43

Chemical Geology (Isotope Geoscience Section), 59 (1986) 43-58

Elsevier Science Publishers B.V., Amsterdam - Printed in The Netherlands

INTERPRETATION OF 40Ar/3gAr AND K/Ar DATING EVIDENCE

FROM THE AILEU FORMATION, EAST TIMOR, INDONESIA
R.F. BERRY
Geology Department,
University
Research School of Earth Sciences, Australian
(Received

October

16,1985;

and IAN MCDOUGALL

of Tasmania, Hobart,
National University,

Tas. 7001 (Australia)

Canberra, A.C.T. 2601 (Australia)

revised and accepted March 25, 1986)

Abstract
Berry, R.F. and McDougall,
I., 1986. Interpretation
of 40Ar/39Ar and K/Ar dating evidence from the Aileu
Formation,
East Timor, Indonesia. Chem. Geol. (Isot. Geosci. Sect.), 59: 43-58.
The Aileu Formation,
East Timor, is a zoned metamorphic
complex exposed in a modern arc-continent
collision zone. During collision, extensive retrogression
occurred. K/Ar and 4oAr/39Ar age measurements
on hornblendes
are interpreted
as indicating
that the retrograde metamorphism,
and hence collision, occurred at N 8 Ma ago, Late Miocene. Mica K/Ar ages from two samples reflect cooling of the terrain to
< 300C by 5.5 Ma ago.
Relict Mg-rich hornblende6
lost most of their pre-existing
radiogenic Ar, and Fe-rich hornblendes
were
completely
reset, during the retrogressive phase at middle amphibolite
facies conditions.
At lower grades
of retrogressive
metamorphism,
the Mg-rich hornblendes
retained appreciable
radiogenic
Ar, whereas
Fe-rich hornblendes
lost most of their accumulated
radiogenic Ar even at upper greenschist facies. Thus,
under these conditions,
chemical composition
is an important
factor controhing
Ar loss from hornblende,
although recrystallization
also plays a significant role.

1. Introduction
The island of Timor
is the largest in a
chain of non-volcanic
islands, the Outer
Banda Arc, adjacent
to the northwestern
of the Australian
continental
boundary
crust (Fig. 1). This island chain is part of
a convergent
plate margin
between
the
Indian-Australian
Plate and the Southeast
Asian Plate(s).
The volcanic
Inner Banda
Arc, to the north, is an extension of the
Sunda Arc and was developed on the Southeast Asian Plate during the Tertiary
in response to subduction
of oceanic crust pre0168-9622/86/$03.50

viously occurring between the island arc and

Australia. Thus the Banda Arcs are an example of a very young island arc-continent
collision
(Audley-Charles
et al., 1972; Griffiths and Burrett, 1973; Carter et al., 1976;
Chamalaun
and Grady,
1978;
Hamilton,
1979).
On the north coast of East Timor, at the
point of closest approach to the volcanic
arc, there is a zoned metamorphic
complex,
the Aileu Formation,
which occurs as a
fault-bounded
massif covering - 2000 km2.
Geophysical
and geological evidence (Chamalaun et al., 1976; Berry, 1981) indicates that

o 1986 Elsevier Science Publishers

B.V.

44

BANDA
SUNDA

. ..-......

-...
!

Fig. 1. Map showing

SEA

SHELF

location

,,

TIMOR

SEA

IL

--

at the study area and its relationship

the Aileu Formation

is the northernmost
extension
of continental
rocks in this orogenie belt.
A detailed
study of the northeastern
section of this massif (Berry and Grady,
1981a) suggested a complex
deformational
history but an apparently
simple metamorphic history. The prograde medium-pressure
metamorphic
event ranged from lower greenschist to upper amphibolite
facies. The
earliest penetrative
foliation
(S1) is everywhere
subparallel
to the compositional
layering.
The metamorphic
peak occurred
after the development
of S1. The second
deformation
(Dz) was associated with the
collision
event (Berry and Grady, 1981b).
It caused widespread transposition
of layering and retrogression
of the prograde mineral
assemblage.
The temperature
at the start
of Dz was - 50C less than the thermal
maximum
during the earlier prograde metamorphism,
and rapid cooling occurred during D2. Reconnaissance
K/Ar dating placed
the Dz event in the Mid- or Late Miocene.
Three
subsequent
deformations
(D3, D4
and D5) produced
folds on all scales and
local retrogression
to quartz-chlorite-muscovite assemblages.

to the neotectonics

of Indonesia.

Our principal
aim in this study was to
determine
the age of the prograde metamorphism
and of the Dz retrogression,
in
the Aileu
Formation,
by application
of
the K/Ar
and 40Ar/3gAr dating methods.
These studies revealed that the K/Ar isotopic
system in individual
samples was profoundly
disturbed.
In this paper, we interpret
the
isotopic
age information
in terms of the
mineralogy
of the rocks and geological
constraints.
The correlation
between these
three factors provides further insight into
the behaviour of the K-Ar system, especially
in homblendes,
during retrogressive
metamorphism.

2. Metamorphic

history

The metamorphic
facies produced
by
the prograde metamorphism
were ,described
by Berry and Grady (1981a). The samples
selected for isotopic analysis have prograde
mineralogies
characteristic
of upper greenschist to amphibolite
facies (Fig. 2). In order
to simplify
the discussion the amphibolites
are considered in three groups (A, B and C)
with both spatial and compositional
signifi-

45

EIOTITE

ZONE

CHLORITE
0
I

ZONE
/

IOkm
I

Fig. 2. A comparison
of the prograde metamorphic
Formation.
Sample locations are shown.

