LETTERS PUBLISHED ONLINE: 23 JANUARY 2011 | DOI: 10.1038/NGEO1060 Tracing two orogenic cycles in one eclogite sample by Lu–Hf garnet chronometry Daniel Herwartz1 *, Thorsten J. Nagel1 , Carsten Münker2 , Erik E. Scherer3 and Nikolaus Froitzheim1 Subduction of rocks into the mantle results in high-pressure metamorphism and the formation of eclogites from basaltic precursor rocks. At the Earth’s surface, eclogites often occur as isolated fragments embedded in crustal rocks that lack evidence for high-pressure conditions1–3 . The high-pressure rocks are therefore often viewed as dismembered fragments that have been assembled and intercalated with rocks devoid of any high-pressure history at shallow crustal levels4–8 , forming a tectonic mélange. Such mélange models were supported by age discrepancies among high-pressure rocks from the Adula nappe (Central Alps)9–12 , which was thought to represent a classic example of such a situation4,5 . Here we present Lu–Hf age data from two populations of the high-pressure mineral garnet, found within a single eclogite sample taken from Trescolmen, in the Central Adula nappe. We report a minimum Variscan age of 332.7 Myr and a maximum Alpine age of 38 Myr for the two populations. We suggest that the Trescolmen eclogite was subducted to mantle depth and subsequently exhumed, becoming part of a continental crust during the Variscan orogeny. Later, during the Alpine orogeny, the Adula nappe must have been subducted to—and exhumed from—mantle depth a second time, as one coherent unit. We conclude that the Adula nappe is not a mélange, and therefore, the crustal rocks that envelope the eclogites have also been subjected to high-pressure conditions through deep subduction during the Alpine event13,14 . Subduction to mantle depths of >40 km and exhumation back to the surface are documented by the occurrence of eclogite-facies rocks formed at high-pressure in Alpine-type orogens. Such rocks occur either in units derived from subducted oceanic crust or, alternatively, in tectonic nappes dominantly made of felsic crust from a subducted continental margin. Rocks that have reached ultrahigh-pressure conditions (that is, the stability field of coesite; >70 km) typically derive from the second type of high-pressure units and are associated with abundant continental basement1–3 . The high-pressure mineral assemblages are usually preserved within isolated blocks of eclogite or garnet peridotite, whereas the enveloping crustal rocks typically lack evidence of high-pressure conditions1–3 . Thus, a paramount question in reconstructing the geologic history of high-pressure domains is whether these nappes represent (1) units having different metamorphic histories that were mechanically juxtaposed within a subduction channel4–8,11 or (2) coherent terranes of pre-existing continental basement that underwent high-pressure metamorphism and exhumation as a whole2,3,14–16 (Fig. 1). The Adula nappe in the Lepontine Alps (Switzerland) has served as a natural laboratory for many studies addressing subductionzone processes4,5,11,13,14,17–20 . It comprises crustal gneisses, metasediments and mica schists, as well as mafic and ultramafic units including eclogites, amphibolites and peridotites13,14,17,19,20 . So far, peak-pressure conditions have been recognized in eclogites, associated garnet mica schists, and scarce garnet peridotites13,14,19,20 . These rocks show a gradient of southward-increasing pressure and temperature (Fig. 2), interpreted to reflect burial in a southwarddipping subduction zone during the Tertiary Alpine orogeny19,20 . After the high-pressure event, the entire unit was subjected to amphibolite-facies (low-pressure, high-temperature) conditions, with the intensity of the overprint also increasing to the south. However, previous geochronology yielded inconsistent results, so the timing of high-pressure metamorphism in the Adula nappe remains ambiguous. Eclogites and garnet peridotites from the southwestern part of the nappe yield ages between 42 and 35 Myr using Lu–Hf and Sm–Nd dating of garnet9,11 and U–Pb dating of zircon10 . In marked contrast, zircon grains from eclogites in the central and northeastern part