Age model of IODP Site U1532
Age constraints used in this study were taken from the shipboard age-depth models, which were established based on biostratigraphy age datums in correlation with magnetostratigraphic polarity zones1. Based on shipboard analyses of Holes U1532A–U1532G, an age-depth model for the Site U1532 was constructed using biostratigraphic age datums (Extended Data Table 1) to constrain correlation of magnetostratigraphic polarity zones at Site U1532 correlated to the Gradstein et al. (2012) geological timescale (GTS2012)2 (see Table T5 in the Expedition 379 methods chapter3). Biostratigraphic age control for the Site U1532 is based on diatom and radiolarian datums3. Sufficient microfossils for biostratigraphic age assignment were only present in the upper ~10 m of the section (i.e. from 0 to 92 m; Lithostratigraphic Subunit IA) which provides an age of middle Pleistocene to recent (0–0.60Ma). Based on diatom and radiolarian biostratigraphy, the interval between ~92 and 156 m is assigned a mid-to-late Pliocene age of 3.2–3.8 Ma. Using these biostratigraphic age control points, interpreted correlation of magnetostratigraphic polarity reversals identified at Site U1532 (Table T16R)4 to the GTS2012 is relatively unambiguous. The interval between 0 and ~45 m is assigned a Pleistocene age, and the interval between ~45 and 150 m represent Pliocene age. Because of an absence of siliceous microfossils, there is no biostratigraphic age control between ~10 and 92 m in Hole U1532A-B4. For Hole U1532A, a reliable shipboard magnetostratigraphy consisting of four normal and four reversed polarity intervals was obtained. These intervals are the Brunhes–Matuyama polarity transition (0.781 Ma), the termination and beginning of the Olduvai Subchron (1.778 and 1.945 Ma), the Matuyama–Gauss polarity transition (2.581 Ma), the termination and beginning of the Kaena Subchron (C2An.1r; 3.032 and 3.116 Ma) and the termination and beginning of the Mammoth Subchron (C2An.2r; 3.207 and 3.330 Ma, respectively) (see Extended Data Table 1). Paleomagnetic measurements in Hole U1532B identified the beginning of the Mammoth Subchron (C2An.2r; 3.330 Ma) and the Gauss–Gilbert polarity transition (3.596 Ma). Total eight magnetostratigraphic tie points were found between 0 and ~100 CSF-A(m) and two tie points between 101 and 146 CSF-A(m) for the basis of the chronology (Extended Data Table 1, Extended Data Fig. 3a). To improve the shipboard chronology further, we have identified more tie points in the present study based on the correlation between geochemical parameters and global benthic δ18O curve (LR04)5 (Extended Data Fig. 2). Elemental ratios of (a) Ba/Al, (b) Ba/Rb, (c) PC1 (first principal component) derived from Principal Component Analysis (PCA) of multiple elemental ratios (Extended Data Fig. 2a, b, c) were compared with the LR04 curve. In addition to previously determined tie points, nine additional new tie-points were identified based on the excursions in the geochemical parameters and its correspondence with the glacial-interglacial signals in the LR04 δ18O curve (shown in Extended Data Fig. 2). Finally, MatLab™-based program “Undatable”6 was used to generate an age-depth model with an uncertainty. The advantage of using Undatable over other available age-depth modelling programs is that it allows for the input of uncertainties in both age and in depth, and for a series of different types of age control points to be incorporated. Undatable was run using 100,000 simulations6. A probability density cloud illustrating the uncertainty envelope around the modeled age‐depth points was computed using Monte Carlo iterations. Blue and black dotted lines show 1σ and 2σ uncertainty, respectively. This revised model is based on sixteen tie-points within the study interval (0–3.5 Ma, Extended Data Fig. 3b, Extended Data Table 1). The age-depth model for the Pleistocene interval is better constrained than the Pliocene interval due to the availability of more tie points/ages and therefore Pleistocene glacial-interglacial variations can be resolved with confidence.
