Polymineral Fine Grains Research Articles

Luminescence based loess chronostratigraphy of the Upper Palaeolithic site Krems-Wachtberg, Austria

The loess section Krems-Wachtberg (Lower Austria) is well known for its Upper Palaeolithic find layer, which contains a double and a single infant burial. The layer containing the grave (archaeological horizon AH 4.4) was dated to 26,580 ± 160 14C BP (Einwögerer et al., 2006), corresponding to ca. 31 ka cal BP and is embedded in an 8 m thick loess sequence. In order to provide a chronostratigraphy of the entire section, 38 samples for luminescence dating were taken at high resolution from below and above the find layer. The samples were dated using the quartz coarse grain fraction, the quartz fine grain fraction and/or the polymineral fine grain fraction. The resulting ages are in correct chronostratigraphic order and, in case samples were measured with different protocols, agree within errors with each other and with the radiocarbon age of the find layer. The polymineral fine grain ages are systematically slightly lower than the quartz ages, although no fading could be detected in laboratory experiments. Loess deposition at the site commenced ca. 40 ka ago and reaches up to ca. 22 ka. The ages indicate nearly continuous loess sedimentation throughout this time span. Short breaks in sedimentation probably exist but cannot be resolved due to the uncertainties of luminescence ages.

A combined luminescence and radiocarbon dating study of the Ili loess, Central Asia

Similar to the loess in the Chinese Loess Plateau (CLP), the loess deposits in the Ili basin of Central Asia arid area play an important role in understanding the climate and environmental changes. However, in contrast to the intensively investigated loess deposits in the CLP, the Ili loess is still insufficiently known and poorly understood. The geochronology study of the Ili loess remains controversial. In order to examine the potential of optically stimulated luminescence (OSL) dating for the Ili loess, we carry out a combined luminescence and radiocarbon dating study on a 6.9 m loess section in the south margin of the Ili basin. Polymineral fine grains were investigated by post infrared (IR) OSL using a Multiple-Aliquot Regenerative-dose (MAR) protocol. Radiocarbon dating of organic carbon were carried in a 3 Megavolt (MV) multi-element Accelerator Mass Spectrometry (AMS). The results indicate that the OSL ages are in agreement with the observed stratigraphy in the field, which is well correlated with that of the CLP, but the AMS 14C ages are much younger than the OSL and assumed stratigraphical ages. Thus, the OSL dating technique may provide an absolute chronology in this loess section. Further methodological approaches and more samples analysis will lead to the improvement of this chronology for high-resolution paleoclimatic interpretation.

A comparative study of the luminescence characteristics of polymineral fine grains and coarse-grained K- and Na-rich feldspars

The IRSL and post-IR IRSL (pIRIR) signal characteristics of polymineral fine grains are investigated and compared with those of K- and Na-rich feldspar extracts. TL signal loss after IR and pIRIR stimulations occurs mainly at around 320 °C for polymineral and Na-feldspar samples and around 410 °C for K-feldspar samples, when a preheat temperature of 250 °C for 60 s is used. After preheating to a higher temperature (320 °C for 60 s) all samples show a TL reduction around 410 °C in the blue detection window. Pulse annealing experiments for IRSL and pIRIR signals for preheats between 320 °C and 500 °C indicate that the signal stabilities are similar among the different feldspar types, when a higher preheat temperature (>320 °C) is used. Thermal activation energies for IRSL and pIRIR signals are largest in K-feldspar and smallest in polymineral fine grains, in both blue and UV detection windows for both fast time-resolved (TR) and continuous wave (CW) signals. These results suggest that IRSL and pIRIR signals in polymineral fine grains originate mainly from Na-feldspar grains; these signals are less thermally stable than those from K-feldspar, but a more stable signal (presumably from K-feldspar grains) can be obtained using a higher preheat temperature. ► Luminescence characteristics of polymineral fine grains are investigated. ► IRSL and pIRIR signals from polyminerals are less stable than from K-feldspar. ► Activation energies of IRSL and pIRIR signals from polymineral are lower than that of K-feldspar. ► Majority of luminescence from polymineral fine grains originates from Na-feldspar.

