Quaternary Science Reviews 20 (2001) 719}724 The potential of OSL and TL for dating Lateglacial and Holocene dune sands tested with independent age control of the Laacher See tephra (12 880 a) at the Section &Mainz-Gonsenheim'夽 U. Radtke *, A. Janotta , A. Hilgers , A.S. Murray Department of Geography, University of Cologne, Albertus-Magnus-Platz, D-50923 Cologne, Germany Nordic Laboratory for Luminescence Dating, Department of Earth Sciences, Aarhus University, Ris~ National Laboratory, DK-4000 Roskilde, Denmark Abstract Optically stimulated luminescence (OSL) and Thermoluminescence (TL) are applied in this study to date a Lateglacial and Holocene aeolian sediment sequence. Quartz and potassium rich feldspars extracted from dune sands from western Germany were dated using both multiple-aliquot (MA) and single-aliquot (SA) protocols for luminescence dating. This particular dune section was chosen for this test study, because an independent age control is provided by a horizon of the Laacher Seetephra (12,880 a). In contrast to the results for potassium feldspars, which show underestimation of up to 25%, the quartz fraction provides promising results with respect to the presumed geological ages. 2000 Elsevier Science Ltd. All rights reserved. 1. Introduction We present the results of a systematic investigation of 12 samples of the dune section &Mainz}Gonsenheim' near the river Rhine close to Mainz (about 50300'25''N, 8311'10''E) in Rhineland}Palatinate, Germany. This study is part of a long-term research project which deals with the di!erent phases of dune accumulation in Central Europe during the Lateglacial and Holocene. One of the main problems is to determine whether the sand was deposited within a small number of short periods of high aeolian activity or if dunes and cover sands result from a more or less continuous accumulation. The dune at Gonsenheim was chosen to test the potential of luminescence dating for Lateglacial and Holocene dune sands because an independent age control is provided by a layer of Laacher See tephra. This stratigraphic marker horizon was dated with varve chronology at 12 880 a (Brauer et al., 1997). 2. Description of the site The dune section &Mainz}Gonsenheim' is located about 2 km south of the river Rhine in an extensive 夽 Paper published in December 2000. * Corresponding author. Fax: 0049-221-4705124. E-mail address: [email protected] (U. Radtke). aeolian sand sheet. The river terrace deposits of the Pleistocene braided river system yielded the material for widespread de#ation processes during the Late Weichselian and Postglacial time. The main accumulating winds are assumed to be from the north west. In Fig. 1 a model is shown which summarises the di!erent phases of dune accumulation at the location &Mainz-Gonsenheim' following the interpretation of StoK hr (1966) and Hanke and Maqsud (1985). A description of the sediments exposed at the section &MainzGonsenheim' and the sampling positions are presented in Fig. 2. The accumulation of the dune started during the late Pleniglacial and Oldest Dryas period, when a low water level of the river Rhine together with a sparse vegetation cover as a result of cold and dry climate conditions caused the exposure of extensive de#ation areas. A charcoal C age of 15.2$0.4 ka (uncal.) BP (Hanke and Maqsud, 1985) from the bottom of Section 9 (Fig. 2) supports this interpretation. An indication on strong aeolian processes with high accumulation rates is the homogeneity of the sediment (Section 9 in Fig. 2). The two weakly developed palaeosols, which are separated by a layer of unweathered windblown sand (Section 7 in Fig. 2, sample MG8), are correlated with the B+lling- and Aller+d-interstadial period, respectively (Sections 8 and 6 in Fig. 2). The chronostratigraphic marker of this section, &25 cm thick layer of the Laacher See tephra (Section 5 in Fig. 2, sample MG7), was deposited directly 0277-3791/01/$ - see front matter 2000 Elsevier Science Ltd. All rights reserved. PII: S 0 2 7 7 - 3 7 9 1 ( 0 0 ) 0 0 0 2 7 - 5 720 U. Radtke et al. / Quaternary Science Reviews 20 (2001) 719}724 eral later phases of remobilization of dune sands after the Subboreal (see Fig. 1 phase VI and VII). These sediments are not exposed at our sampling section, but are documented as widespread in the local area (Hanke and Maqsud, 1985). 