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Contrib Mineral Petrol (2012) 163:67–85

DOI 10.1007/s00410-011-0659-7

ORIGINAL PAPER

Decoding near-concordant U–Pb zircon ages spanning several


hundred million years: recrystallisation, metamictisation
or diffusion?
J. A. Halpin • N. R. Daczko • L. A. Milan •

G. L. Clarke

Received: 27 November 2010 / Accepted: 25 May 2011 / Published online: 14 June 2011
Ó Springer-Verlag 2011

Abstract In situ isotopic (U–Pb, Lu–Hf) and trace ele- episodically at c. 1145–1140 Ma, c. 1080–1050 Ma and
ment analyses of zircon populations in six samples of the c. 985–960 Ma. Core-outer core-rim and core-rim textures
intrusive Mawson Charnockite, east Antarctica, emphasise were identified but are not correlated with U–Pb ages. We
complex zircon behaviour during very high-grade meta- establish that recrystallisation (mainly of zircon rims) must
morphism. The combination of geochemical data sets is have occurred shortly following igneous crystallisation and
used to distinguish xenocrysts and identify a population of that metamictisation/cracking is a Paleozoic to Recent
primary igneous zircon in situations where U–Pb data event. Therefore, intra-zircon diffusion in a high-T, high-
spread close to concordia over a few hundred Myr. The strain environment during Meso-Neoproterozoic orogene-
population is filtered to exclude grains with: (1) U–Pb ages sis is inferred to have caused the extensive U–Pb isotopic
[2% discordant, (2) anomalous trace element-content (Th, disturbance. Charnockitic magmatism prior to c. 1,000 Ma
U, Y, REE) and (3) outlying Hf-isotopic values. Rare has not previously been recorded in the Mawson region and
metamorphic-type grains were also excluded. Upon filter- indicates that orogenesis may have commenced c. 150 Myr
ing the population, minimum emplacement ages for each earlier than previously thought. Correlations with similar
sample were determined using the oldest grain(s). This aged rocks in adjacent regions have implications for
approach improves upon age determinations in complex supercontinent reconstructions.
data sets that use weighted mean or isochron methods. Our
results suggest that the Mawson Charnockite was emplaced Keywords Rayner Orogen  Mawson Charnockite 
East Antarctica  Hf-isotopes  Trace elements  Pb-loss 
Laser Ablation-Inductively Coupled Plasma Mass
Communicated by T. L. Grove. Spectrometer
Electronic supplementary material The online version of this
article (doi:10.1007/s00410-011-0659-7) contains supplementary
material, which is available to authorized users. Introduction

J. A. Halpin (&)
Regional high-grade metamorphism may promote zircon
ARC Centre of Excellence in Ore Deposits,
University of Tasmania, Private Bag 126, Hobart, growth, the modification/recrystallisation of older zircon or
TAS 7001, Australia a combination of the two processes (e.g. Hoskin and
e-mail: jahalpin@utas.edu.au Schaltegger 2003). Geochronological studies of zircon in
orogenic belts now make use of an array of techniques to
J. A. Halpin  N. R. Daczko  L. A. Milan
Department of Earth and Planetary Sciences, decode zircon genesis including microstructural charac-
GEMOC ARC National Key Centre, Macquarie University, terisation via BSE and CL imaging (Corfu et al. 2003;
Sydney, NSW 2109, Australia Hanchar and Rudnick 1995; Rubatto and Gebauer 2000)
and trace element patterns in zircon and co-existing silicate
G. L. Clarke
School of Geosciences, The University of Sydney, minerals (Kelly and Harley 2005; Rubatto 2002; White-
Sydney, NSW 2006, Australia house and Platt 2003). In addition, combined in situ U–Pb

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68 Contrib Mineral Petrol (2012) 163:67–85

and Lu–Hf analysis of zircon domains have the potential to methodology allows for the zircon growth and modification
decipher the crustal growth history of complex terranes history in these rocks to be unraveled and ‘conservative’
(Scherer et al. 2007). Multiple studies now show that the constraints to be placed on protolith emplacement ages.
initial 176Hf/177Hf value, once incorporated into the zircon This methodology is broadly applicable to refining geo-
lattice during growth, is not modified by processes that may chronology and terrane evolution where protracted and
disturb or reset the U–Pb isotopic system (e.g. Kinny et al. repeated tectonothermal events have occurred. Our results
1991; Kinny and Maas 2003; Patchett 1983) and that this point to a reevaluation of the Grenvillian terrane definition
holds true even in high-grade metamorphic terranes (Ger- in east Antarctica.
des and Zeh 2009; Halpin et al. 2005).
End-members of zircon U–Pb age datasets range from
the common situation of a limited concordant Gaussian Regional geology of the Mawson Coast
distribution interpreted as a single population, through an
array spread along discordia reflecting an isotopically dis- Geological setting, petrography and metamorphism
turbed population, to a series of random ages distributed
along concordia. The first case is usually interpreted to Geological mapping by Crohn (1959), McLeod (1964) and
reflect a geologically significant event, such as crystalli- McCarthy and Trail (1964), Trail et al. (1967) and Trail
sation, metamorphism or a maximum deposition age. A (1970) divided the rocks of the Mawson Coast, MacRob-
systematically discordant population is commonly inter- ertson Land (between 60°E and 66°530 E; Fig. 1) into a large
preted in terms of variable Pb-loss during a second event. orthopyroxene-bearing orthogneiss body, the Mawson
However, concordant igneous zircon U–Pb age data spread Charnockite ([3,000 km2 and possibly even [5,000 km2)
across several hundred million years are not easily inter- and older paragneiss and felsic orthogneiss units. The rocks
preted (Mezger and Krogstad 1997). Some high-grade are part of the Proterozoic Rayner Complex (Kamenev
terranes, such as the Rayner Complex in east Antarctica, 1972), which extends from MacRobertson through Kemp
present zircon populations involving the third case (Halpin and Enderby lands (Fig. 1). This belt records a protracted
et al. 2005; Kelly et al. 2002; Kelly et al. 2004). In this c. 1,000–900 Ma tectonothermal event (Black et al. 1987;
paper, we analyse a series of random near-concordant ages Dunkley et al. 2002; Grew et al. 1988; Kelly et al. 2002;
that reflect the effects of two or more geological events, by Sheraton et al. 1987; Young and Black 1991) correlated with
exploring the crystallisation age and isotopic disturbance of c. 1,000–950 Ma events in the central and northern Eastern
the Mawson Charnockite, a [3,000 km2 composite pluton. Ghats Belt (EGB) in India (Aftalion et al. 1988; Grew and
Our approach integrates: (1) Backscattered Electron (BSE) Manton 1986; Mezger and Cosca 1999; Paul et al. 1990;
and cathodoluminescence (CL) imaging; (2) trace element Shaw et al. 1997). The orogeny is commonly interpreted as
analysis and (3) Hf isotopic analysis, via Laser Ablation- reflecting convergence between part of the Antarctic craton
Inductively Coupled Plasma Mass Spectrometry (LA-IC- with proto-India (Harley 2003). The significance of the
PMS) to resolve complexity in the U–Pb zircon data. event(s) in assembly of the Rodinian supercontinent is con-
Imaging methods reveal a wide variety of growth, re- troversial (Fitzsimons 2000a, b; Yoshida 1995) largely
crystallisation and/or structural modification textures in because of complexity in the geochronological datasets.
zircon (Corfu et al. 2003). However, similar textures may Intensely foliated paragneiss and orthogneiss bodies
form via different processes; e.g. distinction between tex- occur as xenoliths within the Mawson Charnockite; a
tures formed during the final stages of magmatic crystalli- composite S1–S2 gneissosity is cut by charnockite contacts
sation (dissolution/precipitation) compared to those formed (Clarke 1988; Clarke et al. 1989; Dunkley et al. 2002;
during later metamorphism or fluid ingress is not always White and Clarke 1993). Post-emplacement deformation
straightforward. The decoupling of U–Pb and Lu–Hf sys- (D3–D4) resulted in open to tight, upright folding of S1 and
tematics in zircon is particularly useful in the interpretation S2 and recrystallised mineral assemblages in the char-
of age data smeared along concordia (Bomparola et al. nockite. Metapelitic gneiss from the Forbes Glacier and
2007; Halpin et al. 2005). In contrast, though trace element Cape Bruce (Fig. 1) records evidence for an anticlockwise
content may also define chemically distinct zircon popula- P–T-t path involving peak T & 850–920°C and P & 5.4–
tions (Rubatto 2002), the expulsion of non-essential cations 6.2 kbar (Halpin et al. 2007). Emplacement of the char-
(e.g. Th, Y, LREE, MREE) can accompany Pb-loss during nockite is interpreted to have accompanied or immediately
recrystallisation (Hoskin and Black 2000; Hoskin and followed peak metamorphic conditions and accompanied
Schaltegger 2003; Schaltegger et al. 1999). crustal thickening to P & 6.0–6.8 kbar followed by near-
For this study, we analysed five charnockitic gneiss isobaric cooling (Halpin et al. 2007).
samples and one gabbroic gneiss sample of the Mawson The Mawson Charnockite is a composite body; composi-
Charnockite composite pluton (Fig. 1). Our integrated tions are dominantly intermediate (SiO2 from *54–68 wt%;

