Paleoclimate change since the Miocene inferred from clay-mineral records of the Jiuquan Basin, NW China

Journal Pre-proof Paleoclimate change since the Miocene inferred from claymineral records of the Jiuquan Basin, NW China

Yitong Liu, Chunhui Song, Qingquan Meng, Pengju He, Rongsheng Yang, Ruohan Huang, Shuo Chen, Daichun Wang, Zhenxing Xing PII:

S0031-0182(20)30175-9

DOI:

https://doi.org/10.1016/j.palaeo.2020.109730

Reference:

PALAEO 109730

To appear in:

Palaeogeography, Palaeoclimatology, Palaeoecology

Received date:

26 July 2019

Revised date:

1 April 2020

Accepted date:

2 April 2020

Please cite this article as: Y. Liu, C. Song, Q. Meng, et al., Paleoclimate change since the Miocene inferred from clay-mineral records of the Jiuquan Basin, NW China, Palaeogeography, Palaeoclimatology, Palaeoecology (2020), https://doi.org/10.1016/ j.palaeo.2020.109730

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© 2020 Published by Elsevier.

Journal Pre-proof Paleoclimate change since the Miocene inferred from clay-mineral records of the Jiuquan Basin, NW China Yitong Liua, Chunhui Songa, *, Qingquan Menga, Pengju Hea, Rongsheng Yangb,c,d, Ruohan Huanga, Shuo Chena, Daichun Wanga, Zhenxing Xinga a

School of Earth Sciences & Key Laboratory of Mineral Resources in Western China (Gansu Province), Lanzhou

University, Lanzhou 730000, China Key Laboratory of Continental Collision and Plateau Uplift, Institute of Tibetan Plateau Research, Chinese

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Academy of Science, Beijing 100101, China

University of Chinese Academy of Science, Beijing 100049, China

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Centre de Recherches Pétrographiques et Géochimiques, UMR7358, CNRS, Université de Lorraine, 54500 Nancy,

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France

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*Corresponding author: [email protected] (C. Song)

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E-mail addresses of other authors: [email protected] (Y. Liu), [email protected] (Q. Meng), [email protected] (P. He), [email protected] (R. Yang), [email protected] (R. Huang), [email protected] (S. Chen), [email protected] (D. Wang), [email protected] (Z. Xing)

Abstract

Global cooling and the uplift of the Tibetan Plateau have long been considered the crucial controls of the climate change in inland Asia since the Cenozoic. However, which of these factors has played the leading role is unknown. To understand climate change and the controlling factors in inland Asia, here, we present new records of clay mineralogy and trace elements of clay fractions from the Neogene sedimentary sequence in the Jiuquan Basin of the northeastern Tibetan Plateau. The clay-mineral records reveal four stages of paleoclimate changes. From ca. 24 Ma to 17 Ma, the low total smectite and (smectite+I/S+kaolinite)/(illite+chlorite) and high illite contents suggest

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weak chemical weathering and hence arid climatic conditions. For ca. 17-14 Ma, the high total smectite and (total smectite + kaolinite)/(illite + chlorite) and low illite contents suggest strong chemical weathering, indicating a change in climate from cold and dry to warm and humid. There was no palygorskite during this warm and humid period. From ca. 14 Ma to 8 Ma, the low total smectite content, high illite content and the appearance of palygorskite indicate that the climate turned to cold and dry. Since 8 Ma, low total smectite as well as high illite and

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chlorite contents suggest a colder and drier period. The records of clay mineralogy illustrate that the Jiuquan Basin

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has experienced increasing aridity since ca. 14 Ma, synchronous with the inland Asian aridification. Given the synchroneity with the global cooling, we suggest that the climate evolution in the Jiuquan Basin from the late

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Oligocene to middle-late Miocene was mainly controlled by global climate change. Since the late Miocene, the

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uplift of the Tibetan Plateau and global cooling have significantly influenced the decreasing temperature and

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reaching the Jiuquan Basin.

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humidity of the Jiuquan Basin. The uplift of Tibetan Plateau may intensify the aridity by blocking moisture from

1 Introduction

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Key words: Neogene; Inland Asia; Aridification; Global cooling; Tibetan Plateau

The Asian paleoenvironment and paleoclimate have varied significantly since the Cenozoic (Ruddiman et al., 1989; Manabe et al., 1990; Ma et al., 1998, 2004; An et al., 2001; Guo et al., 2008; Sun et al., 2013; Miao et al., 2011, 2012, 2013; Liu et al., 2015; Caves et al., 2016; Ye et al., 2018). The most striking shift in the paleoenvironment of Asia was from a planetary-wind-dominant pattern to a monsoon-dominant pattern around the boundary of the Oligocene and Miocene (Guo et al., 2002; Qiang et al., 2010; Sun et al., 2010). Central Asian aridification as well as the origin and evolution of the Asian monsoon have attracted considerable attention (An et al., 2001; Guo et al., 2002; Ding et al., 2005; Zhuang et al., 2011, 2014; Lu et al., 2014; Sun et al., 2015; Zhang et al., 2015; Wu et al., 2019; Zhang et al., 2020; Zhao et al., 2020). Moreover, intensified arid conditions and

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reduced precipitation in Central Asia have led to the widespread distribution of deserts and loess deposition (Miao et al., 2012). Numerous studies have showed that the uplift of the Tibetan Plateau following the India-Asia collision has blocked moisture transport from the ocean to inland Asia as well as reorganized the regional atmospheric circulation, causing the central Asian aridification (Harrison et al., 1995; Li et al., 1999; An et al., 2001; Graham, 2005; Kent-Corson et al., 2009; Zhuang et al., 2011; Li et al., 2014). Some researchers have emphasized that global

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cooling was the primary factor of these changes (Guo et al., 2004; Dupont-Nivet et al., 2007; Lu et al., 2010; Fang

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et al., 2015). The regression of the Paratethys Sea has also been identified as an essential factor for the intensified arid conditions in Central Asia (Shen et al., 2017; Kaya et al., 2019). However, when, how, and to what extent these

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three potential factors affected the central Asian aridification remain debated, largely because of a lack of reliable

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records based on continuously long sedimentary sequences in the critical zone, which limits our ability to examine

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these issues.

