Meteoritics & Planetary Science 54, Nr 7, 1401–1430 (2019) doi: 10.1111/maps.13295

The early geological history of the Moon inferred from ancient lunar meteorite Miller Range 13317

N. M. CURRAN 1,2,*, K. H. JOY1, J. F. SNAPE3, J. F. PERNET-FISHER1, J. D. GILMOUR 1, A. A. NEMCHIN4, M. J. WHITEHOUSE3, and R. BURGESS1

1School of Earth and Environmental Sciences, University of Manchester, Oxford Road, Manchester M13 9PL, UK 2NASA Goddard Space Flight Center, 8800 Greenbelt Road, Greenbelt, Maryland 20771, USA 3Department of Geosciences, Swedish Museum of Natural History, SE-104 05 Stockholm, Sweden 4Department of Applied Geology, Curtin University, Perth, Western Australia 6845, Australia *Corresponding author. E-mail: natalie.m.curran@nasa.gov (Received 17 October 2018; revision accepted 14 March 2019)

Abstract–Miller Range (MIL) 13317 is a heterogeneous basalt-bearing lunar regolith breccia that provides insights into the early magmatic history of the Moon. MIL 13317 is formed from a mixture of material with clasts having an affinity to Apollo ferroan anorthosites and basaltic volcanic rocks. Noble gas data indicate that MIL 13317 was consolidated into a breccia between 2610 Æ 780 Ma and 1570 Æ 470 Ma where it experienced a complex near- surface irradiation history for ~835 Æ 84 Myr, at an average depth of ~30 cm. The fusion crust has an intermediate composition (Al2O3 15.9 wt%; FeO 12.3 wt%) with an added incompatible trace element (Th 5.4 ppm) chemical component. Taking the fusion crust to be indicative of the bulk sample composition, this implies that MIL 13317 originated from a regolith that is associated with a mare-highland boundary that is KREEP-rich (i.e., K, rare earth elements, and P). A comparison of bulk chemical data from MIL 13317 with remote sensing data from the Lunar Prospector orbiter suggests that MIL 13317 likely originated from the northwest region of Oceanus Procellarum, east of Mare Nubium, or at the eastern edge of Mare Frigoris. All these potential source areas are on the near side of the Moon, indicating a close association with the Procellarum KREEP Terrane. Basalt clasts in MIL 13317 are from a very low-Ti to low-Ti (between 0.14 and 0.32 wt%) source region. The similar mineral fractionation trends of the different basalt clasts in the sample suggest they are comagmatic in origin. Zircon-bearing phases and Ca-phosphate grains in basalt clasts and matrix grains yield 207Pb/206Pb ages between 4344 Æ 4 and 4333 Æ 5 Ma. These ancient 207Pb/206Pb ages indicate that the meteorite has sampled a range of Pre-Nectarian volcanic rocks that are poorly represented in the Apollo, Luna, and lunar meteorite collections. As such, MIL 13317 adds to the growing evidence that basaltic volcanic activity on the Moon started as early as ~4340 Ma, before the main period of lunar mare basalt volcanism at ~3850 Ma.

INTRODUCTION basaltic volcanism is currently unknown, although the majority of the Apollo mare basalts erupted between Determining the distribution and duration of ~3850 and ~3200 Ma (Head 1976; Head and Wilson ancient lunar volcanism is vital to our understanding of 1992; Nyquist and Shih 1992; Stoffler€ and Ryder 2001; the early evolution of the interior and thermal history Hiesinger et al. 2003). Ancient lunar volcanism of the Moon, and in the wider context of volcanism on (>3900 Ma) has been documented in the Apollo sample other planetary bodies. The products of these volcanic collection by KREEP basalt fragments (Ryder and eruptions infilled large impact basins, most of which are Spudis 1980; Taylor et al. 1983; Terada et al. 2007) and situated on the lunar near side. The earliest timing of the ~4300 to 3900 Ma Apollo 14 high-Al mare basalt

1401 © 2019 The Authors. Meteoritics & Planetary Science published by Wiley Periodicals, Inc. on behalf of The Meteoritical Society (MET) This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited. 1402 N. M. Curran et al. group (Taylor et al. 1983; Nyquist and Shih 1992; Zeigler and Korotev 2016) indicated that the sample is a Snyder and Taylor 2001; Neal and Kramer 2006). mixture of both anorthositic and mafic components, Lunar basaltic meteorites extend the range of these and likely belongs in the category of a “mingled” magmatic processes in representing both the youngest regolith breccia (e.g., Korotev et al. 2009). MIL 13317 (e.g., ~2930 Ma, Northwest Africa [NWA] 032: Borg can be further subclassified as moderately mafic (FeO et al. 2009) and oldest (~4350 Ma, Kalahari 009: ~9.0 to 16.0 wt%) and Th-rich (5.4 ppm), similar to Terada et al. 2007; Sokol et al. 2008) known samples. only seven other lunar stones/meteorite groupings Stratigraphic relationships inferred from remote sensing including Lynch 002, the NWA 4472/4485 paired data and crater counting model age calculations have stones, Calcalong Creek, Sayh al Uhaymir (SaU) 169, also indicated occurrences of ancient >3850 Ma Dhofar (Dho) 1442, and NWA 6687 (Korotev 2018). volcanism over widespread regions including Mare Initial studies of Zr-bearing and Ca-phosphate minerals Frigoris, Mare Australe, Mare Tranquillitatis, and Mare indicated crystallization ages of basalt clasts of Serenitatis (e.g., Schultz and Spudis 1979, 1983; 4332 Æ 2 Ma (Snape et al. 2018), 4351.8 Æ 8.7 Ma, and Hiesinger et al. 2000, 2003, 2008; Whitten and Head 4270 Æ 24 Ma (Shaulis et al. 2016), which are similar in 2015). age to the youngest lunar ferroan anorthosites and The age of the oldest known volcanic sample at ancient magmatic rock suites. ~4350 Ma (Kalahari 009: Terada et al. 2007), implies an overlap between the beginning of lunar basaltic ANALYTICAL TECHNIQUES volcanism with ancient feldspathic crustal rocks. For example, the ferroan anorthosites (FAN), formed 4560– Analyses of MIL 13317 were performed on a 4280 Ma (Carlson and Lugmair 1988; Nyquist et al. polished thin section (MIL 13317,7), a small polished 1995, 2010; Borg et al. 1999, 2011; Nemchin et al. block (MIL 13317,11a), and bulk chips (from MIL 2009a; Elkins-Tanton et al. 2011; Gross and Joy 2016; 13317,10 and MIL 13317,11b), all provided by the Pernet-Fisher and Joy 2016) and ancient magmatic NASA Meteorite Working Group. The MIL 13317,10 intrusions such as the high-Mg suite (HMS) and the subsplit is from a regolith portion of the sample and high-Alkali suite formed ~4500 to 4100 Ma, and 4370– MIL 13317,11 is from a fragmental portion. The 4030 Ma (extending to 3800 Ma), respectively (Carlson methodology we employed is outlined below and in and Lugmair 1981; Meyer et al. 1989, 1996; Nyquist more detail in Data S1 and Table S1 in the supporting and Shih 1992; Nyquist et al. 2010; Borg et al. 2011; information. Carlson et al. 2014). Lunar meteorites represent invaluable additional Sample Petrography and Chemistry samples that provide information about different rock types, originating from regions that are remote from the Two sections (MIL 13317,7 and MIL 13317,11a) near side equatorial Apollo and Luna landing sites, were carbon-coated and analyzed at the University of including samples from the lunar far side (Warren and Manchester. Petrographic characterization was Kallemeyn 1991; Korotev et al. 2003; Korotev 2005; performed using a FEI XL30 field emission gun Joy and Arai 2013; Calzada-Diaz et al. 2015). In this environmental scanning electron microscope with paper, we report a detailed petrographic, geochemical, electron dispersive spectrometer and EDAX Genesis and noble gas investigation of lunar meteorite Miller software. Montaged backscattered electron (BSE) Range (MIL) 13317, coupled with in situ U-Pb analyses images (Fig. 1a) and element maps (Fig. 1b) were of zircon-rich (Zr-rich) and calcium-phosphate (Ca- processed using the ImageJ software package (Rueden phosphate) phases. We demonstrate that this meteorite et al. 2017). Optical microscope-cathode luminescence- contains various clasts originating from ancient basalts, imaging (CL-imaging) was acquired using a CITL 8200 shedding further light on the earliest phase of the mk3 “cold” CL system coupled to a transmitted-light Moon’s magmatic history. microscope; typical conditions were ~10 to 15 kV and a current of ~300 mA. Miller Range 13317 Mineral phases were analyzed using a Cameca SX 100 electron microprobe (EMPA) equipped with a BSE Miller Range 13317 is a 32.2 g lunar meteorite that detector and five wavelength-dispersive spectrometers. was found in Antarctica in 2013 by the Antarctic Major (Si, Al, Fe, Ca, Mg, Ti) and minor (Na, K, P, Search for Meteorites program (ANSMET). The Mn, Cr, S, Ni) elements were analyzed with a 15 kV meteorite was initially classified as an anorthositic accelerating voltage, a beam current of 20 nA, and a breccia (NASA 2015). However, preliminary focused beam diameter of 1 lm. Counting times examinations (Curran et al. 2016; Shaulis et al. 2016; between 10 and 50 s were used for each element. Lunar meteorite Miller Range 13317 1403

Fig. 1. a) Montaged backscattered electron images of thin section (MIL 13317,7) and polished block (MIL 13317,11a) of subsplits of MIL 13317. b) False-color element maps of two sections of MIL 13317 where colors correspond to: Ca = yellow (phosphates), Mg = green (pyroxene cores), Si = blue (silica), Fe = red (olivine, pyroxene rims), Al = white (plagioclase), Ti = pink (ilmenite and spinel), and K = cyan (k-feldspar). The false-color maps were used to assess the diversity of clasts within MIL 13317 (see approach of Joy et al. 2011c). Figure S6 in supporting information shows the difference between the two subsplits of MIL 13317. c) Backscattered electron image of MIL 13317,7 with clasts studied in this work outlined in red. The clasts are described in Table S1. (Color figure can be viewed at wileyonlinelibrary.com.)

