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Dissertation Roman aqueducts and Calcareous sinter deposits as a proxy for environmental changes Dissertation zur Erlangung des Grades „Doktors der Naturwissenschaften“ im Promotionsfach Geologie am Fachbereich Chemie, Pharmazie und Geowissenschaften der Johannes Gutenberg-Universität Mainz vorgelegt von M.Sc. Emine Gül Sürmelihindi Geboren in Gaziantep/ Türkei Mainz, Januar 2013 Abstract The ancient cities of Aspendos and Patara, located in southern Turkey, were two very important trade centers for Roman era with a dense population. Aqueducts supplied both cities with water that deposited calcium carbonate in their channels, here referred to as calcareous sinter. In this study, laminated sinter deposits from the water channels are investigated by geochemical and petrographical analysis to determine the nature of laminae couplets and to try and correlate them with seasonal environmental changes. Along both aqueduct lines, samples were taken from several locations to see if there was any variation in the nature of sinter due to changes in slope of the water channel or channel type. Laminated calcareous sinter deposits were examined by optical microscopy and EBSD (Electron Backscatter Diffraction) analysis to investigate crystal shape and orientation in different laminae couplets. EPMA (Electron Probe Micro-Analyzer) analysis was used to determine major element distribution and stable isotope analysis showed the seasonal temperature variations in the water. LA-ICP-MS (Laser Ablation- Inductively Coupled Plasma-Mass Spectrometry) trace element analysis was implemented to find small changes in minor elements. Based on these analyses, it was concluded that laminated calcareous sinter deposition can record seasonal changes in water chemistry, temperature and degassing rate during the year, besides lateral changes due to aqueduct structure and slope. Calcareous sinter deposits show a noticeable lamination of fine-grained, porous and coarse-grained, dense layers, which were shown to correspond to dry and wet seasons respectively. Fine-grained layers show high epifluorescence due to an organic rich content, which may be a result of bacterial activity during the dry, warm season. Stable oxygen and carbon isotope curves also correspond to seasonal variations in different laminae couplets; especially δ 18O curves reflect annual changes in temperature and seasonal changes in discharge. The most important result is that periodicity in δ 18O is caused by warming of water in the aqueduct channel, and not due to evaporation or source water characteristics. Periodicity in δ 13C is of a more complex nature, but mostly, δ 18O and δ 13C have anti-correlation along the laminae couplets. This is probably mainly due to degassing inside the aqueduct channel. Trace element results are mostly inconsistent and do not show significant and repeated changes through the different laminae couplets, although Magnesium, Strontium and Barium isotopes have positive correlation with each other in some samples and reach highest values within fine-grained, porous layers. In addition to this, major element results show that Iron, Potassium, Silicium and similar detrital elements reach relatively higher values inside the fine-grained, porous layers. Precise dating of calcareous sinter deposits is desirable, but should be very precise since the age of the aqueducts is already fixed by archaeological constraints within 200-300 years. Paleomagnetic and 14C dating has not given satisfactory results, and U/Th is hampered by high initial Th in the samples; however dating of a test sample from the Béziers aqueduct gave promising results. Deposition mechanisms and geochemical evolution of laminated sinter can be better understood if modern analogues of sinter deposition in water channels can be investigated. Another on-going project of this PhD work is the monitoring of sinter deposition and seasonal water composition changes in some still working aqueduct sites. The aim is to investigate recent environmental conditions that generate calcium carbonate deposition in aqueduct channels. First results show that few regular seasonal changes exist in the isotopic composition of the source water, and that observed periodicity in stable isotopes must be due to changes in the channel itself. In conclusion, calcareous sinter deposits from Roman aqueducts show promising results for practical use as environmental and archaeological proxies, especially for the Roman Era. This study only gives first results on two aqueducts. Further study of more aqueducts, combined with dating and more monitoring on still functioning aqueducts will give more precise results, and can lead to exploration of a new proxy for ancient climate, archaeology, and possibly archaeoseismology. I Zusammenfassung