OSL dating of individual quartz 'supergrains' from the Ancient Middle Palaeolithic site of Cuesta de la Bajada, Spain

Dose saturation represents a fundamental limitation for obtaining finite optically stimulated luminescence (OSL) quartz ages over Middle Pleistocene timescales. Single-grain OSL studies typically reveal significant intra-and inter-sample variability in quartz dose saturation properties at the individual grain level. This enhanced variability may offer the potential to obtain extended-range chronologies exceeding the traditional upper age limits of multiple-grain OSL dating. However, there have been relatively few detailed assessments of single-grain OSL properties over high dose ranges. In this study we investigate extended-range single-grain OSL dating potential at Cuesta de la Bajada, one of the most important Ancient Middle Palaeolithic sites in the Iberian Peninsula. The quartz samples from this site exhibit exceptional dose saturation properties and contain significant populations of individual 'supergrains' with bright OSL signals, very high characteristic saturation dose (D-0) limits of 200 to >600 Gy, and dose response curves that closely conform to single saturating exponential functions. Assessments of OSL signal composition and the ability to successfully recover a known laboratory dose of 470 Gy support the potential for obtaining high equivalent dose (D-e) values with reasonable fitting uncertainties. A series of novel sensitivity tests are used to assess potential biases in supergrain D-e estimation over high dose ranges related to (i) thermally transferred signal contributions, (ii) choice of dose-response curve fitting function, and (iii) insufficient dose saturation properties of individual grains. The single-grain D-e values obtained using the standard quality assurance criteria and novel sensitivity tests are consistent at 2 sigma, and are in agreement with quartz Ti-centre ages obtained on two of three paired electron spin resonance (ESR) samples collected from Cuesta de la Bajada. These comparisons support the suitability of our single-grain OSL results and suggest there may be good potential for using quartz supergrains to establish extended-range chronologies at some Middle Pleistocene sites. Comparisons with other single grain OSL studies across the Iberian central plains suggest that favourable dose saturation properties may be influenced by regional-scale geological controls. The importance of undertaking single-grain OSL dating at Cuesta de la Bajada is also demonstrated by the results of synthetic aliquot experiments, which reveal multiple-grain age offsets of 60-170 ka when unsuitable grain types are inadvertently included in the final age calculations. The single-grain OSL results indicate that the main archaeological horizon at Cuesta de la Bajada (unit CB3) accumulated between 264 +/- 22 and 293 +/- 241 a. These ages are consistent with the chronologies of other key early Middle Palaeolithic sites in the region (Ambrona AS6 and Gran Dolina TD10) and indicate that the Ancient Middle Palaeolithic techno-complex likely spread across Iberia from at least Marine Isotope Stage 9 onwards. (C) 2016 Elsevier B.V. All rights reserved.