See discussions, stats, and author profiles for this publication at: https://www.researchgate.net/publication/230283873 Cypriot Byzantine glazed pottery: a study of the Paphos workshops Article in Archaeometry · October 2009 DOI: 10.1111/j.1475-4754.2009.00502.x CITATIONS READS 23 514 6 authors, including: Andreas Charalambous Anastasios Sakalis University of Cyprus General Chemical State Laboratory of Greece 23 PUBLICATIONS 238 CITATIONS 24 PUBLICATIONS 465 CITATIONS SEE PROFILE SEE PROFILE Nikolaos Kantiranis Lambrini Papadopoulou Aristotle University of Thessaloniki Aristotle University of Thessaloniki 214 PUBLICATIONS 1,698 CITATIONS 174 PUBLICATIONS 1,846 CITATIONS SEE PROFILE SEE PROFILE Some of the authors of this publication are also working on these related projects: Environmental Natural Radioactivity studies - Dose Assessment View project NOVEL APPROACHES FOR SURFACE LUMINESCENCE DATING IN ARCHAEOLOGICAL & GEOARCHAEOLOGICAL CASE STUDIES View project All content following this page was uploaded by Andreas Charalambous on 29 April 2020. The user has requested enhancement of the downloaded file. Archaeometry 52, 4 (2010) 628–643 doi: 10.1111/j.1475-4754.2009.00502.x CYPRIOT BYZANTINE GLAZED POTTERY: A STUDY OF THE PAPHOS WORKSHOPS* A. C. CHARALAMBOUS,1,2 A. J. SAKALIS,2 N. A. KANTIRANIS,3 L. C. PAPADOPOULOU,3 N. C. TSIRLIGANIS,2 and J. A. STRATIS1† 1 Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, GR-54124, Thessaloniki, Greece Laboratory of Archaeometry, Cultural and Educational Technology Institute, ‘Athena’ Research Centre, Tsimiski 58, GR-67100, Xanthi, Greece 3 Department of Mineralogy-Petrology-Economic Geology, Aristotle University, GR-54124, Thessaloniki, Greece 2 Twenty-five samples of Byzantine glazed pottery from two archaeological sites between Limassol and Paphos region (Cyprus), dated between the 12th and 15th century AD were studied using micro X-ray fluorescence spectroscopy, scanning electron microscopy and X-ray diffraction analysis. It was found that all the glazes contain lead, following the main manufacturing process of medieval pottery in the Mediterranean territory, while some of them contain tin, possibly for better opacity. Furthermore, it is shown that copper, iron and cobalt with nickel are responsible for the decoration colours. Finally, the application of principal component analysis revealed significant differentiation for some of the samples. KEYWORDS: CYPRUS, MICRO X-RAY FLUORESCENCE SPECTROSCOPY, X-RAY DIFFRACTION ANALYSIS, SCANNING ELECTRON MICROSCOPY, PRINCIPAL COMPONENT ANALYSIS INTRODUCTION Cyprus presents a long tradition in glazed pottery, mainly dated from the 12th to the 15th century ad. Archaeological findings confirm the presence of several glazed pottery workshops in many areas of Cyprus. The most important workshops were in the area of Paphos, on the southwestern side of the island, and in the area of Lapithos, on the northern side of the island, near the city of Kyrenia. The specific workshops of Paphos and Lapithos were active from the 12th century and some of them, especially in the area of Lapithos, until the 19th century. Because of the location of the island, between three continents and near the Middle East, occupation by the Franks (1192–1489) and the Venetians (1489–1572), and due to trade, the manufacture and the decoration technology of the local glazed pottery exhibits significant influences from these areas (Papanikola-Bakirtzis 1996). Pottery receives more attention perhaps than any other type of artefact since large amounts are continuously excavated at archaeological sites. Its typological and analytical study enables the investigation of many interesting aspects of ancient culture, trade and technology (Rice 1987). Lead-glazed pottery was widely spread around the regions of the Mediterranean Sea. The main characteristic of the 12th century Byzantine glazed pottery, developed mainly within the Byzantine Empire, was the application of the sgraffito technique. Sgraffito is the term used to describe redware pottery in which, with the aid of a sharp tool, decorations have been *Received 7 November 2008; accepted 27 June 2009 †Corresponding author © University of Oxford, 2009 Cypriot Byzantine glazed pottery 629 scratched into a thin layer of clay slip. Byzantine potters used to apply a coating of white slip and a colourless lead (Pb) glaze over the ceramic body, and further decorated the surfaces with a colourful variety of incised and painted designs (Papanikola-Bakirtzis 1999). The Byzantine Pb glazes are easily formed, obtain lustrousness and opacity at low temperatures and are also easily coloured with oxides of other metals, such as copper (Cu) and iron (Fe). The main characteristics of the Paphos workshops are the reddish