Luminescence properties and optically (post-IR blue-light) stimulated luminescence dating of limnic sediments from northern Lake Malawi – Chances and limitations

Affected by the shifting Intertropical Convergence Zone, Lake Malawi holds an outstanding limnic sediment archive storing palaeo-environmental information of a climatically highly responsive landscape in the East African Rift Valley. Reliable chronological data are essential to interpret the lake-bottom sediments and optically stimulated luminescence (OSL) dating is an important method to build up the chronology. We report on material-property studies and OSL-dating results for polymineral fine grains extracted from piston cores obtained from the northern basin of Lake Malawi during the 1998 campaign of the International Decade of the East African Lakes (IDEAL). OSL-dating is based on a post-IR blue (pIRB) light stimulation single aliquot regeneration (SAR) protocol. Our results support earlier publications demonstrating the general applicability of OSL-dating on Lake Malawi sediments of Holocene and late Pleistocene age. However, the study also shows that dose rate estimations imply major challenges which need to be investigated in more detail to improve future OSL-dating results.

Testing the potential of elevated temperature post-IR IRSL signals for dating Romanian loess

In this study we test the potential of the elevated temperature infrared stimulated luminescence (IRSL) signals for dating Romanian loess. The recently developed post-IR IRSL protocol is applied to Romanian loess using polymineral fine grains extracted from the loess-palaeosol sequence at Mircea Vodă (SE Romania). This approach is aimed at obtaining an additional age control to examine the age discrepancy obtained from previous optically stimulated luminescence (OSL) studies using different grain-sizes of quartz (4–11 μm and 63–90 μm).Two preheat post-IR IR stimulation temperature combinations were used, 250–225 °C and 325–300 °C, respectively. The signals obtained are documented in terms of dose response curve, laboratory tests and fading. Although both post-IR IRSL signals exhibit small fading rates, dose response characteristics indicate that these rates may be laboratory artefacts. The post-IR IRSL signal stimulated at 300 °C is observed to suffer from dose dependent initial sensitivity changes as both natural and regenerated signals are observed to lie above the saturation level of the dose response curve. Uncorrected age results obtained using both post-IR IRSL signals are in general agreement with previously reported silt-sized quartz OSL ages for samples collected from the uppermost loess unit L1. For older material, the post-IR IRSL signal stimulated at 225 °C is considered to provide reliable age results, in agreement with independent age control available for this sequence.

Combined IRSL and post-IR OSL dating of Romanian loess using single aliquots of polymineral fine grains

The paper reports on continuing luminescence investigations of Romanian loess using samples collected from the loess-palaeosol sequence near Mircea Vodă (SE Romania). Previous optically stimulated luminescence (OSL) studies using different grain-sizes of quartz (4–11μm and 63–90μm) yielded discrepant chronologies for the last interglacial–glacial cycle. In this study, a double-SAR protocol is used to determine the age of polymineral fine (4–11μm) grains through their infrared stimulated luminescence (IRSL) and post-IR optically stimulated luminescence (post-IR OSL) emissions in the UV. Laboratory tests confirm the suitability of the protocol for both signals. Fading measurements indicate a significant feldspathic contribution to the post-IR OSL signal. In general, the fading-corrected IRSL and post-IR OSL age results are mutually consistent, and they agree with previously reported OSL ages for fine-grained (4–11μm) quartz. This agreement enhances the reliability of the ages obtained using luminescence signals from fine-grains, and allows more confident correlation of the weakly-developed palaeosol in the uppermost loess unit (L1) with marine isotope stage 3 (MIS3). The fading-corrected ages underestimate the depositional age of older material (units L2–L4), probably owing to limitations of the correction model.

Testing a multi-step post-IR IRSL dating method using polymineral fine grains from Chinese loess

The potential of multi-elevated-temperature post-IR IRSL (MET-pIRIR) dating [Li, B., Li, S.H., 2011. Luminescence dating of K-feldspar from sediments: a protocol without anomalous fading correction. Quaternary Geochronology 6, 468–479] using polymineral fine grains (FG) (4–11μm) is tested using loess samples from the Luochuan section in the Chinese Loess Plateau. Nine FG samples with ages within the last glacial–interglacial period are tested using the MET-pIRIR protocol. The MET-pIRIR results for FG are compared with both the coarse grain (63–90μm) K-feldspar MET-pIRIR dating results and the coarse grain quartz OSL dating results. The stratigraphic age of the profile also provides an independent age control. Our results indicate that the FG MET-pIRIR signals of 200°C and 250°C have negligible anomalous fading and they can give reliable ages for the Chinese loess within the last glacial–interglacial period.

