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4.32 Billion Year Old Impact Melts at Apollo 14: Dating the Procellarum Basin?

Introduction: Recent work has improved our understanding of lunar crustal structure and basin evolution on the Moon, but its early impact history and implications for solar system dynamics remain poorly established [1,2]. In particular, there is a derth of absolute ages, especially for the period >4.0 Ga, that could be related to basin-forming events. Here we present U-Pb isotopic data for Zr-rich minerals found in impact-melt fragments from Apollo 14 soil sample 14163 that, when combined with previously published data, dates an impact event at 4324±15 Ma. The compositions and ages of these impact-melt fragments provide unique information about the timing of early impact events and the composition of the lunar crust. Results: Fourteen rocklets ranging in size from 1 to 3 mm were extracted from soil 14163. Most are impactmelt rocks with 10-30% clasts of mostly pyroxene and plagioclase (100 to 500 μm) in a crystalline matrix. Textures of the matrix vary from subophitic, formed by intergrowths of 10-20 μm plagioclase and pyroxene crystals, to poikilitic, with plagioclase and pyroxene reaching 20-50 μm size. Some fragments that contain no visible clasts have similar textures are also interpreted as impact-melt rocks. All fragments contain notably large proportions of euhedral to subhedral ilmenite, zircon, apatite/merrillite and less abundant zirconolite and baddeleyite in the melt matrices. These grains often form intricate intergrowths with each other and rock-forming minerals, indicating their crystallization from the melt (Fig. 1). However, some slightly larger (~50 μm) zircon and phosphate grains can be interpreted as relict clasts based on their granular textures and relationships with the surrounding phases (Fig. 1). This implies that zircon and phosphate minerals were present in the target rocks. Some of these grains were profoundly remelted during the impact, which resulted in an oversaturation of the melt in Zr and P and crystallization of new grains of Zrrich minerals and phosphates during melt solidification. The presence of zircon and phosphates indicates that the melts were significantly enriched in KREEP components and ties their provenance to the Procellarum- KREEP Terrane (PKT) [3]. Combined U-Pb zircon data obtained for all fragments form two main clusters on a concordia diagram (Fig. 2), between about 4.3 and 3.9 Ga. Phosphate data mostly concentrate on the younger end of this age range but some analyses are almost as old as the older zircon grains (Fig. 2). Figure 1: Zircon (Zr) and phosphate (Apt; Mer) grains in impact melt fragments from Apollo 14 soil 14161. A-zircon grains crystallized from impact melt; B-phosphate grain inherited from the target; C- granular zircon grains Our interpretation of these data is that all U-rich minerals experienced variable resetting of the U-Pb system, with phosphate, where closure temperature is significantly lower than that in zircon, affected more profoundly by Pb loss than zircon. Our best estimate of the time of formation of zircon and phosphate is based on statistically valid analysis of grains interpreted texturally as grown from the impact melt (Fig. 2). Ten of these analyses define an age of 4324±15 Ma (MSWD=3.0, probability of fit P=0.002). Our best estimate for the time of resetting is obtained by combining data from phosphates that are statistically indistinguishable from 3.9 Ga within the analytical uncertainties. This group is represented by 18 analyses of 15 phosphate grains from different fragments (Fig. 2) and defines an age of 3922±6 Ma (MSWD=1.2, P=0.23). Conversely, a minimum age of the target lithologies, remelted in the impact that produced the rocklets studied here (Fig. 2), can be determined from the five oldest analyses of zircon clasts at 4338±13 Ma (MSWD=1.5, P=0.2), which is indistinguishable from the age of the impact melt within the uncertainties. The obtained ages, combined with textural evidence, imply that the impact melt was formed at 4324±15 Ma, and that it occurred in a zircon-rich target with a minimum age of 4338±13 Ma. Further reworking occurred during a second impact event at 3922±6 Ma. Discussion: The younger age of 3922±6 Ma can be interpreted as the time of the Imbrium impact. The older age of 4324±15 Ma would then be the time of formation of the impact melt, which was