Journal of Archaeological Science 34 (2007) 2109e2114 http://www.elsevier.com/locate/jas Mass spectrometric U-series dating of Laibin hominid site in Guangxi, southern China Guanjun Shen a,*, Wei Wang b, Hai Cheng c, R. Lawrence Edwards c a College of Geographical Sciences, Nanjing Normal University, Nanjing 210046, PR China Natural History Museum of Guangxi Zhuang Autonomous Region, Nanning 530012, PR China c Department of Geology and Geophysics, University of Minnesota, Minneapolis, MN 55455, USA b Received 13 September 2006; received in revised form 25 January 2007; accepted 25 February 2007 Abstract The Laibin hominid represents one of the rare finds of modern Homo sapiens in China, rare for its relative completeness and well-established stratigaphic provenance. This paper presents the results of mass spectrometric U-series dating of intercalated calcite samples from the Laibin site. The capping flowstone and the calcite vein, which sandwich the hominid fossil-containing deposits, date to 38.5 1.0 and 44.0 0.8 ka, setting respectively the minimum and maximum ages to the fossils. The second flowstone layer is 112.0 1.4 ka old, indicating that the cultural sequence may possibly extend to somewhere between 44 and 112 ka. Securely dated Laibin finds should be of importance in reconstructing human physical and cultural evolution in the region. Ó 2007 Elsevier Ltd. All rights reserved. Keywords: Laibin hominid; Morphologically modern humans; U-series dating; Speleothem calcite; Late Pleistocene; Southern China 1. Introduction Qilinshan Hill is located at ca. 1.5 km north of Qiaogong Town in Laibin County, Guangxi Zhuang Autonomous Region, southern China (Fig. 1). This isolated peak of Permian limestone, which forms the characteristic landscape of the region, is ca. 45 m in height, and ca. 150 m east to west and ca. 110 m south to north. Its basement rock has experienced extensive karstic processes, resulting in numerous caves, some filled with fossil-containing detrital sediments. Gaitou cave (23 430 3500 N, 109 050 2900 E) is situated at the southern slope of the hill. The cavern is ca. 7 m above the present ground surface with an entrance facing south, ca. 2.7 m high and ca. 1.3 m wide. In January 1956, a field team led by the late archaeologist Lanpo Jia carried out a test excavation in the cave. A fragmentary hominid skull base was recovered together with tooth fragments of Cervus and Sus and a considerable amount * Corresponding author. Tel.: þ86 25 85891829; fax: þ86 25 85891347. E-mail address: [email protected] (G. Shen). 0305-4403/$ - see front matter Ó 2007 Elsevier Ltd. All rights reserved. doi:10.1016/j.jas.2007.02.008 of freshwater shells. Three lithic artifacts and a thin ash layer containing burnt bones were also found (Jia and Wu, 1959; Wu and Poirier, 1995). The Laibin specimen consists of three disconnected pieces: a nearly complete hard palate with several teeth and the adjoining lower part of the body of the maxilla, a large part of the right zygomatic and an occipital fragment, which are all grayish-white in color and moderately fossilized. Based on morphological studies, Jia and Wu (1959) concluded that ‘‘for lack of distinct archaic features, the hominid fossils from Qilinshan Hill should be taken as modern Homo sapiens’’. This attribution has been widely cited in the literature (e.g., Wu and Poirier, 1995). For about two decades, the time and location of the origin of modern H. sapiens has been the subject of an intensive debate mainly between the exponents of two competing hypotheses, ‘‘regional continuity’’ (e.g., Wolpoff et al., 1984, 2001) and ‘‘recent out of Africa’’ (e.g., Stringer and Andrews, 1988; White et al., 2003). The accurate dating of relevant finds is key to addressing the controversial issues. 2110 G. Shen et al. / Journal of Archaeological Science 34 (2007) 2109e2114 Fig. 1. Map showing the location of Gaitou cave, the burial site of Laibin hominid and neighboring hominid localities, Tongtianyan, Bailiandong, Ganqian and Dalongtan, which are discussed in the text. The validity of the U-series dating of pure and dense cave calcites has been well demonstrated (e.g., Ludwig and Renne, 2000; Richards and Dorale, 2003; Schwarcz, 1992). Mainly with this chronometer we have, in recent years, studied a number of modern H. sapiens localities in southern China, those in Guangxi including Liujiang (Shen et al., 2002b), Ganqian (Shen et al., 2001a) and Bailiandong (Shen et al., 2001b) caves. The results demonstrate that these sites, previously estimated at 20e30 ka, should be earlier Late Pleistocene in age, certain lower horizons may even be later Middle Pleistocene. The possibility of a much earlier appearance of modern H. sapiens in China than previously estimated will impact profoundly on the afore-mentioned debate. However, the above dating results also point to the necessity of further studies. The reason for this is that the Liujiang skull, though quite complete, is an amateur recovery. Its exact stratigraphic provenance can hardly be unequivocally