unraveling crustal growth and reworking processes in

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Precambrian Research 267 (2015) 285–310

Contents lists available at ScienceDirect

Precambrian Research

jo ur nal homep ag e: www.elsev ier .com/ locate /precamres

nraveling crustal growth and reworking processes in complexircons from orogenic lower-crust: The Proterozoic Putumayorogen of Amazonia

auricio Ibanez-Mejiaa,∗, Alex Pullena,b, Jesse Arensteinc, George E. Gehrelsa,ohn Valleyd, Mihai N. Duceaa,e, Andres R. Moraf, Mark Pechaa, Joaquin Ruiza

Department of Geosciences, The University of Arizona, Tucson, AZ 85721, USADepartment of Earth and Environmental Sciences, University of Rochester, Rochester, NY 14627, USAAlicat Scientific Inc., Tucson, AZ 85743, USAWiscSIMS, Department of Geoscience, University of Wisconsin, Madison, WI 53706, USAUniversitatea Bucuresti, Facultatea de Geologie Geofizica, Str. N. Balcescu Nr 1, Bucuresti 010041, RomaniaInstituto Colombiano del Petroleo ICP-ECOPETROL, Piedecuesta, Santander, Colombia

r t i c l e i n f o

rticle history:eceived 6 March 2015eceived in revised form 3 June 2015ccepted 23 June 2015vailable online 2 July 2015

eywords:–Pb–Hf–Omazoniaodiniautumayo Orogenrustal evolution

a b s t r a c t

High-grade basement massifs exposed in the northern Andes and the buried basement of the adjacentPutumayo foreland basin contain a record of Amazonia’s involvement in the supercontinent Rodinia.Metasedimentary granulites and orthogneisses, strongly deformed during at least one metamorphicepisode dated at ca. 0.99 Ga, provide critical information on the pre-collisional history of the Mesopro-terozoic continental margin. Here, new U–Pb, Lu–Hf, Sm–Nd and O isotopic data from outcrop samples ofthe Garzón and Las Minas Cordilleran basement massifs as well as fragments of drill-core recovered fromthe Putumayo basin basement are reported. We explore the application of a dual-ICP-MS approach toobtain concurrent U–Pb and Lu–Yb–Hf information on complexly zoned zircon from orogenic lower-crust,and demonstrate its use to retrieve reliable pre-metamorphic information despite possible complexitiesintroduced by mixed-domain ablation and isotopic disturbance of the U–Pb system by thermally inducedrecrystallization. In combination with �18O compositions from the same zircon growth domains, andbulk-rock Nd isotope information, we reconstruct segments of the tectonic and crustal evolution of a long-lived accretionary orogen that developed along the (modern) NW margin of Amazonia during most of theMesoproterozoic. Inherited zircons in metaigneous samples from the Cordilleran massifs, with protolithcrystallization ages in the range from ca. 1.47 to 1.15 Ga, have Hf–O compositions that indicate significantcrustal reworking in their source region, but denote a trend of increasing 176Hf/177Hf with decreasing agethat can be attributed to rejuvenation by progressive addition of radiogenic components during this timeinterval. Detrital zircons within this same age range found in metasedimentary granulites of the Garzónmassif also follow this trend, further supporting previous inferences that their protoliths were depositedin arc-proximal basins with little to no coarse-grained detritus delivered from an older cratonic domain. Ashift in orogenic deformation style starting at ∼1.15–1.10 Ga, inferred to be associated with the accretionof fringing-arc terranes against the continental margin, triggered an early amphibolite-grade metamor-
phic episode; this was accompanied by pervasive partial melting and migmatite development in fertilemetasedimentary units and is interpreted to be responsible for enhanced crustal reworking evidenced
176 177
from the shallowing of Hf/ Hf vs. age trends in detrital and metamorphic zircons from the Garzónand Las Minas massifs. Convergent tectonism along the Putumayo margin came to an end during the finalincorporation of Amazonia to the core of the Rodinia supercontinent, possibly during collision againstthe Sveconorwegian segment of Baltica at 0.99 Ga. Although the position and role of Amazonia withinRodinia remains controversial, the new Nd and Hf isotope data provide additional evidence to link the
∗ Corresponding author at: Department of Earth, Atmospheric and Planetary Science, Massachusetts Institute of Technology, Cambridge, MA 02139, USA.el.: +1 6172532927.

E-mail address: [email protected] (M. Ibanez-Mejia).

ttp://dx.doi.org/10.1016/j.precamres.2015.06.014301-9268/© 2015 Elsevier B.V. All rights reserved.

dx.doi.org/10.1016/j.precamres.2015.06.014

http://www.sciencedirect.com/science/journal/03019268

http://www.elsevier.com/locate/precamres

http://crossmark.crossref.org/dialog/?doi=10.1016/j.precamres.2015.06.014&domain=pdf

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286 M. Ibanez-Mejia et al. / Precambrian Research 267 (2015) 285–310

evolution of this orogenic segment with the basement of Oaxaquia, as well as continue to draw funda-mental differences with the timing and nature of the tectonic processes associated with the developmentof the Sunsás-Aguapeí Orogen of SW Amazonia.

1

t(2ethsZrtadgms(aBithodic

ccptViff2gts(ccppopsgpecB2

iA

. Introduction

Zircon isotope geochemistry is fundamental to understandinghe formation and differentiation of continental crust on Earthe.g., Patchett et al., 1981; Valley et al., 2005; Belousova et al.,010; Dhuime et al., 2012; Cawood et al., 2013; Hawkeswortht al., 2013), but becomes increasingly challenging when appliedo fragments of strongly modified continental lithosphere thatave undergone poly-phase tectonic-thermal histories and perva-ive metamorphic recrystallization (e.g., Whitehouse et al., 1999;eh et al., 2007; Kemp et al., 2009a). High-temperature crustaleworking has the potential to induce multi-phase growth his-ories within single-zircon crystals, which complicate the agessignment to complementary geochemical indicators. However,espite their possible textural complexities, reliable primaryeochronologic and geochemical information can still be deter-ined from reworked zircon crystals owing to the extremely

low volume-diffusion properties of U–Pb–Hf–O in this mineralCherniak et al., 1997; Watson and Cherniak, 1997; Cherniaknd Watson, 2000, 2003; Peck et al., 2003; Page et al., 2007;owman et al., 2011). Therefore, the continuous improvement

n spatial resolution, precision, and accuracy of in situ radioiso-opic methods for studying minerals with multi-phase growthistories continues not only to revolutionize our understandingf the geochemistry of zircon, but also to provide unprece-ented insights into crust-forming and reworking processes at

ncreasingly finer resolutions in strongly deformed orogenicrust.

Continental collision tectonism has been inferred to play arucial role in the shaping and stabilization of Earth’s preservedontinental lithosphere (Hawkesworth et al., 2009), and exerted arimary control on the global detrital-zircon geochronologic pat-ern of ancient and modern sediments (Campbell and Allen, 2008;oice et al., 2011; Spencer et al., 2015). If major peaks and troughs

n the global detrital-zircon age distribution are indeed an arti-act of selective preservation instead of arising from changes inundamental crust-generating processes (e.g., Hawkesworth et al.,009, 2013; Condie et al., 2011), then further scrutinizing theeochemical and isotopic record of major pre-collisional orogenshrough time should provide fundamental insights into under-tanding the composition of Earth’s preserved continental crustRudnick and Gao, 2014). Furthermore, in addition to providinglues for evaluating the mechanisms responsible for long-termrustal differentiation, linkages between isotopic compositions andarticular tectonic processes can be used to impose robust tem-oral and geodynamic constraints on the developmental historyf complex and/or poorly represented orogens. This informationlays a critical role in the study of processes associated with theupercontinent cycle, as any proposed topological model for thelobal agglomeration of continental masses has to satisfy the tem-oral, tectonic, and structural constrains dictated by the geologicalvolution of lithospheric fragments formed prior, during and afterontinental collision (e.g., Dalziel, 1991; Pisarevsky et al., 2003;ogdanova et al., 2008; Li et al., 2008, 2009; Evans and Mitchell,011).

The recently defined Putumayo Orogen of northern South Amer-ca holds critical information for understanding the participation ofmazonia in the assembly of the supercontinent Rodinia (Cordani

© 2015 Elsevier B.V. All rights reserved.

et al., 2009; Ibanez-Mejia et al., 2011), and the role that Mesopro-terozoic accretionary orogenesis had in the growth of one of Earth’slargest Precambrian landmasses (Cordani and Teixeira, 2007). Inorder to elucidate the Proterozoic crustal development history ofthe NW Amazon Craton and to provide a more comprehensiveunderstanding of its role within Mesoproterozoic tectonics, weapplied a combination of texturally resolved U–Pb, Lu–Hf and Oisotopic techniques to investigate the record of complex polycyclicmeta-igneous and meta-sedimentary zircon crystals from high-grade rocks of the Putumayo Orogen. These results, complementedby bulk-rock Nd isotopic data, are used to reconstruct segmentsof a long-lived history of Mesoproterozoic convergent tectonismalong this segment of the Amazonian margin, as well as draw stronggeochronologic and isotopic correlations between the now dis-membered fragments that have been proposed to once make anintegral part of this orogen. In an effort to assign the most reli-able U–Pb ages to each Lu–Hf isotopic composition, a critical steptoward accurately interpreting such data, U–Pb and Lu–Yb–Hf iso-topic data were simultaneously acquired from the same ablatedzircon volumes by a laser ablation dual-ICP-MS approach calibratedat the University of Arizona during the course of this study. Weshow that this analytical strategy offers the possibility to study avariety of processes such as igneous and metamorphic petrogene-sis, detrital-zircon provenance, and paleogeographic developmentof orogenic crustal fragments where complex zircon growth his-tories are the end result of their poly-phase tectonothermalevolutions.

2. Tectonic context of the Putumayo Orogen and samplinglocations

The Amazon Craton, commonly referred to as Amazonia(Fig. 1A), is thought to be one of the major Precambrian continentalnuclei that occupied the core of the Rodinia Supercontinent duringthe late Meso- to early Neoproterozoic (Hoffman, 1991; Li et al.,2008; Cordani et al., 2009). The occurrence of a late Mesoprotero-zoic collisional metamorphic belt in the lowlands of eastern Boliviaand western Brazil, the Sunsás-Aguapeí belt, has traditionallyprovided support for this idea (Litherland and Bloomfield, 1981;Teixeira et al., 1989, 2010). Although paleogeographic, geochrono-logic and paleomagnetic evidence indicate the Grenville margin ofLaurentia as a feasible hypothesis for a conjugate collisional marginto the Sunsás, debate still persists over the specific segment of Lau-rentia against which Amazonia collided (Sadowski and Bettencourt,1996; Tohver et al., 2002, 2004, 2006; Loewy et al., 2003; D’Agrella-Filho et al., 2008; Gower et al., 2008; Johansson, 2009, 2014). Apossible northern continuation of the Sunsás belt along the fringeof the Amazon Craton has been contentious, as fragments of lateMesoproterozoic crust east of the Andean deformation front inmodern-day Peru, Ecuador, and Colombia had not been previouslyrecognized (Fig. 1A). There is now, however, growing geologicaland geochronological evidence that supports the existence of acollisional Stenian–Tonian orogenic belt hidden under the northAndean foreland basins in northwestern South America, herein
called the Putumayo Orogen, which provides important new con-straints for the role of Amazonia prior and during the assembly ofthe Rodinia supercontinent.

brian

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M. Ibanez-Mejia et al. / Precam

.1. North Andean Precambrian basement massifs

High-grade Precambrian basement massifs of late Meso- toeoproterozoic age comprise the basement of the Eastern and por-

ions of the Central Cordilleras of the Colombian Andes (Fig. 1A;roonenberg, 1982; Priem et al., 1989; Restrepo-Pace et al., 1997;ordani et al., 2005; Jimenez Mejia et al., 2006; Cardona et al.,010; Ibanez-Mejia et al., 2011). Despite their modern geographic

ocation in the NW South American margin, intense segmentationaused by Phanerozoic deformational events, including significanttrike-slip displacement along the Meso-Cenozoic proto-AndesBayona et al., 2006, 2010), has made their interpretation a chal-enging task within the context of Amazonia and greater Rodiniaeconstructions (Cardona et al., 2010). Crustal development of theorth Andean Precambrian basement massifs prior to Neoprotero-oic collisional deformation took place within an active marginetting possibly along the western edge of Amazonia (Cardonat al., 2010 and references therein). Although faunal assemblages inaleozoic sequences that overlie the Garzón, La Macarena, and Lasinas massifs (Fig. 1) provide evidences to support a NW Gond-anan affinity of these basement domains by early Phanerozoic

imes (Harrington and Kay, 1951; Forero-Suarez, 1990; Ordonez-armona et al., 2006; Borrero et al., 2007; Moreno-Sanchez et al.,008a, 2008b), Proterozoic correlations with the proximal non-emobilized cratonic basement are hampered by the lack of isotopic
ata from a coeval orogenic belt east of the Andean deformationomains.
Compelling geochronologic and isotopic evidence has beenound to establish Proterozoic tectonic correlations and a shared

ig. 1. Location of the study area within the context of the Amazon Craton. (A) Tectonrchitecture and highlighting one model for the provinces of Amazonia (after Ibanez-Meji2007) and Fuck et al. (2008). Distribution of crustal fragments interpreted as associated toelt. (B) Digital elevation model of SW Colombia and N Ecuador showing the location of dith respect to the Garzón massif (DEM image and outline of major rivers from http://julalley (UMV) area with emphasis on exposed Precambrian units and showing sampling lore: (a) volcanic/plutonic rocks of Jurassic age, (b) Paleozoic clastic sedimentary rocks, (c)

o as “El Vergel” unit), (d) metaigneous rocks of the Guapotón-Mancagua orthogneiss, (e)g) metaigneous rocks of the Las Minas orthogneiss.

Research 267 (2015) 285–310 287

metamorphic evolution of the Andean massifs with the Precam-brian basement exposures of Mexico, specifically those includedin what is known as the Oaxaquia terrane (Ortega-Gutierrez et al.,1995; Restrepo-Pace et al., 1997; Ruiz et al., 1999; Weber et al.,2010). Similarly to the north Andean Precambrian massifs, the Oax-aquian basement is also characterized by a protracted late Meso- toearly Neoproterozoic history of back-arc related magmatism, sedi-mentation, intrusion of intermediate to acidic volcanic-arc plutons,massif-type anorthosite–mangerite–charnockite–rapakivi granite(AMCG) magmatism, and Tonian granulite-facies metamorphism(Patchett and Ruiz, 1987; Ruiz et al., 1988, 1999; Ortega-Gutierrezet al., 1995; Lawlor et al., 1999; Weber and Köhler, 1999; Keppieet al., 2001, 2003; Lopez et al., 2001; Solari et al., 2003, 2013; Weberand Hecht, 2003; Cameron et al., 2004; Keppie and Dostal, 2007;Keppie and Ortega-Gutierrez, 2010; Weber et al., 2010). Thesevarious geochronological, isotopic and structural evidences couldprovide the tectonic framework to reconstruct a long-lived Meso-proterozoic history of convergence along the NW portion of theAmazonian margin, if evidences from an autochthonous belt in thisregion of South America can be reconciled with the geologic evolu-tion of the joint Oaxaquian-North Andean Precambrian basement.

