Kibarogluetal.2017.Srisotope NMMW

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Kibaroğlu, M., Falb, C., Hartmann, G., 2017. Application of strontium isotope
analysis to provenance studies of Early Bronze Age North-Mesopotamian
Metallic Ware. Journal of Archae...
Article in Journal of Archaeological Science: Reports · January 2017

DOI: 10.1016/j.jasrep.2017.09.024
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Journal of Archaeological Science: Reports xxx (xxxx) xxx–xxx
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Journal of Archaeological Science: Reports

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Application of strontium isotope analysis to provenance studies of Early

Bronze Age North-Mesopotamian Metallic Ware
Mustafa Kibaroğlua,⁎, Christian Falbb, Gerald Hartmannc
a
Institute for Pre- and Protohistory and Medieval Archaeology, Eberhard Karls University of Tübingen, Schloß Hohentübingen, D-72070 Tübingen, Germany
b
Institute for Archaeological Sciences, Archaeology and Cultural History of the Near East, Goethe University of Frankfurt am Main, Norbert-Wollheim-Platz 1., D-60629
Frankfurt a. M., Germany
c
GZG-Geochemie, Georg-August-Universität Göttingen, Goldschmidtstr. 1, D-37077 Göttingen, Germany
A R T I C L E I N F O A B S T R A C T
Keywords: Sr isotopic analysis was carried out on Early Bronze Age (c. 2800–2200 BCE) North-Mesopotamian Metallic Ware
Ancient ceramics and clay samples collected from south-eastern Anatolia and north-eastern Syria with a view to determining the
Archaeometry provenance of this characteristic ceramic type, in particular of its non-calcareous variant. The non-calcareous
Ceramic provenance studies and calcareous variants of North-Mesopotamian Metallic Ware, which have been defined in previous archaeo-
Cultural development
metric studies, show a clear distinction in their Sr isotopic signatures. The non-calcareous group is characterised
Early Bronze Age
by high 87Sr/86Sr ratios, whereas the calcareous variant has much lower values. The Sr isotopic signature of the
Northeastern Syria
North-Mesopotamian Metallic Ware non-calcareous group shows similarities with clay samples from the Pütürge Massif area in south-east Anatolia.
Southeastern Anatolia Combining the results of the present study with previous investigations, it is thought that the raw material used
Sr isotope analysis for the production of non-calcareous North-Mesopotamian Metallic Ware could have been originated from the
southern part of the Pütürge Massif area. Furthermore, this study proves that Sr isotope analysis is a useful tool
for the characterisation and identification of archaeological ceramic provenance.
1. Introduction 1976; Kühne and Schneider, 1988). Archaeologically, NMMW is con-

sidered to be the product of a craft tradition common to a special cul-
North-Mesopotamian Metallic Ware (NMMW; Fig. 1) is one of the tural group, displaying a high level of technological skill by the potters
most characteristic ceramic types of the Early Bronze Age in south- (Falb et al., 2014).
eastern Anatolia and northeastern Syria, dated to the period between Because of its archaeological significance for the Early Bronze Age
the Syrian Early Bronze Age II and Early Bronze Age IV A, c. in the Near East and its remarkable technological features, NMMW has
2800–2200 BCE (Falb, 2009a; Falb et al., 2014; Kibaroğlu and Falb, been the subject of numerous archaeological and archaeometric studies
2013). It is related to the cultural group characterised by a heavily (e.g. Broekmans et al., 2002, 2006, 2008; Falb, 2009a; Fitz, 1984;
fortified type of settlement, the Kranzhügel settlements in the middle of Kibaroğlu, 2008; Kibaroğlu et al., 2008; Kibaroğlu and Falb, 2013;
northern Syria (see below; Fig. 2; Falb, 2009a). The main distribution of Klenk, 1987; Kühne, 1976; Kühne and Schneider, 1988; Pruß, 2000;
NMMW is located within an extensive area between the southern Schneider, 1989; Schneider and Daszkiewicz, 2001). In earlier archae-
foothills of the Taurus Mountains in south-eastern Turkey and the re- ological studies, NMMW was thought to represent local production in
gion south of the Jebel 'Abd al-Aziz in northern Syria (Fig. 2; e.g. Falb, the alluvial region of the Jazirah, between the Euphrates and the Tigris
2009a; Kühne, 1976; Pruß, 2000). NMMW is characterised by a very rivers, and the Mardin High in the north. However, archaeometric
hard and dense fabric; as a result of the firing process at high tem- studies of examples of NMMW collected mainly from northeastern Syria
peratures, at around 1000–1100 °C, it is closely related to modern stone have demonstrated that this pottery was produced from two very dif-
ware (Fitz, 1984; Kühne and Schneider, 1988; Schneider, 1989). The ferent clay types, which are clustered according to their calcium oxide
majority of the ware is greyish in colour, although the surface colours (CaO) content into calcareous and non-calcareous chemical groups
can vary from buff over reddish-brown to grey and black, and occa- (Kühne and Schneider, 1988). The calcareous group is characterised on
sionally even bicoloured orange–grey surfaces can occur. The clay paste average by high concentrations of CaO (up to 20%), magnesium oxide
is very pure, virtually free of coarse inclusions (e.g. Falb, 2009a; Kühne, MgO (5.2 wt%), Sr (320 ppm), Cr (203 ppm) and Ni (180 ppm). In
⁎
Corresponding author.
E-mail addresses: kibaroglu@gmail.com (M. Kibaroğlu), Falb@em.uni-frankfurt.de (C. Falb), ghartma@gwdg.de (G. Hartmann).
http://dx.doi.org/10.1016/j.jasrep.2017.09.024
Received 10 July 2015; Received in revised form 9 April 2017; Accepted 27 September 2017
2352-409X/ © 2017 Elsevier Ltd. All rights reserved.
Please cite this article as: Kibaroğlu, M., Journal of Archaeological Science: Reports (2017), http://dx.doi.org/10.1016/j.jasrep.2017.09.024
M. Kibaroğlu et al. Journal of Archaeological Science: Reports xxx (xxxx) xxx–xxx
Fig. 1. Characteristic vessel types of NMMW