clay ceramics with white slip coating and mainly sgraffito decoration with a glaze of green, yellow, brown and orange colour. Cypriot glazed pottery should be considered and studied as a branch of Byzantine glazed pottery displaying the same technology and decorative techniques as pottery in Byzantium (Papanikola-Bakirtzis 1996). An important category of glazed pottery is the tin-opacified glazes, originally produced in Iraq during the eighth century ad (Mason and Tite 1997). Initially, tin-opacified glazes were alkali glazes containing only 1–2% PbO. However, in Spain and for the early production of Italian majolica, the lead oxide contents tended to be higher (up to about 55% PbO) with lower alkali contents (down to about 3% Na2O plus K2O) (Tite et al. 1998). Glazed pottery from Cyprus has not attracted much interest in terms of analytical studies. To date, only a few studies on the provenance of the Cypriot ceramics have been performed. Specifically, instrumental neutron activation analysis (INAA) was used to study pottery samples from southwestern Cyprus (including the Paphos area) obtained from 38 archaeological sites, dated from the Neolithic through to the Roman period. The results indicated that the large majority of the ceramics are likely to be local products (King et al. 1986; King 1987). Furthermore, Megaw and Jones studied glazed ceramic material dated from the fifth to the 15th century from three regions in Cyprus (Lapithos, Lemba and Dhiorios) with optical emission spectroscopy, revealing discrimination of the three regions (Megaw and Jones 1983; Jones 1986). Micro X-ray fluorescence spectroscopy (m-XRF) is a non-destructive, fast, multi-elemental technique, which analyses the surface layer and determines major, minor and trace elements in thin and thick samples of all sizes and forms (Padilla et al. 2005; Papadopoulou et al. 2006). Together with the micro-XRF technique, X-ray diffraction (XRD) and scanning electron microscopy (SEM-EDS) techniques are widely used to complete an archaeometric characterization of pottery (Rice 1987). In the present work, a portable m-XRF spectrometer is used for the non-destructive analysis of 25 medieval glazed ceramics from two different archaeological sites in Cyprus. Additionally, XRD and SEM-EDS are used to study certain samples in order to confirm the experimental results from m-XRF analysis.The basic aims of this study were: (1) To determine the mineralogical and chemical composition of the ceramic bodies in order to investigate their manufacture technology and the provenance of the specific samples. (2) To determine the chemical composition of the glazes in order to characterize the colours of the decorations. (3) To suggest possible origins of the studied material and to contribute to the explanation of observed technological differences based on existing archaeological knowledge which claims that the material originates from Paphos workshops. Furthermore, the statistical treatment of the quantitative data using multivariate exploratory techniques (principal component analysis, PCA) in combination with the archaeological information provides certain indications concerning the provenance of the studied material and offers possible justifications for any observed discrimination of the material. This study is expected to provide useful knowledge on the local glazed pottery technology. © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 630 A. C. Charalambous et al. EXPERIMENTAL PROCEDURE Description of samples The investigated glazed ceramic sherds were excavated at the Kepir Mosque in the city of Limassol and at the church of Panagia Galactotrofousa in the Fasouri area, 15 km west of Limassol, both located in the south of Cyprus. Kepir Mosque was built during the 16th century near a Byzantine church, while Panagia Galactotrofousa was built during the 11th century. The excavation of the Kepir Mosque was performed in 1993 and the church of Panagia Galactotrofousa in 2002 under the supervision of the Cyprus Department of Antiquities (Prokopiou 1997). The samples are dated between the 12th and the 15th century ad. The archaeologists believe that the origin of the samples is from the Paphos area workshops, due to the similarities in the manufacture technology (plain, painted and especially scraffito decoration with glaze layer mainly on the inner side of the ceramic object) and the colour of the glazes (green, yellow, brown and orange). Quantitative analysis was performed for all the samples by non-destructive means, using m-XRF spectroscopy, while further analysis applying SEM-EDS and XRD techniques was performed on specific samples of interest in order to minimize the destruction of samples. Samples K1–K18 were excavated in the Kepir Mosque, while the