U-series dates in Yabrudian and Amudian layers at Qesem Cave, Israel

Quaternary International 398 (2016) 6e12

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New ESR/U-series dates in Yabrudian and Amudian layers at Qesem Cave, Israel res a, *, M. Richard a, O. Tombret a, Q. Shao b, J.J. Bahain a, A. Gopher c, R. Barkai c C. Falgue D epartement de Pr ehistoire, Mus eum national d'histoire naturelle, UMR7194, 1, rue Ren e Panhard, 75013, Paris, France Department of Geography Sciences, Nanjing Normal University, Nanjing, Jiangsu, China c Institute of Archaeology, Tel Aviv University, 69978, Tel Aviv, Israel a

b

a r t i c l e i n f o

a b s t r a c t

Article history: Available online 13 March 2015

Qesem Cave is a Middle Pleistocene site situated 12 km east of the Mediterranean coast of Tel Aviv, Israel. It is attributed to the Acheuleo-Yabrudian Cultural Complex (AYCC) of the late Lower Paleolithic period, dated to ca. 420e200 ka. This site exhibits a unique prehistoric sequence where the Amudian blade dominated industry is the main cultural component, however the scraper-dominated Yabrudian industry is also represented in distinct contexts at the cave. The chronology established by TL applied on burnt flints, ESR/U-series on herbivorous teeth and U-series on spelothems, suggests that Qesem Cave is one of the oldest sites yielding such a blade industry and a fully-fledged trajectory of Quina scrapers production. This work presents new ESR/U-series dates on four animal teeth unearthed from an Amudian central hearth recently published and four other teeth from a Yabrudian industry-bearing layer in the shelf area. The dates range from 249 to 296 ka for the Amudian hearth (mean age of 280 ka) and from 279 to 382 ka for the Yabrudian layer (mean age of 313 ka). These radiometric dates provide new information on the chronology of the Amudian and Yabrudian industries in the hearth and shelf areas and contribute towards a better understanding of the chronology of Qesem Cave as a whole. This is the first time we have direct dates from Amudian and Yabrudian context from a single site. © 2015 Elsevier Ltd and INQUA. All rights reserved.

Keywords: ESR/U-series Middle Pleistocene Qesem Cave Yabrudian Amudian Middle East

1. Introduction Qesem Cave, located in the Levantine corridor is one of the keysites for the understanding of human dispersal during the Middle Pleistocene. This site allows studies providing information on both the paleoenvironment and human behavior (e.g., Barkai et al., 2003; Lemorini et al., 2006; Stiner et al., 2009, 2011; Gopher et al., 2010; Maul et al., 2011, 2016; Mercier et al., 2013; ShahackGross et al., 2014; Blasco et al., 2014). Human dental remains at the cave exhibit affinities with the Anatomically Modern Human dental material from Qafzeh and Skhul caves in the northern part of Israel (Hershkovitz et al., 2011) as well as traits that may be assigned to Neandertals (for discussion see, Weber et al., 2016; Fornai et al., 2016; Sarig et al., 2016; Hershkovitz et al., 2016). The presence of both the Amudian and Yabrudian industries in the

* Corresponding author. res). E-mail address: [email protected] (C. Falgue http://dx.doi.org/10.1016/j.quaint.2015.02.006 1040-6182/© 2015 Elsevier Ltd and INQUA. All rights reserved.

same site provides a unique opportunity to constrain these two AYCC industries using radiometric dates. Previous U-series readings made on calcite, yielded a general chronological framework with maximum and minimum dates for the occupational levels of the cave (Barkai et al., 2003; Gopher et al., 2010). Recently, analyses performed on burnt flints using TL and on fossil enamel teeth using combined ESR/U-series method (Mercier et al., 2013) confirmed human bearing occupations during MIS 9 to MIS 7 for Amudian lithic artefacts in some specific areas of the site. Three dates (one flint and two teeth) suggest a possible earlier occupation during MIS 11. It is worthy of note that while the MIS 11 ca. 400 ka date for the beginning of the AYCC range is corroborated by TL, ESR and Useries dates from other sites (see Gopher et al., 2010 and references therein), the MIS 7 ca. 200 ka date for the end of the range might be debated. Following dates of Mousterian layers in the region as well as dates from other AYCC sites, the end of this range is usually set at a date somewhat earlier than 200 ka. A close look at the statements made using U-series dates of Qesem Cave indicates that we were cautious and said that “Occupation continued until between 220 and 194 ka, when the cave was altered to a degree that did not favour human occupation. A U-Series age of 218 ka for the