fixed. This explains the general reluctance of the paleoanthropology community to accept the age dating, although we deem that the inferences involved in arriving at the new age assignments should be highly rational. At other sites we have studied, hominids are mostly known through isolated teeth, so their phylogenetic position cannot be assuredly defined. Moreover, the re-assignment of the above-mentioned sites to around 100 ka not only contrasts strongly with the previously accepted time-scale, but also leaves an important gap in the sequence of human occupation. To address these issues, we have been searching for more modern H. sapiens sites suitable for chronological studies. Laibin hominid came to our attention because it was found in the course of a well-organized excavation and from a wellestablished stratigraphic position, i.e. some 0.12 m below the capping flowstone (Jia and Wu, 1959). Moreover, judging by previous publications (Jia and Wu, 1959; Wu and Poirier, 1995), in spite of their incompleteness the hominid fossils are diagnostically significant to represent modern H. sapiens. Similar finds are rare among the inventory of fossil hominids in China. Thus precise dating of this specimen should be of importance. However, apart from relative age estimate at a late Paleolithic stage, no radiometric dating has ever been performed. Jia and Wu (1959) reported that the fossiliferous deposits of the site were interbedded with flowstone layers. We confirmed the existence of intercalated speleothem formations in the G. Shen et al. / Journal of Archaeological Science 34 (2007) 2109e2114 course of a field investigation. Several calcite samples were taken then and trial U-series measurements performed with classical alpha spectrometry. However, due to detrital contamination as reflected in rather low 230Th/232Th activity ratios, the results suffer from major uncertainty. To circumvent the difficulty, the raw samples were closely examined and it was found that thin sub-layers of quite pure and dense calcite exist in several of them. The purer portions were carefully picked out and analyzed with high precision inductively coupled plasma mass spectrometry (ICP-MS), yielding U-Th dates with much improved reliability. Subsequent fieldwork enabled collection of several more small (gram or sub-gram) and, therefore, purer samples. In this paper we present the U-series results of these samples and discuss their implications for human physical and cultural evolution in the region. 2. Samples in stratigraphic context The ca. 10-m deep cave consists of three parts: Outer Corridor, Inner Corridor and East Branch Corridor (Fig. 2). In the Outer Corridor only about 3 m3 of deposits near the eastern wall survived fertilizer mining, of which about 1 m3 was consumed by the test excavation in 1956 (Jia and Wu, 1959). The deposits inside the East Branch Corridor, consisting of brownish loose clay containing a few fossils, were almost completely dug out by the fertilizer miners. In contrast, about half of the 2111 deposits in the Inner Corridor remain intact, probably owing to the protection of a thick capping flowstone. The disturbed portions there show that the deposits under the capping flowstone are composed of brownish loose clay, containing some gravels but no fossils or shells. The present work is concentrated on the extant cross-section near the eastern wall in the Outer Corridor (line AB in Fig. 2), which is now represented by less than 1 m3 of deposits as the result of natural weathering processes. Jia and Wu (1959) gave a brief stratigraphic description, in which the depositional sequence was divided into two layers: a lower layer of consolidated red loam and an upper layer of slightly consolidated yellowish gray breccia. The upper layer was further divided into three sub-layers by intercalated thin flowstones. Having performed in situ stratigraphic studies, we deem it pertinent to redescribe the depositional sequence in more detail and to divide it into the following four layers (Fig. 3, numbers from top to bottom). 1. Capping flowstone, ca. 10 cm thick, brownish white, consisting of 3e5 sub-layers. 2. Sandy clay, 70e115 cm thick, brownish, moderately consolidated, containing fossils and gravels, shell-bearing except for the lowest ca. 20 cm. The deposits are intercalated with several thin and heavily muddy flowstone layers of limited extent. Its middle to lower sections are intersected by a calcite vein, presumably resulting from a partial washing-out and re-deposition event. Although no depositional hiatus is obvious, whether the lowermost shell-lacking deposits contain any trace of human activity remains unclear. 3. Second flowstone layer, 1e3 cm thick, brownish white. 