1. bookAHEAD OF PRINT
Journal Details
License
Format
Journal
First Published
04 Jul 2007
Publication timeframe
1 time per year
Languages
English
access type Open Access

Chronology of the Huxushan Paleolithic site in south China: Inferred from multiple luminescence dating techniques

Published Online: 25 Mar 2021
Page range: -
Received: 16 Feb 2019
Accepted: 09 Feb 2021
Journal Details
License
Format
Journal
First Published
04 Jul 2007
Publication timeframe
1 time per year
Languages
English
Abstract

The Huxushan archaeological site in northern Hunan Province, China, was recently excavated, from which stone tools including handaxes were unearthed. The deposits of the site are chemically weathered, which makes it difficult to date the site using numerical dating techniques except for optically stimulated luminescence (OSL) method. Here, we used various luminescence procedures including single-aliquot regenerative-dose (SAR), sensitivity-corrected multiple-aliquot regenerative-dose (SMAR) and thermally transferred optically stimulated luminescence (TT-OSL) SAR procedures on fine-grained quartz, and two-step post-infrared infrared stimulated luminescence (pIRIR) and multi-elevated-temperature pIRIR (MET-pIRIR) procedures on fine polymineral fractions. The results show that the fine quartz grains have excellent luminescence properties and the quartz SAR-, SMAR- and TT-OSL ages for the samples agree with each other and in stratigraphical order except for one sample. The fine polymineral fractions exhibited relatively weak pIRIR and MET-pIRIR signals, resulting in difficulty in constructing the dose-response curve for MET-pIRIR signals and the stratigraphically inconsistent pIRIR(100, 275) ages. The seven samples yielded their quartz OSL ages ranging from about 62 ka to 133 ka. The two samples from the cultural layer was dated to 78 to 92 ka using different procedures on fine quartz . However, given the systematically older pIRIR ages obtained with the fine polymineral grains for the two samples, their quartz OSL ages are considered to represent the minimal ages of this layer, and their pIRIR(100, 275) ages of 118 and 110 ka represent the upper age limit, indicating that the site was occupied by hominins during Marine Isotope Stage 5.

Keywords

Introduction

In recent years, substantial progress has been achieved in the discoveries and studies of the Chinese Paleolithic, especially for the Late Pleistocene period (Lu et al., 2011; Sun et al., 2012; Gao, 2013; Liu et al., 2015; Zhang et al., 2018). The fact that numerous open-air Paleolithic sites have recently been found and excavated in south China implies that south China plays a pivotal role in understanding the origin and prehistory of humanity in East Asia (Liu et al., 2008; Zhu et al., 2008). In addition, according to genetic studies (Chu et al., 1998; Piazza 1998; Wang and Li, 2013), south China is also the possible gateway for hominin to migrate into the hinterland of China, and thereby more detailed analyses of Paleolithic sites in south China are of great archaeological significance. However, it is hard to construct their chronological framework, because an intensive chemical weathering of the deposits results in the lack of suitable materials for numerical dating such as radiocarbon dating.

Optically stimulated luminescence (OSL) dating provides an estimate of the time elapsed since luminescent minerals, such as ubiquitous quartz or feldspar, were last exposed to sunlight (Huntley et al., 1985; Aitken and Smith, 1988), and it directly determines the burial ages of sediments. This method has already been extensively applied to Paleolithic archeology (Slimak et al., 2011; Roberts et al., 2015; Li et al., 2017; Hu et al., 2019). Various procedures have been developed to measure equivalent dose (De) of dated materials, including single-aliquot regenerative-dose (SAR) (Murray and Wintle, 2000), sensitivity-corrected multiple-aliquot regenerative dose (SMAR) (Zhou and Shackleton, 2001; Lu et al., 2007) and thermally-transfer SAR (TT-OSL SAR) (Wang et al., 2006) procedures on quartz, and post-infrared infra-red stimulated luminescence (pIRIR) (two-step pIRIR and multi-elevated-temperature pIRIR (MET-pIRIR)) procedures on potassium feldspars (Thomsen et al., 2008; Thiel et al., 2011; Li and Li, 2011, 2012a, 2012b).

In this paper, we used the above procedures on the fine-grained quartz and polymineral fractions of seven samples from the Huxushan Paleolithic site in northern Hunan Province, China. The luminescence ages obtained using the procedures were compared to evaluate their reliability, and the chronology of the site was established.

Geomorphology, stratigraphy and archaeology

The Paleolithic site of Huxushan (28°56′20″N, 112°17′22″E) is located at the Chishan Island surrounded by the Dongting Lake in the northern part of Hunan Province, China (Fig. 1a). The Dongting Lake, located in the middle reach of the Yangtze River, is the second largest freshwater lake in China. The Lishui, Yuanjiang and Zishui rivers in the study area discharge water into the lake from the northwest, west and south, respectively. The length and width of the island are about 30 and 4 km, respectively. The elevation of the island is between 30 m above sea level (asl) in the north, and 80 m asl in the south. The covering sediments are characterized by the great thickness of red earth. The region is located in the humid subtropical monsoon climate zone, and has an annual mean precipitation of 1322 mm and the mean monthly temperature ranging from 4.3°C (January) to 29.1°C (July).

Fig. 1

(a) Map showing the location of the study site, and (b) photograph of the excavation pit showing the stratigraphy and the positions of OSL samples.

The Huxushan site is situated on the western gentle slope of a hill, and is one of the discoveries in this region during the archeological survey in 2016 led by archeolo-gist Yi-Yuan Li from the Institute of Cultural Relics and Archeology of Hunan Province. The area of 350 m2 of the site has been excavated, and the deposits are divided into five layers numbered 1 to 5, from top to bottom (Fig. 1b). Layer 1 (0.2–0.8 m thick) is topsoil consisting of grey-yellow silty clay disturbed by human activities. Layer 2 (0.8–1.0 m thick) is composed of reddish-brown silty clay. Layers 3–5 comprise mottled red clay with worm-or net-like white stripes. Layer 3 (0.5–1.2 m thick) is reticulate red silty clay that is characterized by light yellow veins and massive Fe-Mn nodules. Layer 4 (2.0–2.5 m thick) consists of dark reddish-brown reticulate silty clay with a few Fe-Mn nodules. Layer 5 (0.4–0.5 m thick) is composed of deep reddish reticulate silty clay with short and thick white veins.

Stone artifacts were unearthed largely from Layer 3 and a few from the lower part of Layer 2 and the upper part of Layer 4. Raw materials in excavated assemblages are mainly comprised of quartz sandstone, quartz, siliceous limestone, quartzite and relatively small quantities of chert. We deduce that the raw materials were from the adjacent rivers because of the consistency in lithological characteristics and sedimentary types between the raw materials and the gravels found in the modern rivers. The stone artifacts include cobbles (manuports), cores, flakes and tools, suggesting a suit of incomplete technological assemblage. The sizes of lithic assemblage primarily have large tools and a few small productions such as flakes and scrapers. The cores are mainly composed of ordinary cores including single, dual or multiplatform and the others are discoidal and multi-faced. The flakes reflect low efficiency in using raw materials. The stone tools include chopping tools, picks, hand axes and heavy scrapers. Of these tools, though heavy tools are dominated, the number of picks and hand axes are relatively few but they are typical. The picks are triangular and tongue-shaped. The hand axes are made of siliceous breccia with delicately bifacial retouching.

Methods
Sampling and sample preparation

Seven sediment samples were collected from the stratigraphic profile of the south wall of the excavation pit for luminescence dating at the Luminescence Dating Laboratory of Peking University. The samples were taken by hammering stainless steel tubes (5 cm in diameter and 20 cm in length) horizontally into the vertical wall of freshly cleaned exposures. The tubes were then covered with aluminum foil and sealed with opaque tape.

Sample preparation for De determination was done under subdued red light in the dark room using the procedure described in Zhang and Zhou (2007). Carbonates in the samples were dissolved in 10% HCl acid, and organic matter was oxidized in 30% H2O2. The samples were then separated by wet sieving to attempt to obtain medium-grained (45–63 μm) fractions, but failed to obtain enough amount of the grains for De measurements. The polymineral fine (4–11 μm) grains were obtained by settling after Stokes’ Law. To obtain fine-grained quartz, some of the polymineral fine-grained fractions obtained were further purified with silica saturated fluorosilicic acid (H2SiF6) for three days followed by treatment with 10% HCl to remove any fluorides produced. The purity of the quartz extracts was checked by infrared stimulation followed by an OSL measurement. The IRSL signals detected were less than 0.1% of the OSL signal for all seven samples, indicating that feldspar contaminants were completely removed. The fine quartz and polymineral grains were respectively dispersed in acetone and then deposited onto 0.97 cm diameter aluminum discs for De measurements.