Typical errors were ~0.1 wt% for major elements and 90Zr, 93Nb, 95Mo, 133Cs, 137Ba, 139La, 140Ce, 141Pr, ~0.05 wt% for minor elements for both calibration and 146Nd, 147Sm, 153Eu, 157Gd, 163Dy, 165Ho, 166Er, 172Yb, sample analyses. The instrument was calibrated against 175Lu, 178Hf, 181Ta, 208Pb, 232Th, and 238U. Samples well-characterized mineral standards. Acceptable were ablated using a spot size of 60 lm, at a repetition analytical totals were taken to be between 98 and rate of 8 Hz with the laser energy at the target (fluence) 101 wt% and mineral compositions were checked for regulated at ~5.5 J cmÀ2. Laser ablation times of 60 s stoichiometry. A defocused beam of 10 lm was used to were used with 10 s dwell times between analyses. SRM assess the bulk composition of fine-grained clasts and NIST 612 was used as the calibration standard. Calcium homogenous glass areas within the fusion crust. and Si were used as the internal normalizing standards To further assess the bulk rock composition of MIL for plagioclase and other phases, respectively. Repeat 13317, we used glass beads that were produced by NIST 610 and NIST 614 analyses were measured over fusing MIL 13317,10 (Bulk 1) and MIL 13317,11b the analytical campaign in order to assess the data (Bulk 2) by laser heating for noble gas analysis (see the quality (supporting information Table S2). Typical Noble Gas Analysis section). Glass beads were mounted %RSD for most elements in NIST 610 is better than on glass slides using superglue adhesive, polished, and 5% (except for Ni—19%, Ti—8%, Cr—6%, Sr—10%). carbon-coated. A 10 lm defocused beam was used to Typical %RSD for elements in NIST 614 is better than determine major elements by EMPA (Table 1). It is 10% (except for Sc—38%, Cr—27%, Mn—31%, Co— noted that as a result of the high temperatures 23%, Zr—24%, Mo—14%). Detection limits varied by experienced during melting, there is a potential for the <10 ppb. The abundances obtained for NIST 610 and loss of some volatile elements using this approach, 614 are within range of certified values reported within although we assume these losses to be negligible as we the GeoReM database (georem.mpch-mainz.gwdg.de). detected Na in the glass beads made after laser heating Data reduction was conducted using Iolite software (v3) (Table 1). using the “Trace Elements IS” data reduction scheme, where the time-resolved display and segment-picking for Mineral Trace Element Chemistry data integrations allow signal spikes from inclusions to be identified and avoided. Mineral trace element analyses were conducted on an ASI RESOlution 193 nm excimer laser ablation Noble Gas Analysis system coupled to an Analytik Jena PlasmaQuant MS Elite ICP-MS at the University of Portsmouth. Data Two rock chips, from subsplits MIL 13317,10 and were acquired for isotopes of 27Al, 29Si, 43Ca, 31P, 39K, MIL 13317,11b, were investigated for their bulk rock 45Sc, 49Ti, 51V, 52Cr, 55Mn, 59Co, 60Ni, 85Rb, 87Sr, 89Y, noble gas content. Neon, Ar, and Xe were analyzed on a 44N .Cra tal. et Curran M. N. 1404

Table 1. Fusion crust chemistry data for MIL 13317,7, bulk rock chemistry data of MIL 13317,10 and MIL 13317,11b (after laser heating during noble gas analysis), and bulk clast composition data for fine-grained impact melt breccia (imb) clasts in MIL 13317,7. Errors are given as 2r SD values, where the value represents the average of a sum of analysis (number of points analyzed: fusion crust on MIL 13317,7 = 28, MIL 13317,10 = 27, and MIL 13317,11b = 25). b b Number of SiO2 TiO2 Al2O3 Cr2O3 FeO MnO MgO CaO Na2OK2OP2O5 NiO SO3 Ba La analysisa wt% Total ppm 13317,7 Fusion 28 49.13 1.04 15.98 0.13 12.31 b.d 5.87 11.60 0.31 0.27 b.d b.d b.d 96.65 272.32 25.04 Æ0.76 Æ0.11 Æ0.90 Æ0.01 Æ0.98 Æ0.27 Æ0.32 Æ0.02 Æ0.04 Æ48.51 Æ5.13 13317,10 Bulk 1 27 48.95 0.71 19.01 0.20 9.66 b.d 6.37 12.05 0.26 0.13 0.10 0.02 0.05 97.51 Æ3.44 Æ0.50 Æ4.50 Æ0.12 Æ2.68 Æ3.75 Æ3.75 Æ0.14 Æ0.06 Æ0.144 Æ0.05 Æ0.08 13317,11b Bulk 2 25 49.90 1.22 9.83 0.34 16.85 0.25 5.35 10.70 0.52 0.34 0.28 b.d b.d 95.57 Æ2.63 Æ0.76 Æ2.24 Æ0.81 3.59 Æ0.09 4.95 Æ3.07 Æ0.42 Æ0.18 Æ0.19 Clast Type Clast 9a imb 30 48.48 0.43 23.65 0.14 6.60 0.10 4.14 14.21 0.28 0.24 b.d b.d 0.15 98.42 Æ4.58 Æ0.77 Æ7.20 Æ0.13 Æ6.16 Æ0.09 Æ4.29 Æ3.23 Æ0.09 Æ0.37 Æ0.83 Clast 9b imb 10 46.31 0.10 27.84 0.10 4.27 0.06 3.20 16.51 0.29 0.08 b.d b.d 0.18 98.93 Æ5.65 Æ0.34 Æ22.78 Æ0.37 Æ15.75 Æ0.23 Æ11.49 Æ8.70 Æ0.25 Æ0.12 Æ1.12 Clast 19 imb 23 49.78 0.51 18.44 0.20 9.69 0.14 5.93 12.96 0.27 0.14 b.d b.d 0.10 98.17 Æ6.56 Æ0.68 Æ19.50 Æ0.24 Æ13.62 Æ0.20 Æ9.74 Æ8.71 Æ0.24 Æ0.21 Æ0.25 Clast 20 imb 15 46.45 0.36 25.43 0.12 5.58 0.08 3.91 15.37 0.27 0.09 b.d b.d 0.12 97.80 Æ1.73 Æ0.25 Æ4.87 Æ0.08 Æ3.51 Æ0.05 Æ2.54 Æ2.15 Æ0.06 Æ0.04 Æ0.24 Detection limits for EMPAc 0.02 0.04 0.01 0.01 0.04 0.02 0.008 0.03 0.05 0.01 0.02 0.018 0.04 aNumber of analysis refers to the number of spot analysis during EMPA for a specific clast. bData from Zeigler and Korotev (2016). cIf the average oxide (wt%) composition fell below the detection limits shown here they were determined to be below detection (b.d.). Lunar meteorite Miller Range 13317 1405

Thermo ScientificTM HELIX-MC noble gas mass CAMECA IMS 1280 ion microprobe at the NordSIMS spectrometer at the University of Manchester. A facility at the Swedish Museum of Natural History, PhotonmachinesTM fusion diode laser (3 mm beam Stockholm, using a methodology similar to that diameter) was used to step-heat samples from 0.6 to 21 W outlined in previous studies (Whitehouse et al. 1997, (in six to nine steps depending on mass of the sample) 2005; Nemchin et al. 2009b; Snape et al. 2016). Full corresponding to the complete melting of the sample. details of the secondary ion mass spectrometry (SIMS) Prior to analysis, chips were loaded into an aluminum methodology are included in Section S1.3 in Data S1. holder in the laser port and baked for 24 h at 200 °Cto These data were processed using in-house SIMS remove any absorbed atmospheric gases. During analysis, data reduction spreadsheets and the Excel add-in any active gases released from the sample were removed Isoplot (version 4.15; Ludwig 2012). Three different sets by two SAES getters (NP10 and GP50) during of ages were calculated (1) Pb-Pb isochron ages, using the gas preparation stage (see Section S1.2 in the Pb isotope compositions uncorrected for Data S1 for full experimental technique). Blanks contamination with terrestrial common Pb, (2) and air calibrations were performed before and after terrestrial common Pb corrected 207Pb/206Pb ages (using every sample analysis. Typical blanks were 6.1 9 the model of Stacey and Kramers [1975] and their 10À12 cm3.STP 20Ne, 8.6 9 10À11 cm3.STP 40Ar, and 1.2 values for present-day terrestrial Pb isotopic ratios), and 9 10À14 cm3.STP 132Xe. All isotopes were background (3) U-Pb concordia ages. A U-Pb concordia age was and blank corrected. Neon-22 was corrected for not calculated for the baddeleyite and merrillite grains ++ interferences from CO2 . The sensitivity and mass due to the lack of analyses on appropriate matrix- discrimination of the mass spectrometer were determined matched external standards and the well-known matrix- using 0.2 cc aliquots of pure air at a known pressure. orientation problems associated with U-Pb calibration Neon-isotope systematics reflect a mixture of of baddeleyite (Wingate and Compston 2000). All age cosmogenic (c), trapped solar wind (tr), and trapped uncertainties are reported at the 95% confidence limit in fractionated solar wind (fSW) with the following the following discussion. Following SIMS analysis, 20 22 20 endmember isotope ratios ( Ne/ Ne)c = 0.8, ( Ne/ SEM images were acquired of the targeted phases to 22 20 22 21 22 Ne)tr = 13.8, ( Ne/ Ne)fSW = 11.2, ( Ne/ Ne)c = 0.76, assess the exact locations of the SIMS pits, to ascertain 21 22 21 22 ( Ne/ Ne)tr = 0.033, and ( Ne/ Ne)fSW = 0.0295 if any overlapped with mineral grain boundaries (see (Wieler 2002a, 2002b; Lorenzetti et al. 2005). For argon, supporting information Fig. S1). Four such analyses 38 36 Arc and Artr were derived using the endmember were identified (supporting information Table S3) and 36 38 36 38 cosmogenic ( Ar/ Arc = 0.65) and trapped ( Ar/ Artr excluded from the combined age calculations (e.g., = 5.35) compositions (Wieler 2002a, 2002b). Xenon weighted averages of 207Pb/206Pb ages or Pb-Pb isotopic measurements were first treated as the sums of isochrons), and are not considered further. contributions from cosmic ray spallation, fission, and trapped solar wind components (see Section S1.2 RESULTS in Data S1). The following assumptions were 132 126 128 126 made: ( Xe/ Xe)REE = 0.06, ( Xe/ Xe)REE = 1.22, The petrology and geochemistry of MIL 13317 are 132 126 128 126 ( Xe/ Xe)Ba = 1.053, ( Xe/ Xe)Ba = 1.621; for the consistent with a lunar origin. The Fe/Mn ratios of 132 136 trapped components, we assumed: ( Xe/ Xe)tr = 3.33, pyroxene and olivine in MIL 13317 plot on previously 134 136 ( Xe/ Xe)tr = 1.22; and for fission components, we determined lunar meteorite trend lines (Fig. 2) (Papike 132 136 134 136 assumed: ( Xe/ Xe)238U = 0.577, ( Xe/ Xe)238U 1998; Karner et al. 2003, 2006; Joy et al. 2014). MIL 132 136 134 136 = 0.828, and ( Xe/ Xe)244Pu = 0.885, ( Xe/ Xe) 13317 also contains trapped “solar” noble gases with 244Pu = 0.939 (Pepin et al. 1995; Swindle 2002; Crowther similar compositions to other lunar meteorites (see the and Gilmour 2013; Meshik et al. 2014). The method of Regolith History section). Hohenberg et al. (1978) was used to calculate production 21 38 126 rates to determine t21 ( Nec), t38 ( Arc), and t126 ( Xec) Petrography and Mineral Chemistry of MIL 13317 exposure ages (t = cosmogenic isotope abundance/ production rate). The antiquity of the sample based on Miller Range 13317 is a well-consolidated regolith 40 36 ( Ar/ Ar)tr was calculated using the method of Joy et al. breccia, comprising a diverse array of polymict lithic (2011a). clasts (black, dark-gray, clear, and cream) fused together in a heterogeneous matrix of the same material, with Secondary Ion Mass Spectrometry shocked melt veins and mineral fragments (supporting information Figs. S2 and S3). Lithic clasts are up to The Ca-phosphate (apatite and merrillite), zircon, ~7 mm in size and include regolith breccias, basalts, and baddeleyite U-Pb systems were analyzed using a feldspathic fragments, symplectites, norites, and granulites 1406 N. M. Curran et al.