Testing the application of post IR-IRSL dating to fine grain waterlain sediments

The polymineral fine grain fraction of a set of ten known age samples were used to test the suitability of elevated temperature post-IR infrared stimulated luminescence (pIRIR) to date waterlain sediments in Switzerland. Equivalent Dose (De) values were obtained using elevated temperatures of 225 °C (pIRIR225) and 290 °C (pIRIR290) and IRSL50/225 (preceding measurement of pIRIR225), and these displayed a systematic increase with increasing stimulation temperature, which brought those derived from the pIRIR protocols into saturation for the older half of the samples (>100 ka). Significant residuals were recorded for the pIRIR signals, and these were found to further increase following attenuation of the bleaching source confirming that these signals are harder to bleach than the IRSL measured at 50 °C. Fading tests recorded g-values of between 1 and 4%, and displayed no obvious decrease with increasing stimulation temperature. For the younger half of the samples, fading corrected ages for all protocols resulted in overestimation compared to robust independent dating for all samples, and draw into question the relationship of fading measured in a laboratory generated signal to that which is naturally generated. Uncorrected IRSL50/225 ages for all samples were in good agreement with independent dating, but still displayed a general overestimation using pIRIR signals. These overestimations may largely be due to the significant residual doses resulting from the harder to bleach nature of the elevated temperature signal, and present a considerable problem when dating waterlain sediments. A considerable challenge when using the pIRIR signal is to be able to separate the effects of both residual doses and fading and confirm that one is not masking the other. Despite this, the pIRIR protocols were successful at one site, although they offered no benefit compared to dating with more conventional luminescence signals. A comparison of De values derived from a standard IRSL signal to that from IRSL50/225, suggest that the latter overestimates by ∼10% due to a decrease in sensitivity of the sample prior to measurement of the test dose.

On the applicability of post-IR IRSL dating to Japanese loess

Recent work on infrared stimulated luminescence (IRSL) dating has focussed on finding and testing signals which show less or negligible fading. IRSL signals measured at elevated temperature following IR stimulation at 50°C (post-IR IRSL) have been shown to be much more stable than the low temperature IRSL signal and seem to have considerable potential for dating. For Early Pleistocene samples of both European and Chinese loess natural post-IR IRSL signals lying in the saturation region of the laboratory dose response curve have been observed; this suggests that there is no significant fading in nature. As a contribution to the further testing of post-IR IRSL dating, we have used 18 samples from two Japanese loess profiles for which quartz OSL and tephra ages up to 600 ka provide age control. After a preheat of 320°C (60 s), the polymineral fine grains (4–11 μm) were bleached with IR at 50°C (200 s) and the IRSL was subsequently measured at 290°C for 200 s. In general, the fading uncorrected post-IR IRSL ages agree with both the quartz OSL and the tephra ages. We conclude that the post-IR IRSL signal from these samples does not fade significantly and allows precise and accurate age determinations on these sediments.

OSL dating of a Holocene loess-paleosol sequence in the southern Loess Plateau, China

Optically stimulated luminescence (OSL) dating of polymineral fine-grained loess samples collected from the southern Loess Plateau of China was conducted using the single-aliquot regenerative-dose (SAR) protocol. A ‘Double-SAR’ procedure in which aliquots are subjected to both infrared (IR) and blue stimulations was used, and two sets of equivalent dose (D e ) determinations were produced. These doses are assumed to be predominantly related to the feldspathic and quartz fine grain populations, respectively. The results revealed that the OSL ages estimated by infrared stimulated luminescence (IRSL) signals and those estimated by [post-IR] stimulated luminescence ([post-IR] OSL) signals disagreed. Specifically, the ages estimated using the IRSL signals were smaller than those estimated using [post-IR] OSL signals. The results of an anomalous fading test of the two types of OSL signals revealed that the [post-IR] OSL signals from the etched sub-sample (by H2SiF6 and HF) and the un-etched sub-sample did not fade significantly. However, the IRSL signals from the un-etched sub-sample showed obvious signs of fading. These findings indicate that the lower age estimated by IRSL is due to the anomalous fading of feldspar IR signals in the polymineral fine grains. For samples collected from greater than 100 cm, the estimates of their OSL ages using two types of luminescence signals generally agreed with their pre-estimated ages, especially those of the [post-IR] OSL signals. However, for the three samples that were collected from a depth of less than 100 cm, their OSL ages were remarkably underestimated, possibly due to the enhanced human activity (such as soil cultivation) that has occurred in the region since 3000 a B.P.

