STUDIES IN MEDITERRANEAN ARCHAEOLOGY
VOL. XLV:12
_______________________________________________
HALA SULTAN TEKKE
12
TOMB 24, STONE ANCHORS, FAUNAL REMAINS
AND POTTERY PROVENANCE
Edited by
PAUL ÅSTRÖM AND KARIN NYS
SÄVEDALEN 2007
PAUL ÅSTRÖMS FÖRLAG
53
PROVENANCE DETERMINATION OF POTTERY FROM HALA SULTAN TEKKE USING
LEAD ISOTOPIC ANALYSIS: PRELIMINARY RESULTS1
Virginie Renson*, Jan Coenaerts**, Karin Nys**, Nadine Mattielli***,
Paul Åström**** and Philippe Claeys*
*
Dept. of Geology, Vrije Universiteit Brussel, Pleinlaan 2, B-1050 Brussels (Belgium),
Dept. of Art Sciences and Archaeology, Vrije Universiteit Brussel, Pleinlaan 2, B-1050 Brussels (Belgium),
***
Dept. Sciences de la Terre et de l’Environnement, Université Libre de Bruxelles, 50 Av. F. D. Roosevelt, B-1050
Brussels (Belgium),
****
Paul Åströms förlag, Mimersvägen 44, SE-43364 Sävedalen (Sweden)
**
1. INTRODUCTION
In pottery provenance studies, two approaches are
generally applied, namely mineralogical investigations
using petrography and chemical analyses of elemental
bulk concentrations. Although this approach led to many
interesting insights during the last decades, it remains
difficult to correlate pottery with the sources of the raw
material2. Potters levigated the clay, added temper, or
even mixed clays from different origins, consequently the
chemical composition of the paste may differ significantly
from that of the original deposits (Mommsen 2004).
The purpose of this study is to test the use of Pb isotopes
as a tracer of the pottery sources by comparing the isotopic
composition of pottery sherds with that of the surrounding
sediments. Pb isotopes are commonly used to determine
the provenance of metal artefacts or lead-rich materials
like glazes (e.g., Niederschalg et al. 2003; Wolf et al.
2003), but so far, they were not applied for the analysis of
the raw material used for pottery making.
This paper presents preliminary results of the
comparison of the mineralogy and Pb isotopic signatures
of eighteen pottery sherd samples from the Late Bronze
Age site near Hala Sultan Tekke with that of thirteen
lithological samples collected from outcrops of geological
formations in a periphery of c. 15 km around the site. The
lithologies were chosen on the basis of their potential to be
used as raw material for pottery making (Fig. 1, Table 2).
2. MATERIAL
2.1. Pottery samples
The pottery samples are taken from sherds that were found
in LC IIA to LC IIIA2 contexts in Rooms 94 and 95 S.
The following wares are present: Base-ring I, Black Slip
Wheel-made, Bucchero Wheel-made, Canaanite, Coarse
Hand-made, Coarse Wheel-made, Plain White Wheelmade, Plain White Wheel-made II, Pithos, White Painted
Wheel-made, White Painted Wheel-made III and White
Slip II (Table 3). The samples represent a selection of
pottery wares commonly found at Hala Sultan Tekke.
Samples 1a and 1b are taken from misfired sherds, and as
such are likely to be considered as local products.
2.2. Outcrop samples
The outcrop samples are composed of Holocene alluvium
and colluvium deposits (clays), Pleistocene terrace deposits
and Palaeogene marls and chalks (Fig. 1, Table 2)
3. METHOD
3.1. Mineralogy
Bulk mineralogy of the outcrop samples was assessed using
x-ray diffraction (D8 Brucker Advance diffractometer,
URAP, ULg) on unoriented powder. The samples were dried
(40°C) and crushed in an agate mortar. The main mineral
species (i.e. >5%) were identified based on x-ray patterns
using their diagnostic peaks. The intensities of these peaks
were measured and corrected using the factors proposed
by Cook et al. (1975). Sherds mineralogy and petrography
will further be characterized using microscopy observation
of thin-sections coupled with X-ray diffraction.
