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1 1 Data Repository Item The formation of high 18 O fayalite-bearing A-type granite by high temperature melting of granulitic metasedimentary rocks, South China Hui-Qing Huang 1, 2, 3, Xian-Hua Li 4, Wu-Xian Li 1, Zheng-Xiang Li 2 1 Key Laboratory of Isotope Geochronology and Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou , China 2 The Institute for Geoscience Research (TIGeR), Department of Applied Geology, Curtin University, GPO Box U1987, Perth, WA 6845, Australia 3 Graduate School of Chinese Academy of Sciences, Beijing, , China 4 State Key Laboratory of Lithospheric Evolution, Institute of Geology and Geophysics, Chinese Academy of Sciences, Beijing , China Supplementary Materials: Analytical procedures and results

2 2 Figure DR1 Figure DR1. Geochemical plot of Zr + Ce + Nb + Y vs. 10,000 * Ga/Al showing that the Jiuyishan suite is typical A-type granite (after Whalen et al., 1987). The data are as listed in Table DR2. The two samples selected for zircon studies are highlighted (filled circles).

3 3 Figure DR2 Figure DR2. Ion microprobe zircon U-Pb concordia age plots for A: 17-6 and B: The sample 17-6 is a coarse-grained granodiorite, whereras the sample 18-1 is a porphyritic subvolcanic rock containing plagioclase and quartz as the main phenocrysts. The data are as listed in Table DR4.

4 4 Figure DR3 Figure DR3. Plots of A: Rb vs.sr and B: Ba vs. Sr for the Jiuyishan suite (circles). The data are as listed in Table DR2. The two samples selected for zircon studies are highlighted (filled circles). Data from contemperaneous mantle-derived rocks (triangles) are shown for comparison. The data are from Jiang et al. (2009), Li et al. (2004a), and Wang et al. (2003).

5 5 Figure DR4 Figure DR4. A plot of Nd(t) vs. Initial 87 Sr/ 86 Sr showing the isotpe composition of the Jiuyishan suite (circles). Samples chosen for in-situ zircon study are shown as filled circles. The data are as in Table DR3. Data from contemperaneous mantle-derived rocks (triangles) are shown for comparison. The data are from Jiang et al. (2009), Li et al. (2004a), and Wang et al. (2003). Figure DR5 Figure DR5. Chondrite normalized rare earth element pattern for the Jiuyishan granites (30 samples in total). The data are as listed in Table DR2. The normalization values are from Sun and McDonough (1989).

6 6 Analytical Procedures: 1. Mineral chemistry of olivine and orthopyroxene Analyses of minerals on carbon-coated thin sections were carried out at GIG (Guangzhou Institute of Geochemistry, Chinese Academy of Sciences (Guangzhou)) with a JEOL JXA Superprobe. The electron beam was 1 2 m with accelerating voltage of 15 kv at 10 na beam current. Standards olivine (for Si and Mg), magnetite (for Fe) and garnet (for Ca and Al) were used for olivine analyses. Standards employed for orthopyroxene are different. Only diopside (for Si, Ca, Mn, Mg and Fe) and jadeite (for Al, Na and K) were used. Cr 2 O 3 and rutile were applied for Cr and Ti, respectively for both minerals. The data reduction was carried out using ZAF correction. The results are listed in Table DR1. 2. Major and trace elements Sample powders small than 200 mesh were dried at 105. After loss on ignition (LOI) determination, ca. 50 mg of the cauterants were then fused with the aid of lithium tetraborate, at a ratio of 1:9, to produce glass discs. The discs were later on analyzed by Rigaku RIX 2000 X-ray fluorescence spectrometry (XRF) at GIG for major elements. Samples and standards GSP-2, RGM-1, and AGV-2 were dissolved in pressured Teflon bombs using a heated HF + HNO3 mixture. The solutions were dried and re-dissolved with 2% HNO3 for testing. Trace elements were measured using an Agilent 7500a quadruple ICPMS (inductively coupled plasma mass spectrometry) at the Institute of Geology and Geophysics, Chinese Academy of Sciences (Beijing) (IGG). The signal drift of the spectrometer was monitored by an internal standard Rh solution. The precision are better than 5% for most major and trace elements. The results are listed in Table DR2. 3. Whole-rock Sr-Nd isotopes Around 100 mg whole-rock powders were digested using a mixed acid of HF and HNO 3 in Teflon beakers at 100 for 20 days. Strontium and REE (rare earth elements) fractions were separated by quartz columns with resin bed of AG50-8X and Nd fractions were further separated from REE by HDEHP-coated Kef columns. All procedure blanks are smaller than 100 pg for Sr and 10 pg for Nd. Triton thermal ionized mass spectrometry (TIMS) and micromass isoprobe multi-collector (MC-) ICPMS, both are hosted at GIG, were separately employed to analyze Sr and Nd isotope compositions following the procedures described by Chen et al. (2010) and Li et al. (2004b). The measured Sr and Nd isotope ratios were normalized to 86 Sr/ 88 Sr = and 146 Nd/ 144 Nd = The reported Sr and Nd data were adjusted to SRM NBS-987 standard with 87 Sr/ 86 Sr = and Shin Etsu JNdi-1 standard with 143 Nd/ 144 Nd = , respectively. are listed in Table DR3. 4. In-situ zircon U-Pb study Zircon grains, extracted from rock specimens using standard density and magnetic separation techniques, were mounted in epoxy mounts together with zircon standards TEMORA 2 and and then polished to expose their interior for future analysis. Transmitted and reflected light micrographs and cathodoluminescence (CL) images of zircons were documented to reveal their internal structures. After that, zircon mounts were vacuum-coated with highpurity gold prior to SIMS analysis. Measurements of U, Th and Pb were conducted using the CAMECA IMS 1280 ion microprobe at IGG in Beijing. U-Th-Pb ratios and absolute abundances were determined relative to the standard zircon (Wiedenbeck et al., 1995), analyses of which were interspersed with those of unknowns as well as the TEMORA 2 zircon standard as an

