XM1/331 XM1/331 BLFX-3 XM1/331
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- Candice Houston
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1 a b AkC AkC strontian fluoro-apatite clinopyroxene phlogopite K-richterite XM1/331 clinopyroxene XM1/331 Fe-Ti ox c d clinopyroxene kric AkC ilmenite Sr-barite AkC XM1/331 BLFX-3 Supplementary Figure 1. Back-scattered electron (BSE) SEM images of primary inclusions in XM1/331 clinopyroxene (a, b, c) and BLFX-3 ilmenite (d). AkC: zemkorite/ Na-K-rich calcite; kric: K-richterite; ox: oxide.
2 tetraferriphlogopite Na-rich fluoro-apatite a clinopyroxene XM1/331 fluoro-apatite shortite b Na-bearing dolomite ilmenite alkali-bearing dolomite BLFX-3 5 µm Supplementary Figure 2. SEM images and energy dispersive spectroscopy (EDS) x-ray spectra of phases included in XM1/331 clinopyroxene (a) and BLFX-3 ilmenite (b)
3 K/Na K-richterite XM1/331 BLFX-3 a Al 2 O 3 (wt.%) Phlogopite b Mg# Mg# TiO 2 (wt.%) K-richterite c TiO 2 (wt.%) Phlogopite d Mg# Mg# Supplementary Figure 3. Major element variation diagrams of K-richterite (a, b) and phlogopite (c, d) grains in MARID samples XM1/331 and BLFX-3. Fields of MARID K- richterite and phlogopite from refs Mg# = 100 Mg/(Mg+Fe)
4 100 values/pm XM1/331 K-richterite a MARID K-richterite 0.01 Rb Ba Th U Ta Nb La Ce Pb Pr Sr Nd Zr Hf Sm Eu Ti Gd Tb Dy Y Ho Er Yb Lu 100 values/pm BLFX-3 K-richterite b MARID K-richterite 0.01 Rb Ba Th U Ta Nb La Ce Pb Pr Sr Nd Zr Hf Sm Eu Ti Gd Tb Dy Y Ho Er Yb Lu Supplementary Figure 4. Trace element variation diagrams of K-richterite (a, b) and phlogopite (c, d) grains in MARID samples XM1/331 and BLFX-3. Previous analyses of MARID K-richterite and phlogopite grains from [4]. Primitive mantle (PM) values from ref 5. Supplementary Figure 4 continues overleaf.
5 values/pm XM1/331 Phlogopite c MARID phlogopite Rb Ba Th U Nb Ta La Ce Pb Pr Sr Nd Zr Hf Sm Eu Ti Gd Tb Dy Y Ho Er Yb Lu values/pm BLFX-3 phlogopite d MARID phlogopite Rb Ba Th U Nb Ta La Ce Pb Pr Sr Nd Zr Hf Sm Eu Ti Gd Tb Dy Y Ho Er Yb Lu
6 Ti (ppm) δ 18 O ( ) age (Ma) Z_3 6.2 traces O isotopes U-Pb dating 89.0 Hf isotopes Supplementary Figure 5. Cathodoluminescence (CL) images of zircon grains in MARID sample XM1/331 showing the location of areas analysed for trace element concentrations, O, U-Pb and Hf isotope composition. Measured values of Ti concentration (ppm), δ 18 O ( ) and U-Pb age (Ma) are also shown. Supplementary Figure 5 continues overleaf.
7 331Z_ Z_ Z_ Supplementary Figure 5 continues overleaf.
8 b Z_ Z_ Z_X Supplementary Figure 5 continues overleaf.
9 BIG.1 331Z_BI G 54 BIG.2 74 BIG.6 70 BIG BIG.3 40 traces BIG.4 Hf isotopes Supplementary Figure 5 continues overleaf.
10 A_ A_ b A_
11 ΣREE (ppm) dark CL areas intermediate brightness or mixed areas bright CL areas Yb/Sm U (ppm) Ti (ppm) 331Z Z Z Z Z Z Z Z Z Z-9b. 331Z Z- 331Z- 331Z- 331A_ A_ A_ A_ A_ Z Z-5b. 331Z Z Z Z Z Z Z Z- 331Z- 331A_ Z Z-5b. 331Z-X.1 331Z Z- 331A_ M_1 Supplementary Figure 6. Relations between trace element concentrations, U-Pb ages, O and Hf isotopic compositions and cathodoluminescence (CL) response of analysed areas of XM1/331 zircons Supplementary Figure 6 continues overleaf.