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A series of sedimentary basins developed on the northeastern Tibetan Plateau and deposited with thick Cenozoic

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sediments. These sedimentary sequences contain abundant information regarding paleoenvironmental changes and are thus considered reliable archives to establish the history of central Asian aridification. Recently, many studies have been completed on the northeastern Tibetan Plateau. Neogene climate and environment changes have been widely studied. Numerous studies have recorded the mid-Miocene climatic optimum via sporopollen studies (Andrews et al., 1996; Ma et al., 1998; Miao et al., 2008; Jiang et al., 2008), calcium-carbonate and clay-mineral indices (Han et al., 2008; Wang et al., 2013) and fossil records (Coombs et al., 1983; Andrews et al., 1996; Semprebon et al., 2011; Li et al., 2015). Additionally, the Tibetan Plateau has experienced multiple stages of uplifting and exhumation throughout the Cenozoic. Many studies have shown the widespread uplift of the northeastern Tibetan Plateau at approximately 8-9 Ma, as revealed by sedimentology studies (Huang et al., 2006; Fang et al., 2007, 2016, 2017) as well as paleoaltimetry and low-temperature thermochronology studies (Lease et

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al., 2007; Zheng et al., 2003, 2006, 2010; Zhuang et al., 2014; 2018; 2019). Generally, the uplift of the Tibetan Plateau blocked the moisture transportation from the ocean to inland Asia and reorganized the Asian atmospheric circulation; thus, the uplift of the Tibetan Plateau influenced the regional and global environment and affected the Asian monsoon as well as central Asian aridification (Raymo et al., 1992; Harrison et al., 1995; Li et al., 1999; Graham, 2005; Kent-Corson et al., 2009; Zhuang et al., 2011). Hence, the Asian monsoon formed and inland Asian

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aridification increased at approximately 6-9 Ma, as demonstrated by the accumulation of aeolian red clay across the

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Chinese Loess Plateau (An et al., 2001; Ding et al., 2001; Qiang et al., 2001), abrupt changes in geochemical indices (Wan et al., 2010; Yang et al., 2016) and the rapid development of steppes (Quade et al., 1989, 1995; Ma et

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al., 1998, 2005; Hui et al., 2011). Thus far, the long-term paleoenvironmental changes recorded by clay-mineral

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analysis are lacking for the northeastern Tibetan Plateau. Indicators of clay minerals and their assemblages have the

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potential to determine the paleoclimate and paleoenvironment (Singer, 1984; Thiry et al., 2000). Thus, it is vital to

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provide clay-mineral records to reveal the linkage between tectonics and climate during the Neogene in this region. The Jiuquan Basin is located in the northeast of the Tibetan Plateau, NW China, and is filled with thick and

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continuous Cenozoic sediments (Fig. 1a, b). The chronology has been established via the magnetostratigraphy (Zheng et al., 2004; Fang et al., 2005; Dai et al., 2005; Song, 2006; Wang et al., 2016). Long-term paleoecology and tectonic evolution have been reconstructed using various geological records and numerical modeling (Ma et al., 1998, 2004; Zhao et al., 2001; Lin et al., 2010; Miao et al., 2013; He et al., 2017). Here, we present clay-mineral records of the clay fraction (<2 μm) in the Jiuquan Basin since the Neogene and discuss the process as well as mechanism of Asian paleoclimate changes in the context of the uplift of the Tibetan Plateau, central Asian aridification, and global climate change.

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Fig. 1: (a) The location of study area and related region; (b) Digital elevation map of the northeast margin of the Tibetan Plateau; (c) geological schematic diagram of the Jiuquan Basin (modified from Yan et al., 2013); (d) transverse cross-section plan of the Jiuquan Basin (modified from Dai et al., 2005).

2 Geological setting

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The Jiuquan Basin is a significant oil and gas basin in the western Hexi Corridor. The basin is bounded by the North Qilian Shan marginal thrust to the south, the Longshou Shan-Kuantan Shan Fault to the north, the Altyn Tagh Fault to the west, and the Yumu Shan to the east (Song et al., 2001; Zhu et al., 2005; Zhang et al., 2005; Wang et al., 2016) (Fig. 1c). The basin has an area of 3408 km2 and reaches altitudes between 1350 and 1500 m. This basin is highest in the south and decreases gradually to the northeast. Climatically, the basin is situated at the intersection of

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the East Asian monsoon and inland Asian arid zone. The average annual temperature, precipitation and evaporation

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in the basin are 7.4 ℃, 83 mm and 2149-2539 mm, respectively. This region is characterized by an arid climate, low rainfall and long hours of sunshine. The modern natural vegetation is typical, sparse desert vegetation (Wu et al.,

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1998).

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The Cenozoic deposits in the Jiuquan Basin consist of the Huoshaogou, Baiyanghe, Shulehe, Yumen, Jiuquan

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and Gobi Formations in sequence (Song et al., 2001; Zheng et al., 2004; Wang et al., 2016; He et al., 2017).