Equivalent dose determination

All luminescence measurements were performed in an automated Risø TL/OSL-20 luminescence reader. Irradiations were carried out using a 90Sr/90Y beta source equipped in the reader. Quartz grains were stimulated using blue LEDs (λ = 470 ± 30 nm), and the OSL signal was detected using an EMI 9235QA photomultiplier tube (PMT) with a 7.5 mm Hoya U-340 filter in front. Polymineral grains were stimulated using IR diodes (λ = 870 ± 40nm) with the IRSL signal collected through the same PMT with a Schott BG39/Corning 7-59 filter combination in front (Bøtter‒Jensen et al., 2003).

Three procedures in Table 1 were employed to determine the equivalent dose of quartz extracts. In the SAR protocol (Murray and Wintle, 2000, 2003), regenerative beta doses include a zero-dose used for monitoring recuperation effects and a repeat of the first regeneration dose used for checking the reproducibility of the sensitivity correction (i.e. recycling ratio). Test doses were irradiated immediately after measuring natural or regenerative-dose OSL signals (Li) to produce the OSL signal (Ti) for correcting sensitivity changes due to preheating/OSL measurements. De value is obtained by projecting the corrected natural OSL intensity (LN/TN) onto the dose-response curve (DRC) constructed using the corrected regenerative-dose OSL intensity (Li/Ti). Preheat of 250°C for 10 s (determined from preheat plateau tests, see the following section) and a cut-heat of 160°C were applied. A 280°C blue LED stimulations for 40 s was conducted at the end of each round of the measurement to reduce recuperation. The SMAR protocol (Zhou and Shackleton, 2001; Lu et al., 2007) was also used for the quartz extracts under the same conditions as in the SAR protocol. Six regeneration doses were performed, and their corrected OSL signals were used to construct DRC. Three aliquots were used for each regeneration dose.

Protocols used for De measurements of fine quartz grains.

Step OSL-SAR protocolObservedStep OSL-SMAR protocolObservedStep TT-OSL SAR procedureObserved
1 Give dose, DiPart 1 Detection of natural OSL signalPart 1 Detection of thermal-transferred OSL signal
2 Preheating at 250°C for 10 s1-1 Preheating at 250°C for 10 s1-1 Give dose, Di
3 Blue stimulation at 125°C for 40 sLi1-2 Blue stimulation at 125°C for 40 sLn1-2 Preheating at 250°C for 10 s
4 Give test dose, Dt (18.3 Gy)1-3 Give test dose, Dt (18.3 Gy)1-3 Blue stimulation at 125°C for 300 s
5 Cut heat at 160°C for 5 s1-4 Cut heat at 160°C for 5 s1-4 Preheating at 250°C for 10 s
6 Blue stimulation at 125°C for 40 sTi1-5 Blue stimulation at 125°C for 40 sTn1-5 Blue stimulation at 125°C for 40 sLTTOSL
7 Blue stimulation at 280°C for 40 sPart 2 Detection of regenerative OSL signal1-6 Give test dose, Dt (18.3 Gy)
8 Return to step 12-1 Bleaching at 125°C for 60 s1-7 Cut heat at 160°C for 5 s
2-2 Give dose, Di1-8 Blue stimulation at 125°C for 100 sTTTOSL
2-3 Preheating at 250°C for 10 sPart 2 Detection of basic-transferred OSL signal
2-4 Blue stimulation at 125°C for 40 sLi2-1 Annealing to 300°C for 10 s
2-5 Give test dose, Dt (18.3 Gy)2-2 Blue stimulation at 125°C for 100 s
2-6 Cut heat at 160°C for 5 s2-3 Preheating at 250°C for 10 s
2-7 Blue stimulation at 125°C for 40 sTi2-4 Blue stimulation at 125°C for 100 sLBTOSL
2-5 Give test dose, Dt (18.3 Gy)
2-6 Cut heat at 220°C for 10 s
2-7 Blue stimulation at 125°C for 100 sTBTOSL
2-8 Blue stimulation at 280°C for 100 s

Note that Di=0 when measuring natural signals.

In order to check the upper age limit of the quartz OSL-SAR and OSL-SMAR methods for our samples, the samples were also measured using the TT-OSL procedure proposed by Wang et al. (2006) (Table 1). The TT-OSL can be separated into two parts, the recuperated OSL (Re-OSL) and basic transferred OSL (BT-OSL). It is shown that the Re-OSL signal continues to grow with increasing dose up to 20, 000 Gy, while this is not the case for the BT-OSL signal. Using the equation LRe-OSL = [LTT-OSL/TTT-OSL] ‒ [LBT-OSL/TBT-OSL], Wang et al. (2006) showed that the ages for loess using both the OSL signal and the Re-OSL signal were consistent from modern to ~ 130 ka, demonstrating that Re-OSL could be used for dating. Here six aliquots were measured to obtain the intensity of natural TT-OSL (LTT-OSL) and basic transferred OSL (LBT-OSL), respectively. Test doses were used immediately to obtain TTT‒OSL and TBT‒OSL signals in exactly the same way as in the SAR protocol. The Re-OSL De value was then obtained by projecting the corrected natural LRe-OSL intensity to the DRC constructed using the corrected regenerated LRe-OSL intensities. For quartz extracts, the initial 0.64 s signal minus the last 3.2 s integral as a background in the decay curves was used for dose calculation.

Two procedures listed in Table 2 were used to determine the equivalent doses of the polymineral fine grains. In the MET-pIRIR protocol proposed by Li and Li (2011, 2012a), the preheat of 320°C for 60 s was applied after both regenerative and test dose to clear great influence from residual signals from measurements (steps 7 and 14). The regenerative and test dose IRSL signals after preheat were measured for 100 s at stimulated temperatures of 50, 100, 150, 200, 250, 290°C, respectively. A 100 s IR bleaching at 325°C was applied at the end of each cycle to clear recuperation. The two-step pIRIR protocol was also employed to determine the equivalent doses of the fine-grained polymineral fractions (Thomsen et al., 2008; Thiel et al., 2011; Buylaert et al., 2012), in which the polymineral aliquots were preheated at 320°C for 60 s, and IR stimulation time is 200 s. The first IR stimulation temperature was 100°C (IRSL signal) determined by De plateau tests (see the following section for details) (Li and Li, 2012a), and the subsequent IR stimulation temperature was 275°C (post-IR IRSL signal, pIRIR(100, 275)). The IR clean-out at the end of each SAR cycle was carried out at 325°C for 200 s. The first 2 s signal minus a background estimated from the last 50 s in the decay curves was used for dose calculation. It is noted that the experiments for anomalous fading and residual doses were not carried out (see the following section for details).

Procedures used for De measurements of fine polymineral grains.

StepMET-pIRIR procedureObservedStepTwo-step pIRIR procedureObserved
1Give dose, Di1Give dose, Di
2Preheating at 320°C for 60 s2Preheating at 320°C for 60 s
3Infrared stimulation at 50°C for 100 sLx(50)3Infrared stimulation at 100°C for 200 s
4Infrared stimulation at 150°C for 100 sLx(150)4Infrared stimulation at 275°C for 200 sLi
5Infrared stimulation at 200°C for 100 sLx(200)5Give test dose, Dt (91.5 Gy)
6Infrared stimulation at 250°C for 100 sLx(250)6Cut heat at 320°C for 60 s
7Infrared stimulation at 290°C for 100 sLx(290)7Infrared stimulation at 100°C for 200 s
8Give test dose, Dt (91.5 Gy)8Infrared stimulation at 275°C for 200 sTi
9Preheating at 320°C for 60 s9Infrared stimulation at 325°C for 200 s
10Infrared stimulation at 50°C for 100 sTx(50)10Return to step 1
11Infrared stimulation at 150°C for 100 sTx(150)
12Infrared stimulation at 200°C for 100 sTx(200)
13Infrared stimulation at 250°C for 100 sTx(250)
14Infrared stimulation at 290°C for 100 sTx(290)
15IR bleaching at 325°C for 100 s
16Return to step 1

Note that Di=0 when measuring natural signals

Dose rate measurements

The annual dose estimation was based on U, Th and K concentrations. U and Th concentrations were determined by laser ablation inductively coupled plasma mass spectrometer (ICP‒MS), and K concentrations were determined by a Wavelength Dispersive X-Ray Fluorescence spectrometer. Water contents (weight water/dry sediment weight) for all samples were measured in the laboratory, but the experiment results (13–14%) were probably lower than the natural values since the sediment section had been exposed to air for a long time. Therefore, we prefer to use a higher value of 23% obtained by similar samples from the Fengshuzui site (Zhang et al., 2018) close to the studied site. U, Th, K and water contents were assumed to have an uncertainty of 5% to cover analytical errors. The cosmic ray contribution for each sample was calculated as a function of depth, altitude, and geomagnetic latitude (Prescott and Hutton, 1994). The α-efficiency was taken as 0.04 ± 0.02 for quartz and 0.08 ± 0.02 for polymineral grains, respectively (Lai and Brückner, 2008). Finally, annual dose rates and ages were calculated using the DRAC calculator (v1.2) (Durcan et al., 2015).