In this study, we provide new data from metaigneous andmetasedimentary units exposed within the Garzón, Las Minas andLa Macarena massifs (Fig. 1). The western segment of the Garzónmassif is dominantly comprised by a banded sequence of metased-
imentary migmatites and granulites of the “El Vergel” unit andhornblende-biotite augen gneisses of the “Guapotón-Mancagua”orthogneiss (Fig. 1C; Kroonenberg, 1982; Jimenez Mejia et al.,2006). We studied one sample of a felsic orthogneiss from the
ic overview of the South American continent with emphasis on its Precambriana et al., 2011), modified from Tassinari and Macambira (1999), Cordani and Teixeira

the Putumayo Orogen are shown as: AB – autochthonous belt, and RB – remobilizedrilling-sites in the north Andean foreland discussed in this study, and their positiones.unavco.org/Voyager/Earth). (C) Detailed geological map of the Upper Magdalenacations from the Garzón and Las Minas massifs. Stratigraphic units shown in figuremigmatites and granulites of the “El Vergel granulites” unit (hereafter only referred

Toro gneiss, (f) metasedimentary migmatites of the “El Zancudo migmatites” unit,

http://jules.unavco.org/Voyager/Earth






2 brian

GcMtmaeoITi“SpfCtbsetisTcpt(

2

AaEToohce2arTtul–tatpseuiftttfggt

88 M. Ibanez-Mejia et al. / Precam

uapotón-Mancagua unit (sample MIVS26), one sample from a leu-osome of a stromatic migmatite within the El Vergel unit (sampleIVS16A), a deformed granitic pegmatite spatially associated to

hese migmatites (sample MIVS15A), and two massive metasedi-entary granulites also from the El Vergel unit (samples MIVS12

nd MIVS13). Located to the west of the Garzón massif, in the east-rn flank of the Central Cordillera, the Las Minas massif consistsf a core of meso- and leucocratic augen gneisses denominated bybanez-Mejia et al. (2011) as the “Las Minas” orthogneiss (Fig. 1C).his unit is overlain by a series of stromatic metatexites of metased-mentary origin denominated by Ibanez-Mejia et al. (2011) as theEl Zancudo” migmatites, best exposed in the eastern flank of theerrania de Las Minas range. We provide new data from one sam-le of the Las Minas orthogneiss (sample MIVS41) and one samplerom a melanosome of the Zancudo stromatic metatexites (sampleB006). The Serrania de La Macarena range is a basement uplifto the north of the Putumayo basin, exposed along a series ofasement-high structures that divide the Putumayo basin to theouth and the Llanos basin to the north (Fig. 1B and C). Due to thextremely difficult access to this area in the Andean foothills junglehe Serrania de La Macarena still remains very poorly mapped, butts core is known to consist of a series of mylonitic gneisses andchists crosscut by deformed syenogranitic dikes (Gansser, A., inrumpy, 1943). We analyzed one sample of a mylonitic gneiss unitollected in the northeastern flank of the La Macarena uplift (sam-le Macarena2). For a more detailed description of these samples,he interested reader is referred to the study of Ibanez-Mejia et al.2011) and the supplementary material to this article.

.2. The Northwestern Amazon Craton

The Guyana Shield, exposed over a vast area in northern Southmerica, comprises the northern half of the larger Amazon Cratonnd is offset from the southern half (the Guaporé shield) by the–W trending Amazon River graben (Fig. 1A; Teixeira et al., 1989;assinari and Macambira, 1999; Cordani and Teixeira, 2007). Previ-us workers have shown that this shield exhibits a general patternf westward younging basement domains with Paleoproterozoicigh-grade gneiss, granite-greenstone belts and supracrustal vol-anic sequences associated to the Transamazonian orogeny in theast (e.g., Santos et al., 2000; Teixeira et al., 2002; Roever et al.,003; Delor et al., 2003; Fraga et al., 2009; Hildebrand et al., 2013)nd younger Paleo- to Mesoproterozoic granite-gneiss terranes andapakivi granites dominating in the west (Gaudette et al., 1978;assinari et al., 1996; Ibanez-Mejia et al., 2011). In proximity tohe Andean fold and thrust belt, the shield flexurally subsidednder the load of this thickened active orogen, and a series of

arge retroarc foreland basins – the Llanos and Putumayo basins have buried a sizable portion of the Precambrian basement inhis area (Fig. 1A and B; Milani and Thomaz Filho, 2000). In thebsence of basement outcrops, the only evidences available onhe age and nature of the craton beneath the Cenozoic cover arerovided by deep exploratory wells that reach the bottom of theometimes kilometer-thick sedimentary successions (e.g., Kovacht al., 1976; Feo-Codecido et al., 1984). Deformed granitoids andpper-amphibolite to granulite-facies metaigneous and metased-

mentary rocks recently described from wells in the Putumayooreland basin of south-central Colombia (Fig. 1A and B), providedhe first direct evidence to support the occurrence of a sizable Meso-o early Neoproterozoic collisional belt hidden along this margin ofhe Amazon Craton (Putumayo Autochthonous Belt – AB – Fig. 1A;
rom Ibanez-Mejia et al., 2011). Furthering our understanding of theeochronologic and isotopic characteristics of this belt can provideeological constraints that might serve as piercing points to tracehe history of the Oaxaquian and North Andean terranes back to an
Research 267 (2015) 285–310

Amazonian ancestry, which is one of the objectives of the presentcontribution.

This study provides new U–Pb geochronologic and Nd–Hf–O iso-topic results on some of the basement drill-core samples previouslyreported by Ibanez-Mejia et al. (2011), namely from the Mandur-2,Payara-1, and La Rastra-1 exploratory wells. All these wells weredrilled in the Putumayo foreland basin just east of the GarzónCordilleran massif and south of the La Macarena uplift (Fig. 1Aand B), and pierced the crystalline basement at depths between∼940 and 1700 m below the modern day surface east of the modernAndean deformation front.

3. Analytical methods

3.1. Zircon oxygen isotopes by SIMS

Oxygen isotope measurements on zircon crystals were per-formed by secondary ion mass spectrometry (SIMS), using aCAMECA IMS-1280 at the University of Wisconsin WiscSIMS Lab-oratory. Details on the sample preparation, analytical proceduresand data processing strategies are discussed in detail by Kitaet al. (2009) and Valley and Kita (2009). Zircons were mountedin epoxy plugs within a 0.5 cm radius from the center, wherelarge fragments of the KIM5 zircon reference crystal were located(�18O = 5.09‰ VSMOW; Valley, 2003). Fragments of the SL2, R33,Mud Tank, Plesovice and FC-1 reference zircons were placed aroundthe margin of the unknowns, so U–Pb–Hf measurements on thesame crystals analyzed for oxygen isotopes could later be obtainedfrom these sample mounts. All samples were imaged by cathodo-luminescence using a secondary electron microscope (SEM-CL)prior to isotopic analysis in order to reveal their internal zoningstructures. SIMS data was acquired prior to laser ablation splitstream–inductively coupled plasma–mass spectrometry (LASS-ICP-MS) in order to avoid possible sample topography-inducedinaccuracies in the oxygen isotope measurements that could arisedue to the presence of laser ablation craters in the crystals (Kitaet al., 2009). Analyses were conducted using a 10 �m diameter Cs+

primary ion-beam with a 1.5–2.0 nA current and using a normallyincident electron gun for charge compensation. The secondary-ionaccelerating voltage was set to 10 kV, and measurements of 16Oand 18O were conducted simultaneously in two Faraday cup detec-tors. Corrections for instrumental mass fractionation (IMF) biaseson the raw measured �18O values were conducted by referencematerial (RM) sample bracketing using repeated analyses of theKIM5 crystal; six analyses of KIM5 were conducted at the beginningand at the end of each session, with another four measured every12 unknowns. The average value of eight KIM5 analyses bracket-ing each set of unknowns was used to correct the latter for IMF,and the individual spot uncertainties for all analyses are reportedas the external reproducibility of the particular set of RM analysesused for IMF correction (i.e., 2 S.D. of the eight bracketing KIM5analyses). All IMF-corrected values reported here and discussedthroughout the text are quoted in �18O notation with respect toVSMOW. After oxygen isotope analyses were performed, but beforeU–Pb–Hf analysis, all ion-probe sputtering pits were carefully eval-uated by back-scattered electron imaging (SEM-BSE) in order toidentify possible complexities that could compromise the accuracyof individual �18O measurements (Cavosie et al., 2005). Accord-ingly, pits that intersected obvious cracks and/or inclusions or thatoverlapped zircon growth domains were excluded from calcula-
tions of the mean �18O values. Analyses conducted in areas wheresubsequent U–Pb analyses exhibited discordance of a magnitudegreater than 10% were also avoided for establishing primary zircon�18O compositions.

M. Ibanez-Mejia et al. / Precambrian

Fig. 2. Schematic diagram showing the configuration of our laser ablation “split-stream” (LASS-ICP-MS) setup. Details of instrumental operating conditions andbalancing of gas flows are provided in Table 1 and in the analytical appendix.

Table 1Instrument operating parameters used in this study for: (a) mass-spectrometers and (b) lcollected masses on the Element2 and measuring parameters.

(a) Instrument operating parameters – mass spectrometersManufacturer Nu instrumentModel Nu Plasma I

Forward power 1300 W

Mass resolution Low

Cooling gas flow (SLPM Ar) 13.0

Auxiliary gas flow (SLPM Ar) 0.800

Sample gas flow (SLPM Ar) 1.200

Total flow on MFM1 to Nu Plasma (see Fig. 2) ∼1.468

Ion-counting deadtime (E2 only) –

Analog calibration factor (E2 only) –

(b) Instrument operating parameters – laser ablationManufacturer Photon MachinesModel Analyte G2Type 193 nm – ArF ExcimerEnergy fluence 7 J/cm2

Energy attenuation 8%Repetition rate 7 HzNumber of pulses 560Spot diameter 40-50 �mAblation depth ∼30 �m (from opticalMass Flow Controller 1 (Helex) 0.050 SLPM HeMass Flow Controller 2 (Cell volume) 0.340 SLPM He

(c) Collector configuration and measured masses in the Nu Plasma MC-ICP-MS

H2 Ax L1 L2 L3

180Hf 179Hf 178Hf 177Hf 176Hf176Lu176Yb

(d) Measured masses and dwell-times in the Element-2 SC-ICP-MS

238U 232Th 208Pb

Dwell time (ms) 5 1 1

Collection mode Both Counting Counting

No. of samples/peak 4 4 4

Research 267 (2015) 285–310 289

3.2. Zircon U–Pb–Hf coupled isotopic analyses

Analyses of the U–Pb and Yb–Lu–Hf isotopic compositions ofzircon presented in this study were all conducted at the ArizonaLaserchron Center (ALC; www.laserchron.org) at the Univer-sity of Arizona. Two plasma-source mass-spectrometers, a singlecollector–inductively coupled plasma–mass spectrometer (SC-ICP-MS) and a multicollector–inductively coupled plasma–massspectrometer (MC-ICP-MS), were simultaneously connected to asingle ArF Excimer laser ablation (LA) system in order to obtainconcurrent U–Pb and Yb–Lu–Hf isotopic measurements from thesame volumes of ablated zircon material. A schematic diagramillustrating our analytical configuration is shown in Fig. 2; the SC-ICP-MS used was a Thermo-Finnigan Element2 equipped with anenhanced-sensitivity ‘Jet interface’, and the MC-ICP-MS a Nu Instru-ments Plasma I equipped with 12 fixed faraday detectors using3 × 1011 � resistors. Details on the instrumental parameters, col-lector configuration for Yb–Lu–Hf measurements, scanned masseson the Element2 and their respective dwell-times, are summarizedin Table 1. Given that this is the first contribution from the ALClab using this laser ablation ‘split-stream’ approach (abbreviatedLASS-ICP-MS herein), only a brief description of the method is givenin this section whereas a more extensive explanation of the pro-cedures is provided as an analytical appendix. A series of zirconreference crystals with a wide range of U–Pb ages and U concentra-tions previously determined by ID-TIMS, 176Hf/177Hf compositionsobtained by solution-MC-ICP-MS, and HREE concentrations, were
analyzed during the course of this study in order to validate the pre-cision and accuracy of the obtained results. A summary of the U–Pband Lu–Hf results determined from reference crystals during thecourse of this study, showing the consistency with their respective
aser-ablation system. (c) Detector configuration used in the multicollector and (d)

s Thermo-FinniganElement21200 WLow (400)16.00.8001.507–16 ± 3 nsAuto

interferometry)

L4 L5 L6 L7 L8

174Hf175Lu

173Yb 172Yb 171Yb

207Pb 206Pb 204(Pb + Hg) 202Hg

9 6 4 2Counting Counting Counting Counting4 4 4 4

http://www.laserchron.org/




Table 2Summary of U–Pb and Lu–Hf isotopic compositions obtained for secondary zircon reference crystals during our LASS-ICP-MS session.

