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UNIVERSIDADE AUTÓNOMA DE LISBOA LUIS DE CAMÕES Departamento de História Tese de Doutoramento em História Conservação de Materiais Orgânicos Arqueológicos Subaquáticos (Conservation of Underwater Archaeological Organic Materials) Tese apresentada para a obtenção do grau de Doutor em História Orientador: Adolfo Silveira Martins Co-orientador: Donny L. Hamilton Doutoranda: Andreia Ribeiro Romão Veliça Machado Junho, 2013 ACKNOWLEDGEMENTS The work presented here would not have been possible without the help and collaboration of a group of people I would like to thank. To start with, the members of my committee, Prof. Adolfo Silveira Martins and Prof. Donny L. Hamilton. They kindly accepted me as their student and since then have been most supportive and helpful. Enough cannot be said about the help I received from Helen Dewolf, at the Conservation Research Laboratory, and also Dr. Wayne Smith. They were willing to teach me everything that they knew, get me any supplies and samples that I needed and they were always there to check my work and to guide me when needed. Deep gratitude is reserved for Fundação para a Ciência e Tecnologia (SFRH / BD / 49007 / 2008), to Dr. Jorge Campos of the Câmara Municipal de Portimão , without whose interest in supporting me, this research would not have been accomplished. A thank you to Madalena Mira, Universidade Autónoma de Lisboa Library Director, and to Doctors Mike Pendleton and Ann Ellis from the Microscopy & Imaging Center, at Texas A&M. Another word of appreciation to Dr. Adolfo Miguel Martins and Dr. João Coelho from DANS, for the enlightening conversations and help during the research. An especial thanks to Tiago Fraga as without his believing in me, his support and friendship, this study would never have happened. Also to my friends Paula Costa, Vanda Germano, Jorge Baptista and Maria João Reis Rocha who always gave me the encouragement I needed. To Luísa Veloso, who opened my eyes, and to Catherine Sincich (TA&MU). Finally, to my husband, António Machado, who went with me on this journey, and to my family for their incredible support. 1 ABSTRACT The main proposal of the thesis "Conservation of Underwater Archaeological Organic Materials" is to present to archaeologists and archeology technicians, in an understandable way, the principles and procedures of the conservation of underwater archaeological organic materials, thus maximizing the efforts and results of the preservation of underwater cultural heritage. The aim to this study is, also, to define new interventional procedures concerning the conservation and restoration of underwater archaeological heritage and combine these with information and training. In this sense, after the characterization of the type of organic materials, commonly found in underwater archaeological sites, the identification of conservation status is followed. From this, the causes and their levels of degradation are recognized and understood. This step provides information and is also essential to ensure the future integrity of organic archaeological remains. From critical research-based methods and laboratory tests, specific methodologies are presented for the preservation of organic materials from underwater contexts, which can be implemented by the various technicians and experts in the field of underwater archeology and thus contribute to the safeguarding of heritage. Key-words: underwater archaeology; organic materials; state of conservation; methods of conservation. 3 RESUMO O objetivo principal da tese “Conservação de Materiais Orgânicos Arqueológicos Subaquáticos” é apresentar a arqueólogos e técnicos de arqueologia, de forma simples, os princípios e os procedimentos da conservação de materiais orgânicos de proveniência subaquática. Maximizando, assim, os esforços e os resultados da preservação do património subaquático. Pretende-se, igualmente, com este estudo definir novos procedimentos de intervenção relativos à conservação e restauro do património arqueológico subaquático e com estes aliar a informação e a formação. Neste sentido, após a caracterização do tipo de materiais orgânicos comummente encontrados em sítios arqueológicos subaquáticos, segue-se a identificação do estado de conservação. A partir deste reconhece-se e compreende-se quais as causas e os respetivos níveis de degradação. Esta etapa permite obter informação e é também fundamental para assegurar a integridade do espólio. A partir de uma pesquisa crítica baseada em métodos e análises laboratoriais, são apresentadas metodologias específicas para a preservação de materiais orgânicos provenientes de contextos subaquáticos, as quais podem ser implementadas pelos vários técnicos e especialistas no campo da arqueologia subaquática e, assim, contribuir para a salvaguarda do património. Palavras-chave: arqueologia subaquática; materiais orgânicos; estado de conservação; métodos de intervenção. 