European Middle and Upper Palaeolithic radiocarbon dates are often older than they look: problems with previous dates and some remedies.

European Middle and Upper Palaeolithic radiocarbon dates are often older than they look: problems with previous dates and some remedies. Introduction The European Middle to Upper Palaeolithic is widely accepted asbeing the transitional period over which the final Neanderthals becameextinct and were replaced by anatomically modern humans (Mellars 1989,1999; Zilhao & D'Errico 1999; Zilhao 2006 and referencestherein). Questions of major importance arise. Did Neanderthalsindependently develop symbolic and adaptive behaviours before the ~36500 [sup.14]C BP arrival of modern humans in Western Europe Western EuropeThe countries of western Europe, especially those that are allied with the United States and Canada in the North Atlantic Treaty Organization (established 1949 and usually known as NATO). ? Did theycopy incoming modern human behaviour ('acculturation') whilstthe two co-existed in the few millennia prior to Neanderthal extinction?Where, when and how did Neanderthals become extinct and how did theirextinction relate to the spatial dispersai of modern human populations?Did Neanderthals and modern humans meet, were they contemporaries insome or all parts of Europe, and did they mate? The resolution of many of these questions awaits an unambiguous andreliable chronology, bur for 50 years, this has been unattainable.Radiocarbon dates exhibit an asymptotic tendency as they approach themeasurement limit, which is itself determined in individual laboratoriesby careful repeat radiocarbon measurements of material known to bebeyond the reach of the technique, i.e. greater than about 60 000 or 70000 years old (Chappell et al. 1996). Subsequent radiocarbonmeasurements can never be older than this, since if a radiocarbon dateis within two standard deviations of the background value, a'greater than' age is calculated. Several scholars have attempted to explore the issues usingdatabanks of radiocarbon dates obtained from archaeological sites (e.g.Bocquet-Appel & Demars 2000, bur see Pettitt & Pike 2001; Joriset al. 2003; van Andel et al. 2003; Dolukhanov & Shukurov 2004;Gamble et al. 2004, 2005; Kuzmin & Keates 2005) and receivedguidance on how best to view the many available dates (Pettitt et al.2003). But research undertaken by the Oxford Radiocarbon AcceleratorUnit (ORAU ORAU Oak Ridge Associated Universities ) over the last decade throws doubt on the validity of many ofthese published dates. The principal areas of error lie in the selectionof inappropriate samples and the effects of inadequate pre-treatment toremove contamination. This paper addresses some of the problems andillustrates recent progress and a way forward. Sample selection It is clear that many samples dated in the past have failed to passthe basic test of bearing witness to the presence of humans. Types ofuseful samples include cut-marked or humanly-modified bones, humanremains, organic artefacts or charcoal from clearly identified features,such as hearths. It is axiomatic ax��i��o��mat��ic? also ax��i��o��mat��i��caladj.Of, relating to, or resembling an axiom; self-evident: "It's axiomatic in politics that voters won't throw out a presidential incumbent unless they think his challenger will that all of these samples must comefrom secure archaeological contexts, bur even if they do not, they havethe distinct advantage over other types of nondescript bone of stillbeing able to provide information regarding the age of human presence.Samples of bone without cut marks ought to be avoided because they maybe deposited by animals such as hyena that regularly use the same typesof cave and rockshelter sites frequented by humans. Such problems havebeen particularly acute in the British Paiaeolithic (Jacobi et al.2006), but are almost certainly more widely applicable. In some contextsit is exceedingly difficult to identify cut marks, since surfaceetching, degradation, overprinting by animals and deposits of carbonateand sediment can obscure them. Without careful sample selection, noamount of improved pre-treatment chemistry will result in accurate ages. Contamination Samples of Middle/Upper Palaeolithic age are particularlysusceptible to errors from contamination. Whilst laboratory and chemicalbackground is quantifiable, however, trace contamination derived fromarchaeological contexts rarely is. It is this material that may beresponsible for producing