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Application of Tetraether Membrane Lipids As Proxies for Continental Climate

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Application of Tetraether Membrane Lipids As Proxies for Continental Climate Institut de Ciència i Tecnologia Ambientals Universitat Autònoma de Barcelona Application of tetraether membrane lipids as proxies for continental climate reconstruction in Iberian and Siberian lakes Marina Escala Pascual Tesi doctoral Institut de Ciència i Tecnologia Ambientals Universitat Autònoma de Barcelona Application of tetraether membrane lipids as proxies for continental climate reconstruction in Iberian and Siberian lakes Memòria presentada per Marina Escala Pascual per optar al títol de Doctor per la Universitat Autònoma de Barcelona, sota la direcció del doctor Antoni Rosell Melé. Marina Escala Pascual Abril 2009 Cover photograph: Lake Baikal (Jens Klump, Continent Project) Als meus pares i al meu germà. INDEX Acknowledgements .................................................................................i Abstract .................................................................................................iii Resum ....................................................................................................iv Chapter 1 Introduction 1.1. Paleoclimate and biomarker proxies ....................................................3 1.2. Distribution of Archaea in freshwater environments ........................5 1.3. Origin and significance of GDGTs .......................................................9 1.4. Calibration of GDGT-based proxies ..................................................14 1.5. Objective and outline of this thesis ....................................................19 Chapter 2 Methodology 2.1. A review of GDGT analysis .................................................................23 2.1.1. Development of GDGT analysis ..................................................23 2.1.2. The future: intact polar lipids analysis .........................................29 2.2. GDGT determination in the present thesis .......................................31 2.2.1. Material and chemicals ................................................................31 2.2.1.1. Laboratory material cleaning .........................................................31 2.2.1.2. Solvents ...........................................................................................31 2.2.1.3. Standards..............................................................................31 2.2.2. Analytical instrumentation ..........................................................32 2.2.2.1. HPLC/APCI-MS systems ................................................................32 2.2.2.2. GDGT identification ......................................................................32 2.2.2.3. Linear range .........................................................................35 2.2.2.4. Limit of detection ........................................................................... 36 2.2.2.5. Precision and reproducibility ..................................................37 2.2.3. Interlaboratory comparison ..........................................................40 2.3. Rapid screening of glycerol dialkyl glycerol tetraethers in continental Eurasia samples using HPLC/APCI-ion trap mass spectrometry................................................................................42 2.3.1. Experimental section ....................................................................42 2.3.2. Results and discussion .................................................................43 2.4. Analytical considerations for the use of the paleothermometer TEX86 and the BIT index regarding the choice of clean-up and instrumental conditions ...............................................................46 2.4.1. Experimental section ...................................................................46 2.4.1.1. Comparison of clean-up procedures .........................................47 2.4.1.2. Comparison of adsorbents ......................................................47 2.4.1.3. GDGT determination by HPLC/APCI-MS ................................47 2.4.1.4. Comparison of HPLC columns ................................................48 2.4.1.5. Comparison of mass spectrometers .........................................49 2.4.2. Results and discussion .................................................................49 2.4.2.1. Clean-up methods .................................................................49 2.4.2.2. Comparison of adsorbents ......................................................50 2.4.2.3. HPLC column effects .............................................................51 2.4.2.4. Comparison of mass spectrometers .........................................52 2.4.3. Conclusions .................................................................................55 Chapter 3 Exploration of GDGT-based proxies in Iberian lakes for climate reconstruction 3.1. Introduction ..........................................................................................59 3.2. Study area and sample collection ........................................................61 3.3. Methodology ..........................................................................................65 3.3.1. GDGT analysis ............................................................................65 3.3.2. Statistics .......................................................................................65 3.3.3. Lake surface versus air surface temperature ................................67 3.4. Results from Iberian lakes ...................................................................70 3.4.1. Distribution of GDGTs and proxy indices ..................................70 3.4.2. Results from Principal Component Analysis ..............................76 3.4.3. Results from Hierarchical Cluster Analysis .................................82 3.4.4. Comparison of Iberian lakes with other lacustrine sites ..............89 3.5. Discussion and conclusions ..................................................................91 Chapter 4 Appraisal of GDGT proxies in Lake Baikal 4.1. Site description: Lake Baikal region ..................................................97 4.1.1. Location, geomorphology and hydrology ...................................97 4.1.2. Climatology, hydrography and productivity ................................99 4.2. Rationale for this study in Lake Baikal ...........................................104 4.3. Sediment traps and surface sediments ............................................106 4.3.1. Sample description ....................................................................106 4.3.2. Results and discussion ...............................................................107 4.4. GDGTs in Baikal sediment cores as climatic proxies .....................116 4.4.1. Sediment core description .........................................................116 4.4.2. Lake Baikal record of GDGT proxies for the last glacial-interglacial cycle ............................................................118 4.4.3. Comparison with other proxies .................................................121 4.4.4. Comparison with models ...........................................................125 4.5. Conclusions and outlook ...................................................................129 Chapter 5 Archaeal lipids in new archives 5.1. Archaeal lipids in drill core samples from the Bosumtwi impact structure, Ghana ...................................................................133 5.1.1. Introduction ...............................................................................133 5.1.2. Samples and methods ................................................................134 5.1.3. Results and discussion ...............................................................135 5.1.4. Summary and conclusions .........................................................139 Chapter 6 Conclusions and outlook Advantages and pitfalls of GDGT proxies and outlook for future studies ................................................................................143 Glossary ..............................................................................................149 Index of figures and tables ................................................................151 References ..........................................................................................155 Appendices 1. Analytical protocols .......................................................................179 2. Data compilation ............................................................................184 3. Published manuscripts ..................................................................209 An interlaboratory study of TEX86 and BIT analysis using high-performance liquid chromatography-mass spectrometry.......211 Rapid screening of glycerol dialkyl glycerol tetraethers in continental Eurasia samples using HPLC/APCI-ion trap mass spectrometry ..........................................................................225 Analytical considerations for the use of the paleothermometer Tetraether Index86 and the Branched vs Isoprenoid Tetraether Index regarding the choice of cleanup and instrumental conditions.......................................................................................229 Archaeabacterial lipids in drill core samples from the Bosumtwi impact structure.............................................................237 Agraïments - Acknowledgements Agraïments - Acknowledgements Vull donar les gràcies a l’Antoni Rosell, per donar-me l’oportunitat d’investigar en el camp del paleoclima i per tot el que
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