Lithos 70 (2003) 91 – 110 www.elsevier.


Very fast exhumation of high-pressure metamorphic rocks with excess 40Ar and inherited 87Sr, Betic Cordilleras, southern Spain
Koen de Jong *
Department of Isotope Geochemistry, Vrije Universiteit, Amsterdam, The Netherlands ´ ´ CNRS, UMR 6526 Geosciences Azur, Universite de Nice-Sophia Antipolis, Nice, France

Abstract ´ In order to attempt to further constrain the age of the early Alpine tectonic evolution of the Mulhacen Complex and to explore the influence of inherited isotopes, micas from a small number of well-characterised rocks from the Sierra de los ´ Filabres, with a penetrative tectonic fabric related to the exhumation of eclogite-facies metamorphic rocks, were selected for 40 Ar/39Ar and Rb – Sr dating. A single phengite grain from an amphibolite yielded an 40Ar/39Ar laser step heating plateau age of 86.9 F 1.2 Ma (2r; 70% 39 Ar released) and an inverse isochron age of 86.2 F 2.4 Ma with an 36Ar/40Ar intercept within error of the atmospheric value. Induction furnace step heating of a biotite separate from a gabbro relic in an eclogite yielded a weighted mean age of 173.2 F 6.3 Ma (2r; 95% 39Ar released). These ages are diagnostic of excess argon (40ArXS) incorporation, as they are older than independent age estimates for the timing of eclogite-facies metamorphism and intrusion of the gabbros. 40ArXS incorporation probably resulted from restricted fluid mobility in the magmatic rocks during their metamorphic recrystallisation. Rb – Sr whole-rock – phengite ages of graphite-bearing mica schists from Paleozoic rocks (Secano unit) show a dramatic variation (66.1 F 3.2, 40.6 F 2.6 and 14.1 F 2.2 Ma). An albite chlorite mica schist from the Mesozoic series of the Nevado – ´ Lubrın unit has a whole-rock – mica – albite age of 17.2 F 1.9 Ma, which is within error of an 40Ar/39Ar plateau age published previously and of the youngest Rb – Sr age of the Paleozoic series obtained in this study. The significant spread in Rb – Sr ages implies that progressive partial resetting of an older isotopic system has occurred. The microstructure of the samples with preMiocene Rb – Sr ages reveals incomplete recrystallisation of white mica and inhibited grain growth due to the presence of graphite particles. This interpretation agrees with previously published, disturbed and slightly dome-shaped 40Ar/39Ar age spectra that may point similarly to the presence of an older isotope component. The progressively reset Rb – Sr system is a relic ´ of Variscan metamorphism of the Paleozoic series of the Mulhacen Complex. In contrast, the origin of the ca. 17.2 Ma old sample from the Mesozoic series precludes any isotopic inheritance, in agreement with its pervasive tectono-metamorphic recrystallisation during the Miocene. ´ Exhumation of the eclogite-facies Mulhacen Complex occurred in two stages with contrasting rates of about 22.5 mm/year during the early phase and 9 – 10 mm/year during the late phase; the latter with a cooling rate in the order of 330 jC/Ma. D 2003 Elsevier B.V. All rights reserved.

Ar/39Ar dating; Excess argon; Isotope inheritance; Phengite; Biotite; Fluids

* Present address. Argon Geochronology Laboratory, Department of Geosciences, National Taiwan University, 245 Choushan Road, Taipei 106, Taiwan, ROC. Tel.: +886-2-3365-1899; fax: +886-2-2363-6095. E-mail address: (K. de Jong). 0024-4937/$ - see front matter D 2003 Elsevier B.V. All rights reserved. doi:10.1016/S0024-4937(03)00094-X


K. de Jong / Lithos 70 (2003) 91–110

1. Introduction Phengite has yielded meaningful 40Ar/39Ar plateau ages for eclogite-facies metamorphic rocks (Bosse et al., 2000), but research during the last decade of the 20th century provided a lot of evidence for the incorporation of excess argon (40ArXS) in its lattice (e.g. Tonarini et al., 1993; Li et al., 1994; Arnaud and Kelley, 1995; Inger et al., 1996; Sherlock et al., 1999). 40ArXS uptake occurs in association with partial recrystallisation of high-pressure phengite during subsequent metamorphism at lower temperature and pressure (Hammerschmidt and Franz, 1992; Hannula and McWilliams, 1995; Ruffet et al., 1995; Reddy et al., 1996; de Jong et al., 2001). Alternatively, strongly restricted fluid mobility, leading to the incorporation of locally derived (inherited) argon, is commonly quoted as the mechanism responsible for the frequently observed elevated phengite 40ArXS ages in (ultra-) highpressure metamorphic rocks (Scaillet, 1996; Boundy et al., 1997; Li et al., 1999; Giorgis et al., 2000), and is also seen as the reason for the survival of pre-orogenic Rb –Sr ages in biotite (Verschure et al., 1980; Kuhn et ¨

al., 2000). It appeared that incorporation of argon into phengite may have been controlled by very low lattice and grain boundary diffusion under dry, eclogite-facies conditions and that the gas has been internally derived from within the eclogite protoliths. de Jong et al. (2001) attempted to constrain the age ´ of early Alpine exhumation of the Mulhacen Complex of the Internal Zone of the Betic Cordilleras of southern Spain, or Betic Zone (Fig. 1). They obtained widely scattered 40Ar/39Ar laser step heating plateau ages between 15.8 F 0.4 and 90.1 F 1.0 Ma (2r) on well-crystallised single phengite grains from orthogneisses in a small area in the easternmost Sierra de los ´ Filabres (Fig. 2). Age discordance was observed at the outcrop scale as well as in individual grains. The authors explained these phenomena by 40ArXS uptake that seems to be associated with the gneisses, since the Rb – Sr ages in these rocks are systematically younger than the K – Ar and 40Ar/39Ar ages. Specific to this case is the occurrence of hydraulic cracks in the gneisses, high atmospheric contamination and submicroscopic illitisation of phengite, permitting 40ArXS storage in interlayer vacancies and other lattice imper-

´ Fig. 1. Tectonic map of the eastern Betic Cordilleras, modified after de Jong (1993a). The sampled areas in the eastern Sierra de los Filabres (Figs. 2 and 3) are outlined. Stars: samples from the Sierra de Baza (SdB) and from Cerro del Almirez (CdA) are discussed.

K. de Jong / Lithos 70 (2003) 91–110


´ Fig. 2. Geological map of the easternmost Sierra de los Filabres, modified after de Jong et al. (2001), with the sample locations indicated by arrows. The Ar/Ar total gas ages obtained by these authors on single phengite grains at different locations (stars) in gneiss body of the Macael – Chive unit are indicated.