finite dates for samples that are, in reality,older than the [sup.14]C limit. Historically, this has left us asituation in which we now have many radiocarbon ages that areartificially younger than they ought to be. In some rare instances, it is possible to recognise the scale oferror. The Spanish site of El Sidron is important because it containsone of the largest groups of Neanderthal bones ever found: the remainsof nine individuals (Fortea et al. 2003). It is interesting for datingbecause it is likely that the individuals in the site died at the sametime. Their bones are covered in innumerable cut marks (Fortea et al.2003) and some of the associated lithics could be refitted (Santamariaet al. 2010). A series of direct radiocarbon dates from the site areshown in Figure 1 (after De Torres et al. 2010). A wide range of datesis apparent, from 49 000--48 000 BP to 11 000-10 000 BP. OSL OSL Open Source LabOSL Office of Student LifeOSL Open Source LicenseOSL Oregon State LibraryOSL Order of St Luke the PhysicianOSL Optical Stimulated LuminescenceOSL Oud Strijders Legioen (Dutch)OSL Order of Saint Luke datesbracketing the human remains suggest that they were deposited between47-30 ka cal BP. This suggests, therefore, a significant problem withthe radiocarbon ages, particularly the youngest samples. Sensibly, DeTorres et al. (2010) consider the youngest ages to be severelyunderestimating the real age and blame unremoved contamination. [FIGURE 1 OMITTED] A second example comes from work on Neanderthal DNA DNA:see nucleic acid. DNAor deoxyribonucleic acidOne of two types of nucleic acid (the other is RNA); a complex organic compound found in all living cells and many viruses. It is the chemical substance of genes. by Krause etal. (2007), in which radiocarbon dates were obtained from a singleNeanderthal sub-adult humerus humerus:see arm. from Okladnikov Cave in the AltaiMountains Altai MountainsRussian Altay Chinese Altay Shan Mongol Altayn NuruuMountain system, Central Asia. The range extends about 1,200 mi (2,000 km) in a southeast-northwest direction from the Gobi Desert to the West Siberian Plain, through parts of of Siberia. Despite very well-preserved bone being dated, theresults from three laboratories showed great variation, from 29 990 [+or -] 500 BP (KIA-27011), to 34 860 [+ or -] 360 BP (Beta-186881) and 37800 [+ or -] 450 BP (OXA-15481). Krause et al. (2007) lend more credenceto the Oxford determination than the others, but chose to average theresults (to 34 190 [+ or -] 760 BP) to estimate the age of the specimen.It is highly doubtful whether this is a meaningful value because not allof these dates can possibly be accurate. These results do not inspire confidence, but why is there suchvariation? Although ancient carbon contaminants are of concern, theirpresence is virtually insignificant compared with the equivalentproportion of modern contamination. The addition of l0 per cent oldcarbon to a sample dating to 40 000 BP would yield a date of 40 800 BP,only marginally too old even accounting for the sometimes large errorterms on measurements of this age. Even 20 per cent old carboncontamination would only give an age of 41 600 BP. And these arecontamination levels that radiocarbon specialists would considerunusually high. The effect of more recent contamination is dramatically different;add 10 per cent modern carbon to the sample and the age is 18 000 BP.Even 0.5 per cent of modern contamination gives a wholly distorted age(35 600 BP). Therefore, in assessing the reliability of radiocarbon agesfrom the Palaeolithic, it is usual to consider older ages as being morelikely to be closer to the 'true' age than younger ones. Theyounger dates from El Sidron or Ohkladnikov mentioned above, therefore,are almost certainly erroneous and the reason is probably due tonon-autochthonous carbon. Remedial measures--bone About half of the available corpus of [sup.14]C dates from theEuropean Palaeolithic are dates of bone, the material targeted fordating being almost always the protein collagen, which has awell-defined structure. Most facilities pre-treat bone in a similarmanner using a two-step process, the first removes the mineral fraction(hydroxyapatite hydroxyapatite/hy��droxy��ap��a��tite/ (-ap��ah-tit) an inorganic calcium-containing constituent of bone matrix and teeth, imparting rigidity to these structures. , about 80 per cent of the bone by weight), and thesecond stage gelatinises the bone collagen using a technique firstapplied by Longin (1971). This process brings the collagen into solutionand separates it from insoluble residues. Since 2000, the ORAU has applied an additional ultrafiltration stepto the process, based on Brown et al. (1988). An ultrafilter is a typeof molecular sieve A molecular sieve is a material containing tiny pores of a precise and uniform size that is used as an adsorbent for gases and liquids.Molecules small enough to pass through the pores are adsorbed while larger molecules are not. , which separates protein chains above and below acertain molecular weight (MW). Since an undegraded polypeptide polypeptide:see peptide. chainfrom a collagen molecule weighs 110kD (a Dalton is defined as 1/12th ofthe mass of one [sup.12]C atom) we use a Vivaspin[TM] 30kD ultrafilterthat traps these larger particles above the filter, and separates lowerMW components below it using centrifugation CentrifugationA mechanical method of separating immiscible liquids or solids from liquids by the application of centrifugal force. This force can be very great, and separations which proceed slowly by gravity can be speeded up enormously in centrifugal (Bronk Ramsey et al. 2004).One would expect this to result in a better quality of collagen, sincedegraded amino acids, salts, insoluble particles and lower MWcontaminants pass through the filter. Earlier work by our group (Bronk Ramsey et al. 2004; Higham et al.2006a & b; Jacobi et al. 2006) has shown that the use ofultrafiltration often (but not always) results in older ages for bonesthan those previously obtained. This suggests that pre-treatment is avery important influence on accuracy and that previous determinations,less rigorously pretreated, can sometimes be affected by residualcontamination Contamination which remains after steps have been taken to remove it. These steps may consist of nothing more than allowing the contamination to decay normally. . Confidence in this diagnosis is increased because thesamples we tested were dated in the same laboratory, in which similarprotocols operated. The differences can, therefore, be ascribed largelyto pre-treatment variation. By way of example, dates from a bone or antler point excavated atthe British site of Hyaena Den (Wookey Hole, Somerset) are given (Table1). The first date obtained was prepared in 1991 using an ion-exchangedgelatin gelatinor animal jelly,foodstuff obtained from connective tissue (found in hoofs, bones, tendons, ligaments, and cartilage) of vertebrate animals by the action of boiling water or dilute acid. method to extract collagen (denoted as code AI). The result was24 600 [+ or -] 300 BP. In 2004, two other dates were obtained, usingthe gelatinisation (AG), and the ultrafiltration (AF) methods,respectively. The AF method produced the oldest and probably morecorrect date of the three. Other examples obtained in the last 5-10years show similar patterns (see Higham et al. 2006a; Jacobi et al.2006), and these downward revisions appear to make far morearchaeological sense. A bone or antler point in the British Isles British Isles:see Great Britain; Ireland. at 24600 BP appeared an unlikely proposition owing to owing toprep.Because of; on account of: I couldn't attend, owing to illness.owing toprep → debido a, por causa dethe extremely coldclimate of the time. The new earlier result fits neatly alongside otherevidence for osseous osseous/os��se��ous/ (os��e-us) of the nature or quality of bone; bony. os��se��ousadj.Composed of, containing, or resembling bone; bony. point manufacture during the Evolved Aurignacian ofEurope. Another example is provided by the Palaeolithic site of theGeissenklosterle, in the Swabian Jura of Germany, which is important forthe chronology and dispersai of the first anatomically modern humans(represented by the Aurignacian) in Western Europe (Hahn 1988; Conard& Bolus 2003, 2008). Conard and Bolus (2003, 2008) have publishedradiocarbon results from the site that show a wide variation and areinconsistent with the stratigraphic stra��tig��ra��phy?n.The study of rock strata, especially the distribution, deposition, and age of sedimentary rocks.strat sequence. Two different explanationshave been proposed to account for this. First, that the results arecaused by mixing and movement of material between the principalAurignacian horizons (AHII AHII Animal Health International, Inc. (distributor of animal health products)and AHIII) (Zilhao & D'Errico 1999),which themselves are an amalgamation of what may be a series ofdiscrete, brief occupations (Teyssandier et al. 2006). Second, that thevariation in date is due to significant variations in the production ofradiocarbon, as attested to in the datasets obtained by Beck et al.