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65 records · Page 4

Investigating Variations in Water Abundances in Lunar Felsite Clasts Using Coordinated Field-Emission STEM and NanoSIMS Analyses

As representatives of petrochemically-evolved igneous rocks on the Moon, the granitic felsite clasts in lunar breccias have come under renewed focus as part of new efforts to use feldspars for assessing the inventory of lunar water and other volatiles. Previous petrologic studies of these clasts were tilted towards finding those assemblages and relationships most likely to be direct products of magmatic processes. In support of our on-going NanoSIMS (Nanoscale Secondary Ion Mass Spectrometry) measurements of trace water contents in the feldspars in these clasts, we are using coordinated analytical SEM (Scanning Electron Microscopy), electron probe microanalyzer (EPMA) and analytical field emission scanning transmission electron microscopy (FE-STEM) techniques to re-evaluate the full diversity of processes under which the feldspar-bearing assemblages in these clasts formed. Here we report a comparison of FE-STEM imaging and microanalysis results obtained on focused ion beam (FIB) sections extracted from felsite (alkali feldspar plus SiO2 plus or minus plagioclase) clasts in lunar breccias 15405 and 12013. The feldspars in these clasts have water contents which, although relatively low (7-18 ppm) by terrestrial standards, still show values significantly higher than measurements (approximately 0.5 ppm) of nominally anhydrous NanoSIMS standards.

Christoffersen, Roy↗

Capturing an Evolving Nebular Environment: A Petrographic and Geochemical Study of a Type A, B & C CAI

Calcium, Aluminum-rich Inclusions (CAIs) were the first formed solids in our Solar System, with mineral assemblages reflecting the first phases predicted to condense out of a hot nebular gas of Solar composition. Geochemical, textural and crystallographic information in CAIs can be used to constrain the temperature, pressure, and composition (e.g., oxygen fugacity) of the gaseous reservoir(s) from which they formed, as well as any secondary (nebular and parent body) processes they underwent. Coordinated geochemical and textural analyses provide information on nebular conditions (i.e., astrophysical environments and dynamics of nebular gas reservoirs) in which these CAIs formed. In order to better understand the evolution of nebular reservoirs at the time of CAI formation, we analyzed a Type A, B and C CAI using Electron Probe Micro-Analyzer (EPMA) and Electron BackScatter Diffraction (EBSD) at NASA Johnson Space Center (JSC).

Comins, M. B.↗

Analysis of "Stone" Samples from C-Type Asteroid Ryugu

As a part of activities of initial analysis, we analyzed eighteen Ryugu “stone” samples of 1 ~ 8mm in size: seven stones from the 1st touch down site and eleven from the 2nd touch down site. Ryugu stones were analyzed first using X-rays, UV, visible, near-infrared, mid-infrared, and muon probes for surface reflectance spectra, internal 3D structure and element distribution, crystal structures, and bulk composition of light elements such as C, N, and O. Measurements for magnetic, thermal, and physical properties using some stones were also performed. TOF-SIMS analysis of fluid inclusions as being continued. Small particles separated from some stones were analyzed by IR-CT. Based on 3D-CT images of individual stones, objects of interests were identified, separated by pFIB cutting, and exposed by polishing on the surface of epoxy disks. FE-EPMA/FE-SEM analysis was made on ~40 polished epoxy disks for chemical composition and textural observation. FIB sections and small (~15 μm in size) fragments were separated from polished surface and analyzed by TEM, STXM,XRF, and nano-CT.

T. Nakamura↗

Sample Polishing Without Epoxy

In recent years, we have received requests for meteorite sample sections to be prepared without using epoxy impregnation or mounting. The reasoning for these requests ranges from potential contamination of analyses from epoxy chemical components to degradation of instrumental vacuum from epoxy outgassing (e.g., SEM, SIMS, EPMA, etc.). An alternative approach that we employ involves sawing off a 1-5 mm thick wafer of the sample. The wafer is ground using silica carbide lapping media wetted with 190 proof ethyl alcohol to make both sides flat and parallel. The sample is then polished on one or both sides using diamond paste or dry diamond powder on a rotating lap wheel until the desired finish is obtained. The sample is cleaned in between steps using 200 proof ethyl alcohol in an ultrasonic cleaner. Friable and altered samples need to have higher thickness in order for polishing to be attempted. Without epoxy to hold the sample together or a glass slide for backing, the sample needs additional material to provide the necessary support structure. The machining steps of this process need to be undertaken at a much slower speed than in traditional thin or thick section preparation.

