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ALMA MATER STUDIORIUM UNIVERSITA DI BOLOGNA

SCUOLA DI SCIENZE

CORSO DI LAUREA IN SCIENZE GEOLOGICHE DIPARTIMENTO DI SCIENZE BIOLOGICHE, GEOLOGICHE E AMBIENTALI

TESI DI LAUREA

GLACIAL-INTERGLACIAL PALEOCEANOGRAPHIC VARIATIONS IN THE WESTERN TROPICAL INDIAN OCEAN

Tiago Jos Zuanazzi Biller Teixeira RELATORE: Stefano Claudio Vaiani CORRELATORE: Rik Tjallingii

Anno Accademico 2011/2012 Sessione III 1

Riassunto
Questo studio fornisce una ricostruzione paleoclimatica e paleoceanografica del tardo Quaternario nella zona del Canale del Mozambico tramite lo studio del carotaggio 64PE304-26 (Latitudine 09.76985 S; Longitudine 39.91055E; profondit dacqua 482m). Le analisi condotte in questo sondaggio comprendono: 1) analisi dei rapporti isotopici di ossigeno e carbonio ( 18O; 13C) eseguite nei gusci di foraminiferi planctonici appartenenti alle specie Globigerinoides ruber (dOrbigny, 1839) e Neogloboquadrina dutertrei (dOrbigny, 1839); 2) analisi dei rapporti elementari, in particolare Ca/Ti e Mg/Ca; 3) distribuzione granulometrica dei sedimenti; 4) analisi della suscettibilit magnetica.

Il quadro cronologico della successione stato ricostruito utilizzando un modello di et basato sulla correlazione con la scala di riferimento LR04 Global Pliocene-Pleistocene Benthic 18O Stack (Lisiecki e Raymo, 2005). Questo ha permesso di attribuire la successione esaminata agli ultimi 400 mila anni.

I dati ottenuti evidenziano: 1. I rapporti isotopici dellossigeno sono stati eseguiti sui gusci di G. ruber e N. dutertrei. Le analisi su G. ruber registrano le variazioni del rapporto nelle acque di superficie (0-50m di profondit), mentre quelle eseguite su N. dutertrei al termoclino (100-200m di profondit). Si osserva che i picchi di 18O presenti allinizio dei periodi interglaciali si registrano prima al termoclino (dati misurati su N. dutertrei) che nelle zone superficiali (dati misurati su G. ruber). Si evidenzia che la composizione isotopica dellossigeno, strettamente legata alle variazioni di temperatura, prima ha cambiato al termoclino, poi nelle acque di superficie. Gli stadi isotopici dellossigeno (MIS) dei periodi interglaciali mostrano un picco iniziale del 18O a cui segue una graduale fase decrescente. 2. La variazione del rapporto Mg/Ca, considerato un proxy per le paleotemperature, sostanzialmente confrontabile, limitatamente alle analisi eseguite su G. ruber, con il record del 18O. La variazione del rapporto Mg/Ca su esemplari di N. dutertrei ha fornito risultati non pienamente interpretabili per problemi analitici. 3. I dati di 13C del G. ruber presentano un intervallo di valori che decresce verso lOlocene ed alcuni livelli anomali durante il MIS 9. Qu esti dati mostrano che i livelli di 3

produttivit biologica sono significativamente variati nelle acque superficiali (0-50m di profondit). Il confronto fra la curva del 13C e quella del 18O mostra variazioni spesso opposte, specialmente durante il MIS 9. 4. Le analisi granulometriche evidenziano che il contenuto in sabbia aumenta durante i periodi glaciali e mostra un andamento inversamente proporzionale al tasso di sedimentazione. 5. Il rapporto Ca/Ti (ottenuto con analisi XRF) ha permesso di registrare la variazione del contenuto in sedimenti carbonatici (alto Ca/Ti) e litici (basso Ca/Ti) in relazione alla ciclicit climatica. Da ci emerso che le variazioni della componente litica sono proporzionali alle variazioni del contenuto in sabbia e sono pi alte durante i periodi glaciali. 6. I dati di suscettivit magnetica sono stati usati per definire lorigine marina (bassa suscettivit magnetica) o terrigena (alta suscettivit magnetica) dei sedimenti. Questi dati sono confrontabili, sebbene con locali differenze a quelli ottenuti con il rapporto Ca/Ti.

Keywords: Marine isotope stage, Isotope ratio, foraminifera, G. ruber, N. dutertrei, Paleoceanography, Paleogeochemistry

Contents
Riassunto ................................................................................................................................................. 3 1 2 3 Introduction ..................................................................................................................................... 6 Regional setting ............................................................................................................................... 9 Materials and methods.................................................................................................................... 13 3.1 3.2 Sampling and treatment .......................................................................................................... 13 Data acquisition ...................................................................................................................... 20

3.2.1 X-ray fluorescence (XRF)...................................................................................................... 20 3.2.2 Magnetic susceptibility .......................................................................................................... 22 3.2.3 Mass spectrometry ................................................................................................................. 22 4 Results and interpretation ............................................................................................................... 24 4.1 Age Model ................................................................................................................................... 24 4.2 Sedimentation rate and sediment composition ............................................................................... 26 4.3 Stable isotopes ............................................................................................................................. 28 5 Discussion...................................................................................................................................... 32

Conclusions ........................................................................................................................................... 34 Acknowledgments ................................................................................................................................. 35 References ............................................................................................................................................. 36 Appendix ............................................................................................................................................... 39