K. de Jong / Lithos 70 (2003) 91–110

fections. The oldest phengite was from a coarsegrained gneiss with closely spaced late-stage hydraulic cracks, which are lacking in fine-grained mylonitic gneiss that yielded the youngest micas. Hence, the interaction of meteoric waters with the hot metamorphic rocks, phengite recrystallisation and 40ArXS uptake were much more intense in the coarse-grained gneiss. Like the fine-grained mylonitic gneisses, mica schists and mica-bearing foliated amphibolites lack such extensively developed hydraulic crack networks, rendering them less liable for the incorporation of 40 ArXS by this mechanism. Accordingly, white mica from albite –chlorite – mica schists and marbles with a penetrative S2 yielded 15.4 –17.6 Ma 40Ar/39Ar plateau and total fusion ages (de Jong et al., 1992) that are not obviously affected by significant levels of incorporated 40ArXS. The aim of the present study is to investigate further the occurrence and source of excess argon as well as the role of limited fluid mobility in the incorporation process during the early tectono-meta´ morphic evolution of the Mulhacen Complex in the ´ Sierra de los Filabres. For this purpose, we used biotite from a gabbro with a Late Jurassic Rb –Sr isochron age, in which 40ArXS incorporation has been established, and that occurs in the core of an eclogite, which is chemically well characterised. In addition, we selected a phengite grain from an amphibolite, which occurs in the same level as the eclogite, and that acquired a penetrative fabric during the main tectono-metamorphic phase, D2, subsequent to the eclogite-facies metamorphism. Also, we applied Rb –Sr dating to a small number of mica schists with a tectono-metamorphic fabric that was formed during D2 and which, in a previous study, yielded 40Ar/39Ar age spectra that are in part slightly dome-shaped and in one case flat. Our data set has a large spread in ages, which is interpreted as due to the occurrence of 40 ArXS and partially inherited radiogenic 40Ar and 87 Sr isotopes, but, the least affected samples permitted ´ to date the timing of exhumation of the Mulhacen Complex as Middle Miocene.

External Zone, which crops out in windows as the ´ (very) low-grade metamorphic Almagride Complex (Fig. 1; Simon, 1987; de Jong, 1993a). These are, ´ from top to bottom: (1) the Malaguide Complex, (2) ´ rride Complex, (3) Mulhacen Complex and (4) ´ Alpuja Veleta Complex (Egeler and Simon, 1969; Puga and ´ Diaz de Federıco, 1978; de Jong, 1993a,b; Puga et ´ ´ al., 1999, 2002). The Alpujarride and Mulhacen complexes have basal series of graphite-rich metapelites and cover series of metapelites and metapsammites with abundant metacarbonates and greenstones and locally gypsum (Egeler and Simon, 1969; de Jong and Bakker, 1991; de Jong, 1991). The carbon´ ate series of the Alpujarride Complex are well dated as Middle to Late Triassic by microfossils (Kozur et al., 1985; Simon, 1987), whereas the basal series of some tectonic units yielded Variscan ion-microprobe zircon ages (Zeck and Williams, 2001, and references ´ therein). The Mulhacen Complex experienced an Alpine metamorphism composed of a sequence of different metamorphic facies (de Roever and Nijhuis, 1963), as well as pre-Alpine recrystallisation, as will ´ be outlined below. The Malaguide Complex has a Paleozoic basal series covered by a condensed, but almost complete Mesozoic and Tertiary section (Egeler and Simon, 1969). Sediment petrographical analysis of its Late Paleozoic series implies that it experienced a Variscan orogeny (Herbig and Stattegger, 1989; Henningsen and Herbig, 1990), although a major angular unconformity between the Paleozoic and younger series did not form (Makel, 1988). The ¨ Veleta Complex comprises a monotonous lithological sequence of graphite-bearing mica schists and quartzites that yielded rare Middle Devonian (Lafuste and ´ Pavillon, 1976) and Riphean (Gomez-Pugnaire et al., 1982) fossils. The Alpine tectono-metamorphic recrystallisation has essentially obliterated the preAlpine fabrics and mineral assemblages, except for inclusions in chloritoid porphyroblasts in some mica schists that are very rich in graphite (Puga and Diaz ´ ´ de Federıco, 1978; Gomez-Pugnaire and Sassi, 1983; Puga et al., 2002). ´ 2.1. The Mulhacen Complex

2. Tectonic setting The Betic Zone comprises a stack of four nappe complexes that have overthrust the southernmost ´ The Mulhacen Complex in the Sierra de los ´ Filabres is composed of three superimposed nappes (Figs. 2 and 3), each with a probably Paleozoic

K. de Jong / Lithos 70 (2003) 91–110


´ Fig. 3. Geological map of the northern part of the central Sierra de los Filabres, modified after de Jong et al. (1992), with arrows indicating the ´ ´ sampled sites. Thrust slices on top of the Alpujarride Complex consisting of rocks of the Mulhacen Complex, north of Huertecicas Altas, have been omitted for clarity. Triangles indicate nappe contacts.


K. de Jong / Lithos 70 (2003) 91–110

basal series of graphite-rich garnet mica schists that contain orthogneisses and metagranites in the uppermost two nappes (de Jong and Bakker, 1991). The cover series are generally regarded as Triassic and younger and comprise alternating quartzites and (albite-bearing) mica schists with marble levels in the upper parts (de Jong and Bakker, 1991; Tendero et al., 1993), hereafter called Mesozoic series. Ultramafic rocks, mainly serpentinites, and abundant greenstones occur in these higher levels, in part as a mapable unit of amphibolites and amphibole mica schists ((Figs. 2 and 3); de Jong and Bakker, 1991, encl. 1). Early Alpine eclogites occur locally in these greenstones (Morten et al., 1987; Bakker et ´ al., 1989; Gomez-Pugnaire et al., 1989; Puga et al., 1989, 1999), which are wrapped by the main foliation (S2) in the matrix. Part of the eclogitefacies metabasites are derived from often cumulitic gabbros, with partly preserved igneous paragenesis, a MORB-like chemical composition and 143Nd/ 144 Nd ratios higher than 0.5130 and 87Sr/86Sr ratios below 0.705 (Puga et al., 2002). Morten et al. (1987) inferred that crystallisation of the gabbros occurred at pressures below 1 GPa. A troctolitic gabbro in the core of an eclogite yielded an Rb –Sr mineral isochron age of 146 F 3 Ma (Hebeda et al., 1980). The serpentinites are derived from spinel lherzolites and secondary harzburgites with spinifex-like textures, which both contain abundant partly rodingitised dolerite dykes (Puga et al., 2002). The origin of the greenstone association is still a matter of debate, with models ranging from a dismembered ocean floor sequence (Puga et al., 1989, 1999, 2002) to continental, rift-related mag´ matism (Gomez-Pugnaire et al., 2000). Glaucophane-bearing dolerites have locally well-preserved intrusive contacts with calcite marbles (de Jong and Bakker, 1991). The greenstone association may have developed in small oceanic pull-apart basins situated in a major continental strike-slip zone that connected Late Jurassic spreading centres in the Atlantic and Ligurian Oceans (de Jong, 1991, 1993a). Maximum pressures of 2.0 –2.2 GPa have been estimated for kyanite eclogites (Puga et al., 1999, ´ 2002) and metamorphic ultramafic rocks (Lopez ´ ´ ´ Sanchez-Vizcaıno et al., 2001) in the Mulhacen Complex at temperatures of about 700 jC. Strong