(2001) and Voelker et al. (2000) through this period (see Conard &Bolus 2003, 2008 who term this the 'Middle Palaeolithic DatingAnomaly'). It is important to say immediately that the latter explanation canessentially be addressed in the light of more recent work on thecalibration of radiocarbon between ~25 000-55 000 cal BP, which showsthat the large discrepancies in [sup.14]C production cannot beduplicated (Hoffman et al. 2010), and that the Beck et al. (2001)dataset was affected by a dead carbon influence. Insofar in��so��far?adv.To such an extent.Adv. 1. insofar - to the degree or extent that; "insofar as it can be ascertained, the horse lung is comparable to that of man"; "so far as it is reasonably practical he should practice as the firstexplanation is concerned, we decided to test the reliability of theprevious corpus of dates by redating using ultrafiltration. The resultsare shown in Table 2. For each sample of animal bone, there are tworadiocarbon determinations. The first radiocarbon determination in eachcase was obtained in the 1990s, mostly using gelatinisation. The secondis a new ultrafiltered gelatin date from the same bone. With someexceptions, the differences between the two are, once again, oftendramatic, with the original dates underestimating the real age. Thissuggests strongly that the reason for the variation in the originalradiocarbon series is not due to changes in radiocarbon production, aspreviously mooted, but lies instead in a combination of factors amongstwhich contamination must be considered alongside taphonomic orpost-depositional influences. The next challenge is to demonstrate that these newer results areaccurate and not themselves underestimating the true age. In the absenceof ancient bone of known age, radiocarbon laboratories attempt toquantify the background limit for the small traces of [sup.14]C that areinevitably taken up during the processing of the material. During thecombustion stage, for instance, we estimate that 0.0007 [+ or -]0.0010mg modern carbon is added. This figure, based on repeatcombustions and measurements of radioactively 'dead' material,is subtracted from the final radiocarbon measurement. In addition, smallamounts of modern radiocarbon are also taken up during the several stepsof the chemical pre-treatment of the bone, which must also be accountedfor. To quantify this, the ORAU use a >70 000 BP bison bone, from theAsh Bend site in Alaska (Brock et al. 2010), analysed multiple times toproduce a background correction subtracted from all bone dated in thelaboratory. These measurements enable us to determine the maximumdateable age for bone at the ORAU of just under 50 000 BP (Wood et al.2010). It follows that a failure to account for this in the radiocarbondating of old bone would result in ages that are, once again, too youngby varying degrees. A measure of the methodological improvement evident can be seenwhen we redate bones suspected of being beyond the [sup.14]C limit. InTable 3, the results of dates of bones from the so-called 'Banwellfauna' are shown. This fauna has been suggested by Currant currant,northern shrub of the family Saxifragaceae (saxifrage family), of the same genus (Ribes) as the gooseberry bush. The tart berries of the currant may be black, white, or red; the white gooseberry becomes purple when mature. andJacobi (1997, 2001) as most likely to date to Marine Isotope Stage 5,specifically MIS5b or a (Gilmour et al. 2007), and therefore to be wellbeyond the radiocarbon limit. The fauna is a cool climate, low speciesdiversity fauna dominated by bison (Bison priscus) and reindeer(Rangifer tarandus Rangifer tarandussee reindeer. ). Some of the results obtained in Oxford in the1990s, however, were younger than ~40-45 ka BE Table 3 also showsresults of the same bones redated using ultrafiltration which are almostalways 'greater than' ages and/or substantially older thanpreviously. This suggests that the age of the fauna is greater than ~50ka BP, and it also shows the previous ages to be underestimates again.Once more, an ultrafiltration treatment appears to remove the types ofcontaminants that appear not to have been removed before and confirm anolder, beyond background age, for this fauna. Redating charcoal Radiocarbon dates of charcoal from Palaeolithic sites, previouslyassumed to be