4. Sandy clay, an exposed section of 40e60 cm with unknown total thickness, brownish, strongly consolidated, sterile, gravel-bearing. Samples QLS-6 and 7 were taken from localized 1e2-mm thick pure sub-layers of the capping flowstone, while QLS11 was taken from an overlying small stalagmite. QLS-12 and 16 represent the purest possible sub-layers of the calcite vein in Layer 2. QLS-9 was collected from the second flowstone layer, enclosed in which a tiny piece (ca. 0.2 g) of fossil bone was taken as QLS-5. QLS-17 is a fragment of deer tooth ca. 20 cm below the capping flowstone. The samples’ stratigraphic positions are shown in Fig. 3. It should be noted here that to avoid post-depositional calcite in small erosional cavities, only the purest possible portions with clear laminae and natural contact with their less pure surroundings were picked out for dating. 3. Dating results Fig. 2. Plane figure of Gaitou cave, showing the position of the Outer Corridor, Inner Corridor and East Branch Corridor. The present study is concentrated on the extant cross-section (line AB) near the eastern wall, where the hominid fossils were recovered in course of the test excavation in 1956. The samples’ 230Th/234U dates were determined with ICPMS (Finnegan Element) at the Minnesota Isotope Laboratory, University of Minnesota, USA except for QLS-5 and the dentine of QLS-17 which were measured with classical alpha spectrometry at the first author’s laboratory in Nanjing. The G. Shen et al. / Journal of Archaeological Science 34 (2007) 2109e2114 2112 Fig. 3. Sketch showing the preserved cross-section, corresponding to the line AB in Fig. 2. Samples for dating were collected from three speleothem horizons: capping flowstone, second flowstone and a calcite vein running from middle to lower sections of Layer 2. A sectional view of the calcite vein is given in the upper right inset. analytical procedure for ICP-MS measurements is shown in Shen et al. (2002a). The instrumental bias correction, 230Th and 234U half lives, standards and spikes used in age determinations are as discussed in Cheng et al. (2000). U-Th isotopic ratios and derived age results are presented in Table 1. In spite of our great carefulness in sample collection and pretreatment, the calcite specimens for ICP-MS determinations are still not sufficiently pure. This is shown by the 230 Th/232Th ratios between 5.4 and 31.1, which are not as high as expected. Nevertheless, for each of the three speleothem horizons, we have one 230Th/232Th ratio greater than Table 1 Mass spectrometric U-Th isotopic ratios and 15, high enough to ensure the reliability of the dates obtained. The general consistency between coeval samples with higher or lower 230Th/232Th ratios lends support to their reliability. The very young age of QLS-6 (7.9 0.2 ka) indicates recent speleothem formation in the cave. As the sample is located at the surface, no meaningful age constraint can be inferred from this date. QLS-7 and 11 from the capping flowstone yield dates consistent within errors with a weighted mean of 38.5 1.0 ka. Duplicated analyses on QLS-12 and 16 from the calcite vein all give consistent results with a weighted mean of 230 Th age results Sample number 238 230 234 230 230 Th age (ka) (corrected) QLS-6 QLS-7 QLS-11 QLS-12 QLS-12 QLS-16 QLS-16 QLS-9 QLS-17 QLS-17 QLS-5a 0.4461 0.0006 0.7557 0.0009 0.3200 0.0005 0.2180 0.0003 0.2892 0.0003 0.3135 0.0004 0.3012 0.0004 0.4753 0.0008 6.525 0.013 54.5 29.3 8.3 0.2 5.4 0.1 15.5 0.1 10.3 0.1 15.8 0.1 9.5 0.1 12.3 0.1 31.1 0.2 667 10 53.9 229.9 1.0284 0.0015 0.9204 0.0013 1.0366 0.0015 1.0500 0.0013 1.0341 0.0014 1.0269 0.0013 1.0275 0.0016 1.0377 0.0017 1.0516 0.0015 1.035 0.034 1.182 0.022 0.0873 0.0015 0.3061 0.0065 0.3207 0.0023 0.3445 0.0026 0.3570 0.0024 0.3718 0.0036 0.3540 0.0033 0.6755 0.0035 0.1019 0.0004 0.131 0.012 0.537 0.020 9.7 0.2 44.4 1.2 40.3 0.4 43.3 0.4 46.1 0.4 48.9 0.6 46.0 0.5 113.8 1.1 11.1 0.5 15 2 82 4 7.9 0.2 38.7 3.2 38.5 1.0 40.4 2.9 44.2 1.1 45.5 1.8 43.5 1.4 112.0 1.4 (I) (II) (I) (II) (enamel) (dentine)a U (ppm) Th/232Th U/238U Th/238U Th age (ka) 230 *All isotopic ratios are in activity, errors 2s. Decay constants used: l230 ¼ 9.1577 106 year1, l234 ¼ 2.8263 106 year1. Corrected 230Th ages assume the initial 230Th/232Th atomic ratio of 4.4 2.2 106, a value for a material with the bulk earth 232Th/238U atomic ratio of 3.8 at secular equilibrium, with an arbitrarily assumed error of 50%. The dates in bold are cited in the text. a Measured with alpha spectrometry at the first author’s laboratory in Nanjing. G. Shen et al. / Journal of Archaeological Science 34 (2007) 2109e2114 44.0 0.8 ka. As the hominid specimen was recovered from the deposits in-between, its age can be securely bracketed between 39 and 44 ka. The date on QLS-9 indicates that the second flowstone layer formed 112.0 1.4 ka ago, thus giving a maximum age to the overlying deposits. It should be noted here that due to the highly episodic deposition in caves and to the presence of an intervenient shell-lacking sub-layer, human occupation of the site may happen substantially later than the maximum age defined by the underlying flowstone layer. The deer tooth fragment QLS-17 comes from about the same horizon as the hominid fossils. Its enamel and dentine give broadly consistent dates of 11.1 0.5 and 15 2 ka respectively, much younger than indicated by the correlated flowstone layers. The bone fragment QLS-5 (82 4 ka) is also much younger than its encasing calcite (112.0 1.4 ka). These results are in line with our previous studies, which indicate that fossil bones are susceptible to post depositional U migration, leading generally to underestimated dates in a cave setting (Shen, 1996). 