12 140 U/Pb age (Ma) dark CL areas intermediate brightness or mixed areas bright CL areas δ 18 O ( ) Hf/ 177 Hf present Z Z Z Z Z Z Z-5.1b 331Z Z Z-9b.1 331Z Z-BIG.1 331Z-BIG.5 331Z-BIG.6 331A_ A_ A_ A_3.1b 331A_ Z Z-5b.1 331Z Z Z Z Z Z Z Z-BIG.2 331Z-BIG.3 331A_ Z Z-5b.2 331Z-X.1 331Z Z-BIG.4 331A_ M_1
13 Y (ppm) lamproite carbonatite a mafic Y (ppm) d kimberlite XM1/331 XM1/331_low-trace Yb/Sm excess Ti-Fe Ti (ppm) Y (ppm) b Fe (ppm) e U (ppm) Ti (ppm) Y (ppm) c values/c1 f XM1/331 zircons Nb/Ta La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Supplementary Figure 7. Trace element variation diagrams and chondrite-normalised rare earth element (REE) patterns for zircon grains in MARID sample XM1/331. Excess Ti-Fe refers to analyses where Ti and Fe concentrations are affected by diffusion from adjacent rutile. Fields of zircons in various terrestrial rocks from ref. 6; C1 chondrite values from ref. 5.
14 Pb/ 206 Pb Intercepts at 89.6±1.2 & 4513±730 Ma n=18/23; MSWD = 1.09 XM1/331 zircons data-point error ellipses are Pb/ 238 U age (Ma) box heights are 2 Mean = 90.07±0.58 [0.65%] 95% conf. n=16/18; MSWD = U/ 206 Pb Supplementary Figure Pb/ 206 Pb vs 238 U/ 206 Pb Tera-Wasserburg Concordia diagrams and histograms of 206 Pb/ 238 U ages for in situ SHRIMP analyses of zircon grains in MARID sample XM1/331. The ellipses (Concordia) and bars (histograms) represent two sigma uncertain es; red and blue ellipses and bars are accepted and rejected analyses, respec vely. The histogram does not include old zircon ages (i.e. > 95Ma)
15 7.0 δ 18 O ( ) a 400 ΣREE (ppm) d XM1/331 XM1/331_low trace U-Pb Age (Ma) δ 18 O ( ) U (ppm) b Yb/Sm e U-Pb Age (Ma) δ 18 O ( ) Yb/Sm c εhf present f U-Pb Age (Ma) δ 18 O ( ) εhf present g Yb/Sm Supplementary Figure 9. U-Pb age vs δ 18 O (a), U concentration (b) and Yb/Sm (c), δ 18 O vs εhf present (d), ΣREE concentration (e) and Yb/Sm (f), and Yb/Sm vs εhf present (g) for zircon grains in MARID sample XM1/331.