__________
1. This research is part of a multidisciplinary project pertaining to the study of man and paleoenvironments in Cyprus at the Vrije Universiteit Brussel
(Belgium). The authors gratefully acknowledge the support of the Research Foundation Flanders (FWO grants KN137 to Karin Nys and G.0585.06 to
Philippe Claeys) and that of the Research Council of the Vrije Universiteit Brussel (grant HOA11 to Karin Nys and Philippe Claeys).
2. For an overview of pottery provenance studies in Cyprus until 1993 see Knapp and Cherry 1994, table 1.3. For a list of subsequent studies see Table
1.
54
Fig. 1: Google Earth map with site and sample locations indicated
55
Technique
Sherd and/or clay samples
Date
Source
Raman
Spectroscopy
38 sherd samples (wares not
EC
specified) from Lapatsa Tomb
Sendova et al. 2005, 829-833.
INAA
95 samples Red Lustrous
Wheel-made ware and related
LC
wares from 7 sites in Cyprus,
Egypt and Turkey
Knappett et al. 2005, 225-259.
16 inscribed clay artefacts and
Peeling/ICP-MS/
24 clay outcrop samples from LC
ICP-AES
all over Cyprus
Goren et al. 2004, 48-75;
Goren et al. 2003, 233-255.
NAA
6 Mycenaean sherds from Hala
LC IIIA2
Sultan Tekke
Mommsen et al. 2003, 5-10.
NAA
White Slip sherd samples
samples (+ Late Roman
LBA and
Cypriote Red Slip, Cypriote
Roman
Sigiliata) and 132 clay samples
from all over Cyprus
Gomez et al. 2002, 23-36.
Thin Section/
XRD/XRF/SEM
35 White Slip sherd samples
from Palaepaphos-Terasoudhia
LC
and 20 from Cyprus Museum
(uncertain origin)
Aloupi et al. 2001, 15-26.
Thin Section /
INAA
Red Lustrous Wheel-made
Ware: Cyprus, Syria or Anatolia; LC
sherd samples from Kilise Tepe
Knappett 2000.
Thin Section
34 sherd samples of pithoi from
Alassa, Apliki, Enkomi, Hala
Sultan Tekke, Kition, MarkiLC
Alonia, Myrtou-Pighades, PylaKokkinokremnos and MorphouToumba tou Skourou
Xenophontos et al. 2000, 167182.
SEM/WDA
5 White Slip II sherd samples
from Sanida, Maroni-Tsaroukkas LC
and Aredhiou-Kolades
Gomez & Doherty 2000, 109118.
ICP-MS /ICPAES
1 terracotta figurine from the
LC III
Louvre (uncertain origin)
Karageorghis & Caubet 1998,
83-86.
NAA
412 sherd samples from pottery
LC
wares from different LC sites
Bryan et al. 1997.
ICP-AES
15 clay samples from Sanida,
LC
Kornos & Kellaki
Gomez et al. 1995, 113-118.
INAA
25 Hand Burnished Ware sherd
samples from Apliki, Enkomi, LC II-III
Hala Sultan Tekke and Kition
Robinson 1994, 113-121.
NAA
217 sherd samples: 20 LC
Neolithic
WS II and 8 clay samples from
to Roman
Kalavasos Valley
Gomez et al. 1993, 233-264.
Table 1: Cypriote Bronze Age pottery provenance studies since 1994
56
Sample
Lat. Nº
Long. Eº
Remarks
Formation/Age
1
2, 3
4, 5, 6
7, 8
9, 10
11
12
13
34°53’3.70’’
34°53’4.06’’
34°54’1.56’’
34°53’5.38’’
34°53’3.81’’
34°54’7.28’’
34°55’6.61’’
34°58’5.38’’
33°36’3.18’’
33°36’3.34’’
33°35’0.87’’
33°32’2.38’’
33°32’2.45’’
33°35’9.43’’
33°33’7.78’’
33°31’6.66’’
Clay sediment near Salt lake
Clay under marine terrasse’s gravel beds
Clay deposits
Marls and chalks
Marls and chalks
Clay deposits
Gypsum alternating with marls layers
Marls layers
Holocene colluvium and alluvium
Pleistocene marine terrasse deposits
Holocene colluvium and alluvium
Paleogene Lefkara formation
Paleogene Lefkara formation
Holocen colluvium and alluvium
Upper Miocene Kalavassos formation
Paleogene Lefkara formation
Table 2: Samples location and description
Sherd
No.