Luminescence chronology of the upper part of the Stari Slankamen loess sequence (Vojvodina, Serbia)

A thick Middle and Late Pleistocene loess-palaeosol sequence is exposed at the Stari Slankamen section in the Vojvodina region situated in the south-eastern part of the Pannonian basin, Serbia. The profile exposes an about 45 m thick series of loess intercalated by at least eight pedocomplexes. Ten samples were dated by luminescence methods using a modified single aliquot regenerative dose (SAR) protocol for polymineral fine grains and for quartz extracts from the upper part of the Stari Slankamen loess sequence. The infrared stimulated luminescence (IRSL) and post-IR optically stimulated luminescence (OSL) signals from all polymineral samples showed anomalous fading, suggesting that the post-IR OSL signal is still dominated by feldspar OSL. The ages ranging from 4.6 to 193 ka were obtained after fading correction. These ages indicate that the loess unit V-L1L1, the weakly developed soil complex V-L1S1 and the loess unit V-L1L2 were deposited during marine isotope stage (MIS) 2, 3, and 4, respectively, and also indicate that the loess unit V-L2 is of the penultimate glacial age.

Infrared stimulated luminescence and radiofluorescence dating of aeolian sediments from Hungary

Anomalous fading of the infrared stimulated luminescence (IRSL) signal from the polymineral fine-grain and K-feldspar fractions of aeolian sediments from Hungary has been studied. The samples in this study have previously been dated using the multiple aliquot additive dose (MAAD) protocol to measure the IRSL signal. The IRSL measurements using MAAD were conducted ∼4 weeks after the irradiation, making it difficult to assess to what extent these age estimates were affected by anomalous fading. In this study, equivalent doses were obtained using the single aliquot regenerative dose (SAR) protocol. The fading rate for each sample was calculated using the different IRSL components and different parts of the decay curve. For each sample, the middle part of the decay curve always showed a lower fading rate than the initial part of the decay curve. The difference between the fading rates for different parts of the decay curve was greater for the K-feldspars than for the polymineral fine grains. Fading corrected ages were calculated by integrating both the initial and the middle part of the decay curve. These ages were compared with optically stimulated luminescence (OSL) ages from quartz, infrared radiofluorescence (IR-RF) ages obtained from K-feldspars and also with independent ages, provided by radiocarbon dating of shells and charcoal, and uranium-series dating of travertine.

Assessment of diagnostic tests for evaluating the reliability of SAR D e values from polymineral and quartz fine grains

In this study, we applied optically stimulated luminescence (OSL) dating to two fine grain sediment samples collected at Jeongokri, Korea. A single aliquot regenerative dose (SAR) procedure was applied to both polymineral grains and to chemically isolated (H 2SiF 6) quartz grains of 4–11 μm diameter. For polymineral fine grains, the OSL IR depletion ratio and the equivalent dose (D e) plateau test appear to be equally sensitive indicators of appropriate IR stimulation time for use in the ‘double SAR’ protocol. Additionally, the OSL IR depletion ratio test gives an indication of the relative mineral composition of the samples, hence providing an assessment of the likelihood of obtaining a quartz-dominated [post-IR] OSL signal. Use of higher preheat temperatures would assist in thermally eroding the non-quartz component of the [post-IR] OSL signal from polyminerals. For the quartz fine grains, data from both natural D e determinations and laboratory dose recovery tests are required to identify the appropriate preheat temperatures for dating, due to problems of thermal transfer. This phenomenon is particularly exaggerated for these samples due to the large D e values (≥350 Gy) and hence low slope of the dose–response curve. The double SAR method cannot be applied ubiquitously, even after careful and rigorous study of one sample from a section. Quartz OSL dating using a range of preheat temperatures is suggested to be the most suitable method for OSL dating of fine grain sediments.