then caught in the Imbrium ejecta either at the Apollo 14 landing site or within the target rocks of the Imbrium impact. The presence of abundant accessory phases such as zircons and phosphates is consistent with a substantial KREEP component in the analyzed particles. The current distribution of KREEP on the lunar surface appears to be strongly influenced by Imbrum ejecta [4] so interpretation of the 4.32 Ga age depends in part on assumed structure of the pre-impact crust and distribution of KREEP within the crust. If KREEP was present only in the deep crust at 4.32 Ga, then a basin-scale impact possibly analogous to Imbrium or larger may be necessary to excavate a KREEPy impact melt at this time. However, if KREEPy materials were present closer to the surface perhaps due to redistribution related to Mg-suite magmatism, then smaller impacts might be able to rework KREEPy compositions at shallower depths. The coherence of the data on the particles analysed here suggests a large volume of melt that has been preserved since 4.32 Ga, consistent with a large impact event. Relict zircons and mineral clasts suggests that the igneous crust in the vicinity of this impact was well developed by at least 4.34 Ga, similar to the model age of KREEP and older than the isochron ages of many Mg-suite cumulates [5]. A problem that confronts all lunar sample studies using the current collection is that the pre-Imbrium geology of the PKT (the source of these 4.32 Ga impact melts) is not well constrained. The South Pole-Aitken basin contains regions that are moderately enriched in Th, but its ejecta is Th-poor [6]; therefore these A14 fragments are probably not SPA ejecta. Alternatively, these fragments may represent formation of a hypothesized Procellarum basin [7] although the lack of a clearly defined basin ejecta signature is a potential problem with that interpretation. In any case, they provide a younger limit on the age of lunar differentiation and formation of KREEP within the lunar crust. Figure 2: U-Pb data for zircon and phosphate grains from impact melt fragments. A-all data; B-data used for age calculations. References: [1] Orgel C., Michael G., Fassett C. I., van der Bogert C. H., Riedel C., Kneissl T., and Hiesinger H. (2018) J. Geophys. Res. Planets 123, 748- 762. [2] Evans A. J., Andrews-Hanna J. C., Head J. W., Soderblom J. M., Solomon S. C., and Zuber M. T. (2018) J. Geophys. Planets. 123, 1596-1617. [3] Jolliff, B.L., Gillis, J.J., Haskin, L.A., Korotev, R.L. and Wieczorek, M.A. (2000) J. Geophys. Res: Planets 105, 4197-4216. [4] Haskin L. A. (1998) J. Geophys. Res. Planets 103, 1679-1689. [5] Borg L.E., Gaffney A.M., and Shearer C.K. (2015) MAPS 50, 715-732. [6] Moriarty, D.P., Watkins, R.N., Valencia, S.N., Kendall, J.D., Evans, A.J., Dygert, N. and Petro, N.E. (2021) J. Geophys. Res. Planets 126. [7] Zhu, M.H., Wünnemann, K., Potter, R.W., Kleine, T. and Morbidelli, A. (2019) J. Geophys. Res: Planets 124, 2117-2140

M D Norman↗
NASA NTRS2021

Understanding the Space Weathering of Mercury Through Laboratory Experiments

Introduction: Airless surfaces across the solar system are continually modified by energetic particles from solar wind and micrometeoroid bombardment [1,2]. This process is known as space weathering, and it alters the chemical, microstructural, and optical properties of surface regoliths on airless bodies, including Mercury. On the Moon and S-type asteroids, the reflectance spectral signatures of space weathering include reddening (increasing reflectance with increasing wavelength), darkening (lowering of reflectance), and the attenuation of characteristic absorption bands [2]. Such spectral changes are driven by the production of Fe-bearing nanoparticles(npFe) through both solar wind irradiation and micrometeoroid bombardment. While our understanding of space weathering for the Moon and near-Earth S-types asteroids is advanced, insight into how these processes operate on other planetary bodies is limited. In particular, Mercury experiences a uniquely intense space weathering environment than planetary counterparts at 1 AU, including a moreintense solar wind flux and higher velocity micrometeoroid impacts [4]. Additionally, Mercury has a surface composition unique in the inner solar system, including regions of the surface with very low albedo known as the low reflectance material (LRM), which is enriched in carbon, likely graphite, up to 4wt.