Optical Microscopy (OM) and X-Ray Diffraction (XRD) Studies of Ceramic Slag Samples from Tatarlı Höyük (Adana, Turkey)

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MORS IMMATURA

MORS

IMMATURA

AMANOSLARIN GöLGES‹NDE

HAYR‹YE AKIL ANISINA

IN THE SHADOW OF AMANUS

IN MEMORIAM HAYR‹YE AKIL

AMANOSLARIN

GöLGES‹NDE

HAYR‹YE AKIL ANISINA

IN THE SHADOW

OF AMANUS

IN MEMORIAM HAYR‹YE AKIL

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Amanosların Gölgesinde

Hayriye Akıl Anı Kitabı

MORS IMMATURA

In the Shadow of Amanus

In Memoriam Hayriye Akıl

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Kizzuwatna Araştırmaları Projesi Yayınları | Kizzuwatna Researches Project Publications No: 1

Amanosların Gölgesinde Hayriye Akıl Anı Kitabı MORS IMMATURA

In the Shadow of Amanus in Memoriam Hayriye Akıl

Editörler

K. Serdar Girginer, Gonca Dardeniz, Ayça Gerçek, Fatih Erhan, Elif Genç, İrfan Tuğcu, Özlem Oyman-Girginer, M. Cem Fırat, Hakan Gerçek, M. Furkan Tufan

Bu kitapta yayınlanan makalelerdeki bilimsel içerik ve etik ile ilgili tüm sorumluluklar yazarlarına aittir. Kaynak gösterilerek alıntı yapılabilir.

The academic content and ethical responsibility of the articles published here rest upon their authors. Quotations may be made with proper citation.

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Kizzuwatna Araştırmaları Projesi Yayınları | Kizzuwatna Researches Project Publications

No: 1

Amanosların Gölgesinde

Hayriye Akıl Anı Kitabı

MORS IMMATURA

In the Shadow of Amanus

In Memoriam Hayriye Akıl

Editörler | Edited by

K. Serdar Girginer, Gonca Dardeniz, Ayça Gerçek, Fatih Erhan, Elif Genç, İrfan Tuğcu,

Özlem Oyman-Girginer, M. Cem Fırat, Hakan Gerçek, M. Furkan Tufan

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İçindekiler

Önsöz . . . .ix Öğr. Gör. Hayriye Akıl (MA) Hakkında… . . . .xi Oda Arkadaşım Hayriye’nin Anısına: Mezarlık Gelinleri

Nesibe Çakır xv Öğretim Görevlisi Hayriye Akıl Tarih Turları…

Gülsün Özyurt – Caner Enver Özyurt xxi 2013 Yılı Tatarlı Höyük İskeletleri

Ayşen Açıkkol-Yıldırım – İbrahim Sarı 1 Tatarlı Höyük’te Ele Geçen Olynthos Tipi Değirmen Taşları

İlkay Aklan 9 Soğmatar Nekropolü Roma Dönemi Kaya Mezarları

Yusuf Albayrak 19 Tarihi Yapıların Yeniden İşlevlendirilmesine Bir Örnek:

Burdur Kavaklı Rum Kilisesi’nin Burdur Doğa Tarihi Müzesi’ne Dönüşümü

Ayşe Aydın 29 A General Overview on the Stepped Tunnels in Pontos Region

A Emirhan Bulut 47 Tatarlı Höyük Geç Tunç Çağı Savunma Sistemi ile İlgili Bir Değerlendirme

Mehmet Cevher 63 A Group of Late Bronze Age Faience Beads from Tatarlı Höyük (Adana, Turkey)

Gonca Dardeniz 75 Transport Jars from Tatarlı Höyük in Cilicia Pedias: First Observations

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Afyon’un Kuzeybatısındaki Karacaahmet ve Yeniceköy Köylerinden Gelen ve Afyon Arkeoloji Müzesi’nde Muhafaza Edilen Bir Grup Çanak Çömlek