from several sites in northeastern Syria and
southeastern Anatolia. 1, Kurban Höyük (Algaze,
1990, plate 77R); 2, Tell Chuera (Kühne, 1976,
Fig. 2); 3, Tell Chuera (Othmann and Pruß, 1995,
173, Fig. 86.123); 4, Tell Brak (Oates, 2001, 405,
Fig. 394.82); 5, Tell Chuera (Othmann, 1995, 66,
Fig. 25.45); 6, Harran (Prag, 1970, 82, Fig. 7.37);
7, Tell Qara Quzaq (Valdéz Pereiro, 1993, 131,
Fig. 32.3); 8, Tell Qara Quzaq (Valdéz Pereiro,
1993, 131, Fig. 32.1); 9, Tell Shiyukh Tahtani
(Falsone, 1998, 52, Fig. 7.9); 10, Tell Bi'a
(Strommenger and Kohlmeyer, 1998, plate
128.4); 11, Tell Qara Quzaq (Valdéz Pereiro,
1993, 131, Fig. 33.9); 12, Tell Brak (Oates, 2001,
407, Fig. 395.104); 13, Tell Bi'a (Strommenger
and Kohlmeyer, 1998, plate 97.3); 14, Tell Brak
(Emberling and McDonald, 2001, 37, Fig. 13.4).
contrast, the non-calcareous group on average shows very low CaO northeastern Syria (Fig. 2), labelled as an ‘intermediate group’, with
(1.9%) and MgO (1.2%), low Sr (140 ppm) and Cr (103 ppm) and high about 8.5% CaO. A fourth, small, chemical group has also been dis-
Al2O3 (21.5%) contents compared with the calcareous group. The bulk tinguished by Klenk (1987) and assigned to the region of Lidar Höyük
of the samples collected from northeastern Syria in previous studies in southeastern Anatolia. In previous archaeometric studies it has been
(e.g. Falb, 2009a, 2009b; Kibaroğlu, 2008) and the new ceramic sam- demonstrated that the calcareous group of NMMW has a close chemical
ples from southeastern Anatolia (Kibaroğlu and Falb, 2013) belong to affinity with clays from northeastern Syria and it has been suggested
the non-calcareous group. In addition to these two major groups, that the vessels of this group must have been produced from local clays
Broekmans et al. (2002) have reported the presence of a third chemical in that area (Broekmans et al., 2002, 2006, 2008; Falb, 2009a;
group, distinguished within the samples from Tell Beydar (Nabada) in Kibaroğlu, 2008; Kühne and Schneider, 1988; Schneider and
2
Fig. 2. A topographic map of the study area, the distribution area of NMMW and the location of Kranzhügel settlements within the main geographical distribution of NMMW in
southeastern Anatolia and northern Syria.
Daszkiewicz, 2001). Additionally, the intermediate group is related to Falb, 2013), was re-examined using principal component analysis
the calcareous group, and is also thought to represent local production (PCA). In addition to the previous clay samples from the Pütürge re-
in northeastern Syria (Broekmans et al., 2006). gion, for this study we included new clay samples collected from the
As mentioned above, the majority of NMMW was produced from a Upper Khabur, Upper Tigris Valley and Harran Plain (Fig. 2, Table 1).
special non-calcareous clay with an element composition that is very As a second step, the 87Sr/86Sr values of the NMMW and reference
different from the typical clay deposits available in northeastern Syria. samples were interpreted in terms of provenance identification of the
Subsequently, it has been assumed that the source of the raw clay of the NMMW.
non-calcareous NMMW came from somewhere outside its core dis- Sr isotope (87Sr/86Sr) analysis is a powerful tool that has been ap-
tribution area in northeastern Syria (Broekmans et al., 2002, 2006; plied largely in the research of earth sciences (e.g. Dickin, 2005; Faure
Falb, 2009a; Kibaroğlu, 2008; Kibaroğlu et al., 2008; Klenk, 1987; and Mensing, 2005); it has also been applied successfully to the in-
Kühne and Schneider, 1988; Schneider, 1989; Schneider and vestigation of archaeological artefacts, such as vitreous materials (e.g.
Daszkiewicz, 2001). Although numerous archaeometric studies have Brems et al., 2013; Degryse et al., 2009), and human and animal re-
already been carried out, the geographical location of the raw clay mains (Slovak and Paytan, 2011). Its application in archaeological
source has long remained undiscovered, which makes it difficult to ceramic studies has been limited, although its use has increased over
answer important questions about, for example, the origin, extension, the last few years (Alex et al., 2012; Carter et al., 2011; Knacke-Loy
identity and organisation of the people who produced NMMW and its et al., 1995; Li et al., 2005, 2008; Pintér, 2005; Makarona et al., 2014,
related cultural group (Falb, 2009a; Kibaroğlu et al., 2008). In a recent 2016). In previous studies the method has been suggested as a useful
archaeometric study, based on major and trace element analysis, tool for the provenance study of archaeological ceramics (e.g. Carter
Kibaroğlu and Falb (2013) suggested that the clay sources available in et al., 2011; Makarona et al., 2016).
the Pütürge Massif area, located at the border of the main distribution
area of NMMW (Fig. 2), share compositional similarities with the non-
calcareous NMMW and, accordingly, suggested that the Pütürge Massif 2. The archaeological background
area may have provided the source of raw clay for non-calcareous
NMMW production (see also below). In order to test this result, we The cultural–historical questions behind this study arose within the
analysed 17 NMMW sherds, including both calcareous and non-cal- framework of Frankfurt University's South-East Anatolia Project
careous examples, and 22 reference clay samples using Sr isotope (SOAP). Archaeological excavations and surveys in northeastern Syria
analysis, by determining their 87Sr/86Sr ratios. The ceramic samples and southeastern Turkey have shown that during the Early Bronze Age
came from southeastern Anatolia, and the clay samples from the Upper II and IV (c. 2900–2200 BCE) particular groups of people were closely
Khabur region, Upper Tigris Valley, Harran Plain and Pütürge Massif connected by common traditions and culturally differed traits from
area (Fig. 2 and 3). The focus of this study was provenance identifica- other groups in Upper Mesopotamia at that time, across a vast settled
tion of the non-calcareous group of NMMW. As a first step, the element region between the Jebel 'Abd al-Aziz and the southern foothills of the
analysis of NMMW and the reference clay samples from the Pütürge Taurus Mountains (Fig. 2). While the northern part of the settlement
area, which have been reported in a previous study (Kibaroğlu and area was presumably mainly occupied by agricultural societies, with
small villages and only a few larger major sites, the southern part was
3
(caption on next page)
4
Fig. 3. A geological map of the study area illustrating the geographical distribution area of NMMW in southeastern Anatolia and northeastern Syria, and the location of the clay samples
analysed for Sr isotopes [the map was compiled following the geological maps of the SAR, 1986 and MTA, 2002]. Upper Tigris and Harran Plain: 1, Pliocene–Quaternary deposits; 2,
Miocene–Quaternary basaltic rocks; 3, Lower Miocene clastics and carbonates; 4, Lower Miocene limestone; 5, Oligocene evaporate sedimentary rocks; 6, Lower–Middle Eocene lime-
stone; 7, Cretaceous–Palaeocene clastic and carbonate rocks; 8, Triassic–Cretaceous limestone, radiolarite, chert and shale; 9, Silurian–Permian carbonate and clastic rocks. Upper Khabur
region: 1, Quaternary alluvial deposit; 2, Palaeogene and Neogene basalt; 3, Pliocene conglomerate, sandstone, limestone, clay, marl; 4, Upper Miocene limestone, marls, conglomerate,
sandstone; 5, Middle Miocene limestone, marls, conglomerate, sandstone, clay; 6, Oligocene–Lower Miocene limestone, sandstone; 7, Eocene limestone, marls; 8, Cretaceous limestone
interbedded with flints. Bitlis–Pütürge Massif: 1, Quaternary alluvial deposit; 2, Eocene and Miocene clastic and carbonate rocks; 3, Eocene volcanic rocks; 4, Jurassic volcanics; 5,
Mesozoic basic and ultrabasic rocks; 6, Upper Palaeozoic schist, quartzite, marble, phyllite; 7, Upper Palaeozoic–Permian marble; 8, Precambrian gneiss. T, Bitlis suture.
characterised by strongly fortified circular cities, in some cases en- of the material culture within the research area. Hence, as well as ar-
dowed with massive upper and lower city walls, called Kranzhügel chaeological and geological surveys of south-east Anatolia, the study
(Lyonnet, 1998; Meyer, 2010; Meyer and Orthmann, 2013). These large includes archaeological and geochemical analyses of samples of NMMW
and highly developed urban settlements of unusual shape and infra- (cf. Kibaroğlu, 2008; Kibaroğlu et al., 2008; Kibaroğlu and Falb, 2013).
structure, which may also have served as refuge from aggressors for the
people living in the hinterland, consisted of accurately planned and 3. Material and methods
organised functional quarters within an upper and a lower town
(Meyer, 2013; Orthmann, 1990). However, while much is known about 3.1. NMMW samples
the socio-political and economic structures, the religious concepts and
artistic expression, as well as the languages spoken and written to the A total of 127 NMMW samples, from 33 different sites in the Upper
west, south and east of the region, within the area of interest much still Tigris (n = 85 sherds) and 16 sites in the Mardin and Şanlıurfa region
remains culturally unclear. At the time, around 2400 BCE, the king- (n = 36 sherds), as well as six samples from Tepecik and Arslantepe in
doms of Ebla and Mari to the west and south, with their homonymous eastern Anatolia (Table 1), were considered for element analysis. The
capitals, played important political roles in Syria, and their political and major and trace element concentrations of these samples have been
economic influence extended to the territories up and east of the Eu- published previously in Kibaroğlu and Falb (2013) (Table 1) and
phrates and even to southern Anatolia. For example, the c. 20,000 clay therefore are not listed here.
tablets with cuneiform writing found inside the destroyed royal ar- For the isotopic analysis, we selected 22 potsherds from the NMMW
chives of the ancient city of Ebla (modern Tell Mardikh) reflect the assemblage, including both non-calcareous (n = 15) and calcareous
socio-cultural, administrative and courtly life of a flourishing Early (n = 7) chemical groups (Table 2). The potsherds consisted of examples
Bronze Age state (Astour, 1988). Similarly, thousands of written sources originating from various sites in the Upper Tigris (n = 11) and from
from Mari (modern Tell Hariri) reveal the political circumstances and sites between Mardin and Viranşehir (n = 9) in southeastern Anatolia
cultural aspects of the society, and from the kingdom of Nagar in the (Fig. 2 and 3). Two examples came from the Upper Euphrates region
Khabur region of the most north-easterly area of Syria, with its capital (see Table 2 for site names and the number of samples from each site).
of Nagar (modern Tell Brak) and administrative centre of Nabada Ceramic samples were selected after evaluation of the chemical ana-
(modern Tell Beydar), much information about the economic manage- lysis, in order to gain representative examples from both chemical
ment and administration of the state is known from cuneiform texts groups.
(Archi, 2013; Charpin, 1987; Milano et al., 2004). In contrast, because
of the lack of writing and a paucity of artistic expression, very little is 3.2. Reference clay samples
known of the cultural phenomena occurring between these political
centres. However, aside from the lack of discriminating cultural fea- In order to compare the Sr isotopic signature of the ceramics with
tures and the unusual circular shape of the settlements, there is the those of local clays, a total of 17 samples was selected from the main
special type of Early Bronze Age pottery, NMMW (Fig. 1), that is distribution area of NMMW (Fig. 2 and 3, Table 2). The samples were
widespread throughout the research area in the third millennium BC primarily considered as reference material for the element analysis
and closely related to its cultural group(s). Because of its specific (Table 3; see also table 1 in Kibaroğlu and Falb, 2013) and came from
technical characteristics, similar to modern stone ware (Fitz, 1984), this five different geological–geographical zones; the Upper Khabur area
distinctive ceramic ware represents a high technological standard and (n = 3), the Upper Tigris Valley (n = 3), the Karacadağ volcanic area
must have been a well-known, unique trademark handed down tradi- (n = 1), the Harran Plain (n = 2) and the Pütürge Massif area (n = 8).
tionally by the people connected with it. It is assumed to be a specific To obtain a fine clay paste similar to NMMW, coarse clay examples
cultural indicator of the Early Bronze Age population in the area of were first purified by levitation using distilled water in the laboratory.
research, and is therefore of great significance to archaeological and Subsequently, all clay samples were oven-fired for 24 h at a tempera-
archaeometrical studies (cf. earlier studies: Broekmans et al., 2002; ture interval between 950 and 1050 °C, to produce replica material.
Falb, 2009a, 2009b; Falb et al., 2014; Kibaroğlu, 2008; Kibaroğlu et al., Both ceramics and clay powders were then submitted to chemical and
2008; Kibaroğlu and Falb, 2013; Klenk, 1987; Kühne and Schneider, isotopic analyses.
1988; Pruß, 2000; Schneider, 1989; Schneider and Daszkiewicz, 2001).
Because for a long time the origin of the special non-calcareous clay 3.3. Major and trace element analysis
used to produce the NMMW was not clear, questions remain about the
cultural identity, origin, organisation and geographical extent of the The major and trace element composition of the ceramic and clay
settlement area of the owners of NMMW and the builders of the Early samples was determined on glassy fused beads (1.5 g sample, 7.5 g
Bronze Age circular cities, including the Kranzhügel. The inter- fluxes) using a Bruker AXS S4 Pioneer wavelength dispersive X-ray