Introduction

The isotopic composition of seawater varies considerably with geographical location and with depth in the water column, as a result of ocean current and heat transfer dynamics. The continuum of water column isotopic composition can be best assessed examining geochemical proxies such as stable isotopes of oxygen, carbon (180, 13C) or Mg/Ca ratios from tests of planktonic foraminifera species that live in different water depths, thus calcifying at different temperature, salinity, chlorophyll content, light intensity, etc. (Mohtadi et al., 2011) The choice for the oxygen isotopic ratios (18O) as a proxy has as support: The liquid and solid oxygen deposits display linear variation of composition according to temperatures; 1) Changes in isotopic concentrations can be precisely and relatively easily measured; 2) Oxygen compounds are sufficiently stable in time. Although changes in kinetic processes can also induce changes in the isotope abundances, precise measurements from carbonate fossils are reliable to determine the temperatures in which they were formed (Urey, 1947; Emiliani, 1970; Barker et al., 2003) Water molecules with different oxygen isotopes in their structure require different amounts of energy to vaporize as a result of the different masses; as H 216O is more prone to evaporation than H218O, the warmer it is (more evaporation) more H216O is preferentially removed from the water basin and trapped in eventual ice caps (e.g. during glacial periods), inducing a variation in the ratio of oxygen isotopes. Thus, H2O that is part of the terrestrial water cycle is enriched in the light 16O isotope (i.e. is isotopically depleted) and sea water is enriched in the heavier 18O. Glacial ice is therefore made primarily of water with the light 16O isotope. This leaves the oceans enriched in the heavier 18O during glacial periods, when more 16O is trapped in glacial ice. During interglacial periods, 16O melts out of ice and the oceans become less 18O rich (Figure. 1).

Figure. 1. The amount of 18O is tendentially much lower in ice shields than in sea water, where it tends to remain. (Ruddiman, 2007)

Carbon isotope ratio (13C/ 12C) was selected for analysis for giving an insight on the biologic activity at the selected location. The interpretation of the 13C is based on the fact that through 6

photosynthesis organisms incorporate preferentially 12C instead of 13C, which makes organic matter poor in 13C (Figure 2). Some of the carbon in the organisms living issue is removed from the biological cycle by, in case of oceans, being incorporated as seafloor sediment. This makes surface waters gradually enriched in 13C (Ruddiman, 2007). The amount of 13C is therefore dependent on the biological productivity in superficial waters. Such process induces a specific 13C concentration in the seawater and this concentration is incorporated in the foraminiferal calcite that eventually becomes part of sediment.

Figure 2. Photosynthesis converts inorganic carbon into the organic form, and by a biological preference for incorporating 12C, this induces negative shifts in 13C values in the environment (Ruddiman, 2007).

Foraminifera are amoeboid protists that incorporate the available oxygen and carbon of the seawater in their calcium carbonate tests. Each species prefers a certain depth range within the water column. When these organisms perish, their calcite skeletons precipitate and accumulate at the seafloor, where they are abundantly preserved in sea-bottom sediments. Foraminifera tests are a predominant share of calcareous sediments above the carbon compensation depth (CCD) (Pytkowicz, 1970). In the sedimentary sequence of a basin, such organisms provide a record of past isotopic compositions, therefore being useful for investigating the local paleoclimatic and paleoceanographic evolution and its insertion in a global framework.

This research thesis aims to reconstruct the past climatic patterns of the Western Tropical Indian Ocean. Piston Core 64PE304-26 (Latitude 09.76985 S; Longitude 39.91055E) was examined through the analysis of Ca/Ti, Mg/Ca, X-Ray Fluorescence (XRF) and Magnetic Susceptibility in its sedimentary content and the analysis of Mg/Ca and stable isotopes ( 18O; 13C) specifically in its fossils of Globigerinoides ruber and Neogloboquadrina dutertrei. The calcite tests, produced by the foraminifera that inhabited the upper water layer ( G. ruber; 0-50m depth) and the thermocline layer (N. dutertrei; 100-200m depth), allow for the study of past isotopic compositions at different water depths.

Regional setting

Piston Core 64PE304-26 was obtained in the north-western part of the Mozambique Channel, Indian Ocean, about 12km off the coast of Tanzania (Latitude 09.76985 S; Longitude 39.91055E; water depth 482m) (Figure 3).

Figure 3. Location of core 64PE304-26, 12km off Tanzania, NW of the Mozambique channel.

Oceanic conditions The regional oceanic conditions are predominantly set by the local ocean currents, the monsoonal patterns (Figs. 4 and 5) and the position of the ITCZ (inter tropical convergence zone where northern and southern tradewinds meet) ( Fig 5).

Figure 4. The Indian Ocean and its dominant Currents (Bigg, 1995)

Summer Monsoon: It is the response to an atmospheric pressure difference between the High Tibetan Plateau and the tropical Indian Ocean. During northern hemisphere summer, low atmospheric pressure at the Tibetan Plateau is faced with higher pressure over the cooler Indian Ocean, provoking the cyclonic summer-monsoon wind patterns. The cyclonic wind enforces upwelling at the Somali margin (Fig. 6), allowing cold, nutrient rich waters to approach the surface. Tropical Indian Ocean vapour provides moisture and enhances the monsoon. Sea surface temperatures (SST) and the displacement of the Inter-tropical Convergence Zone (ITCZ) (Fig. 5) influence the monsoonal intensity. (Rashid et al., 2011). Late summer conditions are strong air flow from the Arabian Sea northeast ward into India ("Southwest monsoon"), accompanied by large precipitation over land. Wind along Arabia is especially intense ("Somali Jet" or "Findlater Jet"), like an atmospheric western boundary current. The Somali jet forces major upwelling along the Arabian coast (offshore Ekman flow). Circulation in the Arabian Sea is anti-cyclonic and the northward Somali Current (western boundary current) is fully developed.