Zircon name U–Pb age (Ma)a Ref. ageb 176Hf/177Hf(0) ± 2 S.D. Ref. 176Hf/177Hf(0)b 176Yb interf (%)c

49127 134.1 ± 1.3/1.4 (n = 15, MSWD = 0.8)* ca. 136.4 (a) 0.282944 ± 47 (n = 15, MSWD = 0.9) N.A. 5–15Plesovice 338.7 ± 3.1/3.4 (n = 15, MSWD = 0.5)* 337.13 ± 0.37 (b) 0.282498 ± 41 (n = 15, MSWD = 0.6) 0.282482 ± 13 (b) 1–3Temora 417.0 ± 3.8/4.2 (n = 15, MSWD = 0.9)* 416.78 ± 0.33 (c) 0.282668 ± 56 (n = 15, MSWD = 1.2) 0.282686 ± 8 (h) 10–22R33 417.3 ± 3.6/4.0 (n = 13, MSWD = 0.9)* 419.26 ± 0.38 (c) 0.282764 ± 59 (n = 15, MSWD = 1.5) 0.282764 ± 14 (i) 7–5891500 1067 ± 12/13 (n = 13, MSWD = 1.8)** 1066.4 ± 0.3 (d) 0.282299 ± 66 (n = 15, MSWD = 1.4) 0.282313 ± 12 (i) 3–4FC-1 1104 ± 5/7 (n = 15, MSWD = 0.8)** 1098.8 ± 0.25 (e) 0.282182 ± 72 (n = 15, MSWD = 1.2) 0.282183 ± 12 (i) 2–35FC-52 1103 ± 5/7 (n = 15, MSWD = 1.1)** ca. 1099 (f) 0.282171 ± 93 (n = 15, MSWD = 2.3) ca. 0.282183 (f) 5–21OG-1 3467 ± 3/14 (n = 15, MSWD = 0.6)** 3465.4 ± 0.6 (g) 0.280630 ± 74 (n = 15, MSWD = 1.7) N.A. 6–25

a Uncertainties are 2�. * Reported age is the 206Pb/238U weighted-mean. ** Reported age is the 207Pb/206Pb weighted-mean.f. (a)

e head76Hf/1

bdc

Lttsee2rapatfsmtMloM(tr2s∼atia1

siIart2ifahpw(r�

b Reference values are ID-TIMS for U–Pb and solution-MC-ICP-MS for 176Hf/177Ht al. (2006), (e) Hoaglund, 2010, (f) similar to FC-1, (g) Stern et al. (2009), (h) Wood

c Isobaric interference of 176Yb calculated as Interf. (%) = 100 * ((176Yb/177Hf)Corr/(1

enchmark values, is presented in Table 2. Uranium–Pb concordiaiagrams and 176Hf/177Hf vs. 176Yb/177Hf plots for these referencerystals are provided as supplementary material.

One of the most critical corrections applied to LA-MC-ICP-MSu–Hf data is the subtraction of the 176Yb isobaric contribution tohe 176Hf mass. This correction, whose magnitude is proportional tohe relative HREE content of the analyzed zircon, commonly repre-ents an adjustment on the order of hundreds or even thousands ofquivalent �Hf units to the raw measured 176M/177M values (Chut al., 2002; Woodhead et al., 2004; Wu et al., 2006; Fisher et al.,011, 2014b). Therefore, it is extremely important that this cor-ection be accurately applied for the reported 176Hf/177Hf to haveny meaningful geological significance. Ytterbium corrections wereerformed using the isotopic compositions of Vervoort et al. (2004),nd the determination of an empirical instrumental bias factoro the ‘natural’ 176Yb/173Yb composition (see analytical appendixor details) achieved by repeated measurements of the Yb-dopedynthetic zircon crystals introduced by Fisher et al. (2011). Theean measured value from 80 analyses of these synthetic crys-

als during our LASS-ICP-MS session was 0.282131 ± 61 (2 S.D.,SWD = 2.0; Fig. 3), which is in close agreement and within ana-

ytical uncertainty from the reference solution-MC-ICP-MS valuef 0.282135 ± 7 (Fisher et al., 2011), and similar to the original LA-C-ICP-MS values reported by Fisher et al. (2011) of 0.282139 ± 53

2 S.D., MSWD = 2.5, n = 134). After Yb and Lu interference correc-ions were performed, all 176Hf/177Hf ratios were normalized withespect to a Mud Tank value of 0.282507 (Woodhead and Hergt,005; reported relative to a JMC-475 value of 0.282160); mea-urements of this reference crystal were performed twice every15 unknowns during the session. The mean measured value forll analyses of Mud Tank zircon performed during the course ofhis study was 0.282463 ± 50 (2 S.D., MSWD = 1.1, n = 107), whichs slightly lower than the accepted solution-MC-ICP-MS valuend indicates an average bias of ca. 4.4 × 10−5 in the measured76Hf/177Hf ratios. Such deviations of laser data from referenceolution values have been observed by different laboratories andnstruments in numerous previous studies (e.g., Wu et al., 2006;izuka et al., 2009; Fisher et al., 2014a; Kemp et al., 2015), and so

normalization procedure using a well characterized low-Yb–Lueference zircon crystal has been proposed as an effective wayo reduce the magnitude of inter-laboratory bias (Fisher et al.,014b). Furthermore, in order to monitor the accuracy of the Yb

nterference and Hf bias correction throughout the entire session,ragments of the R33 and FC-1 reference zircon were frequentlynalyzed along with the unknowns; these crystals are known toave elevated Yb/Hf ratios and are therefore well suited for this pur-ose. The mean values obtained for R33 and FC1 during our session
ere 0.282752 ± 46 (2 S.D., MSWD = 2.0, n = 118) and 0.282193 ± 61
2 S.D., MSWD = 2.1, n = 63), respectively. These values are accu-ate with respect to solution-MC-ICP-MS results to within ±0.5Hf and further validate the accuracy of our analytical routine

Mattinson et al. (1986), (b) Slama et al. (2008), (c) Black et al. (2004), (d) Schoene et al. (2004), (i) Fisher et al. (2014a,b).77Hf)Corr).

(also see results of secondary reference crystals presented inTable 2).

For the U–Pb analyses, weighted mean ages for cogenetic suitesof zircons (i.e., igneous samples or metamorphic rims) reportedin the Figures and Tables are quoted with two increasing lev-els of uncertainty in the form ±(A)/[B], where (A) represents theweighted-mean uncertainty calculated using the internal inte-gration and within-session normalization uncertainties, while [B]represents the total uncertainty on the mean including all othersources of systematic error (i.e., decay constant errors and pri-mary reference material calibration). Since all the data presented inthis study were acquired using the same analytical protocols andnormalized with respect to the same primary reference material(SL2 zircon), internal comparisons between our U–Pb geochrono-logic results can be performed using the level of uncertainty (A).However, the reader should be aware that for comparing theseresults with respect to external data acquired using different ageochronologic system (e.g., Ar–Ar), or normalized against a dif-ferent reference material (e.g., Plesovice zircon), the uncertaintylevel [B] should be preferred as it accounts for systematic sourcesof uncertainty which, in our case, are dominated by the calibrationof the primary reference material used for fractionation correction.For a detailed description of the procedures involved in these calcu-lations the interested reader is referred to the extended analyticalappendix.

3.3. Whole-rock Sm–Nd isotopes

Fresh whole-rock samples were crushed to a fine powder usinga shatter-box, and then dissolved in Savilex® vials with a hotconcentrated mixture of HF-HNO3. The dissolved samples werespiked with a mixed 147Sm–150Nd isotopic tracer (Ducea andSaleeby, 1998) and allowed to equilibrate on a hot-plate beforeion-exchange chromatography. The bulk REE’s were separated incation-exchange columns using AG50W-X4 resin, and then Sm andNd were separated using anion-exchange columns with LNSpec®

resin using ultra-pure 0.1 N and 0.5 N HCl. Sm and Nd were loadedonto single Re filaments using platinized carbon and resin beads,respectively. Isotopic analyses were carried out in a VG Sector mul-ticollector thermal ionization mass spectrometer (TIMS) equippedwith adjustable 1011 � Faraday collectors and a Daly photomul-tiplier. Concentrations of Sm and Nd were calculated by isotopedilution, and isotopic compositions were determined from thesame spiked run. Each individual analysis consisted of 100 integra-tions of the isotopic ratios, and uncertainties were calculated as thestandard error of the mean (2 S.E. = 2 S.D./

√100). Instrumental mass

discrimination was corrected by normalization with respect to thereference ratio 146Nd/144Nd = 0.7219, and repeat analyses of theLaJolla standard were used to monitor the accuracy of the measuredcomposition; the average 143Nd/144Nd value for this standard was

brian

0i

4v

UtoyoazarSsKaKatdatcap1tteemgitSHan(Ct

Frat


.511849 ± 4 (2SD). More details on the methods used are describedn Ducea and Saleeby (1998) and Otamendi et al. (2009).

. U–Pb and Lu–Hf systematics of complex zircon: pitfalls,isualization and interpretations

Various potential pitfalls on the interpretation of coupled–Pb–Hf isotopic data could be introduced by (a) complexities in

he U–Pb systematics of discordant zircon, (b) incorrect assignmentf ages to a particular Hf composition, or (c) from inadvertent anal-ses of mechanical mixtures caused by the simultaneous ablationf different growth-zoning domains. These complexities, whichre especially prevalent when dealing with multi-phase zonedircons from tectonically complex terranes, impose importantnalytical challenges that need to be considered for the accu-ate measurement and interpretation of U–Pb–Hf isotopic data.ome of these issues can be circumvented by the use of quasi-imultaneous U–Pb–Hf measurements (Woodhead et al., 2004;emp et al., 2009a), or fully simultaneous dual-mass spectrometrypproaches (Xie et al., 2008; Yuan et al., 2008; Tollstrup et al., 2012;ylander-Clark et al., 2013; Fisher et al., 2014a, this study). Thesenalytical strategies can help prevent incorrect age assignmentso Hf isotopic compositions and to identify mixing complexitiesuring excavation of the ablation pit. Nevertheless, even whenssuming that an accurately determined U–Pb isotopic composi-ion is adequately assigned to an accurate 176Hf/177Hf value, naturalomplexities in the isotope systematics can introduce further vari-bility. Post-crystallization thermal events affecting a zircon canerturb its radiogenic Pb (Pb*) composition (Mezger and Krogstad,997; Hoskin and Black, 2000; Valley et al., 2014), specially ifhe crystal has been partially amorphized by accumulated radia-ion damage (Cherniak et al., 1991; Murakami et al., 1991; Ewingt al., 2003). Ancient events of Pb-remobilization cause the appar-nt 207Pb/206Pb dates of affected grains to yield values that areeasurably younger (if Pb* is locally lost) or older (if Pb* is locally

ained) than their true age of primary crystallization, an issue thats specially problematic for the accurate determination of detri-al zircon ages (Nemchin and Cawood, 2005; Valley et al., 2006)uch complexities in the U–Pb system are relevant for interpretingf isotope systematics, especially when the latter are evaluatednd visualized in terms of �Hf values. Given the time-dependent
ature of the reference frame utilized for calculating �Hf valuesi.e., the theoretical 176Hf/177Hf composition of the chondritic –HUR – or bulk silicate Earth – BSE – reference frames at a givenime t; Patchett et al., 1981), the magnitude of this parameter is
ig. 3. Yb–Hf isotopic results for synthetic zircon crystals (Fisher et al., 2011) analyzed seetrieval of statistically undistinguishable 176Hf/177Hf values with increasing magnitudepplied 176Yb interference correction. Error bars for individual measurements are shownhis article for further details on how this interference correction is addressed.

Research 267 (2015) 285–310 291

strongly dependent on the age that is assigned for a particular Hfisotope composition, and therefore only minimum apparent �Hfvalues for any given apparent single-crystal date t can be retrieved.However, given the almost negligible changes in 176Hf/177Hf valuesthrough time that occur within a zircon, the determination of theinitial isotopic ratio is almost independent of age. Consequently,when dealing with complex zircons – particularly of detrital ori-gin – that have undergone important post-crystallization thermalevents, our ability to retrieve accurate initial �Hf values for thesecrystals might be severely impaired by complexities in their U–Pbsystematics, whereas establishing an accurate initial 176Hf/177Hfvalue is readily achievable (see discussion in Amelin et al., 2000).For this reason, all Hf isotope vs. age plots shown and discussedbelow are constructed in terms of 176Hf/177Hf vs. time insteadof using �Hf. Mean �Hf values are only reported for groups ofcogenetic zircon (e.g., igneous protoliths) for which a robust crys-tallization age could be calculated, as it should be evident that insuch cases the calculated �Hf(t) are likely accurate and not just aminimum estimate like in the case of single detrital zircon crys-tals. One of the samples analyzed in this study, MIVS-13, providesa good natural example to illustrate the implications of the abovediscussion and highlights the power of the LASS-ICP-MS techniqueto filter out extremely perturbed analyses that would otherwiseintroduce noise to the interpretation of detrital zircon U–Pb–Hfdata (Fig. 10).

Key to the application of Hf isotopic compositions in crustal evo-lution studies is the fact that different terrestrial reservoirs divergein terms of their 176Hf/177Hf signatures as a function of time, owingto their contrasting parent/daughter compositions and at a ratethat is proportional to their relative Lu enrichments (Patchett et al.,1981). Therefore, evaluating the rate of change in isotopic ratios (or,graphically, the slope) of a particular reservoir or group of genet-ically related rocks – or zircon crystals – as a function of time, isarguably as useful for the study of crustal evolution as accuratelydetermining their absolute 176Hf/177Hf ratio at the time of crystal-lization. The rate of these isotopic evolutionary trends (or slopes)can be directly linked to an apparent 176Lu/177Hf composition, andprovide not only valuable insights into the source(s) from whichthe samples were derived, but also the mechanisms responsiblefor these secular changes (Fig. 4).

Following from the discussion on ancient Pb-remobilization
above, inaccurate determinations of crystallization ages on a givensuite of zircon crystals due to ancient Pb-loss will result in horizon-tal 176Hf/177Hf(t) vs. time arrays, or an apparent evolutionary trendwith a slope of 176Lu/177Hf ≈ 0 (Fig. 4). This horizontal reference line
veral times during our analytical session using methods described in the text. Thes of Yb interference (expressed as 176Yb/177Hf) demonstrates the adequacy of the

at 95% confidence; the interested reader is referred to the analytical appendix of


Fig. 4. Schematic diagram of the different mechanisms that can cause changes in176Hf/177Hf compositions as a function of time for a particular crustal reservoir, andthe interpretations that can be derived from time-integrated apparent 176Lu/177Hfcompositions or trends in 176Hf/177Hf vs. time. See Section 4 in text for discussion.(For interpretation of the references to color in text, the reader is referred to thew

atoorslasooraiot2ac1Hm0Tittatircsldonewthf

Table 3Sample location coordinates and codes for those analyzed by LASS-ICP-MS usedthroughout the manuscript and in data repository (see text for details).