000

.
.
0

SYN-D2
BIOTITE
SAMPLE
LOCALITY
PERIDOTITE
+
SERPENTINITE

isograds and the distribution

Fig. 3. Histograms of the anorthite content of plagioclase and the Ti content of hornblende.
Detection
limit for Ti was 0.02 atoms/23 oxygens. Suggested
equilibrium
temperatures
for plagio&e
(Plyusnina, 1982) and upper limits for Ti in each facies
(Raase, 1974) are shown for comparison.

of syn-D, biotite

in the Aileu

cance. The pelitic

samples are discussed
separately.
The group-A amphibolites
(83-191, -195,
-384 and -385) crystallized
in the upper
amphibolite
facies and were retrogressed at
lowest amphibolite
facies conditions.
The
prograde assemblage includes high-Ti
homblende
and calcic plagioclase
(An60--85),
whereas the retrograde
assemblage includes
low-Ti hornblende
and more sodic plagioclase
(Anls--45,
Fig. 3). Optically,
hornblende
can be grouped into clear prograde granoblastic grains, retrograde mottled granoblastic
grains, and fibrous grains and rims which
crystallized
during
the Dz retrogression.
The relative abundances
of these types of
hornblende,
in the samples dated, are shown
in Table I.
The group-B amphibolites
(83-192, -193,
194 and J-1-172) crystallized
at upper amphibolite
facies .and were retrogressed
at
low to middle amphibolite
facies. The prograde mineralogy
is the same as group A
but the retrogressive assemblage has An45--60
plagioclase and the Ti content of hornblende
is only slightly lower than in the prograde
assemblage (Fig. 3). The experimental
results
of Plyusnina (1982) suggest that an increase
in An content from An2, to Ana in this assemblage is equivalent
to a temperature
rise
from 520 to 570C. The textural re-equilibration during the syn-Dz retrogression
is more
advanced in the group-B amphibolites
than

46

TABLE

3. Analytical

Hornblende
types:
in the amphibolites
K/Ar
(Ma)

Group

Group
83-193
83-l 94
l-l-l
72

Group
3-1-192
83-196
3-1-186

l-2- 76

age

of different

pre-D,

hornblende
syn-D,
W)

types

Average
100 x
Mg/(Mg
Fe)

clear
(%)

altered
(W

67.9
29.4
56.3
20.1

::
12
63

44
55
26
42

2
9
i

68
46
58
49

14.0
10.2
15.8
16.5*

32
19
36
59

63
70
48
31

6
11
16
10

56
65
57
53

74
64

6
1
26
9

40
50
56
37

A:

83.191
83-195
83.384
83-386

83-192

Percentage

B:

C*:
7.v2
13.0
11.o*l
lO.S*

41
13
1
27

*I Because of difficulties
in recognizing
the different
types
of hornblende
for group C proportions
are only
accurate to
1 significant
figure.
*K/Ar
ages from Berry and Grady (198la).

in group A but the same three types of

hornblende were recognized (Table I).
The group-C amphibolites
(83-196,
3-1192, 3-1-186 and 1-2- 75) are more variable
in composition
and crystallized
over a range
of conditions
from upper amphibolite
(3-J192) to upper greenschist
facies (I -2- 75).
Sample 3-1-192 was retrogressed at similar
conditions
to the group-B
amphibolites;
the low Ti in its hornblende
reflects the
lower activity
of Ti in these ilmenite-free
sphene-bearing
assemblages (Ghent and Stout,
1984). Samples 3-1-186, 83-196 and 1-2-75
were retrogressed at upper greenschist facies.
Isotopic ages on micas were obtained from
two samples of pelitic schist. Sample 83198 comes from the higher-grade area where
biotite
was stable throughout
D?. Sample
83-197 is from a slightly
lower-grade area
where the temperature
apparently
dropped
to below the biotite isograd, - 4OOC, during
Dz. In both samples the micas were strongly
recrystallized
during the retrogression.

techniques

Mineral
separates of hornblende,
white
mica and biotite
were obtained
by heavy
liquid
and magnetic
separator techniques.
Most of these separates were better than
97% pure. Hornblende
separates typically
contain 1% plagioclase,
1% sphene and 0.5%
ilmenite
as inclusions
and in composite
grains. The hornblende
separate from 83193 contained
92% hornblende
and 5%
diopside;
that from sample 83-195
contained 94% hornblende,
3% plagioclase and
2% sphene. Trace amounts of chlorite and
epidote
were observed but there was no
biotite
or other high-K phase in any of
the hornblende
separates. All samples were
separated at grain sizes between 0.25 and
0.12 mm. These samples were subjected
to conventional
K-Ar
dating and to 4oAr/
3gAr analysis (Merrihue
and Turner, 1966).
Standard
analytical
techniques
were used,
as described
by Walker
and McDougall
(1982).
All samples for 40Ar/3gAr dating
were irradiated for 120 hr. in the X33 facility
of the Australian
Atomic
Energy Commission HIFAR@ reactor at Lucas Heights, N.S.W.
During Ar extraction,
sample temperatures
were monitored
by a Pt-PtRd,,%
thermocouple and an optical pyrometer.
The temperatures
quoted
in Table II are precise
to f 10C within a single run and f 20C
between samples. The temperature
quoted
is derived from an average of the two monitored temperatures
over the range where
they are both accurate (700-950C),
with
extrapolations
to higher and lower temperatures
being made using the thermocouple. The accuracy of these temperatures
is probably - ?r 50C. The Ar isotopic analyses for K/Ar dating were done mainly in
an AEI@ MS10
mass spectrometer,
substantially
modified
for this purpose. The
isotopic
composition
of Ar extracted
in
each step in the 4oAr/3gAr study was measured using a VG-Isotopes@
MM1206
mass
spectrometer.

