Magnetic Stratigraphy of the Danube Loess a Composite Titel-Stari

Journal of Asian Earth Sciences 155 (2018) 68–80

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Journal of Asian Earth Sciences

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Full length article Magnetic stratigraphy of the Danube loess: A composite Titel-Stari T Slankamen loess section over the last one million years in Vojvodina, Serbia ⁎ Yang Songa,b, Zhengtang Guoa,c,d, , Slobodan Markoviće,f, Ulrich Hambachg,f, Chenglong Dengh,c, Lin Changa,i, Jianyu Wua, Qingzhen Haoa,c a Key Laboratory of Cenozoic Geology and Environment, Institute of Geology and Geophysics, Chinese Academy of Sciences, Beijing 100029, China b State Key Laboratory of Urban and Regional Ecology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China c University of the Chinese Academy of Sciences, Beijing 100049, China d CAS Center for Excellence in Tibetan Plateau Earth Sciences, Beijing 100101, China e Physical Geography, Faculty of Sciences, University of Novi Sad, Trg Dositeja Obradovića 3, Novi Sad 21000, Serbia f Laboratory for Palaeoenvironmental Reconstruction, Faculty of Sciences, University of Novi Sad, Trg Dositeja Obradovića 3, Novi Sad 21000, Serbia g BayCEER & Chair of Geomorphology, University of Bayreuth, Bayreuth 95440, Germany h State Key Laboratory of Lithospheric Evolution, Institute of Geology and Geophysics, Chinese Academy of Sciences, Beijing 100029, China i Department of Physics, Tsinghua University, Beijing 100084, China

ARTICLE INFO ABSTRACT

Keywords: In Europe, the most complete loess-paleosol sequences over the past million years are preserved in the Serbian Magnetostratigraphy part of the Danube River drainage basin. The similarity in stratigraphy and climatic cycles between the Serbian Serbian loess and the Chinese loess sequences suggests that the loess deposits in these two regions could play an important role Danube loess in the study of intercontinental climatic correlations and linkage. However, previous magnetostratigraphic Chinese loess studies of the Serbian loess, mainly conducted using the alternating field (AF) demagnetization approach, show Intercontinental correlations significant differences with the Chinese loess, especially the stratigraphic positioning of the Matuyama-Brunhes boundary (MBB). Here, we conduct a detailed magnetostratigraphic investigation of a composite Titel-Stari Slankamen loess section in the Vojvodina (northern Serbia), using thermal and hybrid demagnetization methods, aiming to establish new chronological constraints for the Danube Basin loess. Based on the analyses of the mineral magnetic properties, anisotropy of magnetic susceptibility, progressive thermal and hybrid demagnetization, the MBB was determined within S8, broadly consistent with the MBB position seen in the Chinese loess. Present evidence supports the hypothesis that the overall normal polarity in the upper part of L9, with a thickness of 2.1 m, was possibly caused by a combination of the remagnetization of remanence-carrying coarse- grained magnetite during the Brunhes normal chron and bioturbation during the forming of the overlying paleosol S8. Thus, our magnetostratigraphic results provide solid chronological evidence for the coherence of pedostratigraphy and climatostratigraphy for the loess deposits in the Danube Basin and China. The synchronous occurrence of the strongest developed paleosol S5 (corresponding to MISs 15–13) and the least weathered thick loess unit L9 (corresponding to MISs 24–22) in the two regions confirms that extreme climatic events during these two intervals are possibly common features of the climate in the Northern Hemisphere at those times.

1. Introduction reconstruction of the loess, etc.(Smalley et al., 2001; Marković et al., 2016). Up until now, the chronology (e.g., Singhvi et al., 1987; Butrym Thick loess deposits on the Eurasian continent, mainly distributed in et al., 1991; Oches and McCoy, 1995; Fuchs et al., 2008; Novothny northern China, central Asia and Europe, have long been intensively et al., 2009; Stevens et al., 2011; Timar-Gabor et al., 2011; Timar-Gabor investigated as important terrestrial Quaternary paleoclimate archives and Wintle, 2013; Murray et al., 2014; Újvári et al., 2014a), sedi- (Kukla, 1975; Liu, 1985; Dodonov, 1991). European loess research mentology (e.g., Kukla, 1975, 1977; Fink and Kukla, 1977; Pécsi et al., started in the late 17th century in the Danube River drainage basin, and 1995; Koloszár and Marsi, 2005; Vandenberghe et al., 2014; Zeeden has made great contributions to developments in the scientiﬁc study of et al., 2016), paleopedology (e.g., Bronger, 2003), environmental loess, including the concept, origin, formation and paleoclimatic magnetism (e.g., Heller and Evans, 1995; Forster et al., 1996; Heller