largely reliable (Joris et al. 2003), have also seen someimportant developments in pre-treatment chemistry that hint at potentialproblems with the previous corpus of dates. The Grotta di Fumaneprovides an example. This site lies at the southern fringe of theVenetian Pre-Alps within a complex karst Karst(kärst), Ital. Carso, Slovenian Kras, limestone plateau, W Slovenia, N of Istria and extending c.50 mi (80 km) SE from the lower Isonzo (Soča) valley between the Bay of Trieste and the Julian Alps. system comprising a number ofcavities containing a sedimentary succession over 10m thick that spansthe Middle to Upper Palaeolithic, from MIS5-2 (Peresani et al. 2008).Previous dates were extremely variable and disclosed little age-depthpatterning. Once again, some have suggested that the reason for this maybe due to larger than expected variations in the production of [sup.14]Cin the atmosphere (Giaccio et al. 2006). To test this, we decided toredate previously analysed samples using a much more rigorous technique. The routine pre-treatment for charcoal samples is the so-calledacid-base-acid protocol (ABA). This method removes carbonates and humic hu��mic?adj.Of, relating to, or derived from humus.Adj. 1. humic - of or relating to or derived from humus; "humic acid" complexes using acidic and basic solutions respectively. Evidencesuggests that this is adequate in the majority of cases, particularlyfor samples less than about 20 ka BE However, when dating oldermaterial, several workers have shown that it is not always effectiveenough and contamination may remain (Chappell et al. 1996; Bird et al.1999; Turney et al. 2001; Santos et al. 2003; Higham et al. 2008, 2009;Brock & Higham 2009; Douka et al. 2010). In Table 4, samples ofcharcoal previously dated at the ORAU using the ABA method are comparedwith those dated using a more rigorous technique called ABOx-SC(acid-base-oxidation: stepped combustion) developed by Bird et al.(1999). The ABOx-SC results are uniformly older, and almost certainlymore reliable, than the ABA dates. When the dates are analysed within aBayesian model calibrated against INTCAL09 (Reimer et al. 2009) theyappear to exhibit much greater age-depth consistency (Higham et al.2009). Samples from the same phase yield closely similar ages. Resultsfrom the A2 level of the site, which is the Proto-Aurignacian, allcluster around ~40 000 cal BE Interestingly, in the south of the Italianpeninsula Noun 1. Italian Peninsula - a boot-shaped peninsula in southern Europe extending into the Mediterranean SeaItalia, Italian Republic, Italy - a republic in southern Europe on the Italian Peninsula; was the core of the Roman Republic and the Roman Empire between the , the independently-dated Campanian Ignimbrite ig��nim��brite?n.A volcanic rock formed by the welding together of tuff material from an explosive volcanic eruption.[Latin ignis, fire + imber, imbr-, rain + (dated at ~39300 cal BP by Ar-Ar) seals identical cultural horizons beneath it (DeVivo et al. 2001; Giaccio et al. 2006). This suggests that the A2 agesought to be older than this, and indeed they are (Higham et al. 2009). [FIGURE 2 OMITTED] We also obtained new ultrafiltered bone dates from the site andthese can be compared with the charcoal ABOx-SC series. The results areshown in a Bayesian model in Figure 2. The overall level of agreement isexcellent and there is only one outlier in the assemblage (this resultis considered more likely to be caused by sedimentary and cryoturbationprocesses in the upper parts of the site). Taken together, the level ofagreement suggests that the chronometric chro��nom��e��ter?n.An exceptionally precise timepiece.chrono��met framework is strong and theresults reliable. This good news is tempered by the fact that while wesee good agreement now, a comparison with previous published ages(Peresani et al. 2008) shows that around 70 per cent of the publishedages appear to be erroneous. Our experience suggests that one useful indicator of potentialproblems with bone determinations is collagen yield. When these fallbelow ~0.5-1 per cent by weight, CN atomic ratios often increase andamino acid amino acid(əmē`nō), any one of a class of simple organic compounds containing carbon, hydrogen, oxygen, nitrogen, and in certain cases sulfur. These compounds are the building blocks of proteins. profiles indicate greater instability, implying the potentialfor problematic AMS AMS - Andrew Message System determinations (e.g. Ambrose 1990; van Klinken1999). Radiocarbon