47

TABLE

II

Potassium-argon
Laboratory
No.

ages,

East

Timor
Radiogenic
(lo-*
mol

Lt.%)

40Ar
g-)

(rad.
x (total

loo

OAr)
40Ar)

Calculated
x + 1 s.d.

age (Ma)

Hornblende:
83-l 96
83-194
83-l 93
83-192
83-l 95
83-191
83-384
83-385

0.320,
0.324,
0.354,
0.343,
0.691,
0.410,
0.275,
0.461,

0.315*
0.322
0.365*
0.351*
0.690
0.419*
0.277
0.470*

7.17
8.89
6.40
8.45
35.47
49.70
26.92
16.29

36.8
15.1
34.7
40.2
63.7
72.6
60.8
29.7

13.0
15.8
10.2
14.0
29.4
67.9
55.3
20.1

2
t
i
i
t
f
*
i

0.2
0.3
0.2
0.2
0.3
1.2
0.6
0.4

5.32,
7.80,

5.25
7.80

50.6
77.0

76.3
67.0

5.51
5.68

+ 0.06
t 0.07

6.62,
7.58,

6.59
7.62

62.4
73.5

44.4
53.7

5.44
5.56

f 0.06
t 0.07

Muscovite:
83-197
83-l 98
Biotite:
83-197
83-198

a-;
h, + A; = 0.581.1O-O
*Rather
poorly
reproducible

hp = 4.962.10-
Ks.

a-;

OK/K

= 1.167*104.

4. Results
4.1. Mica
K/Ar ages have been obtained for 8 hornblendes
and 2 white
mica-biotite
pairs
(Table II). The biotite and white-mica
K/Ar
ages are in the range 5.4-5.7 Ma, and nearly
concordant.
As, in general, isotopic measurements
of coexisting
micas suggest white
mica has a 50C higher closure temperature
for Ar than biotite
(Wagner et al., 1977),
the concordant
mica ages suggest that rapid
cooling was occurring 5.5 Ma ago. Alternatively, both minerals
may have been reset
by strain-induced
recrystallization
as the
micas were strongly
recrystallized
by the
The
textural
evidence
D2 deformation.
suggest that the closure temperature
for
Ar retention
in the micas was reached after
D?. Thus K/Ar mica ages of 5.5 + 0.2 Ma

Tp=5.36t0.05

O.1
0

0.2

0.4
FRACTION

Fig.
mica.

4.

40Ar/99Ar

age

Tp is the plateau

Ma

0.6
A,

spectrum
age.

0.8

I .o

RELEASED

for

83-197

white

48

provide a minimum
estimate
for the time
since Dz ended.
The 4oAr/3QAr release pattern
of white
mica in sample 83-197 is essentially
flat
(Fig. 4), suggesting rapid cooling through
the closure temperature
for Ar. The calculated
average age over all ten steps is
5.36 f 0.05 Ma. Excluding
the last step
gives a plateau age of 5.31 Ma. The isochron
age calculated
from all ten steps using the
York (1969) method
is 5.23 f 0.13 Ma,
with an intercept of 4oAr/36Ar of 312 + 17.

4.2. Hornblende
All the K/Ar hornblende
ages are older
than those of the micas. The group-3 and -C
hornblendes
from this paper and Berry and
Grady
(1981a)
have conventional
K/Ar
ages in the range 7.7-16.5
Ma (Table II).
The spread of the K/Ar hornblende
ages
greatly exceeds that which can be accounted
for by experimental
error. This is true even
for the group-B amphibolites
which come
from a 2-km section within the high-grade
rocks and are expected to have a very similar
cooling
history.
The group-A amphibolites
have much older K/Ar hornblende
ages in
the range 20.1-67.9
Ma, and no specific
cooling age can be identified
from the results
on these four samples. Likewise, this large
spread in measured age for rocks sampled
in very close proximity
cannot be explained
by differences
in cooling history.
Because
the wide variation
in KfAr hornblende
ages
cannot be directly
interpreted
in terms of
distinct
metamorphic
events, the 4oAr/3QAr
method
was employed
on six homblendes
to provide
additional
information.
Two
samples were analyzed from group A, three
from group B and one from group C. All
the homblendes
analyzed yielded age spectra
showing high apparent ages in the early part
of the Ar release (Table III; Fig. 5), interpreted
as the result of incorporation
of
excess Ar (Harrison and McDougall,
1980).
The excess 40Ar component
has a strong