Turan Efe – Deniz Sarı – Burçin Aydınbek 101 Augusta Antik Kenti

Fatih Erhan 131 Tatarlı Höyük Hellenistik Dönem Mimarisi

M Cem Fırat – K Serdar Girginer 149 Malatya-Elazığ Bölgesi’nde Erken Transkafkasya Mimarisi

Erkan Fidan – Ufuk Özdemir 167 Tilbaşar’da Yeni Kazılar (2015-2018): Başlıca Sonuçlar

Elif Genç 181 Tatarlı Höyük Hellenistik Dönem Kandilleri

Hakan Gerçek 195 Tatarlı Höyüğün Stratigrafisi Üzerine Ön Sonuçlar

K Serdar Girginer – Özlem Oyman-Girginer 211 Urartu Krallığı’nda Ritüel Kaplar

Bilcan Gökce 251 Gods on the Mountain? The Case of the Votive Statuettes from Sykhari-Lakkin on Cyprus

Hazar Kaba 275 Tatarlı Höyük’de Neolitik Dönem: Ön Değerlendirme

Orkun H Kayci – K Serdar Girginer 295 Optical Microscopy (OM) and X-Ray Diffraction (XRD) Studies of Ceramic Slag Samples from

Tatarlı Höyük (Adana, Turkey)

Nergis Kılınç-Mirdalı – K Serdar Girginer – Özlem Oyman-Girginer 309 Sirkeli Höyük: Kompleks Kent Yapısının Keşfi ve Araştırılma Süreci

Mirko Novák – Deniz Yaşin 317 Antik Çağ’da Kemiğin Takı ve Aksesuar Olarak İşlenmesi

Kasım Oyarçin – Halil Özkan 329 MÖ III. Binyıl Anadolu’sunda Oda Mezar Geleneği ve Sosyo-Ekonomik Açıdan Değerlendirilmesi

Umut Parlıtı 341 MÖ II. Binyılda Tatarlı Höyük’ün Adı

Tolga Pelvanoğlu – Metin Alparslan – Erkan Konyar 359

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Oylum Höyük Erken Tunç Çağı Popülasyonunun Çene ve Diş Patolojileri

İbrahim Sarı – Ayşen Açıkkol-Yıldırım 389 Ovalık Kilikya’da Pers Egemenliği

Mustafa Hamdi Sayar 403 Archaeozoological Remains in Tatarlı Höyük (Turkey) from Hellenistic Period

Derya Silibolatlaz-Baykara 411 Tatarlı Höyük’ten Bir Grup Black On Red (BoR) Seramiği ve Mikromorfolojik Özellikleri

Mehmet Furkan Tufan – K Serdar Girginer 427 Arkeolojik Seramikler ve Arkeometri: Üretim Teknolojisi ve Karakterizasyon Yöntemleri

Mine Taykurt-Daday – Nergis Kılınç-Mirdalı 449 Milas Müzesi’nde Bulunan İon Tipi Sütun Başlıkları

Akın Temür – Murat Sarıgül 465 Tatarlı Höyük Taş Kapları

İrfan Tuğcu 481 Osmaniye-Domuzdamı Kalesinde Bulunmuş Terra Sigillata Seramikler

Füsun Tülek 491 Frigler’de Mühürcülük

Birgül Yıldız-Köse 515 Ordu Müzesi’nde Korunan ve MÖ 2. Bine Tarihlendirilen Tunç Kolcuklu Balta

Davut Yiğitpaşa – Aynur Yağcı 531

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Optical Microscopy (OM) and X-Ray Diffraction (XRD) Studies of Ceramic

Slag Samples from Tatarlı Höyük (Adana, Turkey)

*

Nergis Kılınç-Mirdalı - K. Serdar Girginer - Özlem Oyman-Girginer**

Özet

Tatarlı Höyük’ten Seramik Cüruf Örneklerinin Optik Mikroskop (OM) ve

X-Işını Kırınımı (XRD) Çalışmaları (Adana, Türkiye)