Pottery type
Context
Preliminary
context date
SH 1a
Plain White
Wheel-made,
misfired
Room 94, layer 2 below
the surface layer
LC II / III
SH 1b
Plain White
Wheel-made,
misfired
Room 94, layer 2 below
the surface layer
LC II / III
SH 2
Plain White
Wheel-made II
Room 95 S, F 10012 =
fragments of Plain White
Wheel-made II big jug in
semi-circular pit
LC IIIA2
SH 3a
Base-ring I
Room 95 S, F 10007 =
pit with mud bricks and
ochre in the eastern part
of the excavated area
Room 95 S, F 10007 =
pit with mud bricks and
ochre in the east of the
excavated area
LC IIA
SH 3b
Black Slip
Wheel-made
SH 4a
Pithos
Room 95 S, above lower
floor along west wall
LC IIIA1
SH 4b
White Painted
Wheel-made
Room 95 S, above lower
floor along west wall
LC IIIA1
SH 4c
Canaanite
Room 95 S, above lower
floor along west wall
LC IIIA1
Table 3: Overview of pottery sherd samples
LC IIA
57
Sherd
No.
Pottery type
Context
Preliminary
context date
SH 4d
White Slip II
Room 95 S, above lower
floor along west wall
LC IIIA1
SH 5
Bucchero
Wheel-made
Room 95 S, grid FMa
483, layer 3
LC IIIA1
SH 6a
White Painted
Wheel-made III
Room 95 S, grid FMc
469-470, layer A
LC IIIA2
SH 6b
Plain White
Wheel-made II
Room 95 S, grid FMc
469-470, layer A
LC IIIA2
SH 6c
Coarse Wheelmade
Room 95 S, grid FMc
469-470, layer A
LC IIIA2
SH 6d
Coarse Handmade
Room 95 S, grid FMc
469-470, layer A
LC IIIA2
SH 6e
Plain White
Wheel-made,
nozzle fragment
of lamp
Room 95 S, grid FMc
469-470, layer A
LC IIIA2
SH 6f
Plain White
Wheel-made
Room 95 S, grid FMc
469-470, layer A
LC IIIA2
SH 6g
Plain White
Wheel-made II?
Room 95 S, grid FMc
469-470, layer A
LC IIIA2
SH 6h
Plain White
Wheel-made II
Room 95 S, grid FMc
469-470, layer A
LC IIIA2
Continuation of Table 3
58
3.2. Pb isotopes
The samples were dried at 40°C and crushed in an agate
mortar under an extracting hood. The entire acid digestion
process was achieved in a class 100-laminar air flow
cabinet. About 200 mg of powder were dissolved in
closed Savilex beakers using HF-HNO3 at (130°C, 48h)
followed by evaporation, addition of HCl 6N, second
evaporation and final dissolution in HBr 0.5N. Lead
separation was performed using successive acid elution
on anionic resin (AG1-X8) column (for further details see
Weis et al. 2006).
Collected lead samples were then evaporated and
dried residues dissolved in 100 µl of concentrated HNO3,
evaporated and finally dissolved in 1.5 ml of HNO3 0,05
N. Tl was added to each sample and standard to control the
instrumental mass fractionation. Solutions were prepared
to obtain a Pb/Tl rate of 4 or 5, a signal of minimum 100
mV in the axial collector (204Pb) and to reach the Pb and
Tl concentrations of the standard (200 ppb of Pb and 50
ppb of Tl).
Pb isotopes were measured using a Multi-Collector
Inductively Coupled Plasma Mass Spectrometer (MCICP-MS) Nu Plasma (Nu 015) (ULB, Brussels). NBS981
international standard was repeatedly measured (n=57)
during the four days analyses. All the measurements
were automatically corrected according to the Tl mass
fractionation and then using sample standard bracketing
method with the recommended values of Galer and
Abouchami (1998).