7 7 unknown to monitor the external uncertainty, using operating and data processing procedures the same as those described by Li et al. (2009). Results are presented in Table DR4. Uncertainties on individual analyses in data table are reported at a 1 level; mean ages for pooled U/Pb and Pb/Pb analyses are quoted with 95% confidence interval, unless otherwise noted. Data reduction was carried out using the Isoplot/Ex v program (Ludwig, 2001). The weighted average of 206 Pb/ 238 U age for 29 analyzed TEMORA 2 zircons during the course of this study is Ma (MSWD = 0.26, 95% confidence interval), which is in good agreement with the recommended value (Black et al., 2004). 5. In-situ zircon O isotope study The oxygen isotope data were also acquired by CAMECA IMS 1280, using a ~2 na primary Cs + ion beam which was accelerated at 10 kv. The same parts for U-Pb analysis were targeted wherever possible. The analytical procedures are the same as those described by (Li et al., 2010). The spot size is about 20 m in diameter including 10 m beam diameter and 10 m raster. Negative secondary ions 18 O - and 16 O - were extracted at 10 kv and measured in multicollector mode using two off-axis Faraday cups with intensity of 16 O typically at cps. Each analysis takes ca. 4.5 min consisting 2 min pre-sputtering, 1 min automatic beam centering and 80 seconds (20 cycles) data collection. Oxygen isotope ratios are expressed as δ 18 O, representing deviation of measured 18 O/ 16 O values from the Vienna standard mean ocean water (VSMOW) in parts per thousand (Table DR5). All data were then corrected using Temora 2 which has 8.20 (Black et al., 2004). Uncertainties on individual analyses are usually better than (1σ). 6. In-situ zircon Lu-Hf study In-situ Hf isotope analyses of previously dated zircons were carried out at the IGG on a Neptune MC-ICPMS which is equipped with a Geolas 193 nm excimer ArF laser-ablation system. The analytical procedures and calibration method are detailed by Wu et al. (2006). The laser ablation pits for this study is ca. 50 m in diameter and the ablation time is 26 seconds for each measurement at a repetition rate of 10 Hz at 10 J/cm 2. During analysis, an isotopic ratio of 176 Yb/ 172 Yb = was applied to make correction for isotopic interference of 176 Yb on 176 Hf (Wu et al., 2006). Measured 176 Hf/ 177 Hf ratios were normalized to 179 Hf/ 177 Hf = Because the weighted average 176 Hf/ 177 Hf ratio of standard Mud Tank analyzed during the whole session is (MSWD = 0.91, n = 51), identical within analytical errors to the accepted value of measured using the solution method (Woodhead and Hergt, 2005), there is no need to make further external adjustment. Results were combined with U-Pb results in Table DR4.

8 8 Table DR1 Chemical compositions of olivine and orthopyroxene. Sample Mineral Olivine SiO TiO Al 2 O FeO Cr 2 O MnO MgO CaO Na 2 O K 2 O NiO Total cations per 4 oxygens Si Al Ti Fe Fe Cr Mg Mn Ca Na K Ni Sum Fe # Sample Mineral Olivine Orthopyronexe SiO TiO Al 2 O FeO Cr 2 O MnO MgO CaO Na 2 O K 2 O NiO Total cations per 4 oxygens cations per 6 oxygens Si Al Ti Fe

9 9 Fe Cr Mg Mn Ca Na K Ni Sum Fe # Wo En Fs : not determined or calculated; 0 : under detection limit; Fe # = molar [Fe/(Fe+Mg)].

