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At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Reproduction of melting behavior for vitrified hillforts based on amphibolite, granite, and basalt lithologies

Abstract European Bronze and Iron Age vitrified hillforts have been known since the 1700s, but archaeological interpretations regarding their function and use are still debated. We carried out a series of experiments to constrain conditions that led to the vitrification of the inner wall rocks in the hillfort at Broborg, Sweden. Potential source rocks were collected locally and heat treated in the laboratory, varying maximum temperature, cooling rate, and starting particle size. Crystalline and amorphous phases were quantified using X-ray diffraction both in situ, during heating and cooling, and ex situ, after heating and quenching. Textures, phases, and glass compositions obtained were compared with those for rock samples from the vitrified part of the wall, as well as with equilibrium crystallization calculations. ‘Dark glass’ and its associated minerals formed from amphibolite or dolerite rocks melted at 1000–1200 °C under reducing atmosphere then slow cooled. ‘Clear glass’ formed from non-equilibrium partial melting of feldspar in granitoid rocks. This study aids archaeological forensic investigation of vitrified hillforts and interpretation of source rock material by mapping mineralogical changes and glass production under various heating conditions.

42 ENGINEERING↗
DOE OSTI2021

The gallium isotopic composition of the Moon

Here, in this study, we present new Ga isotope data from a suite of 28 mare basalts and lunar highland rocks. The δ 71 Ga values of these samples range from -0.10 to +0.66‰ (where δ 71 Ga is the relative difference between the 71 Ga/ 69 Ga ratio of a sample and the Ga-IPGP standard), which is an order of magnitude more heterogeneous than δ 71 Ga values in terrestrial magmatic rocks. The cause of this isotopic heterogeneity must be established to estimate the bulk δ 71 Ga value of the Moon. In general, low-Ti basalts and ferroan anorthosite suite (FAS) rocks have δ 71 Ga values that are lower than high-Ti basalts and KREEP-rich rocks. The observation that rocks derived from later forming LMO cumulates have higher δ 71 Ga values suggests that Ga isotopes are fractionated by processes that operate within the chemically evolving LMO, rather than localized degassing or volatile redistribution. Correlations between indices of plagioclase removal from the LMO (e.g. Eu/Eu*) with Ga isotope ratios suggest that a Δ 71 Ga plagioclase-melt of -0.3‰, (where Δ 71 Ga plagioclase-melt is the isotopic fractionation associated with crystallization of plagioclase from a melt), could drive the observed isotopic fractionation in high-Ti mare basalts and KREEP-rich rocks. This would be consistent with the observation that FAS rocks have δ 71 Ga values that are lower than mare basalts. However, the addition of KREEP-like material into the mare basalt source regions would not contribute enough Ga to perturb the isotopic composition outside of analytical uncertainty. Thus, basalts derived from early formed LMO cumulates such as those from Apollo 15, would preserve light Ga isotopic compositions despite containing modest amounts of urKREEP. We estimate that the δ 71 Ga value of the LMO was ~0.14‰ prior to the onset of plagioclase crystallization and extraction. Whether this δ 71 Ga value is representative of the initial BSM cannot be ascertained from the current dataset. It remains plausible that the Moon accreted with a heavier Ga isotopic composition than the Earth. Alternatively, the Moon and Earth could have accreted with similar isotopic compositions (BSE = 0.00 ± 0.06‰, Kato et al., 2017) and volatile loss drove the LMO to higher δ 71 Ga values prior to formation of the lunar crust.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

U-Pb zircon age constraints on the earliest eruptions of the Deccan Large Igneous Province, Malwa Plateau, India

Climate instability driven by emission of volatiles during emplacement of large igneous provinces (LIPs) is frequently invoked as a potential cause of mass extinctions. However, documenting this process in the geologic record requires a holistic understanding of eruption rates, the location of eruptive centers, and potential sources of climate-changing volatiles. We present new chemical abrasion–isotope dilution–thermal ionization mass spectrometry (CA-ID-TIMS) U-Pb zircon geochronology from Malwa Plateau basalts on the northern margin of the Deccan LIP, India. These basalts have been previously interpreted as either an extension of the province's main volcanic stratigraphy or as an independent eruptive center active up to millions of years prior to the main eruptive phase. Our data instead demonstrate that the lower Malwa Plateau basalts are temporally correlative with the first pulse of Deccan volcanism and provide new constraints on its initiation and duration. Paleomagnetic data further indicate that upper Malwa Plateau basalts may be age-equivalent to the second, third, and fourth pulses of Deccan volcanism. The relative thicknesses of age-equivalent packages of basalt are consistent with eruption of the Deccan LIP from a southward-migrating eruptive center. The first eruptive pulse is coeval with a ~200 kyr Late Maastrichtian warming event preserved globally in contemporaneous stratigraphic sections. We propose that the first pulse of Deccan magmatism was more voluminous in the north, where it erupted through organic-rich sedimentary rocks of the Narmada-Tapti rift basin. Thermal metamorphism of these sediments could have been a source of sufficient CO 2 to drive the Late Maastrichtian warming event, which if true would reconcile the apparent dampened warming signals associated with later Deccan eruptive pulses.

