for certain oceanographic uses

The author has identified the following significant results. According to Lake Michigan records, the pH levels have been steadily increasing as the lake becomes more eutrophic. Numerous upwellings during the summer of 1973, beginning with the late July event, appear to be triggering a chemical precipitation of calcium carbonate. The upwelling provides abundant carbon dioxide into the surface water and results in massive blooms of phytoplankton. As the CO2 is utilized by these microscopic plants the pH is increased (acidity decreases) and CaCO3 no longer is able to remain in solution. The precipitation takes place where the phytoplankton are living, near depths of 10 meters. Therefore, the whiting observed by ERTS-1 is only seen in the green band, as red cannot penetrate but a few meters. With these whitings, secci disc readings lower in July from 10-15 meters to 3-5 meters and green, milky water is observed by research vessels. It appears that whitings have been becoming more frequent since the middle 60's but until ERTS-1 the extent had never been realized. Calcium levels are too low, presently, for a similar precipitate in Lakes Huron or Superior. However, whitings have been seen by ERTS-1 in Lakes Erie and Ontario where the calcium ion and pH levels are more like those found in Lake Michigan.

Strong, A. E.↗

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↗