disciplinary project SOAP, which was funded from 2009 to 2012 by the fluorescence (WD-XRF) spectrometer (Rh X-ray tube, 4 kW) at the
German Research Foundation (Deutsche Forschungsgemeinschaft, Eberhard-Karls University in Tübingen, Germany. Details of the ana-
DFG), has been focused on these questions. The project is led by Pro- lytical procedure are given elsewhere (e.g. Kibaroğlu et al., 2008;
fessor Dr. Jan-Waalke Meyer at the Institute for Archaeological Sciences Kibaroğlu and Falb, 2013).
at Goethe University Frankfurt am Main, and carried out by Christian
Falb, an archaeologist, and Dr. Mustafa Kibaroğlu, a geochemist. Both
3.4. Sr isotope measurement
archaeological and archaeometrical methods are being used to gain
information about the homogeneity, continuity and provenance/origin
The samples were prepared and analysed using the procedure
5
Table 1
Major and trace element concentrations of NMMW from the Upper Tigris Valley.
Sample Material SiO2 TiO2 Al2O3 Fe2O3 MnO MgO CaO Na2O K2O P2O5 Ba Co Cr Ni Rb Sr V Y Zn Zr Ce La Nd Sm Yb Sum
M. Kibaroğlu et al.
MW101-6 NMMW 68.9 1.3 19.7 5.1 0.01 0.9 1.2 0.12 2.5 0.09 314 13 103 114 87 163 127 45 0 322 173 49 79 10 5 100.0
MW101-7 NMMW 60.6 1.0 16.0 7.6 0.08 3.8 7.7 0.33 2.4 0.24 169 33 163 138 80 391 139 18 88 162 93 40 41 7 2 100.0
MW101-10 NMMW 61.7 1.0 19.8 7.9 0.12 2.9 4.5 0.11 1.7 0.14 234 41 156 147 65 112 159 24 74 159 101 32 49 6 3 100.0
MW104-2 NMMW 64.8 1.3 21.5 4.7 0.01 1.1 4.1 0.13 2.1 0.10 369 0 62 103 57 163 112 26 0 222 188 47 26 8 3 100.0
MW218-1 NMMW 59.5 1.1 23.2 7.3 0.03 1.5 1.9 0.18 4.9 0.16 557 11 129 120 151 191 148 34 34 212 154 52 63 6 4 100.0
MW218-2 NMMW 60.0 1.1 21.3 8.2 0.09 2.5 4.5 0.13 1.9 0.17 240 27 152 145 75 146 159 21 83 174 122 54 66 5 2 100.0
MW218-3 NMMW 63.7 0.9 18.8 7.6 0.07 2.8 4.0 0.13 1.9 0.12 189 25 137 129 69 110 138 22 74 153 106 39 44 6 2 100.0
MW218-6 NMMW 63.3 1.2 21.9 6.4 0.02 1.3 1.2 0.14 4.2 0.11 508 5 117 110 153 157 135 33 15 253 148 50 69 7 4 100.0
MW222-1 NMMW 64.5 1.3 22.3 5.7 0.01 1.1 1.3 0.16 3.6 0.09 415 0 69 110 113 132 145 37 17 241 113 41 45 10 3 100.0
MW222-2 NMMW 64.5 1.3 22.3 5.6 0.01 1.1 1.2 0.15 3.6 0.08 418 0 72 108 113 131 141 36 17 242 115 44 41 6 3 100.0
MW249-1 NMMW 62.5 1.2 22.9 6.5 0.02 1.4 1.0 0.14 4.0 0.14 512 5 120 112 152 167 139 34 16 229 155 52 74 8 4 100.0
MW249-2 NMMW 66.3 1.2 20.7 5.1 0.01 1.0 0.7 0.17 4.5 0.09 545 0 91 98 151 145 115 27 6 286 161 37 61 5 3 100.0
MW234-1 NMMW 66.8 1.3 22.2 4.6 0.01 1.1 1.2 0.13 2.4 0.10 338 3 108 84 71 156 95 17 3 244 154 47 83 7 2 100.0
MW313-1 NMMW 68.0 1.1 16.4 5.1 0.01 0.9 5.9 0.14 2.2 0.07 308 0 51 100 65 128 126 33 0 324 90 31 30 4 3 100.0
MW310-1 NMMW 66.7 1.3 21.6 4.8 0.01 1.0 1.7 0.16 2.5 0.08 262 0 61 98 77 139 127 28 0 252 101 44 32 7 2 100.0
MW318-4 NMMW 64.0 1.3 23.4 5.5 0.01 1.0 2.6 0.17 2.0 0.08 278 0 70 102 71 113 136 39 6 296 97 38 34 6 3 100.0
MW319-7 NMMW 61.9 1.3 25.5 5.7 0.01 1.1 2.0 0.12 2.2 0.09 315 10 124 87 81 129 118 28 10 268 124 40 49 4 3 100.0
MW322-1 NMMW 65.5 1.3 21.3 6.1 0.01 1.1 0.8 0.14 3.4 0.11 388 0 119 104 119 133 117 21 6 268 145 38 51 7 2 100.0
MW329-2 NMMW 62.5 1.2 20.5 7.7 0.02 1.2 2.1 0.16 4.3 0.10 516 9 118 112 128 147 136 30 27 263 151 40 62 8 3 100.0
MW329-3 NMMW 62.6 1.2 21.6 6.8 0.03 1.4 1.7 0.17 4.4 0.10 475 11 123 128 136 132 126 29 18 228 136 45 61 0 3 100.0
MW536-1 NMMW 66.9 1.3 21.7 5.0 0.01 1.0 1.4 0.13 2.3 0.08 329 23 104 108 69 146 112 26 4 266 149 42 65 2 3 100.0
MW536-2 NMMW 61.6 1.3 24.1 6.0 0.01 1.4 1.4 0.16 3.8 0.09 414 29 125 102 144 141 138 25 47 237 150 46 55 6 3 100.0
MW500-1 NMMW 62.4 1.3 23.6 5.9 0.01 1.3 2.5 0.13 2.6 0.10 335 15 124 122 91 129 135 31 6 279 127 39 62 9 3 100.0
MW500-3 NMMW 65.1 1.2 20.4 4.8 0.01 1.2 1.8 0.19 5.0 0.08 517 24 92 92 125 104 111 32 24 267 138 26 56 8 4 100.0
MW505-1 NMMW 64.3 1.3 22.1 6.1 0.02 1.3 1.0 0.16 3.6 0.09 413 10 124 93 131 135 127 26 25 253 124 37 52 5 3 100.0
6
MW510-1 NMMW 62.9 1.2 22.1 7.0 0.01 1.1 1.0 0.16 4.2 0.07 478 14 118 123 131 112 129 25 16 235 115 30 53 9 3 100.0
MW510-3 NMMW 66.3 1.3 21.2 5.3 0.01 1.1 2.3 0.13 2.1 0.09 286 12 107 106 66 157 119 25 4 266 166 51 58 11 2 100.0
MW532-1 NMMW 63.4 1.3 22.8 5.4 0.03 1.5 2.8 0.15 2.4 0.10 356 12 125 96 85 136 119 29 38 266 128 34 52 7 3 100.0
MW532-2 NMMW 59.0 1.2 24.4 7.3 0.01 1.3 2.8 0.16 3.7 0.10 399 32 127 114 127 138 143 34 19 219 162 50 66 8 4 100.0
MW532-3 NMMW 61.8 1.3 25.5 5.3 0.01 1.0 2.5 0.12 2.2 0.09 292 12 111 99 78 137 114 27 3 253 101 33 47 7 3 100.0
MW537-1 NMMW 68.1 1.5 20.2 4.3 0.01 0.7 3.5 0.11 1.2 0.09 200 8 96 105 36 117 101 34 0 340 141 20 52 5 3 100.0
MW539-1 NMMW 63.6 1.2 22.3 6.1 0.01 1.2 0.8 0.14 4.4 0.10 478 9 108 120 140 156 135 29 17 253 152 38 61 7 3 100.0
MW539-2 NMMW 60.4 1.1 21.1 7.6 0.03 1.9 2.7 0.16 4.6 0.19 571 15 130 118 170 150 148 35 43 245 141 41 60 5 4 100.0
MW539-3 NMMW 63.3 1.3 22.9 7.0 0.03 1.3 1.3 0.19 2.4 0.08 426 16 143 98 96 120 138 28 22 277 123 28 52 8 3 100.0
MW539-4 NMMW 61.5 1.2 22.4 7.5 0.02 1.4 1.4 0.17 4.2 0.11 545 13 123 110 157 165 143 57 23 231 147 46 60 8 7 100.0
MW541-1 NMMW 60.7 1.2 22.9 6.6 0.02 1.3 3.4 0.17 3.3 0.13 391 34 120 115 110 145 134 32 33 236 158 42 71 10 3 100.0
MW544-3 NMMW 63.1 1.3 22.0 5.8 0.01 1.2 3.0 0.14 3.3 0.10 395 6 110 98 116 155 125 21 9 256 117 28 45 4 2 100.0
MW546-2 NMMW 68.7 1.4 19.6 4.5 0.01 0.9 1.9 0.13 2.3 0.45 313 0 110 123 65 108 102 33 0 369 139 18 71 7 3 100.0
MW548-1 NMMW 62.2 1.3 23.5 6.7 0.02 1.3 0.8 0.12 3.7 0.22 488 13 128 119 166 167 148 38 16 232 161 51 69 9 5 100.0
MW548-2 NMMW 61.4 1.2 22.3 7.7 0.02 1.4 1.3 0.14 4.3 0.15 527 7 125 126 150 159 137 41 22 261 159 44 63 0 5 100.0
MW548-3 NMMW 60.5 1.2 22.5 7.9 0.03 1.5 1.1 0.14 4.7 0.26 661 10 123 136 181 168 146 33 31 242 163 42 64 11 4 100.0
MW548-4 NMMW 61.8 1.2 22.0 7.7 0.02 1.4 1.2 0.14 4.2 0.13 573 5 130 118 148 163 132 37 18 265 152 42 77 7 4 100.0
MW549-3a NMMW 60.0 1.1 21.3 8.2 0.09 2.5 4.5 0.12 1.9 0.16 253 29 146 143 77 137 166 25 85 174 134 45 56 6 3 100.0
MW647-2 NMMW 63.6 1.1 19.5 6.4 0.02 1.4 2.6 0.16 4.8 0.21 588 11 110 167 140 174 124 40 18 306 177 41 70 7 4 100.0
MW647-3 NMMW 63.5 1.1 19.5 7.1 0.02 1.1 2.7 0.14 4.2 0.33 506 25 105 145 124 177 135 41 11 290 153 42 65 8 4 100.0
MW312-1 NMMW 70.0 1.5 18.1 5.1 0.01 1.0 1.9 0.18 2.1 0.08 241 0 56 106 74 123 144 45 0 356 96 39 37 9 4 100.0
MW311-1 NMMW 64.4 1.3 22.3 6.1 0.01 1.2 1.1 0.13 3.2 0.16 423 0 71 102 111 121 159 30 13 253 88 29 33 5 3 100.0
MW323-1 NMMW 64.1 1.3 23.5 5.6 0.01 1.0 1.1 0.13 3.0 0.13 341 5 111 118 94 139 114 29 8 307 161 38 60 0 3 100.0
MW323-2 NMMW 61.0 1.2 22.9 7.5 0.01 1.4 1.0 0.13 4.5 0.17 565 2 123 110 160 180 149 43 27 201 178 49 82 8 5 100.0
MW323-4 NMMW 64.4 1.2 22.1 5.9 0.01 1.2 0.7 0.13 3.9 0.14 442 0 114 103 129 125 123 22 15 249 139 37 59 0 2 100.0
MW542-1 NMMW 73.5 1.4 15.5 5.0 0.02 0.8 1.7 0.25 1.5 0.09 177 5 86 118 45 96 114 45 0 405 167 34 76 6 4 100.0
MW542-2 NMMW 65.7 1.1 16.7 6.5 0.02 1.2 5.2 0.16 3.2 0.10 417 4 99 124 95 138 117 32 5 325 150 31 64 6 3 100.0
MW 542-3 NMMW 63.6 1.3 22.4 6.4 0.02 1.3 0.9 0.19 3.7 0.09 469 1 120 134 128 152 112 22 10 266 154 47 83 5 2 100.0
MW542-4 NMMW 65.0 1.5 23.2 5.2 0.01 1.0 1.8 0.12 1.9 0.09 280 7 126 125 61 206 117 29 11 302 176 53 71 7 3 100.0
(continued on next page)
Table 1 (continued)
Sample Material SiO2 TiO2 Al2O3 Fe2O3 MnO MgO CaO Na2O K2O P2O5 Ba Co Cr Ni Rb Sr V Y Zn Zr Ce La Nd Sm Yb Sum
MW543-1 NMMW 65.5 1.2 20.6 6.0 0.02 1.2 1.5 0.16 3.6 0.12 428 2 134 118 119 130 124 23 12 265 136 39 49 0 2 100.0
MW543-2 NMMW 63.9 1.2 21.3 6.5 0.02 1.1 1.2 0.15 4.2 0.14 550 2 112 113 127 149 125 26 15 255 138 34 61 6 3 100.0
MW543-3 NMMW 66.0 1.3 23.0 4.9 0.01 1.1 1.0 0.12 2.3 0.09 237 3 108 96 69 139 110 23 0 245 167 45 69 7 2 100.0
MW543-4 NMMW 67.5 1.3 21.6 4.3 0.01 1.0 0.8 0.12 3.1 0.07 353 0 92 93 88 106 102 24 0 293 139 27 52 0 2 100.0
MW297-3 NMMW 62.5 1.3 22.4 6.4 0.03 1.6 0.8 0.22 4.4 0.21 532 30 141 164 168 155 146 36 24 270 168 46 81 8 4 100.0
MW297-4 NMMW 57.8 1.3 22.8 7.0 0.02 1.6 6.9 0.15 2.3 0.08 350 7 122 146 100 127 142 24 26 271 123 31 53 7 2 100.0
MW297-7 NMMW 69.3 1.3 20.1 4.5 0.01 1.0 0.9 0.11 2.6 0.07 323 0 94 94 73 124 103 26 0 301 151 39 56 8 3 100.0
MW297-8 NMMW 59.4 1.3 23.8 7.2 0.02 1.6 1.1 0.22 4.9 0.15 576 24 140 192 209 194 158 39 32 290 179 59 77 10 5 100.0
MW307-1 NMMW 60.2 1.2 23.0 8.4 0.01 1.4 1.2 0.18 4.0 0.11 521 0 84 99 163 161 175 61 25 197 142 59 51 10 6 100.0
MW297-9 NMMW 62.0 1.2 21.1 6.9 0.02 1.4 1.5 0.21 5.2 0.32 599 0 113 120 160 177 120 31 28 225 163 44 82 6 4 100.0
MW296-1 NMMW 62.7 1.1 21.1 6.4 0.02 1.5 2.0 0.19 4.5 0.36 689 0 90 117 124 214 173 36 38 235 136 55 50 9 3 100.0
MW298-1 NMMW 68.4 1.3 20.4 5.0 0.01 1.0 1.4 0.11 2.1 0.07 370 0 61 91 64 125 131 30 5 264 109 42 36 5 3 100.0
MW299-1 NMMW 64.1 1.2 21.0 6.2 0.01 1.1 2.8 0.14 3.3 0.12 419 0 61 102 95 130 135 30 12 241 103 37 42 7 3 100.0
MW301-1 NMMW 59.8 1.2 22.5 7.7 0.01 1.4 2.3 0.18 4.7 0.11 548 0 68 108 167 166 169 40 32 207 119 46 48 9 4 100.0
MW302-1 NMMW 65.9 1.3 21.6 5.5 0.01 1.1 2.0 0.13 2.3 0.09 261 0 64 107 67 175 142 37 3 294 131 51 44 7 3 100.0
MW305-1 NMMW 64.4 1.2 21.6 5.3 0.01 1.2 1.2 0.19 4.4 0.37 582 0 63 106 131 137 144 37 19 264 114 37 43 7 3 100.0
MW306-1 NMMW 66.4 1.3 21.4 5.2 0.01 1.2 2.2 0.15 2.0 0.08 330 0 62 107 65 154 130 31 6 262 132 53 40 7 3 100.0
MW309-1 NMMW 65.6 1.1 18.5 6.5 0.01 1.2 2.6 0.19 3.9 0.18 419 0 67 114 108 119 139 30 20 252 80 35 28 6 3 100.0
MW215-1 NMMW 65.5 1.3 21.3 6.6 0.01 1.2 0.6 0.14 3.1 0.09 360 0 82 118 113 112 148 33 50 295 80 24 26 4 3 100.0
MW224-2 NMMW 70.6 1.4 16.1 4.5 0.01 1.0 3.7 0.18 2.4 0.09 290 0 55 108 78 128 127 45 2 353 101 34 45 6 4 100.0
MW221-6 NMMW 65.1 0.9 18.7 7.7 0.05 2.7 2.5 0.20 1.9 0.15 162 9 88 124 73 103 160 29 83 153 83 34 29 5 3 100.0
MW050-1 NMMW 62.5 1.4 25.1 6.4 0.02 1.0 1.4 0.13 1.8 0.08 299 0 106 177 77 144 137 31 16 362 345 49 160 0 0 100.0
MW78-1 NMMW 64.3 1.4 23.0 5.3 0.16 1.0 1.4 0.13 2.4 0.70 301 0 0 25 82 123 90 31 0 283 282 28 133 3 0 100.0
MW 84-2 NMMW 62.7 1.3 22.4 6.7 0.02 1.2 0.8 0.16 4.4 0.11 497 0 181 172 143 179 133 23 14 232 275 41 142 0 2 100.0
MW101-4 NMMW 54.6 1.1 13.3 7.6 0.09 7.1 12.9 0.46 2.5 0.25 162 4 199 212 64 536 164 25 81 145 82 39 24 4 2 100.0
MW101-5 NMMW 59.1 1.0 15.4 7.2 0.08 4.1 10.2 0.29 2.2 0.30 140 0 125 151 66 388 145 26 64 136 158 38 32 4 3 100.0
7
MW101-8 NMMW 56.5 1.0 14.3 7.6 0.10 6.1 11.2 0.34 2.4 0.24 128 34 264 181 68 321 152 17 86 147 79 30 45 6 2 100.0
MW104-1 NMMW 55.4 1.0 14.8 7.7 0.10 6.2 11.4 0.76 2.1 0.30 163 0 218 177 54 306 174 23 61 114 107 26 11 4 2 100.0
MW 218-4 NMMW 61.0 1.0 15.9 6.9 0.09 3.6 8.7 0.32 2.2 0.27 154 22 162 155 67 365 117 17 72 199 116 38 57 0 2 100.0
MW218-5 NMMW 60.9 1.0 15.8 7.6 0.10 3.7 8.0 0.32 2.3 0.20 153 26 169 169 75 387 133 20 89 168 114 39 49 7 2 100.0
MW219-1 NMMW 56.9 1.0 14.6 7.6 0.08 5.7 11.2 0.30 2.3 0.23 104 10 172 178 69 349 168 26 93 150 70 32 24 13 2 100.0
MW223-1 NMMW 53.2 0.9 16.5 8.3 0.12 6.2 10.5 1.07 2.8 0.21 572 9 181 208 91 217 186 32 98 149 80 28 28 5 3 100.0
MW223-2 NMMW 54.6 0.9 17.1 7.9 0.12 5.1 9.5 1.11 3.3 0.27 707 7 166 158 94 239 177 38 124 177 94 34 33 7 3 100.0
MW225-1 NMMW 55.5 1.0 14.0 7.5 0.10 6.6 12.3 0.37 2.2 0.24 123 12 214 188 65 274 168 28 90 146 68 30 24 5 2 100.0
MW225-2 NMMW 57.0 1.1 14.8 8.1 0.09 7.4 8.5 0.29 2.3 0.30 127 13 213 211 68 231 170 28 96 152 77 25 26 3 2 100.0
MW316-1 NMMW 55.2 1.0 15.2 8.3 0.13 5.8 10.4 1.52 2.1 0.25 287 6 348 258 55 257 166 31 76 159 79 22 24 4 2 100.0
MW314-1 NMMW 56.3 1.1 14.1 7.8 0.09 5.9 11.0 0.38 2.5 0.69 205 0 202 195 65 339 171 25 83 143 80 34 27 5 2 100.0
MW318-1 NMMW 55.4 1.1 13.9 7.5 0.08 5.2 13.8 0.41 2.2 0.26 148 0 175 188 65 305 170 24 84 143 78 27 29 5 2 100.0
MW318-2 NMMW 55.1 1.0 13.8 7.3 0.08 6.3 13.6 0.39 2.1 0.21 125 0 173 188 63 244 165 24 79 137 70 24 21 8 2 100.0
MW318-3 NMMW 57.5 1.0 14.4 7.6 0.07 6.2 10.0 0.36 2.4 0.33 119 0 164 179 67 316 169 27 86 145 87 31 22 7 2 100.0
MW318-5 NMMW 59.7 1.0 15.0 7.5 0.08 3.8 9.9 0.35 2.2 0.24 188 0 130 154 72 345 152 26 81 156 92 38 27 7 2 100.0
MW318-6 NMMW 53.7 1.0 13.6 7.5 0.09 6.6 14.4 0.33 2.4 0.27 121 0 185 186 61 250 174 24 86 136 76 27 24 4 2 100.0
MW319-6 NMMW 53.3 1.0 14.1 8.3 0.11 7.1 12.8 0.42 2.4 0.24 156 36 290 190 70 297 158 19 95 160 99 25 54 7 2 100.0
MW 329-1 NMMW 55.4 1.2 14.2 8.8 0.11 7.5 9.7 0.28 2.4 0.28 160 40 281 274 62 279 144 18 87 150 88 32 44 0 2 100.0
MW536-3 NMMW 56.4 1.1 13.9 8.1 0.10 6.4 10.9 0.29 2.4 0.25 161 63 286 243 63 267 151 20 98 149 94 24 35 5 2 100.0
MW536-4 NMMW 55.4 1.0 14.0 7.7 0.10 6.8 11.8 0.24 2.4 0.30 143 34 251 222 66 283 148 19 89 144 89 28 39 3 2 100.0
MW506-1 NMMW 53.5 1.0 13.6 7.8 0.11 7.3 13.7 0.45 2.2 0.24 143 35 298 173 62 306 158 19 88 148 80 31 41 6 2 100.0
MW507-1 NMMW 55.5 1.0 14.0 7.5 0.10 6.4 12.5 0.33 2.2 0.24 139 33 263 191 64 278 155 17 85 141 77 23 37 8 2 100.0
MW509-1 NMMW 54.3 1.0 13.5 8.0 0.11 6.0 13.6 0.61 2.5 0.19 154 31 272 76 72 495 141 17 95 159 100 41 38 7 2 100.0
MW509-2 NMMW 60.1 1.0 15.8 7.4 0.09 3.8 8.8 0.34 2.3 0.25 217 33 179 167 74 410 140 18 85 155 110 43 39 7 2 100.0
MW510-2 NMMW 54.9 1.1 13.9 7.6 0.10 6.6 13.1 0.21 2.2 0.23 125 33 247 193 66 308 159 18 95 145 82 28 38 2 2 100.0
MW513-1 NMMW 54.3 1.0 13.2 7.2 0.10 5.7 15.2 0.37 2.4 0.23 224 35 250 196 67 645 148 14 84 164 89 38 44 3 1 100.0
MW513-2 NMMW 52.9 1.0 13.5 8.3 0.11 6.6 14.2 0.36 2.5 0.32 184 38 261 180 69 322 153 23 98 166 104 34 43 0 2 100.0
MW513-3 NMMW 55.2 1.1 13.8 7.8 0.10 5.4 13.5 0.46 2.2 0.27 226 30 269 186 66 315 160 19 88 154 83 27 37 3 2 100.0
MW532-6 NMMW 60.8 1.0 15.7 7.5 0.09 3.7 8.3 0.27 2.3 0.20 213 35 187 169 75 253 137 19 84 155 100 33 39 5 2 100.0
described by Mamani-Huisa (2006). One hundred milligrams of powder
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
Sum
from each ceramic and clay sample were digested using a pressure di-
gestion system in a closed PFA/Savilex beaker, under high pressure
Yb
with an acid mixture of double-distilled nitric acid (HNO3) and hy-