Results
Luminescence properties and ages of quartz extracts

Examples of quartz OSL decay curves and SAR- and SMAR-OSL DRCs for our studied samples are illustrated in Fig. 2. Note that the DRCs for all samples were fitted with a single exponential saturation (SE) or saturating exponential plus linear function (SEPL) using the Risø luminescence Analyst version 4.53 software. The shine-down curve indicates that the quartz natural OSL signal is reduced to 4.3% of its initial intensity after 0.96 s of blue simulation at the sample temperature of 125°C, demonstrating that the quartz grains are very bright, and the OSL signal is dominated by the fast component. The DRCs demonstrate that the OSL signals are not saturated at a dose up to about 1000 Gy, and have the characteristic saturation doses (D01 and D02) of 35 and 464 Gy, if the curve is fitted with a double saturating exponential function. The shapes of the SAR- and SMAR-OSL DRCs are identical when regeneration dose is less than about 400 Gy if errors are considered. The recycling ratios for all samples using the SAR protocol are within the range of 1.0 ± 0.1 and the recuperation less than 5%, suggesting that the sensitivity correction for these samples is successful and thermal transfer negligible.

Fig. 2

Comparison of dose-response curves constructed using the quartz OSL-SAR and OSL-SMAR protocols for sample L3481. The inset shows a natural decay curve for the same aliquot.

Preheat plateau tests were carried out to determine a suitable preheat temperature for quartz aliquots. The De values of aliquots from sample L3478 were measured using the SAR procedure in Table 1 with different preheat temperatures ranging from 180 to 280°C at 20°C increments. Three aliquots were measured at each preheat temperature. The results shown in Fig. 3a indicate that there is no dependency on De values on preheat temperature in the range of 200–280°C. The recycling ratios are within the range of 0.9 to 1.1, and the recuperation is less than 2% for all samples (Fig. 3b), indicating that the preheat temperatures of 200–280°C are suitable for De determination on the quartz aliquots.

Fig. 3

(a) Plot of De values as a function of preheat temperature in the range of 180 and 280°C at 20°C increments for sample L3478, and (b) recycling ratios and recuperation against preheat temperature. Three aliquots were determined at each preheat temperature.

Dose recovery tests were also performed on the same sample as used in the preheat plateau tests to confirm the results of the preheat plateau tests. Prior to irradiating a laboratory dose, the natural OSL signals were removed by two 100 s blue light (blue LED) exposures at room temperature, separated by a 10 ks pause to allow any photo-transferred charge in the 110°C thermoluminescence trap to decay. The bleached aliquots were then irradiated with a given dose approximately equivalent to the De values of the sample, and the irradiated aliquots were measured using the SAR procedure in Table 1.

Three aliquots were measured for each preheat temperature, and the results are shown in Fig. 4. It shows that the ratios of measured dose to the given dose (dose recovery ratio) are closest to unity at the preheat temperature of 250°C. Therefore, the preheat of 250°C for 10 s was used in the quartz OSL-SAR, OSL-SMAR and TT-OSL SAR procedures.

Fig. 4

Plot of recovery ratios versus preheat temperature for sample L3478. Three aliquots were tested at each preheat temperature.

Examples of the decay curves of the natural TT-OSL (Fig. 5a) and BT-OSL (Fig. 5b) signals and the regeneration dose TT-OSL (Fig. 5c) and BT-OSL (Fig. 5d) signals are shown in Fig. 5. It is evident that there was a significant rise in the intensities of LTT-OSL with increasing doses, and this is not the case for LBT-OSL. The corrected recuperated intensity, LRe-OSL, was obtained by the equation (mentioned above). The corresponding DRCs and one of the LRe-OSL signals are shown in Fig. 5e and 5f, respectively, for which the recycling ratios fall into the acceptance range of 0.9–1.1, and recuperation is 1.01 ± 0.03. The DRC in Fig. 5f was fitted with a single saturating exponential, the De value obtained is much less than the D0 value of about 470 Gy for the curve. In order to determine the residual TT-OSL signal of the studied samples, the natural aliquots of sample L3481 were exposed to light from a solar simulator (SOL2, Hönle UVACUBE400) for 1 min, 9 h and 2 days, respectively, and then measured using the TT-OSL procedure in Table 1. Three aliquots were used for each bleaching time. The residual TT-OSL De values of 230.5 ± 10.1 Gy, 70.0 ± 5.7 Gy and 33.4 ± 1.6 Gy were obtained for the three bleaching times, respectively. The dose of 33.4 Gy was taken as a residual TT-OSL dose for subtraction for all samples.

Fig. 5

Decay curves of natural (a) thermally-transferred (TT) and (b) basic-transferred (BT) OSL, regenerative-dose (c) TT-OSL and (d) BT-OSL signals; dose-response curves for the sensitivity-corrected TT-OSL (square) and BT-OSL (solid circle) signals (e) and recuperated OSL (Re-OSL) signals (f). The insets in (a–d) showing the test-dose (18.3 Gy) OSL signals following natural and regenerative-dose OSL measurements.

The dose rates and De values obtained using the above three procedures on fine-grained quartz are summarized and listed in Table 3. It shows that the calculated dose rates range from 4.3 to 3.5 Gy/ka, and the De values varying from about 269 to 460 Gy obtained using the three procedures. The ages were obtained by dividing the De values by the dose rates and listed in Table 3 and displayed in Fig. 6. The top sample (sample L3475) was dated to SAR-OSL 67 ± 4 ka, SMAR-OSL 66 ± 4 ka and TT-OSL 62 ± 4 ka, and the bottom sample (sample L3481) to SAR-OSL 133 ± 9 ka, SMAR-OSL 123 ± 9 ka and TT-OSL 127 ± 9 ka. The figure demonstrates that the SAR-OSL, SMAR-OSL and TT-OSL ages for each sample are consistent within errors except for sample L3478, and they are in stratigraphical order.

Fig. 6

Age – depth model showing the quartz SAR-, SMAR-, TT-OSL ages and the polymineral pIRIR(100, 275) ages of the seven samples. The shaded area shows the sedimentary layer where stone artifacts were unearthed.

The results of luminescence dating of fine-grained quartz using different procedures and fine polymineral grains using the pIRIR(100, 275) procedure.

Lab No.LayerDepth (cm)U (ppm)Th (ppm)K (%)Water (%)Cosmic dose rate (Gy/ka)aMineralNumber of Aliquot bMethodDose rate (Gy ka-1)De (Gy)Age (ka)
L34752504.119.71.823.00.20Quartz9OSL-SAR4.3 ± 0.3290.8 ± 7.367 ± 4
3(6)OSL-SMAR283.1 ± 5.166 ± 4
6(6)TT-OSL SAR268.9 ± 8.962 ± 4
Polymineral3pIRIR(100, 275)5.1 ± 0.3389.5 ± 27.877 ± 7
L347631003.718.01.723.00.18Quartz9OSL-SAR4.0 ± 0.2361.8 ± 9.691 ± 6
3(6)OSL-SMAR334.7 ± 10.184 ± 6
6(6)TT-OSL SAR307.5 ± 21.778 ± 7
Polymineral3pIRIR(100, 275)4.6 ± 0.3546.3 ± 24.4118 ± 8
L347731503.719.01.723.00.17Quartz9OSL-SAR4.0 ± 0.2371.4 ± 21.092 ± 8
3(6)OSL-SMAR364.4 ± 25.790 ± 8
6(6)TT-OSL SAR334.0 ± 21.2383 ± 7
Polymineral3pIRIR(100, 275)4.7 ± 0.3518.3 ± 7.2110 ± 6
L347842003.216.51.623.00.16Quartz9OSL-SAR3.6 ± 0.2466.2 ± 18.3129 ± 9
3(6)OSL-SMAR380.4 ± 9.1105 ± 7
6(6)TT-OSL SAR400.1 ± 24.4111 ± 9
Polymineral4pIRIR(100, 275)4.2 ± 0.2732.4 ± 60.8174 ± 17
L347942503.817.51.523.00.15Quartz9OSL-SAR3.8 ± 0.2423.9 ± 7.6113 ± 7
3(6)OSL-SMAR398.1 ± 8.7106 ± 7
6(6)TT-OSL SAR396.8±5.3105 ± 7
Polymineral3pIRIR(100, 275)4.4 ± 0.3458.0 ± 18.8103 ± 7
L348043004.019.31.423.00.14Quartz9OSL-SAR3.9 ± 0.3442.3 ± 20.1114 ± 9
3(6)OSL-SMAR423.9 ± 21.9110 ± 9
6(6)TT-OSL SAR442.2 ± 20.1114 ± 9
Polymineral3pIRIR(100, 275)4.6 ± 0.3465.2 ± 9.9101 ± 6
L348153503.616.71.323.00.13Quartz9OSL-SAR3.5 ± 0.2459.6 ± 6.2133 ± 9
3(6)OSL-SMAR426.9 ± 17.4123 ± 9
6(6)TT-OSL SAR440.0 ± 9.5127 ± 9
Polymineral5pIRIR(100, 275)4.1 ± 0.2586.6 ± 74.3143 ± 20

aCosmic dose rates (Gy/ka) were calculated according to Prescott and Hutton (1994).

bNumbers in brackets are the total numbers of aliquots measured.

pIRIR ages of polymineral grains

All the samples show relatively dim IRSL, pIRIR and MET-pIRIR signals, and their natural intensities decrease as depth increases (Figs. 79). Note that the intensity of the natural IRSL signals measured at the sample temperature of 250°C are much larger than at lower temperatures (Fig. 7). Fig. 7 demonstrates that the MET-pIRIR signals are very dim and close to the noise background, and this is especially the case for the test dose (91.5 Gy) signals. The dim MET-pIRIR signals result in very large uncertainties in MET-pIRIR De values. In this case, the MET-pIRIR Des of the samples were not further determined.