The isotopic ratios of the standard are stable and the
mean values are 36.7134 ± 0.005 (2SD) for 208Pb/204Pb
ratio, 15.4964 ± 0.0019 (2SD) for 207Pb/204Pb ratio,
16.9396 ± 0.0019 (2SD) for 206Pb/204Pb ratio. These values
are in good agreement with the mean internal laboratory
measurements (n≈1000, 208Pb/204Pb = 36.7130 ± 0.012
(2SD), 207Pb/204Pb = 15.4950 ± 0.004 (2SD), 206Pb/204Pb
= 16.9393 ± 0.0044 (2SD)) and with the values measured
and published by Galer and Abouchami (1998). To control
the reproducibility, four replicates and four duplicates
were also measured (Table 5).
Quartz Plagioclase K-Feldspar Calcite Dolomite Gypsum Amphibole Clay miner. Halite
Sample 1
Sample 2
Sample 3
Sample 4
Sample 5
Sample 6
Sample 7
Sample 8
Sample 9
Sample 10
Sample 11
Sample 12
Sample 13
Trace
Trace
Present
Present
Present
Present
Present
Trace
Trace
Trace
Trace
Present
Present
Present
Present
Trace
Present
Present
Present
Abundant
Abundant
Abundant
Abundant
Major
Abundant
Major
Major
Major
Major
Abundant
Trace
Present
Trace
Trace
Trace
Trace
Trace
Abundant
Abundant
Abundant
Abundant
Abundant
Abundant
Abundant
Present
Trace
Abundant
Major
Trace
Major
Table 4: Qualitative estimations of the bulk mineralogy. Trace, < 5%; present, 5-25%; abundant, 25-65%; major, >
65% (Cook et al., 1975).
4. RESULTS
4.1. Bulk mineralogy on samples from outcrops
The results are presented in Table 4 using the qualitative
scale proposed by Cook et al. (1975). Except for sample
12 that is composed of pure gypsum, the main minerals
are calcite and clay minerals. Quartz and plagioclases are
frequent while K-feldpars, dolomite, gypsum, amphiboles
and halite are present in some samples.
4.2. Comparison outcrop – sherds based on Pb isotope signatures
207
Isotopic composition of both outcrop and pottery sherd
Pb/204Pb values and for S1, S11, S13, also distinctive
samples ranges from c. 38.47 to 39.08, 15.64 to 15.71 and
lower 206Pb/204Pb. The Pb isotopic compositions of most
18.41 to 18.93, respectively for 208Pb/204Pb, 207Pb/204Pb and
of the pottery samples fall within the range of the cluster
206
Pb/204Pb ratios (Table 5). Among the outcrop samples,
formed by outcrops S4, S5, S6, S7, S8, S9, S10, S12. Only
S4, S5, S6, S7, S8, S9, S10, S12 share a similar isotopic
sherd samples SH3a, SH3b, SH4a, SH4c and SH6e, plot
composition and cluster in a well defined region of the 206Pb/
outside this field. Sherd sample SH4c displays a distinct
204
Pb versus 207Pb/204Pb diagram (Fig. 2). The other outcrop
lower 207Pb/204Pb value while pottery samples SH3a, SH3b,
samples (S1, S2, S3, S11, S13) display characteristic lower
SH4a and SH6e display higher 207Pb/204Pb values.