positive correlation
with the measured K/Ar
age.
The youngest hornblende
analyzed (group
B, 83-193) showed a small amount of excess
Ar in the first few percent of gas release
followed
by an essentially flat release pattern, yielding
an age of 7.5 Ma over 90%
of the gas and 8 heating steps (Fig. 5a).
This age is 2.7 Ma younger than the K/Ar
age from this mineral and is equivalent
to
the youngest K/Ar hornblende
age reported
from the Aileu Formation
(3-I-192;
Berry
and Grady,
1981a). The cumulative
total
fusion age for 83-193 is slightly less than
the total fusion and K/Ar ages (Tables II
and III), suggesting that there may be systematic errors because of the low radiogenic
Ar content and the small size of the gas
fractions.
We regard 7.5 Ma as a good estimate
for final closure of hornblende
to
diffusion of Ar in this rock.
The oldest hornblende
(group A, 83191) has a well-developed
Ar loss profile
(Fig. 6b) with a superimposed
Ar gain profile
in the early stages of gas release. For comparison,
a theoretical
loss profile
derived
from the equation of Turner (1968) is shown
and fits the data remarkably
well considering
the gross approximations
(uniform
spheres, episodic
heating)
involved
in its
application
to metamorphic
homblendes.
The
loss profile
was calculated
for an initial
closure at 67 Ma with a subsequent
20%
loss of radiogenic
Ar at 7.5 Ma, the latter
age being that of sample 83-193. The 4oAr/
39Ar age spectrum
for 83-l 93 hornblende
is most plausibly
interpreted
as indicating
virtually
complete
resetting
at - 7.5 Ma,
but the Ar loss exhibited
by hornblende
83-191 could have occurred
at any time
< 20 Ma.
Three other samples of hornblende,
83192, 83-194
and 83-l 96, have 4oAr/39Ar
age spectra that are very similar (Table III;
Fig. 5c-e).
In each case, following
high
apparent ages in the early stages of the gas
release, there is a monotonic
rise in age of
successive gas fractions,
although
for 83-

49

TABLE III
Arisotopic composition of gasextracted during step heating
Temperature, T
W)
Sample 83-191

36Ar
(X 10-l")

37Ar
(X 10-16)

39Ar
(X 10-l')

40Ar
(X 10-15)

40Ar*/40Ar X 100
WI

Apparent age(Ma)
x t 1 s.d.

579.8 t 3.1
142.6
2.0
61.2
2.0
42.3
2.3
39.0
1.0
21.5
0.9
31.3
1.1
41.2
0.5
46.6
0.6
51.1
0.5
55.2
0.4
63.1
0.3
62.8
0.4
65.0
0.4
64.3
0.4
64.4
0.9

(1.0170 g; J = 0.002344):

620
680
730
770
810
860*
900
925
960
985
1,000
1,020
1,040
1,060
1,075
1,105
1,200
Total

14,800
4,144
4,476
3,858
5,101
92,300
6,036
3,664
3,612
3,732
5,721
7,268
12,210
14,300
5,501
8,006
2,064
104,493

1,620
674
794
774
1,435
2,185
6,016
7,618
12,730
14,370
25,750
33,620
65,620
86,920
33,670
48,700
7,602
347,913

5,225
3,800
3,767
2,545
3,846
4,599
7,708
7,091
10,430
11,680
21,130
27,850
56,340
75,280
29,730
42,900
6,373
315,695

12,790
2,552
1,870
1,391
1,853
26,960
2,124
1,541
1,973
2,267
4,029
5,511
11,520
14,750
5,941
8,524
1.523

65.9
52.2
29.6
18.5
19.3
0
18.5
34.1
51.6
57.0
63.7
66.4
73.7
76.5
77.6
77.3
64.4

80,159

65.4

69.3

0.6

TF
FM
Plateau

16,490
12,110

47,350
35,620

42,710
25,160

11,580
30,680

61.5
89.4

69.7

0.4

63.5

0.4

Sample 83-192

620
710
790
870
930
950
970
990
1,010
1,030
1,050
1,080
Total
TF
FM
Sample 83-193

615
710
790
870

(1.4579

g; J = 0.002645):

10,470
11,650
39,480
32,810
14,800
5,739
4,917
6,072
6,429
5,273
8,895
12,490
___
159,025

3,346
2,770
4,110
10,710
53,560
30,710
23,070
42,920
54.950
45,720
94,590
159,100
525,556

1,887
1,162
2,174
6,024
44,760
24,160
18,070
34,080
42,830
34,970
73,540
123,300
406,957

4,552
3,833
11,910
9,821
4,931
1,948
1,607
2,098
2,370
1,938
3,597
5.413

32.7
10.9
2.3
2.2
20.9
26.9
22.3
32.5
40.3
40.4
50.1
57.8

345.7 f
120.8
60.6
17.6
11.1
10.4
9.5
9.6
10.7
10.8
11.8
12.2

9.3
11.0
9.4
2.8
0.2
0.4
0.4
0.2
0.1
0.2
0.1
0.1

54,018

21.8

13.7

iz

16,620
13,180

63,060
45,080

48,620
31,550

5,778
33,970

24.7
89.6

14.1

0.3

907
870
1,276
2,920

4,244
3,320
7,920
10,740

15.7
4.7
2.6
1.8

343.5
89.2
77.6
32.7

18.8
25.7
15.3
12.0

(1.4663 g;J= 0.002631):

12,400
10,950
26,260
35,940

9,640
8,014
5,176
8,625

50

TABLE III (continued)

Temperature, T
("C)
Sample 83-193

930
950
970
990
1,010
1,030
1,050
1,080
1,200
Total
TF
FM
Plateau
Sample 83-194

500
620
695
780
860
910
940
960
980
1,000
1,020
1,040
1,055
1,070
1,100
Total
TF
FM
Sample 83-195

630
710
780
850
900
930
950
970
990
1,010
1,035
1,055
1,070
1,085

36Ar
(x lo-'s)

3'Ar
(X 10-16)

"9Ar
(X lo-")

'OAr
(X 10-15)

40Ar*/GPArx 100
(%I

Apparent age(Ma)
x * ls.d.