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speleothem fragment within the sediments below Q3 (see Barkai et al., 2003) may indicate occupation at this time also, or end of occupation and collapse causing this speleothem become broken” (Gopher et al., 2010: 653). We tend to think that the Qesem Cave occupation ended sometime closer to 220 ka than to 194 ka thus leaving a smaller “gap” between the end of the AYCC and the beginning of the Mousterian. Our study consists of dating new herbivorous teeth by the combined ESR/U-series method. The teeth originate from the central hearth assigned to the Amudian and from Yabrudian levels under the shelf (see Fig. 1 for location of samples areas of origin). Ages obtained for these two areas from similar elevations below datum, allow a chronological assessment of these two important lithic industries of the Acheuleo-Yabrudian Cultural Complex.

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2. Methods The combined ESR/U-series (US-ESR) model takes into account both ESR and U-series data including radioelement contents, isotopic ratios, palaeodoses and external gamma-dose rate allowing for the reconstruction of the uranium uptake history in each dental tissue using a specific U-uptake parameter (p-value) (Grün et al., 1988). The model cannot account for uranium loss. The relevance of the method was discussed in Grün (2009a). A new model combining ESR and U-series data (called the Accelerating uptake model, AU-ESR) allows an extension to samples exhibiting slight uranium leaching (Shao et al., 2012). The application of the combined approach has been used for dating of the entire Middle Pleistocene on both human and animal teeth (Grün, 2006; res et al., 2010). Falgue

Fig. 1. Location of the teeth analyzed in this study in the hearth and in the shelf area (1 and 2 blue squares respectively). Burnt flints and the teeth of similar elevations below datum frp, the Deep Pit Area published in Mercier et al., 2013 are shown in green circles and red squares respectively. In The K10 area, only flints were dated in the Mercier paper. The A and B areas correspond to the main areas were calcite samples were taken for U-series analyses. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

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3. Sample selection and preparation Two previously undated areas of Qesem Cave were selected for study and 8 herbivorous teeth were prepared for ESR/U-series analyses at the geochronology laboratory of department of Prehistory of National Museum of Natural history at Paris. Fig. 1 presents the locations of analysed samples in this study and also the previous dated samples at similar elevation in the “deep pit area”. To prevent confusion, the different names used for the excavated areas from which the samples were taken are marked on Fig. 1. The “shelf area” located in the western part of the cave provided four teeth from elevations 560e580 cm below datum in Squares F/ 9, F/10 and G/10. The “hearth area”, situated to the northeast of the “deep pit area” (between 2004 and 2006; enlarged to the south since 2010 and known as “The southern area” in other papers, e.g., Assaf et al., 2016; Parush et al., 2016, Gopher et al., 2016) provided four other teeth samples from elevations 555e590 cm below datum. The new data enlarge the scope of previous sampling of burnt flints and teeth performed from higher elevations in Squares K/10 and Squares L, M, N/13, 14, 15 between 375 and 545 cm below datum, and the “deep pit area” in the central part of the cave at elevations ranging between 550 and 750 cm below datum whose results were recently published (Mercier et al., 2013). Fig. 2 represents our samples among the samples already dated and contributing to the chronology of the site.

power of 1 mW and a modulation amplitude of 0.1 mT. A scan range of 10 mT and a scan time of two minutes with a modulation frequency of 100 kHz were used for each spectrum. Each ESR measurement was repeated four times for each dose. The equivalent doses (DE) were determined from the asymmetric enamel T1-B2 signal at g ¼ 2.0018 (Grün et al., 2008) by fitting a single exponential function (SSE) (Yokoyama et al., 1985). An exponential plus linear fitting was also used to check an eventual DE overestimation linked to the SSE use and yielded the same values but with a larger error range. ESR age calculations were carried out with the ESRDATA program of Grün, (2009b) which uses an alpha efficiency of 0.13 ± 0.02 (Grün and Katzenberger-Apel, 1994) and Monte-Carlo beta attenuation factors (Marsh, 1999) based on the thickness of tooth enamel and after removal of outer layers. In addition, the following parameters were used: - The water content was estimated to be 3 wt% in the enamel, 7 wt % in the dentine and in the cement, and 15 wt% in the sediment. - Gamma-ray spectrometry was used to determine the sediment radioisotopes U, Th and K in the areas having provided the teeth. The dose rate was calculated according to Adamiec and Aitken (1998). Teeth samples were chosen considering their proximity to the TL dosimeters which were inserted for the flints and teeth already analysed (see Mercier et al., 2013). - The effect of Ra and Rn loss in each tissue was determined by combining alpha-ray and gamma-ray measurements (Bahain et al., 1992).