16 Supplementary Table 1. Major oxide composition (wt.%) of K-richterite, clinopyroxene, phlogopite, rutile and ilmenite in MARID samples XM1/331 and BLFX-3 measured by electron microprobe XM1/331 K-richterite Sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/ Amph- 331-Amph- 331-Amph- 331-Amph- 331-Amph- Label 331-Amph Amph Amph-3 1b SiO TiO Al 2 O Cr 2 O FeO MnO MgO NiO bdl 0.06 CaO SrO bdl Na 2 O K 2 O F Cl bdl bdl 0.01 Total O=F,Cl Total rec Mg# Sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/ C-Amph- 331C-Amph- 331C-Amph- 331C-Amph- Label 331-Kric kric kric kric SiO TiO Al 2 O Cr 2 O FeO MnO bdl MgO NiO bdl 0.02 CaO SrO 0.04 bdl Na 2 O K 2 O F Cl bdl Total O=F,Cl Total rec Mg# bdl: below detection limit Mg#=100 Mg/(Mg+Fe)
17 Supplementary Table 1. continued XM1/331 K-richterite Sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 Label 331-kric-5 331B-kric-1 331B-kric-1b 331B-kric-2 average 1sd SiO TiO Al 2 O Cr 2 O FeO MnO <0.06 MgO NiO <0.04 CaO SrO bdl <0.05 Na 2 O K 2 O F Cl 0.01 bdl <0.01 Total O=F,Cl Total rec Mg# bdl: below detection limit; sd: standard deviation of the mean Mg#=100 Mg/(Mg+Fe) XM1/331 clinopyroxene Sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 Label 331-Cpx Cpx Cpx B- Cpx-1 331B-cpx core1 331Bcpx-3 331Bcpx rim 331B-cpx core2 331Bcpx cpx round average 1sd SiO TiO Al 2O Cr 2O FeO MnO MgO NiO bdl <0.05 CaO Na 2O K 2O bdl <0.01 V 2O Total Mg# bdl: below detection limit; sd: standard deviation of the mean Mg#=100 Mg/(Mg+Fe)
18 Supplementary Table 1. continued XM1/331 phlogopite Sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 Label 331-Phl Phl Phl Phl Phl B-phl B-phl B-phl B-phl- 3b average 1sd SiO TiO Al 2O Cr 2O FeO MnO MgO NiO CaO bdl bdl bdl 0.01 bdl <0.01 BaO bdl <0.09 Na 2O K 2O F Cl Total H 2O calc O=F,Cl Total rec Mg# bdl: below detection limit; sd: standard deviation of the mean Mg#=100 Mg/(Mg+Fe) XM1/331 rutile Sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 Label 331-Rt Rt Rt Rt Rt rut rut rt-4 average 1sd SiO 2 bdl bdl bdl bdl 0.02 bdl <0.01 TiO Al 2O bdl bdl bdl 0.03 <0.02 Cr 2O FeO MnO bdl bdl bdl bdl <0.01 MgO bdl bdl bdl bdl <0.33 NiO 0.04 bdl bdl <0.04 CaO 0.02 bdl bdl <0.06 V 2O Nb 2O Total bdl: below detection limit; sd: standard deviation of the mean
19 Supplementary Table 1. continued XM1/331 ilmenite Sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 Label 331-Ilm Ilm ilm ilm-1b 331-ilm-3b average 1sd SiO bdl bdl <0.04 TiO Al 2O 3 bdl <0.02 Cr 2O FeO MnO MgO NiO CaO V 2O Nb 2O Total bdl: below detection limit; sd: standard deviation of the mean BLFX-3 ilmenite sample BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 Label B3-iml-1 B3-iml-2 B3-iml-3 B3-iml-4 B3-iml-5 average 1sd SiO 2 bdl bdl bdl bdl 0.04 <0.04 TiO Al 2O Cr 2O FeO MnO MgO NiO CaO 0.01 bdl bdl bdl 0.02 <0.01 V 2O Nb 2O Total bdl: below detection limit; sd: standard deviation of the mean