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Additionally, Neogene strata are continuous and well exposed in the southern Jiuquan Basin (Zheng et al., 2004; He et al., 2017). In this study, we chose two typical sections with continuous Neogene strata dated by

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magnetostratigraphy, i.e. the Shiyangjuan (SYJ) and Laojunmiao (LJM) sections (Fig. 1c). The SYJ section (39˚30′39″N, 98˚26′21″E to 39˚31′8″N, 98˚26′55″E) is >1300 m thick. The Baiyanghe and Shulehe Formations are exposed in this section (Fig. 2). The exposed portion of the Baiyanghe Formation is >60 m thick and is characterized by brownish-red mudstone that is interbedded with sandstone. The Shulehe Formation unconformably overlies the Baiyanghe Formation. Macroscopically, the Shulehe Formation consists of a sedimentary cycle with a coarse-fine-coarse sequence from bottom to top. The Shulehe Formation ranges in age from ca. 23 Ma to 8 Ma (Zheng et al., 2004; Song, 2006) and can be divided into three lithological members upward: the Gongxingshan, Getanggou and Niugetao Members (Fig. 2). The Gongxingshan Member is characterized by grayish-white, thick gravel sandstone, conglomerate, brownish-red mudstone and siltstone. The

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Getanggou Member consists of brownish-red mudstone, siltstone that is interbedded with sandstone and conglomerate. The Niugetao Member is characterized by grayish, thick gravel sandstone and conglomerate with brownish-red shaly sandstone. The LJM section (39˚47′46″N, 97˚32′45″E to 39˚48′12″N, 97˚33′5″E) is >2000 m thick and ranges in age from ca. 13 Ma to 0 Ma (Fang et al., 2005). This section includes portions of the Shulehe, Yumen, Jiuquan and Gobi

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Formations (Fig. 2). The Shulehe, Yumen, Jiuquan and Gobi Formations are bounded by unconformities below and

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between. The Getanggou and Niugetao Members in the Shulehe Formation are exposed. The Yumen and Jiuquan Formations are characterized by thick, dark-gray pebble- or cobble-conglomerate layers, sandy conglomerates that

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are intercalated with lenticular or banded sandstones and shaly sandstones. The Gobi Formation mainly consists

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primarily of dark-gray, 7-10 cm gravels (maximum of 50-70 cm).

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Fig. 2: Magnetic stratigraphy diagram of Cenozoic strata in the Jiuquan Basin (Fang et al., 2005; Song, 2006).

3 Materials and methods Clay minerals are the products of rock weathering. Paleoclimate changes, continental morphology and tectonic activities associated with the evolution of margin structures all influence rock weathering (Chamley, 1989). Additionally, the weathering intensity is mainly restricted by the lithology, morphology and climate, which further

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control the formation and transformation of clay minerals (Torgersen et al., 1986; Chamley, 1989). Clay-mineral

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analysis can be used to reestablish paleoclimatic changes over different timescales (Ahlberg et al., 2003; Chamley et al., 1989; Deconinck et al., 2005; Dera et al., 2009) because clay minerals carry a variety of indicators of climate

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change during formation and evolution. Compared to other proxies, clay-mineral assemblages are possibly more

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useful for reconstructing the Cenozoic paleoenvironmental changes in the northeastern Tibetan Plateau. First, clay

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minerals have a wide distribution in various lithologies of the upper continental crust and are relatively easy to

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sample (Taylor et al., 1985). Second, other indicators may be influenced by the sedimentary environment. For example, organic indicators and sporopollen are not easy to obtain under oxidized environments. Additionally,

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element indicators could be affected by diverse sedimentary environments (Zhong et al., 1998). The clay-mineral distributions of modern continental soils show the main controls of climate change rather than changes in the lithology (Chamley, 1989; Xiong et al., 1986). Thus, compared to other proxies, clay-mineral assemblages are relatively less influenced by provenance changes. Furthermore, previous studies have shown that most clay minerals in fresh/brine water are nearly eroded from the drainage area, with negligible contributions from their formation at the sediment-water interface or in the water tier (Chamley, 1989). Furthermore, diagenetic clay minerals are always insignificant in continental drainage basins (Chamley, 1989; Gao et al., 2017), and we can distinguish them using classical methods (Dunoyer et al., 1970; Hillier et al., 1995; Hong et al., 2007; Huyghe et al., 2011; Ye et al., 2018). For instance, typical diagenesis models show that the illite content and its proportion in

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mixed-layer I/S increase gradually with increasing temperature, pressure and burial depth (Weaver et al., 1984). Illite crystallinity can also be used to estimate the influence of diagenesis on clay minerals. Moreover, the genesis of clay minerals can be discerned through the SEM analysis of the microscopic structure. Generally, clay-mineral analysis is a useful method for restoring paleoclimate and paleoenvironment changes over diverse timescales, especially for the comparatively longer timescales in continental fluvial basins and ocean basins (Singer et al., 1980,

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1984; Thiry et al., 2000; Liu et al., 2003, 2010; Hong et al., 2010, 2017; Wang et al., 2011, 2013; Shen et al., 2017;

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Song et al., 2018).

In the study area, approximately 600 fresh rock samples were taken. Mudstone, silty mudstone and siltstone were

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sampled at intervals of 2 m, while sandstone and conglomerate were sampled at intervals of 10 m. Samples were

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assigned an age via comparison with magnetostratigraphy. Forty-five samples were chosen for XRD analysis to

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reconstruct the history of the paleoenvironmental evolution since the Miocene in the Jiuquan Basin, including the

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mineral type, composition, and ratios. The isolation of clay fractions (<2 µm) was conducted according to standard SYT 5163-2018 of the Chinese oil and gas industry. The clay components were separated by sedimentation and