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Contrib Mineral Petrol (2012) 163:67–85 69

Mawson Charnockite
(c) 61°0'E Mawson Charnockite 62°0'E 63°0'E
(LM01, this study) 64°0'E
(RW28, this study)
Cape Bruce Mawson area/Framnes Mts 2.12-1.94 Ga (THf(c)DM)
2.19-2.01 Ga (THf(c)DM) c.2.1 Ga; Mawson Charnockite (THf(c)DM)5
1.90-1.71 Ga (THfDM) 1.91-1.71 Ga (THfDM)
2.17-2.04 Ga; Mawson Charnockite (TNdDM)1, 6 c.1 145 Ma (U-Pb)
Chapman Ridge c.1080 Ma (U-Pb) 1.87-1.79 Ga; Mawson Charnockite (THfDM)5

zone
RW28 Ufs Island c.2.0-1.7 Ga felsic gneiss xenolith (U-Pb inherited ages)2
Macey Island
1254±13, 1153±47 Ma; banded gneiss (Rb-Sr whole rock)2

one
z644 982±33 Ma; Mawson Charnockite (U-Pb)5 LM01

tern
tral z
Falla Bluff c.970-910 Ma; metapelite (U-Th-Pb mnz)4

Wes
z542 921±19 Ma; felsic gneiss xenolith (U-Pb)2

Cen
67°30'S
67°30'S
Holme Macklin Island
Bay LM12
Mawson Charnockite
Austskjera
Cape Bruce/Ufs Is/Falla Bluff Mawson (LM12, this study) LM11
1.98-1.80 Ga; Mawson Charnockite (TNdDM)1 2.36-2.08 Ga (THf(c)DM)
Mawson Charnockite
LM53 (LM11, this study)
992±10 Ma; bi-opx dyke (U-Pb)3 Mawson Charnockite 1.74-1.63 Ga (THfDM)
985±29, 954±12 Ma; Mawson Charnockite (U-Pb)2 (LM53, this study) 90030 c.1050 Ma (U-Pb) 2.16-1.94 Ga (THf(c)DM)
c. 930-915 Ma; metapelite (U-Th-Pb mnz)4 2.52-1.90 Ga (THf(c)DM) 1.88-1.76 Ga (THfDM)
c. 910 Ma; paragneiss, charnockitic gneiss c.1 140 Ma (U-Pb)

one
1.95-1.76 Ga (THfDM)

zone
granitic gneiss, pegmatite (U-Pb)3 c.985 Ma (U-Pb)

tral z
Mawson eastern &

tern
NS
(b) nPCM western zone

Cen
1.98 - 1.89 Ga (TNdDM)1

Eas
NTAI
Study area

Mawson Charnockite 45°W 0° 45°E

MOU
(LF60, this study)
Kemp Hf(c)
c.2.06-2.02 Ga (T DM) Study
Enderby Land c.1.76-1.74 Ga (THfDM)
Land MacRobertson area
957±6 Ma (U-Pb)

NES
Land
ben

Rayner Complex Mt Horden 90°W 90°E

FRAM
Gra

ca.1000 - 900 Ma LF60


Archaen Napier Complex
bert
Lam

reworked Napier Complex 0 20 40


ca.940 - 900 Ma
km (a)
135°W 180° 135°E

Fig. 1 a Location of the study area in east Antarctica. b Distribution Pb mnz, monazite U–Th–Pb chemical age; Rb–Sr, whole-rock Rb–Sr
of the Napier and Rayner complexes in Enderby, Kemp and HfðcÞ
isochron age; THfDM , zircon Hf model age; TDM zircon Hf model
MacRobertson lands. c Regional diagram summarising sample crustal average age (using a crustal average value; see Halpin et al.
locations and relevant previously published geochronological data 2005 and this study); TNd DM , whole-rock Nd model age. Geochrono-
for MacRobertson Land within the Rayner Complex. Samples z644 logical references: 1Young et al. (1997); 2Young and Black (1991);
and z542 are from Young and Black (1991) and Young et al. (1997), 3
Dunkley et al. (2002); 4Halpin et al. (2007); 5Halpin et al. (2005);
sample 90030 is from Halpin et al. (2005) and the remaining samples 6
Black et al. (1987) and this study
are from this study. Dating methods: U–Pb, zircon U–Pb age; U–Th–

Sheraton and Black 1983; Sheraton and Black 1988; Young felsic gneiss xenolith at Mawson Station have a complex
and Ellis 1991; Young et al. 1997) and range from quartz age spectrum: cores give c. 1,040–2,460 Ma concordant
monzodiorite through granodiorite to granite, with minor ages, with a chord reflecting Pb-loss at c. 1,000–900 Ma
gabbro (Young et al. 1997). Exposures are mostly foliated (Young and Black 1991). Data cluster between 1,700 and
dark brown to orange-brown (when highly weathered), 2,000 Ma, but a few concordant analyses at 1,300–
medium- to coarse-grained gneiss with or without K-feldspar 1,400 Ma mean that a protolith age is poorly defined.
megacrysts. They typically comprise K-feldspar, orthopy- Zircon rims and young grains in the xenolith yield a U–Pb
roxene, plagioclase, quartz and biotite, and accessory age of 921 ± 19 Ma interpreted to date effects of recrys-
zircon, apatite, ilmenite and magnetite, with or without tallisation during D3 (Young and Black 1991). Chemical
garnet or clinopyroxene. High crystallisation temperatures U–Th–Pb dating of monazite from metapelitic gneiss
interpreted for orthopyroxene-bearing granitoids (Frost and (Halpin et al. 2007) and ion-microprobe U–Pb zircon dat-
Frost 2008) are supported by feldspar geothermometry ing from both pre-D1 and pre/syn-D4 intrusives (Dunkley
(950–1,000°C; Young and Ellis 1991). Retrograde biotite et al. 2002) from Forbes Glacier and Cape Bruce (Fig. 1)
and hornblende are common. suggest that the D1-D4 events occurred between c. 990 and
910 Ma and cannot be individually resolved. It is likely
Previous geochronology and isotopic studies that progressive deformation was accompanied by a con-
tinuous protracted high-grade metamorphic evolution over
Paragneiss c. 80 Myrs (Halpin et al. 2007).

The age of hosts to the Mawson Charnockite is poorly Mawson Charnockite


constrained (Fig. 1). Rb–Sr whole-rock isochrons that yield
ages between c. 1,150–1,250 Ma (Tingey 1982; Young and Early studies of the age of charnockite at Mawson Station
Black 1991) probably represent at least partial metamor- were via multi-grain U–Pb zircon and whole-rock Rb–Sr
phic overprints of a protolith age. Zircon grains from a isochrons (P. A. Arriens unpublished data, see Young and

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70 Contrib Mineral Petrol (2012) 163:67–85