Meteorite↗

Preservation of Organic Carbon in Dolomitized Cambrian Stromatolites and Implications for Microbial Biosignatures in Diagenetically Replaced Carbonate Rock

Stromatolites have been a major focus in the search for ancient microbial life, however, the organic carbon biosignatures of dolomitized stromatolites have not yet been fully characterized or correlated with their dolomitizing conditions. Although dolomitization rarely preserves microbial morphology, the presence of organic carbon can provide valuable information for characterization of fossils’ biogenicity, syngenicity, and indigeneity to their host rock. The Cambrian Allentown Formation in New Jersey, USA, is an excellent example of dolomitized stromatolites and thrombolites containing diagenetically modified microbial biosignatures. Based on XRD and EPMA data, the dolomite composition is typically stoichiometric, with varying degrees of cationic ordering. The outcrop underwent early dolomitization in a marginal-marine setting and later burial diagenesis resulting in multi-generational dolomite formation: (1) 2 microspar dolomite formed by early diagenetic replacement at or near the surface, (2) zoned dolomite formed penecontemporaneously with the microspar phase as rhombohedral crystals by infilling primary pore spaces within the microspar matrix. The rhombic crystals continued to grow outward in alternating stages of Fe-enriched and -depleted fluids, which were preserved in zoned rims and revealed by cathodoluminescence, and (3) saddle dolomite formed during late stage deep burial with Fe- and Mn-rich fluids, and occurs as a void-filling, high-temperature phase. Organic carbon, characterized using confocal Raman microscopy, has an exclusive distribution within the microspar dolomite, and the D and G bands’ characteristics reveal similar thermal alteration to the host rock, indicating that the mapped organic carbon is indigenous and syngenetic with the Cambrian carbonates. The findings presented in this study reveal organic matter found within microspar of various dolomitized facies deriving from different source pools of organic carbon. This study sheds light on biosignatures in secondary dolostones and may aid biosignature detection in older carbonate rocks on Earth and Mars.

Dolomitization↗

Additional Trials & Tribulations in Synthesizing a Sulfide Standard

Well-characterized sulfide reference materials that can serve as matrix-matched calibrants for in-situ trace element analyses via laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) remain elusive. Here, we describe the creation an in-house sulfide standard at NASA JSC that will be used to measure siderophile and chalcophile trace elements in low pressure experimental products, specifically pentlandite ([FeNi]9S8) and pyrrhotite ([FeNi]1-xS), as well as natural sulfides in terrestrial and meteoritic mineral assemblages. Recent methods in creating a homogenous sulfide standard include pressed pellets, synthesized chips, or fused glass [e.g. 1-3]. Other studies, however, have had success in forming homogenous FeS standards via synthesization methods [e.g. 4-6]. We present a variation of the method described in [4], in which we create a pyrrhotite standard doped with a variety of trace elements (Zn, As, Se, Mo, Ru, Rh, Pd, Sn, Sb, Te, W, Os, Ir, Pt, Au) at ~10-40 ppm and Cu at ~200 ppm. Sulfide compositions were constructed using Fe and Ni metal and elemental sulfur powders. Trace elements were added to elemental sulfur from Atomic Absorption Spectroscopy (AAS) elemental standards as either nitrate or chloride solutions to prevent oxidation of the metal powders. The dried sulfur mixture was mixed with Fe and Ni powders and mechanically mixed before two aliquots were placed in separate SiO2 tubes. Each tube was held under vacuum for ~30 minutes, sealed under vacuum, and then heated at 800C for 48 hours. Like [4], the synthesis products were composed of pourous sulfide crystals. Major element analyses of both experimental aliquots, collected using an Electron Probe Microanalyser (EPMA), yield indistinguishable major element compositions (uncertainties in 2SE & 2RSE[%]), with an average of 57.90  0.09 (0.16 %), 4.95  0.03 (0.55 %), and 39.70  0.14 (0.34 %), for Fe, Ni, and S, respectively. Trace element data were measured using a Photon Machines 193nm laser ablation system coupled to a Thermo-Scientific Element-XR ICP-MS. Spot sizes were limited to 50 μm due to the porous nature of the sulfide target material. Trace element abundances, normalized to Fe as an internal standard, were also found to be homogenous between the two aliquots, with weighted mean 2RSE (%) values of <3.0 for all trace elements. Synthesized products were re-powdered and absolute concentrations measured via solution ICP-MS. Although the sulfide appears to be homogenous, sintering experiments will be performed to more closely match the standard density to natural sulfides and minimize differences in ablation behavior. Improved density also allows for higher sensitivity (i.e. more compact target material) and larger spot sizes or traverses, as void space is eliminated. Additional major and trace element analyses on the products of the sintering experiments will be undertaken.