Codea Sample name Latitudeb Longitudeb IGSNc

(a) MIVS-26 N 2◦ 03′ 19.2′ ′ W 75◦ 42′ 47.6′ ′ IEURI0001(b) MIVS-41 N 2◦ 13′ 34.0′ ′ W 75◦ 50′ 30.3′ ′ IEURI0002(c) Macarena-2 N 3◦ 01′ 45.0′ ′ W 73◦ 52′ 13.5′ ′ IEURI0003(d) MIVS-15A N 2◦ 08′ 28.2′ ′ W 75◦ 36′ 44.7′ ′ IEURI0004(e) MIVS-16A N 2◦ 08′ 11.7′ ′ W 75◦ 36′ 55.7′ ′ IEURI0005(f), (g) Mandur-2 well N 0◦ 55′ 25′ ′ W 75◦ 52′ 34′ ′ IEURI0013 & 14(h) Payara-1 well N 2◦ 07′ 31′ ′ W 74◦ 33′ 36′ ′ IEURI0012(i) MIVS-12 N 2◦ 09′ 20.7′ ′ W 75◦ 35′ 27.4′ ′ IEURI0007(j) MIVS-13 N 2◦ 08′ 09.0′ ′ W 75◦ 35′ 22.7′ ′ IEURI0008(k) CB-006 N 2◦ 13′ 26.5′ ′ W 75◦ 50′ 22.0′ ′ IEURI0011

Solita-1 well N 0◦ 52′ 29′ ′ W 75◦ 37′ 21′ ′ IEURI0015La Rastra-1 well N 1◦ 09′ 58′ ′ W 75◦ 30′ 13′ ′ IEURI0016MIVS-37a N 2◦ 15′ 37.3′ ′ W 75◦ 49′ 49.9′ ′ IEURI0009

a Codes only used for samples analized by split-stream U-Pb-Hf.

used toward the reported mean values are provided as supplemen-

eb version of the article.)

lso represents a divide between contrasting geological processeshat can result in trends of decreasing 176Hf/177Hf over time (fieldf apparent time-integrated 176Lu/177Hf < 0; green area in Fig. 4)r its increase (field of apparent time-integrated 176Lu/177Hf > 0;ed and blue areas in Fig. 4). Because both 176Hf and 177Hf aretable and mass-dependent fractionation induced by typical geo-ogical processes is not analytically resolvable, the only way for

negative trend in 176Hf/177Hf(t) over time to be achieved is byignificant progressive addition of less radiogenic material (e.g.,lder crust) to a mixed source. This scenario could conceivablyccur in areas were extensive underplating of supracrustal mate-ials is a prevalent process induced by subduction erosion (Schollnd von Huene, 2007; Roberts et al., 2012), or where underthrust-ng of continental lithosphere along accretionary and collisionalrogens transports large volumes of old lithospheric crust intohe melt generation zone (e.g., DeCelles et al., 2009; Hacker et al.,011). Recent datasets and global data compilations show system-tic variations for the Lu/Hf compositions of different terrestrialrustal reservoirs (Vervoort and Patchett, 1996; Vervoort et al.,999, 2000; Plank and Langmuir, 1998; Rudnick and Gao, 2003;awkesworth et al., 2010); in general, it is observed that the meanodern Lu/Hf compositions of typical crust lie between 0.052 and

.224, or approximate 176Lu/177Hf between 0.0072 and 0.0312.herefore, positive 176Hf/177Hf vs. age trends (or apparent time-ntegrated 176Lu/177Hf values >0) can be further subdivided inwo fields; one that is characterized by small positive slopes withime-integrated 176Lu/177Hf values ≤0.0312 (red area in Fig. 4),nd the other one with steeper time-integrated slopes equivalento a 176Lu/177Hf ≥ 0.0312 (blue area in Fig. 4). Accordingly, time-ntegrated 176Lu/177Hf values between 0 and ∼0.0312 could beeasonably explained by radiogenic decay within a closed-systemrustal reservoir without the need of mixing with any externalources, whereas steeper trends (176Lu/177Hf ≥ 0.0312) would mostikely involve the progressive addition of a radiogenic componenterived from a depleted reservoir (e.g., depleted mantle) to theverlying crust. Lastly, vertical arrays in 176Hf/177Hf vs. age space, ifot derived from instrumental variations, incorrect 176Yb interfer-nce corrections of LA data, or domain convolution during ablation,ould represent geologically short-lived events of mixing between

wo compositionally contrasting sources that were not isotopically
omogenized. This simple geometrical construct serves as the basis
or some of our data interpretations discussed below.

b All cordinates in WGS-84 system.c International Geo Sample Number, www.geosamples.org.

5. Results

A total of 13 samples collected from the Garzón, Las Minas andMacarena massifs in the Northern Andes as well as from drill coresthat reached the basement of the Putumayo foreland basin wereanalyzed in this study (Fig. 1, Table 3). For some of these samples,U–Pb results obtained by LA-MC-ICP-MS have previously been pub-lished by Ibanez-Mejia et al. (2011). These existing data provideexcellent reference values for critically assessing the accuracy of thenew U–Pb results obtained using the LASS-ICP-MS approach. TheU–Pb–Hf and �18O isotopic results obtained here are shown graphi-cally in Figs. 5–10 and summarized in Table 4. Given the contrastingspot sizes necessary for conducting the different types of analyses(i.e., ∼10 �m for �18O and 40–50 �m for simultaneous U–Pb–Hf),not all the growth domains analyzed for �18O were amenable tobe analyzed for U–Pb–Hf with the same textural resolution (seeFigs. 6 and 9). To simplify the discussion and the correlation ofanalyses obtained from the same portion of a zircon grain betweenthe different methods, a simple nomenclature was adopted asfollows: each samples analyzed for U–Pb–Hf was assigned a let-ter code (first column of Table 3), which is then followed with asequentially assigned number in the same chronologic order asspots were ablated during LASS-ICP-MS. When the LA spots coin-cide with domains previously analyzed by SIMS for �18O, this LAspot code is also shown next to the �18O composition both in thefigures and in the supplementary material to facilitate their corre-lation. For the sake of simplicity, analyses that occur in tight U–Pband/or Hf compositional clusters are not labeled unless relevant tothe discussion, and only the calculated mean values for these clus-ters are quoted in the text. Results for all the individual U–Pb–Hfand �18O analyses are available as supplementary material to thispaper. Discordance values quoted in the text and data tables arecalculated as Disc. (%) = 100 − (100 * (206Pb/238U date)/(207Pb/206Pbdate)). All U–Pb figures were plotted and weighted mean ages cal-culated using U–Pb Redux (Bowring et al., 2011), by importing theLASS-ICP-MS data as a legacy format. The individual redux filesfor all the samples reported in this study are available from theGeochron data repository and can be freely accessed through theGeochron database (www.geochron.org). All Nd isotopic results aresummarized in Table 5.

Given the complexity of the obtained results and correlationsbetween the different isotopic systems, detailed descriptions ofsample data processing, outlier filtering and selection of analyses

tary material to this communication. In addition to the detailed datadescription presented in the supplementary material, comments

http://www.geosamples.org/



http://www.geochron.org/



M. Ibanez-Mejia et al. / Precambrian Research 267 (2015) 285–310 293

Fig. 5. Uranium–Pb–Hf–O isotopic results in zircons from metaigneous units included within cordilleran basement massifs. Sample codes are according to Table 2 and color-coding of symbols is as follows: open symbols (circles for �18O and squares for Hf) were rejected due to sputtering pits intersecting cracks and/or inclusions for �18O (based onSEM-BSE imaging), or identifiable zircon growth-domain mixing during sputtering or ablation for both �18O and Hf (identified from SEM-CL imaging, or mixing evidenced inchanging 207Pb/206Pb time-resolved ratios; see analytical appendix for details of the latter). Solid black symbols are �18O results that passed the crater morphology inspectionby post-analysis SEM-BSE imaging. However, some of these analyses were not considered toward the weighted mean calculations after subsequent U–Pb data from the samedomains showed evidences of partial age resetting by metamorphic overprint or discordance greater than 10%; these analyses lie outside of the gray boxes in the O panelsthat denote the range of the mean ± 2 S.D. of �18O values. Solid red squares (and filled concordia ellipses) are U–Pb–Hf analyses considered reliable and used toward theinterpretations (see supplementary material). Solid gray symbols – circles for �18O and squares for Hf – were analyses conducted on rims and or older xenocrysts; these werenot considered toward the reported mean values of most samples, but are mentioned in the text when meaningful for the discussion. (For interpretation of the references tocolor in this figure legend, the reader is referred to the web version of the article.)


Fig. 6. Detailed high-resolution cathodoluminescence imaging of representative zircons from metaigneous units included within the cordilleran basement massifs. Locationo ined

w aluesf

witgdHUMtpt

6

pt

f SIMS and LASS-ICP-MS analyses are shown along with the individual results obtaithout their associated uncertainties (refer to supplementary material for these v

or reasons explained thoroughly in the supplementary materials.

ere annotated on a spot-by-spot basis in the tabulated analyt-cal results (also provided as supplementary material) in ordero facilitate their identification and further data evaluation. If aiven analysis displayed complexities in its U–Pb systematics thateemed it unusable for accurate age estimation, then the associatedf isotope composition was also not considered in the discussion.ranium-Pb results obtained from zircon of one particular sample,IVS-13 (Fig. 10), showed extreme perturbed isotopic systematics;

hese results are still included here for illustrating the data inter-retation complexities discussed in Section 4, but they were givenhe least weight in the following discussion and conclusions.

. Discussion

The U–Pb, Lu–Hf, O, and Sm–Nd isotopic data presented hererovide new insights into the long-term history of crustal evolu-ion along the leading margin of Mesoproterozoic Amazonia prior

for each one of the isotopic systems. For simplicity, values in this figure are quoted). Spots marked with an asterisk are analyses not included in the final calculations

to its amalgamation at the core of the Rodinia supercontinent. Thesedata also allow us to better establish tectonic correlations betweenthe NW Amazon Craton, high-grade basement massifs exposed inthe northern Andes, and the Proterozoic basement of Oaxaquiain SW North America. In the following sections we explore theimplications of our data for evaluating the chronology of majortectonic events within Putumayo Orogenic phase, place first orderconstraints on the timing and possible nature of crust formingand reworking processes, and discuss these interpretations in thecontext of Amazonia’s Mesoproterozoic tectonics prior to Toniancollision.

6.1. Mesoproterozoic magmatism within the Putumayo Orogen

Uranium-Pb results by LASS-ICP-MS support previous observa-tions indicating that magmatism occurred within crustal domainsrepresented by the north Andean Precambrian basement massifs


Fig. 7. Uranium–Pb–Hf isotopic results from a graphic-textured segregation of a pegmatitic dike (MIVS-15A) and a garnet-bearing leucosome from a metasedimentarym and coc terprw

fbL(dmm7tamgwtasBptbHi

igmatite (MIVS-16A) in the Garzón massif. Sample codes are according to Table 2

ence images for these samples are included in the supplementary material. (For ineb version of the article.)

rom 1.33 to 1.15 Ga, and possibly as early as 1.47 Ga as impliedy igneous protolith crystallization ages of the Guapotón (MIVS26),as Minas (MIVS41) and La Macarena (Macarena-2) orthogneissesFigs. 5 and 11). In addition, U–Pb data from oscillatory-zonedetrital zircon cores found in the Garzón and Las Minas massifetasediments further support this inference and suggest thatagmatism may have extended to as young as 1005 Ma (Fig.

of Ibanez-Mejia et al., 2011), just prior to the early Neopro-erozoic collisional metamorphism at 990 Ma. The lack of U–Pbges >1.47 Ga in detrital zircons from the Garzón and Las Minasassif metasediments strengthens the hypothesis that coarse-

rained detritus delivered to these late Mesoproterozoic basin(s)ere not derived from cratonic Amazonia; sediment derived from

he cratonic interior during late Mesoproterozoic time would havebundant detrital zircon crystals >1.5 Ga (Ibanez-Mejia et al., 2011),uch as those observed in the Aguapeí Group metasediments inrazil (Geraldes et al., 2014). Consequently, our observations sup-ort a local sourcing of these detrital zircon crystals and lead us
o argue that they were deposited within intra-arc or arc-proximalasins preserved in the Putumayo Orogen. This implies that thef isotopic values from these detrital zircon crystals can be used
n conjunction with the data from the orthogneiss samples (i.e.,

lor-coding of symbols follows the description provided for Fig. 5. Cathodolumines-etation of the references to color in this figure legend, the reader is referred to the

MIVS26, MIVS41 and Macarena-2) to understand the magmatic evo-lution of this long-lived peri-Amazonian accretionary arc system.

6.2. A multi-phase tectono-metamorphic history duringprotracted continental collision

Zircon U–Pb geochronological results obtained from a deformedpegmatitic body included within the ‘El Vergel’ metasediments(1022.3 ± 7.9 Ma, MIVS-15A, Fig. 7), as well as from a foliation-coherent leucosome band from stromatic metatexites within thissame unit (1001 ± 11 Ma, MIVS-16A, Fig. 8), indicate that they crys-tallized during periods that preceded the granulite-facies eventpreviously determined from this unit at ∼990 Ma (Ibanez-Mejiaet al., 2011). The age of emplacement for the MIVS-15A pegmatitedike is similar to an age of migmatite development obtained fromnearby metasedimentary gneisses of the ‘Las Margaritas’ unit whichare exposed in the eastern Garzón massif and display upper-amphibolite mineral assemblages (zircon U–Pb SHRIMP age of
1015 ± 7.8 Ma presented by Cordani et al. (2005) for their sampleGr-15). These results indicate that some of the preserved struc-tures and metamorphic textures observed within the Garzón groupmust be associated with at least one, if not more, metamorphic


F enogr1 ayara-r

eggo

ig. 8. Uranium–Pb–Hf–O isotopic results for zircons from drill-core samples of a sy c7) from the basement of the Putumayo basin. Samples of the Mandur-2 and the Pespectively. All other conventions follow the description provided for Fig. 5.

vents that predate the widespread Neoproterozoic granulite-rade metamorphism at 990 Ma. Although still difficult to ascertainiven the analytical precision limitations and current coveragef the geochronological dataset, it is permissible to suggest that

anitic sill (Mandur-2 Leuco) and metaigneous units (Mandur-2 Melano and Payara-1 wells come from depths of ca. 1700 m and 1400 m below the present day surface,

the observed deformation within the Garzón massif could be theresult of at least two distinct metamorphic phases: (1) an earlierphase occurring between ∼1030 and 1000 Ma that resulted in thewidespread migmatization observed in metasedimentary units of


F ll-coreP

tatdfmt(ct

ig. 9. Detailed high-resolution cathodoluminescence imaging of zircons from driutumayo basin. See legend in Fig. 8 for conventions.

he Garzón group (i.e., ‘Las Margaritas’ and ‘El Vergel’ migmatites);nd (2) the later 990 Ma event associated with the main collisionalectonic burial of the Putumayo Orogen. Migmatite formationuring the first phase may have been facilitated by heating of melt-ertile sedimentary protoliths, which would be prone to develop

igmatitic textures even under amphibolite-facies conditions due
o the relatively low melting temperatures of average wet pelitesThompson, 1982; Chen and Grapes, 2007). The second event ata. 990 Ma, which formed dominantly granoblastic metasedimen-ary and metabasic granulite-facies rocks with scarce evidence
samples of a syenogranitic sill and metaigneous units from the basement of the

of migmatization, suggests that peak metamorphic conditions inour study area during this later event were likely attained underlow aH2O conditions. Leucocratic granulites with granoblastic tex-tures, characterized by abundant perthitic K-feldspar and quartz inmetasedimentary orthopyroxene-bearing assemblages (e.g., sam-ple MIVS-12 in this study – see supplementary sample descriptions
– and MIVS-11 from Ibanez-Mejia et al. (2011); Jimenez Mejia et al.,2006; Kroonenberg, 1982) support the observation that low or neg-ligible degrees of water-assisted partial-melting may have occurredin this unit during the 990 Ma metamorphic event, and that peak


Fig. 10. Uranium–Pb–Hf isotopic results from metasedimentary granulites (MIVS-12 and MIVS-13) of the Garzón massif and a metasedimentary migmatitic melanosome(CB-006) of the Las Minas massif. Light red vs. solid red areas in the probability density diagrams correspond to calculations made considering the results of all analyzedzircons, and the most reliable analyses kept after discordance filtering, respectively. Peak-ages labeled on top of the curves correspond to calculations made after discordancefiltering was applied (see supplementary material for detailed discussion). Green shaded areas in the 176Hf/177Hf vs. 207Pb/206Pb panels represent the estimated age range formetamorphic zircon crystallization. Diagonally hatched area in MIVS-13 represents the range of significantly younger 207Pb/206Pb dates by ancient Pb-loss observed in thissample – data points in this last range are excluded from further graphs and discussion. The goodness of fit for the highlighted regressions is described using the reducedchi-squared value �2

v , taking into consideration the 176Hf/177Hf uncertainty of each point at 95% confidence (the expectancy value of this test is unity when the scatter canbe explained by quoted uncertainties alone). Cathodoluminescence images for these samples are included in the supplementary material. See text for further details. (Forinterpretation of the references to color in this figure legend, the reader is referred to the web version of the article.)

brian

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etamorphic temperatures must have remained mostly below thery granitic solidus.