Fig. 7

Decay curves of IRSL (50°C) and MET-pIRIR signals measured at different stimulation temperatures for a single polymineral aliquot of sample L3478.

Fig. 8

Natural decay curves of the polymineral pIRIR(100, 275) signals for the study samples.

Fig. 9

Dose-response curves of pIRIR(100, 275) signals for single polymineral aliquots of the top sample (L3475, a) and the bottom sample (L3481, b). Insets show the natural decay curves for the two samples.

In the two-step pIRIR procedure (Table 2), the effect of the first IR stimulation temperature on pIRIR De values was tested using the temperatures of 50, 100, 150 and 200°C, respectively, and the results shown in Fig. 10 indicate that the pIRIR De values are independent of the first stimulation temperatures between 50 and 150°C, and the recycling ratios are close to unity and the recuperations less than 5%. Therefore, here the sample temperature of 100°C was used for the IRSL signal measurements before measuring the pIRIR signals at 275°C. Two pIRIR(100, 275) DRCs for the top sample (L3475) and the bottom sample (L3481) shown in Fig. 9 demonstrate that the two samples are very far from being naturally saturated as the D0 for samples L3475 and 3481 are 348 Gy and 402 Gy, respectively, and the recycling ratios are scattered but still close to unity. The pIRIR(100, 275) De values and ages obtained are summarized in Table 3 and the ages also shown in Fig. 6. The pIRIR(100, 275) ages obtained range from 77 ± 7 to 174 ± 17 ka, and they are not in strict stratigraphical order. The pIRIR(100, 275) ages of samples L3475, L3479, L3480 and L3481 are in agreement with their quartz OSL (SAR-, SMAR- and TT-OSL) ages, if considering 2σ uncertainties. However, the pIRIR(100,275) ages of samples L3476, L3477 and L3478 are much larger than their corresponding quartz OSL ages. It is noted that the analysis of residual pIRIR(100, 275) dose and fading corrections have not been performed for these samples.

Fig. 10

Plots of pIRIR275 De values against different sample temperatures for the first IRSL measurements for sample L3478. Three fine polymineral aliquots were measured at each temperature for the IRSL measurements.

Discussion

The fine quartz extracts from the studied samples demonstrate excellent SAR or SMAR properties such as very bright, fast-dominated component, recycling ratios close to unity, recuperation less than 5% of the corrected natural signal and high saturation dose. The SAR-OSL and SMAR-OSL ages are in stratigraphical order except for the SAR-OSL age of sample L3478 at the depth of 200 cm. Note that although the quartz SAR-OSL De values of all samples are slightly larger than their SMAR-OSL De values, especially for sample L3478, the SAR-and SMAR-OSL De values are consistent when 2σ errors are considered. The slight difference between the SAR-and SMAR-OSL De values can be explained by the shapes of their DRCs in Fig. 2. This may imply that the quartz SAR-OSL De values of our samples were not underestimated due to the build-up of OSL signal during repeated SAR measurement cycles (Zhou and Shackleton, 2001; Lu et al., 2007). However, the large quartz SAR-OSL and SMAR-OSL De values ranging from 283 to 466 Gy (Table 3, Fig. 2) in the high dose range of quartz OSL may be problematic, resulting in underestimation of the true burial age (e.g. Lowick et al., 2015; Timar-Gabor et al., 2017), although some samples yielded reliable quartz SAR-OSL ages with the De values of up to 600 Gy, (e.g. Murray et al., 2008; Zhang et al., 2015; Buechi et al., 2017). Here, the reliability of the quartz SAR- and SMAR-OSL ages obtained were tested using the TT-OSL SAR procedure on quartz and the two-step pIRIR and MET-pIRIR procedures on fine polymineral grains, which can potentially extend the age range because TT-OSL and pIRIR signals have very high saturation levels (see reviews by Duller and Wintle, 2012, Li et al., 2014, Arnold et al., 2015).

TT-OSL signals were considered to be optically bleached at a much slower rate than the fast component OSL signal (Duller and Wintle, 2012), as demonstrated by the results of bleaching experiments on quartz grains with different origins and the TT-OSL De values of modern analogues (Tsukamoto et al., 2008; Kim et al., 2009; Athanassas and Zacharias, 2010; Hu et al., 2010; Jacobs et al., 2011; Hernandez et al., 2012; Arnold et al., 2019). The bleaching experiment on a sample in this study shows that the TT-OSL signal was reduced to 50% (equivalent to the De value of 230.5 Gy) of its initial value after 1 min bleaching, and 7% (33.4 Gy) after two days of bleaching. Compared with the results of the previous bleaching experiments mentioned above, we considered that the TT-OSL signals from our samples are relatively easily bleached. This is also supported by the fact that the TT-OSL, SAR-OSL and SMAR-OSL De values or ages for each sample are almost identical (Table 3, Fig. 6).

Although residual pIRIR(100, 275) doses have not been determined and fading corrections have not been done, their influence on pIRIR(100, 275) De values for these old samples are negligible (Li et al., 2014). The stratigraphic inconsistency of the pIRIR(100, 275) ages and the relationship between polymineral pIRIR(100, 275) and quartz OSL ages imply that the pIRIR(100, 275) ages may generally be problematic, this is especially the case for samples L3479 at 250 cm depth and L3480 at 300 cm depth, whose pIRIR(100, 275) ages are younger than the overlying samples (L3476, L3477 and L3478). This may be due to the lower samples are too old (>400 Gy), resulting in underestimation of the pIRIR age (Li and Li, 2012b). Relatively, sample L3476, L3477 and L3478 yielded much larger pIRIR(100, 275) ages compared to the corresponding quartz OSL ages. This is similar to the situation for the samples from the nearby Fengshuzui site (Zhang et al., 2018), where the dim feldspar signal due to the chemical weathering of the sediments was shown to yield 35–55% older ages than those based on the quartz SAR protocol (Huang et al., 2019). In this case, we deduce that the true burial ages of the upper samples (L3475–3478) are between the quartz OSL ages and the feldspar pIRIR(100, 275) ages.

As stated above, the stone artefacts were mainly excavated mainly from deposits between the lower part of Layer 2 and the upper part of Layer 4 (Figs. 1b and 6), from which samples L3476 and L3477 were collected and optically dated. Their SAR-, SMAR- and TT-OSL ages are indistinguishable when errors are considered, and their average value is 86 ± 9 ka, while the average of the two pIRIR(100, 275) ages is 114 ± 10 ka. These dates bracket the age of the cultural layers. This indicates that this region was occupied by hominins during the marine isotope stage 5.

Conclusions

The Huxushan Paleolithic site in south China was optically dated using various methods, including OSL-SAR, OSL-SMAR and TT-OSL SAR procedures on fine quartz grains and two-step pIRIR(100, 275) and MET-pIRIR procedures on fine polymineral fractions of seven samples from the site. The fine-grained quartz demonstrated excellent luminescence properties, and the SAR-OSL, SMAR-OSL and TT-OSL ages of the studied samples agree with each other and are in stratigraphical order except for one sample. This good internal consistency would indicate that the quartz OSL ages obtained for the samples are reliable. However, the fine polymineral fractions which exhibited dim pIRIR and MET-pIRIR signals yielded older ages for the layer with stone tools. The MET-pIRIR signals are too weak to yield De values with useful precision. Although the pIRIR(100, 275) ages obtained for the studied samples are stratigraphically inconsistent, the older ages for the two samples from the cultural layer compared to those derived from quartz SAR OSL protocol are considered to represent the upper age limit of the stone tools. The quartz OSL ages obtained using different procedures for the two samples range from 78 to 92 ka, they are considered as the minimum age of the cultural layer. The site was deduced to be occupied by hominins during the marine isotope stage 5.

Fig. 1

(a) Map showing the location of the study site, and (b) photograph of the excavation pit showing the stratigraphy and the positions of OSL samples.
(a) Map showing the location of the study site, and (b) photograph of the excavation pit showing the stratigraphy and the positions of OSL samples.