58 GEOSCIENCES↗
DOE OSTI2024

Coupled feldspar dissolution and secondary mineral precipitation in batch systems: 6. Labradorite dissolution, calcite growth, and clay precipitation at 60 °C and pH 8.2–8.4

Here, we conducted experiments on concurrent labradorite dissolution, calcite precipitation, and clay precipitation in batch reactor systems and tracked reaction processes using multiple isotope tracers. Labradorite was chosen for its role as a major and reactive component in basalt; the experiments thus directly impact our understanding of CO 2 storage in basalt aquifers and enhanced rock weathering. We doped initial solutions with 29 Si, 43 Ca, and Ca 13 CO 3 (s). Experiments were conducted at 60 °C and pH ~ 8.3 for up to 840 h, with isotope ratios in the experimental aqueous solutions measured using MC-ICP-MS. Unidirectional rates of labradorite dissolution near equilibrium were approximately two orders of magnitude slower than far-from-equilibrium rates reported in the literature. Calcite growth occurred near equilibrium and the rates were limited by the labradorite dissolution rates. In the steady state phase, the interplay of these three heterogeneous reactions—labradorite dissolution, calcite growth, and clay precipitation—results in a coupled system that approaches a near-equilibrium state. The system does not reach true equilibrium because labradorite continues to dissolve, albeit at a much slower rate near equilibrium. The overall reaction can be approximated as, Na 0.4 Ca 0.6 Al 1.6 Si 2.4 O 8 + 0.6HCO 3 - + 1·.7H 2 O + 0.4H + → 0.4Na + + 0.6CaCO 3(s) + 0.5Al 2 Si 2 O 5 (OH) 4(s) + 0.6Al(OH) 4 - + 1.4SiO 2 o (aq). The experimental results show that using short-term far-from-equilibrium rate constants would lead to an overestimation of feldspar weathering rates at the Earth’s surface (e.g., basalt weathering and enhanced rock weathering) and CO 2 mineralization in basalt aquifers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Evaluating the Thickness and Stratigraphy of Ejecta Materials at the Chang’e-4 Landing Site

The landing site of China’s Chang’e-4 (CE-4) probe is located on the mare basalts on the floor of the Von Kármán crater on the lunar far side. The Von Kármán crater is inside the ancient and highly cratered South Pole–Aitken basin, which has experienced complex emplacement sequences of both near and distant ejecta materials. These issues complicated the interpretation of the CE-4 surface in situ measurements of the visible and near-infrared spectrometer and the lunar penetrating radar (LPR) onboard Yutu-2 rover. To evaluate the sources and amounts of all principle foreign materials at the CE-4 landing site, we thoroughly examine the ejecta delivered by crater-forming events that occurred later than the formation of the mare basalts at the CE-4 landing site. We found a total of 16 craters that may have delivered ejecta thicker than 10 cm level superposed on the mare basalts at the CE-4 landing site. Crater Finsen, Von Kármán L, Von Kármán L′, and Maksutov are the top four major foreign material sources, and each of them contributed ejecta thicker than 1 m. Our surveys confirm that the ejecta from Finsen crater are the most dominant foreign materials in the uppermost few meters at the CE-4 landing site and the total impact ejecta deposited upon the mare basalts at the landing site is estimated to be thinner than 30 m. We found that the estimations from Pike’s model are the most consistent with the Yutu-2 LPR observations.