of the nappe yield only Palaeozoic ages for the high-pressure stage12 (Fig. 2). These observations spurred models suggesting that the Adula nappe was not always a single coherent unit but rather comprises different tectonic slices that were metamorphosed at different times before final assembly5,11 (Fig. 1a). We have investigated an eclogite from the classic Trescolmen locality in the central Adula nappe (Fig. 2). Pressures and temperatures associated with the main eclogite-facies assemblages are about 2.1–2.2 GPa and about 680 ◦ C (ref. 20; Fig. 2). The sample investigated is composed of garnet, omphacite, minor amounts of quartz, euhedral amphibole, and rutile (Fig. 3). There is no sign of amphibolite-facies retrogression and the sample is feldspar free. Omphacite crystals are equigranular and chemically homogeneous, whereas garnet porphyroblasts exhibit strong chemical zonation and a bimodal grain-size distribution. A few large garnet grains up to 4 mm in diameter comprise dark cores and pale rims. A second population of smaller (0.1– 0.3 mm), euhedral garnet porphyroblasts is distributed throughout the sample. High-resolution X-ray maps confirm the presence of two generations (Fig. 3; Supplementary Fig. S1). Cores of the large porphyroblasts (grt1) are corroded, have oscillatory grossular zoning, and irregular, almandine + spessartine-rich and pyrope-poor patches. These relict cores are cross-cut by jagged fissures filled with grossular-rich garnet (grt2a), which also mantles grt1 cores. The outermost rim (grt2b) is again poorer in grossular component. The small, euhedral garnet population consists solely of grt2a (in cores) and grt2b (at rims). Both garnet generations contain rare inclusions of quartz, rutile and apatite. In addition, grt1 contains inclusions of Al-rich amphibole and grt2 contains omphacite. We interpret the grt1 population to have been partially resorbed at high temperature, thereby producing the fissures. We also attribute the patchy distribution of almandine, pyrope and spessartine components to this event, with 1 Steinmann-Institut, Universität Bonn, Bonn 53115, Germany, 2 Institut für Geologie und Mineralogie, Universität zu Köln, Köln 50674, Germany, 3 Institut für Mineralogie, Universität Münster, Münster 48149, Germany. *e-mail: [email protected]. 178 NATURE GEOSCIENCE | VOL 4 | MARCH 2011 | www.nature.com/naturegeoscience © 2011 Macmillan Publishers Limited. All rights reserved. NATURE GEOSCIENCE DOI: 10.1038/NGEO1060 a LETTERS b 0 20 20 40 40 (km) (km) 0 60 80 100 Unit containing separate ultra (high) pressure a rocks before they are welded together at shallow crustal levels 60 80 Unit comprising a large, coherent ultra (high) pressure body 100 Figure 1 | Two contrasting models for the exhumation mechanism of geological units comprising (ultra) high-pressure rocks. a, Small parts of the subducting slab are plucked off at various depths and then exhumed within a ‘subduction channel’ and welded into a megascale mélange at shallow crustal levels. b, Nappes are subducted and exhumed as coherent bodies. Hence, in model a only small parts of the nappe have reached (ultra) high-pressure conditions, whereas in model b the entire nappe is subjected to high-pressure conditions. a 9° A Bündnerschiefer Zürich Va: Vals 520 °C/ 1.3 GPa 580 °C/ 1.7 GPa About 330 Myr (U¬Pb) N Va Adula European margin Apulian margin Cf: Confin 570 °C/2.2 GPa 700 °C/1.9 GPa About 340 Myr (U¬Pb) Simano Cf Trescolmen A VL: Val Large About 370 Myr (U¬Pb) Le South Penninic ocean Tertiary intrusions A′ A′′ 10 km Simano VL ina nt ve Latitude (° N) 100 km Milano 46° 30′ IL Bergell Tr A′ Cv: Calvaresc About 370 Myr (U¬Pb) 46° 20′ Tr: Trescolmen 660 °C/2.2 GPa 700 °C/2.1 GPa About 370 Myr (U¬Pb) Cv Ga Suretta Tambo 46° 20′ Chiavenna Ga: Gagnone 740 °C/3 GPa About 40 Myr (Sm¬Nd) Ar: Alpe Arami 840 °C/3.2 GPa 1120 °C/5 GPa 1180 °C/5.9 GPa About 35 Myr (U¬Pb) About 39 Myr (Sm¬Nd) About 37 Myr (Lu¬Hf) 46° 10′ Ca: Caurit 720 °C/ 2.4 GPa Ar Ca Go Du Go: Gorduno 750 °C/2.3 GPa About 38 Myr(Lu¬Hf) Bergell Du: Duria 830 °C/3 GPa 830 °C/2.8 GPa About 35 Myr (U¬Pb) 46° 10′ 10 km A′′ Periadriatic (Insubric) line Southern Alps 9° 9° 30′ Longitude (° E) Figure 2 | Location of the Adula nappe and the Alp Trescolmen. a, Tectonic sketch map of the Adula nappe. Stars denote prominent eclogite or garnet peridotite localities. Rectangles illustrate a compilation of peak pressure–temperature conditions20 , as well as known high-pressure ages9–12 . Ambiguous Ar–Ar (ref. 22), K–Ar and Rb–Sr (ref. 23) data are not shown (Va, Vals; Cf, Confin; VL, Val Large; Tr, Trescolmen; Cv, Calvaresc; Ga, Gagnone; Ar, Alpe Arami; Go, Gorduno; Ca, Caurit; Du, Duria). Insets show an overview of the Alpine realm (top) and a tectonic cross-section through the Adula nappe20 (bottom; IL, Insubric line). the almandine+spessartine-rich areas representing the original grt1 composition. Other grt1 domains have apparently been subjected to diffusive re-equilibration. This view is corroborated by the observation that the spessartine content within the patches still reflects original growth zoning; that is, it consistently increases towards the grain centres as defined by the concentric, oscillatory grossular zoning. Garnet generations grt2a and grt2b clearly grew after the resorption event, with grt2a healing the fissures and forming new nuclei within the rock matrix. The presence of sharp chemical gradients between grt1 domains and the surrounding grt2 indicates that the aforementioned diffusive re-equilibration must have occurred before grt2 growth. Enclosed relics of grt1 in NATURE GEOSCIENCE | VOL 4 | MARCH 2011 | www.nature.com/naturegeoscience © 2011 Macmillan Publishers Limited. All rights reserved. 179 NATURE GEOSCIENCE DOI: 10.1038/NGEO1060 LETTERS a b Fe Mg omp A A grt am B B B B A A qtz c d Ca Mn A A B B B A A B 1 mm Oscillatory zoning e 0.7 A′ A Almandine Pyrope f 0.7 Grossular Spessartine B′ 0.5 X in garnet X in garnet 0.5 B 0.3 0.1 0.3 0.1 h g grt1 relics grt1 j i grt2b grt2a Figure 3 | Illustration of the different garnet generations in Trescolmen sample TRC1. a–d, Element maps of Fe (a), Mg (b), Ca (c) and Mn (d). In b, bluish colours are garnet (grt), green is omphacite (omp), yellow is amphibole (am) and black denotes quartz (qtz). e,f, Compositional cross-section through large (e) and small (f) garnet crystals. Location of cross-sections is indicated in a–d. g–j, Illustration of garnet generations. grt1 represents corroded garnet relics from a first (Variscan) orogenic cycle (g,h) that have been partially replaced and overgrown by two successive (Alpine) generations, grt2a (i) and grt2b (j). 180 NATURE GEOSCIENCE | VOL 4 | MARCH 2011 | www.nature.com/naturegeoscience © 2011 Macmillan Publishers Limited. All rights reserved. NATURE GEOSCIENCE DOI: 10.1038/NGEO1060 LETTERS Table 1 | Lu–Hf data obtained from the Trescolmen (Adula nappe) eclogite sample TRC1. Sample ID Fraction Lu (ppm) Hf (ppm) 176 Lu/177 Hf 176 Hf/177 Hf DH55 Whole rock 1 (selective tabletop digestion) Whole rock 2 (PARR bomb digestion) Omphacite Variscan garnet Variscan garnet Variscan garnet Variscan garnet Variscan garnet Variscan garnet Variscan garnet (purest sample) Variscan garnet Variscan garnet Alpine garnets ≤150 µm (purest sample) Alpine garnet ≤150 µm Alpine garnet ≤150 µm Alpine garnet ≥250 µm Alpine garnet ≥250 µm Alpine garnet ≥250 µm (impure garnet separate) Residue of whole rock 1 Residue of Variscan garnet Residue of Variscan garnet Residue of Variscan garnet Residue of Variscan garnet 0.662 0.221 0.4240 (13) 0.283987 (21) 1.27 6.04 0.02990 (9) 0.283074 (9) 0.0205 2.47 2.68 3.29 4.38 2.09 1.91 4.37 0.249 0.0496 0.0752 0.112 0.135 0.0392 0.0746 0.0889 0.01167 (11) 7.114 (23) 5.092 (18) 4.187 (16) 4.638 (4) 7.647 (24) 3.637 (11) 7.037 (25) 0.283171 (14) 0.32333 (14) 0.312218 (30) 0.30722 (11) 0.311691 (7) 0.32567 (16) 0.301684 (30) 0.327306 (36) 4.27 3.72 0.945 0.0813 0.0759 0.0259 7.508 (23) 7.013 (23) 5.174 (18) 0.327553 (30) 0.326723 (46) 0.286748 (44) 0.960 1.02 0.965 0.951 0.974 0.0259 0.0266 0.0294 0.0274 0.0558 5.272 (17) 5.442 (3) 4.665 (14) 4.939 (16) 2.478 (8) 0.287067 (54) 0.287197 (26) 0.287089 (15) 0.287077 (56) 0.285292 (63) – – – – – – – – – – 0.0001875 (7) 0.001832 (6) 0.0009642 (71) 0.001369 (8) 0.002141 (9) 0.283022 (9) 0.283038 (14) 0.282959 (22) 0.283067 (25) 0.283063 (29) DH78 DH61 DH53 DH62 DH63 DH134 DH156 DH157 