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centrifugation. Rock samples were first treated with diluted H2O2 and HCl to remove organic matter and calcium carbonate. Then, the clay fractions (<2 µm) were separated by Stoke’s law determinations through successively washing the sediment after deflocculating with distilled water. Finally, clay was separated and free ions were removed by centrifugation in deionized water. The oriented samples of clay minerals were created by carefully pipetting the clay suspension onto the glass slides and drying at room temperature. Routine X-ray diffraction (XRD) analysis of the clay minerals was implemented for each sample, which included the continuous collection of three XRD patterns under natural conditions (N), after saturation for 24 h in ethylene-glycol in the desiccator (EG), and after heating in a muffle furnace at a temperature of 450℃ for 2 h (H). XRD analysis was conducted at the Key Laboratory of Mineral Resources in Western China (Gansu Province), Lanzhou University. Following treatment,

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XRD diagrams were obtained by XRD with CuKα radiation and an Ni filter by using a Rigaku D/MAX‐ 2000 diffractometer at a voltage of 40 kV and an intensity of 40 mA. The X-ray wave length was 1.540598 Å. Diffraction patterns (2θ) were scanned from 3° to 30°, with a step size of 0.0167°. The varieties and contents of clay minerals have primarily been deduced by XRD patterns with diverse peaks (d-values) and intensities (height or area of peaks) (Biscaye et al., 1965; Moore et al., 1997). Identification of clay minerals was mainly based on the

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001 basal reflections on three XRD diagrams, as described by Moore and Reynolds (1997) (Fig. 3). Normally, illite

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can be identified by peaks at 10 Å (001), 5 Å (002) and 3.33 Å (003) on the AD diffractogram, which display no changes after being treated with ethylene glycol. The (002) peak (7.1 Å) of chlorite nearly coincides with (001)

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peak (7.2 Å) of kaolinite on the EG diffractogram. Chlorite and kaolinite can be distinguished by the 3.53 Å peak

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of chlorite’s 004 reflection and the 3.58 Å peak of kaolinite’s 002 reflection (Liu et al., 2007; Wang et al., 2017).

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Moreover, chlorite is recognised by characteristic peaks on the EG diffractogram, i.e., 14.2 Å (001) and 4.74 Å

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(003), respectively. Smectite and I/S mixed layers have expansibility. I/S mixed layers can be divided into regular (<50%) and irregular I/S mixed layers (>50%) by the content of smectite in the I/S mixed layers (Reynolds, 1980).

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We can discriminate these expandable clay minerals by contrasting AD and EG diffractograms. After being treated with ethylene glycol, the smectite peaks of 12 to 15 Å will be transferred to 17 Å, with new peaks at 8.5, 5.67, and 4.25 Å. The 12 to 15 Å peak of regular I/S mixed layers is not transferred to 17 Å on an EG diffractogram (Fig. 3a). After being treated with ethylene glycol, the irregular I/S mixed layers peaks of 12 to 15 Å on the AD diffractogram will be transferred to 17 Å, with no peaks at 8.5, 5.67, and 4.25 Å on the EG diffractogram (Fig. 3b). Palygorskite has a characteristic peak approximately 10.5 Å on the AD diffractogram, with no change on the EG diffractogram (Fig. 3b). Semiquantitative estimations of clay minerals were obtained using the peak areas of the basal reflections based on standard SYT 5163‐ 2018. The contents of smectite and illite can be determined by the areas of the peaks at 17 Å and 10 Å, respectively. The total kaolinite and chlorite contents were calculated according to the area of the

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7 Å peak. The relative proportions of kaolinite and chlorite were estimated by the areas of the 3.58 Å (kaolinite) peak and 3.53 Å (chlorite) peak on the EG diffractogram (Biscaye, 1965). The remaining portion should represent I/S mixed layer minerals. The relative content of palygorskite was calculated according to the type and intensity of the 10.5 Å peak after peak differentiating and imitating (Yin et al., 2010). The percentage of smectite layers in the

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I/S mixed layer minerals was estimated following the method of Reynolds (1980).

Fig. 3: X-ray diffraction patterns of some representative samples of clay minerals. Black, blue and red lines represent the air-dried, ethylene glycol-saturated and heated (450°C) X-ray diffraction patterns, respectively. (a) Sample from SYJ 20 m with typical regular I/S mixed layers, illite, chlorite and kaolinite. (b) Sample from SYJ 257 m with typical irregular I/S mixed layers, smectite, illite, chlorite, kaolinite and palygorskite.

Provenance is an important factor that affects the composition of clay minerals. Generally, the ratios of trace elements are widely used to analyze provenance changes in diverse sediments (McLennan et al., 1985, 1993). To assess the effects of provenance on clay minerals, we used elemental analysis to restrict potential provenance changes. Approximately 260 samples (<2 µm clay fractions) were pretreated through a closed high-pressure acid-digestion method by using a mixture of hydrofluoric and nitric acid (Yang et al., 2015). The trace elements (<2 µm clay fractions) were measured by an inductively coupled plasma mass spectrometer (X‐ 7; Thermo‐ Elemental,

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USA) at the Key Laboratory of Mineral Resources in Western China (Gansu Province), Lanzhou University.

4 Results 4.1 Clay minerals The XRD analysis of clay minerals demonstrated that the major components were I/S mixed-layers, illite, kaolinite, chlorite, and limited amounts of smectite and palygorskite (Fig. 4). In this paper, we classified the I/S

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mixed-layers and limited smectite as the “total smectite” because I/S mixed-layers is often an intermediate product

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of the transformation between smectite and illite (Chamley, 1989). Moreover, I/S mixed-layers is also produced by weathering (detailed analysis below), often representing the relatively warm and humid climate conditions of the

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smectite (Wang et al., 2011). The contents of total smectite and illite played an important role, with average values

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of 57.6% and 24.1%, respectively. In contrast, chlorite and kaolinite were minor components, with average values

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of 10.3% and 6.9%, respectively. Only some samples contained small amounts of palygorskite. Overall, the

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contents of the total smectite, illite, chlorite and kaolinite varied from 17.0% to 87.0%, 7.0% to 48.0%, 2.8% to 24.3% and 1.9% to 17.7%, respectively. More specifically, illite content showed a relatively high value at 24-17 Ma

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and a sharp decrease at approximately 17 Ma. The content of illite reached its lowest value at 17-14 Ma, and then the illite content showed a gradual increase (Fig. 4a). In contrast, the content of total smectite exhibited the opposite trend (Fig. 4d). Chlorite content also demonstrated an obvious increase since approximately 8 Ma (Fig. 4c). The proportion of palygorskite increased after approximately 14 Ma (Fig. 4e). Notably, the percentage of smectite layers in the I/S mixed-layers were not well correlated with depth (Fig. 4f).