(1.4663 g;J= O.O02631)(cont.):

17,730
9,143
6,776
10,920
11,680
9,240
4,135
8,347
29,580

193,101

28,980
28,540
28,630
75,940
92,040
90,520
35,880
91,280
101,700
604,965

21,640
24,030
24,680
68,110
78,540
73,230
27,510
65,270
45,750

434,733

1,536
9,460

75,080
44,780

54,190
31,120

5,344
2,803
2,113
3,597
3,886
3,113
1,307
2,770
8,542

6.8
12.6
17.2
28.8
32.1
37.9
30.8
40.1
8.3

8.0
7.0
7.0
7.3
7.6
7.7
7.0
8.1
7.4

0.7
0.5
0.3
0.1
0.2
0.1
0.3
0.2
0.5

59,699

13.Q

8.8

0.5

5,030
32,650

23.0
92.7

10.2

0.3

7.7

0.2

(1.3923 g; J= 0.002578):
4,999
7,334
19,720
41,840
34,730
16,380
15,330
8,178
5,804
7,662
4,405
6,194
7,278
6,967
5,405

876
3,231
2,574
4,095
11,450
21,240
92,950
48,210
39,320
57,190
35,470
47,690
57,660
52,050
53,250

600
1,375
$510
2,125
4,774
12,360
70,480
36,540
29,540
41,930
25,430
34,880
42,320
38,550
39,860

1,059.g
415.5
153.8
43.9
31.6
14.4
11.7
10.7
10.5
11.9
12.0
12.5
12.8
13.0
12.9

34.8
8.3
15.6
23.3
4.8
0.9
0.1
0.3
0.2
0.1
0.3
0.3
0.1
0.4
0.3

3,309
3,496
6,319
12,530
10,480
5,031
5,466
2,822
2,031
2,820
1,638
2,343
2,796
2,668
2,227

55.6
38.8
8.1
1.6
3.1
7.6
32.1
29.5
32.7
37.6
39.7
39.9
41.3
40.1
49.4

65,976

21.1

16.9

0.6

17.6

0.2

192,226

527,256

382,274

20,880
13,760

68,820
48,270

49,750
33,900

7,434
37,220

25.2
90.2

4,495
1,671
2,220
4,591
20,230
13,730
14,740
23,310
31,340
94,990
58,770
27,010
29,600
39,910

12,610
2,450
2,890
3,530
3,625
2,325
1,807
2,368
3,132
8,281
5,072
2,378
2,539
3,380

43.8
23.8
15.5
11.5
31.4
39.1
53.9
56.3
59.1
66.7
66.2
65.2
67.6
67.7

(0.8981 g; J= 0.002191):
24,330
6,498
8,361
10,740
9,026
5,169
3,194
4,049
5,023
11,120
6,861
3,295
3,318
4,418

11,680
6,005
3,262
5,443
20,320
12,730
12,680
18,590
23,310
61,200
36,600
16,870
18,400
24,690

465.6
145.9
84.4
37.3
23.8
28.0
27.9
24.2
25.0
24.6
24.2
24.3
24.5
24.2

3.4
3.8
5.2
1.6
0.5
0.4
0.6
0.3
0.3
0.1
0.2
0.3
0.2
0.2

51

TABLE
Temperature,

III

(continued)
T

(C)

37Ar
(X 10-16)

36Ar
(X lo-a)

39Ar
(X lo-)

4QAr
(X 10-15)

40Ar*/40Ar
(%I

x f s.d.

23.4

100

Apparent

Sample 83-195

1,170
Total
TF
FM
Plateau

Sample 83-196
620
710
770
840
900
940
960
980
1,000
1,020
1,040
1,060
1,080
1,100
Total
TF
FM
Plateau

(0.8981

g; J = 0.002191)

(cont.):

13,960
119,362

88,670
360,450

155,300
~
521,907

11,960

71.9

68,347

53.2

19,910
8,420

60,570
36,650

89,550
25,890

11,670
30,310

54.1
92.9

(1.3276

29.3

0.1
0.3

29.8

0.2

24.1

0.2

g; J = 0.002554):

19,030
18,720
21,240
26,750
13,120
6,866
4,824
5.132
3,718
6,866
4,990
3,398
4,636
4,883

25,120
38,190
6,704
8,656
23,520
24,620
22,050
30.920
21,550
49,440
37,360
25,480
37,170
38,020

144,173

16,670
7,190

Sample 83-l 97 (0.6249

age (Ma)

5,475
5,174
3,569
5,729
14,140
18,120
17,050
23,700
16,320
39,070
31,250
21,070
31,330
31,620

6,479
5,528
6,395
8,008
3.983
2,159
1,534
1,691
1,238
2,445
1,830
1,246
1,748
1,804

16.7
6.1
2.8
2.2
7.9
16.1
19.8
26.5
26.6
34.9
37.4
37.4
40.4
38.6

91.8
31.7
23.2
14.5
10.4
8.9
8.3
8.8
9.4
10.1
10.1
10.3
10.0
10.2

388,800

263,617

46,088

15.2

12.2

2.6
2.3
5.9
2.4
0.5
0.4
0.3
0.5
0.3
0.2
0.2
0.2
0.3
0.2
0.5

59,710
31,130

43,810
22,030

5,918
23,880

25.7
92.3

16.1

0.3

10.1

0.2

19.3
66.3
79.0
80.0
78.9
75.8
73.5
73.5
69.1
55.5

5.35
5.40
5.31
5.25
5.27
5.25
5.20
5.34
5.32
5.74

0.27
0.05
0.03
0.04
0.04
0.05
0.07
0.04
0.04
0.05

63.3

5.36

0.05

5.63

0.05

g; J = 0.002470):
39Ar
(X 10-15)

590
720
770
790
810
830
855
890
950
1,100

22,170
9,950
3,942
2,595
1,936
2,033
2,146
2,590
3,808
10.980

1,571
5,703
3,196
1,831
1,249
1,133
1,112
1,388
1,709
9,201

Total

62,150

28,093

25,334

49,334

TF
FM

8,645
14,680

3.622
147

2,873
1,496

6,235
38,140

58.3

flux
monitor;
are reported

GA1550
in moles.