⁎ Corresponding author at: Key Laboratory of Cenozoic Geology and Environment, Institute of Geology and Geophysics, Chinese Academy of Sciences, Beijing 100029, China. E-mail address: [email protected] (Z. Guo). https://doi.org/10.1016/j.jseaes.2017.11.012 Received 14 September 2017; Received in revised form 5 November 2017; Accepted 5 November 2017 Available online 07 November 2017 1367-9120/ © 2017 Elsevier Ltd. All rights reserved. Y. Song et al. Journal of Asian Earth Sciences 155 (2018) 68–80 et al., 1996; Sartori et al., 1999; Evans and Heller, 2001), paleontology demagnetization fails to remove the VRM and isolate the characteristic (e.g., Ronai, 1970; Moine et al., 2002; Sümegi and Krolopp, 2002; remanent magnetization (ChRM) in some cases. Additionally, there are Marković et al., 2004, 2006, 2007; Sümegi et al., 2011) and geo- abundant root channel deposits in the upper layer of L9, arising from chemistry (Újvári et al., 2008, 2014b; Buggle et al., 2011, 2013; Hatté the vegetation growth which occurred during formation of the S8 et al., 2013) of the loess-paleosol sequences in Europe have been in- overlying soil. Some previous sampling has not successfully avoided vestigated. These studies have provided plentiful information about these secondary deposits. Thermal demagnetization and careful sam- regional and local climatic changes during the Quaternary. To date, the pling of the primary loess deposits in the upper part of L9 is therefore high-resolution multi-proxy environmental records for Europe have highly necessary to confirm the magnetostratigraphy of Serbian loess been mainly limited to the most recent climatic cycles (Antoine et al., over the past 1 Ma. 2001, 2009; Frechen et al., 2003; Moine et al., 2017). The long se- In this study, based on rock magnetic analyses and anisotropy of quence of climatic changes spanning several glacial-interglacial cycles magnetic susceptibility (AMS) properties, we employed thermal de- is principally available only within high-resolution environmental magnetization techniques, in combination with hybrid demagnetization magnetism parameters (Forster et al., 1996; Panaiotu et al., 2001; methods, to identify accurately the stratigraphic location of the MBB Marković et al., 2006, 2009a, 2011; Jordanova et al., 2007, 2008; within our composite Titel-Stari Slankamen loess section, the most Buggle et al., 2009). Knowledge of the older interglacials is therefore complete loess-paleosol sequence since the Middle Pleistocene found in crucial for a better understanding of the complex consequences of past Serbia, and even in Europe. Within this context, we first present high- global warming and the mechanisms driving this (Bronger, 2003; Guo resolution magnetic susceptibility variations derived from the entire et al., 2009, 2012; Hao et al., 2012b, 2015; Berger et al., 2016). composite Titel-Stari Slankamen section, then refine its stratigraphic The thick loess-paleosol sequences widespread in the middle and correlation scheme using the Chinese loess record for the lower parts of lower reaches of the Danube River drainage basin constitute the largest the section. Second, we present a detailed rock-magnetic analysis of and most significant European loess region west of the Russian Plain representative samples, in addition to AMS and paleomagnetic results, (Fink and Kukla, 1977; Smalley and Leach, 1978; Haase et al., 2007; for this section. The main aim of this study was to establish a reliable Fitzsimmons et al., 2012; Marković et al., 2012b). These deposits are magnetic polarity sequence for the Serbian loess based on thermal and valuable because well-preserved and continuous terrestrial climatic hybrid demagnetization methods, in order to provide chronological records covering a long time span are very scarce in central and constraints for the past 1 Ma of Serbian loess and allow a potential southeastern Europe (Pécsi and Schweitzer, 1993; Forster et al., 1996; correlation with Chinese loess-paleosol sequences. The extreme climatic Jordanova and Petersen, 1999a, 1999b; Tzedakis et al., 2006; Marković events recorded by these loess deposits were also addressed as part of et al., 2009a, 2011; Radan, 2012). According to previous stratigraphic our study. correlations and paleoclimatic investigations, the most complete loess- paleosol sequences in the Danube basin extending back the last one 2. Materials and methods million years (Ma) are to be found in Serbia (Marković et al., 2011, 2012b, 2015). The close correlation between Serbian loess, Chinese 2.1. Geological setting and sampling loess and the deep-sea oxygen isotopic stratigraphic record would indicate that this Serbian loess possesses great potential when mapping Thick loess deposits are widely distributed in the Vojvodina region, intercontinental climatic correlations, and their linkage with global northern Serbia, in the southernmost part of the Middle Danube Basin paleoclimatic change. (Fig. 1). Typical loess-paleosol sequences in this region are preserved as Previous chronological and paleoclimatic studies of Serbian loess mantle-like loess plateaus with a maximum thickness of ∼55 m. The have provided a solid basis for establishing a stratigraphy, investigating two most famous plateaus are the Srem and Titel loess plateaus. The any climatic correlations, and reconstructing paleoclimates (Fuchs nomenclature of loess and paleosol units in the Vojvodina region fol- et al., 2008; Marković et al., 2011; Stevens et al., 2011). Of the lows that used for Chinese loess stratigraphy (Liu, 1985; Kukla and An, chronological approaches, magnetostratigraphic studies provide the 1989), which designates loess/paleosol layers as “L”/“S”, and numbers key absolute time control for thick loess deposits. The Matuyama- these layers in order of increasing age (Marković et al., 2008, 2009b, Brunhes boundary (MBB), the last change in the Earth’s magnetic field 2011). up to the present-day direction, and dated at ∼781 ka, is one of the Our composite Titel-Stari Slankamen loess section was sampled in most frequently used time markers in Quaternary stratigraphy. Early 2013 and 2014. This composite section consists of four outcrops: the magnetostratigraphic research was conducted on the classical Stari upper three, i.e., the Mošorin Veliki Surduk (MVS), Feduvar and Slankamen loess section over various sampling intervals using the al- Dukatar sections, from the Titel Loess Plateau; and the lower one, the ternation field (AF) demagnetization approach (Marković et al., 2003, Stari Slankamen section, from the Srem Loess Plateau (Fig. 1). These 2011; Hambach et al., 2009). The most recent AF demagnetization four outcrops are typical of Serbian loess sections, as confirmed by study of the lower ∼11 m of this loess section shows that the MBB is numerous previous investigations (Bokhorst et al., 2009; Marković located in layer L9, corresponding to unit L9 of the Chinese loess-pa- et al., 2011). The conjunction of the composite loess section follows the leosol sequence (and also corresponding to Marine Oxygen Isotope scheme of Marković et al. (2015). Stage (MIS) 22) (Marković et al., 2011). This is different from the MBB The MVS section (45.296°N, 20.188°E), Feduvar section (45.287°N, within L8 or the boundary between L8 and the underlying S8 unit in 20.230°E) and Dukatar section (45.267°N, 20.246°E) are located in most of the loess sections from China and central Asia (Heller and Liu, three adjacent outcrops near the terraces of the Tisa River on the 1982; Liu et al., 1988a; Zhou and Shackleton, 1999; Spassov et al., northwestern margin of the Titel Loess Plateau, where the thickest loess 2001; Pan et al., 2002; Wang et al., 2005, 2006; Wu et al., 2005; Jin and sedimentary deposits found in the whole Danube Basin are located. This Liu, 2010; Yang et al., 2010; Liu and Zhang, 2013). The short normal loess contains at least five major loess-paleosol cycles. The Stari polarity within the Basal Complex, which has been interpreted as the Slankamen section (45.132°N, 20.264°E) is situated on the northeastern upper boundary of the Jaramillo normal subchron, is also different from margins of the Srem Loess Plateau (Fig. 1), ∼38 km northeast of the that seen in the Chinese loess record. These discrepancies have caused Serbian capital, Belgrade. The loess profile is exposed on its western serious confusion when attempting to make stratigraphic correlations cliff at the confluence of the Danube and Tisa rivers, and exhibits a total between the loess deposits of Serbia and China. It is well known that the thickness of ∼40 m. At least 10 loess-paleosol couplets have been AF demagnetization is not valid for high-coercivity magnetic carriers. identified (Marković-Marjanović, 1972; Bronger, 1976, 2003; Marković As a secondary viscous remanent magnetization (VRM) can also be et al., 2011). An erosion layer (labeled as EL) marked by gravel frag- carried by high-coercivity minerals, it is possible that AF ments with sizes up to ∼5–10 cm in diameter is located in the lower

