Journal of Geophysical Research: Planets Supporting Information for Magnetism of a Very Young Lunar Glass Jennifer Buz1*, Benjamin P. Weiss1, Sonia M. Tikoo2,3, David L. Shuster2,3, Jérôme Gattacceca4, Timothy L. Grove1 1Department of Earth, Atmospheric, and Planetary Sciences, Massachusetts Institute of Technology, Cambridge, MA 02139, USA, 2Department of Earth and Planetary Science, University of California, Berkeley, CA 94720, USA., 3Berkeley Geochronology Center, Berkeley, CA 94709, USA, 4CNRS, AixMarseille University, CEREGE UM 34, Aix-en-Provence, France, *Now at: Division of Geological and Planetary Sciences, California Institute of Technology, Pasadena, CA 91125 Contents of this file Text S1 to S2 Figures S1 to S9 Tables S1 to S5 Additional Supporting Information (Files uploaded separately) Dataset S1 Introduction This supporting information provides additional details on hysteresis, VRM, PRM, geoand thermochronometry experiments. Demagnetization data for all samples are included in the supplementary figures if not in the main text. Additional elucidating figures and tables are also provided. Demagnetization data is provided in the supplementary dataset. 1 Text S1. Rock Magnetism of 12017 1.1 Hysteresis Hysteresis loops were measured on a single sample of each the 12017 basalt and glass lithologies using a Princeton Instruments MicroMag vibrating sample magnetometer at CEREGE, Aix-en-Provence, France. Hysteresis data are shown in Fig. S1. Magnetic hysteresis parameters are reported in Tikoo et al [2012]. Using the hysteresis data with the diamagnetic and paramagnetic contributions subtracted, we estimated the saturation remanence, saturation magnetization, and coercivity. The ratios of saturation remanence to saturation magnetization (Mrs/Ms) for basalt and glass are 5.05×10-3 and 3.89×10-3, respectively. The mass normalized Ms are 0.14 Am2/kg and 0.68 Am2/kg for the basalt and glass, respectively. The ratios of remanent coercive force to coercive force (Hcr/Hc) are 17.5 and 5.67 for basalt and glass, respectively. Using these parameters as well as the coercivity of remanence determined from back field IRM experiments, we find that both lithologies are dominated by multidomain grains. 1.2 VRM A possible source of magnetization for 12017 is viscous remanent magnetization (VRM) from exposure to the Earth’s magnetic field for 40 years at ambient temperatures. To estimate the possible contribution of VRM on the magnetization of the samples, we placed basalt sample 13B in the Earth’s magnetic field for 2 weeks and we placed glass sample 12B in an artificial bias field of 0.2 mT generated by a coil inside our shielded room for 21 hours. Upon removal of the applied field, we acquired continuous measurements of the magnetization of the samples as they viscously relaxed in our shielded room (< 200 nT) over the following two weeks. To estimate lower and upper bounds on the amount of possible VRM acquired since arrival on Earth, we fit both linear and exponential curves to the VRM decay data, respectively (Fig. S2). We extrapolated the acquired remanence out to 40 years (approximate residence time on Earth) and subtracted the decay time from being in our shielded room (approximately 1 year). Linear fits suggest that VRM can account for 1.95% and 0.5% of the basalt and glass NRM, respectively, and 1.7% and 1.8% of the LC component. Exponential fits suggest that VRM can account for 10% and 11% of the basalt and glass NRM, respectively, and 21% and 34% of the LC component. These are actually all upper limits since they assume that the samples were stationary in the Earth’s field over the last 40 years. 