Black 1991; Black et al. 1987) and yielded ages between University of New South Wales, Sydney (Supplementary
c. 890 and 960 Ma. An ion-microprobe study of two Material 1). Zircon grains were separated from 1–2 kg of
charnockite samples from the Mawson Coast by Young and each sample using conventional heavy liquids and mag-
Black (1991) yielded statistically indistinguishable ages of netic separation techniques at GeoTrack, Melbourne. Zir-
985 ± 29 Ma and 954 ± 12 Ma (Fig. 1). A recent study of con grains representing the spectrum of morphological
charnockite from Mawson Station via LA-ICPMS sug- types were hand-picked from a heavy mineral separate,
gested a minimum emplacement age of c. 980 Ma (Fig. 1), mounted in epoxy resin discs and polished so as just to
but the smear of much of the data along concordia was expose the central portions of the grains. Individual zircons
taken as evidence for complex U–Pb isotopic disturbance, were analysed for a suite of elements (Zr, Si, Hf and Y)
or a mix of inherited zircon and U–Pb isotopic resetting using a CAMEBAX SX50 electron microprobe (EMP) at
and zircon growth/recrystallisation (Halpin et al. 2005). the ARC National Key Centre for the Geochemical Evo-
Hf-isotopic data for zircon grains from charnockite at lution and Metallogeny of Continents (GEMOC), Mac-
Mawson Station yield Hf-depleted mantle model ages quarie University, Sydney. Operating conditions for the
(THf
DM ) between 1.79 and 1.87 Ga and a ‘crustal’ model age
EMP were 15 kV accelerating voltage and a beam current
of 2.1 Ga (where Lu/Hf = 0.01; Fig. 1) and have been of 20 nA.
interpreted as evidence for a lower crustal source, possibly BSE and CL images reveal internal structure and
without the addition of more primitive mantle components zonation and were captured to provide a guide for targeted
(Halpin et al. 2005). A similar Nd-depleted mantle model analyses such that analyses of ‘mixed’ zircon domain types
age (TNd were avoided. Zircon grains were imaged by BSE on the
DM ) of 2.18 Ga was derived by Black et al. (1987)
for charnockite from this location. EMP at GEMOC while CL imaging was performed on a
A detailed study of Sr–Nd isotopic composition of FEI Quanta 600 scanning electron microscope (SEM) at
charnockite and host rocks across the Mawson region was the Central Science Laboratory, University of Tasmania,
undertaken by Young et al. (1997). A large range of initial Hobart. Energy Dispersive Spectrometer software was used
87
Sr/86Sr ratios (0.7076–0.7334), initial eNd values (-4.0 to to identify inclusions in representative zircons using this
-11.1) and Nd-depleted mantle model ages (TNd same SEM.
DM ;
1.6–2.2 Ga) were derived for charnockite, comparable to
that from host gneisses (Young et al. 1997). Regional U–Pb and trace element analysis
variations were used to define three zones (the eastern,
central and western zones; Fig. 1). Central zone char- U–Pb and trace element analysis of zircon was conducted
nockite has higher 87Sr/86Sr values (0.7205–0.7334), lower using an Agilent 7,500 s quadrupole ICPMS instrument,
eNd values (-8.8 to -11.1) and older Nd-depleted mantle attached to a New Wave UP-213 Nd:YAG laser ablation
system at GEMOC. U–Pb isotopes (206Pb, 207Pb, 204Pb,
model ages (TNd DM ; 2.03–2.16 Ga) than that from the wes- 232
Th, 238U and 235U; Supplementary Material 3–8) and
tern and eastern zones (0.7076–0.7263; -4.0 to -8.4;
trace elements (Supplementary Material 9–14) were ana-
1.68–1.96 Ga). The geochemical and isotopic constraints
lysed simultaneously. For a detailed discussion of the
derived by these workers, together with similar data from
analytical procedures, operating conditions, acquisition
the northern Prince Charles Mountains to the south (i.e.
parameters and uncertainties involved in this technique, see
inland) of the Mawson Coast (Zhao et al. 1997), were
Jackson et al. (2004). Typical LA-ICPMS operating con-
interpreted as evidence for charnockite magma generation
ditions and data acquisition parameters in this study were:
from the high temperature anatexis of dry, Proterozoic
c. 60 s background signal prior to ablation; c. 120 s signal
granulitic crust. Regional variation in isotopic composition
analysis; 40 lm beam diameter; 5 Hz repetition rate;
of both charnockite and basement gneisses was interpreted
85–90% laser power output; estimated laser pit depth
to reflect distinct crustal domains in the MacRobertson
*40 lm. A typical run consisted of 10 analyses of our
Land region.
unknowns, 2–3 analyses of the reference zircon standard
91500 (Wiedenbeck et al. 1995), two analyses of a sec-
Analytical procedures ondary standard Mud Tank (Black and Gulson 1978) and
bracketed by at least five analyses of the external calibra-
Sample selection, preparation and imaging tion zircon standard GJ-1 (Elhlou et al. 2006; Jackson et al.
2004). Hf from EMP analyses was used as an internal
Five charnockitic rocks and a gabbroic rock were collected standard for trace element analysis. Analyses of the stan-
for analysis from across the Mawson region as represen- dard reference zircon 91500 (treated as an ‘unknown’)
tative of the three zones (Fig. 1) as defined by Young et al. provide an independent control to assess accuracy and
(1997). Whole-rock XRF analysis was performed at the precision; our 207Pb/206Pb age for 91500 over the course of

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Contrib Mineral Petrol (2012) 163:67–85 71

this study is 1,064 ± 6 Ma which is indistinguishable to Griffin et al. (2002) considered that high precision could
the TIMS age of 1,065.4 ± 0.3 Ma (Wiedenbeck et al. only be achieved where 176Yb/177Hf in zircon is less than
1995). Trace element analysis and average counts are 0.26, which is the case here. The Mud Tank zircon was
within error of published values (Wiedenbeck et al. 2004). used as a reference standard for Hf analysis; our mean
176
Net background-corrected count rates for each isotope Hf/177Hf value for this zircon is 0.282537 ± 0.000034
were used for age calculations. These data were processed (2SD) within error of the published value of
using the in-house GLITTER data reduction program (van 0.282522 ± 0.000042 (Griffin et al. 2007). Uncertainties
Achterbergh et al. 2001) that calculates isotopic ratios quoted are the internal measured uncertainty and do not
(207Pb/206Pb, 208Pb/232Th, 208Pb/238U and 207Pb/235U where include any propagation of error from this reference stan-
235
U = 238U/137.88) for the selected portion of each dard. During the period of this study, analyses of the zircon
ablation. Trace element data were similarly processed standard 61.308 produced a long-term average 176Hf/177Hf
using this software. Optimal output signals (a proxy for value of 0.283004 ± 0.000057 (Pearson et al. 2008), which
ablation-depth profiles) for each analysis were selected and is within error of published solution analyses (Wiedenbeck
automatically matched to signals from the primary standard et al. 1995) and demonstrates the veracity of the correction.
during the same time interval, allowing for correction for The initial 176Hf/177Hf (Hfi) value in zircon is calculated
effects of laser-induced U–Pb fractionation and mass bias. using the measured 176Lu, 176Hf/177Hf and 207Pb/206Pb age.
User interrogation of these time-resolved signals allowed The calculation of eHf values used the 176Lu decay constant
for identification of isotopic heterogeneity within the of Blichert-Toft et al. (1997) of 1.93 9 10-11. Model age
ablation volume. These intervals were also matched to the calculations (TDM) are based on a depleted-mantle source
suite of trace elements. Due to the low 204Pb count rates with Hfi = (176Hf/177Hf) initial = 0.279718 and
176
and isobaric interference from Hg (a contaminant from the Hf/ Hf = 0.0384. This provides a value of 176Hf/177Hf
177

Ar gas supply), common Pb contents were estimated using (0.28325) similar to that of average mid-ocean ridge basalt
the program ComPbCorr (Anderson 2002). This method is over 4.56 Ga. The calculated TDM ages use the measured
176
commonly used in LA-ICPMS studies and assumes that the Lu/177Hf of the zircon and give a minimum age for the
discordance of Pb/U and Pb/Th isotopic ratios observed in source material of the magma from which the zircon crys-
a zircon is a sum of the effects of common lead contami- HfðcÞ
tallised. A ‘crustal’ model age (TDM ) was also calculated
nation and Pb-loss. The use of this method in this study is for each zircon grain; this calculation assumes that the
compromised by poor constraints on the timing of Pb-loss parental magma was derived from the average continental
in each sample. However, in most cases, common Pb crust (176Lu/177Hf = 0.015), which in turn was originally
contents calculated via this method were below the level of derived from the depleted mantle. A second ‘crustal’ model
detection (\0.2%), and no correction was applied. Con- age was calculated using 176Lu/177Hf = 0.01 for the 5
cordia diagrams and age calculations were made using charnockitic samples as they are more felsic than average
Isoplot v.3 (Ludwig 2003). Uncertainties for individual continental crust (Halpin et al. 2005).
analyses as quoted in tables and as error ellipses on U–Pb
plots have been calculated to the one-sigma level.
Weighted mean age calculations are reported at 95% Sample characteristics
confidence limits.
Compositionally, the opx-bearing felsic granitoid gneisses
Hf-isotope analysis studied here range from granite to granodiorite within the
range of compositional variations observed by Young et al.
Hf-isotope analyses were performed in situ on the same (1997). The mafic sample LM12 (Macklin Island) is an
grains analysed for U–Pb using a New Wave UP-213 opx-bearing gabbroic gneiss similar in composition to a
Nd:YAG laser ablation microprobe attached to a Nu sample collected by Young et al. (1997) from the same
Plasma multi-collector (MC)-ICPMS system. Griffin et al. location. Young and Ellis (1991) and Young et al. (1997)
(2000, 2004) describe the methodology in detail. Operating divided samples of the Mawson Charnockite into two
conditions included a beam diameter of 50–55 lm, a 5- to major groups: high-Ti (Stibbs Bay Group) and low-Ti
10-Hz repetition rate and 75% power output; estimated (Holme Bay Group), based on geochemical features,
laser pit depth *40 lm. Ablation times include 30 s of especially TiO2 and P2O5 contents. Based on TiO2, P2O5,
background and a total signal time of approximately 200 s. Cr and Mg-number (Supplementary Material 1), LM12 is
The procedure for measuring 176Hf/177Hf includes cor- part of the low-Ti group, while LF60 belongs with the
recting for 176Yb, and where Yb is significant the degree of high-Ti group. The remaining samples display geochemical
uncertainty in the correction for isobaric overlap increases. characteristics transitional between these two groups.