69 Y. Song et al. Journal of Asian Earth Sciences 155 (2018) 68–80

Fig. 1. Schematic map for the location of the Titel-Stari Slankamen section, Serbia. part of the loess layer below paleosol S1 (see Fig. 3 from Marković et al., paramagnetic contribution. Isothermal remanent magnetizations 2011). (IRMs) were imparted from 0 to 2.2 T, also using the MicroMag series Bulk samples were extracted at 5 cm intervals for each of the four 3900 VSM. Subsequently, the saturation isothermal remanent magne- outcrops. The boundaries between the loess and paleosol layers were tization (SIRM) acquired at the maximum ﬁeld of 2.2 T was demagne- selected to conjoin the composite Titel-Stari Slankamen section (Fig. 2). tized in a stepwise direct current (DC) backﬁeld to obtain the coercivity

This conjunction was compiled using field observations, then verified of remanence (Bcr). using correlations in the changes in magnetic susceptibility measured around the conjunction (Fig. 2). A total of 112 oriented block samples were taken for magnetostratigraphic study, of which 49 samples were 2.2.3. Measurement of anisotropy of magnetic susceptibility (AMS) taken at ∼1 m interval for the upper part of the section, i.e., from the S0 AMS of all oriented cubic specimens belonging to Set A was mea- to upper S7 layers (from 0 to 49.2 m in depth), and 66 samples were sured using a KLY-3s Kappabridge unit before demagnetization to extracted at 10 cm intervals for the lower part of the section, i.e., from characterize the sedimentary fabric. Each cubic specimen was rotated the middle of layer S7 down to the Basal Complex (from 49.2 m to through three orthogonal planes. The susceptibility ellipsoid was cal- 55.9 m in depth). The aim in doing this was to identify exactly the culated using the least-squares method, and the anisotropic parameters polarity of the lower part of the section, including the positioning of the of lineation (L), foliation (F), degree of anisotropy (P) and shape factor MBB. During sampling, we carefully avoided the tree root-shaped bio- (T)(Jelinek, 1981) were obtained with Anisoft software using the sta- turbations found in layer L8 and the upper part of layer L9. All of the tistical method proposed by Constable and Tauxe (1990). oriented samples were sawn into 2 × 2 × 2 cm3 cubes, and at least two parallel sets (named Set A and Set B) were prepared. 2.2.4. Paleomagnetic measurements Oriented specimens were exposed in a magnetically-shielded room 2.2. Methods for at least one week before demagnetization and remanence measuring in order to reduce the viscous magnetization caused by the modern 2.2.1. Magnetic susceptibility measurement magnetic field. A total of 155 samples were subjected to thermal and/or Magnetic susceptibility was measured using a Bartington MS2 meter hybrid demagnetization. Firstly, all 112 samples in the Set A specimens and a MS 2B sensor at the dual frequencies of 470 Hz (χlf) and 4700 Hz were subjected to 16 steps of thermal demagnetization from 100 °C to (χhf), in 5 cm intervals. Samples were air-dried at room temperature 685 °C at temperature intervals of 10–50 °C, using a Magnetic Thermal and gently crushed before measurement. The differences between the Demagnetizer with a residual field set at < 10 nT. Remanences were two susceptibilities rendered the frequency-dependent magnetic sus- measured using a three-axis cryogenic magnetometer (2G Enterprises ceptibility as a mass-specific term (χfd). Model 760-R) installed in a magnetically-shielded space (< 300 nT). Secondly, for the samples which failed to isolate the ChRM, their 2.2.2. Rock magnetic experiments counterparts in Set B were subjected to hybrid demagnetization. This Various rock magnetic experiments were conducted to determine procedure involves stepwise thermal demagnetization, firstly up to the magnetic mineralogy of a total of 19 representative samples from 150 °C, then a stepwise AF demagnetization from 5 to 60 mT at each loess and paleosol layer of our composite Titel-Stari Slankamen 2.5–5 mT intervals. An additional six samples which isolated the ChRM loess section. by thermal demagnetization were also subjected to the hybrid de- – Temperature-dependent saturation magnetization (Ms T) curves magnetization process for cross-checking. The natural remanent mag- were measured using a variable field translation balance system netizations (NRMs) at room temperature were measured for all the (VFTB). The samples were heated in air from room temperature (25 °C) studied samples. The principal components’ directions of ChRM were to 700 °C, and back to ∼55 °C, using an applied field of 1 T. The heating calculated using least-squares fits (Kirschvink, 1980) using at least five and cooling rate was 40 °C/min. continuous steps from above 250 °C, or after 15 mT, with a maximum Hysteresis loop measurements were performed using a MicroMag angular deviation (MAD) < 15°. 3900 series vibrating sample magnetometer (VSM) with a maximum

ﬁeld of 1 T. Saturation magnetization (Ms), saturation remanence (Mrs) and coercivity (Bc) were determined after a correction for any potential

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Fig. 2. Lithostratigraphy of the Titel-Stari Slankamen section.