20 Supplementary Table 1. continued BLFX-3 K-richterite sample BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 B3-Krich- B3-Krich- Label B3-Krich-1 B3-Krich-2 B3-Krich-3 B3-Krich-4 B3-Krich-5 average 6a 6b 1sd SiO TiO Al 2 O Cr 2 O FeO MnO MgO NiO bdl 0.04 <0.04 CaO Na 2 O K 2 O V 2 O bdl bdl <0.03 Total Mg# bdl: below detection limit; sd: standard deviation of the mean Mg#=100 Mg/(Mg+Fe) BLFX-3 phlogopite sample BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 Label B3-phl-1 B3-phl-2 B3-phl-3 B3-phl-4 B3-phl-5 B3-phl-6 B3-phl-7r B3-phl-7c average 1sd SiO TiO Al 2 O Cr 2 O FeO MnO bdl <0.03 MgO NiO CaO bdl bdl bdl bdl 0.01 bdl <0.01 Na 2 O K 2 O V 2 O bdl 0.01 bdl bdl 0.01 <0.01 Total Mg# bdl: below detection limit; sd: standard deviation of the mean Mg#=100 Mg/(Mg+Fe)
21 Supplementary Table 2. Trace element concentrations (ppm) of K-richterite, clinopyroxene and phlogopite in MARID samples XM1/331 and BLFX-3 measured in situ by LA-IPC-MS Sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 Mineral K-richterite K-richterite K-richterite K-richterite K-richterite K-richterite K-richterite K-richterite K-richterite K-richterite K-richterite Label 331-Amph Amph Amph- 331-Amph- 331-Amph- 331A-Kric- 331A-Kric-1 331A-Kric-3 331A-Kric-7 331A-Kric average Rb Ba Th 0.19 bdl 0.06 bdl bdl bdl <0.09 U 0.04 bdl bdl bdl bdl bdl 0.01 <0.03 Ta Nb La Ce Pb Pr Sr Nd Zr Hf Sm Eu Ti Gd Dy Ho bdl bdl <0.01 Er bdl <0.02 Yb bdl bdl bdl 0.01 <0.01 Y Lu 0.01 bdl bdl bdl bdl bdl bdl <0.01 Sc V Ni Li bdl: below detection limit XM1/331 K-richterite: calibration standard NIST612; internal standard Ca
22 Supplementary Table 2. continued Sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 Mineral clinopx clinopx clinopx clinopx clinopx clinopx clinopx clinopx phlogopite phlogopite phlogopite Label 331-Cpx- 331B-Cpx- 331B-Cpx-1 331B-Cpx-3 331B-Cpx-5 331B-Cpx-6 331B-Cpx average 331-Phl Phl Phl-22 Rb Ba Th U bdl 0.01 bdl bdl bdl < Ta bdl bdl bdl bdl bdl bdl bdl bdl Nb bdl < La Ce Pb bdl 0.13 Pr nd Sr Nd bdl 0.01 Zr Hf Sm bdl bdl bdl Eu bdl Ti Gd bdl bdl Dy bdl bdl Ho Er bdl bdl 0.05 Yb bdl 0.05 bdl Y bdl Lu bdl bdl bdl Sc V Ni Li bdl: below detection limit XM1/331 clinopyroxene: calibration standard NIST612; internal standard Ca XM1/331 phlogopite: calibration standard NIST612; internal standard Mg
23 Supplementary Table 2. continued Sample XM1/331 XM1/331 XM1/331 BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 Mineral phlogopite phlogopite phlogopite K-richterite K-richterite K-richterite K-richterite K-richterite Label 331-Phl Phl-3 average B3-Krich-1-10 B3-Krich-2-11 B3-Krich-3-12 B3-Krich-4-13 average Rb Ba Th U 0.01 bdl bdl bdl bdl <0.01 Ta Nb La Ce Pb < Pr Sr Nd < Zr Hf Sm bdl 0.03 < Eu bdl 0.07 < Ti Gd bdl 0.02 < Dy 0.04 bdl < Ho Er bdl bdl < bdl bdl <0.01 Yb 0.01 bdl < bdl bdl <0.01 Y < Lu bdl 0.01 <0.01 bdl bdl bdl bdl bdl Sc V Ni Ca Li bdl: below detection limit XM1/331 phlogopite: calibration standard NIST612; internal standard Mg BLFX-3 K-richterite: calibration standard NIST612; internal standard Ca