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72 Contrib Mineral Petrol (2012) 163:67–85

However, our interpretations that follow do not rely upon Zircon imaging, U–Pb and Lu–Hf isotope and REE
this geochemical discrimination. results
The six samples analysed in this study are divided into
three types on the basis of paragenesis and microstructure Charnockitic and gabbroic gneiss samples have abundant
(Fig. 2, Supplementary Material 2). Samples LM53 and zircon of varied size and morphology (Table 1; Figs. 3, 4).
LF60 (Mawson Station and Mt Horden, respectively) are Individual grains range in length from c. 100 to 1,000 lm;
the least deformed and recrystallised of the felsic samples. the finest grain size is observed in sample LM01, which has
Though their mineralogy is similar to the other felsic the lowest whole-rock Zr-content (Supplementary Material
samples, they are distinguished on the basis of their 1). The majority of grains are interpreted as igneous on the
microstructure and form type 1. The other three felsic basis of elongate doubly terminating grain shapes and
samples (LM01, LM11 and RW28; Macey Island, Aus- commonly having oscillatory zoning (Figs. 3, 4). Rock
tskjera and Chapman Ridge, respectively) share similar forming minerals in the charnockitic gneiss commonly
mineral assemblages and microstructure and form type 2. occur as inclusions in zircon in samples LM53, LM11 and
The mafic sample (LM12; Macklin Island) contains distinct RW28, mostly in grain cores (Fig. 3). Zircon grains in
mineralogy and microstructure compared with the other these three samples have core-outer core-rim structures
five samples and comprises type 3. evident in BSE and CL imaging. Zircon grains in samples

(a) (b) qtz


plag
kfs
opx

qtz

kfs
plag
LM53 LF60
(c) opx (d)
plag
grt

grt qtz qtz


opx
plag
bt LM01 kfs LM11
(e) (f)
kfs
bt
qtz cpx
plag
plag
bt opx
opx

RW28 LM12

Fig. 2 a Coarse K-feldspar with rounded inclusions surrounded by domains and irregular garnet (LM01 and LM11). e Foliation defined
polygonal recrystallised feldspar and quartz. Domains of quartz grains by biotite and elongate quartzofeldspathic domains (RW28). f Equi-
are elongate in the foliation. Orthopyroxene is irregular and tends to granular gabbroic gneiss that contains plagioclase-orthopyroxene-
form clusters of grains (LM53). b Coarse plagioclase and K-feldspar clinopyroxene-biotite (LM12). Field of view is 2.5 mm for all images
porphyroclasts (LF60). c, d Coarse elongate recrystallised quartz

123
Table 1 Summary of zircon characteristics
Sample LM53 LF60 LM01 LM11 RW28 LM12

Petrographic 1 1 2 2 2 3
type
Grain size (lm) 150–640 150–680 120–280 100–700 340–870 170–1,000
Grain shape Sub-angular elongate to Sub-angular elongate to Highly elongate with Elongate with angular- Mainly elongate with sub- Elongate with angular
ovoid morphologies ovoid sub-rounded to rounded broken or sub-rounded to angular to sub-rounded to sub-rounded
morphologies ± angular terminations to stubby rounded terminations, terminations terminations, and
fragments ovoid grains ± angular with some more minor ovoid or
fragments irregularly rounded grains irregular
morphologies
Inclusion mnz, bi, q, ksp, ru, liq bi, q, ksp, ru Rare ap, bi, q, pl, ksp, opx, liq ap, bi, q, pl, ksp, opx, py, liq bi, pl, ksp, opx
Contrib Mineral Petrol (2012) 163:67–85

assemblage
BSE/CL texture Core-outer core-rim, Core-rim, cracks in rim Core-rim, cracks in rim Core-outer core-rim, Core-outer core-rim, Core-rim, limited
inclusion-rich cores, inclusion-rich cores, inclusion-rich cores, cracks
cracks in core and rim cracks in core and rim cracks in core and rim
BSE response High Low High High High Low
CL response Core: low–high, blurred, Core: mod., oscil. Core: low-mod., blurred, Core: low–high, blurred, Core: mod.-high, blurred, Core: low-mod., sector
thickened and/or zoning ± sector zoning thickened and/or thickened and/or thickened and/or zoning ± planar
convoluted oscil. convoluted oscil. convoluted oscil. convoluted oscil. zoning banding
zoning or sector zoning/ zoning or sector zoning zoning ± sector zoning
planar banding
Outer core: oscil. zoned, Rim: low-mod. (\50 lm); Rim: mod.-high Outer core: oscil. zoned, Outer core: oscil. zoned, Rim: high (\50 lm);
concordant around core lobate edges, embays (\90 lm); lobate concordant around core concordant around core lobate edges, embays
core primary zoning edges, embays core core primary zoning
primary zoning
Rim: low inner (\30 lm) Rim: mod.-high (\70 lm) Rim: low-mod. inner
±high outer (\90 lm); (\70 lm) ±mod.-high
lobate edges, embays outer (\20 lm); lobate
core/outer core primary edges, embays core/outer
zoning core primary zoning
No. U–Pb/trace 34 (23 grains) 21 (21 grains) 20 (18 grains) 51 (41 grains) 19 (11 grains) 38 (37 grains)
element
analyses
No. Hf isotope 16 (12 grains) 11 (11 grains) 11 (9 grains) 25 (22 grains) 12 (7 grains) 21 (20 grains)
analyses
Th content 148–1,187 162–651 (most \ 400) 83–1,079 (most \ 300) 147–1,952 (most \ 1000) 117–895 50–2,000
(ppm) (most \ 1,500)
U content (ppm) 98–3,283 (most \ 1000) 122–790 (most \ 300) 84–1220 199–1,914 266–1,900 (most \ 1400) 66–755
Th/U 0.17–3.57 0.68–2.30 (most 1–1.5) 0.20–2.30 (most \ 1.30) 0.12–2.52 (most \ 1.50) 0.26–1.21 (most \ 0.60) 0.61–2.80
(most [ 1.00)
73

123
74

Table 1 continued
Sample LM53 LF60 LM01 LM11 RW28 LM12

123
Y content (ppm) 505–2,978 495–2,270 (most \ 1,500) 316–10,356 345–4,169 (most \ 1,500) 328–3,764 (most \ 1,000) 298–2,739
(most \ 1500) (most \ 2,500) (most \ 2,000)
Sm/La 24 113 15 43 21 85
(normalised to
chondrite)
Lu/Gd 16 14 18 21 24 9
(normalised to
chondrite)
Ce/Ce* 8 14 2 15 17 6
Eu/Eu* 0.1 0.1 0.1 0.2 0.2 0.2
207
Pb/206Pb age 750–1,664 (B43% disc.) 940–992 (B5% disc.) 817–1,506 (B36% disc.) 555–1,222 (B17% disc.) 895–1,238 (B13% disc.) 690–1,048
(Ma) (max. (B11% disc.)
range)
207
Pb/206Pb age 883–1,512 (B5% disc.) 940–992 (B5% disc.) 829–1,149 (B5% disc.) 555–1,222 (B5% disc.) 895–1,238 (B5% disc.) 690–1,048
(Ma) (near- (B5% disc.)
conc. range)
No. analyses 25 (74%) 8 (38%) 12 (60%) 26 (51%) 14 (74%) 19 (50%)
discordant
([ 2%)
176
Hf/177Hfi 0.281846–0.281933 0.281926–0.281945 0.281874–0.281960 0.281841–0.281927 0.281829–0.281963 0.281922–0.282027
(excluding
outliers in Hfi/
REE)
No. analyses 2 1 1 1 0 1
with outlying
Hfi
No. analyses 9 2 4 3 4 0
with unusual
trace elements
Eu/Eu* = Eu(n)/H(Sm(n)*Gd(n)), Ce/Ce* = Ce(n)/H(La(n)*Pr(n))
mnz monazite, bi biotite, q quartz, ksp K-feldspar, pl plagioclase, ru rutile, opx orthopyroxene, py pyrite, liq silicate melt
Contrib Mineral Petrol (2012) 163:67–85
Contrib Mineral Petrol (2012) 163:67–85 75

LM53 (4-04) t.r. LM53 (4-19) LM53 (4-07) LM53 (5-07)


quartz
quartz
d.f. 1.84 Ga (THf DM)
ksp 1.90 Ga (THf DMc)
biotite
it 1664±37 Ma
(72% conc.)

ksp t.r./g.z.
898±19 Ma
(95% conc.) 883±24 Ma 1.83 Ga (THf DM) 969±14 Ma
1.80 Ga (THf DM) (102% conc.) 2.13 Ga (THf DMc) (102% conc.)
2.13 Ga (THf DMc)
1345±14 Ma 1.82 Ga (THf DM)
(92% conc.) 2.13 Ga (THf DMc)
2.03 Ga (THf DM) 975±20 Ma
1223±19 Ma
(a) (97% conc.) 2.32 Ga (THf DMc) 100µm (b) t.r./g.z. t.f./g.z.
100µm (c) (94% conc.) 100µm (d) 100µm

LM11 (2-106) LM11 (2-87)


LM11 (2-84) 979±27 Ma LM11 (1-19)
(100% conc.)
1.80 Ga (THf DM)
2.26 Ga (THf DMc)

570±5 Ma
1140±22 Ma (97% conc.)
(99% conc.)