4. Discussion and conclusion In contrast to the hot debate about the origin of modern H. sapiens, only a small number of securely dated fossils are available for reconstructing recent human evolution in Africa (Shea and Fleagle, 2005). The situation should be about the same in China, if not worse, where only a small proportion of the relevant sites have been numerically dated. Classical 14 C and U-series determinations on fossil materials remain the most utilized chronometers, both however are known for limited reliability (Shen, 1996; Taylor, 1992). Besides, up to a few years ago important representatives of modern H. sapiens in China were all dated to less than 30 ka, and apparently there is a time gap of human presence between 40 and 100 ka (Stringer, 1988). Under such circumstances, a tight assignment of 39e44 ka to Laibin hominid bears important implications. First, the present results contribute a midpoint to the sequence of Late Pleistocene human evolution in the region. Laibin hominid represents modern people in craniofacial morphology. In neighboring areas there are three older hominid finds. The Liujiang skull is reported to be at least 68 ka old, most probably between 111 and 139 ka and possibly still older (Shen et al., 2002b). The Tubo hominid, represented by 17 fossil teeth, is bracketed in the range of 94 and 220 ka (Shen et al., 2001a). At Bailiandong an overlying flowstone layer sets a minimum age of 160 ka to the two hominid teeth (Shen et al., 2001b). Four more or less complete human skeletons recovered from the Dalongtan site represent younger specimens, to which 14C dating of charcoal grains assigned an age of ca. 10 ka (Zhou and Zhang, 1994). The pattern of human evolution will be clarified with the increasing number of reliably dated hominid finds. Second, except for the lowermost w20 cm the Layer 2 deposits are quite rich in freshwater shells, most of them of the species of Viviparus and Semisulcospira. To have an idea about the density, we arbitrarily chose an area of 50 by 50 cm and counted 63 shells. Shellfish gathering is widely 2113 accepted as an archaeological indication of modern behavior (Broadhurst et al., 2002). If finally proved to be the result of human activity, the shells buried in the deposits assuredly dated to older than 44 ka may represent the yet earliest record of systematic mollusk exploitation in China. Third, according to the previous temporal framework, no hominid remains in China are securely dated to the range of 40e100 ka (Stringer, 1988). Proponents of the out-of-Africa model consider that this marks an interruption when the aboriginal populations (H. erectus or archaic H. sapiens) in East Asia had died out and the oncoming African modern people were still on the way (e.g., Jin and Su, 2000). The hominid remains, stone artifacts and molluscan shells recovered from Gaitou cave, dated reliably to the range of 39e44 ka and possibly to somewhere between 44 and 112 ka, may be cited as a supporting evidence for an inhabited southern China during this time interval. This is in line with recent discoveries of stone artifacts in the deposits dated to w70 ka at Jingshuiwan in Chongqing (Pei et al., 2006) and to 55e110 ka in Zhangkou cave, Yunnan Province (Shen et al., 2005). The so-called fossil gap is likely nothing but an artifact due to systematic errors of dating techniques and should be further explored. In conclusion, Laibin hominid dates to the range of 39e 44 ka, while the cultural sequence of the site may possibly extend to somewhere between 44 and 112 ka. The present study marks one step forward in our effort to establish an integrated chronological sequence for recent human evolution in China. Further studies to date more modern hominid fossils are currently under way. Southern China provides a promising ground for research in this direction, as the region abounds in Late Pleistocene hominid sites in limestone caves, where cultural/fossiliferous deposits are often intercalated with speleothem formations. With the possibility of stringent temporal constraints, the hominid finds there will contribute fundamentally to elucidating the much-debated issues concerning the origin, dispersal and evolution of modern H. sapiens. Acknowledgements This project has been jointly supported by National Natural Science Foundation of China (40373031) and WennerGren Foundation (Gr. 6975). ICP-MS U-series analyses were supported by US NSF grants. We thank the government of Guangxi Zhuang Autonomous Region for permission, Dr James L. Bischoff and Dr Qian Wang for helpful discussions and two anonymous referees for constructive criticisms that improved clarity and consistency. 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