Doğu Akdenizde Adana’nın Ceyhan ilçesinde yer alan Tatarlı Höyük’te, 2007 yılından bu yana multidisipliner kazı çalışmaları yürütülmektedir. Makale, 2016 yılı sonunda AY 186 açmasının doğu kesiminde kazılan bir seramik fırın üzerinde yapılan arkeometrik araştırmalara odaklanmaktadır. Seramik fırını, Geç Tunç Çağı (MÖ 1450-1200)’na ait seramik malzeme grubu ile ilişkilidir. Fırında bol miktarda kırık kap parçaları ve seramik cüruflar bulunmuştur. Çalışmada, arkeometrik karakterizasyon için seramik buluntular arasından üç adet seramik cüruf seçilmiştir. Bu cüruflar morfolojik ve mineralojik karakterizasyonları belirlemek amacıyla optik mikroskop (OM) ve X-ışını kırınımı (XRD) yardımıyla analiz edilmiştir.

AY 186/1, AY 186/7 ve AY 186/11 kodlu örneklerin XRD analizleri ile kuvars (SiO₂), labradorit ((Ca,Na)[Al (Al, Si)Si₂O₈]), diyopsit (CaMg[Si₂O₆]), albit (NaAlSi₃O₈), anortit (CaAl₂Si₂O₈) ve ojit ((Ca,Na) (Mg,Fe,Al,Ti) [(Si, Al)₂O₆]) minerallerinin varlığı saptanmıştır. Cüruflarda yeni mineral oluşumların varlığı, seramiklerin fırınlama sıcaklıkları ve hammaddelerinin mineralojik bileşimi ile ilgilidir. Çalışmada tespit edilen bu fazlara göre seramik curufların pişirim sıcaklığının yaklaşık 900-950 °C olduğu tahmin edilmektedir. Örneklerde vitrifikasyon düzeyinin yüksek olduğu görülmektedir. Ayrıca, seramik cüruflarda önemli miktarda kapalı gözenekler tespit edilmiştir. Bu gözenekler kullanılan hammaddelere, fırın atmosferine, fırında pişirme sıcaklığına ve fırının sürekli kullanımına bağlı olarak gelişmektedir.

Çalışmada sunulan bu sonuçlar, Çukurova Üniversitesi tarafından finanse edilen “Tatarlı Höyük’te Hitit Dönemi’ne Ait Bir Seramik Atölyesinden Çıkan Bazı Buluntuların Karakterizasyonu” başlıklı geniş araştırma projemizin bir parçasıdır (Proje ID: 9673).

Anahtar Kelimeler: Arkeolojik Seramikler, Arkeometri, Karakterizasyon, Çömlek Fırını, Geç Tunç Çağı

1 Introduction

Ceramics for all periods since the Neolithic age are common in many archaeological sites and they have survived to the present day. The pottery fragments recovered from the excavations are more preserved than textiles, leath-er, wood and even metal and are very resistant to the physical, chemical and biological changes they were exposed to after deposition. After deposition, the properties of ceramics may vary over time and from one settlement area

* The authors are thankfull to the Çukurova University Scientific Research Projects Coordination Unit for financial support and editorial board for kindly inviting them to contribute to this publication in memory of Hayriye Akıl.

** Asst. Prof. Nergis Kılınç-Mirdalı, Çukurova University, Faculty of Fine Arts, Department of Ceramic, Saricam/Adana/TURKEY; nkilinc@cu.edu.tr Assoc. Prof. K. Serdar Girginer, Çukurova University, Faculty of Science and Letters, Department of Archaeology, Saricam/Adana/TURKEY; sergir@cu.edu.tr

Research Asist. Özlem Oyman-Girginer Çukurova University, Faculty of Science and Letters, Department of Archaeology, Saricam/Adana/ TURKEY; ogirginer@cu.edu.tr

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310 MORS IMMATURA Amanosların Gölgesinde Hayriye Akıl Anı Kitabı | In the Shadow of Amanus in Memorian Hayriye Akıl

to another depending on the deposition and the environmental conditions1_{. Ceramics found in archaeological}

excavations are one of the major sources of our knowledge to understand the transfer of information among civilizations from past to present. Besides typological research (e.g. ceramic seriation, functional studies, etc.) archaeometric investigations conducted on ceramics open a new gate to comprehend production technology, function of the wares, and in some cases ceramic production center and the age of ceramic finding.