1.3 PRM It is possible that the glass or basalt could have acquired a shock remanent magnetization (SRM) from a meteoroid impact. It is important to consider this because SRM is capable of recording very short lived fields like putative impact-plasma generated fields [Crawford and Schultz, 1999]. To assess this possibility, we imparted a laboratory pressure remanent magnetization (PRM) (as an analog for SRM) on basalt sample 12A2 following the methods of Gattacceca et al. [2010]. We immersed sample 12A2 in polyethilsiloxane fluid to facilitate hydrostatic pressurization. We then put the capsule containing the sample and fluid into a nonmagnetic pressure cell and raised the pressure to 1.8 GPa. While maintaining this pressure for a minimum of 1 minute, we applied a field of 800 μT using a coil wrapped around the cell. The field was then turned off, the 1 pressure removed over the course of a minute, and the sample subjected to a full AF demagnetization sequence. A comparison of demagnetization of PRM with NRM is shown in Figs. S5 and S7. Almost all of the magnetization acquired via PRM was removed in the first AF step (20 mT), suggesting that even the LC component is too hard to be explained as an SRM. Text S2. 40Ar/39Ar and cosmogenic 38Ar geochronology analytical details Two basalt aliquots of 12017 and a single aliquot of 12017 impact glass were sequentially degassed to conduct 40Ar/39Ar geochronometry at the Berkeley Geochronology Center following previously published procedures [Shea et al., 2012; Shuster et al., 2010]. The basalt samples were placed into aluminum discs alongside Hb3gr neutron fluence monitors and were irradiated for 100 hours, and the glass aliquot was irradiated for 1 hour alongside ACs fluence monitors, at the Oregon State University TRIGA reactor in the Cadmium-Lined In-Core Irradiation Tube (CLICIT) facility. After irradiation, aliquots (~1 mg) of the irradiated basalt and glass were placed into small metal tubes of high purity Pt-Ir alloy and incrementally degassed using feedbackcontrolled laser heating with a 30 W diode laser (wavelength of 810 ± 10 nm) equipped with a coaxially aligned optical pyrometer. The single-color pyrometer was calibrated against a type-K thermocouple under high vacuum (<10-8 torr) and under the same conditions as the degassing analyses to correct for the temperature dependent emissivity of the Pt-Ir tubes. During sequential degassing, the samples were first held under static vacuum at a controlled temperature to within ± 10°C for 600 s (Table S1). The extracted Ar was then purified using one hot and one cold SAES® GP-50 getter pump fitted with C-50 cartridge (St101 alloy). All five isotopes of Ar were analyzed with a Mass Analyzer Products 215c mass spectrometer using a single Balzers SEV-217 discrete dynode electron multiplier. Corrections for interfering nuclear reaction products [Renne et al., 2005], 37Ar and 39Ar decay, spectrometer discrimination, and extraction line blanks were applied to the measured signals. Apparent 40Ar/39Ar ages were calculated relative to the Hb3gr standard (1081 Ma) or the ACs standard (1.206 Ma) using the decay constants and standard calibration of Renne et al. [2011], and isotope abundances of Steiger and Jäger [1977]; corrections for trapped or cosmogenic 40Ar were not applied. The apparent cosmogenic 38 Ar exposure ages of each degassing step were calculated from the ratio of cosmogenic 38 Ar to