4. Measurements 5. Results Enamel, dentine and cementum were separated mechanically and their radioisotope contents measured by U-series using standard methods of alpha-ray spectrometry (Bischoff et al., 1988), and gamma-ray spectrometry (Yokoyama and Nguyen, 1980). A part of the enamel, after cleaning of its surface on both inner and outer sides in order to eliminate the effect of external alpha radiation, was ground, sieved and the 100e200 mm fraction split into 10 aliquots. Nine of the ten were irradiated with a calibrated 60Co gamma-ray source from 200 to 8000 Gy. ESR measurements were performed at room temperature on an EMX-6 Bruker spectrometer (X band, 9.82 GHz) with a microwave

Table 1 presents the main data necessary for the calculation of combined ESR/U-series ages. The uranium content in the different tissues constituting the teeth samples varies from 0.11 to 4.70 ppm in the enamel and from 4 to 72 ppm in the dentine. In the enamel the uranium content is about twenty times lower in the hearth area samples than in the shelf area, and about 10 times lower in the dentine. On the other hand, a remarkable homogeneity of the DE values ranging between 150 and 167 Gy is observed in the hearth area samples while in the shelf area they vary much more (between 350 and 610 Gy). The isotopic ratios are all comprised in the general

Fig. 2. All kind of dated samples are presented in this figure versus the depth. Brown squares correspond to U-series dates performed in A and B areas (Gopher et al., 2010), Green circles and red triangles represent burnt flints and teeth dated by Thermoluminescence and ESR/U-series respectively 5Mercier et al., 2013. Blue triangles show the samples analysed in this paper. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

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below datum) may be older, ranging between 300 and 400 ka. QC1002 shows unusual uranium content (the lowest content in enamel and the highest in the dentine) with the lowest DE value for the shelf. These data suggest that this sample underwent a complex

values even though some are accompanied by a large error range when uranium content is very low, like in the case of enamel tissue. Table 2 presents the uptake parameters for each tissue, the different contribution doses, and the ages obtained for each sample.

Table 1 ESR and U-series data on fossil herbivorous teeth from Qesem Cave. Italicised values less than one likely underwent geochemical problems (this is the case for QC1005 E and for QC1008 E). Sample

Depth (cm)

Square

Tissue

U (ppm)

234U/238U

Hearth QC1006

555e560

J13d

QC1007

560e570

J13d

QC1005

580e585

J13a

QC1008

585e590

J13d

E D E D E D E D

0.26 7.81 0.23 7.25 0.17 3.97 0.11 4.02

1.233 1.130 1.148 1.159 0.941 1.140 0.905 1.123

± ± ± ± ± ± ± ±

0.092 0.023 0.149 0.032 0.104 0.031 0.174 0.065

0.836 0.874 0.765 0.916 0.696 0.803 0.683 0.801

± ± ± ± ± ± ± ±

Shelf QC1003

555e560

G10c

QC1004

560e565

G10c

QC1001

575e580

F9b

QC1002

575e580

F10d

E D E D E D E D

4.68 60.04 4.56 54.81 4.29 36.31 0.79 72.04

1.305 1.260 1.185 1.184 1.257 1.263 1.329 1.255

± ± ± ± ± ± ± ±

0.001 0.001 0.022 0.019 0.019 0.016 0.056 0.014

0.865 0.930 0.739 0.891 0.825 0.847 0.704 0.812

± ± ± ± ± ± ± ±

222Rn/230Th

T enamel (mm)

Removed enamela (mm)

DE (Gy)

0.069 0.030 0.126 0.039 0.096 0.033 0.165 0.048

1.00 0.46 1.00 0.28 1.00 0.66 1.00 0.66

1290

129/51

167 ± 5

1543

64/62

162 ± 6

1175

144/69

166 ± 7

1269

108/90

149 ± 3

0.01 0.01 0.020 0.041 0.018 0.030 0.039 0.034

0.77 0.31 1.00 0.30 0.25 0.35 0.38 0.33

795

87/33

610 ± 22

1296

143/48

459 ± 26

1467

159/70

397 ± 11

1161

41/39

349 ± 10

230Th/234U

E ¼ enamel, D ¼ dentine, C ¼ cementum. Uncertainties for isotopic ratios are given with ±1sigma. The initial (T) and removed enamel thickness are used for the age calculation. a the first number corresponds to the enamel subtracted in the dentine-enamel side; the second number to the cementum (sediment)-enamel side.