10 10 Table DR2 Major and trace elements Major elements (%) SiO TiO Al 2 O T Fe 2 O MnO MgO CaO Na 2 O K 2 O P 2 O LOI Total A/CNK Minor elements (ppm) Ga Rb Sr Y Zr Nb Ba La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Hf Ta Th U T zr M Ga/Al*10, Major elements (%) SiO TiO Al 2 O T Fe 2 O

11 11 MnO MgO CaO Na 2 O K 2 O P 2 O LOI Total A/CNK Minor elements (ppm) Ga Rb Sr Y Zr Nb Ba La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Hf Ta Th U T zr M Ga/Al*10, Major elements (%) SiO TiO Al 2 O T Fe 2 O MnO MgO CaO Na 2 O K 2 O P 2 O LOI Total A/CNK Minor elements (ppm)

12 Ga Rb Sr Y Zr Nb Ba La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Hf Ta Th U T zr M Ga/Al*10, Note: A/CNK = molar [Al 2 O 3 /(CaO+K 2 O+Na 2 O)]; T Zr = 12,900/[ M + ln(496,000/zr)]; M = (Na + K + 2Ca)/(Al Si). 12

13 13 Table DR3 Whole-rock Sr-Nd isotope compositions. Sample 87 Rb/ 86 Sr 87 Sr/ 86 Sr (2σ) I Sr 147 Sm/ 144 Nd 143 Nd/ 144 Nd (2σ) Nd(t) DM * (Ma) 2DM * (Ma) ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± ± Note: 87 Rb/ 86 Sr and 147 Sm/ 144 Nd were calculated using trace element contents determined by ICPMS. * Single- and two-stage Nd model ages, T DM and T 2DM, are calculated using formulas and parameters the same as Li et al. (2003); t = 154 Ma.

14 14 Table DR4 SIMS zircon U-Pb and LA-MC-ICPMS zircon Hf data Th/ 207 Pb*/ 206 Pb*/ 206 Pb*/ Spot U Th f U ± U 238 ± U 238 ± U 176 Yb/ 177 Hf 176 Lu/ 177 Hf 176 Hf/ 177 C Hf ± 2σ εhf(t) ±2σ T DM T DM ppm ppm (%) (%) (%) (Ma) (Ma) (Ma) A ( N, E) Weighted average (2 ) (n = 16) B ( N, E)

15 Weighted average (2 ) (n = 17) Note: f 206 stands for percentage of common lead in measured 206 Pb; Hf(t), T DM, and T DM C were calculated using parameters and formulas the same as Li et al. (2010); t = 154 Ma.

16 16 Table DR5 Zircon oxygen isotopes analysed by CAMECA IMS 1280 ion microprobe Analysis* 18 O/ 16 O (Meas.) 18 O (Meas.) ±1SE 18 O (Corr.) Analysis* 18 O/ 16 O (Meas.) 18 O (Meas.) ±1SE 18 O (Corr.) Tem@ E E Tem@ E @ E Tem@ E Tem@ E @ E Tem@ E E Tem@ E E @ E E Tem@ E Tem@ E Tem@ E E @ E E Tem@ E E Tem@ E Tem@ E Tem@ E @ E @ E E Tem@ E E E E E Tem@ E Tem@ E E E @ E E E Tem@ E E E Tem@ E E E E E Tem@ E E E Tem@ E E E Tem@ E E Tem@ E @ E Tem@ E E Tem@ E Tem@ E Tem@ E E Tem@ E E E avg E Tem@ E ±SD E E Tem avg E E ±SD E Analysis results listed in sequence as measured. Notes: Meas. = Measured; Corr. = Corrected; SE = Standard Error; Tem = Temora 2; avg. = average; SD = standard deviation. Measured 18 O/ 16 O ratios were normalized by using Vienna Standard Mean Ocean Water compositions (VSMOW, 18 O/ 16 O = ); 18 O Measured = [( 18 O/ 16 O) Measured /( 18 O/ 16 O) VSMOW 1] 1000 ; 18 O Corrected = 18 O Measured IMF; IMF (instrumental mass fractionation factor) = 18 O (Tem avg.) Measured 8.20.

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18 and REE analyses: Geostandards Newsletter, v. 19, p. 1-23, doi: /j x.1995.tb00147.x. Woodhead, J.D., and Hergt, J.M., 2005, A preliminary appraisal of seven natural zircon reference materials for in situ Hf isotope determination: Geostandards and Geoanalytical Research, v. 29, p , doi: /j x.2005.tb00891.x. Wu, F.Y., Yang, Y.H., Xie, L.W., Yang, J.H., and Xu, P., 2006, Hf isotopic compositions of the standard zircons and baddeleyites used in U-Pb geochronology: Chemical Geology, v. 234, p , doi: /j.chemgeo