3. Results kg, respectively. The exceptions are two χlf spikes for the tephra layers in L2 and L5. The tephra layer in L4 (Marković et al., 2012a) is not

3.1. Magnetic susceptibility clearly identified in our χlf curve. The χlf and χfd values are linearly correlated with a high correlation coefficient (not shown), suggesting The variations in the low-frequency and frequency-dependent that the dominant contribution to the variations in magnetic suscept- magnetic susceptibility (χlf and χfd) values for the composite section are ibility are made by neo-formed pedogenic ultra-fine magnetic grains. S7 shown in Fig. 3. The changes are highly consistent with the alternation and S8 are significantly magnetically enhanced relative to S6, due to between loess and paleosol units, with enhanced values in paleosols, strong pedogenesis. The interstadial soil layers in L7 and L9 can be and generally reduced values in loess units. The χlf and χfd values range clearly defined in the magnetic susceptibility curves. − − from 10.84 to 142.72 × 10 8 m3/kg, and −0.50 to 15.54 × 10 8 m3/

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Fig. 3. Magnetic susceptibilities (low-frequency χlf and

frequency-dependent χfd) of the Titel-Stari Slankamen section of Serbia (left) and its correlation with the Luochuan section of China (right).

3.2. Rock magnetic results cooling curves are higher for paleosol samples than for loess samples.

3.2.1. Ms-T results 3.2.2. Hysteresis properties The magnetization versus temperature curve is widely employed to determine the Curie temperature of natural samples. The heating curves We also employed hysteresis loops and IRM acquisition curves to assess magnetic mineralogy. The magnetic parameters of selected of magnetization for all our samples gradually drop along a slightly concave downwards curve before ∼600 °C (Fig. 4a). The concavity is samples are shown in Fig. 4b and Table 1. All the samples display a high paramagnetic contribution. After the removal of the paramagnetic clear at 150 °C for most samples, except for the cases of S7, S8 and the component, the samples from loess and paleosol layers show different Basal Complex (Fig. 4a). There are clear indications at ∼585 °C, the Tc of magnetite for all samples, indicating the predominance of magnetite. behaviors, as shown in Fig. 4b. The hysteresis loops of all samples are Magnetization after the cooling run is always reduced with the onset of closed above 200 mT, indicating the uniform dominance of soft mag- ‘ ’ heating, indicating that the conversion of maghemite to hematite may netic components. Wasp-waisted loops are more marked and more have occurred (e.g., Spassov et al., 2003). The most significant differ- frequent in loess samples (e.g., L6), and the loops of loess units are closed at higher fields than for the paleosol samples, suggesting an in- ence between loess and paleosol couplets is that the Ms values of crease in the contribution of hematite to the total remanence as

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Fig. 4. Magnetic properties of representative loess (dashed lines) and paleosol (solid lines) samples of the Titel-Stari Slankamen section, (a) Ms-T, (b) hysteresis loops and (c) IRM −3 2 Acquisition. (The units for Ms and Mrs:10 Am /kg; Bc and Bcr: mT).