% [5].In addition, the concentration of Fe across Mercury’s surface islow (<2 wt.%) compared to the Moonor S-type asteroids asteroids[6]. Our understanding of the effects of space weathering on C-rich and Fe-poor phases is limited. Since Fe plays a critical role inthe development of space weathering characteristicson other airless surfaces(e.g., npFe), its limited availability may significantly affect the development of space weathering features in Mercury surface materials. We can simulate space weathering processes in the laboratory to explore their effects on the microstructural, chemical, and spectral characteristics of Mercury surface materials[7]. Here we used pulsed laser irradiation to simulate the short duration, high-temperature events associated with micrometeoroid impacts. We performed coordinated analyses including reflectance spectroscopy and electron microscopy to investigate the spectral, chemical, and microstructural changes in these mercurian analog samples. Methods: For these experiments, we usedforsteritic olivine with varying FeOcontents, a mineral phase proposed to be abundant on the surface of Mercury. We mixed each sample with graphite to simulate LRM regions of the surface. Wesynthesized the olivinesamplesat 1-bar at NASA’s Johnson Space Centerand prepared pressed powder pellets for laser irradiation [8].We prepared three samples, each with a base layer of olivineto maintain structural integrity and topped witha surface layer containing the graphite-olivine mixture: 1) Sample SC-001 San Carlos olivine(Fo90.91),2)Sample F-S-002 with0.05 wt.% FeO olivine, and 3) F-T-004 with 0.53 wt.% FeO olivine. Each sample was mixed with 5 wt.% powdered graphite and had grain sizes ranging from 45to 125μm. We irradiated each sample usinga pulsed Nd-YAG laser, (l=1064 nm, ~6 ns pulse duration, energy of 48 mJ/pulse) while undervacuumat Northern Arizona University. The laser was rastered1x and then 5x over the surfaceof each sample to simulate progressive space weathering. We collected in situreflectance spectra from the samples after each laser pulse witha Nicolet IS50 Fourier-Transform Infrared spectrometer (lfrom 0.65-2.5 μm). We used an FEI Nova NanoSEM200scanning electron microscope (SEM) and a Hitachi TM4000 Plus benchtop SEM at Purdue University to image the surface morphology and topography of the samples. We extracted thin sections for analysis in the transmission electron microscope(TEM)using the FEI Helios NanoLab 660 focused ion beam (FIB) SEM at the University of Arizona.We performed analysis of the microstructural and chemical characteristics of the samples using the 200 keV JEOL 2500 scanning TEM at Johnson Space Center. Reflectance Spectroscopy Results:Reflectance spectra for each sample are shown in Fig. 1.SC-001:The spectrum of the unirradiated sample exhibits a weak 1.0 μm absorption feature, associated with Fe2+in the olivine,and low overall reflectance (Fig. 1a). Thereflectance and the depth of the absorption band increases after 1x laser raster but are at their lowest after 5x laser rasters.F-T-004:The unirradiated sample has a blue-sloped spectrum with low reflectance without identifiable absorption features (Fig. 1b). With progressive laser irradiation, the sample reflectance increases and becomes strongly red-sloped.F-S-002:The unirradiated sample exhibits a dark, blue-slopedspectrum. The brightness of the sample increases significantly from <0.2average reflectance over >0.8 reflectance in the most irradiated sampleand thespectral slope also becomesslightly reddened (Fig. 1c). Microstructural and Chemical Analysis: Two primary alteration textures were observed in the samples exposed to simulated space weathering: 1) fluffy C-rich,and 2) vesiculated melt. The fluffy C-rich texture is composed oflow-densitydeposits distributed across the surface of the sample(Fig. 2A). Analysis of a FIB section extracted from a low-density C-rich region in sample SC-001 reveals multiple globule-type deposits, discrete from stacked graphite, likely produced via melting from the laser irradiation [9].The vesiculated melt textureis smooth and uniformly distributed across isolated regions of the sample surface. The vesicles measure up to 100s of nmin diameter. Analysis of a FIB section from this texture was extracted from sample F-T-004 reveals a layer of amorphous melt material, close to 100 nm thick and uniform across the FIB section (Fig. 2B). Isolated regions of this melt layer contain small nanoparticles, <5 