Die, im Süden der Türkei gelegen, antiken Städte Aspendos und Patara, waren in der Römerzeit zwei bedeutende Handelszentren mit hoher Bevölkerungsdichte. Aquädukte versorgten beide Städte mit carbonathaltigem Wasser, wobei sich Kalksinter (Calciumcarbonat) in der Kanalrinne ablagerte. Dabei lagern sich im Wechsel eine hellere und dunklere Kalksinterlage ab, die als Sinterpaar bezeichnet wird. Um die Entstehung dieser Sinterpaare besser zu verstehen, und die beteiligten Prozesse mit saisonalen Veränderungen der Umwelt zu korrelieren, werden in der vorliegenden Arbeit laminierten Sinterablagerungen mit geochemischen und petrographischen Methoden untersucht. Entlang der Kanalrinne beider Aquädukte wurden an mehreren Stellen Proben entnommen. Es wurde untersucht in wieweit sich die Sinterstruktur aufgrund von Änderungen in der Neigung des Wasserkanals oder des Kanaltyps ändert. Um die Kristallform und die kristallografische Orientierung der Kristalle innerhalb der verschiedenen Sinterpaare zu untersuchen, wurden die entnommenen laminierten Kalksinterablagerungen mit Hilfe optischer Mikroskopie und EBSD (Electron Backscatter Diffraction) analysiert. Der Electron Probe Micro-Analyzer (EPMA) wurde verwendet, um saisonale Schwankungen der Hauptelementverteilung und den Anteil der stabilen Isotope im Wasser zu bestimmen. Die LA-ICP-MS (Laser Ablation-induktiv gekoppeltem Plasma-Massenspektrometrie) Spurenelementanalyse wurde durchgeführt, um kleinste Schwankungen der Spurenelemente zu finden. Basierend auf diesen Analysen wurde festgestellt, dass laminierten Kalksinterablagerungen laterale Änderungen in der Aquäduktstruktur und -neigung, jahreszeitliche Änderungen der Wasserchemie, der Temperatur sowie der Entgasungsrate während eines Jahres widerspiegeln. Die Kalksinterablagerungen zeigen eine deutliche Laminierung in Form von feinkörnig-porösen und grobkörnig-dichten Schichten, die trockene und nasse Jahreszeiten anzeigen. Feinkörnige Schichten zeigen eine hohe Epifluoreszenz aufgrund reichhaltiger organischer Inhalte, die vermutlich eine Folge der bakteriellen Aktivität während der warmen und trockenen Jahreszeit sind. Stabile Sauerstoff und Kohlenstoff-Isotop-Kurven entsprechen auch den jahreszeitlichen Schwankungen der verschiedenen Schichtenpaare. Vor allem δ 18O spiegelt jährliche Veränderungen in der Temperatur und jahreszeitliche Veränderungen des Abflusses wieder. Das wichtigste Ergebnis ist, dass die Periodizität von δ 18O durch Erwärmen des Wassers im Wasserkanal und nicht durch die Verdunstung oder der Brunnenwasser-Charakteristik verursacht wird. Die Periodizität von δ 13C ist komplexer Natur, vor allem zeigen δ 18O und δ 13C eine Antikorrelation entlang der Lamellenpaare. Dies wird wohl vor allem durch Entgasungsprozesse im Aquädukt verursacht. Die Ergebnisse der Spurenelemente sind meist inkonsistent und zeigen keine signifikanten Veränderungen in den verschiedenen Lamellenpaaren. Die Isotope Mg, Sr und Ba zeigen hingegen bei einigen Proben eine positive Korrelation und erreichen Höchstwerte innerhalb feinkörnig-poröser Schichten. Auch sind die Hauptelementwerte von Fe, K, Si und anderer detritischer Elemente innerhalb der feinkörnige-porösen Schichten maximal. Eine genaue Datierung der Kalksinterablagerungen ist wünschenswert, da der Zeitraum, in dem die Aquädukte aktiv waren, bereits archäologisch auf 200-300 Jahre festgelegt wurde. Paläomagnetische und 14C-Datierung geben keine brauchbare Ergebnisse. Die U/Th Isotopie wird durch eine hohe Anfangskonzentration von Th in den Proben behindert. Trotz dieser Schwierigkeiten war eine U/Th Datierung an einem Testbeispiel des Béziers Aquädukt erfolgreich. Mit Hilfe von analogen Untersuchungen an aktiven Wasserkanälen der heutigen Zeit, werden die Ablagerungsmechanismen und die geochemische Entwicklung der laminierten Sinterschichten besser verstanden. Ein weiteres laufendes Projekt dieser Doktorarbeit ist die Überwachung von Sinterabscheidungen und der saisonale Zusammensetzung des Wassers an einigen heute noch aktiven Aquädukten. Das Ziel ist die Untersuchung der jetzigen Calciumcarbonatabscheidungen in Aquäduktkanälen unter den heutigen Umgebungsbedingungen. Erste Ergebnisse zeigen, dass kleine regelmäßige jahreszeitliche Veränderungen in der Isotopenzusammensetzung des Wassers vorliegen, und dass die beobachtete Periodizität der stabilen Isotope aufgrund von Änderungen im eigentlichen Kanal entstanden ist. Die Untersuchung von Kalksinterablagerungen in römischen Aquädukten liefern vielversprechende Ergebnisse, für die Untersuchung des Paläöklimas, der Archaeoseismologie und anderer Umweltbedingungen in der Römerzeit. Diese Studie beschränkt sich auf zwei Aquädukte. Die Untersuchungen weiterer Aquädukte und einer Überwachung, der noch in Betrieb stehenden Aquädukte
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