decompression concomitant with cooling of the rocks to 500– 600 jC took place during and subsequent to the main tectono-metamorphic phase, D2, which occurred at a pressure of about 1.5– 1.7 GPa (Puga et al., 2002) and 0.8 – 1.2 GPa (Bakker et al., 1989; de Jong, 1991, 1993a) during the final phase (Fig. 10). This resulted in pervasive amphibolitisation of the eclogites. Further retrogression is marked by widespread albite and chlorite growth that occurs synkinematically with a phase of localised penetrative D3 folding at pressures of about 0.4 – 0.5 GPa and temperatures around 400 jC (Fig. 10; de Jong, 1991, 1993a,c). The cooling was followed by pronounced late stage fluid-assisted reheating shown by the widespread occurrence of rims of oligoclase and biotite around albite and chlorite, respectively, as well as by rare and local growth of staurolite and kyanite during the early stages of D4 in mica schists ´ of the Mesozoic series of the Nevado– Lubrın unit (Bakker et al., 1989; de Jong, 1991, 1993a,c). The absence of garnet constrains the P –T conditions at around 0.4 – 0.5 GPa and temperatures of about 500 jC (Fig. 10). The reheating was related to extension (Bakker et al., 1989; de Jong, 1991, 1993a), which resulted in recrystallisation, isotope resetting and 40 ArXS incorporation (de Jong et al., 2001). Ductile (D5) and brittle – ductile (D6) shear zones, which developed during retrogression, occur at various ´ levels within the Mulhacen Complex, but character´ istically at the contact with the overlying Alpujarride Complex (de Jong, 1991, 1993a,c). Micas from rocks with a penetrative alpine tectonic foliation have Rb – Sr ages that generally range between 12.5 and 16.9 Ma, whereas K – Ar and 40Ar/39Ar ´ dates span 13.7 –90.7 Ma (Monie et al., 1991; de Jong ´ et al., 1992, 2001). Monie et al. (1991) obtained 40 Ar/39Ar ages of 24.6 F 3.6 and 48.4 F 2.2 Ma on amphibole (Sierra de Baza, Fig. 1). Eleven SHRIMP U – Pb analysis on nine zircon grains in a pyroxenite layer in ultramafic rocks (Cerro del Almirez, Fig. 1), which are characterised by high pressure breakdown of antigorite to spinifex-textured olivine and orthopyroxene, yielded a mean age of 15.0 F 0.6 Ma ´ ´ ´ (2r) (Lopez Sanchez-Vizcaıno et al., 2001). This U – Pb zircon age is comparable to the majority of Rb – Sr ages of white mica and to 40Ar/39Ar ages of this mineral that are the least affected by 40ArXS uptake. Zircon fission-track ages of the Sierra de los

K. de Jong / Lithos 70 (2003) 91–110


´ Filabres are in the 11– 14 Ma range (Johnson et al., 1997). ´ 2.2. Pre-alpine history of the Mulhacen Complex Despite the pervasive nature of Alpine tectonometamorphic recrystallisation, the basal series of the ´ Mulhacen Complex contain unambiguous relics of pre-Alpine tectono-metamorphic evolution. Pre-Alpine deformation structures are found in the deeper part of the complex in the Sierra Nevada, in some boudins or layers of graphite-bearing mica schists, which also contain pre-Alpine amphibolite-facies parageneses (Puga et al., 1975, 2002; Puga and Diaz de ´ Federıco, 1978). The occurrence of chloritoid + almandine, chiastolite + almandine + biotite F staurolite parageneses or rare cordierite points to P –T conditions of about 0.2 –0.3 GPa and 500 –600 jC (Puga et al., 2002). Elsewhere, studies of the relationship between mineral growth and superimposed deformation phases have not yielded any evidence for the presence of relic minerals that did not form during ´ Alpine metamorphism (Kampschuur, 1975; Martınez ´ Martınez, 1980; Bakker et al., 1989; de Jong, 1991). However, complex inclusion patterns in the cores of some Alpine porphyroblasts in the Sierra de los ´ Filabres have been interpreted as due to a pre-Alpine orogeny (Helmers and Voet, 1967; Vissers, 1977), especially in garnets and staurolites that are spatially associated with orthogneisses. Gneisses and metagranites of the basal series of ´ this complex in the Sierra de los Filabres have yielded Rb – Sr errorchrons ranging between 275 and 191 Ma (Andriessen et al., 1991), which the authors discussed in the context of partial Alpine resetting and incomplete isotope rehomogenisation. A 267 F 29 Ma Rb – Sr age (Andriessen et al., 1991) and a 307 F 34 Ma Sm – Nd isochron (Nieto, 1996) are regarded as the best estimate of the crystallisation age of the subsolvus granites. The country rock to these intrusives is affected by contact metamorphism, as revealed by the occurrence of hedenbergite skarn and hornfels bodies (Helmers, 1982; de Jong and Bakker, 1991). The petrology of the granites and associated contact metamorphic rocks indicates an intrusion depth of at least 6 km (de Jong and Bakker, 1991), which agrees with P – T estimates for pre-Alpine mineral assemblages described by Puga et al. (2002).

3. Sample description 3.1. Troctolitic gabbro Biotite separate ALM 104 (63 – 125 Am sieve fraction) has been obtained from a 1-m diameter massive troctolitic gabbro that occurs in an eclogite, which yielded a 146 F 3 Ma Rb – Sr mineral isochron age and an initial 87Sr/86Sr ratio of 0.7028 F 0.0001 (Hebeda et al., 1980). The biotite separate is known to have 40ArXS and was used as one of the points that defined the isochron and was selected for analysis to better understand this phenomenon. The gabbro is separated from the underlying albite chlorite mica schists (Tahal schists, de Jong and Bakker, 1991) by a fault that was folded during D4 and subsequently reactivated as a low-angle D6 detachment fault (de Jong, 1993c). This outcrop is part of a series of amphibolites and amphibole mica schists of the ´ Nevado – Lubrın unit (Fig. 2). The course-grained gabbro has a cumulitic texture with olivine and labradorite – oligoclase as cumulus phases and clinopyroxene as well as minor brown hornblende and biotite as intercumulus phases. 3.2. Micaceous amphibolite The slightly elongated (0.75 Â 1.5 mm) single phengite grain, JK 0, which has been used for 40Ar/39Ar dating, was obtained from a well-crystallised amphibolite with a strongly developed tectonic fabric, from the same lithological unit as ALM 104 (Fig. 2). Blue-green hornblende and phengite have a well-developed shapepreferred orientation with respect to foliation S2, whereas c-axes of the amphibole are parallel to the lineation L2. Cores of a number of blue-green hornblendes contain relics of glaucophane. The transformation of glaucophane to blue-green hornblende is a synD2 reaction (Bakker et al., 1989; de Jong, 1991, 1993a,c). 3.3. Mica schists Mineral separates in the 125– 250 Am sieve fraction of four mica schists have been used for Rb –Sr mineral dating. The same white mica separate of three of these samples has been analysed by 40Ar/39Ar furnace step-heating, which yielded a plateau age of