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Table 1 3.4. Paleomagnetic results The hysteresis parameters of representative samples of Titel-Stari Slankamen section. Representative demagnetization diagrams are shown in Fig. 6. Layers Sample ID M M B B B /B M /M s rs c cr cr c rs s Secondary viscous magnetization parallel to the present-day field, or − (10 3 Am2/kg) (mT) acquired during storage, was removed by heating samples to 250 °C. The ChRM components for most samples separated between ∼250 °C S0 MVS2A-0.15m 28.74 3.77 8.74 26.12 2.99 0.13 and ∼550 °C (Fig. 6), indicating that magnetite is the main magnetic L1 MVS2E-28 20.27 2.06 10.06 34.95 3.47 0.1 S1 TM-43 49.26 7.47 6.91 20.57 2.98 0.15 remanence carrier. The high temperature remnant components above L2 TM-70 14.88 2.3 11.84 31.13 2.63 0.15 585 °C are usually highly scattered, while some also retain a relatively S2 MVS2-24 48.7 7.04 7.24 22.32 3.08 0.14 stable direction even up to 620 °C or higher (e.g., Fig. 6a, b and g). L3 MVS1-14 22.32 3.07 12.83 42.59 3.32 0.14 These stable high temperature components decay with increasing S3 TPF-30 59.84 8.51 7.18 22.78 3.17 0.14 temperature toward the origin along nearly the same trajectory as the L4 TPF-70 17.41 2.51 13.96 46.61 3.34 0.14 ∼ – S4 TPF-114 31.3 4.6 7.56 23.91 3.16 0.15 medium temperature components ( 300 585 °C), but exhibit slightly L5 14DK-35 9.66 1.32 13.64 58.49 4.29 0.14 shallow inclinations in some cases (e.g., Fig. 6c, d and f), indicating that S5 14DK-144 58.81 9.03 7.2 22.21 3.08 0.15 hematite also is the ChRM carrier in these samples. The remanent L6 SS6-42 15.41 2.83 13.6 48.42 3.56 0.18 magnetization of some samples (e.g., those shown in Fig. 6c and d), was S6 SS6-14 41.19 5.98 8.26 28.14 3.41 0.15 L7 SS4-33 23.23 3.76 10.66 35.03 3.29 0.16 not stable above 300 °C, but it is clear that the remanent magnetization S7 SS3A-6 56.81 8.44 7.04 24.38 3.46 0.15 of each sample between 300 °C and 550 °C, or a higher temperature, L8 SS3A-10 34.98 5.11 7.58 25.94 3.42 0.15 shows a predominance of normal polarity. S8 SS3A-18 65.16 9.43 6.74 21.93 3.25 0.14 In view of the high failure rate of the thermal method for the bottom L9 SS3A-36 19.51 3.38 11.72 43.24 3.69 0.17 part of the studied section, we used hybrid demagnetization with the BASAL SS2A-56 38.22 5.68 7.37 25.19 3.42 0.15 parallel specimens which failed to isolate the ChRM. This hybrid demagnetization method, by which samples were subjected thermal de- reported by Hao et al. (2012a). Although the values of Mrs/Ms versus magnetization to 150 °C before AF demagnetization in this case, were Bcr/Bc for loess and paleosol samples fall within the PSD range in a Day designed to wipe out the remanence carried by minerals with high diagram (not shown) (Day et al., 1977), these parameters fail to show coercivity but low unblocking temperature, such as goethite. the difference in the magnetic grain size for minerals of pedogenic and Trajectories toward the origin were defined during AF demagnetization detrital origins in loess deposits, as shown in Hao et al. (2012a). to peak fields in the 15 to 45–60 mT interval (e.g., Fig. 6e and h). For All samples show that the rapid increase in IRM values to 90% at the interval below a depth of 52.7 m, a reversed polarity can be clearly ∼150 mT become saturated above 600 mT, indicating that soft mag- observed for samples from L9LL2 (Fig. 6 g and h), confirming the late netic components are dominant (Fig. 4c). The Bcr values determined by Matuyama Chron of this interval. However, for samples from the lowest the SIRM demagnetization curves are higher in loess than in paleosols, part of the Basal Complex below 55.0 m, the remanent components are which are averaged as 40.1 mT and 23.8 mT, respectively. These ob- highly scattered after 15–20 mT, inadequate for reliably defining ChRM servations are consistent with the magnetic characteristics highlighted values (Fig. 6i and j). In the 50.5–52.5 m interval, 5–25% of the NRM by hysteresis loops. was left when the samples from this layer were heated to 300 °C. From In summary, these systematic rock magnetic measurements suggest 200 °C to 300 °C, the remanent direction was unstable, although a that the Titel-Stari Slankamen section contains a primarily soft mag- predominantly normal polarity in these samples can be observed netic mineral assemblage, mainly magnetite and/or maghemite. (Fig. 7). Similar unstable remanence values can be observed on the progressive AF demagnetization curve above the 20–25 mT peak (Fig. 7). 3.3. AMS results In the upper section above a depth of 50.4 m, 56 of the 58 samples carry a ChRM component. Below a 50.4 m depth, a MAD < 20° was AMS has been widely used in loess studies to detect any possible used to interpret the ChRM component. Using thermal demagnetiza- disturbance of the original sedimentary fabric (e.g., Liu et al., 1988b; tion, 18 of the 55 samples carry a ChRM component, while using the Zhu et al., 1999; Guo et al., 2001, 2002). Changes in AMS parameters hybrid approach, 29 of the 43 samples carry a ChRM component. along the depth are shown in Fig. 5. The Magnetic Lineation (L) and the The Virtual Geomagnetic Pole (VGP) latitudes were calculated using Magnetic Foliation (F) vary between 1 and 1.006, and 1.001 and 1.022, the ChRM vectors to define the magnetostratigraphy of the composite respectively. The Degree of Anisotropy (Pj) varies between 1.003 and section (Fig. 8). Above 50.4 m is exclusively normal polarity, corre- 1.027. The susceptibility ellipsoid (T) is mostly oblate shaped (T > 0). sponding to the Brunhes Chron. In the interval between 50.5 m and For the upper 50.4 m, in an L-F diagram (not shown), the samples lie 52.6 m, the middle temperature components are less stable, and some close to the foliation axis, i.e., in the oblate area. The inclinations of the parallel samples yield contrasting results. The polarity of this part is not fi maximum susceptibility axis (K1_Inc) and minimum susceptibility axis clear. Thus the MBB was de ned as being at 50.4 m. From 52.7 m to fi (K3_Inc) have been widely used to detect possible disturbances of the 55.0 m, a distinct reverse polarity has been identi ed with 2.4 m in original sedimentary fabric. In the Titel-Stari Slankamen section, K1_Inc thickness, corresponding to the late Matuyama Chron. At the lowest – values have an average of 11.89°, with 81% of samples < 15°. K3_Inc part of the 55.0 55.9 m interval, the reliable polarity can once again values are 72.30° on average, with 81% > 70° (Fig. 5). These AMS not be defined. features are typical of loess-paleosol sequences and indicate a primary Our magnetostratigraphic data obviously differ from those collated sedimentary fabric without apparent deformation or disturbance during previous investigations (Marković et al., 2003, 2011; Hambach throughout most of the section. However, for the lower part of the et al., 2009). The short normal intervals identified by Hambach et al. section below 50.4 m, the two intervals at depths of 50.4–51.0 m and (2009) and Marković et al. (2011), one with a thickness of ∼0.5 m in ∼ 55.1–55.9 m are characterized by low values of F, Pj, and T, an in- L9SS1, and the other with a thickness of 1.0 m in the lowest part of fi clination in K3 values, and a high value of inclination in K1 values. the Basal Complex, were not con rmed by our results. The latter one These features suggest that these two intervals have potentially been has been thought to be the upper boundary of the Jaramillo subchron disturbed by post-depositional processes, such as deformation or dis- (Marković et al., 2011). Thus, our results reveal a lower reverse polarity turbance. and upper normal polarity for the section, which can be correlated with the geomagnetic timescale since the late Matuyama Chron (Fig. 8).

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Fig. 5. AMS properties of the Titel-Stari Slankamen section.

Fig. 6. Orthogonal projections of the progressive demagnetization of representative samples of Titel-Stari Slankamen section. The solid (open) circles represent the horizontal (vertical) planes. NRM is the natural remanent magnetization.

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Fig. 7. Orthogonal projections of the progressive demagnetization of representative samples in 50.3–52.5 m interval. Upper (lower) ones are projections with thermal (hybrid) demagnetization.