2
2
2
3
1
2
3
2
2
2
2
2
2
2
0
1
1
2
drofluoric acid (HF) at a temperature of 200 °C. Separation of Sr was
Sm
performed on columns filled with the cation exchange resin AG 50W-X8

6
9
5
6
0
0
5
4
0
6
6
4
5
5
0
5
4
0
with 2.5 M hydrochloric acid (HCl). After separation, the samples were
115
100
129
Nd
44
46
49
57
49
52
34
55
55
27
24
27
26
38
63
evaporated to dryness and redissolved in 0.3 mol/l HNO3. A fraction of
this solution containing approximately 150 ng Sr was mounted on a
41
30
39
26
29
32
35
45
37
37
36
38
39
37
44
45
39
36
La
preheated Re single filament. The isotopes of Sr were analysed by

thermal ionisation mass spectrometry (TIMS) using a Finnigan Triton
112
102
110
103
120
212
189
287
97
97
94
97
91
87
93
89
88
72
Ce
mass spectrometer at the Geowissenschaftliches Zentrum Göttingen,

Dept. of Isotopengeologie, Germany. Sr analyses were corrected for
174
160
167
209
141
171
234
160
150
157
156
160
158
157
144
130
146
251
mass fractionation by normalising to 88Sr/86Sr = 8.375209. Repeated
Zr
measurements of the standard NBS987 during the period these analyses

128
103
112
were carried out gave an average value of 0.710244 + 7 (2SD, n = 20).
Zn
97
79
80
65
91
93
88
91
87
90
90
93
83
74
77
The blank was negligible, varying for Sr between 100 and 200 pg.
22
20
18
29
16
21
38
17
18
27
26
27
28
27
12
12
30
Y
4. Sr isotope system
132
129
139
148
137
147
173
134
158
156
151
155
154
151
139
132
139
156
V
Sr (Z = 38) is an alkaline earth element with ionic radius 1.13 Å. It

410
297
312
166
295
317
343
381
246
361
314
368
384
307
537
529
393
426
has four naturally occurring isotopes (84Sr, 86Sr, 87Sr and 88Sr), three of
Sr
which are non-radiogenic (84Sr, 86Sr and 88Sr). The 87Sr isotope
(7.040%) is radiogenic and is a daughter isotope produced by the decay
Rb
80
77
76
70
64
78
75
77
69
73
74
76
75
71
77
63
72
89
of the parent isotope 87Rb, with a half-life of approximately

4.88 × 1010 years (Capo et al., 1998; Faure and Mensing, 2005). The
201
180
160
139
200
240
211
165
180
163
153
158
158
177
144
132
174
297
Ni
parent element Rb (Z = 37) is an alkali and a large-ion lithophile; its

ionic radius (1.52 Å) is similar to that of K (1.38 Å). Rb occurs in
206
187
173
239
268
262
371
171
268
128
117
120
128
146
169
132
299
96
Cr
highest abundance in K-bearing minerals such as muscovite, biotite,

alkali feldspars (orthoclase and microclines), and thus granitic rocks,
Co
37
32
24
20
28
30
10
26
29
10
11
8
9
0
0
0
0
clays (illite) and evaporates (Capo et al., 1998). The main source of Sr
isotopic ratios in soils and sediments is the chemical weathering of si-
191
150
191
483
138
244
642
163
260
137
148
136
129
164
181
211
159
430
Ba
licate and carbonate rocks in their drainage basins, with minor con-
tributions from other lithologies, such as evaporates (Tripathy et al.,
P2O5
0.22
0.34
0.25
0.20
0.42
1.27
0.19
0.43
0.27
0.19
0.26
0.19
0.20
0.22
0.28
0.20
0.22
0.24
2011). The major factors defining the naturally occurring Sr isotopic

ratios are (i) the 87Sr/86Sr value at the time the rock crystallised (the
initial 87Sr/86Sro), (ii) the Rb/Sr ratios of each mineral in the suite, and
K2O
2.5
2.4
2.4
2.5
2.4
2.8
2.1
2.3
2.5
2.2
2.3
2.2
2.3
2.6
2.5
2.0
2.3
2.5
(iii) the age of the parent rocks.