K. de Jong / Lithos 70 (2003) 91–110

17.3 F 0.2 Ma (ALM 270) and in two cases an 40 Ar/39Ar age spectra with progressively increasing apparent ages over the main part of degassing that is somewhat dome shaped as the last important degassing step is slightly younger (Fig. 9). Total gas ages are 19.1 F 0.1 (ALM 272) and 25.9 F 0.1 Ma (ALM 273). The 40Ar/39Ar isotopic data are given in de Jong et al. (1992). The samples were chosen to better understand why some samples yielded disturbed age spectra and others did not. The mica schists have a penetrative quartz– mica differentiated S2 foliation. ALM 272, 273 and 274 are
Table 1 40 ´ Ar/39Ar analytical data of micas from greenstones, Nevado – Lubrın unit Step

graphitic chloritoid garnet mica schists from the Secano unit (Fig. 3; sensu, Helmers and Voet, 1967). This unit, which resembles the basal series of the Macael – Chive unit, however, without gneisses, is ´ separated from the underlying Nevado– Lubrın unit by a D6 detachment fault (de Jong, 1991). ALM 272 and 273 are taken from the same outcrop within 20 m from each other. ALM 274 is the most quartz-rich sample and the least graphite rich. Chloritoid and garnet porphyroblasts were formed pre- and syn-D2, during which the main tectonic foliation of the rocks was formed. Continuous lattice bending and limited

Aratm (%)


ArK (10À 13 cm3)


Ar (%)





Apparent age (Ma) – 75.3 F 50.3 174.1 F 106.6 160.7 F 61.0 147.3 F 21.8 159.9 F 14.4 165.0 F 9.8 164.6 F 3.2 168.3 F 2.2 174.1 F 3.1 181.5 F 3.8 185.2 F 2.0 355.9 F 28.0 948.1 F 2681.4 174.7 F 1.6

– 2.48 F 3.79 5.90 F 2.16 5.43 F 0.77 4.96 F 0.51 5.40 F 0.35 5.58 F 0.11 5.57 F 0.08 5.70 F 0.11 5.91 F 0.14 6.17 F 0.07 6.30 F 1.10 12.71 F 146.52 40.30 F 1.69 Total age: Inverse isochron age steps 450 – 1150 = 173.2 F 8.7 Ma; 40Ar/36Ar intercept = 281 F 82; MSWD = 15 JK 0 (single phengite grain) (laser step heating) (J = 0.01709 F 1%, 2r) 0.35 97.25 110.53 0.65 0.40 92.67 101.01 0.59 0.45 90.65 325.50 1.92 0.56 54.89 4501.07 26.67 0.64 14.24 2846.62 16.86 0.70 14.47 1629.74 9.66 0.82 19.72 2280.95 13.51 0.89 23.11 856.17 5.07 0.99 27.03 838.18 4.96 1.20 23.63 2491.93 14.76 Fuse 19.52 900.83 5.33

ALM 104 (biotite separate, 63 – 125 lm, 6.0 mg) (furnace step heating) (J = 0.01716 F 1%, 2r) 450 100.00 6.14 0.06 3.664 550 88.31 69.35 0.73 0.000 650 75.86 48.22 0.51 0.731 700 68.59 51.79 0.54 4.203 780 79.80 116.91 1.22 0.596 840 39.19 330.87 3.46 0.325 880 15.36 648.98 6.79 0.002 920 9.74 1428.49 14.95 0.000 960 10.60 2128.77 22.28 0.081 1000 13.55 1396.01 14.61 0.015 1050 13.10 1211.42 12.68 0.000 1150 10.99 1994.65 20.88 0.000 1350 26.54 120.59 1.26 1.177 Fuse 92.55 1.56 0.02 24.133

9.87 F 11.82 3.25 F 1.70 3.13 F 0.96 2.91 F 0.08 2.90 F 0.04 2.86 F 0.06 2.85 F 0.04 2.82 F 0.10 2.76 F 0.12 2.80 F 0.06 3.01 F 0.08 Total age: Inverse isochron plateau steps (0.35 – 0.82) = 86.2 F 2.4 Ma; 40Ar/36Ar intercept = 299.0 F 4.8; MSWD = 0.96

0.045 0.011 0.013 0.001 0.001 0.001 0.001 0.002 0.004 0.006 0.007

282.1 F 312.6 98.0 F 50.0 94.3 F 28.0 87.8 F 2.4 87.7 F 1.2 86.3 F 1.7 86.0 F 1.4 85.4 F 2.8 83.5 F 3.7 84.7 F 1.6 90.8 F 2.4 87.9 F 2.2

Step = temperature (jC) or laser output power (in Watt) for material analysed with an induction furnace or a laser probe, respectively. 40Aratm is the atmospheric 40Ar; 40Ar* is the radiogenic argon from natural K-decay; 37ArCa is the Ca-derived argon during irradiation. The volume of 39 ArK (K-derived argon during irradiation) is based on a mass spectrometer sensitivity of 7 Â 10À 10 V cmÀ 3 STP. Uncertainty is quoted at the 2r level; step ages do not include the errors in J and the age of the flux monitor. Decay constant 40Ktot = 5.543 Â 10À 10 yearÀ 1. 40Ar/36Ar measured: 288 F 0.5.

K. de Jong / Lithos 70 (2003) 91–110


recrystallisation to strain-free phengite in microfold hinges is especially prominent in ALM 272 and ALM 273. Continuity between microfold limbs and hinges is often maintained, and hence, the amount of shapepreferred orientation of white mica parallel to S2 cleavage septa is relatively limited. Such a microstructure points to the pinning of mica (sub) grain boundaries and dislocations on graphite particles. Cleavage microlithons contain relics of S1. ALM 270 is an albite chlorite mica schist from the ´ Mesozoic series of the Nevado– Lubrın unit (La Yedra Schists and Marbles, de Jong and Bakker, 1991; Fig. 2). The sample is not affected by D3 crenulations, but chlorite and albite porphyroblasts, which are syn-D3 minerals (de Jong, 1991, 1993a,c), overgrew S2. Phengite grains are well crystallised and strain-free, and generally lie with their basal cleavage plane in the differentiated S2 layering.

1000ETPR electron multiplier. A Pyrex cold finger at À 95 jC and a Zr – Al alloy getter operated at 400 jC purified the extracted gas. System blank runs were carried out at the start of each laser experiment and were repeated every third run. Background values were typically 1 Â 10À 11, 5 Â 10À 14, 2 Â 10À 13 and 1 Â 10À 12 cm3 STP for the 40, 39, 37 and 36 argon isotopes, respectively, and were subtracted from the subsequent sample analysis results. Samples ALM ´ 104 and JK 0 were irradiated in the Melusine reactor (Grenoble, France) for 40.95 h together with flux monitors biotite standard 4B (K – Ar age: 17.25 Ma, Hall et al., 1984 and subsequent analyses in Nice and Toronto) and MMHb (K – Ar age: 520.4 Ma, Alexander et al., 1978), respectively, while being rotated around a vertical axis. The irradiation parameter J was obtained from the 40Ar*/39ArK ratios measured from

4. Experimental procedures and mineral separation Single phengite grain JK 0 was selected for Ar/39Ar incremental heating and separated from the hand specimen after gentle crushing. It was carefully selected under a binocular zoom microscope and subsequently ultrasonically cleaned in demineralised water for 5 min. Mineral separates for Rb – Sr and 40 Ar/39Ar analyses were prepared from the sieve fractions by means of a Faul table, a laboratory overflow centrifuge employing heavy liquids and a Frantz isodynamic magnetic separator. 40 Ar/39Ar analyses were made at the University of Nice-Sophia Antipolis (France) following the procedures outlined in detail by de Jong et al. (2001). Biotite separate ALM 104 was wrapped in high purity Al foil and incrementally heated to fusion with a highfrequency furnace system, whereas phengite single grain JK 0 was step heated using an argon ion laser probe with a continuous beam defocused to at least twice the grain diameter. Homogeneity of the heating of the grain was monitored with a coupled videomicroscope system. The laser extraction line consists of an Innova Coherent 70-4 continuous argon ion laser in combination with a sensitive gas mass spectrometer comprising a 12 cm, 120j M.A.S.S.E.R tube, a Baur-SignerR ion source and an A.E.M. ¨

Fig. 4. 40Ar/39Ar induction furnace step heating age spectrum (lower panel) and 37ArCa/39ArK ratio spectrum (upper panel) of biotite ´ separate ALM 104 from the Mesozoic series of the Nevado – Lubrın unit. The Rb – Sr mineral isochron age obtained by Hebeda et al. (1980) is indicated by the grey horizontal line.