Fig. 2. Fe to Mn ratio (in atoms per formula unit) for lithic components (basalt, basaltic impact melt breccias, impact melt breccias, and highland clasts) and matrix material in (a) pyroxene and (b) olivine. MIL 13317 data are overlaid on Fe/Mn data for lunar meteorites and Apollo mafic phases (see Joy et al. [2014] and references therein of literature sources). Chond. = chondrite, OC = ordinary chondrite. (Color figure can be viewed at wileyonlinelibrary.com.)

(Figs. 1 and 3). Mineral fragments are up to 1.5 mm in tallized residual melt material of basaltic magmas. Other diameter and typically consist of pyroxene, plagioclase, basaltic clasts range from fine-grained (minerals and olivine. Impact melt breccias are abundant in the <0.2 mm) clasts with “pods” of late-stage mesostasis, to sample, including clast-rich and crystalline types. Melt coarse-grained (minerals <1 mm) clasts and fragments veins are variable in size and crosscut both the matrix and with both intergranular and subophitic textures. These clasts in random orientations (Fig. 3a). Rare glass textures suggest a range of cooling histories for basaltic spherules (<100 lm) were found in the sample matrix (see clasts in MIL 13317. Fig. 3i inset), but no agglutinates were identified. Various Pyroxene in basaltic clasts of MIL 13317 are clast types are described below (see Fig. 1c for clast generally anhedral grains <1 mm in size and show a location and number). Mineral and bulk clast wide range in Fe/Mg ratios. Complex chemical zoning compositions are given in supporting information Tables from Mg-rich cores to Fe-rich rims is present in all S4–S8. pyroxene grains, with augite being the modally most abundant species with lesser amounts of pigeonite Basaltic Clasts (Fig. 4). Chemical compositions of pyroxene are Wo8-37 There are numerous medium- and fine-grained En0.4-54 Fs28-88. Some more evolved basaltic clasts (e.g., basaltic clasts in MIL 13317 (Fig. 1). The largest clasts Clast 15) are Fe-rich, with compositions of Wo17-27 En6- (Clasts 1 and 4, Figs. 3a and 3b) are ~2.0 9 1.5 mm in 10 Fs66-75. Pyroxene grains have both LREE depleted size, and are composed of an intergrowth of pyroxene, and flat LREE profiles ([La/Sm]CI = 0.17–0.96), plagioclase, silica, and areas of mesostasis (e.g., K-glass, display flat HREE profiles ([Dy/Yb]CI = 0.91–1.06) phosphates, zircons) associated with late-stage crys- (Fig. 5a), and have strong negative Eu-anomalies Lunar meteorite Miller Range 13317 1407

Fig. 3. Backscattered electron images of clasts in MIL 13317,7. a) Clast 1 (basalt), (b) Clast 4 (basalt), (c) Clast 2 (basaltic impact melt breccia—bas/IMB), (d) Clast 7 (bas/IMB), (e) Clast 5 (norite), (f) Clast 9 (impact melt breccia, IMB), (g) Clast 12 (IMB), (h) Clast 16 (symplectite), and (i) a 50 lm glass bead. Mineral abbreviations: Si = silica; pl = plagioclase; pyx = pyroxene; ap = apatite; symp = symplectite; IMB = impact melt breccia; meso = mesostasis. Figure 1c shows the location of the different clasts in MIL 13317.

(Eu/Eu*=0.05–0.12). Pyroxene U and Th abundances across the suite of mineral fragments (Fig. 6a). range from 0.02 to 1.47 ppm and 0.02 to 8.80 ppm, Plagioclase REE abundances display fractionated LREE respectively. Elongated silica grains (SiO2 = 90.0– relative to the HREE ([La/Yb]CI = 11.9–12.2) and 99.8 wt%) and plagioclase laths are up to 1 mm in size. positive Eu-anomalies (Eu/Eu*=19.8–22.7). Abundances Plagioclase show a range of An compositions (An78-94) of Sr and Ba in plagioclase range from 222 to 223 ppm 1408 N. M. Curran et al.

Fig. 4. Pyroxene mineral composition data for clasts and matrix in MIL 13317,7 and MIL 13317,11a. a) Pyroxene quadrilateral of these data. b) Fe# (atomic Fe/Fe + Mg 9 100) versus Ti# (atomic Ti/Ti + Cr 9 100). Fields show the extent of pyroxene composition in Apollo VLT, low-Ti and high-Ti mare basalts (from Bence and Papike 1972; Vaniman and Papike 1977; Dymek et al. 1975). c) Fe# (atomic Fe/Fe + Mg 9 100) versus Al/Ti (atoms per formula unit). (Color figure can be viewed at wile yonlinelibrary.com.) Lunar meteorite Miller Range 13317 1409

Fig. 5. a, b) Chondrite normalized (values from Anders and Grevesse 1989) pyroxene REE profiles for (a) pyroxene within basalt Clasts 1 and 4, and norite Clast 5. b) Pyroxene within the sample matrix. c) Chondrite normalized plagioclase REE profiles from impact melt breccia Clast 12 and norite Clast 5. d) Plagioclase [Eu/Sm]CI (CI chondrite normalized) versus Sm (ppm) from impact melt breccia Clast 12 and norite Clast 5 compared with data from different Apollo highland rock suites (data from Papike et al. 1996, 1997; Floss et al. 1998; Shervais and McGee 1998; Cahill et al. 2004). e) Chondrite-normalized REE profiles for basaltic Clast 18, impact melt breccia Clast 9, and the fusion crust. f) Sm (ppm) versus Sc (ppm) for basaltic clast 18, impact melt breccia Clast 9, and the fusion crust of MIL 13317,7. Lunar meteorites with intermediate compositions (from Korotev et al. 2009) have also been plotted for comparison. Fields of lunar rock types from Korotev et al. (2009). Bulk composition of high-K KREEP is shown for comparison in all plots (Warren 1989). (Color figure can be viewed at wileyonline library.com.) and 72 to 73 ppm, respectively. Mineral trace element estimated by averaging together six 60 lm laser ablation analyses of plagioclase and pyroxene grains from basalt spots, which included a representative range of minerals Clasts 1 and 4 display REE systematics similar to those in the clast. The average compositions display LREE reported in minerals from Apollo low-Ti mare basalts enrichments ([La/Sm]CI = 1.46), fractionated HREE (Table S2). Plagioclase CL images (Fig. S3) display a profiles ([Dy/Yb]CI = 1.18), and negative Eu-anomalies deep red-purple color, indicative of maskelynite (a high- (Eu/Eu*=0.21) (Fig. 5e). shock plagioclase pseudomorph) (Kayama et al. 2009; Large regions of symplectites and mesostasis (up to Pernet-Fisher et al. 2017). The bulk trace element 0.7 9 0.4 mm in Clasts 1 and 4) are present, typical of compositions for fine-grained basalt Clast 18 were Apollo mare basalts (e.g., Pernet-Fisher et al. 2014; 1410 N. M. Curran et al.

Fig. 6. Compositions of plagioclase grains in MIL 13317. a) Ternary diagram of anorthite (Ca), albite (Na), and orthoclase (K) for plagioclase in MIL 13317,7 and MIL 13317,11a. b) An content (atomic Ca/Ca + K + Na) for plagioclase in different clast types including basalt, impact melt breccia, highland clasts, and matrix mineral fragments. (Color figure can be viewed at wile yonlinelibrary.com.)

Potts et al. 2016). The mesostasis areas within these plagioclase (Fig. 7a). A 0.6 9 1.2 mm sized noritic clast basaltic clasts consist of predominantly anhedral (Clast 5, Fig. 3e) with an igneous texture contains highly Fe-rich pyroxene (Wo11-29 En0.6-10 Fs61-88), fayalite anorthositic plagioclase (An95-97) and subhedral Mg-rich (Fa96-97), Si- and K-rich glass (3–5 wt% K2O and on orthopyroxene (Mg#71-80, Wo2-9 En65-78 Fs19-27). The average 74 wt% SiO2), ilmenite, and silica. Rare plagioclase grains in Clast 5 display large positive Eu- mineral phases (<100 lm) include irregular grains of anomalies (Eu/Eu*=20.08 and 52.98) and LREE troilite, apatite, merrillite, tranquillityite, baddeleyite, enrichments ([La/Sm]CI = 1.85 and 5.67) (Fig. 5c). Meta- and zircon. igneous gabbroic granulites (Clasts 12 and 14, Fig. 3g) and matrix fragments include feldspathic varieties (Clast Highland and Impact Melt Breccias Clasts 12; An>94, Fig. 7a) and pyroxene and/or olivine with Miller Range 13317 contains a range of nonbasaltic Mg# between 63 and 87. Trace element systematics for rocks and minerals showing an affinity to lunar highland plagioclase from granulitic Clast 12 (Eu/Eu*=15.83; [La/ rock types. Several clasts have mafic minerals (pyroxene Sm]CI = 1.77) are similar to that of plagioclase from and olivine) with high-Mg numbers (Mg#>70) and calcic igneous Clast 5 (Figs. 5c and 5d). Lunar meteorite Miller Range 13317 1411

Fig. 7. a) Anorthite component (mol%) in plagioclase versus Mg# (=Mg/[Mg + Fe] 9 100) in mafic minerals in MIL 13317. Clast compositional relationships where the data points show the average An content in plagioclase (An#) and the Mg# content in pyroxene per clast. The error bars represent the total range of mineral chemistries determined per clast. Rock suite fields are from Shearer et al. (2006). b) Comparison of FeO (wt%) versus Al2O3 (wt%) showing the fusion crust composition for MIL 13317,7. MIL 13317 is compared to other Miller Range and the YAMM group of basaltic meteorites (data from Korotev and Zeigler 2014). MIL 13317 is also compared to another Th-rich meteorite Calcalong Creek (Hill and Boynton 2003) and Th-poor meteorite Kalahari 009. (Color figure can be viewed at wileyonlinelibrary.com.) 1412 N. M. Curran et al.