Tatarlı Höyük is one of our important archaeological sites located on fertile alluvial soil. Its location interlinking coastal and northern Syria, Levantine and Cilicia to Central Anatolia prompts its strategic importance2_{. Its}

stra-tegic location surrounded by abundant water resources must have been the reason of its long history spanning a period from the Neolithic to the Late Hellenistic. Therefore, due to both its location and the abundance of water resources in its vicinity, it has been inhabited from the Neolithic Period to the Late Hellenistic Period3_.

The site is in the middle of important trade routes, Osmaniye-Toprakkale and west-north west and north of Amanous Mountains are about 10 km western part of the site. It locates at the north of the village of Tatarlı, in the Ceyhan district of Adana province, about 5 km from Mustafabeyli district and shown in Fig. 1. The settlement is established on basaltic rocks at an average height of 37 m, south-southwest of the village of Tatarlı. The site has at least 250x360 m the upper city in size; yet, considering also the size of its lower city the settlement is tought to be much larger. It is located about 15-20 km from the Amanos Mountains, east of Çukurova. The Amanos Moun-tains serves as a landmark for Mesopotamia and Northern Syria, which begin at the eastern part of this mountain belt. This area was particularly important for the civilizations/powers of the 2nd_{millennium BC}4_{; and it became a}

land of struggles due to its resourcefull and strategic advantages. For example, due to the special geological struc-ture, there are numerous water sources in the region and around the mound. Even today, tehese water sources meet the needs of Ceyhan and its villages5_{. This water abundance makes the site also viable for a sacred nature of}

the city during the 2nd_{millennium BC, the Iron Age and the Hellenistic period}6_.

2 Experimental

During the 2016 excavation season, a large number of potsherds was unearthed in and around the ceramic kiln which was dated at the Late Bronze Age II (1450-1200 BC) (Fig. 2) This kiln shows significant similarities with the Late Bronze Age kilns of northern Syria and Northern Mesopotamia7_{. In this study, three ceramic slag}

sam-ples (AY 186/1, AY 186/7 and AY 186/11) are selected randomly from trench AY 186 locating at the northwestern part of the mound.

The samples were initially photographed and examined with optical microscopy (hereafter; OM) and X-ray diff-raction (hereafter; XRD). The general body views and textural structure of ceramic slags from the surface were examined via OM by using an Olympus SC50. Mineralogical compositions were determined by Panalytical/Em-pyrean model XRD equipped with Cu Kα radiation. Data were collected at 45 kV and 40 mA in the 5-90° 2θ range with a 0.0130° 2θ step size and a countinuous scan type. Ceramic slag samples were milled in an agate mortar for 20 min before subjected to XRD analysis.

1 Hunt 2017, 233.

2 Dardeniz – Girginer – Girginer-Oyman 2018, 118. 3 Girginer – Girginer-Oyman - Akıl 2010, 466-467. 4 Girginer – Girginer-Oyman – Akıl, op.cit, 453-455. 5 Girginer – Girginer-Oyman – Akıl, op.cit, 465-466. 6 Girginer – Girginer-Oyman - Akıl 2011, 134. 7 Dardeniz – Girginer – Girginer-Oyman, op.cit., 122.

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N. Kılınç-Mirdalı - K. S. Girginer - Ö. Oyman-Girginer | Optical Microscopy (OM) and X-Ray Diffraction (XRD) Studies of Ceramic Slag Samples from Tatarlı Höyük (Adana, Turkey) 311

3 Results and Discussion

In this work, a total of three samples, from Tatarlı Höyük, labeled as AY 186/1, AY 186/7 and AY 186/11 respec-tively were analysed with the aid of OM and XRD. By analyzing the morphology and mineralogical composition of the ceramic slag collected from a kiln context, various microstructures, information on the processes that have occurred within the ceramic body and the nature of the minerals were investigated.