58 GEOSCIENCES↗
DOE OSTI2022

Geochronology of Cambrian Sedimentary and Volcanic Rocks in the Illinois Basin: Defining the Illinois Aulacogen

The Wabash #1 well, drilled for the Wabash CarbonSAFE Project and located in Vigo County, Indiana, USA, was drilled in early 2020 as a stratigraphic test well to characterize and evaluate the basal Cambrian Mt. Simon Sandstone for carbon dioxide storage (TD=8750 ft; 2667 m). The Wabash #1 well is located along the eastern flank of a newly interpreted Cambrian aulacogen that occurs in western Indiana and eastern Illinois. Here we present 938 new detrital zircon U-Pb ages (LA-ICPMS) from early Cambrian sandstones sampled near the base of the well. A basalt lava flow was penetrated at ~8530 ft (2600 m) and has an 40 Ar/ 39 Ar age of 525.03 +/- 1.10 Ma, which represents the first known Cambrian crust in the Illinois Basin. The two sandstone samples from beneath the basalt are dominated by zircons derived from the Midcontinent Granite-Rhyolite terrane. The sandstone samples from above the basalt reflect a mixture of these locally derived Mazatzal and Granite-Rhyolite terrane zircons, but also distal Archean, Grenville, and Yavapai zircons. Each sample has small numbers of Cambrian zircons, which is consistent with those in basal Cambrian sandstones in other deep wells to the west. These early Cambrian detrital zircons and early Cambrian age of the basalt, combined with sediment thickness patterns permit the interpretation of the Illinois aulacogen, which formed during the final stage of Rodinian rifting.

58 GEOSCIENCES↗
DOE OSTI2022

Experimental calibration of an Fe3+/Fe2+-in-amphibole oxybarometer and its application to shallow magmatic processes at Shiveluch Volcano, Kamchatka

Abstract Oxygen fugacity is an important but difficult parameter to constrain for primitive arc magmas. In this study, the partitioning behavior of Fe3+/Fe2+ between amphibole and glass synthesized in piston-cylinder and cold-seal apparatus experiments is developed as an oxybarometer, applicable to magmas ranging from basaltic to dacitic composition. The partitioning of Fe2+ is strongly dependent on melt polymerization; the relative compatibility of Fe2+ in amphibole decreases with increasing polymerization. The Fe2+/Mg distribution coefficient between amphibole and melt is a relatively constant value across all compositions and is, on average, 0.27. The amphibole oxybarometer is applied to amphibole in mafic enclaves, cumulates, and basaltic tephra erupted from Shiveluch volcano in Kamchatka with measured Fe3+/FeTotal. An average Fe3+/Fe2+ amphibole-glass distribution coefficient for basalt is used to convert the Fe3+/FeTotal of amphibole in samples from Shiveluch to magmatic oxygen fugacity relative to NNO. The fO2 of primitive melts at the volcano is approximately NNO+2 and is faithfully recorded in amphibole from an amphibole-rich cumulate and the basaltic tephra. Apparently, higher fO2 recorded by amphibole in mafic enclaves likely results from partial dehydrogenation of amphibole during residence in a shallow andesite storage region. We identify three pulses of mafic magma recharge within two weeks of, a month before, and two to three months before the eruption and find that, at each of these times, the host andesite was recharged by at least two magmas at varying stages of differentiation. Application of the amphibole oxybarometer not only gives insight into magmatic fO2 but also potentially details of shallow magmatic processes.

Geochemistry & Geophysics↗
DOE OSTI2023

Assessing the Behavior of Moderately Volatile Elements on the Moon in Order to Constrain Processes of Magmatic Evolution and Planetary Accretion

Heterogeneous isotopic compositions of Zn and Ga in lunar basalts and highlands rocks indicate that secondary processing affected the stable isotopic composition of major lunar reservoirs. It follows that these fractionating processes must be identified and characterized in order to make robust estimates for the isotopic composition of the mare basalt source regions or the bulk silicate Moon (BSM). Contrary to previous assertions (e.g., Kato & Moynier, 2017), MVEs such as Zn and Ga do not behave similarly on the Moon, in line with differences in their chemical behavior and volatility. There is clear evidence that impact reworking fractionates zinc isotopes but, in addition, zinc isotopes are also highly sensitive to the formation of Ti-bearing oxides such as ilmenite. In contrast, gallium is far less susceptible to volatile reworking, but its isotopic composition is fractionated during incorporation into plagioclase (Wimpenny et al., 2022; Render et al., 2023). Based on these findings we conclude that current isotopic compositions of Zn and Ga in lunar rocks, such as those measured for the mare basalt suite, are unlikely to be representative of the bulk Moon when it accreted. As such, estimates for the MVE isotopic composition of the BSM derived from mare basalts may not be accurate, which may have implications for the incorporation of these data into dynamical models of the Moon’s formation. In the following, we discuss the main findings from this project in more detail, focusing on the behaviour of zinc and gallium isotopic systematics in lunar rocks and the processes that control their isotopic fractionation on the Moon.