The occurrence of the two metamorphic pulses discussed aboves also supported by geochronological results obtained from base-

ent samples of the Putumayo basement, which show a similarwo-stage late Meso- to early Neoproterozoic metamorphic his-ory. The metamorphic evolution of this domain is characterized by

igmatite and granulite formation between ca. 1046 and 1020 Mabserved in the Solita-1, Mandur-2 and La Rastra-1 wells (Ibanez-ejia et al., 2011, in preparation), which was shortly followed by a

econd granulite-grade event recorded at ca. 990 Ma such as thatbserved in the orthopyroxene–garnet migmatitic gneisses of theayara-1 well (Fig. 8; Ibanez-Mejia et al., 2011).

An analogous temporal relation between two closely spacedetamorphic events of widespread migmatite formation followed

y dry granulite facies recrystallization has been proposed for thedirondack Mountains of the Grenville Orogen. In the Adiron-ack scenario, migmatites in metapelitic units have been showno develop during the 1180–1150 Ma heating associated withhe Shawinigan phase and intrusion of the AMCG suite, pre-eding the granulite-grade metamorphism of the ca. 1050 Mattawan orogeny (Heumann et al., 2006; Bickford et al., 2008;cLelland et al., 2010). Pervasive dehydration occurring dur-

ng the early melt-extraction event has been suggested to beesponsible for depleting the system of easily accessible water,hus in part controlling the low aH2O metamorphic assemblagesound in the younger Ottawan granulites of the Adirondack High-ands (Bohlen et al., 1985; Valley et al., 1990; Heumann et al.,006; Lancaster et al., 2009). More detailed petrological andeochronological studies of the migmatites and granulite-facies
ocks of the Garzón massif, however, are yet necessary in ordero substantiate whether an Adirondack-style control on granuliteormation is possibly also the case within the Putumayo Oro-en.
able 4ummary of U–Pb–Hf and O isotopic compositions of samples from the Putumayo Orogen

Code Sample name LASS age (Ma)a Ref. ageb Eve

(a) MIVS-26 1154 ± 20/21 (n = 11, MSWD = 0.5) 1135 ± 6 Ign(b) MIVS-41 1329 ± 14/15 (n = 13, MSWD = 1.1) 1325 ± 5 Ign(c) Macarena-2 1467 ± 12/13 (n = 13, MSWD = 1.3) 1461 ± 10 Ign(d) MIVS-15A 1022.3 ± 7.9/8.8 (n = 23, MSWD = 0.4) – Ign(e) MIVS-16A 1001 ± 11/12 (n = 11, MSWD = 0.5) – Mig(f) Mandur-2 Leuco 1010 ± 19/20 (n = 12, MSWD = 0.4) 1017 ± 4 Ign(g) Mandur-2 Melano 1602 ± 15/16 (n = 21, MSWD = 0.6) 1592 ± 8 Ign(h) Payara-1 c7 1590 ± 8/10 (n = 11, MSWD = 1.7) 1606 ± 6 Ign

Payara-1 c7 986 ± 27/27 (n = 4, MSWD = 0.1) 986 ± 17 Me

a Uncertainties are 2�.b Reference ages are previous results obtained by LA-MC-ICP-MS on the same samples

c Ign-P: crystallization age of igneous protolith, Ign-C: age of igneous crystallization, Md Calculation of uncertainties on the �Hf(t) value only consider errors on the 176Hf/177H

able 5ulk-rock Sm–Nd and Lu–Hf isotopic data for metaigneous and metasedimentary rocks o

Sample Sm Nd 147Sm/144Nd 143Nd/144Nd ± 2�

(ppm) (ppm) (0)

MIVS-26 15 75 0.121097 0.512065 ± 12

MIVS-41 11 48 0.132086 0.512115 ± 12

Mandur-2 (L) 8 37 0.136687 0.512194 ± 19

Payara-1 12 96 0.072948 0.511404 ± 8

MIVS-37a 12 44 0.164007 0.512310 ± 15

Solita-1 7 34 0.120298 0.511969 ± 11

La Rastra-1 3 14 0.123077 0.512042 ± 15

Sample Lu Hf 176Lu/177Hf 176Hf/177Hf ± 2�

(ppm) (ppm) (0)

La Rastra-1 0.23 1.90 0.017105 0.282420 ± 30

Research 267 (2015) 285–310 299

6.3. Petrologic implications of the Hf–O isotopic data

The Hf–O isotopic compositions obtained from igneous/metaigneous units of the Cordilleran terranes and those from thePutumayo basin basement display some systematic differencesthat indicate the contrasting nature of these two crustal domains(Fig. 11). Whereas zircon crystals from the igneous precursors oforthogneiss units included in the Cordilleran basement massifsshow moderately elevated and progressively increasing �18O val-ues between 6.4 and 7.2‰ (squares in Fig. 11), a composition typicalof ‘I-type’ arc granitoids (Eiler, 2001; Valley et al., 2005; Kemp et al.,2007), the basement of the Putumayo basin shows a markedly bi-modal distribution in its �18O values (circles in Fig. 11); mantle-likecompositions are found in igneous zircon from the Mandur-2 bore-hole (5.4–5.6‰), whereas the cores of zircon from the Payara-1 wellgneiss display an ‘S-type’ supracrustal signature (ca. 9.0–9.4‰).

The Hf isotopic ratios of the hornblende–biotite orthogneissesfrom the Cordilleran massifs have relatively enriched composi-tions, with only small positive deviations from CHUR values attheir respective ages (Fig. 11). This evidences an important con-tribution of pre-existing crustal material in their source region,an observation that is compatible with results obtained from theclassic hornblende-bearing I-type granites of the Lachlan FoldBelt, where previous U–Pb–Hf–O studies have demonstrated thecrucial role that metasedimentary-source melting plays in the gen-esis of cordilleran-type calc-alkaline magmas (Kemp et al., 2007).The Hf isotopic compositions obtained from the PaleoproterozoicPutumayo basin basement, on the other hand, are also bi-modallike their �18O values; igneous-protolith zircon cores found inthe Mandur-2 mafic gneisses, which have mantle-like �18O, also
display an elevated mean �Hf(t) of ca. 8.0 (Figs. 8 and 11) thusindicating that portions of the north Andean foreland might beunderlain by true juvenile Amazonian Paleoproterozoic crust. Incontrast, the protolith zircon cores found in the Payara-1 gneiss
.

ntc 176Hf/177Hf(t) ± 2 S.D. �Hf(t) ± 2 SDd �18O ± 2 S.D.

-P 0.282087 ± 39 (n = 10, MSWD = 0.9) +1.2 ± 1.4 7.16 ± 0.22 (n = 8)-P 0.282007 ± 43 (n = 12, MSWD = 1.1) +2.4 ± 1.5 6.55 ± 0.26 (n = 8)-P 0.281868 ± 63 (n = 13, MSWD = 1.6) +0.6 ± 2.2 6.36 ± 0.27 (n = 10)-C 0.282141 ± 40 (n = 23, MSWD = 1.2) +0.1 ± 1.4 –m 0.282099 ± 54 (n = 10, MSWD = 1.8) −1.9 ± 1.9 –

-C 0.282197 ± 45 (n = 12, MSWD = 1.1) +2.0 ± 1.6 5.60 ± 0.22 (n = 11)-P 0.281974 ± 42 (n = 18, MSWD = 0.8) +7.6 ± 1.5 5.43 ± 0.23 (n = 22)-P 0.281796 ± 70 (n = 11, MSWD = 2.1) +0.8 ± 2.5 ca. 9.0–9.4t 0.281981 ± 21 (n = 4, MSWD = 0.3) −6.4 ± 0.8 7.94 ± 0.10 (n = 6)

and reported in Ibanez-Mejia et al. (2011).igm: migmatization age, Met: age of metamorphic zircon.f(0) measurement, not on the 176Lu/177Hf used for age correction.

f the Putumayo Orogen.

Age 143Nd/144Nd �Nd ± 2� fSm/Nd Nd-T(DM)

(Ma) (t) (t) (Ga)

1154 0.511151 0.06 ± 0.24 −0.384 1.601325 0.510970 0.87 ± 0.24 −0.328 1.721017 0.511285 −0.79 ± 0.38 −0.305 1.671606 0.510638 1.50 ± 0.16 −0.629 1.771005 0.511232 −2.13 ± 0.30 −0.166 2.241046 0.511146 −2.77 ± 0.22 −0.388 1.741035 0.511209 −1.82 ± 0.30 −0.374 1.67

Age 176Hf/177Hf �Hf ± 2� fLu/Hf Hf-T(DM)

(Ma) (t) (t) (Ga)

1035 0.282086 −1.53 ± 1.06 −0.491 1.99

3 brian Research 267 (2015) 285–310

wtgmoubboaM

wcem�ptdotvtmtwctmticgsw(

t�ntmwi2

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6

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Fig. 11. U–Pb–Hf–O data from basement igneous and metaigneous rocks ofthe Putumayo Orogen. (A) Age-corrected 176Hf/177Hf vs. age for granitoids,orthogneisses and migmatites analyzed during this study. For reference, �Hf val-ues with respect to CHUR (Bouvier et al., 2008) are shown as dashed light-gray linesparallel to this reservoir, plotted at successive increments of +2 and −2� deviations.Red dotted lines are apparent iso-TDM contours, showing values for the apparentmodel ages that would be obtained by assuming a reservoir Lu/Hf composition of‘average crust’ (i.e., 176Lu/177Hf = 0.015; Condie et al., 2005). Other reservoir slopesshown in inset are for (a) Island arc crust (Hawkesworth et al., 2010), (b) bulk lower-crust (Rudnick and Gao, 2003), (c) global subducting sediments (GLOOS; Plank andLangmuir, 1998), (d) bulk continental crust (Rudnick and Gao, 2003), (e) averagePrecambrian granites (Vervoort and Patchett, 1996), (f) bulk upper-crust (Rudnickand Gao, 2003). DM is the juvenile-crust depleted mantle model using the data ofVervoort and Blichert-Toft (1999); NC is the ‘New Crust’ model of Dhuime et al.(2011). Fields for different terranes within Oaxaquia are from Weber et al. (2010).(B) �18Ozircon compositions vs. age for granitoids and orthogneisses analyzed during


ith a 176Hf/177Hf composition near CHUR (Fig. 11), is in-line withhe interpretation drawn from the �18O data that suggests thisneiss formed via re-working of older Paleoproterozoic crustalaterial. Given these evidences, a possible northward extension

f a Rio Negro-Juruena-like basement (sensu Tassinari et al., 1996)nder the Oriente-Putumayo foreland basins would be plausi-le (RNJ, Fig. 1A) judging by the similar bi-modal nature of thiselt characterized by Paleoproterozoic juvenile magmatism andverlying supracrustal sequences of similar age (e.g., Jauru regionnd Roosevelt supracrustals; Tassinari et al., 1996; Tassinari andacambira, 1999, and references therein).The occurrence of evolved syenogranitic sills in the Mandur-2

ell with mantle-like �18O zircon values and enriched Hf isotopeompositions (sample Mandur-2 Leuco; Figs. 8 and 10) might bexplained in at least two simple ways: (1) these syenogranitic mag-as were formed by melting of pre-existing crustal sources with

18O values that were both higher and lower than mantle-like com-ositions, which were mixed during anatexis in such a proportionhat the resulting melt appears to be mantle-like by mere coinci-ence; or (2) the syenogranitic melts were formed by reworkingf an ancient mantle-derived mafic crust which remained unal-ered for hundreds of millions of years such that mantle-like �18Oalues of the resulting partial melts are preserved, but their Hf iso-ope ratios had enough time to sufficiently diverge from a depleted

antle-like composition. Following from the observation thathese deformed syenogranites are hosted within mafic gneissesith mantle-like �18O and juvenile 176Hf/177Hf(t) compositions at

a. 1.6 Ga (i.e., Mandur-2 Melano sample; Figs. 8 and 11), and thathe host mafic gneisses show structures compatible with partial

elting (Ibanez-Mejia et al., 2011), we favor the second interpreta-ion for the origin of the evolved syenogranitic intrusives retrievedn the Mandur-2 well (sample Mandur-2 Leuco). If this was thease, then the difference in 176Hf/177Hf(t) values between the hostneiss and the syenogranite sills could be explained by closed-ystem radiogenic ingrowth along a whole-rock 176Lu/177Hf ≈ 0.02,hich is in agreement with the average composition of mafic crust

Rudnick and Gao, 2003; Pietranik et al., 2008).The observation that metamorphic overgrowths in zircons from

he Guapotón and Las Minas orthogneiss have undistinguishable18O values with respect to their inherited igneous cores is also sig-ificant (Figs. 5 and 6), as it may provide further evidence to supporthe interpretation that extensive dehydration melting of metasedi-

ents and subsequent rock–fluid interactions (e.g., volatile fluxing)ith the orthogneiss units probably had only a subdued role dur-

ng the granulite-forming event at 990 Ma. The 176Hf/177Hf vs.07Pb/206Pb date correlations in the bulk single-crystal data pre-ented by Weber et al. (2010) for the Guapotón orthogneiss isncompatible with metamorphic rims being developed by solid-tate recrystallization, and indicates that the rims observed in Fig. 6ikely represent newly formed zircon precipitated from a meta-

orphic fluid or anatectic melt (e.g., Bowman et al., 2011). If thiss the case, then the similarity of �18O compositions between theores and rims of zircons from this unit (Fig. 5) is likely an indica-ion of closed-system behavior during metamorphism, and implieshat no externally-derived fluids with contrasting �18O values –s those that would be expected from dehydration of the hostetasediments to these plutons – participated in metamorphic

ircon crystallization of the Guapotón and Las Minas orthogneisses.