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three standards in the tube at the same level as the samples. Rb –Sr dating was carried out at the Vrije Universiteit, Amsterdam, The Netherlands. Pressed powder pellets prepared from splits of whole-rock powder sample were analysed by X-ray fluorescence spectrometry for Rb and Sr contents and Rb/Sr ratios with a Philips PW 1404 automatic spectrometer. Spiked and unspiked Sr analyses were made on an automated Finnigan MAT-261 mass spectrometer with three Faraday cup multicollector system for Sr. Rb-spiked isotope dilution measurements were performed using a computer-controlled Teledyne mass spectrometer with a single Faraday cage collector. For additional analytical details, see footnote on Table 2. Mineral ages are calculated using decay constants given by Steiger and Jager (1977). Plateau, total ¨ fusion and isochron ages include errors in J and the age of the flux monitor and have errors quoted at the 2r level. Isochron calculations are according to Ludwig (2000). Plateau ages were calculated if 60% or more of the 39Ar was released in three or more contiguous steps with a probability-of-fit of the weighted mean of more than 5% (Ludwig, 2000). All argon isotopic measurements were corrected for linear extrapolation to gas inlet time, mass discrimination, atmospheric argon contamination and irradiation-induced contaminant Ar-isotopes derived from

Ca and K in the sample; correction factors applied: (36Ar/37Ar)Ca: 2.79 Â 10 À 4 ( F 3%), (39Ar/37Ar)Ca: 7.06 Â 10 À 4 ( F 4%), ( 40 Ar/ 39 Ar) K : 258 Â 10 À 4 ( F 3%).

5. Results The 40Ar/39Ar analytical data of samples ALM 104 and JK 0 are listed in Table 1 and portrayed as age spectra in Figs. 4 and 6, respectively. Rb – Sr isotopic analyses of mica schist samples ALM 270, 272, 273 and 274 are given in Table 2. 5.1.

Ar/39Ar step heating

5.1.1. Biotite separate ALM 104 Induction furnace step heating of biotite separate ALM 104 yielded an age spectrum with progressively increasing apparent ages from 147 to 185 Ma, subsequent to the first 1% of gas release with irregular apparent ages (Table 1; Fig. 4, lower panel). The weighted mean age of the main flat part of the spectrum (steps 3– 12) is 173.2 F 6.3 Ma. The 37ArCa/39ArK ratio spectrum is flat, with more Ca-rich compositions degassing during the first 6.5% and final 2% of gas release (Fig. 4, upper panel), which probably correspond to impurities. The total fusion age of 174.7 F 1.6 Ma and 36Ar/40Ar vs. 39Ar/40Ar inverse isochron age of

Table 2 ´ Rb – Sr analytical data of white mica; ALM 270, Mesozoic series, Nevado – Lubrın unit; ALM 272, 273, 274 Paleozoic rocks, Secano unit

Estimated errors are 0.5% for X-ray fluorescence spectrometric Rb/Sr and isotope dilution measurements of Rb and Sr, 0.01% for 87Sr/86Sr isotope ratio measurements of whole-rocks and 0.02% for 87Sr/86Sr analysis of minerals. The uncertainty is at the 2r level and based on the above mentioned estimated analytical errors. Decay constant of 87Rb = 1.42 Â 10À 11yearÀ 1. (1) X-ray fluorescence spectrometric data (whole-rock) and mass-spectrometric isotope dilution (minerals). (2) Directly measured on unspiked sample (whole-rock) and calculated from analysis of spiked sample (minerals).

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173.2 F 8.7 Ma (Table 1; Fig. 5) are concordant. However, the large MSWD of 15 renders the meaning of the isochron age and the 40Ar/36Ar intercept of 281 F 82 uncertain. 5.1.2. Phengite single grain JK 0 Laser step heating of a single phengite grain JK 0 yielded a plateau age of 86.9 F 0.8 Ma (Fig. 6. lower panel). The plateau age is concordant to both the 87.9 F 2.2 Ma total fusion age and the 86.2 F 2.4 Ma 36 Ar/40Ar vs. 39Ar/40Ar inverse isochron age of the plateau steps, with an 40Ar/36Ar intercept that is within error of the atmospheric value (Table 1, Fig. 7). The 37ArCa/39ArK ratio spectrum is flat over the main part (Fig. 6, upper panel); the high ratio during the first 3% and the slightly elevated ratio for the final 25% of gas release probably correspond to more Carich inclusions in the grain. 5.2. Rb – Sr ages Rb –Sr analyses of phengites from mica schists have yielded a wide spread of ages (Table 2). Despite unfavourable enrichment factors of radiogenic 87Sr, samples ALM 272 and 273 of the Secano unit preserve a pre-Miocene isotope signal, yielding whole-rock –mica ages of 66.1 F 3.2 and 40.6 F 2.6 Ma. ALM 274 (Secano unit) yielded an age of 14.1 F 2.2 Ma that is concordant with the whole-rock – phengite – albite age

Fig. 6. 40Ar/39 Ar laser step heating age spectrum (lower panel) and 37 ArCa/39ArK ratio spectrum (upper panel) of single phengite grain ´ JK 0 from the Mesozoic series of the Nevado – Lubrın unit.

Fig. 5. Ar/ Ar vs. ArK/ Ar correlation plot for biotite separate ALM 104. Points 1350 and fuse are excluded from the calculation.





Fig. 7. 36Ar/40Ar vs. 39ArK/40Ar correlation plot for single grain JK 0. The open ellipses of steps 8 – 11 are excluded from the calculation.


K. de Jong / Lithos 70 (2003) 91–110

Fig. 8. Rb – Sr albite phengite whole-rock isochron for ALM 270 ´ (Mesozoic series, Nevado – Lubrın unit). The errors are at the 2r level.

´ of 17.2 F 1.9 Ma of ALM 270 (Nevado – Lubrın unit, Fig. 8).