remaining samples, K27 –K33, were excavated in Panagia Galactotrofousa (Table 1). The samples were decorated using green, yellow, orange, brown, black and blue glazes, as shown in Table 1. Furthermore, samples K18, K32 and K33 show optical differences in both the clay microstructure and the glaze decoration style compared with all the other samples. Specifically, these samples have painted decoration of blue and light blue, which is typical of Italian majolica pottery. Therefore they could be trade products due to the occupation of Cyprus by Venice during the 15th century. Micro X-ray fluorescence spectroscopy Quantitative analysis of the ceramic bodies was performed using portable m-XRF spectroscopy. The portable m-XRF spectrometer (SPECTRO, COPRA model, Austria) used in this work incorporates a side window X-ray tube with Mo anode (Oxford Instruments, Series 5011 XTF), a straight monocapillary lens and a solid-state Si Peltier-cooled detector (8 mm Be window, 3.5 mm2 active area, 300 mm nominal thickness). The maximum tube voltage is 50 kV and its maximum current is 1 mA. The nominal beam diameter is <150 mm at the position of the sample. The angle of incidence of the primary X-ray beam on the sample surface is 48° (relative to the surface), while the angle between the sample and the detector is 42°. All measurements are performed under atmospheric pressure and no filters were used. The m-XRF measurements were performed in a point scan mode on several points, which were selected to cover the entire surface of the glaze. In particular, three to five measurements were performed on the surface of the glaze-over-paste in all colour areas. Furthermore, three measurements were performed on the ceramic body for each sample, after removal of a small part of the surface ceramic body layer with a drill and a tungsten carbide cutter to eliminate possible surface contamination effects. All samples were cleaned with ultra-pure water and dried in the oven at 110°C. Reported concentrations are mean values of the three or five measurements per sample. The applied voltage was 40 kV, the current 0.7 mA and the measurement time 300 s, based on a preliminary investigation of the optimum experimental parameters. The standard reference material SARM 69 (MINTEK, Republic of South Africa) was used as a calibration standard, while the standard reference material Geostandard VS-N (SARM-CNRS, France) was © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 K.M. K.M. K.M. K.M. K.M. K.M. K.M. K.M. K.M. K.M. K.M. K.M. K.M. K.M. K.M. K.M. K.M. K.M. P.G. P.G. P.G. P.G. P.G. P.G. P.G. K1 K2 K3 K4 K5 K6 K7 K8 K9 K10 K11 K12 K13 K14 K15 K16 K17 K18 K27 K28 K29 K30 K31 K32 K33 K.M. = Kepir Mosque; P.G. = Panagia Galactotrofousa. Excavation area Sample index Reddish-2.5YR 4/8 Reddish-2.5YR 5/6 Reddish-2.5YR 4/6 Whitish-10YR 7/2 Reddish-10R 5/2 Whitish-7.5YR 7/4 Reddish-10R 5/2 Reddish-2.5YR 4/6 Reddish-2.5YR 6/8 Reddish-2.5YR 5/6 Whitish-10YR 8/4 Reddish-2.5YR 4/6 Whitish-10YR 7/4 Reddish-2.5YR 6/6 Reddish-7.5YR 8/4 Reddish-2.5 YR 4/4 Reddish-2.5YR 5/6 Whitish-5Y 9/2 Reddish-2.5YR 6/6 Reddish-5YR 7/8 Reddish-2.5YR 6/6 Reddish-5YR 7/6 Reddish-2.5YR 5/6 Whitish-2.5Y 9/4 Whitish-2.5Y 9/4 Clay colour (Munsell range) Fine grained Coarse grained Fine grained Fine grained Coarse grained Fine grained Coarse grained Coarse grained Fine grained Coarse grained Fine grained Fine grained Coarse grained Fine grained Fine grained Coarse grained Fine grained Fine grained Coarse grained Fine grained Coarse grained Fine grained Fine-grained Fine grained Fine grained Macroscopic characterization Table 1 Description of the studied samples Green glaze Brown and red glaze Brown glaze Orange glaze Yellow, green and brown glaze Yellow glaze Yellow, brown and green glaze with black lines Brown glaze Green and brown glaze Yellow and brown glaze Yellow glaze Yellow and brown glaze with black lines Blue decoration Orange glaze Brown glaze Green and brown glaze with black lines Yellow and brown glaze Blue glaze Green glaze with black lines Yellow and green glaze Brown glaze Yellow and green glaze Yellow glaze Light blue glaze Blue green glaze Glaze decoration Cypriot Byzantine glazed pottery 631 © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 632 A. C. Charalambous et al. used for the quantification of Pb and the standard reference material GBW07706 (China National Analysis Center for Iron and Steel, Beijing) was used for the quantification of tin (Sn). All standard reference materials were prepared in pressed pellets by thoroughly mixing the powder with a cellulose binder in a 4:1 (reference material/binder) ratio, while pressing was performed using an 11-ton hydraulic press (Specac, UK). X-ray spectra were deconvoluted and fitted using a suitable software