laboratories ought to fall these types of boneroutinely when using gelatinisation pre-treatments. For charcoal, theanalytical indicators are much less apparent, but a decline in carbonyield, indicating degradation, is one useful measure and often, whendating old charcoals, low carbon yields are associated with anomalous,younger results. Conclusions The tendency of radiocarbon dates to cleave cleat, cleaveclaw of any cloven-footed animal. asymptotically to thedating limit means that many European Middle to Upper Palaeolithicresults produced over the last 50 years are underestimates of their realage. Sometimes these underestimates are severe. This means that thereare significant problems with the current database of results and it isvery difficult to be certain that some dates are not prone to undetectederror. Radiocarbon dating has not achieved its potential principallybecause of limitations in the pre-treatment of samples for dating and anunwise selection of material. At the Fumane site, our analysis suggestedthat more than 70 per cent of the previous determinations obtained wereunderestimates of the real age (Higham et al. 2009). What was surprisingwas that these determinations were mostly obtained in the last 10 years.If this estimate is applied to the entire European database, it suggeststhat there is a great deal of work to be done to build new chronologiesin which we can be confident. The results in this paper show that theproblems with decontamination decontamination/de��con��tam��i��na��tion/ (de?kon-tam-i-na��shun) the freeing of a person or object of some contaminating substance, e.g., war gas, radioactive material, etc. de��con��tam��i��na��tionn. of samples from the Palaeolithic aresignificant, but can be overcome. Acknowledgements This paper is dedicated to the late Dr Roger Jacobi (the BritishMuseum British Museum,the national repository in London for treasures in science and art. Located in the Bloomsbury section of the city, it has departments of antiquities, prints and drawings, coins and medals, and ethnography. and the Natural History Museum, London) for his collaboration,his comments on an early manuscript and for encouraging me to write thisin the first place. The Fumane project is undertaken in collaborationwith M. Peresani & A. Broglio (University of Ferrara HistoryThe University of Ferrara was founded on March 4, 1391 by Marquis Alberto V D'Este with the permission of Pope Boniface IX. The Studium Generale was inaugurated on St. Luke's Day (October 18), that same year with courses in law, arts and theology. , Italy), EBrock, R. Wood and K. Douka (all ORAU). I am very grateful to MarcoPeresani for his collaboration on the site and our dating work. Fumanedates were funded by a grant to E Brock and T. Higham from the NERC-AHRCNRCF NRCF Natural Resources of Central Florida programme. The excavation is managed by the Ferrara and Milano IUniversities in the framework of a project supported by theSoprintendenza per i Beni Archeologici del Veneto, CA.RI. VeronaFoundation, Comunita Montana della Lessinia, Comune di Fumane. I amgrateful to Fiona Brock for her invaluable contribution to this datingwork. I also thank Marco de la Rasillas (Oviedo) for comments andsuggestions regarding the El Sidron sequence of dates. The samples fromthe Geissenklosterle were sampled and prepared for AMS dating by RacheiWood and I am grateful for her invaluable input on this and for hercomments on the paper. She is also responsible for the work on thebackground correction for bone at the ORAU. I am also grateful toKaterina Douka for her comments on an earlier draft. I thank the staffof the ORAU, University of Oxford and the team working on the NERC NERC Natural Environment Research Council (UK)NERC North American Electric Reliability Corporation (Princeton, New Jersey, USA)NERC Northeast Recycling CouncilNERC National Environment Research Council (funded by grant NE/D014077/1) radiocarbon project at the ORAU,including C. Bronk Ramsey, R. Wood, K. Douka, L. Basell, J. Davies, A.Bowles, B. Emery, M. Humm, W. Davies and P. Leach. I am very grateful toP. Pettitt, J. Zilhao and W. Davies for their comments. Received: 5 May 2010; Accepted: 20 October 2010; Revised 9 November References AMBROSE, S.H. 1990. Preparation and characterisation of bone andtooth collagen for isotopic analysis. Journal of Archaeological Science Archaeological science (also known as Archaeometry) is the application of scientific techniques and methodologies to archaeology.Archaeological science can be divided into the following areas: 17: 431-51. ANDERSEN, K.K., A. 