6. Interpretation The results obtained on samples with the same tectonic foliation show a wide range of 40Ar/39Ar and Rb –Sr ages, emphasising the fact that they cannot be interpreted in terms of a simple cooling history during exhumation. 6.1. Excess and inherited


The 173 F 6 Ma 40Ar/39Ar weighted mean age and virtually all apparent ages of biotite ALM 104 are much older than the 146 F 3 Ma Rb –Sr mineral isochron age of the host gabbro (Fig. 4), which indicates that 40ArXS has been incorporated into the mineral. The concordant 86.9 F 0.8 Ma plateau age and the 86.2 F 2.4 Ma isochron age of single phengite grain JK 0 are much older than the 15.0 F 0.6 Ma SHRIMP ´ ´ U –Pb zircon age obtained by Lopez Sanchez-Viz´ caıno et al. (2001) in Cerro del Almirez (Fig. 1). The discrepancy between these two estimates for the timing of high-pressure metamorphism in the Mulha´ cen Complex cannot be accounted for by a polycyclic Alpine orogeny (e.g. Puga et al., 2002), as the upper ´ and lower parts of the Nevado –Lubrın unit did not

experience a different tectono-metamorphic evolution, as would be expected following a re-subduction of the lower part, as proposed by the latter authors. Accordingly, the best interpretation is that the ca. 87 Ma age of the phengite is due to the incorporation of 40Ar into its lattice, which may have been inherited from the magmatic precursor of the amphibolite that hosted the white mica and which contained 40ArXS. The 37ArCa/39ArK ratio and atmospheric contamination of phengite grain JK 0 are fairly constant and not elevated during the main argon release (Fig. 6, upper panel; Table 1). It is, therefore, unlikely that 40 ArXS incorporation was the result of late-stage illitisation related to fluid ingress via late cracks, described by de Jong et al. (2001) for phengites in gneisses, which have an atmospheric contamination that is well above 30% and 37ArCa/39ArK ratios that tend to be much higher than those observed for JK 0. The absence of a dense network of cracks in the amphibolite emphasizes this. The fact that the single mica grain yielded a plateau age that is enhanced by inherited 40Ar implies that Ar was not released by volume diffusion during in vacuo step heating. It has been argued that chemical and structural changes, such as dehydroxylisation of white mica during step heating, permit the simultaneous release of 39ArK, 40Ar* and 40ArXS from the cores and rims of crystals, leading to homogenisation of 40 Ar reservoirs and age gradients (Inger et al., 1996; Sletten and Onstott, 1998; de Jong et al., 2001). Trioctahedral micas behave in a similar way (Harrison et al., 1985; Phillips and Onstott, 1988; Lo and Onstott, 1989), however, probably due to sample inhomogeneity, we did not obtain an age plateau for biotite ALM 104. In light of the above discussion, the meaning of the plateau ages of 48.4 F 2.2 and 24.6 F 3.6 Ma of barroisitic amphibole and magnesiohornblende, re´ spectively, obtained by Monie et al. (1991) in the Sierra de Baza (Fig. 1), which both yielded irregular 40 Ar/39Ar age spectra, cannot be taken at face value. The barroisitic amphibole grew in an undeformed metadolerite that contains magmatic plagioclase and clinopyroxene, making inherited 40Ar likely. The well-expressed saddle-shaped age spectrum of the magnesiohornblende clearly points to 40ArXS uptake, and this sample only yielded a plateau age due to the very large errors on the individual steps.

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6.2. Trapped argon component Although 40ArXS often results in 40Ar/36Ar intercepts in isotope correlation diagrams greater than 295.5 (Heizler and Harrison, 1988), examples of phengite (Inger et al., 1996; Sherlock and Arnaud, 1999; de Jong et al., 2001) and biotite (Foland, 1983; Ruffet et al., 1995) show that samples with 40ArXS plateau ages can give 40Ar/36Ar intercepts close to the atmospheric value. The initial 40Ar/36Ar ratio not necessarily reflects the argon composition immediately prior to crystallisation, but might equally well indicate the argon composition added to minerals during later processes (Roddick, 1978; de Jong et al., 2001). This may also be the case for ALM 104, as this sample has an elevated 36ArAIR contamination corresponding to high 37ArCa/39ArK ratios during the first 6.5% of 39Ar release. This is most likely related to impurities of a Ca-rich phase that degasses at low temperature, like carbonates (500 –700 jC: Spray and Roddick, 1981) and/or chlorite (first degassing peak < 600 jC: Lo and Onstott, 1989; Ruffet et al., 1991), which both may have been formed during light alteration. The K contrast between biotite and submicroscopically intergrown chlorite may lead to 39ArK recoil from the former into the latter, which results in hump-shaped age spectra with old apparent ages in the intermediate temperature region (Lo and Onstott, 1989; Ruffet et al., 1991). As we did not observe such spectra, 39ArK recoil was probably not important and does not lie behind the scatter of data point in the isotope correlation diagram and the high MSWD values for the regression. The isotope correlation diagram of biotite ALM 104 thus seems to essentially reflect the mixing of at least three argon reservoirs, viz: a radiogenic component with two trapped components. The first trapped component probably had a non-atmospheric composition and was incorporated during crystallisation, whereas the second and dominant component was atmospheric and was added late in the evolution of the system. Phengite JK 0 (Table 1, Fig. 6) yielded a statistically significant inverse isochron age with an 40Ar/36Ar intercept within error of the atmospheric value. In this case too, the trapped component may be due to later processes, rather than have bearing on the trapped component during recrystallisation of the grain. This is clearly illustrated by the relatively high 37ArCa/39ArK

ratios and the corresponding elevated atmospheric contamination. 6.3. Excess

Ar and restricted fluid mobility

Widely scattered and elevated K – Ar mineral ages from the gabbro from which biotite ALM 104 was separated were interpreted by 40ArXS incorporation (Hebeda et al., 1980). These authors accounted for the presence of much higher amounts of 40ArXS in the whole-rock relative to the constituent minerals by its incorporation in the grain boundary network, fluid inclusions and lattice defects, acquired during Alpine metamorphism due to degassing of the surrounding sediments. Such incipient low-grade metamorphism during the early stages of subduction affected the sedimentary rocks, in which argon had accumulated in minerals since their deposition and diagenesis, and was present as an inherited argon in detrital grains, but not the coarse-grained high temperature minerals of the gabbro. However, the occurrence of 40ArXS in all the degassing steps of biotite ALM 104 implies incorporation in the mineral lattice and not in low retentive sites like cracks, cleavages and defects. The 40 ArXS uptake may thus have occurred during recrystallisation of the biotite under a high argon activity during this low-grade event. 40ArXS was probably incorporated by a carrier fluid without important recrystallisation of the other magmatic minerals of the gabbro. This mechanism is in agreement with the Sr isotopic data. The initial 87Sr/86Sr ratio of 0.7028 (Hebeda et al., 1980) that is close to the primitive mantle value implies that Alpine recrystallisation did not affect the Rb –Sr system of the rock. Morten et al. (1987) noticed a statistically significant increase of the 87 Sr/86Sr ratio with metamorphic grade during progressive eclogitisation, which range from 0.703 (gabbros), via 0.705 (garnet-bearing metagabbro), to about 0.706 (eclogites), in the rock body that yielded the 146 Ma Rb – Sr age. The data presented by ´ Gomez-Pugnaire et al. (2000) similarly show higher 87 Sr/86Sr ratios for dolerites affected by metamorphic recrystallisation. Morten et al. (1987) explained the enrichment in radiogenic 87Sr by a limited ingression of metamorphic fluids derived from the recrystallising metasedimentary country rocks. Although the very formation of eclogites is enhanced by fluid infiltration ´ (Morten et al., 1987; Gomez-Pugnaire et al., 1989), in


