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This volume was edited by Rebecca B. Scott, Dennis Braekmans, Mike Carremans and Patrick Degryse Cover design by Mike Carremans ISBN 978 94 6165 120 4 D/2014/1869/27 © 2014 (Centre for Archaeological Sciences, KU Leuven, Celestijnenlaan 200E, 3001 Leuven, Belgium) All rights reserved. Except in those cases expressly determined by law, no part of this publication may be multiplied, saved in an automated datafile or made public in any way whatsoever without the express prior written consent of the publishers. !
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Table of contents Stone, Plaster and Pigments…………………………………………………………………………….7 Archaeochronometry……………………………………………………………………………………47 Radiocarbon and Historical Chronologies……………………………………………………………71 Metals and Metallurgical Ceramics……………………………………………………………………79 Biomaterials and Bioarchaeology……………………………………………………………………139 Ceramics, Glazes, Glass and Vitreous Materials…………………………………………………..147 Remote Sensing, Geophysical Prospection and Field Archaeology……………………………..291 Human-Environment Interactions……………………………………………………………………311 Colour and Culture…………………………………………………………………………………….317 Index…………………………………………………………………………………………………….322
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Organization
Standing Committee President: M.S. Tite (Oxford) Chairman: Y. Maniatis (Athens) Members: L. Barba (Mexico City) J.-F. Moreau (Chicoutimi) K.T. Biro (Budapest) J. Pérez-Arantegui (Zaragoza) R.M. Farquahar (Toronto)
R.H.Tykot (Tampa) H. Kars (Amsterdam) Ch. Wang (Beijing) I. Memmi Turbanti (Siena) S.U. Wisseman (Urbana)
Organizing Committee: Patrick Degryse (KU Leuven) – chairman Koen Janssens (U.Antwerpen) Dennis Braekmans (KU Leuven) – secretary
Peter Vandenabeele (U.Gent) Frank Vanhaecke (U.Gent) David Strivay (U.Lg.)
Convenors: Stone, Plaster and Pigments (Technology and Provenance) Yannis Maniatis and Robert H. Tykot Archaeochronometry Marco Martini Radiocarbon and Historical Chronologies Christopher Ramsey Metals and Metallurgical Ceramics (Technology and Provenance) Thilo Rehren Biomaterials and Bioarchaeology Henk Kars Ceramics, Glazes, Glass and Vitreous Materials (Technology and Provenance) Josefina Pérez-Arantegui and Michael Tite Remote Sensing, Geophysical Prospection and Field Archaeology Luis Barba Human-Environment Interactions Mark Pollard Colour and Culture Patrick Degryse
Proceedings of the 39th
International Symposium for Archaeometry, Leuven (2012) 060-065
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Optically stimulated luminescence chronology and characterisation of pottery sherds
from Maligrad, Albania
A. Oikonomou1, K. Stamoulis
2, P. Lera
3, S. Oikonomidis
4,
A. Papayiannis5, A. Tsonos
6, C. Papachristodoulou
7, K. Ioannides
2,7*
1. Department of Protection and Conservation of Cultural Heritage, TEI of Ionian Islands, Zante, Greece,
2. ArchaeometryCenter, The University of Ioannina, Ioannina, Greece,
[email protected], [email protected]
3. Institute of Archaeology, Center of Albanological Studies, Tirana, Albania4
4. University College for Global Studies Abroad, Philadelphia, U.S.A. Arcadia,
5. Fifth Ephorate of Prehistoric and Classical Antiquities, Sparta, Greece,
6. Dept. of History-Archaeology, University of Ioannina, Greece,
7. Department of Physics, The University of Ioannina, Ioannina, Greece,
[email protected], [email protected]!