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Winter Monsoon: In autumn, the sea-air temperature contrast decreases. The Somali jet swings to the south and blows eastward ("Transition"). During the Transition, a strong eastward surface jet develops in the ocean along the equator. The Somali Jet weakens in these off seasons. In winter, the wind blows from land to sea ("Northeast monsoon"). Upwelling in the Arabian Sea ceases, circulation in the Arabian Sea weakens and the Somali Current can reverse.

Figure 5. Inter-Tropical Convergence Zone (ITCZ) variation across Africa in boreal summer (left) and winter (right).The position of the core 64PE304-26 (blue circle) is north of the ITCZ in January and south of the ITCZ in July.

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Figure 6. Upwelling associated with Monsoons austral summer (Tomczak and Godfrey, 2003). Upwelling brings to the surface nutrient-rich waters, which increases biological productivity levels.

Geological framework: Mozambique channel: within the Mozambique channel, the Davies ridge runs north-south between about 13 and 18S, rising to nearly 300 m below the surface, with origins reminiscent of old continental or lithospheric fractures left over by the initial separation of Madagascar from the African continent. The African and west Madagascan coasts are the oldest coastlines of the Indian Ocean, dating from their breakup almost 180 Myr. The Mozambique Channel is considered one of the oldest tropical coastlines, and perhaps a stable refuge over many tens millions of years. Africa/Madagascar have moved over the last 65 million years (some northward migration, on the order of 15 latitude), and their relative positions have remained relatively constant (Bigg, 1995).

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Materials and methods

3.1 Sampling and treatment Piston Core 64PE304-26 (Fig. 7) was obtained by the Research Vessel Pelagia, from the northwestern part of the Mozambique Channel, Indian Ocean, about 12km off the coast of Tanzania at a water depth of 482m. Analyses of the core were performed at the NIOZ (Netherlands Institute for sea research, Texel).

Figure 7. Description of core 64PE304-26 done on-board.

The core has been longitudinally divided in two half sections one for sampling and the other for archive. The total length of the core is 674cm, divided in 7 sections. Sample preparation was executed by myself at the NIOZ (Texel) facilities, using the following the procedures: Steps: 13

Core preparation for XRF scanner: As the XRF is a non-destructive method, the archive part of the core is used for the XRF. The core is taken from the fridge (~4C) and left for a few hours to reach room temperature. After removal from plastic protection, in order to remove some eventual impurity that could interfere with test results, the exposed surface of the core is cleaned by removing a thin superficial part of the sediment, which was in contact with protective casings and also a foil from previous tests. When clean, on the exposed part of the core is covered with a particular plastic foil (4m thick) to avoid contamination of the sensor unit. The XRF scanner measures directly at the split-core surface of the sediment core. Core preparation for Magnetic Susceptibility test: The procedure is similar to the preparation for the XRF scanner except for: The foil used is an average plastic sheet; Supports on which the core is put are wooden ones (to avoid magnetic interference). Sampling and Freeze-drying: The working half of the sediment core was sampled every 2.5cm and in two series using 10ml syringes. The 10ml sediment was transferred into a sample vial. These vials are weighed and put in a freezer for at least 3 hours. When completely frozen, the samples are placed in a freezedryer. The freeze dryer applies a vacuum to these samples, which forces sublimation of the frozen water, drying the samples. Once dried, and having the weight of the samples with the full water content, we can follow with acquiring their dry weight, revealing the initial water content. Sieving: The freeze-dried samples are to be sieved, but only the ones obtained every 5cm of depth (that is, every other sample). The used sieves - 63m were cleaned between samples using an ultrasound bath and dried using a pressured air. Samples were sieved using a mild water jet to wash away the fine grained (<63m) sediment content. The larger fraction from each sample is removed from the sieve using ethanol and washed into a separate glass bowl (the ethanol is poured from the bottom to the top of the sieve, opposite to the sieving sense, so that as much as possible of the material falls into the bowl). The bowls are put into an evaporation chamber to dry the samples. Packing (weighing and casing of dry samples after sieving): Using a funnel, the material contained in the glass bowls (thats now dry) into a final glass. A small loss of material is expected. With the sample inside the glass recipient, this is now put on a precision scale, weighed and stored. After finishing with one sample, all objects were cleaned to minimize contamination/mixing before processing the next sample.

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Foraminifera test picking:

Planktonic foraminifera (G. ruber dOrbigny, 1839; N. dutertrei dOrbigny, 1839) Fig 8, were identified following the descriptions of (Parker, 1962) and (Wang, 2000). The selected size range was 250-315m, in order to. minimize ontogenic effects on the geochemical composition of the tests or in order to analyse shells always at the same development stage. Using two different sieves (0.250 and 0.315mm) the material is divided in 3 different size groups: 63 to 250m; 250 to 315m, and >315m. For this study 13500 foram tests were picked: 50 individuals of G. ruber and 50 of N. dutertrei. per sample. For 18O measurements 30 to 80 g of calcite were required for each sample and, as the average weight of each species being determined statistically ( G. ruber 15 g; N. dutertrei 20 g), for each sample measurement 5 individuals of G. ruber and 3 of N. dutertrei were used. For the Mg/Ca measurements, around 300g of calcite were required for each sample, and considering the average weight of each species individual, for each sample measurement 20 individuals of G. ruber and 15 of N. dutertrei were used.