reactor-produced 37Ar and 39Ar following the procedures described in Shuster and Cassata [2015] and using the 38Ar production rate from Ca [Turner, 1971]. In this case, the production of 38Arcos from Ti, Cr, Mn, Fe, and Ni was ignored; therefore, calculated exposure ages represent upper bounds on the true surface exposure. Full datasets, isotopic corrections, neutron irradiation parameters, and calculated step ages (both 40 Ar/39Ar and cosmogenic 38Ar) for the whole-rock and glass aliquots appear in Table S1. For the analysis of impact glass, extractions that yielded Ar abundances below the detection limit are excluded for clarity. The whole-rock analyses are shown as release spectra, along with the apparent Ca/K ratios, in Fig. 7. 2 Figure S1. Hysteresis data for 12017. A) Basalt subsample 12A2. B) Glass subsample 12B. Large plots at left show hysteresis loops corrected for high-field (0.95-1 T) paramagnetic slope while the smaller plots at right show the uncorrected data. 3 Figure S2. VRM decay experiments for 12017. (A) Basalt subsample 13B1. (B) Glass subsample 12B. Black lines indicate exponential fits while red lines indicate linear fits. 4 5 Figure S3. Subsampling and orientation of 12017. A) Whole rock 12017 prior to subdivision at Johnson Space Center (JSC). Underlying basalt is light gray and glass splatter is shiny black. Approximate locations of subsamples used in this study are indicated. NASA photo S70-44098. B) Illustration of saw cuts made at JSC during sample processing, adapted from Lunar Sample Compendium [Meyer, 2005]. We used these drawings to reconstruct how our allocated subsamples were mutually oriented. C) Orientation of final subsamples used in this study. Subsamples 12A1A, 12A1B, and 59B were not used in this study. The JSC and MIT coordinate systems are shown with unprimed and primed labels, respectively, in (B) and (C). Figure S4. Geologic setting of 12017. A) Lunar Reconnaissance Orbiter Wide Angle Camera (LROC-WAC) photograph of the Apollo 12 landing site. Selected craters and the small mound where sample 12017 was thought to have been collected are labeled. B) Astronaut photograph (AS12-46-6825HR) of small mound where sample 12017 was retrieved (sample is not identifiable in the photograph). Scale bar is estimated from the Apollo transcripts. 6 Figure S5. Petrographic constraints on cooling rate of 12017 basalt from Grove and Walker [1977]. Early and late stage cooling of the 12017 basalt based on plagioclase width and pyroxene density are 0.30°C/hr and 0.35°C/hr, respectively. See Fig. 1 for examples of plagioclase and pyroxene. 7 Figure S6. More examples of AF demagnetization over the coercivity range of the LC component. Shown is a two-dimensional projection of the NRM vectors during progressive sanding stages. Solid symbols represent the end points of magnetization projected onto the horizontal N-E planes, and open symbols represent projections onto the vertical U-E planes. All samples except sample 13B show removal of one or more LC components. Sample 59A likely has two LC components, indicated by the grey arrows. Red symbols indicate moment measurement following final sanding of the 8 parent sample for each subsample show here and scaled in intensity to the mass of the subsample relative to its parent sample. These directions differ from the AF 0 mT measurements because of the additional subsampling that occurred prior to beginning AF demagnetization. Figure S7. Comparison of AF demagnetization behavior of the NRM to that of different laboratory-induced magnetizations over the coercivity range of the LC component. (Left) 12A2 basalt subsample demagnetization normalized to the pre-AF moment. (Right) 12B glass subsample demagnetization normalized to the pre-AF moment. 