3. Measurement facilities and equivalent dose (D ) determination Fig. 1. Model of the dune development and the di!erent phases of sediment accumulation at the section &Mainz-Gonsenheim' (modi"ed from StoK hr, 1966; Hanke and Maqsud, 1985). Phase I and II: Last Glacial Maximum-Oldest Dryas (1) B+lling, (2) Older Dryas (3) Aller+d, (4) Plase III: Laacher See Tephra, (5) Reworked sediments (Younger Dryas) (6) De#ation, accumulation and cryoturbations (Younger Dryas), (7) Phase IV and V: Preboreal } initial soild development (8) Atlanticum } development of Luvisol (9) Phase VI and VII: Subboreal } mobilisation and accumulation of wind-borne sands, (10) Subatlanticum } di!erent phases of mobilisation (de#ation, accumulation, younger dunes, Ap-horizon, development of Luvisol, initial Regosol) (11). on the presumably Aller+d-palaeosol. The unusual thickness of the layer is explained by the location of the section on the leeward side of the dune: strong winds short after the deposition caused the de#ation of the tephra on the windward position and the accumulation in the lee. The subsequent covering with reworked sediments during the Younger Dryas period prevented later de#ation of the tephra. Strong aeolian as well as cryogenic processes are typical of the stadial climate conditions of the Younger Dryas. The period of high aeolian activity lasted until the beginning of the Preboreal (Sections 4 and 3 in Fig. 2, samples MG6-3). During the Atlanticum a luvisol developed from these sediments (Section 2 in Fig. 2, samples MG 2-1). With the increased population in the study area, human impact on the landscape caused sev- All samples were prepared in subdued red light ('600 nm). The grain size fraction of 100}200 lm was extracted by dry sieving. Samples were then treated with hydrochloric acid, sodium oxalate and hydrogen peroxide in order to remove carbonates, clay and organic material. For mineral separation solutions of sodium polytungstate (2.58, 2.62 and 2.7 g cm\) were used to concentrate the quartz fraction and separate the potassium rich feldspars ((2.58 g cm\). To avoid contamination with feldspars the quartz samples (MG6, 7 and 8) were etched in 40% hydro#uoric acid for 40 min, followed by a treatment with hydrochloric acid to remove acid-soluble #uorides and re-sieving of the residual-quartz grains. All samples were "xed with silicone oil spray on 10 mm diameter discs, of stainlesssteel in the case of SA and of aluminium in the case of MA measurements. Several luminescence methods were applied: IRSL and TL (regeneration and additive dose method) on K-feldspars and GLSL and TL (regeneration dose method) on quartz. A detailed description of these datasets is given in Radtke and Janotta (1998). Here we report in particular on further investigations on the three samples, MG 6, 7 and 8, taken from above, within and below the Laacher See tephra horizon (see Fig. 2). In addition to the other procedures, single-aliquot measurements were employed using the single-aliquot regenerative-dose protocol (SAR) for quartz, as most recently described by Murray and Wintle (2000). All luminescence measurements were performed using automated Ris+ readers (type TL-DA-12). The multiplealiquot measurements were carried out at the laboratory in Cologne and the single-aliquot measurements at the Ris+ National Laboratory in Roskilde. Important details and di!erences between the protocols employed in this study are summarised in Table 1. The equivalent doses were calculated using the