Figure 8. Foraminifera tests selected for this study with schematization of dwelling position in water column (Auras-Schudnagies et al., 1989)of both studied foraminifera (G. ruber 0-50m, and N. dutertrei 100-200m).

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Sample cleaning for stable isotope measurement:

Collecting an amount of foraminifera that will, after cleaning, be within the 30-80 micrograms range (in this case, their average weight was 15g per individual G. ruber and 20 g per individual N. dutertrei, so it were used 5 specimens of G ruber and 3 specimens of N dutertrei per sample), putting them in 2ml tubes, adding demineralized water (0.550 ml) and placing samples in the ultrasound bath for about one minute. Further 0.550 ml of demineralized water was added and samples were allowed to settle to the bottom of the tube for around 30 seconds. Then, after removing (with a pipette) as much of the water contained in the tubes as possible, samples (with tube lid open) were put in evaporation chamber. After evaporation is complete, samples were stored upon Mass Spectrometry. Foraminifera cleaning for Mg/Ca measurement

1. Foram Cleaning Procedure for Mg Clay removal: For analysis of the elemental composition of the foraminiferal calcite, the following procedure was followed (adopted from Barker et al., 2003). All samples were handled individually in order to maximize cleaning effectiveness (batch treatment for ultra-sonication is appropriate). Separate pipette tips for adding and removing reagents were used for each sample. Having opened the test chambers during crushing, much of the test fill will be loosened and easily brought into suspension. 1. Squirt 500l of UHQ H2O onto the crushed sample (trapped air bubbles may be freed by flicking the tube end). 2. Allow the sample to settle for approximately 30 seconds. 3. Remove the overlying solution (supernatant) with a separate pipette the size of a 1000ml pipette tip is suitable for removing most of the overlying liquid from the tube without risk of sample loss. At this stage, all tubes should still contain about 10-20ml of H2O. 4. Place the sample rack in an ultrasonic bath for 30 seconds - this will encourage separation of more tightly bound clays from the test surfaces. Suspended clays will appear as a milky residue in the liquid just above the sample. 5. Squirt 500l of UHQ H2O onto each sample - this will agitate the sample and bring loose clays into suspension. 6. Briefly allow the sample to settle (minimal settling technique) - sufficient settling will only take a number of seconds (long enough for the distinct carbonate grains to reach the bottom). After this period the remaining settling material will mainly comprise unwanted silicate particles. 16

7. Remove the overlying solution. 8. Repeat steps (4) to (7) a further 4 times. More repetitions may be necessary for as long as clays are being visibly brought into suspension by ultra-sonication. After the water cleaning steps, methanol is used for further clay removal - the lower viscosity of this reagent should dislodge material still attached to the carbonate tests. 9. Squirt 250l of Aristar methanol into each tube. 10. Ultra-sonicate the tubes for 30 seconds. 11. Treating each tube individually, lift the methanol off the sample with a pipette and squirt straight back in to bring clays into suspension. 12. Allow sample to settle for a few seconds and remove the methanol. 13. Repeat steps (9) to (12). 14. Repeat steps (5) to (7) in order to remove any remaining methanol (further ultrasonication may be applied if cleaning is not complete). Removal of organic matter: 1. Add 250l of alkali buffered 1% H2O2 solution to each tube and secure the rack with a lid to prevent tubes popping open whilst under pressure. 2. Place the sample rack in a boiling water bath for 10 minutes. At 2.5 and 7.5 minutes remove the rack momentarily and rap on the bench top to release any gaseous build-up. At 5 minutes place the rack in an ultrasonic bath for a few seconds and return to the water bath after rapping on the bench the aim of these interim steps is to maintain contact between reagent and sample. 3. Flick the sample tubes to remove gas bubbles and ensure the samples have settled then remove the oxidizing reagent using a pipette. 4. Repeat steps (1) to (3). 5. Remove any remaining oxidizing reagent by filling the tube with UHQ H2O and removing after settling. This step should be repeated 1-2 times.

Dilute acid leach: A dilute acid is used to remove any adsorbed contaminants from the test fragments. 1. Add 250l of 0.001M HNO3 to each sample. 2. Ultra-sonicate all samples for 30 seconds. 3. Remove acid from each sample. 4. Squirt UHQ H2O into each tube. It is important to replace the leach acid with H2O as soon as possible for all samples in order to prevent excess dissolution. 5. Remove the overlying H2O. 6. Repeat steps (4) and (5). 7. Using a 10l pipette, carefully remove any remaining solution from each sample. Samples should be stored after this stage, then dissolved and diluted on the day they are to be run. 17