package (WinAxil v 4.0.1). X-ray diffraction The quantitative mineralogical composition of the samples was determined by powder XRD. Powder XRD analysis was performed using a diffractometer with an Ni-filtered Cu Ka radiation (Philips PW1710, The Netherlands) source on randomly oriented samples. Subsamples were cut off the glazed ceramic samples and powdered in an agate mortar. The samples were scanned over the interval 3–63° 2q at a scanning speed of 1.2°/min. Quantitative estimates of the abundance of the mineral phases were derived from the powdered XRD data, using the intensity of specific reflections, the density and the mass absorption coefficient for Cu Ka radiation for the minerals present. Corrections were made using external standard mixtures of the detected mineral phases (Guinier 1963; Kantiranis et al. 2004). Amorphous phase content was calculated according to the methodology proposed by Kantiranis et al. (2004). The detection limit for crystalline and amorphous phases was 12% w/w. Scanning electron microscopy The morphology and chemical microanalysis of the studied glazed pottery sherds was performed on the outer surface and on polished sections by SEM-EDS (Jeol JSM-840, Japan), a scanning electron microscope, equipped with an Oxford ISIS300 Energy Dispersion Analyser. To minimize volatilization of alkalis in the studied samples, the electron beam spot size was enlarged and the counting time decreased. The measuring conditions were: voltage 15 kV, electron beam current ~3 nA and spot size 1 mm2, while counting time was 60 s. Different minerals (micas, carbonates, feldspars) and pure metals were used as probe standards. RESULTS AND DISCUSSION Micro X-ray fluorescence spectroscopy Most of the ceramic bodies have a reddish colour while samples K4, K6, K11, K13, K18, K32 and K33 are characterized by a yellow-white colour (see Table 1). The m-XRF spectra of Figure 1 present the differences between the ceramic body and the glaze composition of sample K18. The main differences were the high amounts of Ca, Ti, Fe and Sr in the ceramic body and the high amounts of S and Pb in the glaze. These significant differences exist in the composition of the ceramic body and the glaze in all samples. All ceramic bodies contain a small amount of Pb as a result of the leaching of Pb from the transparent glaze during firing (Fabbri et al. 2000). The main characteristic of the glazes is the high amount of Pb that follows the main manufacturing trend in Cyprus during the studied Byzantine period (12th–15th centuries ad). The two primary methods of producing lead glazes were either to apply Pb, PbO to the surface of the pottery body, or to apply a mixture of PbO and silica (Tite et al. 1998). The presence of significant amounts of Sn in the ceramic body (0.08–0.18% w/w) of samples K18, © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 Cypriot Byzantine glazed pottery 633 Figure 1 m-XRF spectra of the clay and the blue glaze of the sample K18. K32 and K33 is probably due to the leaching of Sn from the transparent glaze during firing (Fig. 1). Sn was used in glazed pottery for the creation of opacified glass (Allan 1973; Al-Saad 2002). The chemical compositions of both the ceramic bodies and the glazes are presented in Tables 2 and 3, respectively. PCA of the ceramic bodies, based on m-XRF elemental analysis data, illustrates the differences of the samples, as shown in Figure 2. A weak difference of the studied material is observed based on the first principal component. Samples on the left side of the PCA (K1, K2, K10, K13) show increased concentration of K and Si together with low concentrations of Cr and Ca. However, samples on the right of the PCA (K4, K6, K29) present high concentrations of Cr, Ca and Ni. The chemical composition of the ceramic bodies is compared with already analysed material from the Paphos (Lemba, Kouklia) (Megaw and Jones 1983; Jones 1986) and Limassol areas (Amathus) (Jones 1986), taking into consideration the different techniques used for analysis (Fig. 3). According to this comparison, glazed ceramic samples with increased Cr and Ca concentrations seem to originate from Limassol while samples with low concentration of Cr and Ca could possibly originate from Paphos (Fig. 2). Samples K3 and K8 are different from the other samples due to their higher content of Ti while sample K33 has a very high amount of Ca and significant amounts of Mn and Cu. Samples K3, K8 and K33 reveal stronger differences and could possibly have been manufactured in different workshops from other areas of Cyprus or were trade products from other territories. The green colour of the lead glazes is usually related to the presence of Cu2+ or Fe2+ in the glaze, whereas the yellow to brown colours are related