TF = total
fusion
of l/8 split;
77/600
hornblende
for all other
*Not
included
in total.

1,308
4,905
3,921
2,801
1,935
1,692
1,584
1,859
2,192
3,137

FM = gas extraction
from
samples.
Gas components

8,146
8,970
5,920
4,129
2,906
2,632
2,517
3,033
3,789
7,292

biotite

for

sample

83-197

and

52

iaost2-,
18-

, ,

I , / , ,
83-192

16-

40
35
g
30
Y
<
Li
z
<
FL
c

25
20
15
10
5
0
0

0.2

0.4

0.6

0.9

1 .o

53
60

. .a.
. .

50-

P
f
8
z

.
.

0 GROUP

. GROUP
A GROUP

B
C

El

40-

.
30 .
60

presence of minor excess Ar released at the

higher temperatures
giving rise to slightly
saddle-shaped age spectra, are also consistent
with these patterns, and imply a significant
cooling event at or younger than 8 Ma.
One 40Ar/3gAr hornblende
release pattern
is inconsistent
with the interpretation
that
an - &Ma event caused Ar loss after an
original
closure at - 70 Ma. Sample 83195 produced a plateau age of 24.1 + 0.2
Ma over 8 steps and 88% of the gas release
(Fig. 5f). The data suggest a real cooling
event at - 24 Ma, but no evidence of it can
be seen in the 40Ar/3gAr spectrum of adjacent
sample 83-191
which requires partial
Ar
loss at less than 20 Ma. The other 4oAr/3gAr
spectrum cannot be used to reject the 24-Ma
plateau age as they merely imply an initial
closure age older than 13 Ma and are compatible with a first closure age of 24 Ma.
5. Discussion
5.1. KICa ratios in hornblendes

Fig. 6. Graphs of 100 X Mg/(Mg + Fe,,,d) of prograde

hornblende,
percent
clear relict hornblende
and
percent relict plagioclase against K/Ar age of hornblende.

196 the 4oAr/3gAr ages for the last 60% of

gas release are essentially concordant.
These
patterns suggest substantial
Ar loss at less
than 10 Ma, 8.5 Ma for 83-196, with partial
retention
of Ar from original closure at more
than 13 Ma. The spectra are consistent with
very large Ar losses at - 8 Ma from an initial
closure age similar to that of 83-191 (- 70
Ma). Alternative
models
of slow cooling
through
the closure temperature,
or the

The 3gAr/37Ar ratio estimated

for each
step of Ar release indicates the K/Ca ratios
of the material from which the Ar is derived.
Thus, in mixed samples it should be possible to determine
the contribution
of each
component.
The 3gAr/37Ar ratio is calibrated
against the flux monitor
77-600 which has
a K/Ca ratio of 0.0373 f 0.0001 (Harrison
and McDougall,
1981).
Five of the samples have low K/Ca ratios
in the first 5% gas release (Fig. 5). This may
be because of loss of 3gAr from the rims of
grains by recoil (Huneke,
1976) or due to
the presence of minor amounts
of plagioclase and sphene which occur as inclusions
and in composite
grains within all the samples. The exception is sample 83-191, which
has a high K/Ca ratio in the first 10% of gas

Fig . 5 . @Arla9Ar age spectrum and apparent K/Ca ratio for Aileu Formation
hornblendes.
Tp is plateau age.
Detail of early release of Ar shown in insets. K/Ca ratio from total fusion of l/8 split shown as dashed line and
average K/Ca ratio of hornblendes
from microprobe
analysis shown as dotted-and-dashed
line. Only one line is
shown in 83-192 because the two analytical methods gave the same K/Ca ratio.

54

release.
Harrison
and Fitzgerald
(1986)
have shown that some metamorphic
hornblendes exsolve submicroscopic
lamellae of
cummingtonite
which releases Ar at low temperature.
The high K/Ca ratio in the early
release fraction
of 83-191
hornblende
is
consistent
with the presence of a minor
exsolved
phase, although
no high K/Ca
phase was recognised optically
in this homblende separate.
For most of the samples the apparent
K/Ca ratio is remarkably
uniform
across
the last 90% of gas release. This occurs
despite the fact that the samples contain
a range of hornblende
compositions.
For
example,
in sample 83-194 the syn-D, and
altered prograde homblendes
have an average
K/Ca ratio of 0.034. In contrast the unaltered prograde hornblende
has an average
K/Ca ratio of 0.043. If these homblendes
are releasing Ar at different steps in the Ar
extraction
the apparent K/Ca ratio should
vary within these limits. This variation was
not observed and the apparent K/Ca ratio
determined
from the 3gAr/37Ar ratio closely
matches the average for all the hornblende,
0.041, across 95% of the gas release. Similarly, in sample 83-191 there are high-Ti homblendes with an average K/Ca ratio of 0.051
and low-Ti
homblendes
with an average
K/Ca ratio of 0.037, but the apparent K/Ca
ratio measured
from the step heating experiment
lies close to the whole-sample
average of 0.044 and only increases slightly
during release of the last 85% of the gas.
In all the steps the apparent K/Ca ratio indicates contributions
from both hornblende
components
in approximately
equal amounts
(40-70s
of the high-Ti hornblende).
The
apparent K/Ca ratio from samples 83-191 and
-194 indicates that the hornblendes
present
are degassing together. It is concluded that
the age spectra are a result of mixing
of
the radiogenic
Ar components
from the
different types of hornblende.
In two samples, however, the apparent
K/Ca ratio changes significantly
during the
Ar release. In sample 83-193 the apparent