Dissolution: In order to ensure accurate dilutions, all volumes were pipetted with.an accuracy of: 1. Add 350l of 0.075M HNO3 to each sample (for large samples 500l may be used). 2. Ultra-sonicate to aid dissolution. 3. Every few seconds, flick each tube to allow any build-up of CO2 to escape and the reaction to continue. 4. As soon as the production of CO2 ceases, shake the samples to mix. 5. Centrifuge (5000 rpm for 5 minutes) to settle any remaining small silicate particles. 6. Immediately transfer 300l of solution to a clean sample tube, leaving any particles to be discarded in the residual 50l If the dissolution acid is left on a sample containing any silicate or other non-carbonate material for longer than is necessary to dissolve the sample, there is a high risk of contamination by elemental leaching. Dilution: After cleaning and dissolution, 20 planktonic foraminifera should give Ca concentrations in the range 100 200 ppm, depending on the species and sample loss during cleaning. The method for Mg/Ca & Sr/Ca determinations using the Vista ICP-AES requires, for best precision and accuracy, solutions containing known Ca concentrations of typically either 60 or 100 ppm and uses ~250l solution per analysis. Two runs of each sample are required; an initial concentration determination followed by a second run at optimum Ca concentration for Mg/Ca and Sr/Ca determinations. For samples contained in 300l of 0.075M HNO3 after centrifuging, a 5 fold dilution should be done for the initial concentration determination, followed by dilution of the remaining concentrate as required. 1. Set up a series of clean 0.5ml thin walled vials for the dilutions. 2. Add 200 l of 0.075M HNO3 to each. 3. Add 50 l sample to give a 5 fold dilution. It is important that volumes are accurately pipetted e to ensure correct concentration calculations and subsequent dilutions. Run the diluted samples on the Vista to determine Ca concentrations. Calculate dilutions required to give optimum Ca for the intensity calibration of Mg/Ca & Sr/Ca ratios. Dilute the remaining 250l of sample concentrates as calculated and run on the Vista using the intensity ratio calibration at the appropriate Ca concentration. 18

2.

Reagents

Bottle required.

Tip rinse: Acid (10% HNO3) mouth Elga UHQ H2O mouth Removal of fine clays: Elga UHQ H2O Methanol (Aristar) Oxidising reagent (to remove organic matter) Alkali buffered 1% H2O2 solution. 250 l oxidizing solution used per sample. Prepare fresh mixture for each batch of samples. Prepared from: Hydrogen peroxide 30% w/v Aristar grade (stored in fridge). 0.1M sodium hydroxide (Aristar grade) in Elga UHQ water. 0.1M NaOH = 4g / litre. (NaOH = 40.00g g mol-1). Add 100 l H2O2 to ~10 ml 0.1 M NaOH, sufficient for ~ 20 samples.

125 ml w ide 125 ml wide

125 ml wide mouth 125ml dropper bottle

8ml dispense. 500ml

15ml test tube.

Dilute acid leach: QD 0.001 M HNO3 500ml stock 250 l used from 1 - 5 times per sample. 30ml dispense 75 fold dilution of 0.075 M HNO3 1ml 0.075M HNO3 in 75ml UHQ H2O or 6ml 0.075M HNO3 in 450ml UHQ H2O. Dissolution: QD 0.075 M HNO3 1000ml stock 500 l used per sample. 30ml dispense 200 fold dilution of QD conc. HNO3 (15M) 5ml conc. HNO3 in 1 litre UHQ H2O. Reagent bottle sizes are suggestions for typical use. Adjust according to requirements and availability.

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3.2 Data acquisition


After preparing the samples, the following analyses were performed:

3.2.1 X-ray fluorescence (XRF) This is the emission of characteristic "secondary" fluorescent radiation from a sample material after irradiation with high-energy X-rays. The method is widely used for elemental and chemical analysis, particularly in the investigation of metals, glasses, ceramics and building materials, and for research in geochemistry, forensic science and archaeology. Avaatech XRF core scanner (Fig. 9), was used for this research and covers atomic mass ranges from Al to U. Nevertheless, this method has its limitations due to physical properties such as water content, porosity, grainsize differences and surface roughness which may influence the scanner data. Especially lighter elements, such as Al and Si, are affected by water content (Tjallingii et al., 2007). However, a log-ratio calibration adequately minimizes bias originating from physical and geometrical irregularities (Weltje and Tjallingii, 2008).

Figure 9. Avaatech XRF core scanner at NIOZ, Texel. Internal devices include: Canberra Silicon Drift Detector, 500m thick; Internal and external Ag collimator, 25 Be; Peltier cooled, two stages; Canberra DSA-1000 Digital Signal Processing unit.

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Figure 10. Schematization of XRF operational principle: The X-ray induces the ejection of an electron; another electron, from an outer energetic level, will occupy the gap. The provoked energy difference is emitted as electromagnetic radiation, which is detected by the XRF device.

When materials are exposed to short-wavelength X-rays or to gamma rays by the XRF core scanner, ionization of their component atoms may take place. Ionization consists of the ejection of one or more electrons from the atom, and may occur if the atom is exposed to radiation with an energy greater than its ionization potential. X-rays and gamma rays can be energetic enough to expel tightly held electrons from the inner orbitals of the atom. The removal of an electron in this way renders the electronic structure of the atom unstable, and electrons in higher orbitals "fall" into the lower orbital to fill the hole left behind. In falling, energy is released in the form of a photon, the energy of which is equal to the energy difference of the two orbitals involved. Thus, the material emits radiation, which has energy characteristic of the atoms present. The term fluorescence is applied to phenomena in which the absorption of radiation of a specific energy results in the re-emission of radiation of a different energy (generally lower) ( Fig. 10). The X-ray spectrum acquired during the process reveals a number of characteristic peaks. The energy of the peaks leads to the identification of the elements present in the sample, while the peak intensity provides the absolute or elemental concentration (Guevara et al., 2005).