4. Discussion the interglacial and interstadial periods in establishing the pedostratigraphy for loess-paleosol sequences in order to attain a more accurate 4.1. Lithostratigraphy of the Serbian loess and its correlation with the stratigraphic correlation, and thus climatic interpretation. Chinese loess In the early stages of Chinese loess research, the upper part of sequences representing the last 1.2 Ma was numbered from S0 (top) to The pedostratigraphy of the loess-paleosol sequences provides a S14 (bottom) for the soil units, and from L1 (top) to L15 (bottom) for basis for establishing the stratigraphic framework and climatic inter- the loess units (e.g., Liu, 1985). During their study of the loess-paleosol pretation of sections. Paleosols with different morphologies and ap- sequences on the southern CLP, Ding et al. (1993) proposed that only pearances form within the loess-paleosol sequences as a response to paleosols which had undergone pedogenic processes similar to, or changes in the climate (e.g., Liu, 1985; Ding et al., 1993; Guo et al., stronger than, the zonal Holocene soil could be identified as an in- 1996; Kemp, 2001). When establishing a regional pedostratigraphy for dependent pedostratigraphic unit. Using this criterion, the Early Pleis- the loess-paleosol sequence, it is necessary to compare the buried soil tocene part of the loess-paleosol sequence below the S14 layer was genetically and typologically with the Holocene soil of the same region divided into 18 paleosol units (i.e., S15–S32). Guo et al. (1996) further (Kemp, 2001). In most regions, it seems that the balance swings to- explored the polygenetic properties of the paleosols of the Chinese wards pedogenesis during interglacials or interstadials when the cli- loess-paleosol sequences, and identified 56 soil-forming stages in total mate is warmer and/or wetter (Kemp, 2001). In both the central and throughout the Quaternary period. southern Chinese Loess Plateau (CLP), and Serbia, interstadial soil can The establishment of the pedostratigraphy of Serbian loess has a be clearly identified in several loess layers. It is necessary to distinguish long history, as summarized by Marković et al. (2011, 2015, 2016).

Fig. 8. Lithostratigraphy and magnetic stratigraphy of (A) the Titel-Stari Slankamen section and (B) the MBB reversal.

76 Y. Song et al. Journal of Asian Earth Sciences 155 (2018) 68–80

There have been a number of stratigraphic models developed for the Liu et al., 2005), and indicate a primary eolian magnetic fabric without Serbian loess, with different nomenclature and numbers of fossil soils significant disturbance which could potentially yield a reliable ChRM. (Marković-Marjanović, 1972; Bronger, 1976; Butrym et al., 1991; For the lower part of the section, AMS measurements show that the Marković et al., 2003). Marković et al. (2003) designated the loess- three intervals of 49.6–49.8 m, 50.5–50.9 m and 55.1–55.9 m have paleosol units in northern Serbia using the nomenclature of the Chinese lower T, Pj and F values than the neighboring parts of the section. In loess stratigraphic system (e.g., Liu, 1985; Kukla and An, 1989), but these intervals, the T values decrease, indicating the AMS ellipsoid inserting the prefix “SL”, referring to the Stari Slankamen-type section. changes toward a prolate shape. Both the degree of anisotropy Pj and After the discovery that the Stari Slankamen section is not complete in the magnetic foliation F also significantly decrease. As for the inclina- its upper part, Marković et al. (2008) proposed the use of the prefix “V”, tions of the principal axes, samples in the 55.1–55.9 m exhibit a sig- referring to the regional stratigraphic model for Vojvodina Province. nificantly large K1_Inc value (averaging ∼ 54.11°), and a small K3_Inc Finally, Marković et al. (2015) identified a uniform stratigraphy for value (averaging ∼ 14.26°), indicating that the susceptibility ellipsoids Danube loess-paleosol sequences completely the same as Chinese loess are most likely skewed toward the horizontal plane. In 49.6–49.8 m and stratigraphy (e.g., Liu, 1985; Kukla and An, 1989). 50.5–50.9 m intervals, several samples exhibit an increase in the in-

Our new investigation confirms the accuracy of the previous cor- clination of K1, and a reduction in the inclination of K3. All these lines relation between Serbian and Chinese loess-paleosol sequences above of evidence would indicate that these three intervals may have ex- the S8 layer. The loess layers from L6 to L1 in the Titel-Stari Slankamen perienced some kinds of disturbance. The Stari Slankamen section sits section are all characterized by thick loess deposits of up to 10 m; these on the terraces of the Danube River, and the Basal Complex is near the are gray-brown and weakly weathered. The stratigraphic structure is conjunction between the eolian deposits and the fluvial deposits typical quite similar to that of Chinese loess. These features conform to the of these terraces. The difference in mechanical properties may have led dominant quasi-100 ka cycles observed in the global climate over the to the disturbance in the deformation posterior to loess formation. As last 700 ka, during which each glacial MIS stage usually spans two for the 49.6–49.8 m and 50.5–50.9 m intervals, the disturbance may precessional cycles (e.g., Lisiecki and Raymo, 2005). have been arisen from bioactivity during the development of overlying The pedostratigraphy between L6 and L9 in Serbian loess is also soils as root channel deposits. strikingly similar to that of the Chinese loess. In this interval, there are The magnetic mineral assemblages found in the Serbian loess are four clearly defined loess layers, three interglacial soils and only a quite similar to those seen in other typical loess-paleosol sequences weakly pedogenic L7SS1. The L7LL1 is much less weathered than the (e.g., Deng et al., 2005). The remanence carriers are mainly the soft L7LL2. The difference in weathering intensities between these two loess magnetic minerals, i.e., magnetite/maghemite. The behavior of the subunits can be clearly reflected in the changes in their χfd values hysteresis loops for loess-paleosol samples from the Stari Slankamen (Fig. 3). Underlying the S8 is another thick loess layer, L9. The above section indicate the dominance of low-coercivity magnetic phases. This stratigraphic model is strikingly similar to the typical loess-paleosol can be further demonstrated by the rapid IRM acquisition below sequence seen on the central and southern CLP, as represented by 300 mT, in addition to the presence of low Bcr values (21.9–48.4 mT). classic Luochuan section (Fig. 3). Some loess samples contain a higher proportion of high-coercivity