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ABSTRACT This work reports the results of an ongoing research using the optically stimulated luminescence (OSL) chronometry methodology and the radioisotope-induced energy-dispersive X-ray fluorescence (EDXRF) spectroscopy for the characterization of pottery sherds recovered from Maligrad, (NE Albania). Forty eight pottery sherds and surrounding sediment samples were collected from Maligrad. All samples were sent for analysis to the laboratories of the Archaeometry Centre of the University of Ioannina, Greece. A group of samples (n=5) were dated using the Riso TL/OSL DA-20 reader. The single-aliquot regenerative-dose (SAR) protocol was followed for the equivalent dose (De) determination. The OSL natural signal was obtained by stimulating the samples with blue LEDs. Also, each sample was repeatedly irradiated for various periods of time with a
90Sr/
90Y source
with a calibrated dose rate of 0.0982 ± 0.0002 Gy/s. To determine the dose rates, the natural radioactivity of sediments from the surroundings of the original sample location were assessed, due to potassium 40 (
40K) and the
uranium (U) and thorium (Th) series, using gamma spectrometry with a counting system based on a HPGe detector. A first result for the estimated age of the sherd samples is 190 BCE ± 150 years. According to archeological data collected during the seasons 2009-2011, the oldest finds belong to the Middle Bronze Age and are related to a settlement of the same period. Finally, the elemental composition of forty eight ceramic bodies was studied using radioisotope-induced EDXRF spectroscopy. The multivariate statistical treatment of the elemental data revealed different compositional groups. KEYWORDS EDXRF, OSL, PCA, pottery.
Introduction Maligrad, a rocky islet of karstic tectonic formation, is the smaller of the two islands of the Great Prespa Lake situated in SE Albania (Fig. 1). The Institute for Transbalkanic Cultural Cooperation (ITCC) and the Institute of Archaeology of Tirana have been conducting a multi-disciplinary archaeological research on Maligrad since 2009. The main objectives of this Greek-Albanian archaeological expedition are the combined study of both the islet and the neighbouring area along the coastline of Prespa and the definition of the life span of this specific area (Lera P., 2009, 2010, 2011). Maligrad represents a starting point for further scientific research because of its strategic location at the westernmost part of the Great Prespa Lake, near the most crucial ancient roads between Macedonia and Illyria. Maligrad’s archaeology has been, since at least the Mid Bronze Age, strongly connected with the wider area of the geographic and cultural frontier of the Great Prespa Lake region. The earliest archaeological finds of the Greek-Albanian Archaeological Expedition belong to this chronological horizon, while a continuous stratigraphic sequence throughout the Early Iron Age and the first millennium BCE makes the island a unique point of archaeological reference for the nearby district. The CE architectural phases are represented well through the 3
rd, 4
th
and the late 5th
century. The peaceful survival of the settlement at the top of Maligrad was ended in the first decades of the 6
th century CE when the settlement was
destroyed by factors external to the region. An improvised cemetery took its place, all over the highest part of the island. Architectural remains, pottery, metallic tools and weapons provide a clear archaeological environment on Maligrad, while the palaeo-anthropological and palaeo-zoological finds still have to be investigated. In this framework, the present study reports preliminary results from the archaeometric analysis of ceramic samples from the Maligrad islet.
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Fig. 1. Geophysical map of greater Korçë area indicating
the location of the Maligrad islet. Materials and Methods The ceramic collection The pottery samples from Maligrad belong to different chronological horizons, with the oldest, hand-made pottery of the Late Bronze Age and sherds of the Roman and Late Roman period, collected from the cemetery of the early 6
th
century CE. The studied samples (n=48) were recovered, both from excavations at the plateau of the islet and from the survey along its coastline. The sherds were classified according to their method of manufacturing as wheel made and handmade pottery. A selection of five samples were dated by means of the Optically Stimulated Luminescence (OSL) technique, while the entire sample set was characterized by means of EDXRF. The EDXRF elemental data were further treated statistically by Principal Component Analysis (PCA). Optical Stimulated Luminescence Small portions were extracted carefully from the inner part of the head cover, in order not to be mixed with parts from the outer of the sample. These portions were crushed and sieved and grains of 100-150µm were subsequently treated with a HCl solution to eliminate carbonates, a H2O2 solution to oxidize any organic content and finally a HF solution to dissolve any feldspars and etch the outer part of the remaining SiO2 grains. The final samples were placed on small stainless steel discs and the OSL signal was recorded along with repeatedly delivered doses, in order to construct the growth curve of each disc. Details of the measurement conditions along with the OSL protocol used for age determination are given at Oikonomou et al in press. Energy-Dispersive X-ray fluorescence The sample preparation involved cleaning and abrading the ceramic surface, extracting a 0.3g piece, grinding and pressing to a 12mm diameter pellet. In the XRF setup,
annular radio-isotopic sources (109
Cd and 241
Am) were used for sample excitation and a Si(Li) detector was employed for the detection of X-rays. Spectra were analyzed using the WinQXAS software and the IAEA SOIL7 Standard Reference Material was used for quantitative analysis. Results and Discussion OSL Dating A large ceramic head cover excavated from a grave and four pottery sherds were analyzed to determine their age with the OSL dating technique. The equivalent dose was calculated using the growth curve. In the case of the pottery sherds, the outer part was carefully removed and the inner part was subsequently crushed and treated as described above. The calculated ages are presented in Table 1 and the corresponding histograms are shown in Figs. 2 and 3.