Jacob B Setera↗

Olivine Compositional Systematics of CI Chondrites and Asteroid Ryugu

Recent findings of rare anhydrous silicates (especially, olivine) in asteroid Ryugu samples suggest that small amounts of precursor materials escaped subsequent aqueous alteration in the Ryugu parent body [e.g., 1]. The origins of these anhydrous grains are considered to be either AOA-like or chondrule-like materials [2,3]. We have studied CI chondrites Ivuna and Orgueil on the same manner to analyze Ryugu samples and found the similar occurrence of anhydrous silicates in these brecciated meteorites [4]. In this abstract we report the mineralogy of olivine grains in another CI chondrite Alais to compare with Orgueil and Ivuna as well as Ryugu samples to better understand their origins through compositional systematics obtained by detailed FE-EPMA analysis.

T. Mikouchi↗

Ternary Feldspar Within Felste Clasts From Apollo Impact Melt Breccia 72255

Granitic clasts with unique ternary feldspar compositions have been identified within samples of the layered impact melt breccia from Apollo 17 Station 2 Boulder 1 (72215, 72235, 72255 and 72275), and in a felsite clast from station 3 (73215). These “ternary” compositions seemingly plot within the miscibility gap of the albite-anorthite-orthoclase (Ab-An-Or) system. Feldspars with these compositions have not been identified in terrestrial samples, and equilibrium feldspar compositions from laboratory experiments indicate they would not be thermodynamically stable. Thus, the physiochemical processes involved in forming these unique ternary feldspars remain poorly understood. To better constrain the formation of ternary feldspar within lunar breccias, we have undertaken a coordinated scanning electron microscope (SEM)-based coupled electron backscatter diffraction (EBSD) and energy dispersive spectrometry (EDS), electron microprobe analyzer (EPMA) wavelength dispersive spectrometry, and transmission electron microscopy (TEM) study. The goals of this study are twofold: 1) confirm whether ternary feldspar is present as coherent, single-crystals or sub-microscopic intergrowths of normal compositions, and 2) better constrain the formation conditions of clasts containing ternary feldspar.

T. M. Erickson↗

Microstructural Evolution of the Civet Cat Norite (72255)