Rb is an incompatible element and enriched in silica-rich igneous
Na2O
0.36
0.32
0.30
1.34
0.31
0.25
0.87
0.31
0.20
0.43
0.28
0.37
0.34
0.45
0.45
0.43
0.33
1.04
systems (e.g. in granitic and granodioritic rocks), where it substitutes

principally for K in K-bearing minerals, such as K feldspar and mica,
10.5
14.1
13.6
10.1
17.9
10.9
18.1
CaO
whereas Sr is relatively compatible and preferentially substitutes for Ca

8.3
8.5
9.3
7.2
7.5
9.4
9.8
9.0
8.7
9.8
9.3
sites in plagioclase (White, 2015). For example, mantel-derived rocks,

such as basalt, have a lower Rb/Sr ratio than the silica-rich rocks from
MgO
4.2
3.9
3.9
4.0
6.1
6.0
4.1
3.7
7.5
3.8
3.6
3.9
3.8
4.0
3.8
4.3
4.5
5.4
the continental crust (White, 2015). As a result, minerals with a high K/

Ca ratio develop more radiogenic Sr over time. Thus, in a rock suite
MnO
0.11
0.08
0.08
0.13
0.11
0.12
0.06
0.08
0.09
0.08
0.08
0.08
0.07
0.09
0.08
0.09
0.09
0.17
with minerals of the same age, those with high Rb and low Sr content
(e.g. biotite and muscovite) will have higher 87Sr/86Sr ratios compared
with minerals with low Rb and high Sr content (e.g. plagioclase and
Fe2O3
7.7
7.4
7.5
6.9
7.4
8.4
7.2
7.6
8.2
7.3
7.2
7.5
7.5
7.4
6.9
6.7
7.3
8.3
apatite). When the system remains closed with respect to Rb and Sr

elements, the amount of 87Sr in a rock increases with time as radio-
active 87Rb decays to 87Sr, while the amount of other Sr isotopes re-
Al2O3
14.7
15.4
15.6
15.8
13.8
13.5
16.1
16.0
14.3
15.3
15.7
15.3
16.0
15.0
15.1
13.4
14.8
13.8
mains constant. Therefore, older rocks will have higher 87Sr/86Sr ratios
than younger rocks with the same initial Rb/Sr ratio (Capo et al., 1998).
TiO2
The highest 87Sr/86Sr values are found in very old rocks with high Rb/
1.0
1.0
1.0
0.9
1.0
1.1
1.1
1.0
1.1
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
Sr ratios, such as granites and shales, while younger rocks and minerals
with low Rb/Sr ratios have correspondingly low 87Sr/86Sr ratios (Capo
SiO2
58.6
60.8
60.3
58.7
54.2
52.9
60.9
61.0
56.3
59.8
59.5
60.2
59.9
59.4
60.4
53.7
58.5
49.1
et al., 1998; Faure, 1977; White, 2015).

The 87Sr/86Sr ratio of sea water is homogeneous at any given time
Material
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
NMMW
because of the long residence time in the ocean, which is longer than
the oceanic mixing time (Veizer, 1989). Thus, the Sr ratio of marine
Table 1 (continued)
carbonates is identical to that of the sea water at the time of its sedi-
mentation. The Rb concentration is very low relative to Sr in carbonate,
MW 546-1
MW538-1
MW544-2
MW549-2
MW647-1
MW647-4
MW226-1
MW542-6
MW297-5
MW221-2
MW221-3
MW221-4
MW220-1
MW220-2
MW218-7
MW297-1
MW550-1
MW550-3
phosphate and sea water (c. 0.1 ppm). Accordingly, the addition of
Sample
radiogenic 87Sr originating from the decay of 87Rb is negligible. The