9 Figure S8. More examples of AF demagnetization of 12017 over the HC range. Shown is a two-dimensional projection of the NRM vectors during progressive sanding stages. Solid symbols represent the end points of magnetization projected onto the horizontal NE planes, and open symbols represent those projected onto the vertical U-E planes. Note the lack of any consistent moment or directional changes with successive AF steps. 10 Figure S9. Comparison of AF demagnetization behavior for different magnetization types over the coercivity range of the HC magnetization. (Left) 12A2 basalt subsample normalized to the moments after demagnetization to 6.5 mT. (Right) 12B glass subsample normalized to the moments after demagnetization to 8.5 mT. 11 12 Isotope abundances given in nanoamps (spectrometer sensitivity is ~1.4×10-14 mols/nA), and corrected for 37Ar and 39Ar decay, half lives of 35.2 days and 269 years, respectively, and for spectrometer discrimination per atomic mass unit of 1.004535 ± 0.002968. Isotope sources calculated using the reactor constants in Renne et al. [1998], assuming (38Ar/36Ar)cos = 1.54, (38Ar/36Ar)trap = 0.188, and (40Ar/36Ar)trap = 0. No corrections were made for cosmogenic 40Ar. Ages calculated using the decay constants and standard calibration of Renne et al. [2011] and isotope abundances of Steiger and Jäger [1977] and calculated relative to Hb3gr fluence monitor (1081 Ma) and relative to ACs fluence monitor (1.206 Ma), for basalt and glass, respectively. J-Values are 0.0262509 ± 0.0002064 and 0.000272 ± 0.000008, for basalt and glass respectively. Corrections were made for reactor produced 38Ar and 36Ar in age calculations. Average analytical blanks are: 40Ar = 0.015; 39Ar = 0.0001; 38Ar = 0.00002; 37Ar = 0.0001; 36Ar = 0.00007 (nanoamps). Temperature was controlled with approximately ± 10 ºC precision and ± 10 ºC accuracy; each heating duration was 600 seconds. The apparent 38Ar exposure ages are calculated for production only from Ca and K, so represent upper bounds. Table S1. Argon Analytical Details. # Lithology P Ni S Fe Total 1 Glass 0.16 0 0.11 16.53 16.80* 2 Glass 2.53 1.28 0.02 96.21 100.04 3 Glass 8.22 1.97 0.39 88.58 99.16 4 Glass 4.18 1.45 0.38 93.35 99.36 5 Glass 7.44 1.52 9.70 80.39 99.05 1 Basalt 0.01 0 0.25 98.99 99.25 2 Basalt 0.01 0 0.06 98.93 99.00 3 Basalt 0.02 0.79 0.01 97.58 98.40 4 Basalt 0.02 0.78 0.01 99.45 100.28 Note: The first column lists the spot number corresponding to Fig. 2, the second column lists the lithology hosting the metal grain. The second through fourth columns contain the concentrations in wt.% of P, Ni, S, and Fe, respectively. The fifth column contains the sum the previous four columns. Measurements were acquired with a JEOL-JXA-8200 at the Massachusetts Institute of Technology electron microprobe facility. *The low mass percentage total for this spot is likely due to the small size (<1 µm) of this metal grain. The remaining majority of the mass is likely from Si and O from the surrounding glass. Table S2. Wavelength dispersive spectroscopy analyses of metal grains in 12017. 