5 TABLE OF CONTENTS ACKNOWLEDGMENT 1 ABSTRACT 3 RESUMO 5 TABLE OF CONTENTS 7 LIST OF TABLES AND GRAPHIC 13 LIST OF FIGURES 15 ABBREVIATIONS 19 GLOSSARY 21 CHAPTER I – INTRODUCTION 23 1. Background to Dissertation 23 2. Definitions 25 3. Delimitations 26 4. The dissertation aims 26 5. Methods and references 27 6. Thesis outline 29 CHAPTER II – UNDERWATER ARCHAEOLOGY AND ITS CULTURAL HERITAGE CONSERVATION 31 7. The development of underwater archaeology 31 8. Cultural heritage and underwater archaeology 34 9. Brief history of waterlogged organic materials conservation 37 10. Survey of the Portuguese case towards the conservation of underwater cultural heritage 40 11. Discussion 46 CHAPTER III - ORGANIC MATERIALS ANALYSIS 47 12. General properties of organic materials 47 12.1. Leather, skin, bone and ivory 48 12.2. Wool, horn, feathers and tortoiseshell 51 12.3. Silk 54 12.4. Wood and other cellulosic fibers 54 7 12.4.1. Flax, hemp, ramie, cotton, sisal and coconut fiber 58 12.4.2. Wood 62 13. Environment 68 13.1. General characteristics of water 68 13.1.1. Luminosity 70 13.1.2. Temperature 70 13.1.3. Dissolved gases 71 13.1.4. Reduction Potential – Oxidation/Reduction in Marine Environments 72 13.1.5. Salinity 73 13.1.6. Water density 75 13.1.7. Rivers, Estuaries, Lakes and Oceanic currents 76 13.1.7.1. The influence of ocean currents on the Portuguese coast 80 13.1.8. Oceanic Physiographic 82 13.1.8.1. Physiographic types of seafloor 83 13.2. Biological agents and degradation 84 13.2.1. Bacteria 85 13.2.2. Fungal attack 86 13.2.3. Marine Borers 87 14. Organic materials degradation 87 14.1. Leather, skin, bone and ivory 90 14.2. Wool, horn, feathers and tortoiseshell 94 14.3. Hydrolysis and oxidation of silk 95 14.4. Waterlogged wood deterioration 96 14.5. Flax, hemp, ramie, cotton, sisal and coconut fiber 108 15. Discussion 109 CHAPTER IV – FROM EXCAVATION TO DISPLAY: CONSERVATION PROCEDURES 111 16. The excavation process and on-site preservation measures 112 16.1. Project planning 112 16.2. Baseline studies and data recording before excavation 113 16.3. Protective measures while excavating 115 16.4. Lifting and handling 117 16.5. On-site preservation storage 119 17. Intervention criteriae 123 17.1. Terminology and definitions 123 17.2. Ethical code and intervention criteria 124 17.3. Reversibility, retreatment and minimum intervention 125 18. Conservation procedures 127 18.1. In-situ preservation and storage 128 18.2. Pre-Lab measures 132 18.3. Analytical techniques 134 19. Laboratory conservation treatments 137 19.1. Cleaning 139 19.1.1. Leather, bone, antler, teeth and ivory 141 19.1.2. Fur, wool, hair, horn and tortoiseshell 144 19.1.3. Silk 144 19.1.4. Cellulosic materials – textiles, rope and wood 145 19.2. Desalination 147 19.3. Conservation treatments for waterlogged organic materials 148 19.3.1. Polyethylene glycol impregnation 149 19.3.2. Silicone oils and conservation 153 19.3.3. Acetone/Rosin method 157 19.3.4. Sucrose stabilization method 159 19.3.5. Supercritical drying 162 19.4. Preventive conservation 165 19.4.1. Environmental factors and their effects 165 19.4.2. Physical factors and their effects 168 19.4.3. Other damaging factos 169 19.4.4. Waterlogged organic materials and environmental factors 170 19.4.5. Display and storage, preserving waterlogged organic materials 172 20. Discussion 174 9 CHAPTER V – CASE STUDIES 176 21. Methods for the removal of iron stains from cellulosic fabrics 176 21.1. Objectives and research plans 176 21.2. Materials and methods 177 21.3. Results and discussion 178 22. Silicone oil 179 22.1. Paços do Concelho Palmela’s shoes conservation procedure 180 22.1.1. The Paços do Concelho Palmela archaeological excavation 180 22.1.2. First examination and choice of treatment 182 22.1.3. Pre-treatment documentation and diagnostic 183 22.1.4. Silicone treatment procedure 185 22.1.5. Results and discussion 188 22.2. Silicone oil treatment, impregnation of non-degraded wood 190 22.2.1. Objectives and research plans 190 22.2.2. Materials and methods 190 22.2.3. Results 192 22.2.3.1. Pinus taeda L., Loblolly Pine from southern US 192 22.2.3.1.1. Macroanalysis 192 22.2.3.1.2. Microanalysis 194 22.2.3.2. Quercus alba L., White Oak from eastern North America 196 22.2.3.2.1. Macroanalysis 196 22.2.3.2.2. Microanalysis 197 22.2.3.3. Ulmus spp. , Elm from China 199 22.2.3.3.1. Macroanalysis 199 22.2.3.3.2. Microanalysis 200 22.2.4. Discussion 202 22.3. Silicone oil removal, the La Belle treenails experiment 202 22.3.1. Objectives and research plans 202 22.3.2. Materials and methods 203 22.3.3. Scanning electron microscopy (SEM / EDS) 206 22.3.4. Statistical method 206 22.3.5. Results and discussion 207 22.3.5.1. Macroanalysis 207 22.3.5.1.1. Treenail 1 207 22.3.5.1.1.1. Mass 207 22.3.5.1.1.2. Length 208 22.3.5.1.1.3. Thickness 208 22.3.5.1.2.
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