24 Supplementary Table 2. continued Sample BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 Mineral phlogopite phlogopite phlogopite phlogopite phlogopite Label B3-phlog-1 B3-phlog-2 B3-phlog-3 B3-phlog-5 average Rb Ba Th U Ta Nb La bdl 0.02 bdl bdl <0.02 Ce bdl 0.05 bdl bdl <0.05 Pb Pr bdl bdl bdl bdl bdl Sr Nd bdl 0.01 bdl bdl <0.01 Zr Hf Sm bdl bdl bdl bdl bdl Eu bdl bdl bdl bdl bdl Ti Gd bdl bdl 0.01 bdl <0.01 Dy bdl bdl bdl bdl bdl Ho Er bdl bdl bdl bdl bdl Yb bdl bdl bdl bdl bdl Y bdl 0.01 bdl bdl bdl Lu bdl bdl bdl bdl bdl Sc V Ni Ca Li bdl: below detection limit BLFX-3 phlogopite: calibration standard NIST612; internal standard Mg
25 Supplementary Table 3. Trace element concentrations (ppm) of ilmenite and rutile in MARID samples XM1/331 and BLFX-3 measured in situ by LA-IPC-MS Sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 Mineral rutile rutile rutile rutile rutile rutile rutile rutile rutile ilmenite Label 331A-Rt-1 331A-Rt-2 331A-Rt-3 331A-Rt-4 331A-Rt-6 331A-Rt-7 331A-Rt-8 331A-Rt-10 average 331-Ilm on Rt rim-29 Ba bdl 0.02 bdl bdl bdl bdl bdl bdl < Th bdl bdl bdl bdl bdl bdl bdl bdl bdl 0.02 U Ta Nb La bdl 0.01 bdl bdl bdl bdl bdl bdl < Ce bdl bdl bdl bdl bdl bdl < Pb bdl bdl 0.01 bdl bdl < Sr Nd bdl bdl bdl bdl bdl bdl bdl bdl bdl 0.06 Zr Hf Sm bdl bdl bdl bdl bdl bdl bdl bdl bdl bdl Y bdl bdl 0.01 bdl 0.01 bdl bdl bdl < Lu bdl bdl bdl bdl bdl bdl bdl bdl bdl bdl Sc 6.2 V 425 Ni 596 Ca bdl bdl Li 4.0 Zr-in-Rt T ( C) a ±16 [1sd] bdl: below detection limit calibration standard BHVO2-G; internal standard Ti a for P = 3GPa
26 Supplementary Table 3. continued Sample BLFX-3 BLFX-3 BLFX-3 BLFX-3 BLFX-3 Mineral ilmenite ilmenite ilmenite ilmenite ilmenite Label B3-ilm-17 B3-ilm-18 B3-ilm-19 B3-ilm-20 average Ba bdl <0.02 Th 0.03 bdl bdl bdl <0.03 U Ta Nb La bdl bdl 0.02 bdl <0.02 Ce 0.03 bdl bdl bdl <0.03 Pb bdl bdl 0.02 bdl <0.02 Sr Nd bdl bdl bdl bdl bdl Zr Hf Sm bdl bdl bdl bdl bdl Y Lu bdl bdl bdl bdl bdl Sc V Ni Ca Li bdl: below detection limit calibration standard BHVO2-G; internal standard Ti
27 Supplementary Table 4. Trace element concentrations (ppm) and Ti-in-zircon thermometry of zircons in MARID sample XM1/331 sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 label 331Z_ Z_ Z_ Z_ Z_ Z_ Z_ Z_4 331Z_ Z_ Z_5b.1 331Z_5b.2 331Z_ Z_6.2 Th U Ta Nb La 0.37* * Ce Pb Pb 0.01 bdl Pb Pb tot Pr Sr 3.2* * Nd Sm Eu Ti ** ** ** Gd Tb Dy Ho Er Tm Yb Y Lu P Fe ** ** Σ(REE) Yb/Sm Nb/Ta Th/U Ti-inzircon T ( C) ** ** ** calibration standard NIST610; internal standard Hf; Hf 2 O = wt.% (mean = 1.32±0.14 [1sd] wt.%; n=30; measured by EMP) a for P = 3GPa; * contamination; **Ti-Fe diffusion in zircon from adjacent rutile; see Supplementary Note 1 for details of Ti-in-zircon T calculation