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CALCAGNILE & J.-M. DOLO. 2008.Age of the final Middle Palaeolithic and Uluzzian levels at Fumane Cave,northern Italy Northern Italy comprises of two areas belonging to NUTS level 1: North-West (Nord-Ovest): Aosta Valley, Piedmont, Lombardy, Liguria North-East (Nord-Est): Friuli-Venezia Giulia, Veneto, Trentino-Alto Adige/S��dtirol, Emilia-Romagna , using [sup.14]C, ESR ESR - Eric S. Raymond , [sup.234]U/[sup.230]Th andthermoluminescence thermoluminescenceEmission of light from certain heated substances as a result of previous exposure to high-energy radiation. The radiation causes displacement of electrons within the crystal lattice of the substance. methods. Journal of Arehaeological Science 35:2986-96. PETTITT, P.B. & A.W.G. PIKE. 2001. Blind in a cloud of data:problems with the chronology of Neanderthal extinction and anatomicallymodern human expansion. Antiquity 75: 415-20. PETTITT, P.B., W. DAVIES, C.S. GAMBLE & M.P. 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SANTOS, G.M., M.I. BIRD, L.K. FIFIELD, F. PARENTI, N. GUIDON gui��don?n.1. A small flag or pennant carried as a standard by a military unit.2. A soldier bearing such a flag or pennant. &P.A. HAUSLADEN. 2003. The controversial antiquity of the peopling of theAmericas: a review of the chronology of the lowest occupation layer inthe Pedra Furada rockshelter, Piaui, Brazil. Quaternary Science Reviews22: 2303-2310. SVENSSON, A., K.K. ANDERSEN, M. BIGLER, H.B. CLAUSEN, D.DAHL-JENSEN, S.M. DaVIES, S.J. JOHNSEN, R. MUSCHELER, S.O. RASMUSSEN& R. ROTHLISBERGER. 2006. The Greenland ice core chronology 2005,15-42 ka, Part 2: comparison to other records. Quaternary ScienceReviews 25: 3258-67. TEYSSANDIER, N., M. BOLUS & N.J. CONARD. 2006. The EarlyAurignacian in central Europe and its place in a European perspective,in O. Bar-Yosef & J. Zilhao (ed.) Towards a definition of theAurignacian: 241-56. Lisbon: Trabalhos de Arqueologia. TURNEY, C.S.M., M.I. BIRD, L.K. FIFIELD, R.G. ROBERTS, M.A. SMITH,C.E. DORTCH, R. GRON, E. LAWSON, L.K. AYLIFFE, G.H. MILLER, J. DORTCH& R.G. CRESSWELL. 2001. Early human occupation at Devil's Lair,south-western Australia 50 000 years ago. Quaternary Research 55: 3-13. VAN ANDEL, T.H., W. DAVIES, B. WENINGER & O. JORIS. 2003.Archaeological dates as proxies for the spatial and temporal humanpresence in Europe: a discourse on the method The Discourse on the Method is a philosophical and mathematical treatise published by Ren�� Descartes in 1637. Its full name is Discourse on the Method of Rightly Conducting the Reason, and Searching for Truth in the Sciences (French title: , in T. van Andel & W.Davies (ed.) Neanderthals and modern humans in the European landscapeduring the Last Glaciation: 21-9. Cambridge: McDonald Institute forArchaeological Research The McDonald Institute for Archaeological Research is a research institute of the University of Cambridge in England. HistoryThe Institute was established in 1990 through a generous benefaction from the late Dr D. M. McDonald, a well-known and successful industrialist. . VAN KLINKEN, G.J. 1999. Bone collagen quality indicators forpalaeodietary and radiocarbon measurements. Journal of ArehaeologicalScience 26: 687-95. VOELKER, A.H.L., EM. GROOTES, M.-J. NADEAU & M. SARNTHEIN.2000. Radiocarbon levels in the Iceland Sea from 25-53 kyr and theirlink to the earth's magnetic field intensity. Radiocarbon 42:437-52. WOOD, R.E., C. BRONK RAMSEY & T.F.G. HIGHAM. 2010. Refining theultrafiltration bone pre-treatment background for radiocarbon dating atORAU. Radiocarbon 52: 600-611. ZILHAO, J. 2006. Neandertals and moderns mixed, and it matters.Evolutionary Anthropology 15: 183-95. ZILHAO, J. & F. D'ERRICO. 1999. The chronology andtaphonomy ta��phon��o��my?n.1. The study of the conditions and processes by which organisms become fossilized.2. The conditions and processes of fossilization. of the earliest Aurignacian and its implications for theunderstanding of Neandertal extinction. Journal of World Prehistory prehistory,period of human evolution before writing was invented and records kept. The term was coined by Daniel Wilson in 1851. It is followed by protohistory, the period for which we have some records but must still rely largely on archaeological evidence to 13:1-68. Thomas Higham, Oxford Radiocarbon Accelerator Unit, ResearchLaboratory for Archaeology and the History