Table 2 Components of dose-rates for US or CAM models of teeth and sediment, and ESR-US age estimates with correspondent p-values for fossil teeth from Qesem Cave. Italicised values less than one likely underwent geochemical problems (this is the case for QC1005 E and for QC1008 E). Units Samples Depth (cm) Hearth QC1006 QC1007 QC1005 QC1008 Shelf QC1003 QC1004 QC1001 QC1002

Square (bþg) sediment þ cosmic Internal dose rate (a þ b) (mGy/a) enamel (mGy/a)

Total dose rate (mGy/a)

U-uptake parameter p or n Enamel

Dentine 0.84 0.89 0,73 0.59

± ± ± ±

ESR/U-series age (ka) US or CAM

555e560 560e570 580e585 585e590

J13d J13d J13a J13d

557 529 649 505

± ± ± ±

35 33 46 35

103 86 51 34

± ± ± ±

13 14 7 7

660 615 700 539

± ± ± ±

37 37 47 35

0.71 0.46 0.44 0.18

± ± ± ±

0.21 0.54 0.43 0.97

555e560 560e565 575e580 575e580

G10c G10c F9b F10d

332 315 399 486

± ± ± ±

20 25 28 35

1854 1308 897 511

± ± ± ±

240 280 200 115

2186 1623 1296 997

± ± ± ±

255 294 207 124

0.75 0.39 0.60 0,07

± ± ± ±

0.05 0.0047 ± 0.001 279 0.22 0.85 ± 0.14 283 0,13 0.66 ± 0.13 307 0.28 0.44 ± 0.19 382

0,09 0.10 0.11 0.17

279 296 249 295

þ þ þ þ

23/21 27/26 23/21 24/22

± 31 þ 49/46 þ 41/38 þ 45/42

For QC1003, a mixed p-value for enamel and n-value for dentine were determined for calculating the combined age. External dose-rates correspond to both sediment dose and cosmic dose (b þ g). Two types of measurements have been performed. About 100 g of sediment including rock fragments when they are present, were measured at least one month after it has been inserted in a box. Sediments have been sampled in the same square and at the same height as the teeth. TL dosimeters have been placed in different levels at the exact location of the analyzed sediments. All samples lack cementum tissue, and thus the enamel was directly in contact with the sediment.

Teeth from the hearth area exhibit homogeneous results suggesting a similar behavior concerning uranium uptake. Results were obtained using the ESR-US model with p-values ranging between 1 and 0 both for dentine and enamel tissues. The ages obtained range between 250 and 300 ka showing a good reproducibility and are likely close to the real ages. Data obtained on teeth extracted from the shelf area are more heterogeneous, showing ages increasing with depth below datum. All ages were calculated using the US-ESR model except for sample QC1003 for which uranium uptake dentine parameter, n, was determined by the AU-ESR model (Table 2). The two highest samples in the shelf area (555e565 cm below datum) are coeval with those of the hearth area and show the highest annual dose rate due to a strong internal dose rate. The two deeper teeth (575e580 cm

geochemical history. However, all p-values range between 0 and 1. They can be linked with samples of the “deep pit area” dated previously which gave ages older than ~350 ka, possibly indicating an older occupation of the site during MIS 11 and/or 10. 6. Discussion Fig. 3 shows a cumulative Gaussian curve of samples extracted in the two areas presented in this paper (The hearth and The shelf) as well as samples from the deep pit area (Mercier et al., 2013). These dates illustrate a clear mode at ca. 300 ka and another, smaller mode at around 400 ka. The older, nearly 400 ka, date from the shelf samples joins the 400 ka mode (Fig. 2) together with one burnt flint and two teeth presented and discussed in Mercier et al. (2013). Concerning the