to Fe3+ oxides and complexes (Molera et al. 1999). Elemental analysis of the glazes confirms these observations, showing that green glazes are rich in Cu, as seen in Figure 4. The blue glaze (sample K18) contains Co, Sn and significant amounts of Ni. It seems that Co-based pigments were well known for their beautiful blue colour due to the CoO4 complex. Finally, Fe3+ is responsible for the brown, yellow, black and red in the glazes; however, black glazes also contain Mn and yellow glazes also contain Cr. © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 K1 K2 K3 K4 K5 K6 K7 K8 K9 K10 K11 K12 K13 K14 K15 K16 K17 K18 K27 K28 K29 K30 K31 K32 K33 K2O wt% 1 stdev 2.44 1 0.07 3.08 1 0.26 1.37 1 0.11 1.50 1 0.26 3.08 1 0.03 2.00 1 0.05 3.31 1 0.17 0.84 1 0.05 3.47 1 0.03 3.13 1 0.62 2.01 1 0.14 3.13 1 0.45 0.75 1 0.06 3.14 1 0.22 2.96 1 0.28 3.00 1 0.46 3.42 1 0.33 1.63 1 0.21 2.77 1 0.59 3.47 1 0.20 1.37 1 0.21 3.05 1 0.04 2.50 1 0.05 0.48 1 0.02 1.20 1 0.02 SiO2 wt% 1 stdev 61.00 1 2.00 58.00 1 2.00 54.00 1 2.00 58.33 1 3.51 59.55 1 2.08 56.33 1 2.00 55.67 1 2.00 54.00 1 3.00 51.00 1 2.00 53.50 1 2.31 56.33 1 2.52 52.33 1 3.79 52.67 1 5.13 53.67 1 2.52 51.33 1 3.51 54.33 1 6.35 55.67 1 3.03 44.67 1 2.53 56.00 1 4.16 58.00 1 3.00 54.67 1 3.13 55.33 1 1.53 53.67 1 1.53 45.00 1 3.46 47.67 1 2.87 3.63 1 0.20 5.87 1 0.59 4.43 1 0.32 15.80 1 0.66 5.73 1 0.96 22.33 1 1.15 3.27 1 0.31 3.01 1 0.53 8.57 1 0.90 6.20 1 0.85 24.33 1 0.58 8.00 1 1.00 7.03 1 1.17 6.10 1 0.20 19.70 1 3.16 19.33 1 1.23 6.43 1 0.32 19.33 1 3.79 21.33 1 4.04 13.17 1 0.32 13.00 1 3.46 11.93 1 0.55 8.67 1 0.49 16.13 1 0.51 23.33 1 2.65 CaO wt% 1 stdev 0.89 1 0.10 0.82 1 0.16 2.23 1 0.25 0.81 1 0.10 0.86 1 0.12 0.66 1 0.11 0.76 1 0.04 1.40 1 0.17 0.92 1 0.08 0.71 1 0.16 0.64 1 0.03 0.83 1 0.12 0.12 1 0.02 0.79 1 0.06 0.72 1 0.13 1.07 1 0.25 0.93 1 0.15 0.73 1 0.12 0.9 1 0.11 0.92 1 0.07 0.87 1 0.21 0.87 1 0.05 0.81 1 0.13 0.71 1 0.01 0.87 1 0.06 TiO2 wt% 1 stdev 7.60 1 0.50 6.77 1 0.55 12.83 1 0.21 8.80 1 1.01 7.37 1 0.31 6.87 1 0.32 6.83 1 0.35 10.07 1 0.90 7.60 1 0.36 7.07 1 1.47 7.30 1 0.46 8.13 1 1.01 0.83 1 0.15 7.30 1 0.30 5.60 1 0.78 9.27 1 0.60 8.20 1 0.56 6.23 1 1.33 9.33 1 0.58 10.53 1 0.49 11.67 1 2.52 8.47 1 0.15 6.73 1 0.21 7.23 1 0.15 8.00 1 0.52 Fe2O3 wt% 1 stdev 0.11 1 0.02 0.07 1 0.01 0.22 1 0.02 0.21 1 0.02 0.09 1 0.01 0.15 1 0.01 0.09 1 0.01 0.22 1 0.03 0.09 1 0.01 0.07 1 0.02 0.16 1 0.01 0.10 1 0.02 0.07 1 0.03 0.15 1 0.01 0.09 1 0.01 0.15 1 0.04 0.14 1 0.02 0.11 1 0.02 0.13 1 0.01 0.16 1 0.01 0.02 1 0.001 0.13 1 0.01 0.16 1 0.03 0.16 1 0.02 0.27 1 0.08 MnO wt% 1 stdev 250 1 60 150 1 80 130 1 70 470 1 200 330 1 60 700 1 300 500 1 200 230 1 100 500 1 300 120 1 50 230 1 100 465 1 100 160 1 70 500 1 200 120 1 70 400 1 100 190 1 100 170 1 40 500 1 100 200 1 100 450 1 130 230 1 100 160 1 80 260 1 100 240 1 35 Cr ppm 1 stdev Table 2 m-XRF elemental analysis of the clays of the samples 125 1 50 70 1 20 50 1 10 230 1 100 100 1 30 300 1 130 120 1 50 100 1 50 140 1 60 80 1 20 190 1 100 160 1 60 100 1 50 160 1 90 82 1 20 120 1 20 120 1 50 110 1 20 190 1 70 190 1 35 250 1 80 125 1 70 120 1 70 100 1 60 100 1 20 Ni ppm 1 stdev 200 1 40 65 1 10 85 1 20 70 1 20 125 1 25 90 1 20 50 1 10 300 1 60 73 1 20 73 1 20 90 1 20 70 1 20 90 1 20 50 1 10 80 1 20 160 1 50 80 1 20 150 1 40 140 1 30 100 1 20 90 1 20 70 1 20 80 1 20 90 1 20 430 1 60 Cu ppm 1 stdev 125 1 25 85 1 20 120 1 20 90 1 20 70 1 20 90 1 20 80 1 20 80 1 20 90 1 20 87 1 20 110 1 20 50 1 10 80 1 20 80 1 20 100 1 20 70 1 15 110 1 20 90 1 20 85 1 15 120 1 20 60 1 10 110 1 20 80 1 20 130 1 30 70 1 10 Zn ppm 1 stdev 634 A. C. Charalambous et al. © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 K2O wt% 1 stdev 0.55 1 0.06 0.55 1 0.02 0.72 1 0.02 0.3 1 0.04 0.94 1 0.07 0.35 1 0.02 0.4 1 0.04 0.3 1 0.01 0.35 1 0.02 0.36 1 0.01 0.24 1 0.02 0.73 1 0.08 0.48 1 0.04 0.54 1 0.03 0.84 1 0.05 0.87 1 0.03 0.46 1 0.02 0.29 1 0.02 0.71 1 0.05 0.69 1 0.03 0.55 1 0.11 0.59 1 0.05 0.57 1 0.02 1.2 1 0.15 SiO2 wt% 1 stdev 54.19 1 1.58 52.29 1 2.39 59.9 1 1 54.22 1 1.15 54.22 1 0.58 55.45 1 1.69 52.05 1 1.15 52.04 1 1.58 50.64 1 3.51 46.36 1 2.08 57.07 1 0.58 57.79 1 2.24 47.81 1 1.73 58.19 1 1.15 58.51 1 1.63 53.48 1 2.34 53.49 1 1.53 54.92 1 1.72 51.36 1 1.35 53.59 1 2.1 51.34 1 2.13 53.48 1 3.25 49.2 1 1 54.62 1 2.73 Sample K1-Green K2-Brown K2-Yellow K3-Orange K4-Orange K5-Green K5-GreenYellow K5-Orange K5-Yellow K5B-Black K5B-Yellow K6-Orange K6-Yellow K7-Brown K7-Green K7-Yellow K7B-Brown K8-Brown K9-Green K9-GreenOrange K10-Brown K10-Green K10-Orange K10-Yellow 0.55 1 0.01 2.62 1 0.25 2.67 1 0.35 1.34 1 0.36 0.91 1 0.11 0.38 1 0.03 0.6 1 0.02 0.81 1 0.02 0.59 1 0.07 0.92 1 0.03 0.78 1 0.17 5.2 1 0.67 11.89 1 2.13 2.13 1 0.76 13.47 1 1.67 6.11 1 1.13 3.08 1 0.1 0.64 1 0.04 2.7 1 0.1 2.66 1 0.12 