The ‘Civet Cat Norite’ is a ~ 2.5 cm clast within the Apollo impact melt breccia sample 72255 collected during Apollo 17 EVA 2 at Boulder 1. The norite is primarily composed of plagioclase and orthopyroxene with fine-scale exsolution lamellae of augite. The plagioclase and orthopyroxene (OPX) coexist with minor quartz and augitic clinopyroxene (CPX), and accessory apatite, baddeleyite, chromite, ilmenite, loveringite, merrillite, rutile and zircon. The major minerals range from 1 to 4 mm in size and show a cataclastic texture indicated by banding of the light and dark phases]. The chemical composition of the orthopyroxene, augitic exsolution lamellae, and exsolved oxides suggest the norite crystallized in the lower crust of the Moon (10 – 70 km depth) and was subsequently excavated by impact(s). Shock pressure estimates for the norite range from 15 – 35 GPa based on maskeleynite formation within the plagioclase, kink banding in pyroxenes, and granular recrystallization in the accessory phosphates. Previous Rb-Sr and 40 Ar/ 39 Ar analyses recalculated with modern decay constants yield relatively young ages of 4.16 ± 0.05 Ga and 3.99 ± 0.03 Ga, respectively. However, recent U-Pb analyses of some zircon grains from within the Civet Cat yield an age of 4.45 ± 0.03 Ga. While this is the oldest age for any rock recovered from the Moon, the full age spread of zircon from the Civet Cat range from ca. 4.46 to 4.02 Ga, indicating variable Pb-loss and complicating interpretation of the primary age. Recent atom probe analyses indicate minimal Pb mobilization within the oldest zircon grain from Civet Cat, supporting the interpretation that these ancient zircon ages reflect the age of the norite, rather than an apparent antiquity caused by reverse discordance. To investigate the potential antiquity and deep crustal origin of the Civet Cat norite, we have undertaken high resolution microstructural analyses of the major, minor, and accessory minerals to characterize the primary igneous textures and secondary overprinting by impact and metamorphism. The employed analytical techniques include scanning electron microscope-based electron backscatter diffraction (EBSD) analyses, electron probe microanalyzer (EPMA) chemical analyses, and transmission electron microscopy (TEM) of pyroxene, plagioclase, quartz, zircon, and phosphates.

T M Erickson↗

Insights Into Reconstructing REE Compositions of Melt From Zircon-Melt Partition Coefficients Using Zircon-Hosted Melt Inclusions From the Yellowstone Volcanic Province

Establishing the major and trace element composition of the Earth’s melts (Hadean to recent) is essential for understanding crustal evolution. Due to its physical-chemical resilience, zircon spans the complete age spectra of Earth’s history, and thus provides the only physical record from the early Earth. However, the petrological context i.e., the melt from which zircon crystallised, is often lost, except for inclusions of melt preserved within zircon. Melt inclusions in zircon (MI) provide a valuable tool to constrain zircon-melt REE partition coefficients (D REE ), which are used with the zircon REE chemistry to reconstruct melt compositions. Such reconstruction requires accurate partition coefficients, which are particularly sensitive to temperature, but also to pressure and melt composition. We determined the major and trace element compositions of 60 co-existing zircon-MI pairs from two ~ 2 Ma age rhyolites (the caldera-forming Huckleberry Ridge Tuff; HRT-C and the post-caldera Blue Creek Flow; BC-1) of the Yellowstone Plateau volcanic field by EPMA and SIMS, and calculated a set of 60 zircon-MI partition coefficients. The MI from both units are glassy with average silica contents of 78.30 ± 0.74 and 77.19 ± 1.11 wt %, and Ti-in-zircon crystallisation temperatures are 839 ± 36 and 835 ± 35 oC. Measured D REE patterns for each population (n = 30) are tightly constrained and exhibit a smooth pattern spanning ~ six orders of magnitude from La to Lu, (with exceptions at Ce and Eu), and for the HRT exhibit greater curvature (i.e., flatter) between the MREE to HREE compared to the BC-1. D REE patterns for the HRT have small to moderate Ce anomalies (Ce/Ce* Di 50 ± 40), whereas those in the BC-1 are larger (98 ± 45), and both units exhibit negligible to positive Eu anomalies (Eu/Eu* Di 1.07 ± 0.89 and 1.80 ± 2.01, respectively). We compare the trace element compositions of the MI to bulk-glass compositions from Yellowstone to assess any differences, which are small, then compare the measured MI compositions to those reconstructed using published partition coefficients (natural, empirical and experimental). The choice of D REE for reconstruction of the melt REE pattern results in differing petrogenetic interpretations.

