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Characterization of Medieval Glass Artefacts from Miranduolo Site, Chiusdino, Italy

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Characterization of Medieval Glass Artefacts from Miranduolo Site, Chiusdino, Italy University of Évora Erasmus Mundus Master in ARCHaeological MATerials Science Mestrado in Arqueologia e Ambiente (Erasmus Mundus - ARCHMAT) Characterization of Medieval glass artefacts from Miranduolo site, Chiusdino, Italy Ivona Posedi (m34322) Professor Dr. Nicola Schiavon (Supervisor – University of Évora) Professor Dr. Josè António Paulo Mirão (Co-supervisor – Univeristy of Évora) Dr. Vittorio Fronza (Co-supervisor – University of Siena) Évora, September 2016 Abstract (English) This archaeovitreological study deals with artefacts of Miranduolo site, Tuscany region (Italy), dated 1250-1350 AD. The Miranduolo site is a medieval hill-village dated from 7th to 14th century. The information obtained reveal that Miranduolo was under control of noble families, which displayed the social, economic and political power. It is marked by controlling the farmers and metal workers on the site, as well as having control over agricultural surpluses. No in situ glass workshop has been recovered, implying that the glass artefacts were imported. One aim of this work is application of SEM-EDS to visualize textural characteristics and thickness of the pristine glass and corrosion layers. Preliminary qualification and semi-quantification of major and minor chemical elements will provide the data on the glass group present and fluxes employed. The data obtained will be integrated with the one obtained by more sensitive techniques such as PIXE/PIGE and LA-ICP-MS. Twenty cross-sections of transparent glasses (colorless, azure, and different hues of yellow and) have been analyzed by VP-SEM. All the analyzed glasses display a homogenous matrix. Only four samples (MD 24, MD 139, MD 143, MD 259) show corrosion layers of various thickness with 2.25µm, 136-500 µm, 26.8 µm and 17.01 µm. EDS linescan analyses indicate strong depletion in the corrosion layers of Na and K, while Ca depletes to a minor extent. In general, both glass composition and the burial conditions were favorable for preservation. Samples can be classified as mainly plant ash Na-Ca-Si glasses made with both unpurified and purified Levantine ash. Only sample MD 243 is made from Barilla plant ash. Sample MD 139 cannot be classified into main compositional groups as K2O is 1.33 wt% and MgO 5.92 wt%. In 8 samples MnO content is lower than 0.8 wt%, meaning that in these samples MnO is naturally present. In other 12 samples, MnO above 0.8 wt% indicates deliberate addition as a decolorant agent to intentionally obtain different hues or the amount added was not successful in making the glass transparent. The results considering fluxes are compatible with archaeovitreological study from contemporary primary glass workshops in Tuscany. For determining the provenance of silica sources, further analysis with more sensitive techniques has to be carried out. Resumo (Português) Este estudo “arqueovitreologia” lida com artefatos do local Miranduolo, região da Toscana (Itália), datados de 1250-1350 AD. O sitio de Miranduolo é uma colina vila medieval datada do séc.VII ao séc.XIV. As informações obtidas revelam que Miranduolo estava sob o controle de famílias nobres, que exibiu o poder social, económico e político. É marcado por controlar os agricultores e trabalhadores do metal no sitio, bem como ter controlo sobre os excedentes agrícolas. Não há na oficina de vidro in situ foi recuperado, o que implica que os artefactos de vidro foram importados. Um dos objetivos deste trabalho é a aplicação de SEM-EDS para visualizar características de textura e espessura das camadas de corrosão do vidro também como da áreas originais. qualificação preliminar e semi-quantificação de maiores e menores elementos químicos irá fornecer os dados sobre o grupo presente vidro e fluxos empregado. Os dados obtidos são integrados com os dados obtidos por meio de técnicas mais sensíveis, como PIXE / PIGE e LA-ICP-MS. Vinte secções transversais de vidros transparentes (incolor, azul celeste, e diferentes tons de amarelo) foram analisados por VP-SEM. Todos os vidros analisados exibir uma matriz homogénea. Apenas quatro amostras (MD 24, MD 139, MD 143, MD 259) mostram camadas de corrosão de várias espessuras com 2.25μm, 136-500μm, 26,8μm e 17,01μm. Análises Linescan EDS indicam forte esgotamento nas camadas de corrosão de Na e K, enquanto Ca esgota, em menor grau. Em geral, tanto a composição de vidro e as condições de depósito foram favoráveis para a preservação. As amostras podem ser classificados como vidros principalmente Na-Ca-Si feitas com cinzas de plantas do tipo levantino, não purificada e purificada. Apenas a amostra MD 243 é feita a partir de cinzas vegetais tipo “Barilla”. A amostra MD 139 não pode ser classificada em grupos principais de composição porque K2O é 1,33% em peso e MgO 5,92% em peso. Em 8 amostras, o teor de MnO é menor do que 0,8% em peso, o que significa que nestas amostras MnO está naturalmente presente. Em outras 12 amostras, MnO acima de 0,8% em peso indica adição intencional como um agente de colorante para obter intencionalmente diferentes matizes ou o valor acrescentado não foi bem sucedido em fazer o vidro transparente. Os resultados, considerando os fluxos são compatíveis com o estudo “arqueovitreologico” com as principais oficinas de vidro contemporâneos na Toscana. Para determinar a origem das fontes de sílica, uma análise mais aprofundada com técnicas mais sensíveis tem de ser levada a cabo. Table of contents ACKNOWLEDGEMENTS ....................................................................................................................................... I INTRODUCTION.................................................................................................................................................. 1 1. ABOUT GLASS ................................................................................................................................................. 5 1.1. DEFINITION, COMPOSITION, PROPERTIES AND BEHAVIOR OF GLASS ......................................................................................... 5 1.2. HISTORY OF GLASS PRODUCTION AND HISTORICAL DOCUMENTS ........................................................................................... 11 1.3. ARCHAEOVITREOLOGICAL CLASSIFICATION AND TERMINOLOGICAL ISSUES .............................................................................. 14 2. THE ARCHAEOLOGICAL CONTEXT ................................................................................................................... 20 2.1. THE ARCHAEOLOGICAL SITE OF MIRANDUOLO CASTLE ........................................................................................................ 20 2.1.1. Position ..................................................................................................................................................... 20 2.1.2. History ...................................................................................................................................................... 21 2.1.3. Excavation of Miranduolo castle .............................................................................................................. 22 2.1.4. Miranduolo site catchment area .............................................................................................................. 24 2.1.5. Periodization and development of the settlement ................................................................................... 24 2.1.6. Excavation areas ...................................................................................................................................... 32 2.2. STATE OF THE ART OF ARCHAEOVITREOLOGY IN ITALY ........................................................................................................ 35 3. MATERIALS AND METHODS ........................................................................................................................... 39 3.1. ANALYTICAL TECHNIQUES ............................................................................................................................................ 39 3.1.1. VP-SEM-EDS .............................................................................................................................................. 39 3.1.2. PIXE/PIGE.................................................................................................................................................. 42 3.1.3. LA-ICP-MS ................................................................................................................................................. 43 3.2. SAMPLING ................................................................................................................................................................ 47 3.3. EXPERIMENTAL METHODS ............................................................................................................................................ 48 3.3.1. VP-SEM-EDS .............................................................................................................................................. 48 3.3.2. PIXE/PIGE.................................................................................................................................................. 49 3.3.3. LA-ICP-MS ................................................................................................................................................. 51 4. RESULTS .......................................................................................................................................................
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