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3.2.2 Magnetic susceptibility Magnetic susceptibility has been measured on the complete cores with a loop sensor onboard Research vessel Pelagia. For a first impression we plotted the log-ratio of Ti over Ca, which can be interpreted as the relative variation of terrigenous sediment and marine carbonates (Ellwood et al., 2003) (Fig. 5). This measurement is a non-destructive and cost effective method of determining the presence of iron-bearing minerals within the sediments. The whole core, or individual sediment samples, are exposed to an external magnetic field which causes the sediments to become magnetized according to the amount of Fe-bearing minerals present in the core (Fig. 11).

Figure 11. Magnetic susceptibility device (left) and diagram representing the sorts of response to the induced magnetization that are used for identification of core composition (right).

3.2.3 Mass spectrometry In this study a mass spectrometer (MS) Thermo Scientific MAT 253 equipped with a Kiel IV Carbonate Device for CO2 production (Fig. 12) was used. MS is an analytical instrument that measures the mass ratio of elements. It is used for determining masses of particles and elemental isotopic composition of a sample. In order to determine the isotopic ratios in CO 2 molecules, the studied calcite tests undergo the following process: 1. A foraminifera sample is loaded onto the mass spectrometer, and gets dissolved by al acid, releasing CO2 2. CO2 is purified trough different traps to remove any water contamination

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3. The different isotopes of each element are magnetically separated and their ratio measured

Figure 12. Thermo Scientific Kiel IV Carbonate Device, used for the Carbon and Oxygen isotopic ratio analysis in this study.

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Results and interpretation

4.1 Age Model The age model is based on the correlation between the stable oxygen isotope record ( 18O) from the planktonic foraminifera G. ruber in core samples and the LR04 Global Benthic 18O stack of Lisiecki and Raymo (2005) (Fig. 13). Definition of a time frame for the core was provided by (1) plotting the stable isotope measurements and, (2) the obtained graphic (which has as axes 18O and depth) being compared with a reference (LR04 Global Pliocene-Pleistocene Benthic 18O Stack; (Lisiecki and Raymo, 2005) also containing the 18O but already dated. Comparison was done using the program Executor, where the trends/variations were correlated by linear interpolation of the plotted data from Lisiecki and Raymo (2005) and that collected in core 64PE304-26. An important potential error in the reference used in this study (the LR04 age model) is uncertainty in the orbital patterns, with the most recent part of the model having its uncertainty in the sedimentation rates (SR) and in the considered response times of ice sheets (Lisiecki and Raymo, 2005). The age model reveals deposition during the last ~400kyr and was segmented in Marine Isotope Stages (MIS), ranging from the MIS 1 (Holocene) to the transition between MIS 10 and 11. The observed pattern shows glacial periods (troughs in 18O record) corresponding to higher ice mass volumes/lower sea levels and interglacial periods (peaks in 18O record) corresponding to lower ice masses/higher sea levels.

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Figure 13. Age model for core 64PE304-26: Top curve represents 18O from G. ruber of core 64PE304-26; the lower part shows LR04-Stack (Lisiecki and Raymo, 2005) divided in MIS. Correlation uses the selected data-points in both plots and provides the age model through linear interpolation.

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4.2 Sedimentation rate and sediment composition The time frame provided by the Age Model allows for the definition of Sedimentation Rates (SR) (Church and Ryder, 1972), specifically dividing the time spam by the length of core 64PE304-26 it is obtained that the SR of the core is on average 594kyr/cm. In detail, considering the G. ruber 18O variations, this rate is constrained between about 4cm/kyr during interglacial periods and 0.6 cm/kyr during glacial periods (Fig. 14). Considering the granulometric distribution of the sedimentary content in core 64PE304-26 and focusing on the bulk sand fraction (>63m) and its proportion to the total amount of sediment (Fig.14), follows the pattern of rising during glacial periods (up to >50%) and diminishing (to 1020%) during interglacials. The Sand % shows also the tendency of being inversely proportional to the SR. Microscope investigation reveals that the bulk sand fraction is mainly (>50%) formed of carbonatic skeletons. The Ca/Ti ratio, obtained by XRF analyses, was used to record the variation of lithogenic (low Ca/Ti ratio) and carbonatic (high Ca/Ti) sediments showing possible relationships with sand concentration and glacial/interglacial ciclicity. Results reveal that the amount of lithogenic material fluctuates proportionally to the bulk sand fraction ( Fig. 14), being also higher/lower in glacial/interglacial periods. Magnetic susceptibility was used as proxy for the origin of the sediment (Chen et al., 1997).This method highlights Fe-bearing mineral content, thus indicating if the sediment source is marine or terrigenous higher magnetic susceptibility indicates terrigenous and lower magnetic susceptibility indicates marine sediments (Bloemendal and deMenocal, 1989). The general trend of the magnetic susceptibility is the same of the Ca/Ti, but in several points there are relevant disagreements (e.g.: 20cm; 90cm; 200cm; 450cm; 480cm; 580cm; 670cm). No obvious erosion surfaces could be found (Hillgartner, 1998), but stratigraphic hiatus cannot be excluded, especially at the interglacial-glacial transitions that show a strong increase of the bulk sand fraction from 10-20% to about 50% or more. From the observation of Fig. 14 it is noted that moments of higher 18O (interglacials) relate to higher SR with lower sand%, while the situation is inverted in glacial periods. Considering the Ca/Ti and magnetic susceptibility, it can be added that in glacials, when the SR is lower and the sand% is higher, the amount of carbonatic-marine sediments is prevalent compared to the amount of lithogenic-terrigenous material and opposite occurs in interglacials. This can be explained by higher SR (Schlager, 2000) interglacials corresponding to a greater input of fine terrigenous sediments brought by runoff; the addition of terrigenous material with different granulometry dwarfs the sand% relative to the total amount of deposition. During glacials lower SRs sand-grained particles become prevalent relative to the total of deposition. 26