Fig. 2

Comparison of dose-response curves constructed using the quartz OSL-SAR and OSL-SMAR protocols for sample L3481. The inset shows a natural decay curve for the same aliquot.
Comparison of dose-response curves constructed using the quartz OSL-SAR and OSL-SMAR protocols for sample L3481. The inset shows a natural decay curve for the same aliquot.

Fig. 3

(a) Plot of De values as a function of preheat temperature in the range of 180 and 280°C at 20°C increments for sample L3478, and (b) recycling ratios and recuperation against preheat temperature. Three aliquots were determined at each preheat temperature.
(a) Plot of De values as a function of preheat temperature in the range of 180 and 280°C at 20°C increments for sample L3478, and (b) recycling ratios and recuperation against preheat temperature. Three aliquots were determined at each preheat temperature.

Fig. 4

Plot of recovery ratios versus preheat temperature for sample L3478. Three aliquots were tested at each preheat temperature.
Plot of recovery ratios versus preheat temperature for sample L3478. Three aliquots were tested at each preheat temperature.

Fig. 5

Decay curves of natural (a) thermally-transferred (TT) and (b) basic-transferred (BT) OSL, regenerative-dose (c) TT-OSL and (d) BT-OSL signals; dose-response curves for the sensitivity-corrected TT-OSL (square) and BT-OSL (solid circle) signals (e) and recuperated OSL (Re-OSL) signals (f). The insets in (a–d) showing the test-dose (18.3 Gy) OSL signals following natural and regenerative-dose OSL measurements.
Decay curves of natural (a) thermally-transferred (TT) and (b) basic-transferred (BT) OSL, regenerative-dose (c) TT-OSL and (d) BT-OSL signals; dose-response curves for the sensitivity-corrected TT-OSL (square) and BT-OSL (solid circle) signals (e) and recuperated OSL (Re-OSL) signals (f). The insets in (a–d) showing the test-dose (18.3 Gy) OSL signals following natural and regenerative-dose OSL measurements.

Fig. 6

Age – depth model showing the quartz SAR-, SMAR-, TT-OSL ages and the polymineral pIRIR(100, 275) ages of the seven samples. The shaded area shows the sedimentary layer where stone artifacts were unearthed.
Age – depth model showing the quartz SAR-, SMAR-, TT-OSL ages and the polymineral pIRIR(100, 275) ages of the seven samples. The shaded area shows the sedimentary layer where stone artifacts were unearthed.

Fig. 7

Decay curves of IRSL (50°C) and MET-pIRIR signals measured at different stimulation temperatures for a single polymineral aliquot of sample L3478.
Decay curves of IRSL (50°C) and MET-pIRIR signals measured at different stimulation temperatures for a single polymineral aliquot of sample L3478.

Fig. 8

Natural decay curves of the polymineral pIRIR(100, 275) signals for the study samples.
Natural decay curves of the polymineral pIRIR(100, 275) signals for the study samples.

Fig. 9

Dose-response curves of pIRIR(100, 275) signals for single polymineral aliquots of the top sample (L3475, a) and the bottom sample (L3481, b). Insets show the natural decay curves for the two samples.
Dose-response curves of pIRIR(100, 275) signals for single polymineral aliquots of the top sample (L3475, a) and the bottom sample (L3481, b). Insets show the natural decay curves for the two samples.

Fig. 10

Plots of pIRIR275 De values against different sample temperatures for the first IRSL measurements for sample L3478. Three fine polymineral aliquots were measured at each temperature for the IRSL measurements.
Plots of pIRIR275 De values against different sample temperatures for the first IRSL measurements for sample L3478. Three fine polymineral aliquots were measured at each temperature for the IRSL measurements.

The results of luminescence dating of fine-grained quartz using different procedures and fine polymineral grains using the pIRIR(100, 275) procedure.

Lab No.LayerDepth (cm)U (ppm)Th (ppm)K (%)Water (%)Cosmic dose rate (Gy/ka)aMineralNumber of Aliquot bMethodDose rate (Gy ka-1)De (Gy)Age (ka)
L34752504.119.71.823.00.20Quartz9OSL-SAR4.3 ± 0.3290.8 ± 7.367 ± 4
3(6)OSL-SMAR283.1 ± 5.166 ± 4
6(6)TT-OSL SAR268.9 ± 8.962 ± 4
Polymineral3pIRIR(100, 275)5.1 ± 0.3389.5 ± 27.877 ± 7
L347631003.718.01.723.00.18Quartz9OSL-SAR4.0 ± 0.2361.8 ± 9.691 ± 6
3(6)OSL-SMAR334.7 ± 10.184 ± 6
6(6)TT-OSL SAR307.5 ± 21.778 ± 7
Polymineral3pIRIR(100, 275)4.6 ± 0.3546.3 ± 24.4118 ± 8
L347731503.719.01.723.00.17Quartz9OSL-SAR4.0 ± 0.2371.4 ± 21.092 ± 8
3(6)OSL-SMAR364.4 ± 25.790 ± 8
6(6)TT-OSL SAR334.0 ± 21.2383 ± 7
Polymineral3pIRIR(100, 275)4.7 ± 0.3518.3 ± 7.2110 ± 6
L347842003.216.51.623.00.16Quartz9OSL-SAR3.6 ± 0.2466.2 ± 18.3129 ± 9
3(6)OSL-SMAR380.4 ± 9.1105 ± 7
6(6)TT-OSL SAR400.1 ± 24.4111 ± 9
Polymineral4pIRIR(100, 275)4.2 ± 0.2732.4 ± 60.8174 ± 17
L347942503.817.51.523.00.15Quartz9OSL-SAR3.8 ± 0.2423.9 ± 7.6113 ± 7
3(6)OSL-SMAR398.1 ± 8.7106 ± 7
6(6)TT-OSL SAR396.8±5.3105 ± 7
Polymineral3pIRIR(100, 275)4.4 ± 0.3458.0 ± 18.8103 ± 7
L348043004.019.31.423.00.14Quartz9OSL-SAR3.9 ± 0.3442.3 ± 20.1114 ± 9
3(6)OSL-SMAR423.9 ± 21.9110 ± 9
6(6)TT-OSL SAR442.2 ± 20.1114 ± 9
Polymineral3pIRIR(100, 275)4.6 ± 0.3465.2 ± 9.9101 ± 6
L348153503.616.71.323.00.13Quartz9OSL-SAR3.5 ± 0.2459.6 ± 6.2133 ± 9
3(6)OSL-SMAR426.9 ± 17.4123 ± 9
6(6)TT-OSL SAR440.0 ± 9.5127 ± 9
Polymineral5pIRIR(100, 275)4.1 ± 0.2586.6 ± 74.3143 ± 20

Procedures used for De measurements of fine polymineral grains.

StepMET-pIRIR procedureObservedStepTwo-step pIRIR procedureObserved
1Give dose, Di1Give dose, Di
2Preheating at 320°C for 60 s2Preheating at 320°C for 60 s
3Infrared stimulation at 50°C for 100 sLx(50)3Infrared stimulation at 100°C for 200 s
4Infrared stimulation at 150°C for 100 sLx(150)4Infrared stimulation at 275°C for 200 sLi
5Infrared stimulation at 200°C for 100 sLx(200)5Give test dose, Dt (91.5 Gy)
6Infrared stimulation at 250°C for 100 sLx(250)6Cut heat at 320°C for 60 s
7Infrared stimulation at 290°C for 100 sLx(290)7Infrared stimulation at 100°C for 200 s
8Give test dose, Dt (91.5 Gy)8Infrared stimulation at 275°C for 200 sTi
9Preheating at 320°C for 60 s9Infrared stimulation at 325°C for 200 s
10Infrared stimulation at 50°C for 100 sTx(50)10Return to step 1
11Infrared stimulation at 150°C for 100 sTx(150)
12Infrared stimulation at 200°C for 100 sTx(200)
13Infrared stimulation at 250°C for 100 sTx(250)
14Infrared stimulation at 290°C for 100 sTx(290)
15IR bleaching at 325°C for 100 s
16Return to step 1

Protocols used for De measurements of fine quartz grains.