1.76 Ga (THf DM)


2.17 Ga (THf DMc) 1097±17 Ma
(98% conc.)
1.88 Ga (THf DM)
1111±13 Ma d.f. 2.46 Ga (THf DMc)
1.83 Ga (THf DM)
(96% conc.)
(e) 2.29 Ga (THf DMc) 100µm
(f) 100µm (g) t.r.
100µm
(h) 100µm

RW28
W28 (2-13)
2-1 1.86 Ga (THf DM) t.r. RW28 (2-09) 1.87 Ga (THf DM) t.r. t.r.
ksp 2.37 Ga (THf DMc) 2.39 Ga (THf DMc)
RW28 (2-24)
d.f.
1057±21 Ma 1034±22 Ma
biotite (93% conc.)
(95% conc.)
quartz
melt(?)

910±17 Ma biotite
1.90 Ga (THf DM) (108% conc.)
2.42 Ga (THf DMc) 1.71 Ga (THf DM) 1084±20 Ma
2.24 Ga (THf DMc) (105% conc.)

g.z. 1238±94 Ma
quartz(?) 1077±17 Ma 1.77 Ga (THf
THf DM) 1078±17 Ma (97% conc.)
(i) (102% conc.)
100µm (j) 2.21
.21 Ga
a (THf
TH DMc) (101% conc.)
100µm (k) probable xenocryst 100µm

Fig. 3 Representative BSE and CL images of zircon from samples are oscillatory zoned. Rim domains are transgressive (t.r.), inward
LM53, LM11 and RW28. Most grains are elongate with two penetrating, lobate areas that embay outer core domains (most
terminations (except d); these contain core, outer core and rim grains). Some rim domains preserve patchy ghost zoning (g.z.; e.g.
domains. Core domains are variable, but most exhibit faint or b). Inclusions are most common in core domains (e.g. a). Cracks are
modified oscillatory zoning (e.g. i). Outer core domains mimic core common in core and rim domains (most grains). One grain is faceted
shape (e.g. j) with local truncation (dissolution front, d.f.; e.g. f) and with soccer ball shape and sector zoning (d); it lacks rim development

LF60, LM01 and LM12 most commonly have core-rim domains (Fig. 4b). Rare, small sector zoned ovoid (Fig. 4c,
structures and fewer inclusions (Fig. 4). Zircon grains with h) or faceted (Figs. 3d, 4d) grains resemble metamorphic
core-outer core-rim texture have radial cracks in core and grains in all five charnockitic gneiss samples. These grains
rim domains (Fig. 3a, e, i, j), whereas zircon grains with are the least texturally complex zircon lacking secondary
core-rim texture mostly have cracks only in rim domains textures.
(Fig. 4e). Penetrative cracks that propagate across appar- Zircon isotopic data and ages are presented for each
ently coherent domains and around inclusions also occur in sample in Fig. 5 (full dataset in Supplementary Material
some grains in all samples. The core-outer core-rim versus 3–8). REE data are summarised in Table 1 (full dataset in
core-rim zircon types does not correlate with the petro- Supplementary Material 9–14 and representative plots in
graphic types defined above. The BSE and CL response Supplementary Material 15). There is no correlation
and texture of core domains are both highly variable. Outer between the apparent age of zircon domains and the U, Th,
core domains, where present, are oscillatory zoned which Y-contents or Th/U values. However, Th/U values and total
generally mimics the shape of the core (Fig. 3a–c, e, g, i, j), trace element content are generally lower in rim domains
though local truncation of core zoning may be present compared to that of adjacent core or outer core domains in
(Fig. 3f, k). Rim domains have inward penetrating lobate individual grains. Most REE signatures show steeply
edges, commonly penetrate from prism terminations in positive chondrite normalised La-Lu patterns with positive
elongate grains, and embay primary zoning in adjacent Ce and negative Eu anomalies, typical of igneous zircon
core or outer core domains (Figs. 3a–c, g, i–k, 4a, f, g, i–l). grains (Supplementary Material 15). Zircon populations in
Patches of remnant primary zoning (ghost zoning; Figs. 3b, all samples (except LF60) show a broad age range and
c, 4b, f) and weak sector zoning are common in rim variable discordance (Table 1; Fig. 5). The near-concor-
domains. Rare patches within core domains also display dant zircon ages (B 5% discordance) typically span
very high CL-response (bleached) with ghost zoning 350–650 Myr. Intra-sample Hfi values are clustered, and
(Fig. 3i). Very rare sigmoidal domains are inward pene- most analyses are within error of the sample mean (±2SD).
trating and cause convolution of primary oscillatory-zoned Electron Backscattered Diffraction (EBSD) analysis of

123
76 Contrib Mineral Petrol (2012) 163:67–85

LF60 (2-33) LF60 (2-26) g.z. LF60 (2-41) LF60 (3-07)


rutile
947±12 Ma 992±11 Ma
(99% conc.) (95% conc.)
1.75 Ga (THf DM)
2.02 Ga (THf DMc) biotite

976±12 Ma
(96% conc.)

1.74 Ga (THf DM)


2.03 Ga (THf DMc) 1.74 Ga (THf DM)
t.r.
959±11 Ma 2.03 Ga (THf DMc)
(97% conc.)
(a) 100µm (b) t.r. 100µm (c) 100µm (d) 100µm

LM01 (3-16) 1.85 Ga (THf DM) LM01 (3-14) t.r.


2.14 Ga (THf DMc)
LM01 (3-41) 970±15 Ma LM01 (3-70)
(95% conc.)
1427±16 Ma 1.84 Ga (THf DM) 958±12 Ma
(87% conc.)
(92% conc.) 2.29 Ga (THf DMc)
1126±10 Ma
(97% conc.)

t.r./g.z.
1506±30 M
Ma
(93% conc.)
conc.

(e) 2.29 Ga (THf DM)


2.82 Ga (THf DMc)
100µm (f) 100µm (g) 100µm (h) 100µm

1.73 Ga (THf DM)


LM12 (5-03) LM12 (5-21) LM12 (4-35) LM12 (5-22) 2.05 Ga (THf DMc)
805±13 Ma
t.r. (95% conc.)
t.r. t.f./g.z.(?)

934±16 Ma
(98% conc.)

1.63 Ga (THf DM)


988±15 Ma
(99% conc.) 1.97 Ga (THf DMc) 718±20 Ma
690±13 Ma (95% conc.)
1.70 Ga (THf DM) (98% conc.) 1.65 Ga (THf DM)
(i) 1.96 Ga (THf DMc) 100µm (j) 100µm (k) 100µm (l) 1.98 Ga (THf DMc) 100µm

Fig. 4 Representative BSE and CL images of zircon from samples rim texture while metamorphic grains lack rims. Igneous cores are
LF60, LM01 and LM12. Igneous grains are elongate with two commonly oscillatory zoned in samples LF60 and LM01(e.g. a) or
terminations (a, b, f, g, i–k), while metamorphic grains are faceted, banded in sample LM12 (e.g. k). Rim domains are generally narrower
ovoid grains with sector zoning (c, d, h). Igneous grains show core- than for Fig. 3 (e.g. i), otherwise features are similar to Fig. 3

representative zircon grains from the least (LF60) and most analysis (or group of analyses) that satisfies our criteria is
texturally complex (RW28) samples identified small mis- considered a minimum estimate of protolith emplacement.
orientations of a few degrees (strain) within sub-domains Isotopic disturbance of zircon is highlighted by 38–74%
and across cracks (Supplementary Material 16). of analyses being[2% discordant. Commonly, 2–4 (and up
to 9) zircon grains per sample contain anomalous trace
element content. Only sample LM12 had a consistent trace
element pattern across all analysed zircon grains. Despite
Discussion
the broad span in 207Pb/206Pb zircon ages, samples com-
monly showed a narrow range of Hfi consistent with a
Interpretation of results and ‘minimum emplacement
single population. Only a total of 6 analyses outlying Hfi
age’ criteria
values (outside of the mean of the main popula-
tion ± 2SD). All grains with any combination of [2%
Our complex geochronological data warrant a reevaluation
discordance, anomalous trace element content or outlying
of the validity of a c. 970 Ma crystallisation age interpreted
Hfi were excluded from the determination of the minimum
for the Mawson Charnockite (Young and Black 1991). The
emplacement age. Our results resolve three minimum
appreciable disturbance in zircon U–Pb isotopic data for
emplacement age groups: c. 1,145–1,140 Ma (LM01,
the Mawson Charnockite invalidates a simple weighted
LM11), c. 1,080–1,050 Ma (RW28, LM12) and c. 985–
mean approach for age determination. We posit conserva-
960 Ma (LM53, LF60). These age groupings do not match
tive criteria to refine age determinations in complex zircon
populations affected by Pb-loss: ages should be determined
from U–Pb analyses that are robust (98–102% concordant), Fig. 5 Concordia plots with probability density curves (dark grey c
and which have consistent Th, U, Y and REE-content and \5% discordance; light grey all data). Vertical dashed lines on Hfi
versus age plots for each sample mark the minimum emplacement
Hf-isotopic values. This approach facilitates exclusion of ages, and the width of the horizontal grey arrow is equal to two
potential xenocrysts from the age determination. In the standard deviations about the mean of Hfi values. DM Depleted
discussion below, the oldest (non-xenocrystic) zircon Mantle, CHUR Chondritic Uniform Reservoir