DH158 DH159 DH160 DH161 DH64 DH133 DH54 DH65 DH66 DH55-R DH53-R DH156-R DH157-R DH159-R Reported uncertainties on the last decimal places (in parentheses) are the estimated 2σ external reproducibility for 176 Lu/177 Hf and 2σm internal run statistics for 176 Hf/177 Hf. For the isochron regressions, the empirical relationship between external and internal uncertainties was employed, where the 2σ external uncertainties of 176 Hf/177 Hf are about twice the 2σm internal analysis statistics27 . External reproducibility for 176 Lu/177 Hf of ±0.25% (2σ ) includes average error magnification for over- or under-spiked samples. ‘Residues’ are the undigested fraction left after the selective dissolution of whole rock and garnet by the tabletop procedure. grt2-filled fissures are as small as 10 µm and still preserve their distinct chemical composition. We separated several garnet fractions by hand picking dark red fragments of grt1 and light red, euhedral crystals of grt2 in two different grain sizes. Two different digestion methods were applied, one of which, in steel-jacketed Teflon bombs (PARR bombs), ensures full sample digestion21 , whereas a tabletop digestion method efficiently dissolves garnet while leaving behind refractory Hf-bearing phases such as zircon and rutile21 . The undigested refractory minerals (residues) from the tabletop digestion were rinsed several times and then digested in PARR bombs. The Lu–Hf data from the different garnet separates define two well-constrained arrays in 176 Hf/177 Hf versus 176 Lu/177 Hf space, documenting two distinct metamorphic events (Table 1; Fig. 4). Eight out of nine grt1 fractions yield Carboniferous ages (336–299 Myr), whereas <150 µm grt2 fractions consistently define Eocene ages (40–37 Myr). We interpret the Eocene age to date prograde growth of grt2 as Alpine peak-pressure conditions were approached, whereas the Carboniferous age may represent growth or re-equilibration of grt1. As our physical separation of the two main garnet generations was not perfect, the Variscan and Alpine isochrons strictly represent minimum and maximum ages, respectively. There is clear evidence for contamination of >250 µm grt2 fractions by grt1 inclusions, as the former clearly plot above the isochron defined by the smaller grain size fractions of grt2 (<150 µm). Although not visible in thin section, there is probably a minor grt1 component in the <150 µm grt2 fractions as well, as evident from a slight scatter in 176 Hf/177 Hf that is not correlated with 176 Lu/177 Hf. Assuming that the grt2 fraction having the lowest 176 Hf/177 Hf at a given 176 Lu/177 Hf is the least contaminated, we obtain a maximum garnet–omphacite isochron age of 37.10 ± 0.94 Myr for the Alpine event. Alternatively, an age of 38.5 ± 2.5 Myr is calculated using the residues of grt1 and the purest grt2 fraction. As residual components of grt1 cores preserve unradiogenic Hf that was not available when new garnet formed during Alpine eclogite-facies metamorphism, the use of this low Variscan initial 176 Hf/177 Hf is probably unrealistic. Nevertheless, it constrains a firm upper age limit for Alpine garnet growth. Analogous to our reasoning for grt2 fractions, we regard grt1 separates that tend towards lower 176 Hf/177 Hf at a given 176 Lu/177 Hf as being affected by the younger grt2 domains. A minimum age of 336.0 ± 3.3 Myr is obtained for the older event by an isochron defined by grt1 separates with the comparatively highest 176 Hf/177 Hf and the solid residues that remained after garnet dissolution. The residues consist of >99% rutile and should have preserved a Variscan initial Hf isotope composition. Using the fully digested whole rock instead of the residues for isochron regression yields an identical age of 337.1 ± 1.3 Myr. Eclogites from Trescolmen can now be shown to have been subjected to the high-pressure phases of two orogenic cycles17 , a history that may also apply to the entire basement of the Adula nappe, as we will argue below. The Variscan ‘minimum’ age of 332.7 Myr is consistent with more precise U–Pb zircon ages of about 370 Myr typically found at Trescolmen12 . These 370 Myr ages probably reflect the true timing of garnet growth because they NATURE GEOSCIENCE | VOL 4 | MARCH 2011 | www.nature.com/naturegeoscience © 2011 Macmillan Publishers Limited. All rights reserved. 