13 Sample Basalt 12A 12A2 12A1C 13B* Glass 12B 13A 13A1 13A2 59A** Mass (mg) Type Range (mT) N Dec (°) Inc (°) 503 183 Sanding LC HC LC HC Sanding LC MC HC NRM-8.5 8.5-69 NRM-8.0 8.0-64 NRM-11.5 12.0-54.0 54-80 6 17 77 15 74 13 22 66 27 249 294.5 145.7 239.9 127.0 135.6 263.8 121.0 144.9 -38.8 33.7 48.1 81.0 42.6 36.2 -17.4 -70.7 26.9 Sanding LC HC Sanding LC HC LC HC LC1 LC2*** HC n/a NRM-8.5 9-85 n/a NRM-7 7.5-85 NRM-8.5 8.5-85 NRM-4.5 5.0-9.0 9.5-39 5 16 75 14 13 106 16 104 7 9 56 348.8 277.8 346.8 4.8 302.8 209 269.9 206.4 180 303.6 146.5 66.2 24.7 -65.1 -7.6 16.8 17.7 21.1 -78.6 -11.4 -3.9 74.6 104.3 131.6 27.1 132.9 69.9 49.5 15 DANG (°) 127.1 74.26 151.6 132.1 124.6 146.6 91.01 133.7 38.5 129.7 159.6 106.2 52.51 91.63 110.9 114.5 MAD (°) 27.2 12.0 37.1 11.0 35.3 23.3 36.3 35.4 34.0 24 9.8 31.8 27.2 6.1 34.9 14.0 30.0 9.4 15.8 45.5 Pass? N N N N N N N N N N N N N N N N Forced ? No No Yes No Yes No No No Yes No No Yes No No Yes No Yes No No Yes Note: The first column contains sample and subsample names. Subsamples are listed as indented sample names under their parent sample. The second column shows the mass of each subsample. The third column designates whether the row describes the low coercivity (LC), medium (MC), or high coercivity (HC) components of magnetization in the sample. The fourth column contains the AF field values bounding the components identified for each subsample. The fifth column shows the number of points (i.e., AF steps) used in the PCA calculation for each component. Columns 6-9 show the mean declination, mean inclination, DANG, and the MAD, respectively, for each component. The tenth column indicates whether the component passed the DANG/MAD test. The eleventh column indicates whether the component was forced through the origin during the PCA calculation. *In Tikoo et al. [2012] sample 13B was referred to as sample 13b1. **In Tikoo et al. [2012] sample 59A was referred to as sample 59. ***In Tikoo et al. [2012] component LC2 was referred to as MC. Table S3. NRM components. Sample Starting Mass (mg) Ending Mass (mg) % Difference 12A 503.7 492.5 2.3 12B 32.2 29.7 7.7 13A 150.7 149.0 1.1 13B 167.2 152.1 9.0 Note: A ~20 mg flake of glass was chipped from 13B post-sanding. Table S4. Mass changes throughout sanding. 14 Sample Basalt 12A2 12A1C Glass 12B 13A2 Comp ARM slope IRM slope 0.05 mT 0.2 mT 0.6 mT LC 2.71 ± 1.55 1.03 ± 0.19 0.45 ± 0.08 HC 0.13± 0.13 0.12 ± 0.06 LC 1.53 ± 0.64 HC ARM paleointensity (μT) IRM 0.05 mT 0.2 mT 0.6 mT Paleoint (μT) 0.057 ± 0.0062 101.1 ± 57.8 153.73 ± 28.35 201.4 ± 35.82 171 ± 18.6 0.05 ± 0.03 0.0044 ± 0.003 4.104 ± 4.85 16.41 ± 8.95 22.38 ± 13.43 13.2 ± 9 0.9 ± 0.13 0.5 ± 0.08 - 57.08 ± 23.88 134.32 ± 19.40 223.88 ± 35.82 - 0.14 ± 0.17 0.08 ± 0.09 0.03 ± 0.06 - 5.223 ± 6.34 11.94 ± 13.43 13.43 ± 26.86 - LC 3.93 ± 1.24 1.11 ± 0.11 0.33 ± 0.04 0.986 ± 0.11* 146.6 ± 46.26 165.67 ± 16.41 147.76 ± 17.91 HC 0.17 ± 0.07 0.05 ± 0.02 0.02 ± 0.01 0.004 ± 0.001* 6.343 ± 2.61 7.46 ± 2.98 8.95 ± 4.47 13.03 ± 3.94 LC 0.85 ± 0.86 0.39 ± 0.19 0.14 ± 0.06 0.007 ± 0.003* 31.71 ± 32.08 58.20 ± 28.35 62.68 ± 26.86 22.05 ± 8.40 HC 0.24 ± 0.04 0.10 ± 0.01 0.04 ± 0.01 0.002 ± 0.0003* 8.955 ± 1.49 14.92 ± 1.49 17.91 ± 4.47 7.20 ± 0.99 295.8 ± 33.3 Note: The first column lists subsample numbers. The second column designates whether the paleointensity experiment was conducted for the low coercivity (LC) component, high coercivity (HC) component, or a magnetization component defined by AF steps of 23-85 mT in the sample. The third, fourth, and fifth columns show ΔNRM/ΔARM values computed from paleointensity slope fits to the associated AF range using ARM acquisition with 0.05 mT, 0.2 mT, and 0.6 mT DC bias fields, respectively. The sixth column shows ΔNRM/ΔIRM values computed from paleointensity slope