Figure 14. Compilation of data obtained from sedimentary content of core 64PE304-26. From top to bottom: Shell 18O of G. ruber; sedimentation rate (SR) based on age model; Sand (>0.63m) percentage; Log(Ca/Ti) and Magnetic Susceptibility.

27

4.3 Stable isotopes The stable isotopic ratios (18O and 13C) retrieved from the foraminifera shells in the sediment of core 64PE304-26 (Fig. 15), being from the species G. ruber and N. dutertrei, reflect the isotopic composition relative to the depths in which each of the organisms calcify their tests , specifically 0-50 for G. ruber and 100-200m for N. dutertrei (Steph et al., 2009). The changes in 18O of G. ruber and N. dutertrei are synchronous and fluctuate in agreement (Anderson and Leng, 2004), although it is seen that the isotopic composition varied differently at different depths (Fig. 16). The peaks in 18O at the start of interglacials are shown to happen before at the thermocline (measured from N. dutertrei) than at the surface (measured from G. ruber), which demonstrates that 18O varied before at the thermocline than at the surface waters, suggesting a bipolar seesaw 1 (Stocker, 1998). When observing the difference between the G. ruber and the N. dutertrei 18O (Fig. 16, center), it can be pointed out that such difference tends to be substantially higher in the beginning of the MIS 9 and 5, and lower by their end. This could mean a sort of homogenization along the period. An asymmetry is observed at the MIS transitions: in the beginning of each interglacial MIS it is noticed an almost vertical rise in 18O, but at the end of each stage, towards glacials, the decrease in 18O is relatively gradual. This trend is mainly shown in MIS 1, 5, 9 ( Fig. 15). MIS 3, compared to the other interglacials, shows much lower 18O, therefore lower inferred sea surface temperatures. In order to assess the biological productivity levels in the core location, the variations of 13C are observed (Ruddiman, 2008). Such data from G. ruber (Fig. 15) show minor variations in the core with the exception of values recorded in the part of succession attributed to MIS 9, characterized by remarkably low 13C. These data reveal how productivity levels might have varied at 0 to 50m of depth. The interpretation of the variations in these biological productivity levels yields that the N. dutertrei values seem to gain amplitude towards the Holocene, while the opposite (decrease in amplitude) appears in the G. ruber record. This indicates that productivity levels due to adequate living conditions for the foraminifera became more constant at the surface waters than at the thermocline depth. When compared to the 18O curve also of G. ruber, the 13C data, even if with a gradually lower value amplitude towards the Holocene, shows variations generally (though not always) opposite to those of the 18O, especially during MIS 9. The Mg/Ca data provide a further temperature proxy (Fig. 16, bottom) (Barker et al., 2005). These data are passive of imprecision, especially in the 110 to 135kyr interval, possibly for
1

Occurrence of warm temperatures in the Southern Hemisphere while temperatures in the Northern Hemisphere are colder-than-average, or vice versa. This pattern is thought to be caused by changes in the ocean's thermohaline circulation.

28

machinery calibration. Generally it is observed that interglacial periods, as expected (Affek et al., 2008), have higher temperature averages. The timing of the variations in the Mg/Ca (Anand et al., 2003) show that initial temperature peaks in MIS 7 and 9 happen before at the surface waters ( G. ruber) than at the thermocline (N. dutertrei), but these temperature peaks, in MIS 5 and 1 (unclear in MIS 3), seem to be precedent in the thermocline than at the surface waters. No definite interpretation about this is drawn in this study except for such observation being correlated to the bipolar seesaw mechanism.

29

Figure 15. Top two curves represent shell 18O and 13C records of G. ruber and bottom curves represent shell 18O and 13C of N. dutertrei. Vertical bars represent MIS segmentation.

30

Figure 16. Records of 18O from G. ruber and N. dutertrei, difference between the precedent, Mg/Ca of G. ruber and N. dutertrei. Vertical bars indicate relative Marine Isotopic Stages (MIS)