nm in diameter. Chemical analysis through energy dispersive X-ray spectroscopy reveals the composition of this layer is enriched in Si and depleted in Mg and O compared to the underlying sample. Implications for Space Weathering on Mercury: Previous experiments simulating space weathering of Mercury have showndarkening and reddening of spectra[7,10].However, our use of low-Fe materials and graphite to create a sample set more analogous to the mercurian surface. Our results indicate that sample composition plays a significant and important role in the space weathering of Mercury. In particular, our spectral data demonstrates a strong correlation between spectral slope, Fe content, and simulated space weathering. While the variation in FeO content between samples F-S-002 and F-T-004 is <0.6 wt.%, the spectra deviate from flat to strongly red-sloped(F-T-004). This reddeningmay be linked to the presence of very small nanoparticles observed in the melt textures extracted from sample F-T-004. For the SC-001 sample, the fluffy C-rich textures may be developed by the amalgamation of small graphite particles into these unique morphologies. Such observations indicate that space weathering on Mercury may result in both familiar and new microstructural and chemical characteristics. References: [1]Hapke B. (2001) J. Geophys. Res.-Planet.,106,10039–10073. [2]Pieters C.M. and Noble S.K. (2016) J. Geophys. Res-Planet., 121, 1865–1884. [3] Lucey P.G., and Riner, M.A. (2011) Icarus,212, 451-462.[4]CintalaM.J.(1992)J. Geophys. Res.-Planet.,97,947–973.[5]Klima R.L.et al.(2018)Geophys.Res.Letters, 45, 2945–2953. [6]Nittler L.R., et al. (2011) Science 333, 1847-1850.[7]Sasaki S. and Kurahashi E. (2004) Space weathering on Mercury, Adv.Space Res., 33, 2152-2155.[8] Vander KaadenK.E., et al. (2018) LPSCXLIX, Abstract 1230. [9] McGlaun M.L. et al. (2019) LPSCL, Abstract 2019. [10] TrangD.et al. (2018)LPSCXLIX,Abstract2083

M S Thompson↗
NASA NTRSDate not supplied

Pink Spinel in Apollo Impact Melt Rock 68815: Implications for Mg-Suite Magmatism

Introduction: Magnesian rocks from the lunar highlands are collectively termed the Mg-suite. Characterized by high (>60) Mg# (molar 100×Mg/[Mg+Fe]) in mafic phases and calcic plagioclase, these rocks are plutonic to hypabyssal in origin, and include a range of bulk mineralogies such as troctolites, dunites, norites, gabbronorites, and spinel troctolites [1]. These Mg-suite lithologies have distinct trace element concentrations and ratios that differentiate them from other lunar rock types. These rocks are ancient, generally dated to between 4.5 and 4.1 Ga, although it is unknown if this represents the full range of Mg-suite ages [1–2]. Among the Mg-suite lithologies, the spinel troctolites are relatively rare, to date only found in polymict breccias [3]. Spinel troctolites, as their name suggests, consist of calcic plagioclase and forsteritic olivine, with minor amounts of spinel (MgAl2O4), ± pyroxene and cordierite [1,4]. This form of spinel is often called ‘pink’ spinel because of its appearance in thin section under plane polarized light (PPL; Fig. 1), due to minor amounts of Cr. Spinel troctolites are generally plutonic or hypabyssal in origin (subsequently exhumed and incorporated into polymict breccias), or formed through impact processes (e.g., crystalline impact melt) [5]. A spinel-rich lithology has also been found in the Moscoviense region of the Moon via the Moon Mineralogy Mapper (M3) and lacks other mafic phases [6]. Finally, while the Mg-suite sampled thus far consists of plutonic (or hypabyssal) rocks, the question remains if such magmas could have erupted on the surface of the Moon [7]. These magmas have much lower density than mare basalts, but little sample or remote sensing evidence has been found to support the idea that extrusive Mg-suite volcanism occurred [7]. Here, we present a coordinated microanalytical study of spinel-bearing lithic and mineral clasts found in Apollo sample 68815. These data will be used to understand their petrogenesis (magmatic or impact) and modification histories, and to shed light on the existence of volcanic Mg-suite rocks. Sample Description: Apollo sample 68815 is a polymict impact melt breccia containing a variety of lithic and mineral fragments embedded in devitrified impact melt. This sample was chipped off the top of a boulder at Station 8 during the Apollo 16 mission and had an original weight of nearly 1.8 kg. In this