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Fig. 4: Relative abundances and ratios of clay-mineral assemblages in the Jiuquan Basin. I/S = illite/smectite mixed layers.

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4.2 Trace elements

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In this paper, the ratios of (La/Yb)N, La/Th and Th/Sc were used to evaluate the effects of provenance (Fig. 5). During the period of 24-8 Ma, the (La/Yb)N, La/Th and Th/Sc ratios fluctuated gradually, demonstrating a relatively stable provenance. At approximately 8 Ma, the ratios of (La/Yb)N, La/Th and Th/Sc showed a decreasing trend, which indicated that the provenance may have changed at this time (Fig. 5). These ratios showed that the provenance has little effect on clay minerals in the Jiuquan Basin. Thus, we can use the composition and changes in clay minerals to interpret climate change.

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Fig. 5: Depth profiles of provenance indicators in the Jiuquan Basin. Black arrows show the decreasing trends in the (La/Yb)N,

5 Discussion

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La/Th and Th/Sc ratios at approximately 8 Ma.

5.1 Origins of clay minerals in the Jiuquan Basin Generally, clay minerals are products of the erosion and weathering of fresh bedrocks and soils, which can be altered by diagenetic modifications after sedimentation and deposition (Chamley, 1989; Thiry et al., 2000). In some cases, clay minerals from river/lake systems or from diagenesis can influence the climate sensitivity of detrital clay minerals produced by the weathering of bedrocks in sedimentary basins (Singer et al., 1984; Thiry et al., 2000; Huyghe et al., 2011; Ye et al., 2018). We discuss these factors as follows. First, diagenesis can influence the transformation of clay minerals, confounding the clay-mineral analysis of paleoclimate change (Chamley, 1989). Smectite transforms into illite with increasing burial depth, which is known as the illitization of smectite and is the

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most widespread clay-mineral diagenesis in depositional basins (Chamley, 1994). Typical diagenesis models show that the illite content and its proportion in mixed-layer I/S increase gradually with increasing temperature and pressure and burial depth (Weaver et al., 1984). In this study, we found that content changes in the smectite proportions in mixed-layer I/S differed from the typical diagenesis depth profile of clay minerals (Fig. 4f). Additionally, a remarkable negative correlation existed between the I/S mixed-layers and detrital chlorite contents

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(Fig. 6), indicating I/S mixed-layers in the study area were produced by weathering not diagenesis. The very low

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amount of pure smectite is associated with the large amount of I/S mixed layers, showing that smectite in the study area originated from weathering instead of volcanic materials. Thus, diagenesis barely influenced the clay minerals

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in the study area. Second, authigenic clay minerals can influence the clay-mineral analysis of paleoclimate changes.

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Previous studies on clay-mineral sources in modern terrigenous basins have demonstrated that clay minerals in

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rivers and lakes have similarly major detrital features with their circumjacent drainage basins (Court et al., 1972;

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Tomadin et al., 1986; Chamley, 1989). A lack of cations and silicon in rivers and saline lakes may create deficiencies in authigenic clay minerals in fresh and salt water (Gao et al., 2017). For these reasons, we assume that

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fewer authigenic clay minerals may be present in the research area. In conclusion, the clay minerals in our study area had a mostly detrital origin and were barely affected by diagenesis and authigenesis.

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Fig. 6: Correlations between chlorite and illite/smectite mixed layer minerals.

5.2 Provenance changes in the Jiuquan Basin The influence of provenance change should also be considered when clay minerals are used to reconstruct paleoclimate changes. Th is a typically incompatible element, and Sc is a compatible element in igneous systems; thus, the Th/Sc ratio is useful to trace igneous differentiation (McLennan et al., 1993). The Th/Sc, La/Th and

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(La/Yb)N ratios exhibit intense stability during metamorphism and sedimentation, during which these elements

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cannot easily migrate. Therefore, the Th/Sc, La/Th and (La/Yb)N ratios can still retain the geochemical features of the parent rocks even after experiencing a series of complex geological processes, making them good indicators of

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provenance change (Taylor et al., 1985; Prudencio et al., 1989; Crichton et al., 1993). Tectonic movements and

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windblown dust are two potential factors that may cause provenance change. Thermochronologic studies revealed

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that rapid exhumation occurred during the middle-late Miocene in the Liupan Shan (Zheng et al., 2006), the

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northern Qilian Shan (Zheng et al., 2010; Zhuang et al., 2018; Li et al., 2019), the southern Qilian Shan (He et al., 2018; Pang et al., 2019; Yu et al., 2019), and the Jishi Shan (Lease et al., 2011; Xu et al., 2018). A large amount of