The evaluation of the samples from Tatarlı Höyük requires an understanding of local and regional clay deposits. The site is on basaltic rocks. This reinforces the possibility that the pottery produced here is also made of clayey materials containing basaltic rocks and plagioclases, which are the alteration product of basalts. Basaltic miner-als are dark colored and dense looking thin crystalline rocks consisting of plagioclase and augite [(Ca, Na)(Mg, Fe, Al, Ti)(Si, Al)₂O₆]. Plagioclase is the name of the mineral feldspar, which ranges from albite (NaAlSi₃O₈) to anorthite (CaAl₂Si₂O₈) that have the same formula but whose sodium and calcium percentages vary compared to each other.8_{Sodic plagioclase is found in granite and metamorphic rocks, while calcic plagioclase is found in lava}

and basic rocks. The normal feldspar of basalts is labradorite (Na, Ca)(Al, Si)₄O₈)9_.

The archaeometric investigations conducted on the samples confirm existence of these minerals thus linking the pottery production to the local raw materials.

Ceramic slag images (AY 186/1, AY 186/7 ve AY 186/11) are given in Fig. 3. AY 186/7 and AY 186/11 are fused and AY 186/1 is semi-fused.

Crystal phases occurring in ceramics are associated with maximum firing temperature and duration of exposure to temperatures as a result of solid or gaseous reactions during the firing process. In this study, the phases such as anorthite, albite, labradorite, augite and diopside were determined by XRD, which must be results of physico-chemical reactions during the firing process.

Mineralogical results of samples obtained by XRD analyses summarized in the Table 1.

The formation of such phases provides important information about the raw materials used and firing operation of ceramics. In addition, we can obtain information about the firing temperature by the presence or absence of the glassy matrix formed during the firing process10_{. The results indicate that, clayey material containing brown}

and black basalts, plagioclase and volcanic ash might have been incorporated in variable quantity as temper to the ceramic paste. However, it should be noted that the firing atmosphere is a parameter to be considered for all ceramic slags. All of the ceramic slags must have been fired in a reduced kiln atmosphere. In reducing conditions, carbon accumulation on the surface closes the pores in the ceramic surface resulting a decrease in permeability. The OM images demonstrate ceramic slags contain of a network of relatively different sized, spherical and mostly closed pores (Fig. 4).

Quartz is the remaining phase from the raw material is determined in samples AY 186/1 and AY 186/11, even in low quantities. However, no quartz is detected in AY 186/7. This is because the quartz takes place as a new phase within the newly formed crystal diopside. AY 186/1 includes labrodite particle inclusions, which might have been

8 Toktamış –Toktamış – Yazıcı 2017, 109. 9 Velde 1999, 21.

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added as temper. AY 186/7 shows oxidation at the as a result of the cooling process. Large sized albite inclusions are also the remaining phase from the raw material and green/black glassy matrix are present due to vitrification. The presence of diopside suggests that ceramic slags AY 186/1 and AY 186/7 were fired above 900°C. AY 186/11 is including black basalt particles with black glassy matrix. AY 186/11 however contains augite and anorthite minerals. So, AY 186/11 might have been fired at above 950°C. Augite mineral is formed by the reaction of car-bonated raw materials with clay and quartz respectively. In addition, the absence of clay minerals in all ceramic slag samples is an indication that the firing temperatures are above 900° C.

There are significiant amonut of closed pores in the ceramic slags. AY 186/11 is more porous than the others. The closed pores occur due to the raw materials used in the ceramics, oxidizing-reducing conditions and firing temperature in the kiln along with continious use of the kiln. Porosity gives us information about the produc-tion process of ceramics and the raw materials used11_{. Due to decomposition of Fe}2+_{in the reduced atmosphere,}

or crystalline phases with a low melting temperature form eutectic and vitrification levels of the samples are increased.

4 Conclusions

This study presents the results of OM and XRD methods on ceramic slags found in and around the Tatarlı Höyük pottery kiln. The inclusions and temper detected in the samples indicate use of local resources.