Step OSL-SAR protocolObservedStep OSL-SMAR protocolObservedStep TT-OSL SAR procedureObserved
1 Give dose, DiPart 1 Detection of natural OSL signalPart 1 Detection of thermal-transferred OSL signal
2 Preheating at 250°C for 10 s1-1 Preheating at 250°C for 10 s1-1 Give dose, Di
3 Blue stimulation at 125°C for 40 sLi1-2 Blue stimulation at 125°C for 40 sLn1-2 Preheating at 250°C for 10 s
4 Give test dose, Dt (18.3 Gy)1-3 Give test dose, Dt (18.3 Gy)1-3 Blue stimulation at 125°C for 300 s
5 Cut heat at 160°C for 5 s1-4 Cut heat at 160°C for 5 s1-4 Preheating at 250°C for 10 s
6 Blue stimulation at 125°C for 40 sTi1-5 Blue stimulation at 125°C for 40 sTn1-5 Blue stimulation at 125°C for 40 sLTTOSL
7 Blue stimulation at 280°C for 40 sPart 2 Detection of regenerative OSL signal1-6 Give test dose, Dt (18.3 Gy)
8 Return to step 12-1 Bleaching at 125°C for 60 s1-7 Cut heat at 160°C for 5 s
2-2 Give dose, Di1-8 Blue stimulation at 125°C for 100 sTTTOSL
2-3 Preheating at 250°C for 10 sPart 2 Detection of basic-transferred OSL signal
2-4 Blue stimulation at 125°C for 40 sLi2-1 Annealing to 300°C for 10 s
2-5 Give test dose, Dt (18.3 Gy)2-2 Blue stimulation at 125°C for 100 s
2-6 Cut heat at 160°C for 5 s2-3 Preheating at 250°C for 10 s
2-7 Blue stimulation at 125°C for 40 sTi2-4 Blue stimulation at 125°C for 100 sLBTOSL
2-5 Give test dose, Dt (18.3 Gy)
2-6 Cut heat at 220°C for 10 s
2-7 Blue stimulation at 125°C for 100 sTBTOSL
2-8 Blue stimulation at 280°C for 100 s

Aitken MJ and Smith BW, 1988. Optical dating: Recuperation after bleaching. Quaternary Science Reviews 7: 387‒393, DOI 10.1016/0277-3791(88)90034-0.AitkenMJSmithBW1988Optical dating: Recuperation after bleachingQuaternary Science Reviews738739310.1016/0277-3791(88)90034-0Open DOISearch in Google Scholar

Arnold L, Demuro M, Parésc JM, Gonzálezc AP, Arsuaga JL, Castro JMB and Carbonell E, 2015. Evaluating the suitability of extended-range luminescence dating techniques over early and Middle Pleistocene timescales: Published datasets and case studies from Atapuerca, Spain. Quaternary International 389: 167‒190, DOI 10.1016/j.quaint.2014.08.010.ArnoldLDemuroMParéscJMGonzálezcAPArsuagaJLCastroJMBCarbonellE2015Evaluating the suitability of extended-range luminescence dating techniques over early and Middle Pleistocene timescales: Published datasets and case studies from Atapuerca, SpainQuaternary International38916719010.1016/j.quaint.2014.08.010Open DOISearch in Google Scholar

Arnold LJ, Demuro M, Spooner NA, Prideaux GJ, McDowell MC, Camens AB, Reedd EH, Parés JM, Arsuaga JL, José María Bermúdez de Castro and Carbonell E, 2019. Single-grain TT-OSL bleaching characteristics: Insights from modern analogues and OSL dating comparisons. Quaternary Geochronology 49: 45‒51, DOI 10.1016/j.quageo.2018.01.004.ArnoldLJDemuroMSpoonerNAPrideauxGJMcDowellMCCamensABReeddEHParésJMArsuagaJLJoséMaría Bermúdez de CastroCarbonellE2019Single-grain TT-OSL bleaching characteristics: Insights from modern analogues and OSL dating comparisonsQuaternary Geochronology49455110.1016/j.quageo.2018.01.004Open DOISearch in Google Scholar

Athanassas C and Zacharias N, 2010. Recuperated-OSL dating of quartz from Aegean (South Greece) raised Pleistocene marine sediments: current results. Quaternary Geochronology 5: 65‒75, DOI 10.1016/j.quageo.2009.09.010.AthanassasCZachariasN2010Recuperated-OSL dating of quartz from Aegean (South Greece) raised Pleistocene marine sediments: current resultsQuaternary Geochronology5657510.1016/j.quageo.2009.09.010Open DOISearch in Google Scholar

Bøtter-Jensen L, Andersen CE, Duller GAT and Murray AS, 2003. Developments in radiation, stimulation and observation facilities in luminescence measurements. Radiation Measurements 37(4‒5): 535‒541, DOI 10.1016/S1350-4487(03)00020-9.Bøtter-JensenLAndersenCEDullerGATMurrayAS2003Developments in radiation, stimulation and observation facilities in luminescence measurementsRadiation Measurements374‒553554110.1016/S1350-4487(03)00020-9Open DOISearch in Google Scholar

Buechi MW, Lowick SE and Anselmetti FS, 2017. Luminescence dating of glaciolacustrine silt in overdeepened basin fills beyond the last interglacial. Quaternary Geochronology 37: 55‒67, DOI 10.1016/j.quageo.2016.09.009.BuechiMWLowickSEAnselmettiFS2017Luminescence dating of glaciolacustrine silt in overdeepened basin fills beyond the last interglacialQuaternary Geochronology37556710.1016/j.quageo.2016.09.009Open DOISearch in Google Scholar

Buylaert JP, Jain M, Murray AS, Thomsen KJ, Thiel C and Sohbati R, 2012. A robust feldspar luminescence dating method for Middle and Late Pleistocene sediments. Boreas 41(3): 435‒451, DOI 10.1111/j.1502-3885.2012.00248.x.BuylaertJPJainMMurrayASThomsenKJThielCSohbatiR2012A robust feldspar luminescence dating method for Middle and Late Pleistocene sedimentsBoreas41343545110.1111/j.1502-3885.2012.00248.xOpen DOISearch in Google Scholar

Chu JY, Huang W, Kuang SQ, Wang JM, Xu JJ, Chu ZT, Yang ZQ, Lin KQ, Li P, Wu M, Geng ZC, Tan CC, Du RF and Jin L, 1998. Genetic relationship of populations in China. Proceedings of the National Academy of Sciences of the United States of America 95(20): 11763‒11768, DOI 10.1073/pnas.95.20.11763.ChuJYHuangWKuangSQWangJMXuJJChuZTYangZQLinKQLiPWuMGengZCTanCCDuRFJinL1998Genetic relationship of populations in ChinaProceedings of the National Academy of Sciences of the United States of America9520117631176810.1073/pnas.95.20.11763Open DOISearch in Google Scholar

Duller GAT and Wintle AG, 2012. A review of the thermally transferred optically stimulated luminescence signal from quartz for dating sediments. Quaternary Geochronology 7(1): 6‒20, DOI 10.1016/j.quageo.2011.09.003.DullerGATWintleAG2012A review of the thermally transferred optically stimulated luminescence signal from quartz for dating sedimentsQuaternary Geochronology7162010.1016/j.quageo.2011.09.003Open DOISearch in Google Scholar

Durcan JA, King GE and Duller GAT, 2015. DRAC: Dose Rate and Age Calculator for trapped charge dating. Quaternary Geochronology 28: 54‒61, DOI 10.1016/j.quageo.2015.03.012.DurcanJAKingGEDullerGAT2015DRAC: Dose Rate and Age Calculator for trapped charge datingQuaternary Geochronology28546110.1016/j.quageo.2015.03.012Open DOISearch in Google Scholar

Gao X, 2013. Paleolithic cultures in China: Uniqueness and divergence. Current Anthropology 54: 358‒370, DOI 10.1086/673502.GaoX2013Paleolithic cultures in China: Uniqueness and divergenceCurrent Anthropology5435837010.1086/673502Open DOISearch in Google Scholar

Hernandez M, Mauz B, Mercier N and Shen ZX, 2012. Evaluating the efficiency of TT-OSL SAR protocols. Radiation Measurements 47: 669‒673, DOI 10.1016/j.radmeas.2012.04.017.HernandezMMauzBMercierNShenZX2012Evaluating the efficiency of TT-OSL SAR protocolsRadiation Measurements4766967310.1016/j.radmeas.2012.04.017Open DOISearch in Google Scholar

Hu G, Zhang JF, Qiu WL, and Zhou LP, 2010. Residual OSL signals in modern fluvial sediments from the Yellow River (HuangHe) and the implications for dating young sediments. Quaternary Geochronology 5(2‒3): 187‒193, DOI 10.1016/j.quageo.2009.05.003.HuGZhangJFQiuWLZhouLP2010Residual OSL signals in modern fluvial sediments from the Yellow River (HuangHe) and the implications for dating young sedimentsQuaternary Geochronology52‒318719310.1016/j.quageo.2009.05.003Open DOISearch in Google Scholar

Hu Y, Marwick B, Zhang JF, Rui X, Hou YM, Yue JP, Chen WR, Huang WW and Li B, 2019. Late Middle Pleistocene Levallois stone-tool technology in southwest China. Nature 565: 82–85, DOI 10.1038/s41586-018-0710-1.HuYMarwickBZhangJFRuiXHouYMYueJPChenWRHuangWWLiB2019Late Middle Pleistocene Levallois stone-tool technology in southwest ChinaNature565828510.1038/s41586-018-0710-1Open DOISearch in Google Scholar