123
0.28 0.24
LM53 - Charnockite 1500 LM11 - Charnockite
Mawson Station Austskjera
0.24 1200
1300 0.2825 0.20 0.2825
Oldest concordant zircon LM53 - Charnockite, Mawson Station DM Oldest concordant zircon
207 207
LM11 - Charnockite, Austskjera DM
Pb/206Pb age Pb/206Pb age
0.20 984±14 Ma 1140±22 Ma 0.2823
1100
0.2823 1000
0.16
0.2821 CHUR 0.2821 CHUR

Pb/238U
0.16

Pb/238U
900 Mean 176Hf/177Hfi = 0.281880±0.000043 Mean 176Hf/177Hfi = 0.281890±0.000043
800

206

206
0.2819 ? 0.2819
Contrib Mineral Petrol (2012) 163:67–85

0.12
0.12 700 Pb-loss Pb-loss
(g)
Hf/177Hf initial
(a) 0.2817 Minimum emplacement age = c.985 Ma 600 0.2817

Hf/177Hf initial
Age (Ma) (b) Age (Ma) Minimum emplacement age = c.1140 Ma
176 (h)

176
500 700 900 1100 1300 1500 50µm
1700 500 600 700 800 900 1000 1100 1200 1300
0.08 0.2815 0.08 0.2815
0.5 1.5 2.5 3.5 650 750 850 950 1050 1150 0.6 1.0 1.4 1.8 2.2 2.6 650 750 850 950 1050 1150
Age (Ma) Age (Ma)
0.170 0.22
LF60 - Charnockite RW28 - Charnockite
Mt Horden Chapman Ridge 1200
0.166 990 (i)
0.20
0.2825 Oldest concordant zircon 0.2825
Oldest concordant zircon 970 LF60 - Charnockite, Mt Horden DM 207
Pb/206Pb age 1100 Oscil. zoned
0.162 207
RW28 - Charnockite, Chapman Ridge DM
Pb/206Pb age 1078±17 Ma (outer core) outer cores
961±16 Ma 0.2823 0.18 Mean = 1077±15 Ma 0.2823
950 (MSWD=0.13, n=5)
0.158 1000

Pb/238U

Pb/238U
0.2821 CHUR 0.2821 CHUR
930 Mean 176Hf/177Hfi = 0.281936±0.000060 0.16

206
Mean 176Hf/177Hfi = 0.281888±0.000078

206
0.154
0.2819 900 0.2819 ?
910
Mean = 957±6 Ma (c) 0.14
0.150 (MSWD=1.3, n=21)
Pb-loss

Hf/177Hf initial
Hf/177Hf initial

0.2817 800 0.2817


890 Minimum emplacement age = c. 975 Ma
Age (Ma) Age (Ma) Minimum emplacement age = c.1080 Ma

176
176

500 600 700 800 900 1000


(d) 500 700 900 1100 1300
(j)
0.146 0.2815 0.12 0.2815
1.35 1.45 1.55 1.65 650 750 850 950 1050 1150 1.0 1.4 1.8 2.2 2.6 650 750 850 950 1050 1150
Age (Ma) Age (Ma)
0.26 0.19
LM01 - Charnockite LM12 - Gabbro
Macey Island 1400 Macklin Island 1050
0.24 0.2825
0.17 LM12 - Gabbro, Macklin Islan d DM
1300
0.22 Oldest concordant zircon
0.2825 LM01 - Charnockite, Macey Island DM Oldest concordant zircon
950 0.2823
207 Oscil. zoned cores/ 207
Pb/206Pb age 1200 0.15 Pb/206Pb age
0.20 1145±11 Ma outer cores 0.2823 1048±39 Ma
Mean = 1110±20 Ma 850 0.2821 Mean 176Hf/177Hfi = 0.281979±0.000054 CHUR
1100 (MSWD=3.6, n=7) ?
Pb/238U

0.18 CHUR

Pb/238U
0.2821 176 177 0.13 0.2819 Pb-loss
Mean Hf/ Hfi = 0.281919±0.000055
1000 750
206

206
0.16 0.2819
Hf/177Hf initial

900 Pb-loss
0.2817 Minimum emplacement age = c.1050 Ma
0.11 650
176

(l)

Hf/177Hf initial
0.14 (e) 0.2817
(k)
800 Age (Ma) Minimum emplacement age = c.1145 Ma Age (Ma) 0.2815

176
500 700 900 1100 1300 100µm
1500
(f) 500 600 700 800 900 1000 1100 1200 650 750 850 950 1050 1150
0.12 0.2815 0.09
1.0 1.4 1.8 2.2 2.6 3.0 3.4 650 750 850 950 1050 1150 0.7 0.9 1.1 1.3 1.5 1.7 1.9
Age (Ma)
207 Age (Ma) 207
Pb/235U Pb/235U
77

123
78 Contrib Mineral Petrol (2012) 163:67–85

either the petrographic types or zircon core-outer core-rim and textural variation, contacts between these composi-
versus core-rim types. tional types are commonly hidden beneath ice. Where
Relative trace element content between zircon grains contacts are observed, they generally appear gradational.
was undertaken to distinguish possible xenocrysts, but Rare sharp intrusive contacts between porphyroblastic
identified anomalous grains were commonly enriched in (megacrystic) opx-granite and even-grained opx-granodi-
LREE; these analyses may be contaminated by ablation of orite are noted (Sheraton 1982), but trends of xenoliths are
micro-inclusions of, for example, monazite and apatite undisturbed and relative ages cannot be determined (Crohn
(both identified in EDS analysis); therefore, an anomalous 1959). In contrast, two phases of charnockitic-type (i.e.
trace element content is not a robust criterion for identi- opx-bearing) granitoids are mapped further west in the
fying zircon xenocrysts in our study. However, no grains Colbeck Archipelago (White and Clarke 1993) and at Cape
older than our interpreted minimum emplacement ages Bruce (Dunkley et al. 2002) but are distinguished from the
were excluded on the basis of anomalous trace element Mawson Charnockite on both compositional and temporal
content alone, and domains with anomalous REE were grounds. Mafic to felsic opx ± cpx-bearing gneisses,
excluded from calculations of mean Hfi values. Therefore, locally containing pods of ultramafic orthogneiss and
none of the minimum emplacement ages determined are metasedimentary xenoliths, are interpreted to have intruded
influenced by potential ablation of micro-inclusions. prior to D1 (Dunkley et al. 2002; White and Clarke 1993).
It is notable that 6 zircon analyses (2–7% discordant) in A later phase of biotite ± opx-bearing orthogneissic bod-
sample LM11 yield apparent 207Pb/206Pb ages (c. 1,220– ies/dykes cuts S1 but contains an S2 foliation; this rock
1,145 Ma) that are older than the interpreted minimum type is intruded by the Mawson Charnockite on Chapman
emplacement age (c. 1,140 Ma). These exhibit ‘normal’ Ridge (White and Clarke 1993) and is interpreted to have
trace element-contents (Supplementary Material 12) and been emplaced at 992 ± 10 Ma (Dunkley et al. 2002).
Hf signature (in the case of 2_91; Supplementary Material Further detailed geochronological constraints on these
6), suggesting our c. 1,140 Ma emplacement estimate charnockitic phases are required to posit any correlations
could be extended by a further c. 80 Myr. This highlights with the 3 age-types now identified further east within the
the need to analyse a large population of grains in order to Mawson Charnockite.
capture the oldest grains.
An early study of the Mawson Charnockite (Young and Assessment of zircon growth/recrystallisation
Black 1991) determined igneous crystallisation ages of
985 ± 29 Ma (sample z644; Ufs Island) and 954 ± 12 Ma Most zircon in this study is dominantly oscillatory or sector
(sample z542; Falla Bluff) using a weighted mean zoned with euhedral, doubly terminating grain shapes
approach. Without the benefit of high-quality BSE and CL consistent with an igneous crystallisation origin. Char-
images, trace element or Hf-isotopic data, the ages appear nockitic gneiss samples also contain rare sector zoned,
robust, but there are complexities that point to isotopic ovoid or faceted grains consistent with a metamorphic
disturbance identical to our new data. Tentatively revised origin (possibly in the presence of an anatectic melt). A
minimum emplacement ages, based on the oldest concor- common texture identified in igneous grains in three sam-
dant zircon (with common Th- and U-contents), are ples (LM53, LM11 and RW28) involves the definition of
c. 1,010 Ma and c. 980 Ma for the Ufs Island and Falla core, outer core and rim domains. Core domains are vari-
Bluff plutons, respectively. A later study (Halpin et al. able, whereas outer core domains are always oscillatory
2005) similarly identified a complex spread of zircon zoned. Rim domains are defined where oscillatory-zoned
207
Pb/206Pb ages in a sample from the Mawson Station zircon fades into unzoned or weakly sector-zoned zircon
region (sample 90030), which was interpreted to reflect towards the rim. The rim domains commonly occur as
either: (1) variable Pb-loss during orogenesis or (2) a mix of transgressive, lobate, inward-penetrating patches. A second
inherited zircon, Pb-loss and new growth. The narrow range group of samples (LF60, LM01 and LM12) contain zircon
of Hf-isotopic data supports the former interpretation. A identified by core-rim texture alone where rims are similar
revised age estimate using our new criteria for sample to the first group.
90300 is c. 1,060 Ma, older than our minimum age estimate The textural relationship between cores and outer cores
of c. 985 Ma for sample LM53 from a similar location. could be interpreted as a two-stage evolution in the magma
The three phases of magmatism identify chronological chamber; the latter (oscillatory outer core) stage potentially
complexity within rocks originally all mapped as the at fluid-saturated conditions (Schaltegger et al. 2005).
Mawson Charnockite (sensu stricto) (e.g. Crohn 1959; Outer core domains are Th, U and Y-rich compared to
Trail 1970; Young et al. 1997) and long interpreted as adjacent non-xenocrystic cores, and REE-contents are
coeval (Young and Black 1991). Whereas this plutonic similar or higher in all grains in samples LM53 and RW28,
complex exhibits significant geochemical, mineralogical and most grains in sample LM11. The total trace element