.4. Secular changes in Hf isotopic compositions through time

The time-integrated compositional trends defined by the Hfsotopic results of protolith igneous and detrital zircon crystalsbtained here provide a wealth of information on the modesnd mechanisms responsible for crustal development along this

this study. (For interpretation of the references to color in this figure legend, thereader is referred to the web version of the article.)

pre-collisional Mesoproterozoic margin. Long-term changes in176Hf/177Hf and 143Nd/144Nd ratios within a closed system areexpected to occur through time, simply owing to the in situ decayof radiogenic 176Lu and 147Sm, and will occur at ratesthat directly

brian Research 267 (2015) 285–310 301

dtepsca4fgposwacaocbrsjowrtlymttspoaotscpcnitpcwttstHlamaptodi

ipt

Fig. 12. U–Pb–Hf–Nd data from metasedimentary and metaigneous units of thePutumayo Orogen. (A) 176Hf/177Hf vs. apparent 207Pb/206Pb date of detrital zirconsfrom metasedimentary granulites and migmatites of the Garzón and Las Minas NorthAndean Precambrian basement massifs. External reproducibility (at 95% confidence)of low Yb (Mud Tank) and high Yb (R33) reference zircon crystals analyzed duringthis analytical session are shown as reference for the typical uncertainty bars ofindividual analyses. All other symbols are the same as Fig. 11. (B) 143Nd/144Nd vs.age for metasedimentary (plotted at their age of metamorphism) and metaigneousunits of the North Andean basement massifs and the basement of the Putumayobasin. Analogous to the Hf plots, the y-axis of this plot is in 143Nd/144Nd units and�Nd values are also shown as deviations in +2 and −2 increments around the CHURcomposition. Slopes for the evolution of different reservoirs as a function of theirSm/Nd compositions (inset) follow the same nomenclature as Fig. 11. Fields for


epend on the parent/daughter composition of the system. If a par-icular crustal reservoir experiences various episodes of partial meltxtraction over a sufficiently long time-span, then the isotopic com-ositions of those melts will track the long-term evolution of theource or the various possibilities of mixing between the differentontributing components (Murphy and Nance, 2002; Hawkesworthnd Kemp, 2006; Kemp et al., 2009b; see discussion in Section

and Fig. 4). Secular changes preserved in the protolith zirconrom orthogneiss units and in metasediments of the Putumayo Oro-en allow for the identification of two main intervals within itsrotracted Mesoproterozoic tectonic evolution: Interval 1, whichccurred between ca. 1.47 Ga and 1.15 Ga, is characterized by a con-tant steep positive progression in 176Hf/177Hf(t) values versus age,hereas Interval 2, defined between ca. 1.15 and 0.99 Ga, displays

n overall shallowing in the trends of time-changing 176Hf/177Hf(t)ompositions (Figs. 11 and 12). We interpret these two intervalss representing contrasting phases within the tectonic evolutionf the orogen, reflecting the prevalence of different geological pro-esses that exert control on the rates at which juvenile melts areeing extracted and added to the crust or the amount of older mate-ial being reworked at any given time. In this sense, Interval 1 isuggested to be the result of a long-term progressive addition ofuvenile mantle melts at the base of the arc crust. The observedverall trend is unlikely to simply represent radiogenic ingrowthithin a closed-system reservoir, or to be generated by older crustal

eworking (Fig. 4), and thus might be evidencing the cryptic rolehat juvenile magmatic input had in the overall growth of thisong-lived active continental margin. Based on observations fromounger accretionary orogens that preserve a much more completeagmatic record (e.g., Kemp et al., 2009b), it has been suggested

hat rapid periods of crustal growth are intimately linked withectonic processes that enhance mantle melting, such as back-arcpreading associated to slab roll-back events. Therefore, we pro-ose that the long-term trend observed during this first intervalf the Putumayo margin took place in a dominantly retreatingccretionary orogen, thus resulting in a long-term net additionf juvenile material to the overlying arc system. We speculatehat this process, however, is likely not the result of monotonousteady-state juvenile input (as simplified in Fig. 11), but ratherould be the final apparent result of a series of cyclic episodes ofunctuated juvenile melt extraction and older crustal reworking,ontrolled by shorter-lived tectonic pulses typical of active conti-ental margins (DeCelles et al., 2009; Kemp et al., 2009b). Such an

nterpretation could explain the apparent de-coupling in the long-erm trends of the �18O and Hf compositions from the orthogneissrotoliths, which show increasing �18O values through time – indi-ating increased supracrustal material incorporation (Fig. 11B) –hereas our interpretation of the changing 176Hf/177Hf composi-

ions is one of progressive rejuvenation. If the granitic precursorso the Macarena, Las Minas, and Guapotón orthogneisses repre-ent only a snapshot into individual shorter-lived cycles ratherhan a single mixing of two end-member components, then thef–O trends need not be directly linearly correlated. Neverthe-

ess, it is possible to suggest, based on the existing data, thatlthough more surficially altered material is participating in arc-agma generation through time, the composition of the arc system

s a whole – including any underplated sediments from the arc-roximal basins – were experiencing a rapid positive change inheir bulk 176Hf/177Hf compositions. This is interpreted as the resultf progressive rejuvenation of the system by the addition of mantle-erived juvenile magmas to the base of the arc crust throughout this

nterval.
Interval 2 (ca. 1150–990 Ma) is more difficult to define directly
n terms of the magmatic products being produced along the inter-reted arc system as no orthogneisses with protolith age youngerhan the Guapotón unit (i.e., ∼1.15 Ga) have yet been identified

the different units and lithologies within Oaxaquia are recalculated from: P&R87 –Patchett and Ruiz (1987); R&P88 – Ruiz et al. (1988); W&K99 – Weber and Köhler(1999). The composition of metasedimentary migmatites and granulites of the NorthAndean Precambrian basement massifs are recalculated after Restrepo-Pace et al.(1997) and Cordani et al. (2005).

3 brian

imoloiri∼cmmCtotpttrgbitivaeo

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tfm(pbt


n the study region. This interval appears to be a period ofore intense crustal reworking, an inference that is supported by

bservations of the Hf isotope data as well as other lines of geo-ogical and geochronologic evidence that argue for the widespreadccurrence of regional metamorphic events within the orogen dur-ng this time interval. In addition to the U–Pb geochronologicalesults that demonstrate the occurrence of metamorphic eventsn the Garzón massif and the Putumayo basin basement between1.00 and 1.05 Ga as described earlier (Section 6.2), detrital zir-

on populations with clearly sector-zoned textures of interpretedetamorphic derivation occur in metasediments of the Las Minasassif and have ages mainly in the 1.10–1.17 Ga range (sample

B-006; Fig. 10). Although it cannot be unequivocally interpretedhat these detrital populations are directly related to this segmentf the arc system (e.g., possible derivation from distant sources),he limited age distribution of inherited components in this sam-le marked by a tight bi-modal age distribution with ages closeo those of sediment deposition favor a localized provenance ofhese detritus (Cawood et al., 2012). Furthermore, thermobaromet-ic modeling coupled with Sm–Nd and Lu–Hf age constraints fromarnet-bearing metasedimentary granulites in the Putumayo basinasement (i.e., drilling cores retrieved from the La Rastra-1 well),

ndicate that thermal pulses leading to regional metamorphism inhis area may have started as early as ∼1060 Ma (Ibanez-Mejia et al.,n preparation). This further supports the interpretation that Inter-al 2 involved a significant component of contractional tectonismnd crustal reworking, which we tentatively interpret as reflectingarly terrane accretion during the protracted evolutionary historyf this orogen as initially proposed by Ibanez-Mejia et al. (2011).

.5. The along-strike diachronic nature of continental suturing

Comparison of the detrital zircon populations found in metased-ments from the Garzón group (i.e., sample MIVS-12 and MIVS-13rom the Garzón massif) and the Zancudo migmatites (i.e., sampleB-006 from the Las Minas massif) reveals fundamental differences

n the zoning textures and Hf isotopic compositions of zircons thatrystallized within a similar age range. Whereas all post-1.2 Ganherited crystals found in the Garzón group metasediments showextures indicative of igneous crystallization (see CL image reposi-ory) and define positive 176Hf/177Hf vs. time progressions similaro those described above for Interval 1 (Fig. 10, Hf panel of sampleIVS-12), zircon cores from the Zancudo migmatites show tex-

ures indicative of derivation from metamorphic sources (see CLmage repository) and have a sub-horizontal to slightly negativelope in their 176Hf/177Hf vs. age variation (Fig. 10, Hf panel ofample CB-006). These contrasting textural and isotopic character-stics indicate fundamental differences in the dominant processesccurring in their respective sediment source areas during the1.20–1.05 Ga time interval, which can be interpreted in terms of

heir tectonic significance. As discussed in previous sections, steepositive 176Hf/177Hf vs. time trends are indicative of juvenile crustdditions, whereas sub-horizontal or negative slopes – when notue to complexities in the U–Pb system – are indicative of periodsf extensive older crustal reworking. The simultaneous occurrencef these two trends in the detrital-zircon record of the Putumayorogen possibly indicates that these two processes were concurrentn different segments of the orogenic system.

As observed within a modern continental collisional zone,he early stages of interaction of irregularly shaped continentalragments induce a marked along-strike variation in the defor-

ation and magmatism that occurs within the overriding plate
Malinverno and Ryan, 1986). In some instances these diachronousrocesses lead to the widespread development of wide back-arcasins induced by slab roll-back, which causes trench retreat withinhe overriding collisional plate margin (Royden, 1993). Therefore,
Research 267 (2015) 285–310

if back-arc spreading centers constitute a major locus of juve-nile crust generation (Kemp et al., 2009b), then rapid extractionof juvenile continental crust should in many cases be expectedto occur in synchrony with the early stages of continental col-lision along these segmented retreating subducting boundaries.Following these inferences, we speculate that the mixed evidencesof crustal growth and reworking observed for Interval 2, couldpotentially be a result of the terrane accretions occurring withina ‘Mediterranean-style’ tectonic setting (e.g., Pullen et al., 2008);in such a scenario, segments of the arc-basin system could havecontinued to experience subduction-related magmatism and rapidadditions of juvenile melts in extensional back-arc environments,while other segments of the trench were probably chocked bythe underthrusting of buoyant continental lithosphere resulting inolder crustal reworking and the flattening of the 176Hf/177Hf vs.age isotopic patterns (Figs. 5 and 11). The impingement of conti-nental indentors causing localized deformation within the northernsegment of the Grenville Orogen (Gower et al., 2008), might be areflection that this process is more common in ancient orogens thanusually recognized.

6.6. Paleo-tectonic linkages with the Precambrian basement ofOaxaquia

Despite previously available geochronological and isotopic evi-dence that suggested correlations between the North Andeanbasement massifs and the Mexican basement inliers (Restrepo-Pace et al., 1997; Ruiz et al., 1999; Weber et al., 2010), a possibleAmazonian connection for their ancestry remained speculativedue to the dearth of isotopic data from a coeval orogenic belteast of the Andean deformation front in northern South Amer-ica. The new whole rock Nd and Hf data presented here provide,for the first time, direct evidence from cratonic Amazonia in sup-port of these linkages. Neodymium isotopic values from bulk-rocksamples of a syenogranite from the Mandur-2 well, a migmatiticgneiss from the Payara-1 well, and metasedimentary migmatitesof the Solita-1 and La Rastra-1 wells (also bulk-rock Hf from thislast one) provide a reference composition for the NW Amazo-nian basement and the bulk sedimentary load it delivered to itsperipheral Mesoproterozoic basins. Fig. 12B shows a comparisonof the Nd isotopic compositions from Oaxaquia, the north Andeanbasement massifs, and the basement of the Putumayo basin. Thecompositional fields from the different lithologic components ofOaxaquia were delineated by recalculating the Nd isotopic compo-sitions of Patchett and Ruiz (1987), Ruiz et al. (1988) and Weberand Köhler (1999), using the chronology for the different mag-matic and sedimentation events as discussed by Weber and Köhler(1999), Weber and Hecht (2003), Cameron et al. (2004), Keppie andOrtega-Gutierrez (2010) and Weber et al. (2010). Compositionalfields for metasedimentary units of the Colombian basement mas-sifs use the Nd data of Restrepo-Pace et al. (1997) and Cordaniet al. (2005) recalculated using the inferred chronology of sed-imentation discussed in Cordani et al. (2005) and Ibanez-Mejiaet al. (2011). To a first order, the 143Nd/144Nd(t) values of themetasediments from cratonic Amazonia (i.e., Solita-1 and La Rastra-1 wells) are in excellent agreement with the compositional fielddefined by metasediments of the Garzón group, Las Minas massifand Oaxaquia (Fig. 12). These results support the interpretationthat, although not clearly represented in the detrital zircon recordas evidenced by the scarcity of Amazonian-like U–Pb age compo-nents in the north Andean and Oaxaquian metasediments (Cordaniet al., 2005; Ibanez-Mejia et al., 2011; Solari et al., 2013; this
study), the basement and bulk-sediment isotopic composition ofMesoproterozoic NW Amazonia provide a viable match for theolder crustal inheritance found in metasedimentary units of theseremobilized basement domains. The compositions of basic and

brian

i(mdboacijdszrritbtd(ibd�cmoorfaiialteWbtiod

6R

Mmoitochco2mdieob


ntermediate meta-igneous units from the Oaxaquian basementbasic granulites and amphibolites in the Guichicovi complex and

etabasic rocks found elsewhere in Oaxaquia; Fig. 12B), whichisplay more radiogenic 143Nd/144Nd values with respect to theasement of the Putumayo basin basement and the compositionsf the Andean orthogneisses (i.e., MIVS-26 and MIVS-41) and Oax-quian orthogneisses (i.e., felsic orthogneisses of the Guichicoviomplex; Fig. 12B), are consistent with a mixture between an inher-ted crustal component of possible Amazonian descent and youngeruvenile melt additions in an arc environment. The bulk-rock Hfata from the La Rastra-1 well is also compositionally similar, butlightly less radiogenic, than the 176Hf/177Hf(t) values obtained fromircons of the North Andean and Mexican terranes (Fig. 11A). Thisesult also shows that the addition of variable degrees of juvenileadiogenic material to an NW Amazonian reworked components a feasible and simple model in order to explain the Hf iso-opic compositions of the mid- to late Mesoproterozoic basementlocks of the Northern Andes and Oaxaquia (Weber et al., 2010,his study). Finally, we also note that recent detrital-zircon U–Pbata from metasediments of the Oaxaquian Complex of Solari et al.2013) display strikingly similar patterns with respect to metased-ments studied in this contribution (Fig. 10) and presented earliery Ibanez-Mejia et al. (2011). Furthermore, the most radiogenicetrital-zircons from the Garzón group metasediments (apparentHf(t) values between 3 and 6), which have no known bedrockounterpart (i.e., orthogneiss protolith) in the north Andean base-ent domains, are in excellent agreement with the compositions

f the igneous protoliths of the Oaxaca, Guichicovi and Novillorthogneisses (Fig. 12A). This interpretation is also in line with theecent discovery of early Mesoproterozoic (∼1.4 Ga) protolith agesound in orthogneisses and migmatites of the Huiznopala and Oax-ca complex (Weber and Schulze, 2014), which further support thenference that the construction of Oaxaquia also involved rework-ng of older Mesoproterozoic crustal material. These new isotopicnd geochronologic observations, along with all of the previousines of evidence discussed above, continue to reinforce interpreta-ions that postulate a close tectonic, magmatic, and metamorphicvolution of the north Andean and Oaxaquia basement domains.e propose that evidence now exists in order to support linkages

etween these blocks and the basement of NW South America, andhat combined evidences of their mineralogical and isotopic inher-tance store abundant information to identify a long-lived historyf convergent margin tectonism along the (modern) NW Amazoniauring most of the Mesoproterozoic.