Luminescence and amino acid racemization chronology of the loess–paleosol sequence at Süttő, Hungary

The loess–paleosol sequences in Hungary provide an excellent Upper Pleistocene climate archive of the Carpathian Basin. Loess deposits up to 20 m thick cover the Süttő travertine complex, located in the very northern part of Hungary, next to the right bank of the Danube River. The loess is intercalated with two weakly developed greyish horizons, two thinner-brownish steppe-like soils and a pedocomplex, including a reddish-brown clay-enriched horizon covered by a chernozem-like paleosol. Infrared optically stimulated luminescence (IRSL) dating was applied on polymineral fine grain material to determine the depositional age of the loess. The uppermost loess yields IRSL age estimates ranging from 15 to 40 ka. The loess on top of the pedocomplex yields IRSL age estimates ranging from 48 to 60 ka. The pedocomplex most likely correlates with the Marine Oxygen Isotope Stage (MIS) 5 interglacial period. The loess from below the pedocomplex was deposited during the penultimate glaciation, as evidenced by amino acid racemization (AAR) results. Further independent age control is provided by radiocarbon dating for the upper part of the profile and by uranium-series ( 230Th/ 234U) ages correlating the travertine below the loess with MIS 7–8. The magnetic susceptibility record through the sequence shows a strong correlation with the loess layers and soil horizons.

Uncertainties on the Luminescence Ages and Anomalous Fading

It is well known that some minerals give underestimated luminescence ages due to anomalous fading. The anomalous fading follows a logarithmic decay law characterized by its slope, the socalled fading rate or g-value. Using the fading rate, Huntley and Lamothe (2001) suggested some correction for the fading underestimation of young samples (<40-50 ka). For polymineral fine grains, we observe a fading rate of 0-4%/decade for TL and BL-OSL and 4-6%/decade for IR-OSL. Extending the laboratory observation to archaeological age, the underestimation on the age for 10 ka is estimated to a mean of 5% for TL, 10% for BL-OSL and 45% for IR-OSL. Due to the non-linearity of the Huntley and Lamothe's fading correction, the contribution of the fading to the total uncertainty is estimated by a Monte-Carlo simulation. The inference on dating shows that the uncertainty on the anomalous fading can be a significant term of the combined uncertainty on the age, even for low fading rates.

Luminescence Dating of Neolithic Ceramics from Lumea Nouă, Romania

Luminescence dating was applied to four Neolithic pottery fragments excavated at Lumea Nouă (Alba Iulia, Romania), with the purpose of improving the chronology for the archaeological finds, and hence, the occupational history of the site. The single-aliquot regenerative-dose (SAR) protocol was applied to both blue and infrared stimulated luminescence signals from coarse quartz and polymineral fine grains, respectively. A more conventional approach which uses a multiple-aliquot additive-dose protocol and thermoluminescence signals from polymineral fine grains was applied as well. The characteristics of the OSL and IRSL signals were investigated in terms of behaviour in the SAR protocol, dose response and dose recovery. Additionally, anomalous fading measurements of the 410 nm IRSL emission and of the blue TL emission from polymineral fine-grains were performed. Both signals were observed to be affected by anomalous fading. OSL dating of quartz using the SAR protocol is considered to be the technique of choice; it yields an average age of 6.0±0.4 ka (n = 4), which is in agreement with archaeological expectations. The dating results allow refining the typological interpretation of the objects and improve the chronological framework for the site.

Residual Doses in Recent Alluvial Sediments From the Ardenne (S Belgium)

Residual Doses in Recent Alluvial Sediments From the Ardenne (S Belgium) We report on our first investigations into the potential of optical dating for determining the rate of river flood sedimentation in the Ardenne region (S Belgium). Two samples collected from a recent alluvial deposit were used to investigate the extent of resetting in different particle size fractions of quartz (4-11 μm, 63-90 μm, 90-125 μm, 125-180 μm, 180-212 μm and 212-250 μm) as well as in polymineral fine (4-11 μm) grains. Both samples show satisfactory OSL and IRSL characteristics. The IRSL signals from the polymineral fine grains yield an equivalent dose (De) of 3-4 Gy, while a De of 0.3-0.6 Gy was measured using large aliquots of quartz. Small aliquot analyses of 63-90 μm and 212-250 μm quartz grains confirm that the coarser fraction contains more grains with lower De's. Furthermore, for a modern sample (< 3 years old), ~60% of the aliquots yields a De consistent with zero, indicating that these contain only well-bleached grains. These findings suggest that it might be possible to extract the true burial dose from dose distributions measured using small aliquots of coarse-grained (e.g. 212-250 μm) quartz.