integrals as noted in Table 1. For all OSL measurements of quartz the luminescence detected in the last 10 s of stimulation was subtracted as background signal (Murray and Wintle, 2000). To calculate the D based on the SAR measurements the preheat plateau from 1603 to 3003C ("rst dataset, n"24 aliquots) and 180}2803C (second dataset, n"19), respectively, was used (Murray and Wintle, 2000). The gamma-doses used for irradiation of the subsamples (n"35) for the MA measurements were: 4.45, 8.9, 17.8, 35.6, 71.2, 124.6, 178 Fig. 2. The dune section &Mainz-Gonsenheim': description of the horizons, sample positions and results of the luminescence dating. (} D not determinable, n.m. not measured). U. Radtke et al. / Quaternary Science Reviews 20 (2001) 719}724 721 722 U. Radtke et al. / Quaternary Science Reviews 20 (2001) 719}724 Table 1 Measurement parameters for the di!erent protocols Multiple-aliquot protocols Quartz (HF etched) K-rich feldpars Quartz Single-aliquot protocol IRSL-MAR TL-MAR IRSL-MAA TL-MAA GLSL-MAR-1 TL-MAR GLSL-MAR-2 BLSL-SAR Several hours with sunlight Co!csource HA3-BG39 Several hours with sunlight Co!csource HA3-BG39 * * Co!csource HA3-BG39 Several hours with sunlight Co!csource HA3-U340 Several hours with sunlight Co!csource HA3-2;U340 100 s with blue diodes Sr/Y!bsource HA3-3;U340 Preheating * 2303C/60 s Co!csource HA3-BG392;BG3GG400 * Several hours with sunlight Co!csource HA3-U340 2303C/60 s 2203C/300 s * 2203C/300 s Stimulation IR-diodes Heating up to IR-diodes (880$80 nm) 4503C with (880$80 nm) 53C/s 503C * 503C 2}50 s 280}420 s 2}50 s Plateau: 10 s 160}3003C, 180}2803C Blue diodes (470$30 nm) Bleaching Irradiation Filterset for detection Aliquot temp. Integral used for D calculation Heating up to Blue/green 4503C with broad-band 53C/s (420}550 nm) * 503C 280}420 s 2}50 s Heating up to Blue/green 4503C with broad-band 53C/s (420}550 nm) * 1253C 280}420 s 0}0.4 s 1253C 0}0.4 s Note: MAR * multiple-aliquot regenerative-dose protocol, MAA * multiple-aliquot additive-dose protocol Gy. Nine or 13 discs were used to measure the natural luminescence signal for the MA protocols. In Fig. 3 all D values obtained for the samples MG 6, 7, and 8 are compared. The di!erences in the measurement equipment make the comparison di$cult (see Table 1, e.g. di!erent stimulation sources used for MA and SA quartz measurements), but nevertheless the discrepancies are clear. Two facts have to be emphasised: "rst, the distinct di!erence between the D value determined by using the SA protocol and all values obtained by applying the MA protocols, which is not dependent on the mineral fraction used; and secondly the broader error bars of all MA equivalent dose values compared with the SA value. The signi"cant deviation between the MA and the SA equivalent doses of quartz could be possibly due to sensitivity changes, which are measured and corrected for with the SAR protocol, but not with the MAR protocol. The sensitivity changes observed between the SAR natural and the "rst regeneration cycle were by a factor of 1.11 (MG6), 1.10 (MG7), and 1.12 (MG8). This increase in sensitivity must have been present in the MAR data sets as well, but was not measured and not corrected for in the MAR measurement routine. The feldspar MA D results should be &30% greater than the quartz data resulting from the higher internal dose rate of K-feldspars; this is not observed here. Comparing the equivalent doses of the MAR protocols for feldspar (IRSL preheated) and etched quartz (GLSL-2) the feldspar D values for samples MG6-8 are only 8, 3, and 15% higher than those obtained for the quartz fraction (see Fig. 3). This should result in a greater age underestimation of the potassium feldspars compared to the quartz fraction than the calculated ages really show (for samples MG6}8 underestimation &11%). One explanation could be the problems with the determination of the internal K content of the