181 NATURE GEOSCIENCE DOI: 10.1038/NGEO1060 LETTERS a 0.33 ag e 0.31 im um 0.30 Age = 37.1 ± 0.94 Myr (176Hf/177Hf)i = 0.283163 ± 0.000027 M in 176Hf/177Hf 0.32 Age = 336.0 ± 3.3 Myr (176Hf/177Hf)i = 0.283020 ± 0.000034 MSWD = 3.3 0.29 Maximum 0.28 age b 0 2 4 6 8 10 176Lu/177Hf b 0.2835 Age = 336.0 ± 3.3 Myr (176Hf/177Hf)i = 0.283020 ± 0.000034 0.2834 MSWD = 3.3 176Hf/177Hf 0.2833 0.2832 0.2831 Age = 37.1 ± 0.94 Myr (176Hf/177Hf)i = 0.283163 ± 0.000027 0.2830 0.2829 0 0.01 0.02 0.03 176Lu/177Hf WR1 (tabletop) WR2 (PARR bomb) Omphacite grt1 grt2 ≤ 150 μm grt2 ≥ 250 μm Residue of WR1 Residues of grt1 Figure 4 | Isochron plots illustrating the different ages obtained for two garnet generations present in eclogite sample TRC1 from Trescolmen. a, A six-point isochron defined by the purest (with respect to different garnet generations) grt1 separate, four residues of grt1 fractions and one whole-rock residue (WR1) yields a Variscan age of 336.0 ± 3.3 Myr. A two-point isochron defining an Alpine age of 37.10 ± 0.94 Myr is obtained from the purest grt2 fraction and the omphacite separate. MSWD = mean square of weighted deviates. b, Close-up showing the low-Lu/Hf analyses. were interpreted to reflect high-pressure conditions12 . The Eocene ‘maximum’ age of 38 Myr is consistent with high-pressure ages determined by Lu–Hf (ref. 11), Sm–Nd (ref. 9) and U–Pb (ref. 10) chronometry in the southwestern Adula nappe (Fig. 2). It also concurs with Ar–Ar phengite ages (about 40.5 Myr; ref. 22) from the central Adula nappe as well as a prominent Rb–Sr phengite-age population (about 38–35 Myr; ref. 23) that has been interpreted to date the Alpine high-pressure event20,23 . As the intensity of Alpine metamorphic overprint increases towards the south, evidence of the Variscan metamorphism is best preserved in the northeastern part of the nappe. Fortunately, our sample from the central part of the nappe was only partially overprinted such that two distinct garnet generations are present. 182 Clearly, vestiges of Variscan metamorphism are preserved only as relict cores of garnet, whereas the rest of our eclogite has equilibrated to Alpine high-pressure conditions. Hence, the pressure and temperature estimates for the Trescolmen locality probably reflect Eocene conditions13,14,19,20 . This assumption is even more likely to apply for the southwestern Adula nappe where the Alpine overprint was even more pronounced. Although it cannot be resolved here whether the petrological features in the northern Adula nappe record Eocene or Palaeozoic conditions, it is simpler to attribute a coherent pressure–temperature gradient to a single event rather than to two. Collectively, we infer that the north-to-south pressure gradient in the Adula nappe is an entirely Alpine feature and may well reflect the position of the Adula nappe as a coherent unit in an Alpine subduction zone15,20 . Subduction as a coherent unit is also supported by our new age data because (1) Alpine high-pressure metamorphism is consistently dated as upper Eocene within a variety of rocks throughout the Adula nappe and (2) our Variscan high-pressure age in sample TRC1 clearly shows that this sample was part of the continental basement before the Alpine orogeny. These features would be expected for basement nappes that are subducted and exhumed as coherent slabs, whereas they must be viewed as rather coincidental in a mélange model. Although the continental host rocks in the Adula nappe generally lack evidence for deep subduction, ‘coherent unit type’ subduction models require that they must have been subjected to peak pressures similar to those of the associated eclogites2 . Regardless of whether these rocks had actually recrystallized to high-pressure assemblages, they would have had large buoyancies, contributing to fast exhumation1–3,24 . The complete absence of any diffusive re-equilibration between Variscan grt1 and Alpine grt2 populations during the entire Alpine cycle indicates that exhumation indeed occurred rapidly. As evident from the available age