Detrital sediment Nd and Pb isotope measurements
Nd isotopes were measured in the detrital phases of the bulk sediments following the method adopted from earlier studies7,8. Authigenic fractions were extracted and removed from the bulk sediments using the leaching method adopted from previous studies9-11. To ensure complete removal of the authigenic fractions, all samples were leached twice, first for ten seconds followed by a second leach lasting 24 hours. Approximately 0.3 g of powdered and homogenized sediment samples were agitated with a mixture solution of 0.005M hydroxylamine hydrochloride, 1.5% acetic acid, and 0.003M Na-EDTA, buffered to pH 4 with NaOH. Then leachates were removed by centrifugation and washed with Milli-Q water thoroughly. Then residual sediment samples were decarbonated by treating with 0.6 N HCl at 80 °C for ~30 minutes and then supernatant was discarded, and the acid‐free residue was washed with Milli‐Q water. The above steps were repeated to ensure complete decarbonation of the samples and washed with Milli‐Q water and checked with pH paper to ensure that carbonates are removed from the sediments. Subsequently, samples were washed thoroughly with Milli-Q water and dried in the oven at 80° C. Dried samples were then ashed at 600°C to remove organic matter. Approximately 50 mg of ashed samples were digested in precleaned Teflon vials using HF-HNO3-HCL mixture at 120°C. Standard Reference Materials BCR-2 and BHVO-2 were also digested along with the samples. The digested samples were divided in two aliquots for the column chromatography of Nd and Pb. The dissolved samples were subjected to purification by column chromatography. They were passed through columns filled with cation-exchange resin AG50W-X8 (200–400 micron) to separate Rare Earth Elements (REE). Then REE fractions were then passed through the column filled with Eichrom LN specTM (50 – 100 micron) resin to separate Nd from the REEs12.
Nd isotope Analysis
Nd isotope ratios were measured using Multi-collector Inductively Coupled Plasma Mass Spectrometer (Thermo Fischer Scientific, Neptune Plus) at National Centre for Polar and Ocean Research, Goa. Instrumental mass fractionation was corrected using the ratio of 146Nd/144Nd = 0.7219. The mass bias corrected 143Nd/144Nd ratios were normalised to the reported JNdi-1 standard 143Nd/144 value of 0.51211513. A correction for direct 144Sm interference was also applied, with all samples which was below (<0.1% of the 144Nd signal). To ensure the quality of measurement, the international standard JNdi-1 was matrix matched and measured at every five samples. The obtained average ratios were 0.512115 ± 10 ppm (2σ, n= 51). The external reproducibility calculated for each session was 0.12–0.27 eNd (2σ) units based on the repeated measurements of JNdi-1. If the internal error (2σ) is larger than the external error, the internal error is reported as the final uncertainty associated with the individual measurements. Several procedural blanks were also processed along with the samples and ascertained an average blank of ~70 pg for the samples (n=9), which is several orders of magnitude lower than the total Nd typically analysed in samples. Hence, no blank correction was applied. Replicates have an average eNd variation of ±0.17 (n= 16). Over the course of analyses, measurements of rock standard BCR-2 and BHVO-2 processed with the samples gave 143Nd/144Nd = 0.512641 ± 0.000010 (2s, n = 7) and 143Nd/144Nd = 0.513008 ± 0.000012 (2s, n = 7), in excellent agreement with reported values14.
Pb isotope analysis
Pb isotope was analysed in the same aliquot in which Nd isotope was measured. The Pb cuts in the detrital dissolved were purified by column chromatography filled with ∼80 μL AG1-X8 resin. Pb isotopes were measured using a Thermo Scientific Neptune Plus MC-ICP-MS at GEOMAR Helmholtz Centre for Ocean Research Kiel. Mass bias correction during Pb isotope measurements was performed externally using the Tl-doping technique9,15 with added NIST997 Tl standard solution and a Pb/Tl ratio of ~4. The total procedure blanks were ~500 pg which represents less than 0.1% of the sample signal. Blank corrected and uncorrected ratios do not show significant difference and hence blank uncorrected data is reported in this study. The reproducibility of the rock standard BCR-2 and BHVO-2 is listed in Supplementary Table 2. As shown in the table, all measured standard Pb isotopic ratios are within the error of published compositions. Detailed information about the measurement procedure can be found in Süfke et al. (2019)15 and Huang et al. (2021)9.