123
Contrib Mineral Petrol (2012) 163:67–85 79

content of outer cores is consistently higher than its adja- zircon grains are now metamict. Expansion occurs during
cent core. This trend may form during magmatic frac- metamictisation, such that adjacent zircon is commonly
tionation (Silver and Deutsch 1963), recharge by a trace cracked (Lee and Tromp 1995). Cracking is observed
element rich magma or solid-state trace element migration adjacent to all outer core domains (Fig. 3). Cracks were
during slow cooling (Pidgeon et al. 1998). High contents of also observed in rim domains in core-rim-type grains.
contaminant elements distort the zircon lattice (Köppel and Metamorphic studies (e.g. Clarke and Norman 1993;
Sommerauer 1974) and have been proposed to drive re- Dunkley et al. 2002; Halpin et al. 2007; White and Clarke
crystallisation of zircon domains with high trace element 1993) suggest that the Mawson Charnockite resided in the
content (Pidgeon 1992). Incompatible cations within the middle crust at c. 970 Ma such that continuous annealing
zircon structure are expelled during recrystallisation, and of zircon would have delayed metamictisation (and there-
the original euhedral form may be modified such that fore cracking) until exhumation of the terrane, probably
grains become blunt (slightly rounded) in this model. This during or after c. 550–500 Ma. However, with the dis-
process is envisaged here to produce the rim domains in covery of magmatism at c. 1,145–1,140 Ma (LM01,
samples LM53, LM11 and RW28. This interpretation is LM11), c. 1,080–1,050 Ma (RW28, LM12), we cannot
supported by the observation that rim domains contain discount that these older rocks were partially exhumed to
consistently lower trace element content (Supplementary within *10 km of the surface and allowed to cool below
Material 9–15). In addition, similar Hfi values in adjacent the critical amorphisation temperature (discussed further
outer core and rim domains (Fig. 5) suggest modification below). In this case, zircons from these earlier magmatic
of primary zircon rather than new zircon growth (e.g. pulses may have acquired some radiation damage, before
Bomparola et al. 2007; Halpin et al. 2005). The rim being deeply buried (and annealed) during the main phase
domains of zircon with core-rim texture (samples LF60, of the Rayner Orogeny at c. 990–910 Ma. However, alpha-
LM01 and LM12) are generally narrower and less well decay dose calculations suggest that the *150 Myr inter-
developed but have similar characteristics. We suggest the val (between c. 1,145 Ma and c. 990 Ma) is not long
isotopic, chemical and physical attributes of rim domains enough for zircons from the earliest intrusions to have
of igneous zircon in this study are most compatible with evolved past the first percolation point in the crystalline-to-
formation via partial recrystallisation of grain rims. A amorphous transition (Geisler et al. 2003) such that zircon
partial recrystallisation process could occur: (1) in the solid was not amorphous by this time.
state without a fluid phase (Hoskin and Black 2000) (2)
during a solid-state diffusion–reaction process in the Facilitation of Pb-loss
presence of a high temperature fluid ([600°C; Geisler et al.
2007) or (3) during coupled dissolution–precipitation Above we document both zircon recrystallisation and
(Tomaschek et al. 2003). We argue against complete re- metamictisation in our samples. These processes cause Pb-
crystallisation (i.e. construction of a new zircon lattice) in loss and may explain the smearing of our age determina-
rim domains, as this should expel Pb, completely reset the tions along concordia over several hundred Myr (Fig. 6).
U–Pb age and remove all trace of primary zoning. The rare However, the overlapping age determinations for core,
inferred metamorphic zircon grains have similar total trace outer core and rim domains in all samples indicate Pb-loss
element content and Hfi values to the igneous grains and was not specific to any one domain. This also suggests that
span between 990 and 950 Ma. This suggests they formed the recrystallisation identified in rim domains must have
via quantitative replacement of igneous zircon, i.e. disso- taken place shortly following igneous crystallisation;
lution of zircon by melt or metamorphic fluid and repre- otherwise, the rim domains should have a discernibly
cipitation at nearby sites. younger age distribution compared to adjacent core or
outer core domains (Fig. 6). In addition, the metamictisa-
Metamictisation and cracking of zircon tion and cracking are likely too young to have facilitated
the observed Proterozoic Pb-loss. Even if the earliest
Metamictisation in zircon occurs via accumulation of U intrusions (c. 1,145–1,140 Ma) were exhumed and cooled,
and Th radioactive decay causing time-integrated damage prior to reburial during the main phase of orogenesis
of the zircon lattice. Damage is counteracted by recovery, a (c. 990 Ma), there would not have been sufficient time for
type of annealing involving repair rather than construction primary zircons to become metamict. Minor recent Pb-loss
of a new zircon lattice (Nasdala et al. 2001), which takes via leaching of Pb along cracks is indicated by the slightly
place above a ‘critical amorphisation temperature’ younger ages of cracked core domains compared to adja-
(approximately 350°C, but varies as a function of U-con- cent outer core domains (Fig. 6).
tent and age; Meldrum et al. 1998). Calculations of alpha- We exclude these two common processes as key facil-
decay dose (after Holland and Gottfried 1955) suggest most itators of the majority of Proterozoic Pb-loss observed.

123
80 Contrib Mineral Petrol (2012) 163:67–85

(a) (b) (c)

core
inclusion
rim
c. 1130
outer core
c. 1120 c. 1150
Igneous crystallisation 1400 Development of rim: c/oc/r cluster Involving construction Pan-African Pb-loss 1400
at c. 1200 Ma of a new lattice?
c/oc (i) Soon after 1000 Either
crystallisation yes or no We observe:
1000 ad 1000
c/oc cluster
1000 pre
c/r s
ad c/o
(ii) 250 Myr 1000 spre

ki ord
after crystallisation rims No

ac c
ng
cr s
g os
500 500

in -l
c/oc cluster

w Pb
llo t
fo cen
(iii) 250 Myr 1000

e
R
after crystallisation rims cluster Yes

Fig. 6 Cartoon of the development of zircon textures (based on few hundred Myr after crystallisation (U–Pb data for rim domains
sample RW28) and associated hypothetical U–Pb analyses on spread along concordia) or (iii) A few hundred Myr after crystalli-
concordia for core-outer core-rim type zircons. a Core and oscilla- sation via construction of a new lattice (U–Pb data for rim domains
tory-zoned outer core domains develop during a two-stage evolution clustered at a younger age equivalent to the age of the event which
in the magma chamber, possibly reflecting changes in fluid-saturation facilitated complete recrystallisation). c The complex spread of U–Pb
and magma chemistry during melt fractionation or magma recharge. data along concordia and overlapping age determinations for core,
Corresponding U–Pb analyses would cluster on concordia at the age outer core and rim-domains (inset) indicates Pb-loss was not specific
of crystallisation. b Development of transgressive rim domains with to any one domain. Partial recrystallisation of zircon margins
ghost zoning and ‘blunting’ of terminations, interpreted to have occurred soon after crystallisation as shown in b(i), followed by
formed during recrystallisation of core-outer core domains. Recrys- Pb-loss during Proterozoic high-T, high-strain orogenesis via diffu-
tallisation may occur: (i) soon after magmatic crystallisation (clus- sion. Pan-African orogenesis likely also caused minor variable
tered U–Pb data for core-outer core-rim domains, temporal Pb-loss. Cracking of core and rim domains likely facilitated minor
discrimination not possible using the LA-ICPMS technique), (ii) A Pb-loss during Palaeozoic-Recent times. See text for discussion