31

Discussion

The compositional variations here studied indicate that, given the age model, these variations are correlated to orbital cycles (Vimeux et al., 1999). This study confirms the broadly accepted idea of the insolation distribution as predominant forcing agent for glacial-interglacial cycles (Berger, 1992). It remains for further analysis to investigate if such glacial-interglacial variations had their trigger in the area of core 64PE304-26, a tropical area. This question resides in the timing differences at different depths (as recorded by 18O of foraminiferal species living at different depths in the water column) regarding the transitional points between the observed MIS. This study suggests that start in MIS transitions in this area happened first at thermocline depth than at the surface, proposing that the crucial thermal energy increase/decrease was triggered at another geographical location and later delivered at the area of core 64PE304-26. The local sea currents (Fig. 4) must be an important factor in demonstrating how the mentioned heat transfers happened (Boyle and Keigwin, 1985; Kellogg, 1980). The observed data shows low SR (sedimentation rates), high bulk sand fraction and predominantly marine sediments in glacial periods (Anderson and Ashley, 1991; Dunbar et al., 1985) and the opposite association of factors during interglacials. This suggests that in glacial periods there was less runoff (Marshall and Clarke, 1999) due to less precipitation, which is consistent with the decreased terrigenous feature and the lower SR; the high bulk sand fraction is probably due to the predominance in the sediment of foraminifera tests (which represent most of the sand-sized grains), since the terrigenous material amount which is mostly fine-grained (Stow and Piper, 1984)- decreased. During interglacials more runoff due to the higher temperatures (thus higher evaporation and precipitation) could explain the more terrigenous characteristic, the higher SR and the lower bulk sand fraction - the fine product of the runoff could dwarf the foraminifera (therefore sand grain sized) portion of the sediment. This scenario suggests that an increased erosion during glacial periods, due to the low-stand regime (Park et al., 2000), might not always indicate a higher sedimentation rate. Data on 13C indicates the variations in biological productivity levels (Diester-Haass and Zahn, 1996), which are associated with a number of factors, among which the nutrient availability related to upwelling (Anderson and Prell, 1993). At the studied location it can be observed that at a seasonal scale the upwelling is practically constant and at relatively low levels, which indicates low productivity ( Fig. 6). The 13C data of core 64PE304-26 (Fig. 16) has more incremental variations at the thermocline depth (100-200m; N. dutertrei) than at the surface waters (0-50m; G. ruber). This observation conveys the idea of a more constant regime at the surface than at the thermocline depth. This can be explained by pointing out that: 1)At the thermocline, water circulation can be different from that of surface waters, therefore the source of the water mass can also be different (You and Tomczak, 1993). Water masses of different sources tend to contain different thermal energy (higher or lower) (Huber and Sloan, 2001). In this case, the thermocline waters would come from higher latitudes; 2)At low latitudes, (i.e. tropical regions - such as the 32

location of core 64PE304-26), general climatic conditions tend to be uniform/constant; as the latitude increases, climatic patterns tend to become more variable and present greater oscillations (Addo-Bediako et al., 2000).

33

Conclusions
This study provides a late Quaternary paleoclimatic and paleoceanographic reconstruction of the Mozambique Channel area by selected analyses of core samples including: mass spectrometry (18O; 13C), sediment distribution, elemental ratios (Ca/Ti) and magnetic susceptibility. The used age model was reconstructed by the reference LR04 Global Pliocene-Pleistocene Benthic 18O Stack (Lisiecki and Raymo, 2005) and r eveals a sediment deposition covering the past ca. 400kyr. The following conclusions can be derived from the obtained results:

1. The XRF scanning data, providing Ca/Ti ratios, combined with the granulometry shows an increase (decrease) in oceanogenic content whenever the bulk sand fraction rises (falls), indicating that the sand fraction is mostly carbonatic. This might also imply that, realizing that high Ca/Ti tends to be observed in glacial periods, these shifts are probably due to climatic changes. 2. The observed pattern shows interglacial periods (peaks in 18O record) corresponding to higher ice mass volumes/lower sea levels and glacial periods (troughs in 18O record) corresponding to lower ice masses/higher sea levels. The Interglacial MISs observed through the 18O record have shown to systematically begin with a spike in 18O, but move to the end of the period much more gradually. 3. Planktonic foraminiferal shell geochemistry analyses point from core 64PE304-26 point to G. ruber and N. dutertrei to record annual mean surface (0-50m) and thermocline (100-200m), respectively. It is observed that the peaks in 18O at the start of interglacials happen before at the thermocline (measured from N. dutertrei) than at the surface (measured from G. ruber), leading to conclude that the oxygen isotopic composition ,such as temperature, first changed in the thermocline than in the surface waters. 4. The 13C data from G. ruber presents a value range that diminishes towards the Holocene, specially unbalanced negatively during MIS 9, revealing how productivity levels varied at 0 to 50m of depth. When compared to the 18O curve also of G. ruber, the 13C data, even if with a gradually lower value range towards the Holocene, shows variations generally opposite to those of the 18O, especially during MIS 9.

Acknowledgments
I am very grateful to Rik Tjallingii, my super-efficient supervisor at the NIOZ, Stefano Claudio Vaiani, my very helpful and essential supervisor in Bologna, Caroline Cleroux, Piet Van Gaever, Rineke Gieles-Witte, Juliane Steinhardt, and everyone without whom I would not have made it. I also want to thank the NIOZ for providing such adequate facilities and conditions in which scientific research flourishes, the Netherlands, a country that gained my deep admiration, and the University of Bologna, for giving me background to be able to engage in this enterprise. And of course, I cant forget to express my gratitude to all my friends/family for the strength and support that made this journey much more bearable and helped giving meaning to all this. Theres still a lot to come!!!

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Appendix

#: 7 (0 - 22cm)

#: 6 (22 130.5cm)

#: 5 (130.5 236cm)

#: 4 (236 345.5cm)

#: 3 (345.5 454.5cm)

#: 2 (454.5 564cm)

#: 1 (564 673cm)

Image of core 64PE304-26 divided by section number and depth.

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