The only diﬀerence in our pedostratigraphic nomenclature is that phases. As suggested by the Ms-T curves, the low-coercivity magnetic the previous S9 was renamed L9SS1. This revision is based on the fol- minerals present are mainly of magnetite, evidenced by the Tc value lowing evidence: the soil layer at 52.4–53.2 m depth is composed of observed at 585 °C. The high-coercivity magnetic mineral hematite also weakly pedogenic soils with a blocky structure and a slightly more contributes to the NRM, but the main contributor to the primary ChRM reddish brown color than the surrounding loess layers. This soil is more is magnetite. weakly weathered than the L7SS1, which is also indicated by the low The MBB of the studied section was assigned to a depth of 50.4 m, in

χfd values compared to L7SS1. Therefore, this layer should be assigned the lower part of S8. The interval between 50.5 and 52.5 m is char- as an interstatial soil, rather than an interglacial soil. Following these acterized by a repeatedly oscillating magnetic direction (Fig. 8). Two lines of evidence, we named the dominant loess layer between S8 and reasons for this could be: (1) the viscous overprinting of the remanence the basal soil complex L9. The above adjustment is also consistent with signal by coarse-grained magnetites of eolian origin. In these weakly the marine evidence showing that MIS 23 was most likely an inter- weathered loess layers, the ChRM value was usually carried by coarse- stadial climatic event which occurred between the longer glacial stages grained magnetite, i.e., large pseudo-single domain (PSD) or multi-do- of MIS 24 and 22. main (MD) magnetite. These coarse grained eolian magnetites are of low coercivity, thus the viscous remanent magnetization probably can 4.2. Magnetostratigraphy of the Stari Slankamen section and its correlation replace its original detrital remanent magnetization (DRM) (Deng, with the Chinese loess 2008); (2) the root channel tracks and biogalleries indicate that in- tensive vegetation grew during the development of S8. The bioturba- AMS values, which can be described in terms of an ellipsoid with tion from plant roots and animals living may have had an eﬀect on the three orthogonal maximum, intermediate and minimum susceptibility alignment of the magnetic minerals, as seen in the samples with aty-

(K1, K2 and K3) principal axes, have been widely applied to the iden- pical AMS properties reminiscent of eolian dust deposits. The bio- tification of magnetic fabrics, and thus of depositional environments turbation could also have an effect on alignment of the magnetic mi- (Jackson and Tauxe, 1991; Rochette et al., 1992; Tarling and Hrouda, nerals within S8. Based on the above, we would suggest that the ChRM 1993). For weakly weathered loess sediments, the AMS ellipsoid reflects signals in the 50.5–52.5 m interval does not reliably reflect the primary the effects of wind and compaction, so the primary AMS should have an magnetization which occurred during/shortly after the deposition of oblate shape ellipsoid, with the maximum susceptibility axis (K1) par- dust, reinforcing the assignation of a depth of 50.4 m at least to the allel to the horizontal plane, and the minimum susceptibility axis (K3) MBB. perpendicular to the bedding plane (Tarling and Hrouda, 1993). Our Our result therefore defines a reversal of the MBB in S8 of the Titel- results show that the AMS ellipsoids are mainly oblate in shape, and Stari Slankamen section, which is broadly consistent with the results that the mean inclinations of the maximum and minimum axes of from studies of the Chinese loess. Most of the high-resolution magne- susceptibility ellipsoids are generally horizontal and vertical, respec- tostratigraphic investigations of Chinese loess have located the MBB in tively. There is no obvious difference in AMS properties between loess the middle or lower parts of L8 (Burbank and Li, 1985; Liu et al., 1988a; and paleosol layers, suggesting that the pedogenic processes did not Kukla and An, 1989; Rolph et al., 1989; Zheng et al., 1992; Zhu et al., fundamentally alter the AMS values. These results are consistent with 1994; Spassov et al., 2001; Guo et al., 2002; Pan et al., 2002; Wu et al., those of previous studies of typical loess deposits (e.g., Zhu et al., 2004; 2005; Yang et al., 2010; Jin and Liu, 2011), or in the upper part of S8