K-feldspars by Fig. 3. Comparison of the equivalent doses of the samples MG6, 7, and 8 obtained with di!erent protocols for quartz (Q) and potassium rich feldspars (F). U. Radtke et al. / Quaternary Science Reviews 20 (2001) 719}724 723 Table 2 Dose rates (D ), equivalent doses (D ) and calculated luminescence ages for the samples MG6, 7 and 8 Sample D in Gy/ka D in Gy Age in ka NAA (U, Th), X-ray #uores. (K) c-Spec. Quartz GLSL-MAR-2 Quartz BLSL-SAR Quartz - GLSL-MAR-2 and NAA/X-ray-#uores. Quartz - BLSL-SAR and c-Spec. MG6 1.99$0.07 2.58$0.08 26.1$4.2 13.10$2.89 MG7 3.09$0.10 3.81$0.11 30.7$4.9 MG8 2.28$0.13 2.44$0.08 27.8$5.0 36.6$1.4 34.6$1.1 44.4$1.0 45.4$1.0 37.1$0.9 35.6$1.2 14.16$1.37 13.39$1.24 11.65$0.98 11.91$0.99 15.22$1.45 14.60$1.47 9.94$2.17 12.19$3.12 Second dataset: preheat plateau 180}2803C. b-counting. Whereas for MG8 with 11.7% a typical value for potassium feldspars was obtained (Huntley and Baril, 1997), for samples MG6 and 7 with &7.4% very low contents were measured. This problem is presumably sample speci"c. The better precision of the quartz D values obtained with the GLSL-MAR-2 protocol than of the MAR-1 equivalent doses (see Fig. 3) is probably due to the normalisation procedure (0.1 s optical stimulation prior to bleaching and irradiation), which was carried out in the case of MAR-2 but not for MAR-1. Whereas a higher precision of SA measurements in contrast to MA measurements is one advantage of the SA protocols (see, for example, Banerjee et al., 2000), we can give no "nal explanation for the di!erence in the values of the MA and SA protocols. 4. Dose rate (D0 ) estimation The results of the dose rate calculation for all 12 samples, using Neutron-Activation-Analysis (NAA), Xray #uorescence for the determination of the radionuclide contents of the sediment, and beta-counting for measuring the internal K-content of the potassium rich feldspars, are described in detail in Radtke and Janotta (1998). For age calculation based on the results of the MA measurements the uranium and thorium contents as determined by NAA and the potassium contents as measured with X-ray-#uorescence were used (see Fig. 2 for luminescence ages obtained by applying the regeneration method). High resolution gamma-spectrometry was carried out at the Ris+ laboratory on samples MG6, 7, and 8. In Table 2 we compare the annual dose rates resulting from gamma-spectrometry with those based on NAA (for U and Th) together with X-ray-#uorescence (for K). The di!erence in the calculated dose rates is obvious. Radioactive disequilibrium did not cause this di!erence in the dose rates as could be seen from the results of the gamma-spectrometry. The deviation is possibly due to the di!erence in sample sizes used for analysis (more than 200 g for gamma-spectrometry and only several mg for NAA). For the samples MG6 and 7, in particular, an inhomogeneous distribution of volcanic material in the samples could give rise to the variances in dose rates, which are signi"cantly larger than for sample MG8 (taken from unweathered dune sand, see Fig. 2). The ratios of gamma-spectrometry dose rates to NAA/XRF dose rates are 1.30$0.09 (MG6), 1.24$0.08 (MG7) and 1.08$0.10 (MG8) showing the best, but still not good, agreement for sample MG8. 5. Discussion and conclusion We applied several protocols with the aim of testing their potential for dating sediments deposited during the Lateglacial and Holocene. Because of the broad spread of the data and partly because of the broad error bars (see Fig. 3 for samples MG6, 7 and 8) the results of the luminescence measurements are not satisfactory, although the high precision of the equivalent doses obtained with the SAR protocol is encouraging when compared with the results of the multiple-aliquot protocols (see Fig. 3). The comparison of the dose rates based on NAA and gamma-spectrometry, respectively (see Table 2), is also unsatisfactory and further