3.82 1 0.2 3.96 1 0.78 4.48 1 0.82 1.01 1 0.19 CaO wt% 1 stdev 0.4 1 0.01 0.25 1 0.01 0.27 1 0.02 0.33 1 0.02 0.33 1 0.02 0.25 1 0.02 0.3 1 0.01 0.35 1 0.04 0.28 1 0.02 0.23 1 0.01 0.25 1 0.01 0.25 1 0.03 0.28 1 0.03 0.22 1 0.01 0.3 1 0.02 0.32 1 0.02 0.23 1 0.01 0.62 1 0.04 0.24 1 0.02 0.18 1 0.02 0.33 1 0.02 0.18 1 0.02 0.25 1 0.02 0.33 1 0.02 0.5 1 0.08 4.62 1 0.12 3.4 1 0.24 1.34 1 0.1 3.22 1 0.09 0.36 1 0.07 0.34 1 0.02 3 1 0.16 0.37 1 0.04 3.06 1 0.12 2.53 1 0.21 1.49 1 0.14 0.86 1 0.14 2.8 1 0.34 0.79 1 0.14 0.41 1 0.04 5.82 1 0.65 3.75 1 0.49 1.36 1 0.04 1.22 1 0.03 3.2 1 0.25 3.5 1 0.35 3.1 1 0.11 0.34 1 0.01 170 1 50 230 1 40 170 1 30 280 1 50 210 1 40 150 1 30 100 1 30 160 1 40 100 1 40 150 1 40 140 1 50 140 1 40 190 1 40 140 1 40 230 1 50 180 1 40 250 1 40 370 1 50 200 1 40 250 1 30 180 1 40 190 1 40 200 1 40 110 1 70 300 1 100 90 1 50 100 1 50 120 1 50 210 1 60 210 1 70 100 1 50 110 1 60 110 1 60 110 1 40 100 1 50 130 1 50 180 1 60 150 1 50 300 1 100 150 1 60 150 1 70 110 1 60 110 1 60 310 1 100 110 1 60 90 1 50 80 1 30 100 1 60 280 1 70 100 1 50 120 1 70 100 1 50 130 1 60 220 1 90 120 1 60 110 1 60 140 1 80 90 1 40 100 1 50 100 1 50 120 1 50 110 1 60 200 1 80 150 1 80 100 1 40 100 1 30 130 1 70 160 1 90 100 1 60 110 1 60 90 1 50 110 1 60 3600 1 300 350 1 70 300 1 60 90 1 20 190 1 40 4000 1 400 230 1 50 240 1 50 210 1 40 180 1 40 170 1 30 200 1 50 250 1 50 350 1 60 4700 1 800 420 1 80 190 1 40 80 1 20 2700 1 400 2300 1 400 210 1 40 160 1 30 140 1 30 210 1 40 60 1 20 50 1 10 40 1 10 40 1 10 50 1 20 110 1 20 40 1 10 50 1 20 40 1 10 40 1 10 40 1 10 40 1 10 50 1 10 50 1 20 130 1 30 80 1 20 80 1 20 50 1 20 70 1 20 70 1 20 50 1 10 50 1 20 50 1 10 40 1 10 TiO2 Fe2O3 MnO Cr Ni Cu Zn wt% 1 stdev wt% 1 stdev ppm 1 stdev ppm 1 stdev ppm 1 stdev ppm 1 stdev ppm 1 stdev Table 3 m-XRF elemental analysis of the glazes of the samples 22.77 1 0.59 27.18 1 0.95 27.75 1 0.98 24.24 1 0.55 22.63 1 0.71 21.31 1 0.50 21.69 1 0.21 26.52 1 0.38 24.86 1 1.04 22.74 1 0.72 22.7 1 1.21 20.55 1 3.29 25.02 1 1.12 24.24 1 1.97 25.11 1 2.52 26.94 1 1.26 24.64 1 2.79 26.08 1 1.91 24.2 1 0.51 23.55 1 1.85 20.83 1 1.33 25.64 1 0.78 26.69 1 1.03 28.09 1 1.23 PbO wt% 1 stdev 0.17 1 0.05 n.d n.d n.d n.d 0.2 1 0.03 n.d n.d n.d n.d n.d n.d n.d n.d 0.28 1 0.05 0.14 1 0.02 n.d n.d 0.24 1 0.02 0.24 1 0.05 n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d SnO2 CoO wt% 1 stdev wt% 1 stdev Cypriot Byzantine glazed pottery 635 © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 1.4 1 0.34 0.96 1 0.26 0.46 1 0.08 0.39 1 0.08 0.46 1 0.03 0.59 1 0.02 0.57 1 0.07 0.69 1 0.03 1.18 1 0.11 0.44 1 0.03 0.25 1 0.04 0.76 1 0.06 0.42 1 0.05 0.51 1 0.16 0.54 1 0.11 0.92 1 0.11 4.73 1 0.12 5.26 1 0.12 0.48 1 0.06 0.24 1 0.02 1.48 1 0.35 1.24 1 0.12 0.12 1 0.03 0.86 1 0.02 0.76 1 0.03 1.05 1 0.27 0.25 1 0.03 2.54 1 0.04 3.65 1 0.06 51.34 1 1.83 52.9 1 2.68 56.35 1 2.15 60.04 1 2.52 52.09 1 2.08 57.07 1 1.58 49.91 1 0.58 68.46 1 2.89 52.36 1 1.97 54.91 1 1.53 51.34 1 1.77 59.9 1 2 57.76 1 3.43 51.33 1 1.73 51.35 1 3.21 50.63 1 1.53 53.1 1 3.43 52.8 1 2.97 57.77 1 1.53 50.64 1 1.72 56.32 1 2.08 57.05 1 1.58 55.63 1 1.74 62.32 1 3.41 59.64 1 2.65 52.62 1 2.31 54.92 1 1.73 60.16 1 3.12 58.13 1 2.67 K11-Orange K11-Yellow K12-Red K12-Yellow K12B-Black K14-Orange* K14-Orange K14B-Orange K15-Yellow K16-Black K16-Brown K16-Green K16-LightGreen K16B-Red K17-Orange* K17-Yellow K18-Blue K18-LightBlue K27-Green K27-GreenLine K28-Green K28-Yellow K29-Black K30-Green K30-Yellow K30-Yellow* K31-Yellow K32-LightBlue K33-BlueGreen *Decorative pattern. K2O wt% 1 stdev SiO2 wt% 1 stdev Sample 4.38 1 0.76 5.31 1 1.12 2.09 1 0.3 1.12 1 0.1 13.99 1 1.15 9.75 1 1.18 2.49 1 0.56 4.57 1 1.29 8.99 1 2.15 2.79 1 0.26 1.92 1 0.12 2.61 1 0.12 1.44 1 0.06 6.48 1 1.18 1.34 1 0.44 1.23 1 0.35 1.92 1 0.06 3.92 1 0.17 1.64 1 0.15 3.93 1 0.42 1.36 1 0.06 0.71 1 0.08 0.94 1 0.06 1.78 1 0.27 1.76 1 0.5 4.11 1 0.67 1.25 1 0.24 3.32 1 0.54 2.79 1 0.4 CaO wt% 1 stdev 0.23 1 0.03 0.35 1 0.03 0.23 1 0.04 0.22 1 0.03 0.22 1 0.02 0.39 1 0.02 0.19 1 0.01 0.45 1 0.05 0.32 1 0.02 0.35 1 0.02 0.3 1 0.01 0.43 1 0.01 0.45 1 0.06 0.28 1 0.03 0.22 1 0.04 0.17 1 0.01 0.18 1 0.02 0.25 1 0.03 0.35 1 0.01 0.15 1 0.02 0.08 1 0.02 0.05 1 0.02 0.63 1 0.03 0.13 1 0.02 0.09 1 0.02 0.13 1 0.04 0.15 1 0.04 0.23 1 0.02 0.22 1 0.02 1.86 1 0.06 0.63 1 0.12 2.72 1 0.3 2.28 1 0.3 1.62 1 0.15 2.49 1 0.37 1.74 1 0.09 2.96 1 0.17 1.79 1 0.04 1.24 1 0.15 3.53 1 0.29 0.67 1 0.03 0.57 1 0.03 9 1 1.73 1.21 1 0.19 0.54 1 0.03 2.39 1 0.12 1.71 1 0.2 0.67 1 0.02 0.89 1 0.11 1.62 1 0.12 1.14 1 0.05 4.62 1 0.55 0.47 1 0.03 0.3 1 0.01 0.73 1 0.19 0.41 1 0.03 0.97 1 0.16 0.61 1 0.03 160 1 70 90 1 40 160 1 40 130 1 40 180 1 60 360 1 60 280 1 40 380 1 50 260 1 40 240 1 60 270 1 70 130 1 40 150 1 50 280 1 70 260 1 40 160 1 