There are a variety of texturally diverse impact melt Accessory minerals in the matrix are mainly Ca- breccia clasts in MIL 13317 (Figs. 3e–g). The largest is phosphate (merrillite and apatite) and Zr-bearing phases a 2.0 9 7.0 mm feldspathic fragment (Clast 9, Fig. 7b) <100 lm in size. Three Zr-bearing phases were with a noritic anorthosite composition composed of identified: zircon, baddeleyite, and the rare lunar mineral calcic plagioclase (An94-98), low-Ca pyroxene (Mg# 55- tranquillityite (see Fig. S1). These accessory phases are 70, Wo4-11 En49-65 Fs28-40), and minor amounts of typically associated with symplectic areas with pyroxene, troilite. The FAN-like plagioclase (Fig. 7a) and trace minor olivine, K-rich glass, and K-feldspar. element systematics for Clast 9 were estimated by averaging data from six 60 lm laser ablation spots. Evolved Lithologies Clast 9 displays fractionated LREE/HREE profiles Highly evolved lithologies of granitic (granophyric) ([La/Yb]CI = 2.2) and negative Eu-anomalies (Eu/ K-feldspar and silica intergrowths, up to 0.7 mm are Eu*=0.61) (Fig. 5e). Concentrations of Sm are lower present in MIL 13317 (Fig. 1—cyan colored phases). than Apollo mafic impact melt breccia groups (Fig. 5f) The K-feldspar occurs as blocky phases with lath-like (Korotev et al. 2009). They are, however, similar to silica. These assemblages are commonly associated with some lunar meteorites which are more mafic and less regions of mesostasis and areas of K-rich glass, and are feldspathic (i.e., anorthositic norite and troctolite) than most similar to the Apollo high-alkali suite rock types. feldspathic lunar meteorites in general (Korotev et al. It is possible that some of these are fragments of 2009; Korotev 2018). Hypocrystalline impact melt clasts mesostasis from the basaltic clasts. are also abundant, and comprise interstitial plagioclase crystals surrounded by mafic glassy melt. Fusion Crust and Bulk Rock Analysis Other impact melt breccia clasts in MIL 13317 A dark-brown vesicular fusion crust is present on include crystalline types with igneous-like textures (bas/ the MIL 13317,7 section, which has an average IMB in Figs. 3c and 3d). These types (Clasts 2, 7, and composition shown in Table 1 (Fig. S2). The fusion 8) consist of zoned pyroxene (Wo4-40 En19-28 Fs39-68), crust displays LREE enrichment ([La/Sm]CI = 1.40), plagioclase (An64-90), silica, globular Fe-metal, and fractionated HREE profile ([Dy/Yb]CI = 1.15), and a troilite. Plagioclase grains are richer in K (Or0.9-28) than negative Eu-anomaly (Fig. 5e). The Th-composition of those seen in the basalt and highland lithologies in MIL the fusion crust is 5.41 ppm (Table S2). 13317 (Fig. 6a). Pyroxene displays fine exsolution Two bulk compositions we determined from chips lamellae (<1 lm) with pigeonite hosting augite. MIL 13317,10 (Bulk 1) and MIL 13317,11b (Bulk 2). Pyroxene compositions lie on a mixing line between Bulk 1 composition (MIL 13317,10, Table 1) is slightly ferrosilite (average Wo6 En27 Fs66) and Ca-rich augite more ferroan than the fusion crust and most similar to (average Wo36 En20 Fs43). Accessory phases include Ca- the Apollo 17 regolith breccias in terms of Mg# (29–47) phosphates (both apatite and merrillite, <50 lm) and and K2O (0.06–0.15 wt%) contents. Bulk 2 composition zircon grains (<20 lm). (MIL 13317,11b) has a higher K2O content and is richer Rare glass spherules (50–100 lm) are sporadically in Fe (Table 1; Fig 7b) compared to the fusion crust distributed through MIL 13317. One glass spherule and bulk 1. The fusion crust composition is (Fig 3i) was determined to have an impact origin (Mg/ intermediate between bulk 1 and 2 (Table 1; Fig. 7b). Al <1.5 and Mg/Ca <1), rather than volcanically sourced (Mg/Al >1.5 and Mg/Ca >1), as indicated by its Noble Gas Inventory Mg/Al = 0.34 and Mg/Ca = 0.40 ratios (Delano and Livi 1981; Joy et al. 2011a). Five separate chips of MIL 13317 (three from MIL 13317,10 and two from MIL 13317,11b) were analyzed Mineral Fragments for Ne and Ar isotopes and one chip (from MIL The matrix of MIL 13317 consists of single mineral 13317,10) for Xe isotopes. A summary of the noble gas fragments up to 1.5 mm in size. The majority of mineral data is given in Table 2 and Tables S9–S11 in the fragments are plagioclase and pyroxene with a wide supporting information. range of compositions (An78-99 and Wo1-44En1-70Fs12-88, Neon data for MIL 13317,10 are dominated by respectively, Figs. 4 and 6). Trace element compositions trapped 20Ne/22Ne and 21Ne/22Ne ratios (Fig. 8a), of the matrix pyroxene are similar to pyroxene within whereas MIL 13317,11b shows a trend of increasing the basaltic clasts (Fig. 5b). The REE patterns display 21Ne/22Ne and decreasing 20Ne/22Ne ratios with negative Eu-anomalies (Eu/Eu*=0.01–0.05) and increasing laser heating steps (see Table S9). Trapped 20 22 20 22 variable LREE depletions of [La/Sm]CI = 0.09–0.17 Ne/ Ne ratios ( Ne/ Ne)tr were determined using a (Fig. 5b). Silica and ilmenite are also present with minor least squares fitting to the data on a three-isotope amounts of Mg-rich olivine up to 1.5 mm in size. mixing diagram (Fig. 8a). Overall, Ne in MIL 13317 Lunar meteorite Miller Range 13317 1413

Table 2. Summary of trapped, cosmogenic, antiquity, and exposure age noble gas data in MIL 13317,10 and MIL 13317,11b. Errors are 2r SD. 21 Æ 38 Æ 20 Æ 36 Æ 40 * Æ Sub Weight Nec Arc Netr Artr Ar Antiquity Sample split (mg) 10À8 cm3STP/g age (Ma) Æ MIL 13317 10 3.08 12.7 4.98 s.d s.d 17,046 521 s.d s.d –– MIL 13317 10 0.56 51.4 5.75 392 10.2 52,246 1789 253 29.4 15,672 235 1570 471 MIL 13317 10 0.66 57.3 20.9 774 21.8 200,238 10,050 500 63.1 1850 560 MIL 13317 11b 0.63 40.7 1.14 62.6 0.19 440.03 91.4 40.5 0.73 –– MIL 13317 11b 2.26 47.3 0.84 72.8 0.13 368.81 63.6 47.0 0.56 2610 783 MIL 13317 10 4.99 ––

20 22 t21 Æ t38 Æ t126 Æ Sub Weight Ne/ Netr 40 36 131 126 Sample split (mg) (from intercept) Æ Ar/ Artr Æ Xe/ Xec Æ (Ma) MIL 13317 10 3.08 10.8 0.43 n.d n.d 71 28 n.d n.d –– MIL 13317 10 0.56 12.2 0.33 2.03 0.61 287 32 2860 74 –– MIL 13317 10 0.66 12.6 1.15 2.56 0.77 320 117 5652 159 –– MIL 13317 11b 0.63 11.7 0.43 n.d n.d 227 6 457 1.4 –– MIL 13317 11b 2.26 12.6 0.38 4.81 1.44 264 5 532 1.0 –– MIL 13317 10 4.99 5.65 0.40 ––– –835 84 s.d. = saturated detectors; n.d. = not determined.