59
Samples
Outcrops
S1
S1*
S2
S3
S4
S5
S6
S6*
S 6 **
S 6 **
S7
S8
S9
S 10
S 11
S 12
S 13
Sherds
SH 1a
SH 1b
SH 2
SH 2 **
SH 3a
SH 3a *
SH 3b
SH 4a
SH 4b
SH 4b *
SH 4c
SH 4d
SH 5
SH 6a
SH 6b
SH 6b **
SH 6c
SH 6d
SH 6e
SH 6f
SH 6g
SH 6h
Pb/204Pb
208
2se
Pb/204Pb
207
2se
Pb/204Pb
2se
206
Pb/206Pb
208
2se
Pb/206Pb
207
2se
38.4738
38.4747
38.8886
38.8816
38.9530
38.9614
38.9559
38.9517
38.9463
38.9568
38.9054
38.9037
38.8872
38.9168
38.5955
38.9514
38.8345
0.0032
0.0027
0.0018
0.0018
0.0019
0.0025
0.0034
0.0029
0.0024
0.0021
0.0023
0.0021
0.0023
0.0018
0.0017
0.0204
0.0021
15.6425
15.6434
15.6615
15.6596
15.6809
15.6825
15.6815
15.6800
15.6821
15.6846
15.6786
15.6823
15.6808
15.6902
15.6565
15.6887
15.6493
0.0013
0.0009
0.0007
0.0007
0.0007
0.0009
0.0013
0.0011
0.0009
0.0009
0.0009
0.0008
0.0007
0.0007
0.0008
0.0094
0.0009
18.4082
18.4091
18.8361
18.8345
18.9194
18.8808
18.9226
18.9208
18.9221
18.9333
18.8484
18.8634
18.8743
18.8545
18.5463
18.8647
18.7228
0.0014
0.0011
0.0008
0.0009
0.0009
0.0013
0.0016
0.0013
0.0010
0.0010
0.0011
0.0011
0.0010
0.0009
0.0012
0.0107
0.0012
2.09008
2.09000
2.06467
2.06437
2.05893
2.06354
2.05870
2.05870
2.05822
2.05759
2.06414
2.06231
2.06035
2.06417
2.08100
2.06421
2.07422
0.00006
0.00007
0.00004
0.00005
0.00006
0.00008
0.00056
0.00007
0.00005
0.00006
0.00007
0.00006
0.00004
0.00005
0.00005
0.00030
0.00005
0.84973
0.84972
0.83143
0.83138
0.82879
0.83056
0.82873
0.82873
0.82872
0.82837
0.83178
0.83131
0.83074
0.83216
0.84416
0.83146
0.83580
0.00002
0.00002
0.00002
0.00002
0.00002
0.00002
0.00002
0.00002
0.00001
0.00002
0.00002
0.00002
0.00001
0.00002
0.00002
0.00007
0.00002
38.9791
38.9606
38.9492
38.9301
39.0846
39.0876
39.0625
39.0395
38.9319
38.9254
38.6802
38.9910
38.9471
38.9259
38.9422
38.9517
38.9693
38.9355
38.9453
38.9210
38.9368
38.9391
0.0020
0.0023
0.0022
0.0017
0.0021
0.0195
0.0050
0.0026
0.0026
0.0021
0.0019
0.0034
0.0020
0.0020
0.0021
0.0023
0.0022
0.0026
0.0031
0.0023
0.0024
0.0022
15.6869
15.6803
15.6823
15.6814
15.7104
15.7116
15.7006
15.6989
15.6790
15.6765
15.6426
15.6784
15.6795
15.6784
15.6776
15.6796
15.6821
15.6710
15.7081
15.6844
15.6827
15.6849
0.0008
0.0008
0.0008
0.0006
0.0008
0.0007
0.0018
0.0008
0.0010
0.0008
0.0007
0.0012
0.0007
0.0007
0.0008
0.0009
0.0008
0.0009
0.0012
0.0008
0.0008
0.0008
18.9080
18.9054
18.8806
18.8644
18.8081
18.8092
18.9372
18.7823
18.8618
18.8576
18.8006
18.9219
18.8775
18.8519
18.8756
18.8791
18.8893
18.8741
18.8079
18.9311
18.8497
18.8707
0.0009
0.0010
0.0010
0.0007
0.0009
0.0008
0.0013
0.0010
0.0019
0.0010
0.0008
0.0009
0.0009
0.0010
0.0009
0.0011
0.0009
0.0010
0.0013
0.0010
0.0008
0.0009
2.06150
2.06082
2.06290
2.06372
2.07809
2.07811
2.06262
2.07853
2.06416
2.06420
2.05746
2.06051
2.06319
2.06481
2.06310
2.06319
2.06301
2.06291
2.07068
2.05591
2.06558
2.06343
0.00004
0.00005
0.00006
0.00004
0.00005
0.00005
0.00007
0.00006
0.00006
0.00005
0.00006
0.00009
0.00005
0.00005
0.00004
0.00005
0.00005
0.00005
0.00006
0.00005
0.00007
0.00005
0.82960
0.82936
0.83061
0.83125
0.83526
0.83528
0.82901
0.83577
0.83129
0.83130
0.83199
0.82850
0.83059
0.83161
0.83054
0.83048
0.83017
0.83026
0.83514
0.82844
0.83192
0.83111
0.00001
0.00002
0.00002
0.00001
0.00001
0.00002
0.00002
0.00002
0.00001
0.00001
0.00001
0.00001
0.00016
0.00001
0.00001
0.00001
0.00001
0.00001
0.00002
0.00001
0.00002
0.00001
Table 5: Pb isotopic ratios and standard deviation measured in the sherds and the outcrop samples. * means replicate,