40 300 1 80 270 1 70 120 1 40 80 1 30 380 1 90 400 1 100 600 1 100 100 1 40 120 1 30 170 1 40 200 1 40 290 1 40 270 1 70 70 1 20 170 1 80 110 1 40 140 1 40 130 1 30 130 1 60 500 1 200 180 1 80 180 1 70 140 1 40 250 1 100 130 1 40 170 1 50 120 1 40 270 1 80 140 1 50 80 1 30 100 1 40 140 1 40 100 1 30 100 1 30 230 1 50 130 1 40 130 1 40 110 1 40 280 1 70 110 1 40 110 1 50 220 1 60 120 1 60 120 1 70 100 1 40 120 1 40 120 1 40 120 1 60 200 1 70 120 1 50 110 1 40 270 1 80 220 1 60 280 1 70 270 1 80 150 1 30 170 1 60 160 1 50 1800 1 300 600 1 100 150 1 50 110 1 30 130 1 50 150 1 50 140 1 40 140 1 60 100 1 40 150 1 50 140 1 40 160 1 50 220 1 60 TiO2 Fe2O3 MnO Cr Ni wt% 1 stdev wt% 1 stdev ppm 1 stdev ppm 1 stdev ppm 1 stdev Table 3 (Continued) 130 1 30 210 1 40 350 1 100 300 1 100 120 1 40 70 1 20 80 1 20 90 1 20 110 1 20 7700 1 2000 3500 1 800 7700 1 2000 5100 1 1000 1000 1 100 60 1 10 80 1 20 150 1 50 80 1 30 5500 1 600 3100 1 300 6400 1 1000 460 1 70 460 1 100 2400 1 100 120 1 20 190 1 70 200 1 40 80 1 20 5100 1 400 Cu ppm 1 stdev 45 1 10 44 1 10 20 1 10 20 1 10 30 1 10 40 1 10 40 1 20 40 1 10 110 1 20 90 1 20 50 1 10 80 1 20 60 1 20 30 1 10 40 1 10 40 1 20 20 1 10 20 1 10 50 1 20 30 1 10 50 1 20 20 1 10 30 1 10 90 1 20 30 1 10 30 1 10 50 1 20 40 1 10 60 1 20 Zn ppm 1 stdev 26.15 1 3.36 23.39 1 2.99 26.45 1 1.40 24.78 1 1.51 26.54 1 2.48 24.51 1 0.91 25.81 1 1.72 22.8 1 2.12 23.05 1 2.51 25.4 1 1.72 27.51 1 1.06 21.88 1 1.50 20.94 1 0.81 22.23 1 2.06 20.8 1 2.95 21.23 1 1.83 35.8 1 1.57 34.74 1 1.67 27.77 1 1.16 25.07 1 2.67 23.42 1 2.55 24.07 1 1.45 26.45 1 2.69 21.8 1 1.38 24.07 1 2.38 26.52 1 2.64 27.43 1 1.74 30.86 1 1.63 32.28 1 1.26 PbO wt% 1 stdev n.d n.d n.d n.d n.d n.d n.d n.d n.d 0.21 1 0.03 0.12 1 0.02 0.17 1 0.03 0.11 1 0.02 0.1 1 0.02 n.d n.d 2.24 1 0.12 2.37 1 0.12 n.d n.d n.d n.d n.d n.d n.d 0.1 1 0.02 n.d 1.57 1 0.2 1.52 1 0.1 n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d 0.42 1 0.05 0.11 1 0.01 n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d n.d SnO2 CoO wt% 1 stdev wt% 1 stdev 636 A. C. Charalambous et al. Cypriot Byzantine glazed pottery 637 Figure 2 PCA of ceramic bodies, using m-XRF elemental analysis. X-ray diffraction Mineralogical analysis was performed for samples K1, K12, K16, K18, K27, K28, K29, K32 and K33. The results are presented in Table 4. All samples contain quartz and plagioclase. Calcite is present in all samples except K29 and K32, while hematite is present in all samples expect K18, K28, K32 and K33. Gehlenite is present only in sample K18, while analcime is present in samples K32 and K33 (Fig. 5). Additionally, samples K18, K32 and K33 contain high amounts of pyroxene (diopside), while they contain the lowest amount of quartz among all analysed samples. An amorphous phase is also present in significant amounts in all samples. Diopside, plagioclase and gehlenite are the major minerals newly formed during the firing process of the ceramics (Heimman and Maggetti 1979; Maggetti 1981; Buxeda i Garrigós 1999), while analcime is formed after firing, mainly during burial diagenesis, by crystallization from penetrating solutions or by alteration and transformation of certain firing minerals (Maggetti 1981) or from the alteration of the glassy amorphous phase (Buxeda i Garrigós and Kilikoglou 2001; Schwedt et al. 2006). According to Heimman and Maggetti (1979), calcareous sherds of raw and fine ceramics develop diospide and gehlenite during firing. The latter mineral is obviously metastable with respect to the composition of typical potter’s clay, and therefore has the tendency to react with silica to yield anorthite at higher temperatures (>1050°C). This formation of hightemperature minerals depends on the original clay minerals and calcite contents of a sample, their grain size distribution and the duration of firing. For example, K1 is moderately calcareous (3.63% CaO) but contains detectable amounts of CaCO3 but no diopside and therefore it seems to have been fired at a lower temperature than sample K29, which is highly calcareous (13.00% CaO) without any calcite, which means that all the calcite has been decomposed. Furthermore, K29 contains the highest amount of anorthite, which signifies a high firing temperature. Also, sample K32 is highly calcareous without any calcite and all the CaCO3 has been involved in the © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 638 A. C. Charalambous et al. Figure 3 Map of southern Cyprus with the excavation areas of the studied samples and the sites of the other analysed material. Mean values of Cr and Ca concentrations of analysed samples: Lemba (Megaw and Jones 1983), Kouklia (Jones 1986), Amathus 1 and 2 (Jones 1986), analysed samples with low Cr, Ca concentrations, analysed samples with high Cr, Ca