87
Sr/86Sr ratios of sedimentary carbonates show variation throughout
8
Table 2
87
Sr/86Sr values of NMMW and clay samples from northeastern Syria and southeastern Anatolia.
Sample Material Site/location GPS coordinates 87Sr/86Sr 2se CaO (wt%) Sr (ppm)
MW500-1 Non-calcareous NM-Metallic Ware Üçtepe 37°49′34.66″N 40°32′24.15″E 0.72 0 2.5 129
MW532-3 Non-calcareous NM-Metallic Ware Pir Hüyesin 38°6′37.81″N 40°23′17.46″E 0.72 0 2.5 137
MW510-1 Non-calcareous NM-Metallic Ware Gre Hetek 37°57′30.87″N 40°48′37.16″E 0.73 0 1.0 112
MW322-1 Non-calcareous NM-Metallic Ware Gültepe 37°51′38.88″N 40°48′16.22″E 0.73 0 0.8 133
MW539-1 Non-calcareous NM-Metallic Ware Gre Kemal 37°54′1.20″N 40°27′36.06″E 0.72 0 0.7 156
MW539-2 Non-calcareous NM-Metallic Ware Gre Kemal 37°54′1.20″N 40°27′36.06″E 0.73 0 2.7 150
MW 329-2 Non-calcareous NM-Metallic Ware Koğuk 37°44′33.13″N 40°43′24.08″E 0.73 0 2.1 147
MW542-1 Non-calcareous NM-Metallic Ware Çıldız 37°15′14.86″N 40°15′49.49″E 0.72 0 1.7 96
MW323-4 Non-calcareous NM-Metallic Ware Tel Bisim 37°20′36.30″N 40°16′9.06″E 0.73 0 0.7 125
MW543-1 Non-calcareous NM-Metallic Ware Şeyhtacdin 37°14′51.90″N 40°37′40.20″E 0.73 0 1.5 130
MW50-1 Non-calcareous NM-Metallic Ware Tel Cafer 37°18′43.53″N 39°45′19.21″E 0.72 0 1.3 144
MW84-2 Non-calcareous NM-Metallic Ware Kavurga 37°4′44.01″N 39°50′30.53″E 0.73 0 0.8 179
MW78-1 Non-calcareous NM-Metallic Ware Tel Tarik 37°13′48.69″N 39°53′26.37″E 0.72 0 1.4 123
MW297-1 Calcareous NM-Metallic Ware Grekoriye 37°8′43.08″N 40°30′49.21″E 0.71 0 17.9 529
MW218-7 Calcareous NM-Metallic Ware Salat Tepe 37°50′21.94″N 40°54′6.08″E 0.71 0 9.3 537
MW550-1 Calcareous NM-Metallic Ware Karatepe 37°2′25.05″N 39°44′15.40″E 0.71 0 10.9 393
MW550-3 Calcareous NM-Metallic Ware Karatepe 37°2′25.05″N 39°44′15.40″E 0.71 0 18.1 426
MW101-7 Calcareous NM-Metallic Ware Gre Eyşat 37°59′4.03″N 39°55′36.90″E 0.71 0 7.7 391
MW220-2 Calcareous NM-Metallic Ware Arslantepe 38°22′54.17″N 38°21′40.70″E 0.71 0 9.8 307
MW221-3 Calcareous NM-Metallic Ware Tepecık 38°53′4.18″N 38°52′47.76″E 0.71 0 10.1 314
HN2B Clay Upper Khabur 36°55′12.48″N 40°45′4.50″E 0.71 0 21.6 441
VS2F Clay Upper Khabur 37°0′54.18″N 41°0′27.78″E 0.71 0 19.1 342
FAR7 Clay Upper Khabur 36°49′17.34″N 41°27′22.38″E 0.71 0 13.5 432
DER3 Clay Derik/Mardin 37°21′6.11″N 40°16′43.63″E 0.71 0 33.4 124
TIG20 Clay Upper Tigris 37°50′0.75″N 40°33′36.95″E 0.71 0 13.7 227
T401 Clay Upper Tigris 37°49′39.87″N 40°50′13.08″E 0.71 0 11.9 180
HRR7 Clay Harran plain 36°56′44.58″N 38°54′25.70″E 0.71 0 15.3 225
HRR14 Clay Harran plain 36°56′47.52″N 39°5′48.43″E 0.71 0 17.9 270
T12-2 Clay Karacadaǧ 37°37′22.66″N 39°17′55.21″E 0.71 0 3.0 236
P1C Clay Pütürge 38°13′32.24″N 38°51′13.86″E 0.72 0 0.7 131
US5D Clay Pütürge 38°21′10.85″N 39°9′55.84″E 0.72 0 0.6 92
P17 Clay Pütürge 38°7′17.23″N 38°44′1.37″E 0.72 0 1.0 98
UKRZ Clay Pütürge 38°22′9.06″N 39°9′22.92″E 0.72 0 0.8 114
US3 Clay Pütürge 38°21′47.90″N 39°9′8.76″E 0.72 0 0.8 107
P8 Clay Pütürge 38°19′2.15″N 39°3′57.07″E 0.72 0 0.7 112
P18 Clay Pütürge 38°6′39.48″N 38°44′5.63″E 0.72 0 0.8 84
CHL7 Clay Çelikhan 38°1′53.46″N 38°14′30.32″E 0.71 0 0.4 103
geological time because of changes in supply and sources as a result of predominated by Cretaceous to Upper Miocene calcareous units
geological evolution. Their 87Sr/86Sr ratios are not age-dependent and (Fig. 3). These are subdivided into several units and formations (fm). A
are usually low compared with the consonantal rocks, ranging from prevalent series exposed over a large area in this region is the Palaeo-
0.705 to 0.709 (e.g. Banner, 2004; McArthur et al., 2001; Veizer, 1989). gene marine succession of Şelmo fm, overlaid by a lacustrine succession
of Yeniköy fm, dated to the Late Miocene/Early Pliocene. The Yeniköy
5. Geological setting of the study area fm outcrops, which cover a wide area, consist of reddish-coloured la-
custrine deposits of gravel, sandstone, siltstone and mudstone
The present-day geology of the study area of southeastern Anatolia, (Westaway et al., 2009). It is unconformably overlaid by fluvial gravel
northeastern Syria and adjacent regions is the result of a complex and of Gölpinar fm, consisting of polymict lithologies, such as quartzite,
long-standing, multifaceted geological evolution (e.g. Okay, 2008, and amphibolite, peridotite, marble, schist, gneiss and granite. A typical
references therein). Based on the geological and geographical location, geographical formation of the Upper Tigris Basin is the fluvial terrace
the main distribution area of NMMW can be divided into four tenta- system, which is composed mainly of coarse, angular gravel, reddish-
tively defined zones: the Upper Khabur Region, the Upper Tigris Valley, orange sandy–silt layers and clay-rich layers of various thicknesses
the Harran Plain and the Pütürge region (Fig. 3). (Doǧan, 2005). In the western part of the basin, between Diyarbakır and
The geology of the Upper Khabur region (Fig. 3) is related to the Hani in Șanlıurfa, the surface geology consists of Late Miocene–Qua-
general geological evolution of the northern Arabian plate. The surface ternary basaltic lavas of Karacadağ (Fig. 3), covering an underlying
geology consists of Pliocene conglomerate, sandstone, limestone, clay calcareous succession of the Arabian platform over an area of c.
and marls, and Late Miocene limestone, marls, conglomerates and 10,000 km2 (Lustrino et al., 2010).
sandstone. The alluvial basin consists of sediments derived from young The Harran Plain is a north–south trending rift system, known as
calcareous rocks (Ponikarov, 1967; Van Liere, 1965; Westaway et al., Akçakale graben, structured by large north–south orientated faults; it
2009). North-east of the Khabur region, near the Tigris River in the developed as a result of the compressional regime of the Eurasian and
Turkish part of the research area, young basaltic rocks cover a large Arabian plates and the continuing tectonic activity after the closure
area (Drüppel et al., 2011). North of al-Hassake, in the Ard esh-Sheikh phase (Kaya et al., 2010; Tardu et al., 1987). The catchment area of the
plateau and east of the al-Hassake, basaltic rocks cover an area of ap- alluvial deposits is dominated by Eocene–Middle Miocene calcareous
proximately 380 km2, with a thickness of c. 10–15 m. They are dated to rocks, which are exposed in the surrounding area of the basin (Fig. 3).
the Lower Quaternary, c. 1.8–0.7 million years old (Ponikarov, 1966; Additionally, basaltic rocks appear in a limited area in the north of the
Trifonov et al., 2011). basin (Fig. 2). The basin sediments are primarily derived from calcar-
The surface geology of the Upper Tigris valley and its surrounding is eous rocks within the catchment of the basin deposits (Tardu et al.,
9
Table 3
Major and trace element concentrations of the reference clay samples from northeastern Syria (Khabur region), the Upper Tigris Valley, the Harran plain and Pütürge region.
Sample Location SiO2 TiO2 Al2O3 Fe2O3 MnO MgO CaO Na2O K2O P2O5 Ba Co Cr Ni Rb Sr V Y Zn Zr Ce La Nd Sm Yb Sum
T106 Upper Tigris valley 57.1 0.9 15.1 9.0 0.13 6.2 7.0 2.41 1.8 0.19 298 45 646 287 49 204 163 30 96 151 157 18 0 22 3 100.0
TFB Upper Tigris valley 56.1 0.9 14.9 8.1 0.13 5.4 10.4 1.95 1.8 0.16 285 31 435 234 56 201 156 28 96 106 50 36 14 22 3 100.0
YY-1 Upper Tigris valley 54.7 0.9 15.0 7.6 0.18 5.3 13.2 1.21 1.6 0.16 385 32 227 120 51 224 159 28 116 96 32 29 0 18 3 100.0
YY-2 Upper Tigris valley 57.5 0.9 15.3 7.9 0.14 5.6 9.3 0.94 2.1 0.20 401 25 270 163 75 174 186 30 122 123 68 34 17 28 3 100.0
TD-B Upper Tigris valley 56.9 1.0 14.1 7.7 0.12 5.3 10.8 2.29 1.5 0.14 263 8.4 812 309 44 171 159 33 53 183 154 17 0 25 3 100.0
UT1B Upper Tigris valley 39.4 0.7 9.18 4.9 0.1 6.1 37.1 0.66 1.3 0.41 208 4 305 102 38 387 111 33 56 155 104 23 0 29 3 100.0
UCT-1 Upper Tigris valley 43.1 0.8 10.6 5.7 0.11 5.5 31.5 0.82 1.4 0.36 246 17 346 96 45 332 120 28 86 107 51 33 0 26 2 100.0
UCT2 Upper Tigris valley 52.6 0.9 14.4 7.2 0.14 4.7 17.5 0.58 1.7 0.22 367 24 254 160 72 203 138 34 117 121 55 38 17 30 3 100.0
TGT20 Upper Tigris valley 55.3 1.0 15.6 7.5 0.13 4.4 13.7 0.56 1.4 0.14 379 16 390 229 65 227 163 28 66 198 133 25 15 53 3 100.0
GRC5 Upper Tigris valley 51.9 0.8 14.4 7.9 0.15 5.3 16.5 0.90 1.7 0.25 301 35 253 202 58 377 156 26 116 95 45 54 0 25 2 100.0
10
SLT1 Upper Tigris valley 56.7 0.9 13.6 7.1 0.13 5.0 11.9 2.07 2.3 0.17 278 8 401 253 49 252 158 30 63 168 64 22 0 21 2 100.0
TGT22 Upper Tigris valley 61.7 0.7 14.4 5.7 0.09 4.1 9.8 1.42 1.8 0.18 388 0 133 106 56 155 133 20 37 168 100 18 0 37 2 100.0
MUT2 Upper Tigris valley 55.4 0.9 14.9 7.0 0.13 5.2 13.5 1.05 1.8 0.17 357 1 219 178 60 217 152 27 65 164 79 25 0 40 2 100.0
DRK1 Upper Tigris valley 55.0 0.8 14.7 6.7 0.14 4.5 15.7 0.90 1.3 0.13 345 11 231 146 50 358 152 21 53 145 97 21 0 46 2 100.0
TN-21 Upper Tigris valley 55.8 0.9 14.6 6.7 0.13 4.7 14.3 0.81 1.8 0.14 403 7 230 186 69 234 145 27 60 207 141 23 0 56 2 100.0
BTM1 Upper Tigris valley 54.4 0.8 15.2 6.9 0.16 5.3 13.9 1.23 1.8 0.15 198 12 254 159 47 283 200 19 57 106 91 24 0 32 2 100.0
Table 3 (continued)
Sample Location SiO2 TiO2 Al2O3 Fe2O3 MnO MgO CaO Na2O K2O P2O5 Ba Co Cr Ni Rb Sr V Y Zn Zr Ce La Nd Sm Yb Sum
HSK-1 Upper Tigris valley 50.7 0.9 13.8 7.3 0.14 6.2 17.4 1.10 2.1 0.25 419 21 260 174 78 321 120 30 116 127 65 39 16 38 3 100.0
HSK-2B Upper Tigris valley 63.7 0.8 13.2 6.1 0.1 4.1 7.1 2.57 1.9 0.17 382 19 332 106 64 199 112 28 101 188 42 30 0 24 2 100.0
HSK-3 Upper Tigris valley 60.1 0.9 13.5 6.7 0.12 4.8 9.5 2.22 1.9 0.20 388 23 360 129 65 228 121 33 95 186 54 35 17 32 3 100.0
T01-1 Upper Tigris valley 50.4 1.9 15.0 11.0 0.16 3.7 13.7 0.78 1.4 0.87 268 39 309 226 44 238 204 30 113 168 125 0 24 5.8 2.6 98.9
T11-1B Upper Tigris valley 60.2 1.3 17.1 9.9 0.15 4.2 3.4 0.54 2.3 0.60 339 28 282 239 70 103 170 33 111 182 132 14 23 4.5 3.5 99.8
T14 Upper Tigris valley 56.6 2.2 18.4 11.6 0.19 3.8 3.2 0.68 1.9 0.41 454 38 250 247 72 157 240 40 111 229 165 10 30 5.8 4.1 98.9
T20-1A Upper Tigris valley 53.5 1.1 15.8 7.9 0.17 4.1 15.3 0.31 1.5 0.17 452 14 371 230 79 163 148 40 76 213 164 23 32 5.9 4.1 99.8
T20B Upper Tigris valley 55.2 1.1 16.5 8.1 0.15 4.2 12.5 0.34 1.6 0.16 476 13 302 240 84 162 144 39 77 214 156 25 29 5.2 4.0 99.8
T21-B Upper Tigris valley 56.4 1.3 17.7 9.4 0.16 4.3 8.6 0.32 1.6 0.18 397 23 276 267 77 96 173 38 87 203 165 20 28 6.1 3.9 99.8
T94-B Upper Tigris valley 58.1 1.4 16.4 9.1 0.16 4.4 7.7 0.49 1.6 0.36 340 22 266 232 78 223 161 37 101 209 167 25 32 6.3 3.9 99.8
T102B Upper Tigris valley 60.1 1.5 17.8 9.5 0.18 4.4 3.2 0.43 1.6 0.23 390 5 269 277 82 127 183 39 91 218 197 23 31 5.8 4.2 99.1
T104 Upper Tigris valley 51.4 1.3 13.0 7.6 0.16 4.6 19.2 0.54 1.7 0.31 299 16 227 175 63 338 145 30 77 182 135 15 31 5.2 2.7 99.8
DER1 Derik/Mardin 39.5 0.7 10.4 5.2 0.09 6.9 34.0 0.81 2.0 0.45 298 0 68 77 58 144 74 16 65 136 170 19 0 99 0 100.0
DER2 Derik/Mardin 39.7 0.7 10.8 5.3 0.1 7.1 33.1 0.80 2.1 0.44 305 0 65 82 58 144 75 11 69 133 186 17 0 104 0 100.0
11
DER3 Derik/Mardin 37.6 0.6 8.78 4.2 0.08 5.3 40.2 0.95 1.9 0.38 277 0 37 38 46 124 56 13 43 120 151 6 0 90 0 100.0
DER4 Derik/Mardin 37.3 0.6 9.63 4.8 0.1 8.3 36.2 0.79 1.9 0.38 284 0 73 75 51 132 71 14 59 132 164 13 0 103 0 100.0
HN2B NE-Syria 49.5 0.8 13.5 6.6 0.12 5.3 21.6 0.38 1.7 0.16 334 0 209 201 68 441 132 29 63 166 183 29 0 34 3 100.0
VS1 NE-Syria 50.5 0.9 13.5 6.8 0.13 5.0 20.5 0.44 1.8 0.18 351 0 287 210 69 344 139 32 65 201 193 25 15 23 3 100.0
VS2B NE-Syria 51.9 0.9 13.6 6.7 0.12 5.0 19.1 0.48 1.9 0.21 358 0 257 215 69 342 143 33 66 194 174 29 0 23 3 100.0
RAD-1 NE-Syria 47.8 1.0 11.5 6.7 0.12 5.8 24.4 0.50 1.9 0.20 311 21 353 169 61 337 125 30 89 145 51 39 20 35 3 100.0
GEL-1 NE-Syria 38.0 0.6 9.8 5.1 0.08 5.3 39.6 0.26 1.1 0.13 239 15 222 136 46 390 98 21 68 89 0 54 0 34 2 100.0
ASLO-1 NE-Syria 51.3 0.9 12.6 6.4 0.12 5.0 20.9 0.50 1.8 0.23 333 19 284 155 70 414 114 31 93 139 65 52 18 38 3 100.0
HSBIII-B2 NE-Syria 49.6 0.8 12.9 6.3 0.08 4.9 22.5 0.46 1.9 0.32 353 18 257 157 72 535 110 29 100 154 65 62 17 36 3 100.0
KAL-6 NE-Syria 40.6 0.7 10.3 5.4 0.09 7.3 33.4 0.45 1.4 0.17 267 16 243 130 55 393 101 29 72 125 63 58 0 28 2 100.0
JERM-3 NE-Syria 39.4 0.7 11.1 5.5 0.05 7.8 33.6 0.35 1.3 0.14 249 13 221 131 57 222 105 29 84 84 68 47 18 28 3 100.0
FAR-7 NE-Syria 54.2 1.0 15.1 8.1 0.14 4.9 13.5 0.68 1.9 0.24 404 30 259 203 80 432 154 36 108 158 75 67 21 34 3 100.0
KHR-6 NE-Syria 50.0 0.9 13.6 7.1 0.12 5.5 20.1 0.47 1.8 0.20 323 24 299 199 76 325 129 31 96 140 68 49 19 30 3 100.0
WR-38 NE-Syria 54.4 0.9 14.4 7.7 0.13 5.9 13.5 0.53 2.2 0.23 361 27 330 245 79 244 134 30 106 117 51 52 19 27 3 100.0
AY-37 NE-Syria 55.0 0.7 10.9 5.2 0.12 3.9 20.9 1.28 1.6 0.17 323 17 573 148 55 371 104 26 66 121 42 46 0 25 2 100.0
QM1 NE-Syria 49.1 0.8 13.9 6.9 0.11 5.5 21.3 0.32 1.8 0.15 327 0 214 228 70 224 142 33 63 168 162 16 15 32 3 100.0
QP215 NE-Syria 50.2 0.8 11.6 5.9 0.11 4.6 24.4 0.61 1.4 0.20 269 21 354 166 54 187 124 29 119 99 54 28 20 28 3 100.0
HRR1 Harran plain 39.3 0.6 10.6 5.1 0.08 4.9 37.6 0.41 1.2 0.17 257 14 217 64 36 1725 108 0 49 125 98 81 46 3.8 0.0 100.0
HRR2 Harran plain 44.9 0.8 12.6 6.3 0.12 4.4 28.6 0.48 1.6 0.18 306 15 216 0 43 2020 93 0 53 125 114 93 31 4.0 0.0 100.0
HRR3 Harran plain 38.0 0.6 9.8 4.8 0.07 4.7 40.8 0.17 0.9 0.12 265 10 175 70 32 387 125 0 43 117 71 12 42 4.1 0.5 100.0
HRR4 Harran plain 50.2 0.7 10.6 5.6 0.12 4.4 26.8 0.66 0.8 0.12 199 18 289 118 27 391 161 15 41 105 68 22 34 0.0 0.9 100.0
HRR5 Harran plain 35.1 0.6 8.8 4.4 0.08 4.1 45.7 0.27 0.9 0.15 277 8 206 61 29 496 87 0 44 109 69 22 39 4.5 0.1 100.0
HRR6 Harran plain 45.1 0.8 13.0 6.4 0.10 4.9 27.9 0.22 1.4 0.12 324 21 235 144 50 297 118 20 62 158 105 21 53 0.0 1.4 100.0
HRR7 Harran plain 52.3 0.9 16.0 7.8 0.15 4.9 15.4 0.30 2.0 0.22 389 34 245 242 81 223 136 28 91 187 105 22 56 5.8 2.7 100.0
HRR8 Harran plain 45.7 1.0 13.3 7.2 0.13 4.6 25.9 0.45 1.6 0.20 398 27 259 181 60 539 123 24 76 173 111 29 42 7.4 2.1 100.0
HRR9 Harran plain 50.6 1.0 14.2 7.2 0.13 4.1 19.9 0.72 1.9 0.19 395 31 295 205 70 420 133 24 76 202 105 30 47 4.3 2.1 100.0
HRR10 Harran plain 49.2 1.0 15.3 7.7 0.13 4.7 19.4 0.62 1.9 0.20 485 30 253 216 74 371 133 25 85 174 101 31 46 3.4 2.4 100.0
HRR11 Harran plain 46.0 0.9 13.8 6.8 0.13 5.5 23.8 1.02 1.9 0.22 301 19 202 87 61 641 102 18 64 148 111 38 41 2.1 1.5 100.0
HRR12 Harran plain 46.5 0.8 13.2 6.4 0.12 5.2 26.2 0.23 1.3 0.15 433 29 239 229 50 326 155 21 67 162 107 19 44 1.9 1.6 100.0
1987).
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
100.0
Sum
The Pütürge Massif (or Pütürge Metamorphic) is situated on the
northern rim of the Arabian plate and is part of the eastern Taurus
1.3
2.9
2.3
2.4
2.1
3.3
Yb
Mountains, which form a high mountain belt between central Anatolia
4
5
5
4
4
6
5
5
6
6
5
6
6
6
5
4
6
6
5
and the lower lands of the Upper Tigris and northern Syria (Fig. 2). The
2.9
7.1
3.5
8.8
3.1
7.2
4.4
5.8
8.7
4.0
5.8
5.8
5.8
5.8
5.8
5.8
9.9
5.8
7.2
5.8
9.9
5.8
7.0
5.7
6.8
Sm
Pütürge Massif area is geologically very different from the Upper Tigris
and Upper Khabur regions (Fig. 3). It is the western equivalent of the
Nd
42
62
42
54
69
47
35
40
39
35
35
50
37
46
41
23
61
58
77
70
59
41
73
80
70
Bitlis Massif, commonly called the Bitlis–Pütürge Massif (or Bitlis–Pü-
türge complex); it is considered to be part of the Anatolide–Tauride
34
22
16
16
29
31
31
41
33
32
39
39
38
37
18
48
36
43
39
36
33
42
38
42
La
block, a complex Alpine belt with a collage of terranes (Bozkaya et al.,
1087
1109
2007, and references therein; Oberhänsli et al., 2010). The massif forms
135
116
124
101
113
208
236
224
157
303
392
299
343
251
383
663
626
711
141
199
154
153
80
Ce
an arc-shaped metamorphic belt in the eastern part of Taurus Orogenic