data, deep subduction of the Adula nappe did not commence until about 37 Myr ago and the unit reached peak-pressure conditions about 35 Myr ago10 , before it was exhumed to shallow crustal levels (0.55 GPa) about 33–32 Myr ago10,12 . Hence, it seems unlikely that the Trescolmen eclogites have resided in a deep subduction channel for several million years as proposed for other high-pressure rocks in the Adula nappe5,11 and elsewhere in the Alps6,7 . Our data support models where the Adula nappe represents a basement nappe that was subducted and rapidly exhumed as one coherent unit3,14–16,20 . The methods applied here can now be used to test for similar scenarios in other continental high-pressure and ultrahigh-pressure units in the Alps and elsewhere. Methods The eclogite sample was crushed and divided into two splits, one of which was powdered in an agate mill, whereas the other was processed for mineral separation. Two different digestion procedures were applied. (1) Selective dissolution of garnet, omphacite, and one whole-rock fraction (TRC1-WR1) efficiently dissolves major silicate phases, while leaving behind refractory, Hf-bearing accessory phases such as rutile and zircon21 . (2) One whole rock (TRC1-WR2) and the refractory mineral inclusions remaining after selective dissolution (‘residues’) were digested in Savillex vials placed inside steel-jacketed Teflon PARR bombs for 3–5 days at 180 ◦ C, ensuring full sample digestion21 . A mixed 176 Lu–180 Hf tracer was added before all digestions. The refractory mineral inclusions remaining from the selective tabletop digestion were rinsed repeatedly with 3N HCl and deionized water before respiking and digestion in PARR bombs. Separation of Lu and Hf from the rock matrix was achieved by Ln-Spec resin column chemistry25 . Lutetium and Hf measurements were carried out on a Finnigan Neptune multi-collector inductively coupled plasma mass spectrometer (MC-ICP-MS) at the Steinmann Institut, Bonn21,26 . Measured 176 Hf/177 Hf values are reported relative to 176 Hf/177 Hf = 0.282160 for the Münster Ames Hf standard, which is isotopically identical to the JMC-475 standard. For isochron calculations, the external reproducibility was estimated by the empirical relationship 2σ external reproducibility ≈4σm , where σm is the standard error of an individual analysis27 . An external reproducibility of ±0.2% (2σ ) for the 176 Lu/177 Hf is typical for ideally spiked sample solutions if naturally occurring Yb in the Lu cuts is used for mass bias and interference corrections26 . Isochron regressions and ages were calculated using ISOPLOT v.2.49 (ref. 28) and NATURE GEOSCIENCE | VOL 4 | MARCH 2011 | www.nature.com/naturegeoscience © 2011 Macmillan Publishers Limited. All rights reserved. NATURE GEOSCIENCE DOI: 10.1038/NGEO1060 λ176 Lu = 1.867 × 10−11 yr−1 (refs 29,30). Blanks for Lu and Hf ranged between 3–15 pg and 6–25 pg, respectively. Total amounts of Hf analysed ranged from 1.2 to 584 ng. Sample-to-blank ratios were all >80. The blank uncertainty results in slight variations of 176 Hf/177 Hf composition, but the effect on isochron ages is negligible. Electron microprobe analyses were carried out using the JEOL-JXA-8900 at the Steinmann Institut, Bonn. Received 3 March 2010; accepted 7 December 2010; published online 23 January 2011 References 1. 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C.M., N.F. and E.E.S. substantially contributed to the study design, data evaluation and interpretation. E.E.S. developed the selective digestion method and C.M. developed the column chemistry and the analytical protocol. D.H. and T.J.N. wrote the manuscript and contributed equally to the study. Additional information The authors declare no competing financial interests. Supplementary information accompanies this paper on www.nature.com/naturegeoscience. Reprints and permissions information is available online at http://npg.nature.com/reprintsandpermissions. Correspondence and requests for materials should be addressed to D.H. NATURE GEOSCIENCE | VOL 4 | MARCH 2011 | www.nature.com/naturegeoscience © 2011 Macmillan Publishers Limited. All rights reserved. 183
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