investigations will be undertaken to "nd out the reason for the di!erence of the results. All results of luminescence dating, regardless of the method and protocol used (see. Fig. 2), prove the Lateglacial and early Holocene age of the dune, as expected from the relative chronology (see Fig. 1). As described in detail in Radtke and Janotta (1998) the ages of the potassium feldspar fraction tend to show age underestimations when compared with the quartz ages and the independent age control provided by the Laacher See tephra and the C age of about 15 ka uncal. BP for the bottom part of the dune (see Fig. 2). 724 U. Radtke et al. / Quaternary Science Reviews 20 (2001) 719}724 Although there are still problems, we conclude that there is, in general, a high potential for dating Holocene and Late Pleistocene dune sands with luminescence dating. But at this point we cannot decide de"nitively which luminescence dating protocol is the most suitable. Considering the results with respect to the age control provided by the Laacher See tephra, we would give preference to the ages calculated from the results of the SAR measurements of quartz combined with the dose rate determination based on gamma-spectrometry. These ages show both: the highest precision and the best accuracy of the samples dated in this study; in particular the sample from within the tephra layer (MG7, 11.9$1.0 ka) is in good agreement with the independent age of 12.9 ka. Nevertheless, it is not acceptable that for the same samples, di!erent dose rates and equivalent doses could be obtained which result in similar ages. The sample preparation was all carried out in one laboratory, therefore we can exclude that the preparation procedures and laboratory conditions caused the di!erences. Further factors are to be investigated, e.g. the in#uence of di!erent wavelengths used for bleaching in the application of the regeneration method (full sunlight spectrum for MA protocols and blue diodes for SA measurements). Acknowledgements This study was "nancially supported by the Deutsche Forschungsgemeinschaft (DFG, grant Ra 383/3). Our thanks to Prof. Dr. G. Schmitt and Dipl.-Phys. B. Bannach for making possible the irradiation with the Co-source at the Department of Nuclear Medicine of the University of DuK sseldorf, Germany. Prof. Dr. em. A. Semmel is thanked for enabling the sampling at Mainz-Gonsenheim and helpful comments on the "eldwork. The visit of A. H. to the Ris+ Laboratory was funded by the &KaK the-Hack'-foundation (University of Cologne). References Banerjee, D., B+tter-Jensen, L., Murray, A.S., 2000. Estimation of the quartz equivalent dose in retrospective dosimetry using the singlealiquot regenerative-dose protocol. Applied Radiation and Isotopes (2000) in press. Brauer, A., Endres, C., Negendank, J.F.W., 1997. Lake Meerfelder Maar annually laminated record-varve chronology and Lateglacial and early Holocene environmental changes. WuK rzburger Geographische Manuskripte 41, 39}40. Hanke, L., Maqsud, N., 1985. Pedologisch-stratigraphische Untersuchungen in Flugsanden westlich von Mainz. Mainzer Naturwissenschaftliches Archiv 23, 201}222. Huntley, D.J., Baril, M.R., 1997. The K content of the K-feldspars being measured in optical dating or in thermoluminescence dating. Ancient TL 15 (1), 11}13. Murray, A.S., Wintle, A.G., 2000. Luminescence dating of quartz using an improved single-aliquot regenerative-dose protocol. Radiation Measurements 32, 57}73. Radtke, U., Janotta, A., 1998. Ein Beitrag zur Beurteilung der Aussagekraft von Lumineszenzaltern fuK r die Datierung von spaK tpleistozaK nen und holozaK nen DuK nen anhand des Laacher SeeTu!es (12.900 J.v.h.): Der Testfall. DuK ne Mainz-Gonsenheim. KoK lner Geographische Arbeiten 70, 1}18. StoK hr, W.T., 1966. Die Bims-Eruptionen im Laacher-See-Gebiet. Zeitschrift der Deutschen Geologischen Gesellschaft 116, 994}1003.
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