K/Ca ratio decreases monotonically

towards
the higher-temperature
steps and is always
below the average K/Ca ratio estimated from
the
microprobe
analysis.
Conversely
in
sample 83-195 the apparent K/Ca ratio increases monotonically
towards the highertemperature
steps and only reaches the
average K/Ca value of the hornblende
in
the last step. These patterns suggest that
several phases are differentially
degassing
and that the mineral
separates contain
a
contaminating
phase with a low K/Ca ratio.
Polished
grain mounts
of these samples
were prepared, revealing that both contained
substantial
contamination
in composite
grains. The mineral
separate from 83-193
contains
5% diopside whereas the mineral
separate from 83-l 95 contains 3% plagioclase. This contamination
is compatible
with the observed variation
in K/Ca ratio
during step heating provided that plagioclase
loses Ar at lower temperature,
and diopside
at higher
temperature,
than hornblende.
The low K/Ca ratio and high Ca in these
phases adequately
explains the difference in
average K/Ca ratio of hornblende
measured
by microprobe
and the same ratio estimated
over the whole-mineral
separate from the
3gAr/37Ar ratio.
The apparent K/Ca ratio obtained
from
the step heating experiments
indicates that
the hornblende
in the mineral
separates
includes all the hornblende
types in the rock
in proportions
closely similar to those observed in the rock. In addition,
these hornblendes degas together,
under the conditions in our Ar extraction
experiments,
so that no part of the individual
40Ar/3gAr
age spectrum can be attributed
to a particular type of hornblende.
5.2. Group-B

amphibolites

The group-B
positionally
and
samples from a
main block
of
which
crystallized

amphibolites
are a comtexturally
coherent set of
2-km road section in the
the Aileu Formation
and
at upper
amphibolite

55

facies condition
during the prograde metamorphism.
Consideration
of the composition
of syn-Dz mineral assemblages in these samples indicated retrogression
at low or middle
amphibolite
facies, - 570C. As the best
available
estimate
of the closure temperature of hornblende
is 530 + 40C (Harrison,
1981), it would be expected that the groupB hornblendes
would have lost most of
their radiogenic
Ar during the Dz retrogression. The range of K/Ar ages of the group-B
amphibolites
is possibly the result of small
variations in retained pre-D, Ar or absorbed
excess Ar. Because the mineral
separates
contain a mixed population
of hornblende,
the variation
in K/Ar age may reflect the
amount
of inherited
Ar in each of these
groups. The pre-Dz hornblende
in these samples can be separated into two classes; clear,
relatively
inclusion
free and uniformlycoloured
green hornblende,
and mottled
hornblende
with abundant
inclusions.
We
interpret
the latter
hornblende
as partly
re-equilibrated
during D2 and therefore possibly more open to Ar. The proportion
of
clear,
unaltered
hornblende
in group-B
samples correlates strongly with their K/Ar
ages [correlation
coefficient
(R) = 0.861
(Fig. 6). Extrapolation
of this relationship
suggests that syn-Dz and altered
pre-D2
hornblende
has a K/Ar age of 9 Ma and unaltered pre-Dz hornblende
has a K/Ar age of
23 Ma. Because the clear pre-D, hornblende
is expected to have lost substantial
Ar during Dz, the 23 Ma is a minimum
age for
original
closure. The 7.5-Ma age for final
closure of sample 83-193
hornblende
to
diffusion
of Ar, indicated
by a direct interpretation
of the 4oAr/3gAr release pattern,
is consistent with this result.
The positive
correlation
of K/Ar
ages
with
the proportion
of unaltered
homblende is less easily explained
if the range
of age is assumed to be caused by excess
Ar. Because the altered
homblendes
are
expected
to have been more open to Ar
than the unaltered homblendes,
the greatest
amount
of excess Ar is expected
in the

samples with
the highest
proportion
of
altered
hornblende.
However, this presupposes that the Ar absorption
occurred at
the same time as the alteration.

5.3. Group-A amphibolites

The
compositions
of plagioclase
and
hornblende
that
crystallized
during
Dz
retrogression
in group-A
amphibolites
indicate lowest amphibolite
facies conditions
with temperatures
in the range 520 to
550C (Garlick and Epstein, 1967; Winkler,
1976; Plyusnina,
1982). From the analysis
of group-B amphibolites
we are confident
that this retrogression
occurred at - 8 Ma,
yet all the group-A homblendes
have much
older K/Ar apparent ages. As the retrogression occurred
at conditions
close to the
hornblende
closure temperature,
small variations in the closure temperature,
perhaps
related to compositional
factors, may cause
the range of ages. Alternatively,
the degree
of recrystallization
may be the controlling
factor,
as demonstrated
in the group-B
amphibolites.
The conventional
K/Ar age of hornblende
in the group-A amphibolites
has a strong
positive correlation
with the Mg number of
the hornblende
(R = 0.91, Fig. 6). Similar
compositional
controls have been recognized
in other regional studies (e.g., ONions
et
al., 1969) and generally
have been interpreted as indicating that Mg-rich homblendes
have a higher closure temperature
for Ar
than Fe-rich homblendes.
Surprisingly,
the
K/Ar
hornblende
age does not correlate
strongly
with the proportion
of unaltered
relict hornblende
in this group (R = 0.50)
and because there is a wide range in the
degree of alteration
(Table I) this suggests
that the retrogressed hornblende
identified
optically has retained some Ar.
The range of K/Ar ages in the group-A
amphibolites
reflects compositional
effects
on the closure temperature
and possibly
variable
recrystallization.
The K/Ar
and
40Ar/3gAr ages must be considered as mini-