The geological structure of the region demonstrates basaltic rocks spreading over a wide area. The presence of minerals such as albite, anorthite, augite and diopside in the ceramic slags suggest that the raw materials of this region have been possibly the resource areas of the potters/crafts and the firing temperatures were most probably at the ranges of 900-950°C.

The existence of a kiln with the new mineralogical phases determined via archaeometric analysis has reinforced the possibility that this region may be a manufacturing center (might be involved in experimentation in produc-tion). While the production potential of Tatarlı Höyük appears undeniable, extensive amounts of pottery reper-torie dated to different archaeological periods should be investigated with caution before asserting them a local or imported origin.

However, the answer to the question of whether vessels from different periods recovered in archaeological exca-vations since 2007 may be domestic or imported is hidden in extensive provenance studies.

Three samples analysed in this research yielded identical morphology and composition possibly due to same production conditions. OM images and XRD results helped us to estimate the technology used in the kilns for the firing temperature/atmosphere and the raw materials.

Yet, the archaeometric analysis presented here are far beyond being conclusive for the bigger questionrelated to resource and origin, research focusing on the geology around the Tatarlı Höyük.

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Dardeniz – Girginer – Girginer-Oyman 2018

Gonca Dardeniz – K. Serdar Girginer – Özlem Oyman-Girginer, 2018. “A Pottery Kiln from Tatarlı Höyük (Adana, Turkey) and its Implications for Late Bronze Age Pottery Production in Cilicia and Beyond”, Adalya 21, 118-134.

Girginer – Girginer-Oyman – Akıl 2010

K. Serdar Girginer – Özlem Oyman-Girginer – Hayriye Akıl, “Tatarlı Höyük (Ceyhan) Kazısı: İlk İki Dönem”, 31. Kazı Sonuçları Toplantısı 3, 453-476.

Girginer – Girginer-Oyman – Akıl 2011

K. Serdar Girginer – Özlem Oyman-Girginer – Hayriye Akıl, “Tatarlı Höyük Kazısı 2009-2010”,

ANMED Anadolu Akdenizi Arkeoloji Haberleri 9, 128-135.

Hunt 2017 A. M. V. Hunt, The Oxford Handbook of Archaeological Ceramic Analysis, Oxford University Press, Oxford.

Santacreu 2014 Daniel Albero Santacreu, Materiality, Techniques and Society in Pottery Production-the Technological

Study of Archaelogical Ceramics Through Paste Analysis, De Gruyter Open.

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S. Rutishauser – R. Rosenbauer – S. Erasmi – R. Buchbach, “SARchaeology. Detecting Palaeochannels Based on High Resolution Radar Data and Their Impact of Changes in the Settlement Pattern in Cilicia (Turkey)”, Geosciences 7/4, 109 , 1-20.

Toktamış – Toktamış – Yazıcı 2017

Dilek Toktamış – Hüseyin Toktamış – A. Necmeddin Yazıcı, “Thermoluminescence behavior of basaltic rocks collected in southeasternregion of Turkey”, Applied Radiation and Isotopes 12, 109–115. Velde – Druc 1999 B. Velde Toktamış – I. C. Druc, Archaeological Ceramic Materials - Origin and Utilization, Paris.

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Tablo 1 Mineralogical compositions of the ceramic slag samples determined with XRD analysis.

Sample No Quartz Labradorite Diopside Albite Augite Anorthite

AY 186/1 + ++ +++ -

-AY 186/7 - - +++ ++ -

-AY 186/11 + - - - ++ +++

Figure 1 Tophographic map of Tatarlı Höyük and the important archaeological sites within the vicinity.

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Figure 2 Ceramic kiln unearted from the eastern sector of Tatrlı Höyük at trench AY186; a) Shematic overview of the Tatarlı pottery kiln with

possible extensions and the archaeological features (Dardeniz – Girginer – Girginer-Oyman 2018, 132). b) Photograph of archaeological context of the ceramic kiln.

Figure 3 Representative images of ceramic slag samples (AY 186/1, AY 186/7, AY 186/11)

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