-3000 -2000 -1000 0 1000 2000
0
7
14
21
28
Fre
qu
en
cy
Age
Head Cover
BCE CE
Fig. 2. Histogram of calculated ages for the head cover
sample. Vertical line represent year 0, on the left ages are
BCE and on the right are CE.
Also, radioactivity of the surrounding soil and the corresponding calculated dose rate along with equivalent doses and calculated mean ages are given in Table 2. The ages calculated for the head cover are well distributed around the value of 190 BCE ± 150 years, while the results for the sherd samples tend to be dispersed in a wide range of values up to 2880 BCE, with some of the ages being very young. These young ages indicate that there was not a good separation of the inner part of the sherds from the discarded outer part, since the outer part was exposed to sun light and the OSL signal faded out. It can be noted that the dispersion of calculated ages is particularly pronounced for sherds M27 and M33.
Table 1. Ranges (min, max) and mean values of ages with
the associated standard error. See text for further
explanation.
Both samples were characterized macroscopically by the presence of large inorganic inclusions, which are usually
Min Max Mean ! Mean (>
500) !
Head Cover 520 BCE 80 CE 190 BCE 150 - -
M26 900 CE 1990 CE 1390 CE 370 1180 CE 200
M27 1020 BCE 2010 CE 810 CE 1040 290 CE 880
M33 2880 BCE 2000 CE 20 CE 2000 1350 BCE 1430
M34 530 BCE 1590 CE 460 CE 770 90 CE 440
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associated with a wide dispersion of calculated ages. This is especially true in the case of ceramics that were not well fired (note that sherds M27 and M33 belong to Group A identified by PCA; see below). The dispersion of calculated ages is narrower for sherds M26 and M34, which are characterized by a more homogeneous ceramic body (PCA Group B; see below).
-3000 -2000 -1000 0 1000 2000
0
2
4
6
8
Age
M26 BCE CE
-3000 -2000 -1000 0 1000 2000
0
2
4
6
M27 BCE CE
-3000 -2000 -1000 0 1000 2000
0
2
4
6
Frequency
M33 BCE CE
-3000 -2000 -1000 0 1000 2000
0
2
4
6
M34 BCE CE
Fig. 3. Histogram of calculated ages for the sherd samples.
Vertical lines represent year 0, on the left ages are BCE and
on the right are CE.
Excluding ages younger than 500 years, the remaining data show a mean value of 1180 CE ± 200 years for sherd M26, 290 CE ± 880 years for sherd M27, 1350 BCE ± 1430 years for sherd M33 and 90 CE ± 440 years for sherd M34. It may therefore be suggested that sherds M27 and M34 belong to the same period as the head cover, while sherds M26 and M33 are about 1350 years younger and 1150 years older, respectively, compared to the head cover. Overall, the OSL findings confirm that this archaeological site has been used as a settlement over a wide span of centuries. Compositional data and statistical analysis The concentrations of 4 minor and 14 trace elements were determined by EDXRF spectrometry. Maximum, minimum and mean concentration values are shown in Table 3 while the full elemental concentrations are shown in Table 4. To identify samples of similar composition, the elemental data were logarithmically transformed and Principal Component Analysis was carried out using the STATISTICA 8 Statistical Software. A total of 14 elemental variables were retained in the analysis; Mn, Pb, Cu and Ni data were excluded due to poor counting statistics. The PC1-PC2 score plot illustrated in Fig. 4 shows a widely scattered compositional pattern. Table 3. Mean value, standard deviation (S.D.), minimum
and maximum values of the elemental concentrations
obtained from the XRF measurements (values in ppm, unless
otherwise indicated).