K. de Jong / Lithos 70 (2003) 91–110

agreement with the evolution of the 87Sr/86Sr ratio, the observed zonation of the metamorphic minerals implies a state of disequilibrium and a deficit of cations. Such features suggest that fluid mobility was limited during eclogitisation, which consequently conserved the 40ArXS levels in rocks. The ca. 87 Ma 40Ar/39Ar age of phengite JK 0 is most likely the consequence of the incorporation of 40 Ar into the mineral and restricted fluid mobility may have been instrumental in this process. The amphibolite from which single phengite grain JK 0 was extracted occurs in the same tectono-stratigraphic level as the 146-Ma-old gabbro ALM 104, which was plagued by 40ArXS incorporation. Most eclogites and gabbros in this level are pervasively amphibolitised, pointing to the infiltration of water. Thorough amphibolitisation of eclogites resulted in changes in main and trace element chemistry (Morten et al., 1987). The preferred orientation of mica and bluegreen hornblende in amphibolite JK 0 formed during thorough recrystallisation that accompanied exhumation of high-pressure metamorphic rocks during D2. Yet, the presence of glaucophane relics in the cores of some hornblendes in this sample implies that disequilibrium conditions existed during the breakdown of the blue amphibole during this event. Although the hydration of eclogites, leading to their amphibolitisation, resulted in a significant reduction of 40ArXS in the whole-rock, it was not completely removed, as shown by the data of Hebeda et al. (1980). This observation implies that during D2 recrystallisation, a semi-closed system persisted, in which the argon activity remained elevated, at least locally. Amphibolitisation of gabbros and eclogites under such conditions has led to the local redistribution and incorporation of 40Ar in newly formed metamorphic minerals, such as phengite. 6.4. Inherited isotopic components White micas from the basal series of the Secano unit yielded Rb –Sr ages that range from 66.1 F 3.2 to 14.1 F 2.2 Ma (Table 2) and 40Ar/39Ar total gas ages of 25.9 F 0.1 and 19.1 F 0.1 Ma (see Section 3), which imply the progressive resetting of an older isotopic system. White mica from graphite-rich samples ALM 272 and 273 has disturbed 40Ar/39Ar age spectra with apparent ages that are virtually all older

than the 17.3 F 0.2 Ma plateau age of ALM 270 of the ´ Nevado –Lubrın unit (Fig. 9). Disturbed age spectra, whether dome-shaped or composed of progressively rising apparent ages, have been interpreted by degassing of mixed micas, one containing an inherited Ar component due to partial resetting during superimposed tectono-metamorphic recrystallisation and a second that was newly formed during this event, both of which do not release Ar over the same temperature interval (Wijbrans and McDougall, 1986; Hammerschidt and Frank, 1991; de Jong et al., 1992; West and Lux, 1993). Consequently, the age spectra of ALM 272 and 273 imply that a relict inherited Ar component exists in both samples. Their microstructure reveals incomplete recrystallisation of white mica and the pinning of its grain boundaries on graphite particles.

Fig. 9. 40Ar/39Ar induction furnace step heating age spectra (lower panel) and 37ArCa/39ArK ratio spectra (upper panel) of phengite ´ separates from the eastern Sierra de los Filabres. Data from de Jong ´ et al. (1992). ALM 270 (Mesozoic series, Nevado – Lubrın unit) shows a well-developed age plateau, whereas ALM 272 and 273 (Paleozoic series, Secano unit) have disturbed spectra.

K. de Jong / Lithos 70 (2003) 91–110


This inclusion-inhibited growth mechanism may similarly explain why phengites ALM 272 and 273 have partially retained an older Rb – Sr isotope signal, as indicated by their relatively old Rb –Sr ages of 66.1 and 40.6 Ma, respectively. In contrast, the 14.1 F 2.2 Ma Rb – Sr age of the most quartz-rich and least graphite-rich sample ALM 274, which is not affected by inclusion-inhibited growth of white mica, implies a complete resetting of its Rb – Sr system. The Rb – Sr age of this youngest sample of the Secano unit overlaps with the 17.2 F 1.9 Ma Rb –Sr age of ALM 270 of ´ the Nevado – Lubrı n unit. Widespread retrograde growth of albite and chlorite at the cost of phengite in ALM 270 implies complete tectono-metamorphic recrystallisation following D2. The progressively reset isotopic system in the Secano unit may be derived from a pre-Miocene early Alpine signal, or alternatively, its occurrence in probably Paleozoic rocks implies that it may partially retain a pre-Alpine history. The ca. 15 Ma U – Pb SHRIMP zircon age for the high-pressure metamor´ ´ ´ phism (Lopez Sanchez-Vizcaıno et al., 2001) renders the first option unlikely. In contrast, during the pre´ Alpine evolution of the Mulhacen Complex, the basal series were metamorphosed up to about 500 jC (Section 2; Fig. 10). Their crystalline nature and the inhibited recrystallisation of white mica in graphite-rich samples during the Alpine orogeny may lie behind the inherited pre-Alpine Rb – Sr and K –Ar systems in these rocks. Their partial survival in white mica during the Alpine orogeny, when temperatures of about 500 jC were reached, once again underscores that temperature alone is ineffective for isotope resetting, but that fast recrystallisation processes that affect the ionic bonds in minerals, like tectonometamorphic recrystallisation and fluid ingress, are (Chopin and Maluski, 1980; Verschure et al., 1980; Wijbrans and McDougall, 1986; Hames and Cheney, 1997; Villa, 1998; Itaya and Fujino, 1999; Ku et ¨hn al., 2000; de Jong et al., 2001; Dunlap and Kronenberg, 2001; Reddy et al., 2001). In contrast, the occurrence of ALM 270 in the Mesozoic series of ´ the Nevado – Lubrı n unit and its ca. 17.2 Ma 40 Ar/39Ar plateau and Rb – Sr ages precludes the presence of any inherited pre-Alpine isotopic component. Yet, a small 40ArXS component seems likely, taking the ca. 15 Ma U –Pb SHRIMP zircon age at face value.

6.5. Age and rates of exhumation and cooling Despite the occurrence of inherited isotope systems and 40ArXS incorporation in white mica and biotite, our dating sheds light on the timing of exhumation of ´ the Mulhacen Complex and its rates. Albite in ALM 270 was probably formed from the paragonite component in white mica during its recrystallisation at low pressure during D3. The 87Sr/86Sr ratio of this sample shows that the age information obtained essentially pertains to albite, as the 87Sr/86Sr ratios of phengite and the whole-rock are virtually identical (Table 2). The 17.2 F 1.9 Ma whole-rock– mica– albite age consequently has bearing on the decompression to about 0.4 – 0.5 GPa for D3 (see Section 2.2, Fig. 10). However, due to the large uncertainty, the age is within error of the 15.0 F 0.6 Ma age estimate of the high-pressure metamorphism based on the zircon ´ ´ ´ SHRIMP data of Lopez Sanchez-Vizcaıno et al. (2001). Subsequent to the D3 cooling phase temperatures increased to about 500 jC, whereas the pressure probably did not significantly decrease (Fig. 10). de Jong et al. (2001) argued that, in conjunction with this D4 reheating, white mica in the gneisses of the Macael –Chive unit acquired 40ArXS during submicroscopic illitisation, a fluid-assisted recrystallisation process that probably also affected the Rb – Sr system. Rb– Sr white mica ages reported by Andriessen et al. (1991) from the gneisses of the Macael – Chive unit in ´ the eastern Sierra de los Filabres span the 12.5 –15.6 Ma range, with errors of about 2 – 2.5%. It might be argued that the youngest Rb –Sr white mica age of 12.5 F 0.2 Ma is the result of a thorough recrystallisation during D4, which might imply a decompression of about 55 km in roughly 2.5 Ma (Fig. 10). The exhumation rate may consequently be as high as about ´pez 22.5 mm/year, about twice the estimate of Lo ´ ´ Sanchez-Vizcaıno et al. (2001), who based their value on an assumed geothermal gradient and not on available P –T estimates for the late stage evolution. Fission-track data of Johnson et al. (1997) point to an accelerated cooling following the first phase of fast exhumation and cooling. These authors inferred from an 11 Ma apatite fission-track model age that the ´ cooling of the uppermost Mulhacen Complex in the ´ eastern Sierra de los Filabres was essentially completed by that time. This is consistent with the first appearance of detritus derived from this part of the