Robustness of the detrital sediment Nd and Pb isotope records
Unlike other radiogenic isotope systems (for example, Sr and Hf), Nd isotopes are relatively insensitive to grain size variations16, making them a robust indicator of sediment provenance. Their insensitivity to grain size variations makes them more reliable tracers of sediment provenance. However, it is crucial to consider potential complications in provenance interpretations if changes in sediment transport processes result in changing the isotope compositions. In such cases, a link between grain size and Nd isotopes could emerge, impacting the reliability of using these isotopes for provenance analysis. To assess the robustness of Nd isotopes, Pereira P.S. (2018)17 analysed Nd isotopes in fine-grained fraction (<63 μm) of sediment cores from two locations (PS58/254 and PC493) near our core site U1532 (Fig. 1b). The results of this investigation ruled out any significant influence of grain-size variations on the Nd isotope compositions, reinforcing the suitability of Nd isotopes as a dependable proxy for sediment provenance in this particular study area. Among various combinations of Pb isotope ratios, we have used 208Pb/204Pb and 208Pb/207Pb ratios as these displayed the most distinctive, clearest and smoothest signal compared to other ratios and both these ratios co-vary in concert with the eNd record. Observation of changes in the paired Nd-Pb isotope records is more robust to decipher the changes in the sediment provenances than either of the two trace metal isotope compositions alone. This finding further validates the robustness of using these isotopes as tracers of sediment sources and transport processes in the specific study region. In summary, the distinct insensitivity of Nd to grain size fractionation makes them reliable tools for tracing sediment provenance. Pertinent to this, it is important to mention that Pliocene erosional history and ice loss from the East Antarctic Ice Sheet (EAIS) were successfully reconstructed previously using detrital eNd records from the Adélie Land sector of East Antarctica7,18. Distinct sediment sourcing associated with the growth and retreat of the ice sheet margin and multiple collapse events clearly establish a close link between ice sheet dynamics, erosion and variable regional sediment supply. Therefore, our extensive analysis in the present study and successful demonstration in the previous study from this region provides confidence in the applicability of detrital radiogenic isotope compositions of Nd and Pb provide confidence for deciphering sediment sources and transport processes in the studied area.
Wavelet and scaled-average variance of wavelet power analysis
Wavelet transforms decompose time series into time-frequency space and can therefore find localized intermittent periodicities. We used Continuous Wavelet Transform (CWT) i.e. Morlet wavelet to decompose the time series into time-frequency space which enable us to identify the modes of variability and how those modes vary with time19. Statistical significance is estimated against a red noise model. Monte Carlo methods were used to assess the statistical significance against red noise backgrounds20. Wavelet analysis of the temperature record was performed using online Matlab codes http://grinsted.github.io/wavelet-coherence/ to identify nonstationary power at certain frequency bands19,20. Temperature variability at ~40 ka and ~100 ka bands is shown in the wavelet analysis. More detailed information on wavelet analysis is provided elsewhere19,20. Further, to examine fluctuations in power over a range of scales (a band), we used scale-averaged wavelet power which is a time series of the average variance in a certain band. This can be used to examine modulation of one time series by another, or modulation of one frequency by another within the same time series. We have performed this analysis using online Matlab codes http://paos.colorado.edu/research/wavelets/. The scaled average variance of the temperature at 32-64 ka and 64 -100 ka band captured the wavelet analysis show how the ~40 ka and ~100 ka periodities evolved with time (Extended Data Fig. 7).
Change-Point Detection using a Bayesian Ensemble Algorithm (BEAST)
Abrupt changes in the temperature time series were detected using a MATLAB based Bayesian model averaging time-series decomposition algorithm (BEAST)21 (Extended Data Fig. 8). This algorithm offers robust method to detect abrupt change points and nonlinear trend in the Antarctic temperature record. The code and software are available at https://github.com/zhaokg/Rbeast. The Bayesian algorithm—BEAS decomposition time series into three contrasting components: abrupt change, periodic/seasonal change, and trend. Mathematically, BEAST is rigorously formulated, with its key equations being analytically tractable. Practically, BEAST provide estimate of probabilities of change point occurrence and detect both large and low-magnitude disturbances, and uncover complex nonlinear trend dynamics. The details of the Bayesian Ensemble Algorithm (BEAST) are discussed elsewhere21.
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