56

mum estimates of the time of the prograde

metamorphism
because
all the samples
include a mixed population
of hornblende.
The classical Ar loss profile for sample 83191 and the apparent
plateau of sample
83-195 are not reliable
indicators
of the
original
cooling age as they are the result
of analyzing
mixed
populations
of hornblende.
In addition,
there is substantial
evidence that the altered hornblende
is partly open to Ar during the retrogressive phase.
Nevertheless,
the 40Ar/39Ar
spectrum
of
hornblende
from sample 83-191 indicates
a minimum
age of 70 Ma for the prograde
metamorphism.
5.4. Group-C amphibolites
The
group-C
amphibolites
are highly
variable
as they have experienced
a wide
range of metamorphic
conditions.
Sample
3-1-192 is from a high-grade
area with a
history similar to the group-B amphibolites.
This is clearly demonstrated
by the range
of plagioclase
compositions
(Fig. 3). The
low K/Ar hornblende
age of sample 3-1192 (7.7 Ma, Table I) probably
reflects its
Fe-rich composition
because 40% of the
hornblende
in this sample is apparently
unaltered pre-D2 hornblende.
The 40Ar/39Ar spectrum of 83-196 homblende is similar to that found for the groupB samples 83-192 and -194. The retrogression of sample 83-196 was at upper greenschist facies, suggesting that the temperature was too low for equilibrium
diffusional
loss to have been important
in resetting this
age. However, as 86% of the hornblende
in
this sample is heavily dusted with fine inclusions,
there is the possibility
of open
chemical system behaviour during the retrogression. Similarly,
hornblende
from sample
3-J-186
(Table
I) is heavily dusted with
inclusions,
and unaltered
prograde
homblende comprises only 1% of this separate.
The nearly complete resetting of these homblende samples is apparently
related to the
retrogression of early hornblende.

Hornblende
from sample 1-2-75 has a
K/Ar age of 10.8 Ma (Table I). The homblende in this sample is the most Fe-rich of
all those analyzed but the rock was equilibrated entirely within the greenschist facies
both before and during Dz. Sample 1-2-75
has a higher proportion
of relict clear pre-D,
hornblende
(27%) than 83-196 and 3-1-186
but has a lower K/Ar age. This may be because the Fe-rich composition
has allowed
greater diffusional
loss of Ar from the relict
clear hornblende
than the more magnesium
homblendes
of 83-196 and 3-1-186.
6. Summary
The interpretation
of K/Ar and 4oAr/39Ar
isotopic
analyses in metamorphic
rocks requires detailed consideration
of the textural
and mineralogical
relationships
in the samples studied.
Where samples containing
a
range of metamorphic
homblendes
were
analyzed, the 40Ar/39Ar spectra did not differentiate
the Ar from these different hornblende types. The presence of Ar from a
mixed population
of hornblende
cannot be
deduced from a single 40Ar/39Ar age spectrum. For example sample 83-195 contains
36% relict, 55% partly retrogressed and 9%
new hornblende
but it gives an apparent
plateau
at an intermediate
age. Variations
in K/Ca ratios estimated from the 39Ar/37Ar
ratios of each step in this study were found
to correlate with degassing of contaminating phases rather than differential
degassing
of hornblende
types.
In this study, homblendes
retrogressed
at middle
amphibolite
facies conditions
lost most of their radiogenic Ar. The lo-Ma
range in K/Ar hornblende
ages found in
these rocks is probably due to minor retention of Ar in some relict prograde Mg-rich
hornblende.
Homblendes
retrogressed
at
upper
greenschist
and low
amphibolite
facies conditions
exhibit
a wide range of
K/Ar ages. Fe-rich hornblende
was reset at
these conditions
but Mg-rich homblendes
partially
retained
radiogenic
Ar except in

57

samples where textural

and chemical
reequilibration
was extensive.
These results
support previous indications
that Ar retention in hornblende
is influenced
both by
the chemical composition
of the hornblende
and by the extent of recrystallization.
The detailed interpretation
of Ar isotope
patterns in hornblende
from the Aileu Formation indicates a reheating event and retrogression at - 8 Ma. The mica radiometric
ages
demonstrate
that
the
temperature
had
dropped
by more than 200C by 5.5 Ma
ago. The timing
of the prograde metamorphism was not accurately
determined
but
occurred at least 70 Ma ago.
Acknowledgements
We are most grateful to Mark Harrison,
Jan Wijbrans and especially to Peter Zeitler
for their
constructive
criticism
of early
versions of this paper. We thank the Australian Institute
for Nuclear Science and Engineering
for providing
a grant to support
the irradiation
of samples analysed by the
40Ar/3gAr method.
We are indebted
to the
reviewers of this paper for their detailed
and helpful reviews.
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