belt. The Pütürge Massif consists of Precambrian–Permian age meta-
141
211
178
195
202
218
201
235
212
185
185
294
208
244
296
230
218
263
244
245
272
241
261
276
261
Zr
morphic rocks of gneiss, micagneiss–micaschists intercalated with am-

phibolite, amphibolegneiss/schist, granitic gneiss, kyanite–muscovite
183
209
217
153
129
137
157
159
103
153
138
137
103
105
105
Zn
57
93
75
76
68
91
80
17
95
45
gneiss and calcschist/marble (Bozkaya et al., 2007, see also Fig. 4 in
Kibaroğlu and Falb, 2013). In the southern part of the Malatya region,
20
31
26
27
26
34
37
45
44
35
36
52
39
44
51
54
43
49
47
48
43
42
52
49
45
Y
there are also outcrops of so-called Malatya metamorphics, schists

143
127
138
122
133
152
182
193
128
174
210
194
189
136
226
189
210
195
193
146
163
196
177
160
(lower stratigraphic unit) and slate (upper stratigraphic unit) (Yalçın
91
V
et al., 1999).
348
269
239
243
283
261
115
131
141
154
131
112
130
128
124
107
104
114
103
98
84
90
92
70
76
Sr
6. Results and discussion

131
150
171
121
151
150
146
149
136
125
182
168
181
178
136
139
151
161
Rb
41
80
67
70
53
75
98
6.1. Chemical and mineralogical characteristics of NMMW

267
215
214
164
223
122
143
144
108
206
267
241
230
191
227
167
247
205
204
140
158
215
255
205
73
Ni
Previous archaeometric analyses, performed first in the 1980s, re-

vealed that the NMMW vessels were produced from two very different
242
297
261
302
390
229
116
156
164
179
319
246
244
118
167
109
219
121
118
110
122
169
211
153
97
Cr
clay types and clustered into two chemical groups on the basis of the
CaO content of the paste: calcareous and non-calcareous (Kühne and
Co
12
38
28
33
25
31
15
33
22
0
0
0
0
0
0
0
0
0
0
0
0
0
0
4
8
Schneider, 1988). The vast majority of the vessels was produced from a
very special non-calcareous clay, which shows a characteristic and
1035
1105
1121
1122
1268
1019
802
407
471
432
278
382
958
581
589
857
718
431
999
853
857
681
972
463
508
Ba
homogeneous element composition, characterised by on average very

low CaO (1.9%) and MgO (1.2%), low Sr (140 ppm) and Cr (103 ppm)
P2O5
0.19
0.22
0.24
0.21
0.21
0.19
0.16
0.15
0.16
0.37
0.16
0.33
0.13
0.23
0.13
0.19
0.17
0.27
0.26
0.25
0.20
0.16
0.29
0.23
0.18
and high Al2O3 (21.5%) contents. In contrast, the calcareous group is

characterised by on average high concentrations of CaO (up to 20%),
K2O
MgO (5.2 wt%), Sr (320 ppm), Cr (203 ppm) and Ni (180 ppm). Fur-
1.2
2.0
2.7
1.9
1.4
1.9
3.2
3.7
4.0
3.3
4.0
3.6
3.4
3.9
3.3
3.6
3.7
3.7
4.1
4.0
3.1
3.1
2.4
3.9
4.0
thermore, both groups show different mineralogical compositions. The

non-calcareous group contains mineral phases of α-quartz, hematite,
Na2O
0.36
0.45
0.51
0.41
0.45
0.31
1.29
0.99
0.71
2.15
0.95
0.95
1.16
1.16
2.55
0.65
1.20
1.05
0.83
0.87
2.48
2.04
0.78
0.40
1.17
feldspars, rutile, magnetite and Cr(III)-containing aluminium oxide

(Al2O3) (Zoppi et al., 2005). Electron microscope analysis has identified
38.8
17.9
22.4
21.7
28.2
22.4
CaO
0.6
0.7
0.8
3.9
1.0
0.7
1.6
1.2
1.0
0.8
1.0
0.8
0.6
0.6
0.4
0.8
0.4
0.5
0.5
the feldspar as a K feldspar (Zoppi et al., 2005; see also Broekmans

et al., 2006; Schneider, 1989). A typical mineralogical feature of the
MgO
non-calcareous group is the absence of Ca–silica phases. The calcareous

3.2
4.3
4.4
4.5
2.8
3.4
1.5
1.9
2.2
3.1
3.1
2.5
4.4
3.5
2.3
4.2
2.4
2.8
2.3
2.3
1.6
1.8
1.6
2.1
2.4
group has marly clay, composed mainly of Ca-silicates such as diopside,

MnO
anorthite and, in few cases, gehlenite (Schneider and Daszkiewicz,

0.13
0.18
0.15
0.19
0.08
0.14
0.16
0.14
0.09
0.11
0.12
0.20
0.14
0.19
0.07
0.26
0.07
0.14
0.10
0.11
0.14
0.13
0.15
0.13
0.10
2001). Micro-Raman spectroscopic analysis has revealed the presence

of α-quartz, alkali and plagioclases, magnetite, Cr(Ill)-containing Al2O3,
Fe2O3
12.4
10.5
10.5
10.4
10.3
gypsum, calcite and hematite (Zoppi et al., 2005).

5.5
8.0
6.6
7.2
6.8
7.6
8.0
8.8
9.3
7.0
9.1
9.7
9.2
9.3
5.2
9.7
9.6
8.7
8.4
8.4
Al2O3
6.2. Principal component analysis (PCA)

10.8
15.5
13.6
14.3
12.6
15.5
19.4
22.6
25.7
17.7
23.9
21.6
22.3
21.4
21.1
23.6
27.6
23.1
23.9
23.9
19.8
20.7
21.1
23.7
22.9
Because of the calcareous nature of the local clay deposits in north-

TiO2
east Syria, which result from the predominant Miocene and Pliocene
0.8
1.0
0.8
0.9
1.2
0.9
0.9
1.1
1.0
0.9
0.9
1.3
1.0
1.1
1.1
1.6
0.8
1.2
1.1
1.1
1.1
1.0
1.3
1.1
1.1
calcareous marine and lacustrine sediments (Ponikarov, 1967; Van

SiO2
Liere, 1965; see Fig. 3), the clay deposits and local potteries generally
39.0
50.3
48.6
48.7
46.3
47.6
64.6
59.7
55.8
61.3
56.5
58.8
56.5
57.7
63.1
52.3
53.1
57.0
56.1
56.1
62.2
61.6
61.5
57.4
59.1
contained a very high CaO concentration, of up to 20% (Kibaroğlu,

2008; Kibaroğlu and Falb, 2013; Schneider, 1989). In a recent ar-
chaeometric study, based on element analysis, Kibaroğlu and Falb
Harran plain
Harran plain
Harran plain
Harran plain
Harran plain
Harran plain
(2013) reported that the clay occurrence available in the Pütürge Massif
area, located on the border of the main distribution area of NMMW
Location
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
Pütürge
(Fig. 2 and 3), shows compositional similarity with the non-calcareous

Table 3 (continued)
variety (see also below). A bivariate comparison of the element con-

centrations of the Pütürge clays with those of the non-calcareous
NMMW showed a close compositional relationship, although they did
Sample
HRR13
HRR14
HRR15
HRR16
HRR17
HRR18
US 5D
US 5A
US-5C
US-1B
UKRZ
CHL7
YPZ1
YPZ2
P-1D
P-3A
P-1C
P-1B
US3
P13
P15
P17
P18
not completely overlap (Kibaroğlu and Falb, 2013; Fig. 3). We ex-
P6
P8
amined the element composition of NMMW and reference clay samples
12
Fig. 4. A scatter plot of first two principal components (PC1 and PC2) of the NMMW and reference samples.
using multivariate statistical analysis, in order to explore the chemical groups. Samples from northeastern Syria, the Upper Tigris and the
similarity or dissimilarity of the non-calcareous NMMW to the reference Harran Plain form a single group displaying a wide variation. The
materials, particularly to the clays from the Pütürge Massif area. The sample from the Pütürge Massif forms a single compositional group,
ceramic samples comprised 127 NMMW examples collected from south- clearly distinguishable from the other reference samples. The non-cal-
eastern Anatolia within the framework of SOAP project, 120 of which careous NMMW group falls close to the Pütürge clay group, but the
have already been published (see table 1 in Kibaroğlu and Falb, 2013). overlap is not perfect. The non-calcareous NMMW group therefore also
To these data we added seven new NMMW samples (Table 1). The re- shows a clear dissimilarity to the clay samples from northeastern Syria,
ference material comprised the clay samples collected from north- the Upper Tigris, the Harran Plain and the Khabur Plain (Fig. 4a). The
eastern Syria and the Derik region (n = 19), Upper Tigris Valley plot of variable loadings displayed in Fig. 4b shows that the non-cal-
(n = 60), Harran Plain (n = 18) and Pütürge Massif area (n = 19). The careous MMMW and Pütürge samples are mainly characterised by high
major and trace element composition of the ceramic and reference concentrations of Si2O, TiO2, Al2O3, K2O, Zr and Rb, whereas the cal-
samples are listed in Table 3. careous NMMW and clay samples from northeastern Syria, the Upper
Principal component analysis (PCA) is a multivariate statistical Tigris Valley and the Harran Plain are characterised by high con-
method that is widely used in archaeometric studies of archaeological centrations of CaO, Mg and Sr.
ceramics. The method is described extensively elsewhere (e.g. Baxter, The statistical re-examination of the element composition of the
1995, 2003; Shennan, 1997). Prior to the PCA calculation, the com- NMMW and reference samples is in accordance with those of previous
positional data from the NMMW and reference samples were first studies. The close compositional relationship of the non-calcareous
transformed logarithmically to base 10 and then standardised to obtain NMMW and clay samples from the Pütürge Massif area, as demon-
data of a similar order of magnitude with comparable variance (e.g. strated by PCA analysis and previous research, suggests that the clay
Baxter, 2003). The PCA calculation of the samples was based on the occurring in the Pütürge Massif area might be the source of raw clay for
levels of six major (SiO2, TiO2, Al2O3, MgO, CaO and K2O) and five non-calcareous NMMW production. This represents a single area of
trace (Ni, Rb, Sr, Y and Zr) elements, which were thought to be the most source clay with element characteristics comparable with the non-cal-
suitable for achieving this study's aims. The statistical calculations were careous NMMW that lies within the NMMW distribution area. To verify
performed using the multivariate statistical package JMP version 12. this interpretation, an Sr isotopic analysis was carried out on NMMW
The values of the first two principal components of the data, PC1 and local clays from northeastern Syria, southeastern Anatolia and the
and PC2, are represented in a scatter diagram in Fig. 4. In Fig. 4, the Pütürge region (Fig. 2 and 3).
calcareous and non-calcareous NMMW can be clearly distinguished
from each other. The reference samples also show two main conditional
Fig. 5. A plot of 87Sr/86Sr ratios versus 1/Sr