28 Supplementary Table 4. continued sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/ Z_BIG. 331Z_BIG. 331Z_BIG. 331Z_BIG. label 331Z_ Z_ Z_X 331Z_ Z_ Z_ Z_ Z_9.b1 331Z_ Z_ Th U Ta Nb La * 0.74* * 0.06 Ce Pb Pb Pb Pb tot Pr Sr * 6.3* * 0.3 Nd Sm Eu Ti ** ** Gd Tb Dy Ho Er Tm Yb Y Lu P Fe ** ** 73.3* Σ(REE) Yb/Sm Nb/Ta Th/U Ti-inzircon ** ** T ( C) a a for P = 3GPa; * contamination; **Ti-Fe diffusion in zircon from adjacent rutile; see Supplementary Note 1 for details of Ti-in-zircon T calculation
29 Supplementary Table 4. continued sample XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/331 XM1/ Z_BIG. 331Z_BIG. label 331A_ A_ A_ A_ A_3.1b 331A_ A_ A_ A_ A_5 331A_6 331A_7 5 6 Th U Ta Nb La * Ce Pb Pb Pb Pb tot Pr Sr * * Nd Sm Eu Ti ** 439** ** Gd Tb Dy Ho Er Tm Yb Y Lu P Fe Σ(REE) > >162 >192 >348 >82 >284 Yb/Sm Nb/Ta Th/U Ti-inzircon T ( C) ** 1055** ** a for P = 3GPa; * contamination; **Ti-Fe diffusion in zircon from adjacent rutile; see Supplementary Note 1 for details of Ti-in-zircon T calculation
30 Supplementary Table 4. continued sample XM1/331 XM1/331 label 331M_1 average Th U Ta Nb La bdl Ce Pb Pb Pb Pb tot Pr Sr 0.2 Nd Sm Eu Ti 7 64 # Gd Tb Dy Ho Er Tm Yb Y Lu P Fe 4.5 Σ(REE) Yb/Sm Nb/Ta Th/U Ti-inzircon T ( C) ±66 [1sd] # a for P = 3GPa; bdl: below detection limit; # does not include high-ti values/temperatures due to Ti diffusion from adjacent rutile; see Supplementary Note 1 for details of Ti-in-zircon T calculation
31 Supplementary Table 5. Trace element analyses (ppm) of glass standards measured in situ by LA-ICP-MS K-richterite and clinopyroxene analyses standard BCR2-G BCR2-G BCR2-G BCR2-G BCR2-G BCR2-G BCR2-G BCR2-G BCR2-G BCR2-G BCR2-G BCR2-G BCR2-G analysis n Li Sc Ti V Ni Rb Sr Y Zr Nb Ba La Ce Pr Nd Sm Eu Gd Dy Ho Er Yb Lu Hf Ta Pb Th U calibration standard NIST612; internal standard Ca
32 Supplementary Table 5. continued K-richterite and clinopyroxene analyses standard BHVO2-G BHVO2-G BHVO2-G BHVO2-G BHVO2-G BHVO2-G BHVO2-G BHVO2-G NIST610 NIST610 NIST610 NIST610 analysis n Li Sc Ti V Ni Rb Sr Y Zr Nb Ba La Ce Pr Nd Sm Eu Gd Dy Ho Er Yb Lu Hf Ta Pb Th U calibration standard NIST612; internal standard Ca
33 Supplementary Table 5. continued Phlogopite analyses standard BCR2-G BCR2-G BCR2-G BCR2-G NIST610 NIST610 NIST610 NIST610 BHVO2-G BHVO2-G BHVO2-G BHVO2-G analysis n Li Ca Sc Ti V Ni Rb Sr Y Zr Nb Ba La Ce Pr Nd Sm Eu Gd Dy Ho Er Yb Lu Hf Ta Pb Th U calibration standard NIST612; internal standard Mg
34 Supplementary Table 5. continued Rutile and ilmenite analyses standard NIST612 NIST612 NIST612 NIST612 NIST610 NIST610 NIST610 NIST610 NIST610 NIST610 BCR2-G BCR2-G BCR2-G BCR2-G BCR2-G analysis n Li Ca Sc V Ni Sr Y Zr Nb Ba La Ce Nd Sm Lu Hf Ta Pb Th U calibration standard BHVO2-G; internal standard Ti
35 Supplementary Table 5. continued Zircon analyses standard BCR2-G BCR2-G BCR2-G BCR2-G analysis n P Ti Fe Sr Y Nb Ba La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Ta Pb Pb Pb Th U calibration standard NIST610; internal standard Hf