Huang XK, Luo BN and Zhou LP, 2019. Luminescence signals from polymineral fine-grains in strongly chemically-weathered sediments from a Paleolithic site and their usefulness for dating[J]. Quaternary Sciences 39, DOI 10.11928/j.issn.1001-7410.2019.02.16.HuangXKLuoBNZhouLP2019Luminescence signals from polymineral fine-grains in strongly chemically-weathered sediments from a Paleolithic site and their usefulness for dating[J]Quaternary Sciences3910.11928/j.issn.1001-7410.2019.02.16Open DOISearch in Google Scholar

Huntley DJ, Godfrey-Smith DI and Thewalt MLW, 1985. Optical dating of sediments. Nature 313: 105‒107, DOI 10.1038/313105a0.HuntleyDJGodfrey-SmithDIThewaltMLW1985Optical dating of sedimentsNature31310510710.1038/313105a0Open DOISearch in Google Scholar

Jacobs J, Roberts RG, Lachlan TJ, KarkanasPb, Marean CW and Roberts DL, 2011. Development of the SAR TT-OSL procedure for dating Middle Pleistocene dune and shallow marine deposits along the southern Cape coast of South Africa. Quaternary Geochronology 6: 491‒513, DOI 10.1016/j.quageo.2011.04.003.JacobsJRobertsRGLachlanTJKarkanasPbMareanCWRobertsDL2011Development of the SAR TT-OSL procedure for dating Middle Pleistocene dune and shallow marine deposits along the southern Cape coast of South AfricaQuaternary Geochronology649151310.1016/j.quageo.2011.04.003Open DOISearch in Google Scholar

Kim JC, Duller GAT, Roberts HM, Wintle AG, Lee YI and Yi SB, 2009. Dose dependence of thermally transferred optically stimulated luminescence signals in quartz. Radiation Measurements 44: 132‒143, DOI 10.1016/j.radmeas.2008.12.001.KimJCDullerGATRobertsHMWintleAGLeeYIYiSB2009Dose dependence of thermally transferred optically stimulated luminescence signals in quartzRadiation Measurements4413214310.1016/j.radmeas.2008.12.001Open DOISearch in Google Scholar

Lai ZP and Brückner H, 2008. Effects of feldspar contamination on equivalent dose and the shape of growth curve for OSL of silt-sized quartz extracted from Chinese loess. Geochronometria 30(1): 49‒53, DOI 10.2478/v10003-008-0010-0.LaiZPBrücknerH2008Effects of feldspar contamination on equivalent dose and the shape of growth curve for OSL of silt-sized quartz extracted from Chinese loessGeochronometria301495310.2478/v10003-008-0010-0Open DOISearch in Google Scholar

Li B and Li SH, 2011. Luminescence dating of K-feldspar from sediments: A protocol without anomalous fading correction. Quaternary Geochronology 6(5): 468‒479, DOI 10.1016/j.quageo.2011.05.001.LiBLiSH2011Luminescence dating of K-feldspar from sediments: A protocol without anomalous fading correctionQuaternary Geochronology6546847910.1016/j.quageo.2011.05.001Open DOISearch in Google Scholar

Li B and Li SH, 2012a. Luminescence dating of Chinese loess beyond 130 ka using the non-fading signal from K-feldspar. Quaternary Geochronology 10: 24‒31, DOI 10.1016/j.quageo.2011.12.005.LiBLiSH2012aLuminescence dating of Chinese loess beyond 130 ka using the non-fading signal from K-feldsparQuaternary Geochronology10243110.1016/j.quageo.2011.12.005Open DOISearch in Google Scholar

Li B and Li SH, 2012b. A reply to the comments by Thomsen et al. on “Luminescence dating of K-feldspar from sediments: A protocol without anomalous fading correction”. Quaternary Geochronology 8: 49‒51, DOI 10.1016/j.quageo.2011.10.001.LiBLiSH2012bA reply to the comments by Thomsen et al. on “Luminescence dating of K-feldspar from sediments: A protocol without anomalous fading correction”Quaternary Geochronology8495110.1016/j.quageo.2011.10.001Open DOISearch in Google Scholar

Li B, Jacobs, Z, Roberts, RG and Li, SH, 2014. Review and assessment of the potential of post-IR IRSL dating methods to circumvent the problem of anomalous fading in feldspar luminescence. Geochronometria 41(3): 178–201, DOI 10.2478/s13386-013-0160-3.LiBJacobsZRobertsRGLiSH2014Review and assessment of the potential of post-IR IRSL dating methods to circumvent the problem of anomalous fading in feldspar luminescenceGeochronometria41317820110.2478/s13386-013-0160-3Open DOISearch in Google Scholar

Li ZY, Wu XJ, Zhou LP, Liu W, Gao X, Nian XM and Trinkaus E, 2017. Late Pleistocene archaic human crania from Xuchang, China. Science 355: 969–972. DOI 10.1126/science.aal2482.LiZYWuXJZhouLPLiuWGaoXNianXMTrinkausE2017Late Pleistocene archaic human crania from Xuchang, ChinaScience35596997210.1126/science.aal2482Open DOISearch in Google Scholar

Liu C, Xu XM, Yuan BY and Deng CL, 2008. Magnetostratigraphy of the Qiliting section (SE China) and its implication for geochronology of the red soil sequences in southern China. Geophysical Journal International 174: 107‒117, DOI 10.1111/j.1365-246X.2008.03814.x.LiuCXuXMYuanBYDengCL2008Magnetostratigraphy of the Qiliting section (SE China) and its implication for geochronology of the red soil sequences in southern ChinaGeophysical Journal International17410711710.1111/j.1365-246X.2008.03814.xOpen DOISearch in Google Scholar

Liu W, Martinón-Torres M, Cai YJ, Xiong S, Tong XH, Pei SW, Sier MJ, Wu XH, Edwards LE, Cheng H, Li YY, Yang XX, Bermúdez de Castro JM and Wu XJ, 2015. The earliest unequivocally modern humans in southern China. Nature 526: 696‒699, DOI 10.1038/nature15696.LiuWMartinón-TorresMCaiYJXiongSTongXHPeiSWSierMJWuXHEdwardsLEChengHLiYYYangXXBermúdezde Castro JMWuXJ2015The earliest unequivocally modern humans in southern ChinaNature52669669910.1038/nature15696Open DOISearch in Google Scholar

Lowick SE, Buechi MW, Gaar D, Graf HR and Oreusser F, 2015. Luminescence dating of Middle Pleistocene proglacial deposits from northern Switzerland: methodological aspects and stratigraphical conclusions. Boreas 44(3): 459‒482, DOI 10.1111/bor.12114.LowickSEBuechiMWGaarDGrafHROreusserF2015Luminescence dating of Middle Pleistocene proglacial deposits from northern Switzerland: methodological aspects and stratigraphical conclusionsBoreas44345948210.1111/bor.12114Open DOISearch in Google Scholar

Lu HY, Zhang HY, Wang SJ, Cosgrove R, Sun XF, Zhao J, Sun DH, Zhao C, Shen C and Wei M, 2011. Multiphase timing of hominin occupations and the paleoenvironment in Luonan Basin, Central China. Quaternary Research 76: 142‒147, DOI 10.1016/j.yqres.2011.04.001.LuHYZhangHYWangSJCosgroveRSunXFZhaoJSunDHZhaoCShenCWeiM2011Multiphase timing of hominin occupations and the paleoenvironment in Luonan Basin, Central ChinaQuaternary Research7614214710.1016/j.yqres.2011.04.001Open DOISearch in Google Scholar

Lu YC, Wang XL and Wintle AG, 2007. A new OSL chronology for dust accumulation in the last 130,000 yr for the Chinese Loess Plateau. Quaternary Research 67(1): 152‒160, DOI 10.1016/j.yqres.2006.08.003.LuYCWangXLWintleAG2007A new OSL chronology for dust accumulation in the last 130,000 yr for the Chinese Loess PlateauQuaternary Research67115216010.1016/j.yqres.2006.08.003Open DOISearch in Google Scholar

Murray AS, Buylaert JP, Henriksen M, Svendsen JI and Mangerud J, 2008. Testing the reliability of quartz OSL ages beyond the Eemian. Radiation Measurements 43(2‒6): 776‒780, DOI 10.1016/j.radmeas.2008.01.014.MurrayASBuylaertJPHenriksenMSvendsenJIMangerudJ2008Testing the reliability of quartz OSL ages beyond the EemianRadiation Measurements432‒677678010.1016/j.radmeas.2008.01.014Open DOISearch in Google Scholar

Murry AS and Wintle AG, 2000. Luminescence dating of quartz using an improved single-aliquot regenerative-dose protocol. Radiation Measurements 32(1): 57‒73, DOI 10.1016/S1350-4487(99)00253-X.MurryASWintleAG2000Luminescence dating of quartz using an improved single-aliquot regenerative-dose protocolRadiation Measurements321577310.1016/S1350-4487(99)00253-XOpen DOISearch in Google Scholar