.7. Relations with the Sunsás-Aguapeí belt and implications forodinia reconstructions

In addition to providing new compelling evidence to link theeso- to Neoproterozoic evolution of the Putumayo basin base-ent with the North Andean basement massifs and the basement

f Oaxaquia (see discussion is Section 6.6), the new data obtainedn this study allow important distinctions to be drawn betweenhe Putumayo orogen and the late Mesoproterozoic collisional beltf modern SW Amazonia, the Sunsás-Aguapeí orogen (Fig. 1A). Inontrast to the late Mesoproterozoic magmatic history inferrederein for the Putumayo margin, which likely lasted until the finalollisional closure of the hypothesized Putumayo-Sveconorwegianrogen at ca. 990 Ma (Cardona et al., 2010; Ibanez-Mejia et al.,011), no clear geochronologic evidence exists to infer that activeargin tectonism occurred along the Sunsás-Aguapeí belt after the

ocking of the Paraguá block in the mid Mesoproterozoic (mark-
ng the end of the Rondonia-San Ignacio orogeny; Bettencourtt al., 2010; Teixeira et al., 2010). Instead, the geological evolutionf the Sunsás-Vibosi and Aguapeí-Huanchaca (meta)-sedimentaryelts is associated with the development of passive-margin and
Research 267 (2015) 285–310 303

intra-continental rift basins that developed along the fringes ofthe Paraguá block, which were later inverted and variably meta-morphosed during the Sunsás collision at ∼1.1 Ga and intruded byun-deformed post-collisional granites starting at ∼1.08 Ga (Bogeret al., 2005; Santos et al., 2008; Teixeira et al., 2010). Recent detrital-zircon U–Pb data from sedimentary units of the Aguapeí group byGeraldes et al. (2014) indicate that the sedimentary infill of thisbasin was dominantly derived from the cratonic interior to the E-NE (e.g., Rio Negro-Juruena province, RNJ in Fig. 1) and the Paraguáblock to the W (rifted fragment of the Rondonia-San Ignacio com-posite orogen, RSI in Fig. 1), but lacks zircon with ages younger than∼1.25 Ga. If the age estimate proposed by Rizzotto et al. (2014)for the opening of the Aguapeí-Huanchaca rift ca. 1.15 Ga is cor-rect, then the absence of detrital zircon with ages between ∼1.25and 1.15 Ga in sedimentary sequences of the Aguapeí group fur-ther supports an intra-cratonic rift setting for its deposition andthe absence of a nearby arc system such as the one we hypothesizewas concurrently active along the Putumayo margin. Based on thecontrasting geologic histories for the Sunsás-Aguapeí belt and thePutumayo margin during the late Meso- to early Neoproterozoic,paleogeographic models that propose a common accretionary mar-gin to explain the development of both orogenic belts (e.g., SAMBAreconstruction; Johansson, 2009) become unsupported as they failto reconcile these markedly differing tectonic scenarios.

Although paleomagnetic data are still somewhat equivocal withrespect to the exact positioning of Amazonia during mid to lateMesoproterozoic times (see reviews in Evans, 2013; Pisarevskyet al., 2014), reliable poles from basaltic rocks of the Nova Flo-resta Fm. (Tohver et al., 2002) and red beds of the Fortuna Fm. inthe Aguapeí group (D’Agrella-Filho et al., 2008) suggest a trans-lation from lower to higher latitudes for Amazonia from a nearequatorial position during the Stenian. This is in contrast to thenear-polar paleolatitude of Baltica in the late Ectasian and itssubsequent clockwise rotation toward lower latitudes during theStenian (Pisarevsky et al., 2003; Cawood and Pisarevsky, 2006),which, as recently pointed out by Pisarevsky et al. (2014), alsomake the SAMBA reconstruction paleomagnetically unsupportedfor the mid to late Mesoproterozoic paleogeography. Alternatively,the reconstructions proposed by Tohver et al. (2002) and Evans(2013) for Amazonia’s incorporation to Rodinia – independentlyfrom Baltica – using the post-1.3 Ga poles are both consistent withthe geological history of the Putumayo margin as described byIbanez-Mejia et al. (2011) and in this study. Although the alter-native paleogeographic model of Evans (2013) would raise furtherquestions with respect to the evolution of the Sunsás-Aguapeí oro-gen, because a collision between this margin and the Llano segmentof Laurentia (Tohver et al., 2002) would no longer be a feasiblescenario to explain the coeval Sunsás and Llano deformation, itcould be an attractive alternative if a Paleoproterozoic connec-tion between Amazonia and Baltica (e.g., SAMBA-like hypothesis ofBispo-Santos et al., 2013) could be further substantiated. However,as recently noted by Pisarevsky et al. (2014), although paleomag-netically viable the participation of northern Amazonia in Paleo-to Mesoproterozoic Columbia (or Nuna) is still doubtful. Instead,the reconstruction proposed by Pisarevsky et al. (2014) envisionsan independently drifting Amazonia with a long-lived active sub-duction margin along its (modern) western side for most of theMesoproterozoic, a model that is compatible with the protractedhistory of convergence inferred from the geologic and geochrono-logic data (Bettencourt et al., 2010; Ibanez-Mejia et al., 2011).

7. Conclusions

We provide detailed U–Pb, Lu–Hf, Sm–Nd, and O isotopic datafrom the Precambrian basement of NW South America to support

3 brian

todve(wabaoatocmoglmbctecdmbp

edtcg2rfSam2tso

htics‘ttitmptrimtut

split using a regular Y-connector. Since the gas-line pressure to the


he hypothesis that a long-lived accretionary margin was devel-ped along this segment of the Amazon Craton for almost the entireuration of the Mesoproterozoic era. Based on isotope compositions. time trends from granitoids and detrital-zircons, this protractedvolution is proposed to consist of at least two main intervals:a) an earlier one dominated by overall crustal growth associatedith the development of a long-lived accretionary arc system (or

series of) between 1.45 (?) and ∼1.15 Ga, and (b) a later intervaletween ∼1.15 and 0.99 Ga characterized by mixed geochemicalnd geochronological evidence that indicates the simultaneousccurrence of mechanisms that induce juvenile crust additionsnd older crust reworking along the margin. This apparent con-radiction is interpreted as resulting from a strong segmentationf upper-plate deformation styles in the orogenic system, whichan be explained by the accretion of terranes along some seg-ents of the trench while other portions continued to experience

ngoing subduction and possibly fast trench retreat. These neweochronologic and isotopic data also allow us to postulate tectonicinkages for the evolution of the Putumayo basin basement, base-

ent blocks exposed in the northern Andes, and the Precambrianasement of central Mexico, prior to the Tonian collisional climax ata. 990 Ma that resulted in the docking of Amazonia at the heart ofhe Rodinia supercontinent. We provide the first direct geochemicalvidences from autochthonous NW Amazonia in support of theseonnections, and observe that the isotopic compositions of theifferent crustal domains that make up the northern Andean base-ent and the Oaxaquia composite terrane can be accommodated

y different stages of the long-lived history of convergence hereinroposed.

Augmenting the initial hypothesis put forward by Ibanez-Mejiat al. (2011), the new data presented in this study continue toraw fundamental differences between the tectonic history andhe timing of major crustal growth and deformation episodes thatharacterize this margin of Amazonia and the Sunsás-Aguapeí oro-en (Teixeira et al., 2010;Fig. 1A; Fig. 8 of Ibanez-Mejia et al.,011). This has important implications for models of Rodiniaeconstructions, as any paleogeographic scenario advocating eitheror a long-lived connection between Amazonia and Baltica (e.g.,AMBA reconstruction of Johansson, 2009) or collisional inter-ctions along oppositely facing Putumayo and Sveconorwegianargins (e.g., Bingen et al., 2008; Cardona et al., 2010; Li et al.,

008; Weber et al., 2010) would need to simultaneously satisfyhe geodynamic and timing constraints imposed by the pre- andyn-collisional history of the contrasting Sunsás and Putumayorogens.

Analytical results presented in this Putumayo case studyighlight the potential that combined high-resolution imaging,exturally resolved �18O compositions, and concurrent U–Pb–Hfsotopic analyses by LASS-ICP-MS methods have for retrievingrucial information about the tectonics, crustal development andedimentation history of strongly modified orogenic crust. Thesplit-stream’ analytical method calibrated during the course ofhis study, which allows for fine-tuning of the aerosol split-ing proportions and takes advantage of the enhanced-sensitivitynterface of the Element2 SC-ICP-MS, shows that concomi-ant U–Pb and Lu–Hf isotopic information obtained by the

ethods herein described can be acquired with little com-romise to the precision and accuracy typically achieved forhese system using ‘single-stream’ data collection. This approachepresents a tremendous advantage for characterizing complex-ties in the isotope systematics or ablation-induced mechanical

ixtures of growth domains in complex poly-phase zircons
hat, if unresolved, could significantly hinder the effectivese of these data to construct accurate geological interpreta-ions.
Research 267 (2015) 285–310

Acknowledgements

The authors would like to thank the Instituto Colombiano delPetroleo (ICP-ECOPETROL) and the Litoteca Nacional de Colombia forallowing access to the core samples, which were taken with thekind assistance of Ana Milena Rangel. Ariel Strickland tuned andassisted MI with the analysis of oxygen isotope ratios at WiscSIMS.Tom Milster and Melissa Zaverton are acknowledged for facilitat-ing the optical interferometry measurements at the Departmentof Optical Sciences, University of Arizona. We express our grati-tude to journal editor Randy Parrish, as well as Bernard Bingen andan anonymous reviewer for constructive comments that signifi-cantly improved the clarity and the quality of the final version ofthis article. This work was partially supported by the U.S. NationalScience Foundation EAR-1118525, EAR-1032156 and EAR-1338583awards. WiscSIMS is partially supported by NSF-EAR-1053466. TheICP-MS and SEM facilities at the Arizona Laserchron center are par-tially funded by NSF-EAR-1338583 and EAR-0732436 awards. TheALC Element2 SC-ICP-MS was acquired thanks to the support ofExxonMobil.

Appendix A. Analytical methods for concurrent U–Pb–Hfmeasurements using laser-ablation ‘split-stream’

A.1. Analytical setup and data acquisition

All U–Pb–Hf isotopic analyses presented in this study weresimultaneously acquired using a SC-ICP-MS and a MC-ICP-MS inthe Arizona Laserchron Center (ALC) at the University of Ari-zona. This approach is generally known in the literature as laserablation–split stream (LASS), which throughout the text we referto as LASS-ICP-MS. For simultaneous acquisition of the U–Pb andLu–Yb–Hf data using magnetic-sector mass spectrometers, mostprevious workers have utilized SC- and MC-ICP-MS instrumentsbuilt by the same manufacturer (e.g., Nu instruments Attom SC-ICP-MS and Nu Plasma MC-ICP-MS in Kylander-Clark et al., 2013;Thermo-Finnigan Element2 SC-ICP-MS and Neptune MC-ICP-MS inFisher et al., 2014a; Tollstrup et al., 2012). For this study, we uti-lized a Thermo-Finnigan Element2 SC-ICP-MS equipped with anenhanced sensitivity ‘Jet Interface’ for measuring U–Pb isotopesand Yb–Lu–Hf were measured using a Nu Plasma MC-ICP-MS. Thesetwo instruments have considerably different auxiliary and samplegas pressurizations, which make splitting the aerosol generatedafter laser-ablation slightly more difficult than when two instru-ments from the same manufacturer and with similar primary gasline pressures are used. A schematic plumbing diagram for thesplit-stream setup herein described is shown in Fig. 2 of the maintext.

Samples were ablated using a Photon Machines Analyte G2,ArF Excimer LA system, equipped with a fast-washout two-volumeHelEx® cell and adapted with custom-made Au traps placed alongthe carrier gas line upstream from the sample cell in order tominimize Hg contributions to the 204 mass (Gehrels et al., 2008).Ultra-high purity He was used as the sample carrier gas, flow-ing through the cell at a total rate of 0.390 SLPM (MFC1 = 0.050SLPM, MFC2 = 0.340 SLPM; Fig. 2). After the exit of the abla-tion cell, Ar was added flowing at a rate of 1.200 SLPM beforethe aerosol + He + Ar mix entered a mini cyclonic spray chamber(Cinnabar spray-chamber by Glass Expansion®), which served as amixing volume in which the gas-analyte blend was homogenizedbefore splitting. After exiting the cyclonic chamber the mixture was

Nu Plasma is lower than that of the Element2, if un-obstructed, thetotal gas flow will tend to go toward the MC-ICP-MS. To overcomethis problem we placed a high-precision needle valve in the line of

brian

ltstbsaiamc2sflwatfidtm∼d

A

fIuueticifrmslbaWe1

awtlosos(2ˇstRsovsfi


east pressure (i.e., line going to the Nu Plasma), which allowed uso adjust the relative proportion of the total aerosol + He + Ar flowent to the multicollector; the total mass flow in this line was moni-ored on a precision Mass Flow Monitor Whisper unit manufacturedy Alicat Scientific® (MFM1 in Fig. 2). By using this flow-balancingetup, the relative proportion of aerosol sent to both instrumentst the split can be tuned to optimize signal intensity and obtainon beams that would result in accurate and precise analyses, andttain long-term stability for the instrumental drift of LASS-ICP-MSeasurements. We found the optimal splitting proportions to be

lose to 70–80% of the analyte directed toward the Nu Plasma and0–30% toward the Element2. In addition to balancing the gas flowsuch that the MFM1 unit reads a value of ∼80% of the total input gasow, the signal intensity measured on both mass-spectrometersas also used to confirm that the desired split proportions had been

chieved. To do this, the measured signal resulting from the abla-ion of the primary Sri Lanka (SL2) zircon reference material wasrequently monitored. Under typical conditions, where the lasers connected to only one of the mass-spectrometers and a 30 �miameter spot is being used, a 180Hf beam intensity of ∼1.3 V inhe Nu Plasma and a 238U intensity of ∼4 × 107 cps on the Ele-

ent2 are generally observed; these intensities are reduced by20% and ∼80%, respectively, when using our split-stream setupescribe here.