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Fig. 3. Ages obtained in this study (red and blue diamonds), flints and teeth coming from Deep Pit Area (green and yellow diamonds) are presented with a one sigma error range. A cumulative gaussian curve shows a clear distribution mode around 300 ka for most of samples and a second lower peak near 400 ka. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

flint sample from the “deep pit area”, its elevation (580 cm below datum) plays in favor of a reworked sample as suggested in Mercier et al. (2013). Here, in the shelf area too, albeit the fact that the ages increase with depth, the fact that the two older dates are from the same elevation indicates a disturbance that we have no detailed reconstruction for, as was the case in the “deep pit area” (Mercier et al., 2013). However, the presence of burnt flint and animal's teeth dated to ca. 400 ka as well as U-series dates of a similar order (Gopher et al., 2010) confirm the eventuality of great antiquity suggested for the beginning of the sequence at Qesem Cave. The series of dates showing a mode ca. 300 ka presented here, augmented by similar TL, ESR and U-series dates presented in Gopher et al. (2010) and Mercier et al. (2013) are important as they represent both the central, repeatedly used hearth as well as Amudian and Yabrudian layers. The eventual contemporaneity around ca. 300 ka of the samples extracted from the sediments of the hearth and the two (or three) samples from the Yabrudian of the shelf area (Fig. 2) has two significant bearings on the dating of Qesem Cave:  First, the antiquity of the central hearth is confirmed by direct dating of samples taken from its sediments;  Second, since the hearth is assigned to the Amudian and the samples under the shelf originate from the Yabrudian, this

seems to indicate a general contemporaneity of the deposition of sediments bearing the two industries. It is beyond the scope of this paper to go into a detailed discussion on the meaning of AYCC variability and the quality of relationships between the three industries it comprises (e.g., Jelinek, 1982, 1990; Copeland, 1983). Past interpretations of this variability, mainly based on lithic analysis were centered on two major lines:  One, mainly held by pioneering researchers who viewed these industries as reflections of distinct past cultural groups (or cultures, e.g., Rust, 1950; Garrod, 1956).  And two, that the three industries are components of a single cultural complex (Jelinek, 1990; Copeland, 2000) that co-appear in the same layers being only spatially differentiated [as is the case at Qesem (Barkai et al., 2009)]. The idea of different groups (cultures) is unacceptable following the dating results presented here and technological analyses of Qesem Cave lithics confirming that both Amudian and Yabrudian share the same technological framework as shown for blades (Shimelmitz, 2009; Shimelmitz et al., 2016), side (Quina) scrapers (Lev, 2010), and for recycling trajectories (Parush et al., 2014a;

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Fig. 4. Samples dated at Qesem Cave. In brown, calcitic samples yield ages ranging between 200 and 420 ka. In green and red, the dates published in Mercier et al., 2013 showing ages around 250e300 ka with some older dates at 400 ka. In blue, dates obtained in this paper exhibiting also a mean age around 280 to 310 ka with some older dates around 380 ka. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Parush et al., 2016; Assaf et al., 2014b; Assaf et al., 2016) with difference only in relative frequencies of the different categories in each industry. Moreover, use-wear studies confirm a possible functional division between the 'contemporary' Yabrudian and Amudian of the elevations of the hearth (between ca. 555 and 590 cm below datum) (Lemorini et al., 2015; Lemorini et al., 2016; Zupanchich et al., 2016). The inescapable conclusion is that the variability between Amudian and Yabrudian is neither chronological nor group (culture)-related. The two industries seem to have been two manifestations of the same inhabitants of Qesem Cave reflecting different activity areas. 7. Conclusions The new radiometric data obtained for Qesem Cave teeth both from the shelf and the hearth areas reflect human bearing occupations ca.300 ka of both Amudian, including the hearth, and Yabrudian. They are in agreement with the ages obtained by Useries on calcite speleothems and additional TL and ESR dates. Amudian may thus be seen as contemporaneous with the Yabrudian at Qesem Cave at ca. 300 ka. Recognizing the small sample size of readings, some problems with the contexts, and all other limitations, this general contemporaneity between Amudian and Yabrudian is very significant in explaining intraAYCC variability. Human bearing layers at Qesem Cave were dated by U-series and described as unambiguously ranging between 320 and 245 ka (Gopher et al., 2010). However, the range of dates available for Qesem Cave is 420 to ca. 200 ka, with human occupation starting in MIS 11 (Fig. 4). This may push back the limit of the late Lower Paleolithic Acheulian of the Levant to older than 400 ka [for a discussion on Lower Paleolithic (Acheulian) and Middle Paleolithic (Mousterian) chronology, see Gopher et al. (2010)]. Future radiometric dating at Qesem Cave is clearly going to be oriented towards studying specific contexts in detail and the case of the hearth area (as well as the case of Square K/10 (see Mercier et al., 2013)) is very encouraging. References Adamiec, G., Aitken, M.J., 1998. Dose-rate conversion factors: update. Ancient TL 16, 37e50.

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