36 Supplementary Table 6. SHRIMP U-Pb data for zircons in MARID sample XM1/331 Label U (ppm) Th (ppm) 232 Th/ 238 U 206 Pb* (ppm) % 206 Pb c 206 Pb/ 238 U Age (Ma) a ±2sd 238 U/ 206 Pb (uncorr.) ±2sd 207 Pb/ 206 Pb (uncorr.) ±2sd 238 U/ 206 Pb* ±2sd XM1/ A_ A_ A_ A_ A_ Z Z Z Z Z Z Z Z Z Z Z Z Z Z Z Z Z M_ Pb c and Pb* indicate the common and radiogenic portions, respectively. a Common Pb corrected by assuming 206 Pb/ 238 U- 207 Pb/ 235 U age-concordance
37 Supplementary Table 7. Oxygen isotope composition of zircons in MARID sample XM1/331 and of Temora_2 zircon standard measured in situ by SHRIMP Label δ 18 O ( SMOW ) 2se a 2sd b Temora-2 zircon standard TEM TEM TEM TEM TEM TEM TEM TEM TEM TEM TEM TEM TEM TEM TEM TEM TEM TEM TEM TEM weighted mean 8.22±0.11 c XM1/331 zircons 331A A A A Z Z Z Z Z Z Z-X z z z z z z z z weighted mean 5.94±0.17 MSWD 8.6 a internal reproducibility; b external reproducibility; c nominal value of Temora-2 = Uncertainties of weighted mean is two times standard deviation
38 Supplementary Table 8. Lu-Hf isotopic composition of zircons in MARID sample XM1/331 and of Temora_2 and zircon standards analysed in situ by multi-collector ICP-MS Label Hf signal (V) 176 Lu/ 177 Hf ±2se 176 Hf/ 177 Hf ±2se εhf present ±2sd 176 Hf/ 177 Hf (90Ma) εhf (90Ma) 176 Hf/ 177 Hf (120Ma) εhf (120Ma) 176 Hf/ 177 Hf (180Ma) εhf (180Ma) XM1/331 zircons 331Z Z Z Z Z Z Z Z-5b Z-5b Z Z Z Z Z Z Z-X Z Z Z Z Z-9b Z-BIG Z-BIG Z-BIG Z-BIG Z-BIG Z-BIG Z Z A_ A_ A_ A_
39 Supplementary Table 8. continued Label Hf signal (V) 176 Lu/ 177 Hf ±2se 176 Hf/ 177 Hf ±2se εhf present ±2sd 176 Hf/ 177 Hf (90Ma) εhf (90Ma) 176 Hf/ 177 Hf (120Ma) εhf (120Ma) 176 Hf/ 177 Hf (180Ma) εhf (180Ma) *331A_ A_ M_ mean min max weighted mean ± -15.9± ± ± ±0.5 (±2se) ± standard deviation mswd Temora-2 zircon standard Temora Temora_ Temora_ Temora_ Temora_ zircon standard _ _ normalised to nominal values of Plesovice zircon 8 standard analysed during the same session; * rejected analysis (based on statistically meaningful difference as defined by Isoplot); # rejected analyses not included εhf values calculated using 176 Lu decay constant of a 1 (ref. 9); ( 176 Hf/ 177 Hf) CHUR = and ( 176 Lu/ 177 Hf) CHUR = (ref 10) Within-run uncertainties (2se) of 176 Hf/ 177 Hf ratios for the unknowns are high (~± ) due to the low Hf signals (3.0 to 4.1 V) obtained. 176 Hf/ 177 Hf ratios for the and Temora-2 standard zircons acquired with similar signals are within error of the respective reference values and indicate a reproducibility of ± and ± , respectively.
TABLE DR2. Lu-Hf ISOTOPIC DATA FOR WHOLE ROCK SAMPLES AND ZIRCONS [Lu] [Hf]
![TABLE DR2. Lu-Hf ISOTOPIC DATA FOR WHOLE ROCK SAMPLES AND ZIRCONS [Lu] [Hf]](/thumbs/72/67409273.jpg "TABLE DR2. Lu-Hf ISOTOPIC DATA FOR WHOLE ROCK SAMPLES AND ZIRCONS [Lu] [Hf]")
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