.2. Yb–Lu–Hf data processing

The data reduction strategy for Yb–Lu–Hf analyses generallyollows that described by Ibanez-Mejia et al. (2014) for the LA-MC-CP-MS analysis of baddeleyite. In this study, data was acquiredsing time resolved acquisition (TRA) analyses on the Nu plasmasing a 1.5 s integration time, and was reduced using Iolite (Patont al., 2011) and an in-house data reduction scheme (DRS) adjustedo process data from our collector-block configuration. The DRS files available from the authors upon request. Mass-bias factors toorrect for hafnium fractionation (ˇHf) were calculated by measur-ng the 179Hf/177Hf value of each analysis and using an exponentialractionation law (Russell et al., 2002) with respect to a referenceatio of 0.7325 (Patchett and Tatsumoto, 1981). In the presence of aeasurable Yb signal (i.e., considered detectable when the ablation

ignal mean of all masses of interest is above 3 S.D. from their base-ine means), its own mass fractionation factor ˇYb can be calculatedy monitoring two non-interfered masses (e.g., 171Yb and 173Yb)nd normalization with respect to a reference ratio as proposed byoodhead et al. (2004). During this study the Yb model of Vervoort

t al. (2004) was adopted, and ˇYb factors were calculated using a73Yb/171Yb reference value of 1.129197 for analyses with an aver-ge total-Yb beam greater than 200 mV. Alternatively, in sampleshere the Yb signal intensities are lower than this value – as is

he case for many natural zircons – the uncertainties on the calcu-ated ˇYb factors are large and consequently have a negative impactn the accuracy of the estimated 176Yb interferences. In this lattercenario, the mass-fractionation of Yb was approximated from thatf Hf by establishing a robust ˇHf–ˇYb relation for each particularession using only those analyses performed on high-Yb zirconse.g., R33 and FC-1) and Yb-doped synthetic zircons (Fisher et al.,011). The observed relationship can then be used to recast theHf of each analysis into a term xˇHf using the following expres-ion: xˇHf = (ˇYb)meas/(ˇHf)meas, which was used in exchange ofhe measured ˇYb values when correcting the moderate- to low-EE zircon analyses for Yb interference measured during that sameession. The validity of this approach is demonstrated by the results
btained from analyses on several secondary reference zircons witharying 176Hf/177Hf values and degrees of 176Yb interference, asummarized in Table 2 of the main text and shown graphically ingures accompanying this supplementary material.
Research 267 (2015) 285–310 305

After this first step for Yb mass-bias and interference subtrac-tion has been applied, a secondary Yb-bias correction (describedin detail by Fisher et al., 2014a,b; Ibanez-Mejia et al., 2014) wasapplied by determining a bias factor to the reference ‘natural’176Yb/173Yb composition such that the slope in 176Hf/177Hf vs.176Yb/177Hf space for the Yb-doped zircons was minimized. Thisapproach is similar to that used previously by Vervoort et al. (2004)to correct solution Hf data for Yb interference. Final mass-bias andinterference-corrected 176Hf/177Hf ratios are thus calculated usingthe following expressions:

176Hf177Hfcorr

=[(

176(Hf + Yb + Lu)meas − 176Ybcalc − 176Lucalc177Hfmeas

)

·(

M176M177

)ˇHf]· BFHf (A1)

176Ybcalc = 173Ybmeas ·[

(176Yb/173Ybref) · BFYb

(M176/M173)(ˇYb) or (xˇHf)

](A2)

176Lucalc = 175Lumeas ·[

176Lu/175Luref

(M176/M175)(ˇYb)

](A3)

where M176/M177, M176/M173 and M176/M175 are the ratios ofthe exact masses of these isotopes of Hf, Yb, and Lu, respectively.The BFYb term is the secondary Yb correction factor derived fromthe Yb-doped zircon measurements, and BFHf is the instrumental-bias factor for Hf. This last term was obtained by normalizationagainst repeated analyses of Mud Tank zircons and using the refer-ence solution-MC-ICP-MS value of 0.282507 (Woodhead and Hergt,2005) as recommended by Fisher et al. (2014b).

A.3. U–Pb data processing

U–Th–Pb isotopes were measured on an Element2 SC-ICP-MSusing the scanning parameters listed in Table 1 in the main bodyof the text. By using the dwell-time values listed, each completescan across the designated mass range is of ∼110 ms in duration.Each individual analysis consists of a 15 s gas baseline measure-ment, which is immediately followed by 80 s of ablation. After thelaser stops firing an additional 5 s of measurement were allowed inorder to capture the tail of the signal dropping back down to base-line values. Therefore, the total measurement time for each spotis of 90 s in duration, during which the Element2 completes 810scans over the defined mass range. The typical washout time, or thetime elapsed between the end of one analyses and the beginningof baseline measurements for the next spot, was typically set to 20or 30 s. Although 80 s of signal from the entire ablation pass werealways collected, only the first 30 s (270 on-peak scans) were usedto calculate the 206Pb/238U and 207Pb/206Pb compositions used forage calculation; the remaining ∼40 s of data (ca. 440 scans) wereused to visually evaluate intra-grain compositional complexitiesand potential zone-mixing that might have occurred deeper in theablation pit when the Hf isotopic analysis were still underway. Themain reasons for not using the entire collection time for U–Pb ratioscalculation are the fast drop in signal observed during the entireablation time and the deviation from linearity of the down-pit frac-tionation, which make the last 40 s of data an unnecessary sourceof scatter in the calculation of the ratios due to the already reducedcount-rates in the detector during LASS-ICP-MS acquisitions. Wenote that, although the LASS-ICP-MS technique described in this
contribution assigns U–Pb dates to particular Yb–Lu–Hf isotopecompositions on a whole-spot basis, future developments usingthis split-stream approach have the potential to take further advan-tage of the time-resolved capabilities of LA-ICP-MS to scrutinize the

3 brian Research 267 (2015) 285–310

d(

f(lptbs(ftvetttc(tyd3ta2

acttitc

iceCSIShtbe2

csIcis2aatraubMiael

A

B

Fig. 13. (A) Cross-sectional profile of an ablation pit in zircon, acquired using a WykoNT9800 optical interferometer. This crater was produced using 200 laser pulses andother laser parameters listed in Table 1. (B) Summary of interferometry measure-ments from various craters excavated with varying numbers of pulses per burst;from this experiment, a laser excavation rate of 0.053 �m/pulse (or 0.37 �m/s) was


ata on a time-slice basis rather than using whole-spot integrationse.g., Tollstrup et al., 2012).

The uncertainty propagation scheme adopted during this studyollows the procedure recommended by the PlasmAge workgroupwww.plasmage.org). The scheme is as follows. (1) Average base-ine values for each mass, calculated from the 15 s of data collectionrior to initiation of ablation, were subtracted line-by-line fromhe time-resolved measured intensities. (2) Uncertainties in theaseline estimation for each mass i were calculated using Pois-on statistics as the square root of the baseline integrations mean�i

baseline= √

xibaseline

). (3) The baseline corrected 206Pb/238U valuesor the first 30 s of ablation were plotted against elapsed acquisitionime and a linear least-squares fit was performed as described pre-iously in Cecil et al. (2011), Gehrels et al. (2008) and Ibanez-Mejiat al. (2014) in order to correct for the laser-induced elemental frac-ionation (LIEF). (4) The first second of ablation data was discardedo allow for the signal to stabilize (e.g., Frei and Gerdes, 2009), andhe LIEF-corrected 206Pb/238U value for each ablation pass was cal-ulated as the intercept of the linear regression at ablation timet) = 1 s; the uncertainty of this ratio (�206Pb/238U) is estimated fromhe uncertainty on the intercept of this parametric fit. (5) For anal-ses with a 204Pb signal above detection level (i.e., consideredetectable when the Hg-corrected ablation signal mean is above

S.D. from the Hg-corrected baseline mean), common-Pb correc-ions were applied using the model of Stacey and Kramers (1975)nd additional uncertainties to the instrumentally-determined06Pb/204Pb and 207Pb/204Pb of 1.0% and 0.3%, respectively, weressigned. These uncertainties were propagated throughout the agealculations as described by Gehrels et al. (2008). At this stage, theotal uncertainty of each spot (which will be henceforth referredo as internal integration uncertainty) consists of the propagationn quadrature of the uncertainties related to the gas blank subtrac-ion (�i

baseline), the LIEF correction (�206Pb/238U) and the common-Pb

orrection (�pbc-corr) if the later was applied.Elemental- and mass-dependent fractionation corrections,

nduced by the ablation process and ICP-MS measurement, are bestorrected by normalization with respect to a matrix-matched ref-rence material (Kosler et al., 2002; Kosler and Sylvester, 2003;hang et al., 2006; Gehrels et al., 2008; Cottle et al., 2009, 2012;lama et al., 2008; Frei and Gerdes, 2009; Thomson et al., 2012;banez-Mejia et al., 2014). To do this, we use fragments of the sameri Lanka (SL2) reference crystal of Gehrels et al. (2008), whichas an ID-TIMS age of 563.5 ± 3.2 Ma and an average U concen-ration of approximately 520 �g/g(Zr). Each session was bracketedy five SL measurements at the beginning, five at the end, and onevery five unknowns. A running mean fractionation factor for the06Pb/238U and 207Pb/206Pb values at each point in the session wasalculated by averaging the measured values for the ratios in theix neighboring SL measurements and dividing it over the referenceD-TIMS ratios. This running-average factor can then be used toorrect the unknowns for fractionation at the same time as correct-ng for any instrumental drift that might occur during a particularession (Gehrels et al., 2008; Paton et al., 2010; Ibanez-Mejia et al.,014). It has been argued by Horstwood (2008), Cottle et al. (2009),nd the PlasmAge community, that the minimum uncertainty ofny given measurement should incorporate the internal integra-ion uncertainty and the excess variability observed on the primaryeference material used for fractionation correction. Therefore,fter applying the instrumental drift correction, a normalizationncertainty factor (or over-dispersion factor, OD) was derived foroth the 206Pb/238U and 207Pb/206Pb ratios in order to make theSWD values of the reference material mean equal to unity. The

nternal integration uncertainty and the normalization uncertaintyre regarded as independent sources of error, and therefore thisxcess scatter factor is propagated in quadrature with the calcu-ated uncertainty of each data point in order to obtain the minimum

determined and proven to be linear with time at least down to the total pit depthsexcavated during this study. The LASS-ICP-MS results presented in this study wereconducted using 560 laser repetitions per spot (∼30 �m total crater depth).

uncertainty of each individual measurement. In the case whenthe calculated MSWD values of the 206Pb/238U and/or 207Pb/206Pbmeans of the primary reference material are unity or below, noover-dispersion uncertainties need to be added. From this it followsthat the reported uncertainties for the apparent dates of LA-SC-ICP-MS analyses are quoted at three levels of increasing uncertainty, inthe form ±[X][Y][Z] (columns ±1�(a), ±1�(b) and ±1�(c) in the U–Pbcolumns of the supplementary material). The first level [X] refersto the internal integration uncertainty of each individual analysis,[Y] accounts for the propagation of the excess scatter (or normal-ization uncertainty) that is specific for each sample or session, and[Z] is the final total uncertainty that includes the systematic errorsassociated with the U decay constant and reference-material (SL2zircon) calibration. Weighted mean ages for cogenetic suites of zir-cons (i.e., igneous samples) reported in the Figures and Tables arequoted with two levels of uncertainty in the form ±(A)[B], where(A) represents the weighted-mean uncertainty calculated using theindividual-spot uncertainties [Y] described above (thus incorpo-rating over-dispersion), and [B] represents the total uncertaintiesafter systematic errors have been propagated (accounted for in theuncertainty level [Z]).

A.4. Dimensions of the analytical pits

In order to fully quantify the dimensions – and most impor-tantly the depth – of the generated analytical pits, the total depthof several ablation craters were measured by means of optical inter-ferometry. This quantification is important to estimate whether
U–Pb–Hf data collected for a particular ablation spot using our ana-lytical approach remains within a relatively shallow depth and istherefore likely to correspond to the zircon growth domain of inter-est. These measurements were performed using a Wyko NT9800
http://www.plasmage.org/



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A

t0

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nterferometer at the College of Optical Sciences at the Universityf Arizona. A series of craters with increasing depths were exca-ated on a Mud Tank zircon fragment, using successive incrementsf 50 pulses from 50 to 450 total pulses. Additional craters wherexcavated with 490 and 560 bursts, with the latter value being usedor the LASS-ICP-MS measurements presented here. Results of thisxperiment are shown in Fig. 13; the upper panel is an example of

profile obtained for a 200-pulse crater (all other lasing settings asisted in Table 1 of the main text), where it can be noted that theottom of the ablation crater is slightly rounded and has a max-

mum topography of ca. 0.9 �m. We therefore adopted ±1 �m ashe uncertainty of the depth estimations. The lower panel of Fig. 13hows a summary of all the interferometry results, which demon-trates that the drilling rate of the G2 laser in zircon is close toinear up to at least 560 pulses and on the order of ∼0.053 �m/pulseequivalent to 0.37 �m/sec using a 7 Hz repetition rate). This rates slightly slower than what was estimated by Ibanez-Mejia et al.2014) for the ablation of baddeleyites using similar lasing param-ters. The total analytical pit generated by the LASS-ICP-MS routineerein described (i.e., 560 pulses) is of approximately 30 �m inepth, thus never exceeding a 1:1 aspect ratio for the excavatedraters and likely mostly staying (in depth) within growth domainshat were wide enough to accommodate a 40 �m or 50 �m diam-ter ablation spot.

ppendix B. Supplementary data

Supplementary data associated with this article can be found, inhe online version, at http://dx.doi.org/10.1016/j.precamres.2015.6.014

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unraveling crustal growth and reworking processes in

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