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aeolian material accumulated between 15 and 13 Ma in inland Asia (Guo et al., 2002). Large-scale aeolian accumulation occurred at 8-7 Ma on the Loess Plateau, suggesting that the interior of Asia became a desert during the late Miocene (Sun and An, 2001; An et al., 2001; Guo et al., 1999, 2002). An obvious increase in dust accumulation occurred at approximately 8 Ma, which was caused by enhanced aridification in Central Asia (e.g., Rea et al., 1998; An et al., 2001; Yang et al., 2017). However, the Th/Sc, La/Th and (La/Yb)N ratios were stable during the period of 24-8 Ma, with no obvious fluctuations during the period of assumed provenance change. Hence, we concluded that windblown dust barely influenced the provenance changes in study area, with no significant provenance changes. Tectonic movements may have influenced provenance change at approximately 8 Ma. In addition, sediments with varying grain sizes may have been redistributed by sedimentary sorting. Sorting

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greatly affects whole-rock paleoenvironmental analysis. However, the effect of sedimentary sorting is not significant for clay minerals (<2 µm fractions) that are concentrated in fine particles. After considering the relevant factors of diagenesis, authigenesis and provenance change, any changes in clay-mineral assemblages can be used to reconstruct the paleoenvironment and paleoclimate changes in the Jiuquan Basin. 5.3 Correlation with regional and global paleoenvironmental records

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Generally, there are four common clay minerals, including smectite, kaolinite, illite and chlorite. Illite is regarded

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as the primary mineral, which is the weathering product of aluminosilicate minerals under slightly alkaline conditions in an arid and cold climate, reflecting decreased hydrolytic processes in continental weathering

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(Chamley, 1989; Weaver et al., 1989). Similarly, chlorite forms under alkaline conditions in a dry climate and under

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low rates of chemical weathering (Biscaye et al., 1965; Ducloux et al., 1976). Kaolinite is a mineral that forms from

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feldspar, mica and pyroxene under acidic conditions in a warm and humid climate and under intense leaching,

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indicating strong weathering (Rateev et al., 1969). Smectite is a direct indicator of atmospheric precipitation and is a secondary mineral that is derived from ferromagnesian silicate and parent aluminosilicate by chemical weathering

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under warm and humid conditions (Kennett et al., 1994). Usually, mixed-layer I/S is an incomplete product of the transition of smectite or illite (Hong et al., 2007). Smectite and I/S mixed-layers can often be regarded as intermediate products under humid and mild climates (Wang et al., 2011). Illite and chlorite are regarded as early weathering products, while smectite and kaolinite often experience relatively long-term weathering. Thus, the (kaolinite+total smectite)/(illite+chlorite) ratio can be used to trace the climate and weathering intensity in source regions (e.g., Bouquillon et al., 1990; Thiry et al., 2000; Shen et al., 2017). From the late Oligocene to early Miocene, the relevant indicators of clay minerals indicate a cold and semi-arid climate in the Jiuquan Basin. The low (smectite+I/S+kaolinite)/(illite+chlorite) ratio indicates relatively cold and arid climatic conditions, dominated by physical weathering. This inference is supported by the increase in herbs and

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conifers in the Xining Basin (Wang et al., 1990), gypsum layers discovered in the Hoh Xil Basin (Liu et al., 2000), and the rock magnetics and n-alkane records across the northeastern Tibetan Plateau (Long et al., 2011; Fang et al., 2015). Compared to the previous stage, the illite content decreases obviously at 17 Ma (Fig. 4a), and the content of total smectite increases (Fig. 4d). Meanwhile, the ratios of (smectite+I/S+kaolinite)/(illite+chlorite) and (smectite+I/S)/(illite+chlorite) are higher and fluctuate (Fig. 7d, e). Changes in the contents and ratios of clay

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minerals indicate a relatively warmer and more humid climate from ca. 17 to 14 Ma. The presence of such a warm

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and humid climate has also been supported by sedimentary facies (Ma et al., 2016) and sporopollen assemblages in the Jiuquan Basin (Fig. 7a, b; Miao et al., 2008). Sporopollen studies in northern China (Andrews et al., 1996; Ma

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et al., 1998), calcium-carbonate and clay-mineral indices in the Qaidam Basin (Han et al., 2008; Wang et al., 2013)

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have suggested warm and humid climatic conditions, increased precipitation and the development of the East Asian

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monsoon. The mid-Miocene mammalian fossil sites are also abundant in China. Their compositional characteristics

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were clearly consistent with a warming event. A large amount of warm-loving and wet-loving mammals emerged, such as Platybelodon, Castor, Anchitherium, Ancylopoda, Kubanochoerus, etc. (Coombs et al., 1983; Andrews et al.,

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1996; Semprebon et al., 2011; Li et al., 2015). Platybelodon fauna in the mid-Miocene are indicative in a fairly warm and humid climate (Semprebon et al., 2011). The illite and chlorite contents both increase, while the total smectite content decreases after 14 Ma (Fig. 4a, c, d). The ratios of (smectite+I/S)/(illite+chlorite) and (smectite+I/S+kaolinite)/(illite+chlorite) also decrease and remain relatively stable after 14 Ma (Fig. 7d, e). The proportion of palygorskite, which represents arid and semi-arid climates, increases after approximately 14 Ma (Fig. 4e), showing that the climate changed from humid to arid at this time. Moreover, the illite and chlorite contents increase sharply, and the total smectite content shows an obvious decreasing trend after ~8 Ma, indicating a colder and drier climate in the Jiuquan Basin (Fig. 4a, c, d). A mid-Miocene climatic cooling event has also been recorded by geochemical studies on teeth fossils (Domingo et al.,

Journal Pre-proof 2009, 2012) and stable δ18O values (Jin et al., 1995). The sedimentary sequences from numerous basins in eastern Asia have revealed aridification at approximately 14 Ma and 8 Ma according to grain-size and clay-mineral proxies (Lu et al., 2004; Wan et al., 2007) as well as a large amount of aeolian material that accumulated between approximately 15 and 13 Ma in inland Asia (Guo et al., 2002). Furthermore, abundant paleoclimate evidence has shown that the paleoclimate in Eurasia was cold and dry in the middle Miocene (Miao et al., 2012). The North

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Pacific dust flux has also indicated a cold climate at this time (Rea et al., 1985, 1998). Sporopollen studies have shown that steppe vegetation had developed at approximately 13 Ma in the Jiuxi, Qaidam and Junggar Basins

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(Miao et al., 2011; Sun et al., 2010; Ma et al., 2005). The stable δ18O isotope in the Linxia Basin (Dettman et al.,

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2003), Tarim Basin (Graham et al., 2005) and Qaidam Basin (Kent-Corson et al., 2009) have revealed more

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positive values at approximately 13 Ma.