58 GEOSCIENCES↗
DOE OSTI2022

SMC Reinforced by Recycled or Textile Carbon Fiber

There is a significant need to expand material options for SMC that has traditionally used glass fibers for decades. There are several integral issues related to chopping and conveying a range of materials including glass, carbon, basalt, thermoplastic tapes, and recycled fibers. These are in a variety of forms including continuous tows, discontinuous agglomerates such as pyrolyzed carbon fibers that could be used to produce a range of SMC intermediates. Standard/conventional SMC processing is limited to cutting rotors specifically for glass and compounding with thermoset polyesters and some epoxies. The multi-material, multi-format line developed in this project is flexible to enable custom conveying and uses an interchangeable rotor dedicated for specific material types. The overall tasks undertaken in this project included: evaluation of the fiber feed mechanism, effect of textile grade carbon, evaluating servo motor controlling of conveyor, evaluate doctor box resin feed, evaluate compaction unit, evaluation of different formulations, and develop automation such as PLC programming. The new multi-material SMC line Version 2 (SCM-V2) incorporated servo motors over induction motors which gave the overall cutter system precision control and made it quiet. The addition of a 14-roll compaction unit at the end of the line in SMC-V2 enabled higher material wet out which was a limitation in the SMC Version 1 (SMC-V1). The cutters were further updated to reduce the cantilever overhang of the fiber which enabled more uniform cut lengths for glass, carbon, and basalt fibers. The overall instrumentation and system control including a remote control operation was enabled in the SMC-V2. The line speed is capable of 10-20 ft/minute. The cutting modules were designed and engineered for cutting glass, basalt and textile grade carbon in 300k and 450-600k format widths. The cutting trials were established for a range of fiber types. The study also demonstrated the utility of the line to cut and produce basalt fiber SMC. Initial trials were conducted on the properties from recycled carbon fiber (rCF) mats in epoxy resin. Overall, the Covid19 situation constrained the team from accessing the SMC line for over 18 months. Despite this challenge major advancements were made.

36 MATERIALS SCIENCE↗
DOE OSTI2023

A Spectroscopic Study of Mars-analog Materials with Amorphous Sulfate and Chloride Phases: Implications for Detecting Amorphous Materials on the Martian Surface

The Chemistry and Mineralogy X-ray diffraction (XRD) instrument aboard the Curiosity rover consistently identifies amorphous material at Gale Crater, which is compositionally variable, but often includes elevated sulfur and iron, suggesting that amorphous ferric sulfate (AFS) may be present. Understanding how desiccating ferric sulfate brines affect the spectra of Martian material analogs is necessary for interpreting complex/realistic reaction assemblages. Visible and near-infrared reflectance (VNIR), mid-infrared attenuated total reflectance (MIR, FTIR-ATR), and Raman spectra, along with XRD data are presented for basaltic glass, hematite, gypsum, nontronite, and magnesite, each at three grain sizes (<25, 25–63, and 63–180 μm), mixed with ferric sulfate (+/–NaCl), deliquesced, then rapidly desiccated in 11% relative humidity or via vacuum. All desiccated products are partially or completely XRD amorphous; crystalline phases include starting materials and trace precipitates, leaving the bulk of the ferric sulfate in the amorphous fraction. Due to considerable spectral masking, AFS detectability is highly dependent on spectroscopic technique and minerals present. This has strong implications for remote and in situ observations of Martian samples that include an amorphous component. AFS is only identifiable in VNIR spectra for magnesite, nontronite, and gypsum samples; hematite and basaltic glass samples appear similar to pure materials. Sulfate features dominate Raman spectra for nontronite and basaltic glass samples; the analog material dominates Raman spectra of hematite and gypsum samples. MIR data are least affected by masking, but basaltic glass is almost undetectable in MIR spectra of those mixtures. NaCl produces similar FTIR-ATR and Raman features, regardless of analog material.