concentrations. formation of high-temperature phases, which means that sample K32 must also have been fired at a higher temperature than the other samples. Mineralogical analysis therefore shows differences in some of the samples such as K29 and K32, which suggests the existence of different manufacturing technology probably involving a different firing process. Scanning electron microscopy The results of the glaze microanalysis of samples K1, K18 and K33 are presented in Figure 6. As can be seen, sample K1 contains a significantly higher amount of alumina and iron oxides (Fe2O3) but a lower amount of PbO compared with the glazes of the other two samples, which is in agreement with Tite et al. (1998). The alkali and the silica content of the glazes are quite similar for all three samples K1, K18 and K33. The optical differences of the quality of the ceramic body and glaze of samples K1 and K18 are shown in Figures 7 (a) and 7 (b). The ceramic body of sample K1 shows detrital quartz in an © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 Cypriot Byzantine glazed pottery 639 Figure 4 PCA of glazes using m-XRFelemental analysis. amorphous matrix. The clay quality of sample K18 is much better. The white bubbles in the glaze of sample K18 (Fig. 7 (d)) are particles of Sn. Therefore SEM-EDS analysis confirms the m-XRF and XRD results on the differences between K18 and K33 compared with K1 (Figs 7 (a) and 7 (c)), which is considered to be a local product, possibly from the workshops of Paphos. Samples K18 (Figs 7 (b) and 7 (d)) and K33 show typical Italian majolica pottery decoration and could possibly be regarded as trade products. CONCLUSIONS The study of 25 Byzantine glazed ceramics from two archaeological sites in the Limassol area provides significant information on the elemental and mineralogical characterization, the provenance and the manufacturing techniques used for their production. In particular, the present study has shown that all samples follow the main technological characteristics of lead-glazed Byzantine pottery. Some of them (K18, K32, K33) are Sn-opacified glazed pottery and, based on XRD and SEM-EDS analysis, they could be either trade products or local products of workshops that followed specific technologies. The chemical composition of the ceramic bodies was compared with already analysed material from the Paphos (Lemba, Kouklia) and Limassol areas (Amathus). According to this comparison, the samples with increased Cr and Ca concentrations seem to originate from the Limassol area while samples with low concentrations of Cr and Ca could originate from the Paphos area. Finally, samples K3 and K8 show significant differences due to the high content of TiO2, and together with samples K18, K32 and K33, which show strong archaeological differences, could be regarded as possible trade products or local products of different decoration technology. Concerning the glazes, the blue colour is due to the presence of Co and Ni oxides, the green colour is due to Cu oxides and the yellow, orange, red and black colours are due mainly to Fe oxides, in combination with Mn and Cr oxides. © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 69 66 58 21 60 45 52 8 31 Quartz Mainly anorthite, 2diopside. 1 K1 K12 K16 K18 K27 K28 K29 K32 K33 Sample 5 6 5 – – 14 – – – Potassium 3 4 6 2 2 11 26 13 8 Plagioclase1 Feldspars – – – 29 – 7 – 27 25 Pyroxene2 4 5 5 20 5 12 – – 5 Calcite – – – – 2 – – – – Mica 5 9 6 – 3 – 12 – – Hematite – – – 14 – – – – – Gehlenite Table 4 Mineralogical composition (wt%) of selected clay samples, carried out by XRD – – – – – – – 36 10 Analcime 14 10 20 14 28 11 10 16 21 Amorphous 640 A. C. Charalambous et al. Cypriot Byzantine glazed pottery 641 Figure 5 XRD spectrum of the clay of the sample K33. Figure 6 SEM-EDS analysis of samples K1, K18 and K33. Further studies on more samples of glazed pottery excavated in Cyprus are in progress to enhance our knowledge of Cypriot glazed pottery. ACKNOWLEDGEMENTS The present work was funded partially by the Greek General Secretariat of Research and Technology and the EC under the programme ‘Excellence in Research Institutes GSRT (2nd round)’, sub-programme ‘Support for Research Activities in C. E. T. I.’ The authors thank the © University of Oxford, 2009, Archaeometry 52, 4 (2010) 628–643 642 A. C. Charalambous et al. Figure 7 Optical microscopy and SEM photomicrographs of the body–glaze interface of the samples K1 (a, c) and K18 (b, d). archaeologist E. Charalambous for cooperation and help during the sampling and the archaeologist E. Prokopiou for the samples and the information about the archaeological sites. REFERENCES Allan, J. W., 1973, Abu’l-Qasim’s treatise on Ceramics, Iran, 11, 111–20. 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