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(Heller and Liu, 1982; Wang et al., 2005, 2006; Jin and Liu, 2010; Liu paleosol sequences. The synchronicity of the prolonged periods of dust and Zhang, 2013). In the latter cases, a relatively thin L8 is observed in deposition, and their dominant climatic conditions, match the marine several sections, e.g., in the Luochuan and Jixian sections (Jin and Liu, oxygen isotope records well, in which MISs 24 and 22 appears to be the 2010; Wang et al., 2014). The MBB recorded in the S8 layer of the dominant glacial stage. Paleoglacial studies have shown that north- composite Serbian loess section is consistent with those Chinese loess- western Eurasia experienced severe glaciations during MISs 24 and 22 paleosol sequences which display a thin L8 unit. (Böse et al., 2012). In the deposits of the last 1.2 Ma in the Bay of In previous investigations, the AF demagnetization has defined a Biscay, Toucanne et al. (2009) identified a significant terrigenous input ∼1.0 m thick normal polarity within the Basal Complex below L9, from European ice sheets during MISs 24 and 22, comparable to the which has been interpreted as the upper Jaramillo subchron. However, inputs recorded during MISs 16, 12, 10, 8, 6 and 2. Moreover, in the in Chinese loess-paleosol sequences, the Jaramillo subchron is recorded fluvial deposits of the Upper Rhine Graben, the sediments assigned to in the L12–L10 interval (e.g., Pan et al., 2002). Our AMS measurements the uppermost Matuyama Chron consist of thick coarse grained clastics show that the Basal Complex was possibly severely disturbed. The de- derived from the glaciated Alps and the neighboring mountain ranges magnetization data also indicate that these samples do not carry a indicating an exceptionally intense glaciation during this period ChRM signal in their lower parts. Thus, the Jaramillo subchron had not (Gabriel et al., 2013; Scheidt et al., 2015). These extreme glacial con- been recorded in the Basal Complex. This is consistent with the results ditions probably provided the climatic context for the formation of L9 from Chinese loess-paleosol sequences, which record the event in a on the Eurasian continent. lower stratigraphic position. Overall, however, this study shows a coherence in the nature of the pedostratigraphy, changes in magnetic 5. Conclusions susceptibility and magnetostratigraphy between both the European and Chinese loess. We conducted detailed stratigraphic and magnetostratigraphic studies of the composite Titel-Stari Slankamen loess section in Serbia, the 4.3. Climate extremes as recorded in the Serbian and Chinese loess most complete loess-paleosol sequence over the past one million years in Europe. Based on characteristics identified in the field and detailed There are several stratigraphic markers in the Chinese loess-paleosol changes in magnetic susceptibility, we propose a revised pedostrati- sequences: strongly developed S4 and S5 soils, corresponding to MIS 11 graphy for the older part of the Stari Slankamen loess site. Rock mag- and 15–13, respectively; and three coarse-grained loess units L9, L15 netic analysis and progressive demagnetization indicate that the re- and L33, corresponding to MIS 24–22 (including the short interstadial manence carriers of the studied section are dominated by soft magnetic MIS 23), 38 and 102, respectively. The L9 and L15 layers have been minerals, such as magnetite/maghemite, and that the principal con- termed the “upper sandy loess layer” and “lower sandy loess layer”, tributor to the ChRM signal is magnetite, consistent with the reported respectively (Liu, 1985). Guo et al. (1998) found that these strati- findings of typical loess-paleosol sequences in semi-arid regions. Using graphic markers represent two kinds of climate extremes, each with the thermal and hybrid demagnetization (samples were thermally de- their own global significance: major warm and humid interglacial cli- magnetized up to 150 °C and subsequently subjected to progressive AF mates; and extremely cold glacial conditions. These events can be demagnetization), the stratigraphic position of the MBB was de- linked with changes in strength of North Atlantic Deep Water (NADW). termined not deeper than the S8 layer. We attributed the unstable Based on correlation with global paleoclimatic records, Guo et al. normal polarity found in the upper part of L9 below the MBB to the (2009) further concluded that upper layer S5 (MIS 13) represents a viscous overprinting of the remanence by coarse-grained magnetites of warm and humid climatic extreme in the Northern Hemisphere, caused eolian origin and/or to the bioturbation. The two short normal pola- by the asymmetrical evolution of glacial-interglacial cycles in the two rities previously observed in the middle of layer L9 and in the Basal polar regions. The Serbian loess stratigraphy provides new evidence to Complex, were not confirmed by the present study. This study therefore support these previous conclusions. provides the first thermal demagnetization-based magnetostratigraphic The S5 soil complex in Serbia consists of three layers of soils in the record of Serbian part of Danube loess, and shows that its lithological Dukatar section, consistent with the S5 pedocomplex found in Chinese stratigraphy, magnetic polarity stratigraphy and rock magnetic changes loess. The S5SS1 soil is the strongest developed pedocomplex in loess are generally coherent with loess deposits in China, further eastward on deposits from the last one million years. The strongly rubified S5SS1, S7 the vast Eurasian continent. The synchronous occurrence of a warm and and S8 layers have been classified as subtropical soils (Bronger, 1976, humid climate during MISs 15–13 and of an arid and cold climate 2003), and are different from temperate forest soils S6 and S4. The during MISs 24–22 in the two regions provides new evidence that ex- consistently strongly developed S5SS1 layer in China and Serbia would treme climatic events during these two intervals are common to the indicate that an extreme warm and humid interglacial climate occurred paleoclimates of the Northern Hemisphere. in the Eurasian continent during MIS 13. However, marine oxygen isotope records and European Project for Ice Coring in Antarctica Acknowledgements (EPICA) temperature records show that MIS 13 was one of coolest interglacials of the past 800 ka (EPICA community members, 2004; Thanks are extended to Mladjen Jovanović, Nebojša Milojković, Lisiecki and Raymo, 2005). Guo et al. (2009) proposed that the ex- Nemanja Tomić, Igor Obreht, Tamara Dulić, Tamara Vazić for help pansion of the Antarctica ice sheets drove a northward displacement of during the field work and to Professors Rixiang Zhu, Chunsheng Jin, the Inter-Tropical Convergence Zone (ITCZ), which in turn drove strong Chunxia Zhang and Luo Wang for constructive discussions. This study summer monsoonal circulations within the Northern Hemisphere. The was supported by the National Natural Science Foundation of China combination of the northward displacement of low-latitude climatic (Projects 41430531, 41690114 and 41625010) and International regimes and strengthening NADW may well be the critical factors which Partnership Program of Chinese Academy of Sciences (Grant led to increased temperature gradients in the North Atlantic during MIS 131C11KYSB20160061). This research was also financially supported 13 (Candy and Mcclymont, 2013). These changes may have led to in- by Project 176020 of the Serbian Ministry of Education and Science, as creases in the moisture transport volumes to the European mainland, well as a grant “Development of novel methods for better under- leading in turn to the formation of a strongly rubified S5 layer in Serbia standing of loess formation and reconstruction of the Pleistocene cli- (Marković et al., 2011, 2012b). mate and environmental dynamics” of Inter-Governmental Chinese- The oldest loess unit in Serbia, L9, is characterized by a weakly Serbian bilateral program. SBM acknowledge the financial support from weathered, thick loess layer, and contains an interstadial soil, L9SS1, a fellowship of CAS President's International Initiative for visiting which is also consistent with the L9 layer observed in Chinese loess- Scientists.

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