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The drier and cooler climate during ca. 8-0 Ma revealed by clay minerals is roughly synchronous with the global

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marine δ18O records (Rea et al., 1998; Zachos et al., 2001). For instance, local seawater δ18O records from ODP Site 1146 in the northern South China Sea have suggested that the paleoclimate in eastern and southern Asia shifted

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to drier conditions after ca. 7.5 Ma (Steinke et al., 2010). Additionally, the paleoclimate in Northwest China became drier after 8 Ma, accompanied by biomarker evidence (Wang et al., 2012) and the sediment color varied from aubergine to isabellinus (Song et al., 2005). Pollen evidence has suggested that the rapid development of steppes occurred at 8.5-6 Ma in the Jiuxi Basin (Ma et al., 2005), ca. 8.5 Ma and 6.9 Ma in the Linxia Basin (Ma et al., 1998), and 8-4 Ma in Pakistan, North America and Africa (Quade et al., 1989, 1995). Xerophytic taxa became dominant after 8.0 Ma, indicating a significant aridification event (Ma et al., 1993; Song et al., 2001; Ma et al., 2016). Large-scale aeolian accumulation occurred at 8-7 Ma over the Loess Plateau, suggesting that the interior of Asia became a desert during the late Miocene (Sun and An, 2001; An et al., 2001; Guo et al., 1999, 2002). The gradual increase in aeolian sediments since 7.4 Ma in the Linxia Basin is indicative of a period of strong

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desertification in central China (Fan et al., 2006). Grain-size records in the Linxia Basin (Xu et al., 2007) and pollen records in the Tianshui Basin (Hui et al., 2011) have shown that NW China’s arid climate originated at 7.4 Ma and strengthened rapidly at 6.4 Ma. In conclusion, climate changes reflected by clay-mineral assemblages in the Jiuquan Basin are consistent with diverse indices of global and regional climate. 5.4 Driving mechanisms of paleoclimate change in the Jiuquan Basin

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Three main potential drivers exist for the paleoclimate changes in the study area: the retreat of the Paratethys Sea,

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global climate change and the uplift of the Tibetan Plateau (Raymo et al., 1988; Ramstein et al., 1997; Ruddiman et al., 1997; Ding et al., 2005). Here, we compare global and regional records of typical climatic and tectonic events

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with our data to reveal the main driving mechanisms. Previous studies have shown that the retreat of the Paratethys

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during the Cenozoic played an important role in the central Asian aridification (Bosboom et al., 2014 a; Carrapa et

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al., 2015; Sun et al., 2015, 2016). Nevertheless, the Paratethys was confirmed to have retreated from the Tarim

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Basin before the Oligocene, although the exact time is uncertain (Bosboom et al., 2014 a; Carrapa et al., 2015; Sun et al., 2015). In this paper, we focus on the paleoclimate changes in the Jiuquan Basin since the late Oligocene. The

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retreat of the Paratethys is irrelevant. The global climate also influences regional climate change. The clay-mineral assemblages in this study showed a warm and humid climate in the Jiuquan Basin during the middle Miocene. The mid-Miocene climatic optimum represented a strong warming event that was unrelated to human activities in geological history. The Antarctic volume decreased by 10-25% compared to the present volume (de Bore B et al., 2010), and the deep-sea temperature increased. Additionally, the temperature of the midlatitude region was estimated to be 6℃ higher than the current value (Flower et al., 1995). After the mid-Miocene climatic optimum, a mid-Miocene climatic cooling event occurred at approximately 14 Ma, accompanied by a sharp increase of approximately 2% in oxygen isotopes (Fig. 7g) and a global temperature decrease of more than 5°C (Kocsis et al., 2009), after which the Antarctic ice sheet developed (Zachos et al., 2001). During this period, climate cooling and

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regression occurred simultaneously, with sea level dropping by 40-50 m (Kennett et al., 1982). Meanwhile, the surface water temperature in the South Pacific decreased, according to calcium-magnesium thermometer data (Shevenell et al., 2004). After combining some global climate events and climate changes in the Jiuquan Basin from the late Oligocene to middle-late Miocene, the climate events recorded by clay minerals in the Jiuquan Basin covary with global cooling or warming period. We conclude that the three climate stages (cold-warm-cold)

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occurred in the Jiuquan Basin from the late Oligocene to middle-late Miocene were mainly influenced by global

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climate change.