20 22 has a ( Ne/ Ne)tr ratio between 10.8 and 12.6 (for on the Moon of about 30 cm. This depth was used to 20 À8 both subsplits, Table 2). The concentrations of Netr in calculate production rates of P21 = 0.1789 9 10 3 À8 3 MIL 13317,10 are higher than in MIL 13317,11b cm STP/Ma, P38 = 0.1369 9 10 cm STP/Ma, and 36 À8 3 (Table 2; Fig. 8a). The Artr concentrations were also P126 = 0.2250 9 10 cm STP/Ma (based on the method ~10 times higher in MIL 13317,10 compared to MIL of Hohenberg et al. 1978). These production rates yield 40 36 13317,11b (Table 2). The ( Ar/ Ar)tr values of 2.03– exposure ages for neon (t21) of between 71 Æ 28 and 4.81 indicates an antiquity age of between 320 Æ 117 Myr, argon (t38) of between 457 Æ 1.4 and 2610 Æ 783 Ma and 1570 Æ 471 Ma (using the method 5652 Æ 159 Myr, and xenon (t126) of 835 Æ 84 Myr of Eugster et al. 2001; Joy et al. 2011b) (Table 2). (Table 2). 38 The concentration of cosmogenic Arc is an order of magnitude higher in MIL 13317,10 compared to U-Pb and Pb-Pb Chronology MIL 13317,11b (Table 2). There is also a factor of 38 approximately 2 difference in Arc within the three Analyses of a zircon and five baddeleyite grains in 21 subsplits of MIL 13317,10. In contrast, Nec MIL 13317,7 yield terrestrial common Pb corrected concentrations for all analyzed chips are similar and 207Pb/206Pb ages between 4326 Æ 12 Ma and mostly within error of each other (Table 2). 4349 Æ 16 Ma (Table 3). The zircon analyses were carried Three-isotope mixing diagrams of 124Xe/130Xe versus out on a single ~70 lm grain. Calculating either a 126Xe/130Xe (see Fig. 8b) illustrate the components weighted average 207Pb/206Pb age (4337 Æ 17 Ma; present in MIL 13317,10. The sample is dominated by a MSWD = 2.9; P = 0.034; Fig. 9), or a Pb-Pb isochron age solar wind component (98%), but contains minor (4331 Æ 49 Ma; MSWD = 4.1; P = 0.016; Fig. 10c) from amounts of spallation products from Ba: the bulk these data results in high MSWD values and low spallation Xe signature corresponds to (30 Æ 11%) (1r) probabilities of fit, potentially due to partial resetting of of 126Xe derived from Ba. Heavy Xe isotopes formed by the U-Pb system within different parts of the grain. fission of U or Pu are not evident in any of the samples Nonetheless, a U-Pb concordia age of 4334 Æ 17 Ma is (supporting information Fig. S4). Petrographic determined for the three zircon analyses with less than observations revealed that MIL 13317 contains REE- 10% discordance (concordance and equivalence bearing phases like zircon, apatite, merrillite, and K-rich MSWD = 1.4; P = 0.24; Fig. 11a). Despite being located glass, which account for the presence of some spallogenic in separate areas within the breccia matrix, the five xenon components. The depth-sensitive shielding baddeleyite grains analyzed were all associated with 131 126 indicator Xe/ Xec is 5.6 Æ 0.4 (1r), assuming an similar symplectite assemblages (Fig. S1) and all yield average lunar regolith density of 1.5 g cmÀ3 (Carrier indistinguishable 207Pb/206Pb ages of between et al. 1991), this corresponds to an average burial depth 4341 Æ 10 Ma and 4345 Æ 8 Ma. Considering the 1414 N. M. Curran et al.

Fig. 8. a) 21Ne/22Ne versus 20Ne/22Ne for MIL 13317,10 and MIL 13317,11b. Each symbol represents a different laser heating step of the individual chips. The cosmogenic (Cos) and solar wind endmember (solar wind, SW) and fractionated solar wind (fSW) are from Wieler (2002a, 2002b). Inserted graph is a close-up of the solar-dominated region of the plot. Errors are shown to 2r. Lunar meteorite, Apollo, and Luna soils and breccia data were taken from Curran et al. (2017). b) 124Xe/130Xe versus 126Xe/130Xe isotopes for MIL 13317,10. Lines indicate mixing between spallation endmembers (REE and Ba), which plot off the plot area, and solar wind (SW). Errors are reported to 2r. (Color figure can be viewed at wileyonlinelibrary.com.) baddeleyite as a single population gives weighted average Two of the 12 matrix apatite analyses were obtained 207Pb/206Pb age of 4344 Æ 4Ma (MSWD= 0.11; from a single ~40 lm apatite grain, within which it was P = 0.98; Fig. 9) and a Pb-Pb isochron age of possible to place two SIMS spots. These two SIMS spots 4344 Æ 5Ma(MSWD= 0.12; P = 0.95; Fig. 10d). yielded the lowest 207Pb/206Pb ratios in the sample, with a Lunar meteorite Miller Range 13317 1415

Table 3. Summary of U-Pb isotope data for phases (zircon, baddeleyite, apatite, merrillites) in matrix minerals and basalt clasts in MIL 13317,7 determined by SIMS analysis. Uncertainties for the isochron ages are stated at the 95% confidence level. Clast/Matrix Phase 207Pb/206Pb Æ1r % Age (Ma) Æ1r (abs.) Clast 4 basalt Apatite 0.5389 0.53 4351 8 Clast 4 basalt Apatite 0.5341 0.46 4338 7 Clast 4 basalt Apatite 0.5322 0.19 4333 3 Clast 4 basalt Apatite 0.5332 0.19 4336 3 Clast 4 basalt Apatite 0.5329 0.20 4335 3 Clast 4 basalt Apatite 0.5307 0.16 4329 2 Clast 10 basalt Apatite 0.5357 0.36 4343 5 Symplectite assemblage Baddeleyite 0.5358 0.41 4343 6 Symplectite assemblage Baddeleyite 0.5365 0.24 4345 4 Symplectite assemblage Baddeleyite 0.5351 0.34 4341 5 Symplectite assemblage Baddeleyite 0.5364 0.47 4344 7 Symplectite assemblage (Clast 16) Apatite 0.5343 0.43 4339 6 Melt glass/symplectite assemblage Baddeleyite 0.5361 0.19 4344 3 Matrix Zircon 0.5296 0.42 4326 6 Matrix Zircon 0.5365 0.37 4345 5 Matrix Zircon 0.5382 0.53 4349 8 Matrix Zircon 0.5318 0.39 4332 6 Matrix Apatite 0.5358 0.39 4343 6 Matrix Apatite 0.5380 0.48 4349 7 Matrix Apatite 0.5366 0.50 4345 7 Matrix Apatite 0.5323 0.47 4333 7 Matrix Apatite 0.5382 0.45 4349 7 Matrix Apatite 0.5328 0.60 4335 9 Matrix Apatite 0.5351 0.48 4341 7 Matrix Apatite 0.5352 0.52 4341 8 Matrix Apatite 0.5373 0.63 4347 9 Matrix Merrillite 0.5253 0.36 4314 5 Matrix Merrillite 0.5268 0.86 4318 13 Matrix Merrillite 0.5363 0.55 4344 8 Matrix Merrillite 0.5577 1.31 4401 19 Matrix Merrillite 0.5259 0.77 4316 11 Matrix Merrillite 0.5121 0.39 4277 6 Matrix Apatite 0.3943 0.70 3888 10 Matrix Apatite 0.3954 0.82 3892 12 Melt clast Merrillite 0.5255 0.60 4314 9 Melt clast Merrillite 0.5138 0.74 4281 11 Melt clast Merrillite 0.5202 0.50 4299 7

weighted average 207Pb/206Pb age of 3889 Æ 16 Ma to form a single population, a weighted average (MSWD = 0.06; P = 0.8) and a U-Pb concordia age of 207Pb/206Pb age of 4342 Æ 4 Ma (MSWD = 0.59; 3890 Æ 33 Ma (concordance and equivalence P = 0.81; Fig. 9) is obtained. A U-Pb concordia age of MSWD = 1.3; P = 0.29; Fig. 11b). The remaining 10 4342 Æ 13 Ma (concordance and equivalence matrix apatite analyses have similar 207Pb/206Pb ratios to MSWD = 1.2; P = 0.28; Fig. 11c) is obtained for the six the zircon and baddeleyite grains, equating to 207Pb/206Pb analyses that are less than 10% discordant; however, the ages between 4333 Æ 14 Ma and 4349 Æ 14 Ma 204Pb/206Pb and 207Pb/206Pb ratios of these matrix apatite (Table 3). It was also noted that one of these analyses analyses do not provide sufficient spread to constitute a was an apatite grain within a large symplectite 10-point isochron. The similar ages of the matrix zircon, assemblage (Clast 16, Fig. 3h), similar to the smaller baddeleyite, and apatite mean that it is possible to symplectite assemblages containing the baddeleyite combine all of these analyses into a single weighted grains. If these 10 matrix apatite analyses are considered average 207Pb/206Pb age of 4342 Æ 3Ma 1416 N. M. Curran et al.

Fig. 9. Terrestrial common Pb corrected 207Pb/206Pb ages for the zircon, baddeleyite, and apatite grains in MIL 13317. Weighted average 207Pb/206Pb ages have been indicated for each type of grain. The gray bar and dashed line represent the combined weighted average 207Pb/206Pb age for the matrix zircon, baddeleyite, and apatite grains. Uncertainties on the weighted average ages are stated at the 95% confidence level. (Color figure can be viewed at wileyonlinelibrary.com.)

(MSWD = 0.99; P = 0.47; Fig. 9), or a Pb-Pb isochron 10b), with the merrillite grains forming a separate trend corresponding to an age of 4342 Æ 4 Ma (MSWD below and to the right of the other phases. = 1.14; P = 0.31; Fig. 10f). Apatite analyses were also obtained from two of the DISCUSSION basaltic clasts (six analyses from Clast 4 and one from Clast 10), which give similar 207Pb/206Pb ages (between Miller Range 13317 represents a mixture of lunar 4329 Æ 4 Ma and 4351 Æ 16 Ma) to the majority of the material which is of basaltic, anorthositic, and impact matrix apatite grains. A Pb-Pb isochron age of origin. The ages of the mineral phases (>3.9 Ga) within 4334 Æ 4 Ma (MSWD = 1.02; P = 0.39; Fig. 10e) was the sample provide unique insights into the nature of calculated for Clast 4, although calculating a weighted ancient lunar volcanism. In the following discussion, we average of the 207Pb/206Pb ages (4333 Æ 5 Ma) results synthesize the results of our study to understand MIL in a relatively high MSWD and low probability of fit 13317’s geological history within the context of other (MSWD = 2.2; P = 0.055; Fig. 9). The relatively good lunar meteorites and Apollo samples. statistical fit of the Pb-Pb isochron for apatite in Clast 4 compared with the scatter in 207Pb/206Pb ages may Constraining the Source Region of MIL 13317 reflect an inappropriate common Pb correction, assumed to have a modern terrestrial Pb composition, Due to the regolithic nature of MIL 13317, remote and the grains actually contain a small proportion of sensing chemical data can be used to help locate more radiogenic (when compared with terrestrial Pb) potential source regions on the Moon. Previous work lunar initial Pb (Fig. 10e). has used this approach to constrain the source regions The merrillite grains show a significantly wider range of specific chemical types of lunar rocks (Kramer et al. of Pb isotopic compositions than the apatite, zircon, or 2015) and lunar meteorites (e.g., Gnos et al. 2004; Arai baddeleyite grains, resulting in 207Pb/206Pb ages from et al. 2010a, 2010b; Joy et al. 2010b, 2011c; Calzada- 4277 Æ 12 Ma to 4401 Æ 38 Ma. This is shown on a Diaz et al. 2015; Zeng et al. 2018). Data from the plot of 207Pb/206Pb versus 204Pb/206Pb (Figs. 10a and Lunar Prospector (published in Prettyman et al. 2006), Lunar meteorite Miller Range 13317 1417