K. de Jong / Lithos 70 (2003) 91–110

´ Fig. 10. Pressure – Temperature – time – deformation path and exhumation history of the Mulhacen Complex. P – T determinations by Bakker et al. (1989), de Jong (1991, 1993a) and Puga et al. (2002). (1) Lower P stability limit of glaucophane after Maruyama et al. (1986); (2) FeChl + Ms = FeCld + Ann; (3) Cld + AS = St + Chl; (4) FeCld + Ann = Alm + Ms; (5) Cld = Grt + Chl + St; according to Spear and Cheney (1989); Stability Al-silicate fields after Holdaway and Mukhopadhyay (1993). Mineral abbreviations according to Kretz (1983). Age ´ ´ ´ constraints: (A) SHRIMP U – Pb mean age of nine zircon grains (Lopez Sanchez-Vizcaıno et al., 2001); (B) youngest Rb – Sr white mica age of Andriessen et al. (1991); (C) apatite fission-track model age (Johnson et al., 1997).

complex (in part as boulders of the marbles and gneisses of the Macael –Chive unit) in latest Serravallian to Early Tortonian deposits around the eastern ´ Sierra de los Filabres (de Jong et al., 2001, and references in therein). Under the assumption of a 12.5 Ma age for D4 during which temperatures were in the order of about 500 jC, the final cooling has taken about 1.5 Ma with a rate of about 330 jC/Ma and much less fast exhumation rate of 9– 12 mm/year compared to the early exhumation phase. The Late Miocene cooling has been accounted for by extension (Johnson et al., 1997). Since the work of Platt and Vissers (1989), the contact between the ´ ´ Mulhacen and Alpujarride complexes has been interpreted as a major low-angle extensional fault. D5 mylonites and D6 brittle– ductile structures are most ´ penetratively developed in the uppermost Mulhacen Complex along the contact with the overlying Alpu´ jarride Complex and show the decreasing temperature (de Jong, 1991, 1993a) during exhumation. But also important low-angle brittle– ductile detachments ´ were formed within the Mulhacen Complex during this event, like e.g. at the base of the Secano unit and at the base of the greenstones that contain the eclogites.

7. Conclusions Radiometric dating of phengite from rocks with a tectonic fabric related to the exhumation of highpressure metamorphic rocks implies that 40ArXS incorporation and isotopic inheritance have occurred under conditions of restricted fluid mobility and tectono-metamorphic recrystallisation. A well-crystallised single phengite grain from an ´ amphibolite (Nevado – Lubrın unit) has yielded a 40 Ar/39Ar laser step heating plateau age of 86.9 F 0.8 (2r; 70% 39Ar released), which is concordant to its inverse isochron age of 86.2 F 2.4 Ma (40Ar/36Ar: 299.0 F 4.8). A biotite separate from a gabbro relic in an eclogite yielded an induction furnace step heating age spectrum with progressively increasing apparent ages and a weighted mean age of 173.2 F 6.3 Ma (2r; 95% 39Ar released). These ages are older than the eclogite-facies metamorphism (15 Ma) and intrusion of the gabbros (146 Ma) and, hence, are the result of 40 ArXS incorporation. 40ArXS uptake by the gabbro was probably caused by infiltration of fluids derived from the country rocks during their incipient metamorphism at the onset of subduction. 40ArXS incorporation in the phengite in the amphibolite was related

K. de Jong / Lithos 70 (2003) 91–110


to metamorphic recrystallisation of the magmatic rocks in an environment with a restricted fluid mobility inherited from the magmatic stage. Rb – Sr whole-rock – phengite ages of graphitebearing mica schists from Paleozoic rocks (Secano unit) show a dramatic age variation (66.1 F 3.2, 40.6 F 2.6 and 14.1 F 2.2 Ma) that has arisen from the progressive resetting of an older isotopic system. This system was probably a remnant of the Variscan low-grade metamorphism of the basal series of the ´ Mulhacen Complex. The microstructure of the samples with pre-Miocene Rb – Sr ages implies that phengite has only partially recrystallised as grain growth was inhibited by the presence of graphite particles. This interpretation corroborates previously obtained disturbed and slightly dome-shaped 40Ar/39Ar age spectra that reveal the presence of an older isotopic component. In contrast, the most quartz-rich and least graphite-rich sample is not affected by inclusioninhibited growth of white mica, and has a completely reset Rb – Sr system, as implied by its 14.1 F 2.2 Ma Rb – Sr age. The latter date overlaps with the 17.2 F 1.9 Ma Rb – Sr whole-rock – phengite – albite age obtained from a schist from the Mesozoic series ´ of the Nevado – Lubrın unit. Comparison of our data and literature data reveals ´ that exhumation of the eclogite-facies Mulhacen Complex occurred at rates in the order of 22.5 mm/year during the early phase and of 9 –12 mm/year during the late phase. During the latter event, the cooling rate was of about 330 jC/Ma.

Geochemistry, Faculty of Earth and Life Sciences, Vrije Universiteit, Amsterdam, The Netherlands) for the use of analytical facilities and the use of sample ALM 104 from the mineral separate collection of the department. Part of the work was carried out while holding a NATO post-doctoral research fellowship and The Netherlands Organisation for Scientific Research (NWO) and the ‘‘Vakgroepfonds Strukturele Geologie’’ of the University of Amsterdam met travel costs incurred during the project. Some of the points addressed in this study came up during a discussion with Igor Villa. Constructive reviews by Sarah Sherlock and Richard Spikings contributed to the clarity of the presentation and the styling of the text. ´n Daniella Rubatto and Encarnacio Puga are thanked for providing pre-prints.

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Acknowledgements I would like to dedicate this article to Prof. W.P. de Roever, who passed away on 24 September 2000, and was one of the pioneers in high-pressure petrology just after World War II. He worked as an undergraduate ´ student in the area around Lubrın and interpreted the occurrence of zoned metamorphic minerals by disequilibrium during a succession of different metamorphic facies in time (plurifacial metamorphism). Only much later would such a notion become general with the reconstruction of P –T – t paths. ´ ´ I would like to thank Drs. Gilbert Feraud (Geo´ science Azur, Universite de Nice-Sophia Antipolis, France) and Jan Wijbrans (Department of Isotope


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