Several experimental (e.g. Cherniak and Watson 2001, and across cracks. However, it is unclear whether this
2003; Cherniak et al. 1991) and field studies (e.g. Möller records high-T Proterozoic strain associated with protracted
et al. 2002) suggest that diffusion in crystalline zircon is a orogenesis or Paleozoic to Recent strain associated with
negligible process, unless zircon grains are exposed to metamictisation and cracking.
upper mantle temperatures. However, Ashwal et al. (1999)
note a c. 80 Myr spread in concordant U–Pb ages, which Grevillian context of the Rayner Orogen
they infer resulted from volume diffusion driven Pb-loss
during protracted granulite facies metamorphism in SW Isotopic mapping via crustal model ages in conjunction
Madagascar. Timms et al. (2006) examined crystal-plastic with high-precision geochronology can help delineate dis-
deformation microstructures in zircon and showed defor- tinct crustal terranes in complex regions. In the case of east
mation enhances diffusion of trace elements. These case Antarctica where outcrop is sparse, such a technique has
studies are analogous to the tectonic history documented potential to shed light on the genetic relationship of adja-
for the Mawson Charnockite that involved T [ 850–900°C cent terranes and assess the probability of a shared history.
during progressive deformation (Halpin et al. 2007). We In MacRobertson Land, geochemical and Sr–Nd isotopic
infer that the combination of high-T and strain during systematics of charnockites and host rocks were suggested
protracted Proterozoic orogenesis most likely caused vari- by Young et al. (1997) to reflect three distinct zones
able Pb-loss that developed the smear of concordant ages (Fig. 1); the provincial distribution of these data was sug-
measured. In this scenario, high temperatures promote gested as potentially important for supercontinent
recovery of lattice strain, which may erase any micro- reconstruction.
structural evidence of the crystal-plastic deformation that Our THfDM model ages for samples collected across the
facilitated Pb-loss. Small misorientations (in the order of a three zones delineated by Young et al. (1997) are indis-
few degrees) identified via EBSD analysis (Supplementary tinguishable (compare Fig. 7a with Fig. 7b), suggesting
Material 16) suggest minimal strain within sub-domains similar source rocks for charnockitic magmatism across the

123
Contrib Mineral Petrol (2012) 163:67–85 81

TNdDM Young et al. (1997) preferred technique for metamorphosed rocks (Scherer
4
et al. 2007).
Our data set, combined with reinterpreted previous
3 geochronology, extends the onset of magmatism in the
Rayner Orogen to the Mesoproterozoic (at least c.
2
1,145–1,140 Ma and possibly [1,220 Ma). The preserva-
tion of igneous microstructure in sample LF60 combined
with a limited concordant Gaussian distribution of
Cumulative total

1 207
Pb/206Pb ages suggests a single igneous zircon popula-
(a) tion that is suited to a weighted mean approach. This
sample yields an age of 957 ± 6 Ma that we interpret as
25 This study &
Western Zone
Halpin et al. (2005)
the igneous crystallisation age, indicating magmatism
Central Zone extended to the Neoproterozoic. These data define episodic
20
Eastern Zone magmatism over at least 3 periods between c. 1,150–
960 Ma for construction of the Mawson Charnockite
15
composite pluton.
Meso-Neoproterozoic intrusive rocks occur in adjacent
10
terranes in east Antarctica. However, the significance of
5
widespread Pan-African-aged tectonism and magmatism in
regions to the east and west of the Rayner Orogen (i.e. the
THf (c)DM (b)
0 Prydz Bay-Denman Glacier and Lutzow-Holm Bay-Central
1600 1700 1800 1900 2000 2100 2200 2300 2400
Dronning Maud Land regions) continues to be debated.
Age (Ma)
0.2821
Pan-African tectonism and magmatism in each of these
regions has been variably interpreted as either intracratonic
C

(c)
DM
H

0.2820
U

(e.g. Yoshida et al. 2003) or intercratonic (suture zones, e.g.


R

(Lu/H
f=0.0
Hf/177Hf initial

0.2819
Pb-loss 1) Fitzsimons 2000b). Fitzsimons (2000a) used a compilation
0.2818 (Lu/H of U–Pb zircon data to infer that neighbouring ‘Grenville-
RW28 f=0.0
1)
0.2817 LF60 age’ fragments in east Antarctica had distinct crustal his-
90030
0.2816 LM53 THf (c)DM tories such that rocks of the Rayner terrane (c. 990–900 Ma)
176

LM12
c. 1920-2220 Ma were considered to have amalgamated with those of the
0.2815 LM01
LM11 Maud terrane (c. 1,090–1,030 Ma) at 650–550 Ma, and
0.2814
500 700 900 1100 1300 1500 1700 1900 2100 2300 with the Wilkes terrane (and Albany-Fraser Orogen
Age (Ma) equivalents in Australia, c. 1,330–1,130 Ma) during the
final assembly of Gondwana at 600–500 Ma. The paradigm
Fig. 7 a Nd model ages reproduced from Young et al. (1997). b Hf
HfðcÞ
shift has gained much support by many workers and has
model ages (TDM where Lu/Hf = 0.01) for the charnockitic samples
been adopted in recent supercontinent reconstructions (e.g.
from Halpin et al. (2005) and this study (excluding gabbroic sample
LM12). c Hfi versus age plot of all data from Halpin et al. (2005) and Li et al. 2008; Pisarevsky et al. 2003).
this study While it is well outside the scope of this paper to
investigate the nature of Pan-African events in east Ant-
arctica and terrane correlations, our U–Pb data indicate that
region. Variations in observed whole-rock Nd model ages charnockitic magmatism commenced earlier than previ-
as observed by Young et al. (1997) are likely the result of ously recognised in the Rayner Orogen, which allows for
variable contamination of magma with assimilated material discussion of possible Late Mesoproterozoic tectonic cor-
incorporated during magma ascent and emplacement, relations, at least within and across the proposed Pan-
probably in conjunction with variable effects of metamor- African Prydz-Denman-Darling (after Fitzsimons 2000a)
phism and strain partitioning during deformation. Assimi- suture zone. Inside the proposed Pan-African suture zone,
lation and interaction with varying amounts of older crustal fragments with c. 1,380–1,000 Ma protolith
metasedimentary rocks may affect 87Sr/86Sr values; meta- ages occur in the Prydz Bay area (Liu et al. 2007, 2009),
somatic interaction with xenoliths has been interpreted to the Larsemann Hills (Carson et al. 2007; Wang et al. 2008),
cause elevated 87Sr/86Sr in some charnockites from Dron- the Prince Charles Mountains (Corvino and Henjes-Kunst
ning Maud Land (Mikhalsky et al. 2006). The durability of 2007), the Naturaliste Plateau offshore Western Australia
zircon, together with the resistance of the Lu–Hf system to (Halpin et al. 2008) and the Northampton Complex in
disturbance, means in situ Lu–Hf analysis of zircon is a Western Australia (Bruguier et al. 1999). Furthermore,

123
82 Contrib Mineral Petrol (2012) 163:67–85

while geochemical and isotopic similarities between char- Project No. 1150). Samples were collected during the 2004/2005 (by
nockites on either side of the Prydz-Denman-Darling suture LAM and JAH) and 1990/1991 (by Richard White) Australian
National Antarctic Research Expeditions. The authors thank the
have been noted (Mikhalsky et al. 2006), our estimation of Australian Antarctic Division and personnel of Mawson Base for their
the onset of magmatism in the Mawson Charnockite now logistic support, and M. Fitzpatrick for expert guidance in the field.
overlaps ages of charnockitic plutons at the Bunger Hills in M. Morffew of the Australian Antarctic Data Centre provided the map
the Wilkes province (c. 1,170–1,150 Ma; Sheraton et al. of the Mawson Coast. We are grateful to J. Payne, N. Pearson,
E. Belousova and S. Piazolo (GEMOC, Macquarie University) and
1992). Varying degrees of Pb-loss have been observed in K. Goemann (CSL, University of Tasmania) for help with analytical
these Proterozoic rocks. This study outlines an approach to work and interpretation of munted zircon. The authors would like to
consider complex zircon data sets, avoiding simple thank two anonymous reviewers for their careful and constructive
weighted mean calculations and highlights the need for a reviews, which greatly improved the paper. This is contribution 758
from the Australian Research Council National Key Centre for the
detailed reevaluation of the Grenvillian terrane definitions Geochemical Evolution and Metallogeny of Continents (http://
in east Antarctica. www.gemoc.mq.edu.au). The analytical data were obtained using
instrumentation funded by DEST Systemic Infrastructure Grants,
ARC LIEF, NCRIS, industry partners and Macquarie University.
Macquarie University Research Development Grant (MQRDG, grant
Conclusions ref. 9200900498) funding provided financial support to conduct the
research.
Magmatic zircon may undergo variable Pb-loss due to
post-crystallisation isotopic disturbance over hundreds of
millions of years such that an individual ‘age’ of each
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