fits to the associated AF range. All data reported are in the format slope ± 95% formal confidence radius from Student’s t-test. The final four columns indicate the calculated paleointensity using f’ = 1.34 and a = 3000. The first six columns are reproduced from Tikoo et al. [2012]. The quoted uncertainties in the third through eight columns only represents that associated with the linear regression and does not take into account systematic uncertainties associated with the unknown values of a and f’. *Tikoo et al. [2012] incorrectly reported IRM paleointensities for subsample 12B as belonging to 13A2. They have been corrected here. Table S5. Paleointensity Values. Data Set S1. NRM AF Demagnetization data. 15 References Crawford, D. A., and P. H. Schultz (1999), Electromagnetic properties of impactgenerated plasma, vapor and debris, Int. J. Impact Eng., 23, 169-180, doi:10.1016/S0734743X(99)00070-6. Gattacceca, J., M. Boustie, L. Hood, J. P. Cuq-Lelandais, M. Fuller, N. Bezaeva, T. de Resseguier, and L. Berthe (2010), Can the lunar crust be magnetized by shock: Experimental groundtruth, Earth Planet. Sci. Lett., 299, 42-53, doi:10.1016/j.epsl.2010.08.011. Grove, T. L., and D. Walker (1977), Cooling histories of Apollo 15 quartz-normative basalts, in Proceedings of the Eighth Lunar Science Conference, p. 1501-1520, Pergamon Press, Inc., New York. Meyer, C. (2005), Lunar sample compendium (online), 6, <http://curator.jsc.nasa.gov/Lunar/lsc/index.cfm>. Renne, P. R., G. Balco, K. R. Ludwig, R. Mundil, and K. Min (2011), Response to the comment by WH Schwarz et al. on "Joint determination of 40K decay constants and 40 Ar/40K for the Fish Canyon sanidine standard, and improved accuracy for 40Ar/39Ar geochronology", Geochim. Cosmochim. Acta, 75, 5097, doi:10.1016/j.gca.2011.06.021. Renne, P. R., K. B. Knight, S. Nomade, K.-N. Leung, and T.-P. Lou (2005), Application of deuteron-deuteron (D-D) fusion neutrons to 40Ar/39Ar geochronology, Applied Radiation and Isotopes, 62, 25-32, doi:10.1016/j.apradiso.2004.06.004. Renne, P. R., C. C. Swisher, A. L. Deino, D. B. Karner, T. L. Owens, and D. J. DePaolo (1998), Intercalibration of standards, absolute ages and uncertainties in 40Ar/39Ar dating, Chemical Geology, 145, 117-152, doi:10.1016/S0009-2541(97)00159-9. Shea, E. K., B. P. Weiss, W. S. Cassata, D. L. Shuster, S. M. Tikoo, J. Gattacceca, T. L. Grove, and M. D. Fuller (2012), A long-lived lunar core dynamo, Science, 335, 453-456, doi:10.1126/science.1215359. Shuster, D. L., G. Balco, W. S. Cassata, V. A. Fernandes, I. Garrick-Bethell, and B. P. Weiss (2010), A record of impacts preserved in the lunar regolith, Earth Planet. Sci. Lett., 290, 155-165, doi:10.1016/j.epsl.2009.12.016. Shuster, D. L., and W. S. Cassata (2015), Paleotemperatures at the lunar surfaces from open system behavior of cosmogenic 38Ar and radiogenic 40Ar, Geochim. Cosmochim. Acta, 155, 154-171, doi:10.1016/j.gca.2015.01.037. Steiger, R. H., and E. Jäger (1977), Subcommission on geochronology: convention on the use of decay constants in geo-and cosmochronology, Earth Planet. Sci. Lett., 36, 359362, doi:10.1016/0012-821X(77)90060-7. 16 Tikoo, S. M., B. P. Weiss, J. Buz, E. A. Lima, E. K. Shea, G. Melo, and T. L. Grove (2012), Magnetic fidelity of mare basalts and implications for a lunar dynamo, Earth Planet. Sci. Lett., 337-338, 93-103, doi:10.1016/j.epsl.2012.05.024. Turner, G. (1971), Argon 40- argon 39 dating: The optimization of irradiation parameters, Earth Planet. Sci. Lett., 10, 227-234, doi:10.1016/0012-821X(71)90010-0. 17