Fig. 10. 207Pb/206Pb versus 204Pb/206Pb compositions of all the phases analyzed by SIMS in MIL 13317 (a, b). These data were also used to determine Pb-Pb isochron ages for the zircon (c), baddeleyite (d), and Clast 4 apatite (e) grains. It is possible to construct a single combined isochron (f) through all of the matrix zircon, baddeleyite, and apatite data, assuming that all of these grains originated from the same igneous precursor. PBC = common terrestrial Pb, calculated following the model assumptions of Stacey and Kramers (1975). Uncertainties on the Pb-Pb isochron ages are stated at the 95% confidence level. (Color figure can be viewed at wileyonlinelibrary.com.) 1418 N. M. Curran et al.

which features FeO and Th abundances in bins of 2° equal area per pixel have been used to identify areas of the lunar regolith showing compositional similarities to MIL 13317 (Fig. 12). A range of FeO (9.6–12.3 wt%, Table 1) and Th (4.6–5.4 ppm) was used to account for compositional heterogeneities between sample subsplits. Regions with similar FeO contents to MIL 13317 (red pixels, Fig. 12) are located mainly in the Procellarum KREEP Terrane (PKT) and a few outcrops in the South Pole–Aitken basin region. However, the high-Th content (blue pixels, Fig. 12) constrains MIL 13317 to the near side of the Moon with matches for the Th content only outcropping in the PKT region. The overlap of both the FeO and Th contents of MIL 13317 (green pixels, Fig. 12) occurs only in a few locations in the near side PKT region. These locations, where the FeO and Th content overlaps, are the most likely source regions of MIL 13317. Regions on the Moon that are most similar in composition to MIL 13317 (i.e., the green pixels in Fig. 12), include the northwest region of Oceanus Procellarum, the eastern edge of Mare Frigoris, and to the east and northeast of Mare Nubium. Crater counting data sets from basalt surface units of these two regions (Hiesinger et al. 2003, 2010) indicate that the lava flows are no more than ~3700 Ma. This suggests that if MIL 13317 originates from one of these regions, then the basalt component in MIL 13317 represents ancient cryptomare basalts that were buried by subsequent lava flows and/or impact ejecta within the PKT (e.g., Head and Wilson 1992).

Relationship to Other Lunar Meteorites

Differences to Other Miller Range Lunar Meteorites MIL 13317 is the seventh lunar meteorite found in the Miller Range region of Antarctica to date. Other Miller Range brecciated meteorites include MIL 090036 and the grouped MIL 090034/090070/090075 (MIL 09 group) stones, which are feldspathic regolith breccias grouped on the basis of their chemical composition and petrography (Korotev et al. 2011; Zeigler et al. 2012), and exposure ages (Nishiizumi and Caffee 2013). The lack of basaltic material in the group of MIL 09 samples (Liu et al. 2011; Korotev and Zeigler 2014; Calzada-Diaz et al. 2015; Martin et al. 2017), and low bulk rock Th and KREEP-rich elements suggest that they are unlikely to be source paired with MIL 13317 (supporting information Fig. S5a). MIL < Fig. 11. U-Pb concordia diagrams for data that are 10% 090036 is chemically distinct from MIL 13317, discordant in the zircon (a), younger matrix apatite (b), and older matrix apatite (c) grains in MIL 13317. Uncertainties on as it is more feldspathic (27.1 wt% Al2O3, 5.0 wt% FeO the concordia ages are stated at the 95% confidence level and —Korotev and Zeigler 2014: compared to MIL include the decay constant errors. (Color figure can be viewed 13317 from this work with 15.9 wt% Al2O3, 12.3 wt% at wileyonlinelibrary.com.) FeO) and has no basaltic material (Fig. S5a) (Liu et al. Lunar meteorite Miller Range 13317 1419

Fig. 12. Identification of lunar regolith with compositional similarities to MIL 13317. Compositional matches are FeO = red, Th = blue, and for both FeO and Th = green. The data here show the MIL 13317 is most compositionally similar in terms of surficial FeO and Th to the PKT terrane, with Mare Frigoris, southeast region of the PKT, or the northwest region of Oceanus Procellarum the most compositionally similar regions. Data are overlaid on Clementine albedo images of the Moon in a cylindrical projection. (Color figure can be viewed at wileyonlinelibrary.com.)

2011; Korotev and Zeigler 2014; Calzada-Diaz et al. Pre-Nectarian age lithics and mineral fragments (Arai 2015; Martin et al. 2017). Similar to MIL 13317, the et al. 2010a, 2010b; Joy et al. 2011a). However, MIL 07006 stone is a regolith breccia that contains pyroxene in basaltic clasts of NWA 4472 are generally basaltic clasts (Korotev et al. 2009; Liu et al. 2009; Joy more Mg-rich and Fe-poor (~25>Mg#<65; Joy et al. et al. 2010a; Robinson et al. 2012). However, MIL 2011a) than the basaltic clast in MIL 13317 07006 basalts are much more Mg-rich, Ti-depleted, (~0>Mg#<60). Therefore, we discount the possibility of and KREEP-poor (e.g., Th = 0.36 ppm, Fig. S5b) a source-pairing relationship between these two compared to MIL 13317, ruling out a pairing meteorites. relationship. Concentrations of Sc and Sm in the MIL 13317 Miller Range 13317 is petrographically similar to fusion crust are similar to those in Th-rich meteorites the mingled anorthositic and basaltic regolith breccia like Calcalong Creek and Lynch 002 (Fig. 5f). Meteorite Hills (MET) 01210, which is grouped with Calcalong Creek (Hill et al. 1991; Hill and Boynton MIL 05035 (as well as Yamato-793169 and Asuka- 2003) and Lynch 002 (Smith et al. 2012; Korotev 2013; 881757, collectively known as the YAMM meteorites: Robinson et al. 2016) are the only lunar meteorites Day et al. 2006; Joy et al. 2008; Arai et al. 2010a, found in Australia (located over 800 km apart from 2010b). MIL 13317 bulk rock Ti compositions are low each other). Although not paired with each other, they (1.0 wt% TiO2, Table 1) like MET (1.53 wt% TiO2; have features in common with MIL 13317. All three Korotev and Zeigler 2014), which is indicative of a very meteorites have a mixed clast assemblage of anorthosite, low-Ti (VLT) to low-Ti source region. However, MIL mare basalts, and KREEP-rich material, and have 13317 has lower FeO (12.3 wt%) and higher K2O comparable Th (~4–5 ppm) and FeO (~9–10 wt%) (0.27 wt%) content than MET (16.4 wt% FeO, contents (Korotev 2018). Calcalong Creek was 0.05 wt% K2O; Korotev and Zeigler 2014). potentially launched from around the edge of the Furthermore, MET 01210 contains agglutinates (Arai Imbrium region (Calzada-Diaz et al. 2015), we et al. 2010a, 2010b), which were not found in MIL suggested a similar region of the Moon for MIL 13317 13317. In summary, we exclude a pairing relationship (Fig. 12). Like MIL 13317, pyroxene in basaltic clasts with any of the other Miller Range lunar meteorites of Lynch 002 show basaltic chemical fractionation found to date. trends typical of VLT to low-Ti mare basalts of the Apollo suite, and the basaltic clasts are rich in silica. Similarity to Th-Rich Brecciated Meteorites These petrographic and compositional similarities may Northwest Africa (NWA) 4472/4485 are KREEP- indicate a source-pairing relationship between Lynch rich lunar regolith breccias (Joy et al. 2011a), which 002 and MIL 13317, although this needs to be tested have incorporated basaltic rock fragments and sampled further by radiogenic and cosmogenic nuclide analysis 1420 N. M. Curran et al.

(e.g., crystallization age, ejection age, terrestrial age, and still require formation of the igneous protolith(s) from trapped and cosmogenic components) of Lynch 002. which the grains originated, prior to this time. Equally, while it is possible that different grains within the Regolith History meteorite breccia matrix originate from different protoliths, the association of the matrix apatite and Miller Range 13317 is a heterogeneous mix of baddeleyite grains with similar symplectite assemblages, phases that have undergone different burial and re- combined with the similarity in their 207Pb/206Pb ages, exposure histories. The few spherules present affirm a suggests that the simplest explanation for the similar ages regolith origin for the sample, but their scarcity suggests identified in the majority of the grains is that they that the parent regolith from which the sample originated from the same igneous protolith. Based on this consolidated was relatively immature (McKay et al. interpretation, the weighted average 207Pb/206Pb age of 1991). 4342 Æ 3Ma(MSWD= 0.99; P = 0.47; Fig. 9), or the The two subsplits analyzed for noble gases have combined Pb-Pb isochron age of 4342 Æ 4Ma sampled different components within MIL 13317: one (MSWD = 1.14; P = 0.31; Fig. 10f) for the matrix zircon, being dominated by a regolith breccia component (MIL baddeleyite, and apatite analyses provides the best 13317,10) and the other (MIL 13317,11b) dominated by a estimate for the crystallization age of the igneous protolith. more fragmental breccia, with smaller amounts of These ages are similar to those reported by Shaulis et al. regolith material (see Fig. S6). Analysis of the two (2016) for matrix phosphate and zircon-bearing phases subsplits of MIL 13317 yields exposure ages that range (4351 Æ 9Ma) in a separate thin section (MIL 13317,5) of from 71 Æ 28 to 2860 Æ 74 Myr (supporting information the same meteorite. The apatite grains within basalt Clast Table S11). The anomalously high argon cosmic ray 4 appear to be slightly younger (an average 207Pb/206Pb exposure durations (2860 Æ 74 and 5652 Æ 159 Myr: age of 4333 Æ 5 Ma and a Pb-Pb isochron age of Table S11) from two of the subsplits, are likely to be a 4334 Æ 4 Ma) than the matrix grains, but are consistent result of the sample being saturated with implanted with Pb-Pb isochron ages (4332 Æ 2 Ma) determined for 40 36 parentless Artr and solar wind implanted Artr.Asa several other basaltic clasts in the MIL 13317 meteorite in result, we cannot adequately correct for the presence of a separate study (Snape et al. 2018). These younger ages these components in these subsplits, which has an effect may indicate that the clasts represent fragments of a 38 on the calculated Arcos. Although the Ne exposure ages separate mafic protolith; however, this is difficult to are generally consistent between subsplits, they are lower confirm given the tight clustering of ages, and the than those obtained from cosmogenic Ar and Xe uncertainties associated with correcting for terrestrial isotopes. This may be explained by partial loss of Ne, Pb contamination. potentially during an impact event. Thus, a cosmic ray The range of Pb isotope compositions in the exposure age of 835 Æ 84 Myr is adopted for MIL 13317 merrillite grains may indicate that the U-Pb system in based on the t126 exposure age, as heavy noble gases are this phase is more easily reset than in apatite. However, less likely to have been affected by shock-related this is contrary to the behavior observed in Ca- diffusional gas loss or subject to large corrections for phosphate minerals in Apollo breccias (e.g., Merle et al. solar wind-derived trapped components. 2014; Snape et al. 2016; Thiessen et al. 2017, 2018), The lithification of MIL 13317 from soil into where breccia formation ages based on consistent breccia components is estimated to be between 207Pb/206Pb ages in both apatite and merrillite phases, 2610 Æ 780 and 1570 Æ 470 Ma (determined from the indicate that the U-Pb system is reset in both phases to 40 36 207 206 Ar/ Artr ratio antiquity indicator). MIL 13317 was a similar extent. Furthermore, the youngest Pb/ Pb consolidated into its current form and exposed to the ages of the merrillite analyses (~4280 Ma) in MIL 13317 cosmic environment for an overall period of 835 Æ 84 are consistent with younger ages reported by Shaulis Myr, where it has experienced a complex history at an et al. (2016) of 4276 Æ 21 Ma for two phosphate grains average depth of ~30 cm. and 4270 Æ 24 Ma for 22 baddeleyite grains, which they interpret as representing the crystallization age of a Implications for the Age Resetting History of MIL 13317 separate basalt lithology. Although the mechanism by which the younger The ages determined from the zircon, baddeleyite, and apatite grain was introduced to the breccia is unclear, it is the majority of the phosphate grains in MIL 13317 notable that the U-Pb age of 3890 Æ 33 Ma is close to provide evidence of ancient lunar volcanism occurring at that determined for the formation of the Imbrium impact or before ~4340 Ma (see also Snape et al. 2018). Although basin in several studies (Gnos et al. 2004; Liu et al. 2011) it is possible that these ages could represent the timing of including analyses of phosphates in breccias from Apollo impact induced resetting of the U-Pb system, this would 12, 14, and 17 (Snape et al. 2016; Thiessen et al. 2017, Lunar meteorite Miller Range 13317 1421