(ppm− 1) and CaO (wt%) of NMMW and clay
samples from the Pütürge Massif area, Upper
Khabur, Upper Tigris, Harran Plain and Derik/
Mardin region.
13
87
6.3. Sr/86Sr composition of NMMW and reference samples element or isotopic composition comparable with the non-calcareous
NMMW has been identified within the NMMW distribution area
The results of the 87Sr/86Sr isotope ratios of NMMW and reference (Fig. 3). Combining our isotopic analysis with results from previous
samples are given in Table 2. In Fig. 5, the 87Sr/86Sr ratios of all the work including element and mineralogical analyses (Kibaroğlu and
samples are illustrated. The 87Sr/86Sr ratios of both the non-calcareous Falb, 2013, and references therein), and considering the geological
and calcareous chemical groups of NMMW show clearly different Sr setting of the study area as well as its geographical location, it is most
isotopic signatures. The non-calcareous NMMW is characterised by likely that the source of the raw clay for non-calcareous NMMW was
much higher 87Sr/86Sr values, ranging from 0.71693 to 0.73088, located within the Pütürge Massif area, where Precambrian–Permian-
whereas the calcareous group has lower 87Sr/86Sr values, ranging from age metamorphic rocks, such as schist/slate and similar rocks, are
0.70828 to 0.70915 (Fig. 5), with the exception of one example widely exposed (Fig. 3), possibly somewhere in the southern part of the
showing a slightly lower value (sample MW542-4, 0.71429). These Pütürge region, where access is easier via the River Euphrates.
different isotopic signatures for the two chemical NMMW groups are in The question of the provenance of the calcareous variant of NMMW
accordance with the results of the element analysis and verify the is less complicated. The low 87Sr/86Sr values of the calcareous group of
previous inferences regarding the use of different raw materials for NMMW plotted close to the clays from the Upper Khabur, Harran Plain
NMMW production. The high 87Sr/86Sr values of the non-calcareous and Upper Tigris (Fig. 5), which suggests its production fell within the
NMMW may be caused by the presence of K-bearing minerals (e.g. K- core area, for example in northern Mesopotamia. This supports the
feldspar) in the raw materials, including clay minerals (e.g. illite). This results of previous work (Kibaroğlu, 2008; Kibaroğlu et al., 2008;
is supported by the mineralogical–petrographic observations given Kühne and Schneider, 1988). However, because of isotopic similarities
above. At the same time, this can be explained by the fact that the between the three regions, it is difficult to identify just one of these
source rocks for the clay consist of predominantly old rocks with felsic areas as the potential source of the clay for the calcareous NMMW. The
affinity (i.e. high Rb/Sr concentrations). In contrast, the low 87Sr/86Sr similarities can be attributed to the lithological and depositional re-
values (0.70828–0.70915) of the calcareous NMMW group may be re- semblance of the surface geology, which is predominated by Mioce-
lated to the fact that its raw clay was derived predominantly from ne–Pliocene calcareous marine sediments accumulated on the Arabian
carbonate-rich rocks, such as fluvial deposits in the Upper Khabur, platform.
which show a similar Sr isotopic signature. The results of the petro-
graphic and mineralogical analyses (e.g., Kühne and Schneider, 1988; 7. Conclusions
Kibaroğlu et al., 2008), as already mentioned above, such as the marly
nature of the clay paste and the presence of Ca-silicate mineral phases The present study demonstrates that the two major groups of
like diopside and anorthite in the calcareous group, also support this NMMW, non-calcareous and calcareous, show clear differences in their
assumption. Sr isotopic composition. Compared with the calcareous variant, which
A clear isotopic discrimination was also observed among the clays shows lower Sr isotope ratios (0.70828–0.70915), the non-calcareous
from the Pütürge Massif area and other regions (from the Upper group shows much higher Sr isotopic ratios (0.71693–0.73088).
Khabur, Upper Tigris and Harran Plain) (Fig. 5). The 87Sr/86Sr ratios of The results of the Sr isotopic analysis on NMMW support those of
the clays from the Upper Khabur, Upper Tigris and Harran Plain (except the compositional analysis reported in a previous study by Kibaroğlu
for the samples from the Karacadağ and Derik/Mardin area) show si- and Falb (2013), which argues that the source of the raw clay for the
milarities in terms of their Sr isotopic signature, with values varying non-calcareous group may be located in the Pütürge Massif area, where
from 0.708617 to 0.709753. The samples from the Pütürge region, Precambrian–Permian-age metamorphic rocks are exposed, for example
however, are characterised by much higher 87Sr/86Sr ratios, ranging in the southern part of the Pütürge region. Furthermore, the results
from 0.71230 to 0.72197, compared with the samples from other re- support other studies on the calcareous variant of the metallic ware
gions (Fig. 5). As predicted, sample T12-2 taken from in situ clay de- suggesting a local northern Mesopotamian origin.
posits in the Karacadağ basaltic area (Fig. 2 and 3) show the lowest This study also demonstrates that Sr isotope analysis is a useful tool
levels of Sr isotopic composition (0.705812). On the other hand, the for the material characterisation and provenance identification of ar-
clay sample from the Derik/Mardin area (DER3) show a relatively chaeological ceramics. The basic principle of the method, which is
higher Sr isotope ratio in comparison with the Upper Khabur and Upper based on the age-related variation of 87Sr/86Sr ratios in the raw mate-
Tigris clays. Clay sample DER3 also came from in situ clay deposits rial, and the general lithological features of the parent rocks, make this
derived from Cretaceous calcareous limestone exposed on the south- method particularly suitable for archaeometric research on ancient
western slope of the Mardin High (Fig. 2 and 3). pottery but, as presented in former studies (e.g. Carter et al., 2011; Li
Considering the 87Sr/86Sr ratios of the reference clay samples, there et al., 2005), it is still used largely as a complementary technique.
is a positive relationship between the 87Sr/86Sr ratios of the clays and
the age and lithology of their source rocks. Clays from the Pütürge Acknowledgements
region, which are derived from Cambrian–Permian (541–252 million
years ago) metamorphic rocks of the Pütürge Massif, have much higher This study is part of the southeastern Anatolian Project (SOAP) at
87
Sr/86Sr values, whereas the samples from Palaeogene–Neogene Goethe-University Frankfurt am Main funded by the German Research
marine deposits of the Arabian platform and Late Miocene–Quaternary Foundation (DFG) between 2009 and 2012. The authors would like to
basaltic rocks are characterised by low 87Sr/86Sr values. express their gratitude to the director of the project, Professor Dr. Jan-
Waalke Meyer (Goethe-University of Frankfurt/M.), who made the
6.4. Comparison of NMMW and reference samples: provenance project possible. We would also like to express our gratitude for colla-
boration and contributions to the project to: Kültür Varlıkları ve
By comparing the 87Sr/86Sr ratios of NMMW and clay samples as Müzeler Genel Müdürlüğü in Ankara, Nihat Erdoğan (Mardin Museum),
illustrated in Fig. 5, we observed that the 87Sr/86Sr ratios of the non- Nevin Soyukaya and Ahmet Duman (Diyarbakır Museum), Istanbul
calcareous NMMW plotted close to the clays from the Pütürge Massif Archaeological Museums; Professor Dr. M. Özdoğan and Professor Dr.
region, although not fully overlapping. This suggests that the raw ma- Necmi Karul (University of Istanbul), Professor Dr. M. Frangipane
terial for non-calcareous NMMW was derived predominately from old (University La Sapienza, Rome), Dr. Deniz Yaşın-Meier (University of
rocks with felsic affinity (high Rb/Sr ratios) and that the rocks exposed Bern), Professor Dr. T. Ökse (University of Kocaeli, Turkey) and
within the Pütürge Massif area may have been the source of the non- Professor Dr. G. Kozbe (University of Ege, Turkey). In particular, the
calcareous clay. So far, no other clay deposit or rock type with an authors are indebted to Associate Professor E. Ay (University of
14
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Article in Journal of Archaeological Science: Reports · January 2017

Gubaz Mustafa Kibaroglu

Caltilar Project View project

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Contents lists available at ScienceDirect

Journal of Archaeological Science: Reports

Application of strontium isotope analysis to provenance studies of Early

1. Introduction 1976; Kühne and Schneider, 1988). Archaeologically, NMMW is con-

Fig. 1. Characteristic vessel types of NMMW

(caption on next page)

described by Mamani-Huisa (2006). One hundred milligrams of powder

with an acid mixture of double-distilled nitric acid (HNO3) and hy-

performed on columns ﬁlled with the cation exchange resin AG 50W-X8

preheated Re single ﬁlament. The isotopes of Sr were analysed by

mass spectrometer at the Geowissenschaftliches Zentrum Göttingen,

measurements of the standard NBS987 during the period these analyses

Sr (Z = 38) is an alkaline earth element with ionic radius 1.13 Å. It

of the parent isotope 87Rb, with a half-life of approximately

parent element Rb (Z = 37) is an alkali and a large-ion lithophile; its

highest abundance in K-bearing minerals such as muscovite, biotite,

2011). The major factors deﬁning the naturally occurring Sr isotopic

(iii) the age of the parent rocks.

systems (e.g. in granitic and granodioritic rocks), where it substitutes

whereas Sr is relatively compatible and preferentially substitutes for Ca

sites in plagioclase (White, 2015). For example, mantel-derived rocks,

the continental crust (White, 2015). As a result, minerals with a high K/

apatite). When the system remains closed with respect to Rb and Sr

et al., 1998; Faure, 1977; White, 2015).

radiogenic 87Sr originating from the decay of 87Rb is negligible. The

Mountains, which form a high mountain belt between central Anatolia

block, a complex Alpine belt with a collage of terranes (Bozkaya et al.,

an arc-shaped metamorphic belt in the eastern part of Taurus Orogenic

morphic rocks of gneiss, micagneiss–micaschists intercalated with am-

there are also outcrops of so-called Malatya metamorphics, schists

6. Results and discussion

6.1. Chemical and mineralogical characteristics of NMMW

Previous archaeometric analyses, performed ﬁrst in the 1980s, re-

homogeneous element composition, characterised by on average very

and high Al2O3 (21.5%) contents. In contrast, the calcareous group is

thermore, both groups show diﬀerent mineralogical compositions. The

feldspars, rutile, magnetite and Cr(III)-containing aluminium oxide

the feldspar as a K feldspar (Zoppi et al., 2005; see also Broekmans

non-calcareous group is the absence of Ca–silica phases. The calcareous

group has marly clay, composed mainly of Ca-silicates such as diopside,

anorthite and, in few cases, gehlenite (Schneider and Daszkiewicz,

2001). Micro-Raman spectroscopic analysis has revealed the presence

gypsum, calcite and hematite (Zoppi et al., 2005).

6.2. Principal component analysis (PCA)

Because of the calcareous nature of the local clay deposits in north-

calcareous marine and lacustrine sediments (Ponikarov, 1967; Van

contained a very high CaO concentration, of up to 20% (Kibaroğlu,

(Fig. 2 and 3), shows compositional similarity with the non-calcareous

variety (see also below). A bivariate comparison of the element con-

amined the element composition of NMMW and reference clay samples

Fig. 5. A plot of 87Sr/86Sr ratios versus 1/Sr

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