Murry AS and Wintle AG, 2003. The single aliquot regenerative dose protocol: Potential for improvements in reliability. Radiation Measurements 37(4‒5): 377‒381, DOI 10.1016/S1350-4487(03)00053-2.MurryASWintleAG2003The single aliquot regenerative dose protocol: Potential for improvements in reliabilityRadiation Measurements374‒537738110.1016/S1350-4487(03)00053-2Open DOISearch in Google Scholar

Piazza, 1998. Towards a genetic history of China. Nature 395: 636‒639, DOI 10.1038/27071.Piazza1998Towards a genetic history of ChinaNature39563663910.1038/27071Open DOISearch in Google Scholar

Prescott JR and Hutton JT, 1994. Cosmic ray contributions to dose rates for luminescence and ESR dating: Large depths and long-term time variations. Radiation Measurements 23(2‒3): 497‒500, DOI 10.1016/1350-4487(94)90086-8.PrescottJRHuttonJT1994Cosmic ray contributions to dose rates for luminescence and ESR dating: Large depths and long-term time variationsRadiation Measurements232‒349750010.1016/1350-4487(94)90086-8Open DOISearch in Google Scholar

Roberts RG, Jacobs Z, Li B, Jankowski NR, Cunningham AC and Rosenfeld AB, 2015. Optical dating in archaeology: thirty years in retrospect and grand challenges for the future. Journal of Archaeological Science 56: 41‒60, DOI 10.1016/j.jas.2015.02.028.RobertsRGJacobsZLiBJankowskiNRCunninghamACRosenfeldAB2015Optical dating in archaeology: thirty years in retrospect and grand challenges for the futureJournal of Archaeological Science56416010.1016/j.jas.2015.02.028Open DOISearch in Google Scholar

Slimak L, Svendsen JI, Mangerud J, Plisson H, Heggen HP, Brugère A and Pavlov PY, 2011. Late Mousterian Persistence near the Arctic Circle. Science 332: 841‒845, DOI 10.1126/science.1203866.SlimakLSvendsenJIMangerudJPlissonHHeggenHPBrugèreAPavlovPY2011Late Mousterian Persistence near the Arctic CircleScience33284184510.1126/science.1203866Open DOISearch in Google Scholar

Sun XF, Lu HY, Wang SJ and Yi SW, 2012. Ages of Liangshan Paleolithic sites in Hanzhong Basin, central China. Quaternary Geochronology 10: 380‒386, DOI 10.1016/j.quageo.2012.04.014.SunXFLuHYWangSJYiSW2012Ages of Liangshan Paleolithic sites in Hanzhong Basin, central ChinaQuaternary Geochronology1038038610.1016/j.quageo.2012.04.014Open DOISearch in Google Scholar

Thiel C, Buylaert JP, Murray AS, Terhorst B, Hofer I, Tsukamoto S and Frechen M, 2011. Luminescence dating of the Stratzing loess profile (Austria) ‒ Testing the potential of an elevated temperature post-IR IRSL protocol. Quaternary International 234(1‒2): 23‒31, DOI 10.1016/j.quaint.2010.05.018.ThielCBuylaertJPMurrayASTerhorstBHoferITsukamotoSFrechenM2011Luminescence dating of the Stratzing loess profile (Austria) ‒ Testing the potential of an elevated temperature post-IR IRSL protocolQuaternary International2341‒2233110.1016/j.quaint.2010.05.018Open DOISearch in Google Scholar

Thomsen KJ, Murray AS, Jain M and Bøtter-Jensen L, 2008. Laboratory fading rates of various luminescence signals from feldspar-rich sediment extracts. Radiation Measurements 43(9‒10): 1474‒1486, DOI 10.1016/j.radmeas.2008.06.002.ThomsenKJMurrayASJainMBøtter-JensenL2008Laboratory fading rates of various luminescence signals from feldspar-rich sediment extractsRadiation Measurements439‒101474148610.1016/j.radmeas.2008.06.002Open DOISearch in Google Scholar

Timar-Gabor A, Buylaert JP, Guralnik B, Trandafir‒Antohi O, Constantin D, Anechitei-Deacu V, Jain M, Murray AS, Porat N, Hao Q and Wintle AG, 2017. On the importance of grain size in luminescence dating using quartz. Radiation Measurements 106: 464‒471, DOI 10.1016/j.radmeas.2017.01.009.Timar-GaborABuylaertJPGuralnikBTrandafir‒AntohiOConstantinDAnechitei-DeacuVJainMMurrayASPoratNHaoQWintleAG2017On the importance of grain size in luminescence dating using quartzRadiation Measurements10646447110.1016/j.radmeas.2017.01.009Open DOISearch in Google Scholar

Tsukamoto S, Geoff AT. Duller GAT and Wintle AG, 2008. Characteristics of thermally transferred optically stimulated luminescence (TT-OSL) in quartz and its potential for dating sediments. Radiation Measurements 43: 1204‒1218, DOI 10.1016/j.radmeas.2008.02.018.TsukamotoSGeoffAT. Duller GATWintleAG2008Characteristics of thermally transferred optically stimulated luminescence (TT-OSL) in quartz and its potential for dating sedimentsRadiation Measurements431204121810.1016/j.radmeas.2008.02.018Open DOISearch in Google Scholar

Wang CC and Li H, 2013. Inferring human history in East Asia from Y chromosomes. Investigative Genetics 4: 11, DOI 10.1186/20412223-4-11.WangCCLiH2013Inferring human history in East Asia from Y chromosomesInvestigative Genetics41110.1186/20412223-4-11Open DOISearch in Google Scholar

Wang XL, Lu YC and Wintle AG, 2006. Recuperated OSL dating of fine-grained quartz in Chinese loess. Quaternary Geochronology 1(2): 89‒100, DOI 10.1016/j.quageo.2006.05.020.WangXLLuYCWintleAG2006Recuperated OSL dating of fine-grained quartz in Chinese loessQuaternary Geochronology128910010.1016/j.quageo.2006.05.020Open DOISearch in Google Scholar

Zhang JF, Huang WW, Hu Y, Yang SX and Zhou LP, 2015. Optical dating of flowstone and silty carbonate-rich sediments from Panxian Dadong Cave, Guizhou, southwestern China. Quaternary Geochronology 30: 479‒486, DOI 10.1016/j.quageo.2015.01.011.ZhangJFHuangWWHuYYangSXZhouLP2015Optical dating of flowstone and silty carbonate-rich sediments from Panxian Dadong Cave, Guizhou, southwestern ChinaQuaternary Geochronology3047948610.1016/j.quageo.2015.01.011Open DOISearch in Google Scholar

Zhang JF, Li YY, Han YS, Wang JK and Zhou LP, 2018. Luminescence dating of weathered sediments from the Paleolithic site of Fengshuzui in northern Hunan province, China. Quaternary Geochronology 49: 211‒217, DOI 10.1016/j.quageo.2018.07.003.ZhangJFLiYYHanYSWangJKZhouLP2018Luminescence dating of weathered sediments from the Paleolithic site of Fengshuzui in northern Hunan province, ChinaQuaternary Geochronology4921121710.1016/j.quageo.2018.07.003Open DOISearch in Google Scholar

Zhang JF and Zhou LP, 2007. Optimization of the 'double SAR' procedure for polymineral fine grains. Radiation Measurements 42(9): 1475‒1482, DOI 10.1016/j.radmeas.2007.06.007.ZhangJFZhouLP2007Optimization of the 'double SAR' procedure for polymineral fine grainsRadiation Measurements4291475148210.1016/j.radmeas.2007.06.007Open DOISearch in Google Scholar

Zhou LP and Shackleton, 2001. Photon-stimulated luminescence of quartz from loess and effects of sensitivity change on palaeodose determination. Quaternary Science Reviews 20(5‒9): 853‒857, DOI 10.1016/S0277-3791(00)00024-X.ZhouLPShackleton2001Photon-stimulated luminescence of quartz from loess and effects of sensitivity change on palaeodose determinationQuaternary Science Reviews205‒985385710.1016/S0277-3791(00)00024-XOpen DOISearch in Google Scholar

Zhu RX, Potts R, Pan YX, Yao HT, Lü LQ, Zhao X, Gao X, Chen LW, Gao F and Deng CL, 2008. Early evidence of the genus Homo in East Asia. Journal of Human Evolution 55: 1075‒1085, DOI 10.1016/j.jhevol.2008.08.005.ZhuRXPottsRPanYXYaoHTLQZhaoXGaoXChenLWGaoFDengCL2008Early evidence of the genus Homo in East AsiaJournal of Human Evolution551075108510.1016/j.jhevol.2008.08.005Open DOISearch in Google Scholar

Recommended articles from Trend MD

Plan your remote conference with Sciendo