** means duplicate.
5. DISCUSSION
The two samples from misfired Plain White Wheel-made
sherds (SH1a and SH1b, Table 3) fall clearly within the
cluster of similar Pb isotopic composition. This could
imply that during LC II / III potters at Hala Sultan Tekke
favoured a particular clay source found at close distance
(c. 7km) from the settlement. The misfired sherds were
part of a layer with mixed LC material, which precludes
a more precise time span. However, the cluster contained
other samples of Plain White Wheel-made from a LC
IIIA2 context (SH2, SH6b, SH6f, SH6g and SH6h), as well
as samples made in other wares from either a LC IIIA1
(SH4b, SH4d and SH5) or a LC IIIA2 context (SH6a,
SH6c and SH6d), indicating that at least the potters of the
LC IIIA period were using this particular clay source for
the preparation of their pottery paste. Moreover, the same
clay source seems to serve as a base not only for kindred
wares such as Plain White Wheel-made and White Painted
Wheel-made, but also for preparing the pastes of Coarse,
Bucchero and White Slip wares.
The samples SH3a (Base-ring I) and SH3b (Black Slip
Wheel-made) plotting outside the cluster, originate from
an earlier stratum dated to LC IIA. Further analyses need
to be carried out to assess whether in LC II the potters at
Hala Sultan Tekke favoured other clay sources than in LC
III. Another possibility is that these two particular types of
pottery were made from another source of raw material.
In terms of Pb isotope signatures, the Canaanite sample
(SH4c) clearly differs from the typical pottery found at the
settlement. This corroborates the fact that it is commonly
considered as an import from the Levant.
Further analyses are being carried out to further refine
these preliminary observations.
60
Fig. 2: 207Pb/204Pb vs 206Pb/204Pb biplot. Black circles: sherd (SH) samples, white diamonds: outcrop (S)
samples, grey area: isotopically homogeneous sherds, white areas: outcrop samples fields
6. CONCLUSION
These preliminary results emphasize the effectiveness
of combining mineralogy and Pb isotopes in pottery
provenance studies. A larger sampling of different
outcrops in the area of the settlement is now being
carried out. Mineralogical and Pb isotopes analyses will
be coupled with elemental geochemistry to decipher the
different pottery types and their potential raw material at a
geological formation level.
61
BIBLIOGRAPHY AND ABBREVIATIONS
AJA
American Journal of Archaeology
Aloupi et al. 1999
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Bietak, M. & Hunger, H. (eds), The White Slip Ware of Late Bronze Age Cyprus.
Proceedings of an International Conference Organized by the Anastasios G. Leventis Foundation, Nicosia, in Honour of Malcom Wiener. Nicosia, 65-73.
Bryan et al. 1997
Bryan, N., French, E., Hoffman, S. & Robinson, V., “Pottery Sources in Bronze Age
Cyprus: A Provenance Study by Neutron Activation”, RDAC, 31-63.
Cook et al. 1975
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