58 GEOSCIENCES↗
DOE OSTI2021

High-precision measurement of U-Pu-Np-Am concentrations and isotope ratios in environmental reference materials by mass spectrometry

Herein, we report results of precise and sensitive mass spectrometric measurements of uranium, plutonium, neptunium, and americium concentrations and isotope ratios in a variety of environmental reference materials. Most of our work has been done on NIST SRM 4350b, River Sediment, but we also present results for NIST SRM 4354, Lake Sediment; NIST SRMs 4355 and 4355a, Peruvian Soil; NIST SRM 4357, Ocean Sediment; NIST SRM 1648a, Urban Particulate Material; NIST SRM 1649b, Urban Dust; IAEA CRM 385, Ocean Sediment; USGS BCR-2, Columbia River Basalt; and USGS BHVO-2, Hawaiian Volcanic Observatory Basalt. These materials reflect a wide range in long-lived actinide concentrations (e.g. 1E4 to 1E10 atoms 239 Pu/g) and isotope ratios. Measurements were performed in a clean laboratory by isotope dilution, multi-collector thermal ionization and multi-collector inductively coupled plasma mass spectrometry. In general, our results are in agreement with, but lower the uncertainty of, literature or certificate values for these reference materials. Our uranium results for the basalts also confirm previously reported high-precision mass spectrometric results from our laboratory. In many cases our measurements of U-Pu-Np-Am nuclides appear to be novel.

58 GEOSCIENCES↗
DOE OSTI2025

Evaluation of desiccation cracking characteristics of inorganic micro-fiber-reinforced engineered barrier material (IMEBM) for geological repository

Abstract Buffer material is crucial for the engineering barrier system to dispose of high-level radioactive waste in a geological repository. A reliable buffer material should be able to maintain good sealing characteristics and minimize desiccation cracking. In this study, the effectiveness of inorganic fiber-reinforced engineering barrier material in reducing desiccation cracks in bentonite was evaluated via desiccation tests, image analysis, and air permeability tests. The effects of fiber type (E-glass fiber and basalt fiber) and fiber content (0.0%, 0.5%, 1.0%, 1.5%, 3.0%, and 5.0% of dry weight of the bentonite) on the development of desiccation cracks in the fiber–bentonite mixtures with the same given initial moisture content were evaluated. The results indicated that the addition of fibers could significantly reduce the crack size and area in bentonite during the drying. Basalt fibers showed a slightly better reinforcement effect than E-glass fibers when the fiber content was lower than 3.0%. The addition of fibers prevented the development of penetrating cracks and significantly reduced the permeability of the bentonite after drying. The permeabilities of basalt fiber- and E-glass fiber-reinforced bentonite composites with 3% reinforcement were 5.81 × 10 –11 m 2 and 7.24 × 10 –11 m 2 , respectively, which were 64 and 51 times smaller than that of pure bentonite. X-ray–CT observation of the internal structure of the samples after drying showed that the addition of fibers significantly changed the crack morphology and potentially increased the tortuosity.

Feng, Yuan↗
DOE OSTI2023

Emerging investigator series: kinetics of diopside reactivity for carbon mineralization in mafic–ultramafic rocks

The ongoing use of fossil fuels to supply modern energy demands has necessitated research on combating carbon dioxide (CO 2 ) emissions and climate change. Carbon storage via mineral trapping in basalt and related rocks is a promising strategy. However, mineralization rates depend on the variable minerology that makes up these rock formations. Diopside (CaMgSi 2 O 6 ) is a common pyroxene mineral in ultramafic and mafic rocks including basalt, but relatively little work has been done to understand its carbon mineralization kinetics using hydrated supercritical CO 2 , which induces the formation of reactive nanoscale interfacial water films. Here, in situ XRD experiments at 50–110 °C and 90 bar indicate that diopside transforms into a myriad of Mg/Ca carbonates, including huntite [Mg 3 Ca(CO 3 ) 4 ] and very high magnesium calcite (VHMC, i.e., protodolomite). Through ex situ characterization, we were able to constrain reaction pathways for the dissolution–precipitation transformation process including metastable intermediate precipitates. Experiments performed at variable temperatures enabled Avrami-derived rate constants and an apparent activation energy of 97 ± 16 kJ mol –1 , implying the dissolution of diopside is the rate-limiting step. Density functional theory (DFT) calculations, used to gain molecular insight into the surface stability of the diopside during dissolution, suggest that exposed calcium cations are susceptible to dissolution when put in contact with water given their coordination environment. The collective results point to the high CO 2 mineralization potential of diopside in basalts, which could help guide parameterization of reactive transport models needed to design and permit commercial-scale subsurface carbon storage operations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