General circulation models have mainly focused on the effects of regional tectonism on Asian and global climate

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(An et al., 2001; Liu et al., 2004), testifying that the uplift of the Tibetan Plateau can increase aridification,

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monsoons and erosion in inland Asia. Furthermore, Tibetan uplift can induce global cooling by perturbing

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atmospheric circulation and lowering carbon dioxide, which are interrelated with strong rock weathering

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(Ruddiman et al., 1977; Raymo et al., 1988). Sedimentary flux and thermochronologic data have shown relatively stable tectonism in the Jiuquan Basin and surrounding areas from the late Oligocene to middle Miocene (Ma et al.,

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2016). Thermochronologic studies have revealed that rapid exhumation occurred in the middle-late Miocene in the Liupan Shan (Zheng et al., 2006), the northern Qilian Shan (Zheng et al., 2010; Zhuang et al., 2018; Li et al., 2019), the southern Qilian Shan (He et al., 2018; Pang et al., 2019; Yu et al., 2019), and the Jishi Shan (Lease et al., 2011; Xu et al., 2018). Additionally, analyses of the thermochronology, strata and physiognomy in the Liupan Shan, which are located in the extreme northeastern portion of the Tibetan Plateau, have indicated the strong uplift of the Liupan Shan and the disassembly of the Erdos planation surface since 8 Ma (Song et al., 2001; Zheng et al., 2006; Zhang et al., 2006). Growth strata and unconformity formed in the Qaidam Basin, Jiuxi Basin, Guide Basin and Linxia Basin at approximately 8 Ma (Song et al., 2001; Fang et al., 2005; 2007; Yuan et al., 2007). Moreover, trace elements (LaN/YbN, La/Th and Th/Sc) have shown that the provenance may have changed at this time, indicating

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the occurence of tectonic movement around the Jiuquan Basin. Meanwhile, the deposition rate, gravel content and grain size increased gradually after approximately 8 Ma (Fig. 7c). We also found that conglomerates and growth strata were exposed in the LJM section after 8 Ma, which were possibly affected by the tectonic movement. All of these studies illustrated that the Tibetan Plateau underwent strong upheaval at approximately 8 Ma, which affected the entire plateau. The Tibetan Plateau’s uplift would have prevented the access of warm and moist monsoonal air

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from the eastern Pacific Ocean and Indian Ocean into a wide region along the northern side of the high plateau,

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changing the environment and ecosystems in Central Asia (Li et al., 1995; Fang et al., 2003, 2007). Combining our analysis and comparison of tectonic events, global climate change and clay-mineral contents in the Jiuquan Basin

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since the middle-late Miocene, it is shown that the cold and dry climate in the Jiuquan Basin since approximately 8

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Ma was mainly affected by the uplift of the Tibetan Plateau, with global cooling being a secondary influence.

Fig. 7: Diverse records of global and regional climate change as well as the uplift of the Tibetan Plateau since the late Oligocene. (a, b) Contents of Ephedripites and Chenopodipollis in the Jiuquan Basin (Ma et al., 1993; Ma et al., 2004; Miao et al., 2008); (c) deposition rate (Song, 2006); (d) the ratio of (Smectite+I/S)/(Illite+Chlorite) in the Jiuquan Basin (this study); (e) the ratio of (Kaolinite+Smectite+I/S)/(Illite+Chlorite) in the Jiuquan Basin (this study); (f) the ratio of (La/Yb)N in the Jiuquan Basin (this study); (g) curve of deep ocean oxygen isotope (Zachos et al., 2001).

6

Conclusions

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In this paper, two sections were studied that cover an age range since 24 Ma. Based on the reliable chronostratigraphic framework, we reconstructed the paleoclimate in the Jiuquan Basin and discussed the mechanism of climate change during the past 24 million years according to clay-mineral indicators. We conclude with the following: (1) Clay-mineral assemblages in the Jiuquan Basin were characterized by mixed-layer I/S, illite, chlorite, kaolinite,

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and limited amounts of smectite and palygorskite. Additionally, the clay minerals in the study area were all of

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detrital terrigenous origin. We identified four stages occurred in the Jiuquan Basin since the late Oligocene based on clay-mineral analysis. From ca. 24 to 17 Ma, the climate was relatively cold and dry, dominated by physical

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weathering. From ca. 17 to 14 Ma, the climate was warm and moist, dominated by chemical weathering. After 14

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colder and drier, dominated by physical weathering.

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Ma, the climate changed from warm and humid to cold and dry. Since approximately 8 Ma, the paleoclimate was

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(2) Climate change in the Jiuquan Basin since the Miocene was associated with global climate change and the uplift of the Tibetan Plateau. Additionally, central Asian aridification and evolution of the monsoon from the uplift of the

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Tibetan Plateau influenced paleoclimate changes in the Jiuquan Basin. Therefore, the climate evolution in the Jiuquan Basin from 24 to ~8 Ma was mainly controlled by global climate change. Since ~8 Ma, the changes in clay-mineral contents in the Jiuquan Basin were affected by the uplift of the Tibetan Plateau and global cooling, and the uplift of the Tibetan Plateau played the dominant role.

Acknowledgments This work was cosupported by the Strategic Priority Research Program of the Chinese Academy of Sciences (Grant No. XDA2007020102), the Second Tibetan Plateau Scientific Expedition and Research (STEP) program (Grant No. 2019QZKK0707), and the National Natural Science Foundation of China (Grant Nos. 41872098 and 41902223). We are grateful to the Key Laboratory of Mineral Resources in Western China (Gansu Province) at Lanzhou

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University and our colleague Chunhua Hu for their assistance with the laboratory work. We are also grateful for the thorough and helpful comments from the editors and two anonymous reviewers, which helped us greatly improve the manuscript.

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Journal Pre-proof Conflict of Interest We declare that we have no financial and personal relationships with other people or organizations that can inappropriately influence our work, there is no professional or other personal interest of any nature or kind in any product, service and/or company that could be construed as influencing the

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position presented in, or the review of, the manuscript entitled.

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Highlights: 1 Clay minerals restore the Neogene cold-warm-cold climate of the Jiuquan Basin. 2 The Jiuquan Basin displayed a continuous aridification trend since ca. 14 Ma. 3 The cold-warm-cold climate from ca. 24 Ma to 8 Ma linked with global climate change.

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4 Colder and drier climate since ca. 8 Ma reflected the uplift of the Tibetan Plateau.