study, we investigated two polished thin sections of 68815: 68815,17 and 68815,148, both containing spinel. Methods: The thin sections of 68815 were studied using optical light microscopy (PPL, cross-polarized light, and reflected light) with a Keyence VHX-7100 Digital Microscope. Each section was then X-ray mapped for 13–14 elements using a Cameca SX100 electron probe microanalyzer (EPMA) located in the Kuiper Materials Imaging and Characterization Facility (KMICF) at the University of Arizona. We have obtained geochemical information about the phases (olivine, plagioclase, spinel, pyroxene) in the thin sections also using the EPMA. In addition, we have used ThermoScientific Helios NanoLab 660 Focused-Ion-Beam Scanning-Electron Microscope (FIB-SEM) and a Hitachi S-4800 SEM (both in KMICF) to obtain backscattered electron (BSE) images and energy dispersive Xray spectrometry (EDS) maps of areas of interest. Using a JEOL 7900F SEM at the Astromaterials Research & Exploration Science (ARES) at NASA Johnson Space Center (JSC), we have obtained electron backscatter diffraction (EBSD) maps of the spinel-bearing portions of the thin sections. The EBSD data were collected under beam conditions of 20 kV, and ~90 μA, with step sizes varying from 0.05 to 2 μm. Following EBSD data collection, we processed the data using AZtecCrystal and MTEX, a free MATLAB toolbox. Results: We have found clasts with subophitic textures, that consist of primarily olivine and plagioclase, with minor amounts of pink Mg-Al spinel and pyroxene (Fig. 1). These clasts are up to ~1 mm in length and contain spinels up to 50 μm across. We have additionally identified pink Mg-Al spinels within the impact melt (i.e., not contained in lithic clasts) in both thin sections. In one instance, a single spinel grain is approximately 300 μm across (Fig. 1b, 2). The spinel fragments embedded in impact melt have varying compositions, typically distinct from the compositions of spinels in the lithic clasts. Spinel-Bearing Clasts: Ten lithic clasts with similar textures and mineral compositions were identified between 68815,17 (two clasts) and ,148 (eight clasts). These clasts fall into two groups. The first has skeletal olivine with intergranular plagioclase, with minor amounts of pyroxene and spinel (Fig. 1a, 2c, 2d). The spinel in these clasts are found amid the plagioclase. The second group have an intergranular texture of olivine and plagioclase, again with minor spinel and pyroxene. The second group may contain spinels surrounded by plagioclase, and spinels enclosed in olivine. Spinels located within both clast types range from no apparent Cr zoning, to reverse zoning (Cr-enrichment inward; Fig. 2d), to normal zoning (Cr-enrichment outward). In the clasts thus far investigated with EPMA, plagioclase compositions range from An# (molar 100×Ca/[Ca+Na+K]) 92–96. Olivine Mg# ranged from 77 to 94, while pyroxene had Mg# from 54–84. Spinel in the clasts have Cr# (molar 100×Cr/[Cr+Al]) 2–4 and Mg# 88–91, which is within the range of pristine and plutonic spinel troctolites [8]. Isolated Spinels: These crystals are generally euhedral to subhedral, and can exhibit reverse Cr zoning (Cr enrichment inward) or no apparent Cr zoning. The spinels thus far investigated via EPMA have Cr# 9–14 and Mg# 65–82. The Cr# for these spinels is within the range reported by [8], but have lower Mg#. Future Work: We will continue to process the EBSD data for these lithic and mineral clasts. We will also continue to characterize these clasts using EPMA and SEM. By thoroughly characterizing the various spinels and spinel-bearing clasts, we aim to constrain the petrogenesis of these minerals and rock fragments. Acknowledgments: We thank NASA for the loan of these thin sections. We thank Ken Domanik and Jerry Chang for their support with data collection. Work was supported by a University of Arizona RII Core Facilities Pilot Program grant and start-up funds to JJB. We acknowledge support from NASA’s Planetary Science Research program for analysis performed at JSC. References: [1] Shearer C. K. et al. (2015) Am. Min. 100, 294–325. [2] Borg L. E. et al. (2020) GCA 290, 312–332. [3] Warren P. H. (1993) Am. Min. 78, 360–376. [4] Dymek R. F. et al. (1976) LPS VII, 2335–2378. [5] Treiman et al. (2019) Am. Min. 104, 370–384. [6] Pieters et al. (2011) JGR: Plan. 116:E00G08. [7] Prissel et al. (2016) Icarus 277, 319–329. [8] Prissel et al. (2016) Am. Min. 101, 1624–1635.

spinel↗