Laura J. Crisp↗

Phosphate Textural Diversity in CI Chondrites and C-Type Asteroids

Introduction: Apatite, Ca 5 (PO 4 ) 3 (CL/F/OH-), is a ubiquitous phosphate found throughout the solar system, including the most primitive solids, CI-chondrites [1,2] and related samples of carbonaceous asteroids Ryugu [3] and Bennu [4], returned by JAXA’s Hayabusa2 and NASA’s OSIRIS-REx missions, respectively. Apatite in these primitive solids is found as individual grains or mineral clusters and has been inferred to form from the hydrothermal sequence during cooling of their respective parent body or bodies. To better understand the formation history and reworking of these early phosphates we have undertaken a highly coordinated study of phosphate microstructures, geochemistry and U/Pb geochronology from a suite of CI meteorites and carbonaceous asteroid samples. These data have identified novel phosphate microstructures and complex relationships across a suite of apatite grains from the early solar system, indicating multiple episodes of growth and modification on the CI parent body(ies). Methods: Samples of CI chondrites, Alais, Ivuna, Orgueil, Oued Chebeika 002, Yamato (Y) 82162, Y980115, Y980134, and two chips of Hayabusa2 Ryugu particles (A0262 and C0263) have been acquired for analysis. The bulk texture of the samples were first scanned by X-ray Computed Tomography (XCT) using the Nikon XT H 320 within the XFACT facility at NASA JSC or the Xradia 620 Versa at the UTCT facility. Based on the identification of petrofabrics or features of interest from the XCT data, samples were chipped, oriented, potted in epoxy and thick sections were prepared. After anhydrously polishing the samples with silicon carbide and dry diamond powder down to 1 µm, the samples were ion polished using a Hitachi ArBlade. Energy dispersive Xray spectrometry (EDS) maps were collected to ID phosphates of interest using a JEOL 7900F SEM. The internal microstructures of identified phosphates were then mapped by electron backscatter diffraction (EBSD) using the JEOL 7900F. Based on the EDS and EBSD data, domains of interest were targeted for quantitative chemical analyses using a JEOL 8530 EPMA. Subsequently, in situ U-Pb and 207 Pb/ 206 Pb ages will be collected using a Cameca ims1290 secondary ion mass spectrometer at UCLA across a range of microstructures. Results: Apatite grains are ubiquitous throughout the CI chondrites and carbonaceous asteroid materials, found as individual grains, disseminated clusters or grain aggregates. Apatite grains are associated with serpentine, magnet-ite, and/or carbonate. Of particular interest, we have identified individual and aggregate polycrystalline grains ex-hibiting an internal ‘honeycomb’ texture (Fig. 1). Some of these grains appear overprinted by subsequent alteration while others remain unaltered. Apatite halogen sites are dominated by the missing component, assumed to be OH, and F, comparable to published values from Bennu, Ryugu and CM-chondrites [3-5]. However, the Yamato CI-like meteorites show a broader range of Cl values, and one grain from Alais is dominated by CL. Summary: Apatite growth features indicate a protracted and complex growth history, consistent with precipitation from an evolving fluid system. The ‘honeycomb’ texture identified in some CI meteorites is, to the best of our knowledge, the first report of such a microstructure in meteoritic phosphate. The microtextures and zoning will guide subsequent age analyses, to better constrain the formation and reworking of phosphate in CI(-like) materials. Acknowledgments: We thank the National Institute of Polar Research, Japan for samples of Y82162, 980115 and 980134 meteorites, ASU’s Buseck Center for Meteorite Studies for samples of Ivuna and Alais meteorites, and JAXA curation for chips of Ryugu material. This work was funded by NASA ROSES LARS grant 24-LARS24-0014. References: [1] Morlok et al., 2016, GCA 70:5371-5394. [2] Alfin g et al., 2019, Geochemistry 79:125532. [3] Nakamura et al. (2022) Science 379:1-15. [4] Seifert et al. (2026) MAPS 61:504-521. [5] Piralla et al. (2021) MAPS 56:809-828.

CI chondrites↗