2018). Without precisely knowing the provenance of the of KREEP, feldspathic, and basaltic material with trace meteorite or this particular apatite grain, it is unclear if element characteristics that are distinct from the Apollo this age is (1) indicative of a link with the formation of impact melts. These compositions and petrology are the Imbrium basin, (2) a reflection of the general last generally represented by the mineral grains in the matrix stage of basin formation, or (3) a coincidental which have an affinity to ferroan anorthosite parent intermediate partial resetting age between the original rocks. crystallization of the apatite and a later impact event. As In general, there is an apparent lack of HMS rock discussed earlier, considering the susceptibility of the types in MIL 13317 considering the likely source region. apatite U-Pb system to be reset by impact events, and the The distribution of HMS rocks has been strongly linked observed tendency for phosphate phases analyzed in to an origin in and surrounding the PKT region due to Apollo breccias to be completely reset (e.g., Nemchin their possible association with KREEP-rich material et al. 2009b; Snape et al. 2016; Thiessen et al. 2017, (Snyder et al. 1995; Korotev 2000; Wieczorek et al. 2006). 2018), the third interpretation seems slightly less likely. Similarly, the FANs have been associated with rocks Without a clearer understanding of the Moon’s impact typical of the feldspathic lunar highlands. However, history, and a resolution to the long-standing debate feldspathic lunar meteorites, which represent a more surrounding the potential ~3900 Ma lunar cataclysm global sampling of the feldspathic lunar highlands, (Bottke and Norman [2017] and references therein; generally lack Apollo-like FAN, KREEP, and HMS Morbidelli et al. [2018] and references therein), it is material, and have a feldspathic component that is more difficult to say which of the first two interpretations are magnesian (e.g., the magnesian anorthosites) than the more likely. Apollo FAN suite (Korotev et al. 2003, 2012; Korotev 2005; Zeigler et al. 2012; Gross et al. 2014). This suggests Geological Context and Significance of MIL 13317 that the typical highland rocks and impact melts found during the Apollo missions (e.g., FANs, HMS) may not Petrology and composition of MIL 13317 suggests be globally distributed across the Moon (Gross et al. that the sample is formed from a regolith in which there 2014). The highland components of MIL 13317 are was a mixture of mare-like basaltic material and compositionally more similar to the Apollo highland rock highland anorthositic material, with a minor KREEP suite than typical feldspathic lunar meteorites, supporting component (Figs. 5 and 7). Based on comparisons with this suggestion. remote sensing data (Fig. 12), our best estimate is that the MIL 13317 meteorite is derived from the edge of the Was There a Single Magmatic Source for Basalt PKT on the lunar near side. Assuming this is the case, Clasts in MIL 13317? the mineral and clast chemistry, and age of components Basalt clasts in MIL 13317 provide further insight can provide new information about the geological into the magmatic processes occurring in regions remote evolution of the lunar crust in this region of the Moon. from the Apollo and Luna landing sites, both in terms of composition and basaltic volcanism through time. The What Types of Highland Rocks and Impact Melts Are abundances of Sc and Sm in some bulk clasts (e.g., Clast Distributed in Different Crustal Regions? 18, Fig. 5f) show that these clasts have also incorporated MIL 13317 contains highland igneous rocks and KREEP-rich material and are intermediate to the Apollo impact melt breccias that are mainly associated with the VLT-mare basalts, KREEP-rich basalts, and Apollo FAN suite found at many of the Apollo landing sites. For impact melts (see also Zeigler and Korotev 2016). The example, plots of [Eu/Sm]CI versus Sm in plagioclase can Fe# to Ti# correlations of pyroxene suggest that all the be used to distinguish parent lithologies (Fig. 5d) (Russell basalt clasts appear to be derived from lavas intermediate et al. 2014) and indicates that plagioclase in Clast 5 falls to the Apollo VLT and the low-Ti mare basalt source within the field of lunar anorthosites as sampled by the regions (Fig. 4b; after Arai et al. 1996; Robinson et al. Apollo missions and lunar meteorites. Trace element 2012). Pyroxene in basalt clasts show a typical systematics for plagioclase from granulitic Clast 12 fractionation trend for lunar basalts of increasing Fe# overlap with that of plagioclase from Clast 5 (Eu/ (atomic Fe/Fe + Mg, Fe# of 0.40–0.99) with increasing Eu*=15.83; [La/Sm]CI = 1.77) and are also similar to the Ti# (atomic Ti/Ti + Cr, Ti# of 0.25 to 1) (Fig. 4b). The Apollo FAN suite (Figs. 5c and 5d). Granulitic Clast 14 is Al/Ti ratio can be compared with the Fe# to indicate more similar to magnesian granulite found in feldspathic element partitioning from the parental melt to further lunar meteorites (Treiman et al. 2010; Gross et al. 2014; understand this crystallization trend (Nielsen and Drake Kent et al. 2017) that fall into the compositional gap 1978; Arai et al. 1996). The trends in MIL 13317 basalt between Apollo FAN and HMS (Fig. 7a). Furthermore, clasts show that pyroxene (Fe# 40 to Fe# 46) was first to Clast 9 in particular has sampled material which is a mix crystallize out of the parent melt (Al/Ti ~>3) (Fig. 4c). As 1422 N. M. Curran et al. the melt evolved, plagioclase began to co-crystallize with (e.g., Kodama and Yamaguchi 2005; Morota et al. 2011; pyroxene (Fe# 46 to Fe# 70) and the Al/Ti ratio decreased Kramer et al. 2015; Sato et al. 2017). The discovery of as Al was removed from the melt. An Al/Ti ratio of ~1.5 new types of high-Al basalts suggests that this variety may indicates that Ti was removed from the melt and ilmenite be a more common basalt type than suggested by their co-crystallized with pyroxene and plagioclase, as the Al/Ti relatively low abundances in the Apollo and Luna sample versus Fe# trend flattens out from Fe# 70 and Al, Ti, and collection (Kramer et al. 2015). Fe are all extracted from the melt. At this point, the Outstanding questions relate to how such early parent magma would have had an Fe-enrichment melting is associated with the timing of LMO ilmenite- allowing for a late-stage formation of symplectites. These driven density instabilities and overturn (e.g., Hess and trends support a common igneous origin for the basalt Parmentier 1995; Elkins-Tanton et al. 2002), and the clast in MIL 13317 and suggest that the clasts are role of urKREEP (Apollo 14: e.g., Neal and Kramer comagmatic, and that differences in texture must be 2006) or lack thereof (MIL 13317 and Kalahari 009: caused by slightly different crystallization histories. Terada et al. 2007; Snape et al. 2018) driving this earliest phase of magmatic activity. Terada et al. (2007) Implications for Ancient Lunar Volcanism promoted impact-driven decompression melting as a Based on ages of the Ca-phosphate phases in basalt possible mechanism of such ancient KREEP-poor Clast 4, and the ages determined for the basalt clasts volcanism. However, partial melting of the earliest analyzed by Snape et al. (2018), the basaltic material olivine and pyroxene LMO cumulates during LMO sampled by MIL 13317 is interpreted as having overturn and adiabatic ascent is also feasible (Joy et al. crystallized at ~4330 Ma (Figs. 9–11; Table 3). Thus, 2008; Elkins-Tanton and Bercovici 2014). VLT and low-Ti basaltic volcanism on the Moon The relationship between high-Al abundances in the recorded by lunar meteorites extended across 1.4 billion earliest >4300 Ma volcanism is also intriguing. High-Al years, from ~4330 to ~2930 Ma (recorded by young lunar abundances in Apollo 14 basalts have been modeled via meteorite NWA 032: Borg et al. 2009). The ancient ages assimilation fractional crystallization, where the assimilant of MIL 13317 places it among the oldest suite of lunar was a high-Al granitic component either added during basalt samples, including the Apollo 14 high-Al basalts ascent (Neal and Kramer 2006; Hallis et al. 2014) or via (Taylor et al. 1983; Snyder and Taylor 2001), Apollo 17 thermal erosion of the underlying regolith during the flow KREEP basalts (Nyquist et al. 1975; Shih et al. 1992), of lava across the lunar surface (Hui et al. 2011). However, and the high-Al, VLT lunar meteorite Kalahari 009 both MIL 13317 and Kalahari basalts are KREEP-poor (Terada et al. 2007; Shih et al. 2008; Sokol et al. 2008; (Terada et al. 2007; Snape et al. 2018; this study), and the Snape et al. 2018) (Fig. 13c). Observations from the high-Al component instead could have been contributed Apollo suite (e.g., Nyquist and Shih 1992) indicate a from assimilation of ITE-poor ferroan anorthositic crust. correlation between the age of the basalt and Ti-content, There are challenges with assimilating such refractory with older mare basalts (e.g., Apollo 11 basalts; ~3900 to materials into early lunar VLT/low-Ti mafic magmas 3500 Ma) having higher Ti-content, and the younger (Finnila et al. 1994) during magma chamber storage (Neal basalts (e.g., Apollo 12, ~3400 to 3200 Ma; Luna 24 et al. 1988; Head and Wilson 1992) or dyke conduit ~3200 Ma) having more intermediate to lower Ti-content magma transport (Andrews-Hanna et al. 2013). For (Fig. 13a). Using the method of Robinson et al. (2012), example, magmas must be at a higher temperature than we calculate the parent bulk-rock Ti-contents of basalt the country rock it melts and assimilates: the melting clasts in MIL 13317 to be between 0.14 and 0.32 wt% temperature (solidus) of lunar plagioclase in highland making it a VLT basalt (Fig. 13a), as well as having a rocks (~1250°C: Finnila et al. 1994) is higher than or high-Al content (Fig. 13b; Table 1). MIL 13317 and similar to the liquidus of typical lunar basaltic VLT another ancient high-Al, VLT lunar meteorite Kalahari (~1180°C: Grove and Vaniman 1978) or low-Ti systems 009 (Figs. 13a and 13b) indicate that the most ancient (~1273 to 1222°C: Grove and Bence [1977] and references (>3800 Ma) mare and mare-like basalts in lunar therein). Thus, anorthitic FAN-like plagioclase dissolution meteorites tend to have some of the lowest Ti-contents by a mare basaltic melt might be thermodynamically and highest Al-contents of all lunar sampled basalts challenging. Moreover, on the Moon, FAN host rock (Figs. 13a and 13b; see also Joy and Arai 2013). Further would melt to form a more viscous and denser crystal age dating of basaltic clasts in other lunar meteorites is mush than the basaltic ascending fluid, inhibiting ascent needed to see if this trend is supported across a wider and eruption (Finnila et al. 1994). However, the age geographic distribution of lunar material. However, the overlap between ferroan anorthosite samples, the HMS, observation of the most ancient lunar basalts being low in and ancient basaltic meteorite ages (Figs. 13b and 13c), Ti (<3 wt% TiO2) is also seen in coupled crater counting- suggests that the lunar highlands crust may still have been chemical remote sensing studies of mare basalt regions accumulating and was likely warmer and more ductile at Lunar meteorite Miller Range 13317 1423