Mean
Value S.D. Min. Max.
K (%) 2.0 0.8 0.7 3.9
Ca (%) 1.6 1.0 0.5 7.4
Ti (%) 0.9 0.4 0.3 1.9
Fe (%) 5.4 1.4 2.7 10.2
Mn 709 491 28 1916
Zn 170 70 77 370
Rb 157 43 52 257
Sr 313 239 56 853
Y 44 25 19 158
Zr 247 53 130 399
Nb 29 9 11 55
Pb 33 22 6 166
Ba 1030 469 280 2233
La 58 25 20 135
Ce 110 44 53 283
Nd 75 31 25 185
Cu 14 5 7 26
Ni 69 63 9 306
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Table 2. Equivalent doses (mean ± 1!), radioactivities, total dose rates and calculated ages of surrounding head cover and
sherds collected at Maligrand.
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However, two distinct chemical groups, group A and B, may be suggested, as indicated with green and red ellipses, respectively. The separation of these two groups is due to differences in their Sr content (Fig. 4, inset); mean Sr concentrations amount to 614ppm for Group A and 136ppm for Group B. Sr is an element typically associated with Ca. Limestones, the main source of Ca, exhibit high variation in Sr values (Mabrouk et al 2006). Also their concentration in Ca ranges from 0.4% to 2.4% and is generally characterized as low calcerous in nature. Furthermore, Rb content ranges from 70ppm to 257ppm. These two elements are known to scatter considerably even in pottery from a common origin and their spread mainly reflects the use of different clay fractions, indicating different manufacturing procedures (Papachristodoulou et al 2010).
Fig. 4. A PC1-PC2 scatter-plot of the analyzed sherds. The
elemental variables loading-plot is shown in the inset.
From the archaeological evidence, the majority of the group A samples contain inclusions of inorganic material in their main body. It is suggested that the concentration of Sr in the Group A samples is derived from such inclusions. In the PC2-PC3 score plot (Fig. 5), a group of samples (Group C, blue ellipse) is separated, mainly due to low Zn and Ti and to a lesser extent due to high K levels. According to the archaeological evidence, these samples are wheel-made and date from a period subsequent to the handmade ones (Groups A and B). It should also be noted that they were extracted from the survey along the coastline of the islet. Differences in Zn and Ti may possibly provide a geochemical signature, as these elements are highly immobile and tend to concentrate in the clay fraction. The variation in K content may be associated with post-burial alterations resulting from the exposure of these samples to different environmental conditions. Ongoing analysis of ceramics from Maligrad is expected to provide additional archaeometric insight to the history of the area. Conclusions
OSL measurements on a group of ceramic samples from Maligrad, Albania, provided the date of a ceramic head cover with the value of 190 BCE ± 150 years, giving the indirect dating of the burial in this period of time. Also, the dating of the rest of the ceramics tended to be dispersed in a wide range of values up to 2900 years BCE, with some of the ages being very young, indicating that there was not a good separation of the inner part of the sherds from the
discarded outer part, since the outer part was exposed to sun light and the OSL signal faded out. Furthermore, forty eight samples where studied by means of EDXRF and PCA in order to extract information about pottery provenance and manufacturing process. From the statistical analysis two different compositional groups were revealed indicating a different manufacturing procedure.
Acknowledgements All analytical measurements were carried out in the OSL laboratory of the Centre of Archaeometry and in the EDXRF laboratory unit, at the University of Ioannina.
Fig. 5. A PC2-PC3 scatter-plot of the analyzed sherds. The
elemental variables loading-plot is shown in the inset.
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! 64
Table 4. Elemental concentrations mean value, standard deviation (S.D.), minimum and maximum values of the elemental
compositions determined through EDXRF spectroscopy (values in ppm, unless otherwise indicated, n.d.: not detected).
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References Aitken, M. J., 1998. An Introduction to Optical Dating. Oxford
University Press, Oxford. Guerin G., Mercier N., Adamiec G. 2011.Dose rate conversion
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