Optimization of the ‘double SAR’ procedure for polymineral fine grains

The “double SAR” protocol has been used to measure the equivalent dose of polymineral grains from fine-grained samples. However, the optical ages obtained with this protocol using the different luminescence signals from a sample are not always consistent. Quartz optical ages are believed to be more reliable than feldspar ages. The post-IR OSL signals from polymineral fine grains are believed to be dominated by the signal from quartz. The ages obtained with the “double SAR” protocol using the post-IR OSL signals from polymineral fine grains are therefore considered to be more reliable than those obtained using the IRSL signals. Thus, the feldspar contribution to the post-IR OSL signals should be reduced as much as possible. In this paper, the effects of IR-stimulation temperature and duration before OSL measurement on the post-IR OSL signals from quartz extracts and polymineral grains, and their equivalent dose values were tested. The results show that the IR stimulation causes the quartz post-IR OSL signals to be reduced even at room temperature if the IR stimulation lasts long enough, but does not affect quartz equivalent dose estimation using post-IR OSL signals. In the ‘double SAR’ procedure, the IR-stimulation time should be determined by an IR-bleaching D e plateau test, and the bleaching should preferably be performed at room temperature.

Optical dating of Chinese loess using sand-sized quartz: Establishing a time frame for Late Pleistocene climate changes in the western part of the Chinese Loess Plateau

The Chinese Loess Plateau (CLP) is of major interest to Quaternary geologists because it represents an important terrestrial archive of palaeoclimatic fluctuations. Previous multiple-aliquot luminescence dating studies of Chinese loess mainly used thermoluminescence (TL) and infrared stimulated luminescence (IRSL) signals of polymineral fine-grains; these are known to be subject to anomalous fading and thus will tend to yield age underestimations. In this paper we investigate whether the blue-light stimulated luminescence (BLSL) signals from 63 to 90μm quartz grains extracted from three western Chinese loess sites (Zhongjiacai, Le Du and Tuxiangdao) can be used to establish a reliable chronology. The single-aliquot regenerative-dose (SAR) procedure is used for the equivalent dose (De) determinations and the suitability of our measurement protocol is confirmed by dose recovery tests. The influence of an IRSL signal on the quartz De measurements derived from BLSL has been investigated. From these results we conclude that an IRSL contamination, expressed as an IRSL/BLSL ratio, of up to 10% can be accepted before the values of De are significantly affected. All three sites yield stratigraphically consistent and spatially highly reproducible optical ages up to about 50–70ka. At the Tuxiangdao site a marked hiatus in the record is identified between ∼20 and ∼30ka; this remained undetected in previous studies and clearly highlights the importance of high-resolution optical dating in Chinese loess research. The optical ages presented in this work provide more evidence for episodic loess deposition and varying loess accumulation rates in the western part of the CLP. Our study seems to confirm the potential of optically stimulated luminescence (OSL) dating using the SAR procedure applied to the very fine sandy quartz fraction in Chinese loess back to ∼40–50ka (∼120–150Gy).

Chronology of an oyster reef on the coast of Bohai Bay, China: Constraints from optical dating using different luminescence signals from fine quartz and polymineral fine grains of coastal sediments

Fossil oyster reefs are indicators of past sea levels, and their formation is usually dated by means of radiocarbon. However, radiocarbon dating of the shells from coastal areas may be complicated by the varying sources of carbon. Here we applied optical dating methods to date the samples from above and below a fossil oyster bed in a section on the coast of Bohai Bay, China. The optical ages of the sediments were used to constrain the oyster bed. Single-aliquot regenerative-dose procedures using the OSL signal from fine grain quartz, the IRSL and post-IR OSL signals from polymineral fine grains were employed to determine equivalent dose ( D e). The behaviors of the different luminescence signals from quartz and polymineral grains during D e measurements were examined. The results showed that the quartz OSL signal is more reliable than the polymineral IRSL and post-IR OSL signals with respect to dating for these coastal samples. The optical ages indicated that the oyster reef formed between ca. 6.2 and 5.0 ka.