Fig. 13. Comparison of MIL 13317 mineral phase ages with (a) lunar basalts TiO2 content (adapted from Joy and Arai 2013), (b) lunar basalt Al2O3 content, and (c) the range in crystallization ages for non-mare ancient highlands rocks and KREEP basalts (see text for references). (Color figure can be viewed at wileyonlinelibrary.com.) 1424 N. M. Curran et al.

~4300 Ma (Elkins-Tanton and Bercovici 2014). Such The basaltic clasts in MIL 13317 provide evidence of elevated crustal thermal conditions may have facilitated ancient (~4340 Ma) VLT, high-Al basaltic volcanism that dissolution (Reiners et al. 1995) of anorthitic plagioclase was not sampled by the Apollo missions, possibly derived from the warm country feldspathic rock. This would allow from cryptomare deposits that were buried by subsequent an Al-rich assimilant to be available in ancient high-Al lava flows and/or impact ejecta. These ancient ages basaltic lava flows. Alternatively, the Hui et al. (2011) suggest that basaltic volcanism, in particular high-Al, model of post-eruption assimilation by a lava flow VLT basaltic volcanism, on the Moon started as early as thermally eroding the underlying KREEP-poor feldspathic 4350 Ma and before the bulk onset of lunar mare glass-rich regolith might be an attractive alternative hybrid volcanism at ~3850 Ma, providing further constraints on magma-surface interaction model. The nature of transport the earliest volcanic activity of the Moon. of basalt magmas through, and onto, hot and cold lunar crust should be explored to better understand ancient Acknowledgments—U.S. Antarctic meteorite samples are basalt petrogenesis (Finnila et al. 1994) and investigate recovered by the Antarctic Search for Meteorites effects of how crustal assimilation could mask isotopic (ANSMET) program, which has been funded by NSF signatures of mantle sources (Reiners et al. 1995) in such and NASA, and characterized and curated by the ancient basalts. Department of Mineral Sciences of the Smithsonian Institution and Astromaterials Curation Office at NASA Johnson Space Center. We thank Julia Cartwright, James SUMMARY Day, and two anonymous reviewers for providing helpful reviews on an earlier version of the manuscript and Miller Range 13317 is a mingled regolith breccia of Timothy Jull for editorial handling. We thank Jon lunar origin comprised of fragments of basalts, impact Fellows (University of Manchester) for assistance with melts, and feldspathic material (including clasts with an the ESEM and EMP analyses, and John Cowpe for noble affinity to the Apollo FANs). It is one of a handful of gas expertise. We acknowledge the Science and lunar meteorites available that have sampled ancient Technology Facilities Council (PhD studentship to > ( 3800 Ma) basaltic volcanism. It is distinct from any Natalie Curran and consolidated grants ST/M001253/1 of the other lunar meteorites collected to date and there and ST/R000751/1) and Royal Society (UF140190) for is no substantial evidence that MIL 13317 is paired with funding. Joshua Snape, Alexander Nemchin, and Martin any other Th-rich lunar meteorite, although further Whitehouse acknowledge grant funding from the Knut investigation is needed on Lynch 002 to confirm this. As and Alice Wallenberg Foundation (2012.0097) and the a result, MIL 13317 provides new perspectives on the Swedish Research Council (VR 621-2012-4370). The diversity of rocks on the lunar surface, and in particular NordSIMS facility operates as a Swedish-Icelandic lunar volcanism through time. MIL 13317 shows a infrastructure, supported by the Swedish Research complex regolith history with a range in trapped and Council, the University of Iceland, and the Swedish cosmogenic noble gas isotope concentrations. However, Museum of Natural History, of which this is publication all parts of the meteorite have resided in the top 595. We also thank Randy Korotev (Washington millimeter of the lunar surface at some point in history, University) for his informative Lunar Meteorite List, and where trapped gases from the solar wind and lunar Chuck Meyer (JSC) and Kevin Righter (JSC) for the 40 36 atmosphere were acquired. The ( Ar/ Ar)tr antiquity Apollo and Lunar meteorite compendiums. indicator suggests that compaction from the parent soil Æ into breccia components occurred between 2610 780 Editorial Handling—Dr. A. J. Timothy Jull and 1570 Æ 470 Ma, which closed the fragments off from further space weather processes. MIL 13317 then REFERENCES experienced exposure to the cosmic environment for a period of approximately 835 Æ 84 Myr, where it resided Anders E. and Grevesse N. 1989. Abundances of the elements: in the regolith at an average depth of 30 cm. Meteoritic and solar. 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SUPPORTING INFORMATION 2018) with the fusion crust data for MIL 13317 (Table 1). Note the log scale for the Th concentrations. Additional supporting information may be found in Fig. S6. Chips of Miller Range 13317,10 and Miller the online version of this article: Range 13317,11. Subsplits from both chips were used Data S1. Analytical techniques. for noble gas analyses. A polished block was made of Fig. S1. Backscattered electron images of grains MIL 13317,11b. MIL 13317,10 represents a regolith used in SIMS U-Pb dating work. Image directory and dominated chip and MIL 13317,11 represents a large corresponding data for each grain analysis can be found brecciated basaltic clast. in Table S3. Zirc = zircon; badd = baddeleyite; Table S1. Summary and types of analysis conducted phos = phosphate. on clasts in MIL 13317,7 and MIL 13371,11a. Fig. S2. Thin section images of MIL 13317 in plain Table S2. Trace elements abundances (ppm) for polarized light (ppl) and crossed polarized light (xpl). clasts and matrix minerals and bulk compositions in Fig. S3. Cathodoluminescence images of basalt MIL 13317,7. Errors are 1r SD from the averages of Clast 1 in Miller Range (MIL) 13317,7. Unshocked several measurements (number of analysis displayed in regions of the plagioclase grains show up as yellow. brackets with the mineral, where px = pyroxene and Plagioclase regions that are shocked show up as deep plag = plagioclase). red-purple. Table S3. U-Pb isotope data for phases (zircon, Fig. S4. 134Xe/132Xe versus 136Xe/132Xe for MIL baddeylites, apatites, merrillites) in MIL 13317,7 13317,10. The data for MIL 13317,10 plot in the solar determined by SIMS analysis. dominated region with the 238U, 235U, and 244Pu Table S4. Plagioclase compositional summary data endmembers plotting far off to the right of the plot. for MIL 13317,7 and MIL 13317,11a. Fig. S5. a) Comparison of FeO (wt%) versus Al2O3 Table S5. Olivine compositional summary data for (wt%) showing the fusion crust composition for MIL MIL 13317,7. 13317,7. MIL 13317 is compared to other Miller Range Table S6. Pyroxene compositional summary data and the YAMM group of basaltic meteorites (data from for MIL 13317,7 and MIL 13317,11a. Korotev and Ziegler 2014). MIL 13317 is also Table S7. Fusion crust and vein compositional compared to another Th-rich meteorite Calcalong Creek summary data for MIL 13317,7. (Hill and Boynton 2003) and Kalahari 009. b) FeO Table S8. Bulk values and averages of compositional (wt%) versus Th (ppm). Plot shows a comparison of data for fine-grained clast in MIL 13317,7. lunar meteorite (blue dots and markers) and Apollo and Table S9. Summary and raw data of Neon and Luna soils (represented by the colored fields, Korotev Argon noble gas data for bulk rock chips of MIL 1430 N. M. Curran et al.

13317,10 and MIL 13317,11b. Raw data include blank include blank corrected and mass spectrometer corrected and mass spectrometer sensitivity corrected sensitivity corrected data. Errors are to 1r. data. Errors are to 1r. Table S11. Summary of endmember noble gas Table S10. Summary and raw data of Xenon noble components, production rates, cosmic ray exposure ages, gas data for bulk rock chips of MIL 13317,10. Raw data and antiquity ages in MIL 13317,10 and MIL 13317,11b.