of Art The Research Laboratory for Archaeology and the History of Art is a laboratory at the University of Oxford which develops and applies scientific methods to the study of the past.As of 2005, the Laboratory is directed by Prof. Mark Pollard. , University of Oxford,Oxford OX1 3QY, UKTable 1. Radiocarbon determinations from a bone or antler pointexcavated from the Hyaena Den, Wookey Hole (see Higham et ad 2006a andJacobi et al. 2006). Stable isotope ratios are expressed in [perthousand] relative to vPDB and nitrogen to AIR. Mass spectrometricprecision is [+ or -] 0.2 [per thousand] for carbon. Gelatin yieldrepresents the weight of gelatin or ultrafiltered gelatin inmilligrams. %Yld is the percent yield of extracted collagen as afunction of the starting weight of the bone analysed. %C is the carbonpresent in the combusted gelatin. C:N is the atomic ratio of carbon tonitrogen. At ORAU this is acceptable if it ranges between 2.9 and 3.5.* Denotes a solvent extraction prior to collagen preparation. Radiocarbon Std Chemical Used YieldOxA age BP error prep code (mg) (mg) %Yld13323 30 240 380 AG * 480 26 5.413803 31 550 340 AF * 568 11.7 2.13451 24 600 300 AI 260 9.4 3.6 [[delta].sup.13]COxA ([per thousand]) C:N13323 -19.3 3.413803 -19.3 3.43451 -20.7 ndTable 2. Radiocarbon determinations from the Geissenklosterle,Germany. There are two determinations from each bone, an AG(gelatinisation treatment) and AF (gelatinisation andultrafiltration). See caption to Table 1 for details of the analyticaldata.OxA Sample i.d. Species5707 (AG) AH IIa GK-41 Equus ferus, scapula21656 (AF)6076 (AG) AH IIIc GK43, Cervus elaphus, tibia 657.17, 243021657 (AF)6077 (AG) AH IIIc GK44, alpine Capra ibex, left tibia 57.17, 238921658 (AF)6256 (AG) AH III GK-48 Rangifer tarandus, tibia21659 (AF)5229 (AG) AH It GK-38 Mammuthus Primigenius, rib21660 (AF)5161 (AG) AH le GK 32- Rangifer tarandus, metacarpal Ica21661 (AF)OxA Radiocarbon age BP Used (mg) Yield (mg) %Yld5707 (AG) 33 200 [+ or -] 800 720 29.7 4.121656 (AF) 33 000 [+ or -] 500 540 25.9 4.86076 (AG) 33 600 [+ or -] 1900 500 20.3 4.121657 (AF) 39 400 [+ or -] 1100 480 20.4 4.26077 (AG) 32 050 [+ or -] 600 520 12.6 2.421658 (AF) 38 300 [+ or -] 900 420 12.6 36256 (AG) 30 100 [+ or -] 550 560 4.9 0.921659 (AF) 35 050 [+ or -] 600 480 12.1 2.55229 (AG) 27 950 [+ or -] 550 1000 11.3 1.121660 (AF) 27 960 [+ or -] 290 1040 22.5 2.25161 (AG) 30 300 [+ or -] 750 500 8.7 1.721661 (AF) 32 900 [+ or -] 450 300 12.2 4.1 [delta][sup.13]COxA %C ([per thousand]) C:N5707 (AG) 43.8 -20.521656 (AF) 45.8 -20.9 3.26076 (AG) 40.8 -22.321657 (AF) 43.9 -19.4 3.16077 (AG) 39.6 -19.421658 (AF) 44.2 -18.3 3.16256 (AG) 41.3 -19.121659 (AF) 44.1 -18.9 3.25229 (AG) 42 -20.421660 (AF) 41.5 -20.4 3.25161 (AG) 41.7 -19.121661 (AF) 44.2 -18.3 3.1Table 3. AMS radiocarbon determinations of bones from Banwell BoneCave mammal assemblage-zone sites previously AMS dated in Oxford(Higham et al. 2006a). Once again, AF denotes ultrafiltered gelatindeterminations, AG denotes a filtered gelatin determination whilst theterm Al denotes ion exchanged gelatin. See caption for Table 1 fordetails of the analytical parameters. ([dagger]) Duplicatemeasurements. Ages greater than the current limit of 50 000 BP reflectthe fact that the background in the laboratory at the time these ageswere determined was assessed to be lower than now.Element/species OxA Radiocarbon age BPWindy Knoll, DerbyshireBison priscus, radius OxA-4579 37 300 [+ or -] 1100 OxA-15001 > 51 700Steetley Quarry, NottinghamshireBison priscus, metacarpal OxA-2846 > 44 700 OxA-15000 > 53 200Brean Down, north SomersetCanis lupus, humerus OxA-4582 41 200 [+ or -] 1600 OxA-15002 > 52 700Ash Tree Cave, Derbyshire (clay)Bison priscus, cervical vertebra OxA-7736 > 41 500 OxA-15003 > 57 700Ash Tree Cave, Derbyshire (clay)Bison priscus, metatarsal OxA-13800 > 54 100Bone fragment OxA-13801 > 56 500Bone fragment OxA-13802 52 800 [+ or -] 3100Banwell Bone Cave, north SomersetBison priscus, calcaneum OxA-14136 > 59 500Bison priscus, calcaneum OxA-14137 52 700 [+ or -] 1900 ([dagger]) OxA-14138 > 53 900 ([dagger])Hunter's Lodge Inn Sink, SomersetBison priscus, scapula OsA-13566 >54 800 [delta][sup.13]CElement/species Method C:N ([per thousand])Windy Knoll, DerbyshireBison priscus, radius AI -20.1 AF 3.2 -20.8Steetley Quarry, NottinghamshireBison priscus, metacarpal AI -22.2 AF 3.2 -20.6Brean Down, north SomersetCanis lupus, humerus AI -19.8 AF 3.2 -19.5Ash Tree Cave, Derbyshire (clay)Bison priscus, cervical vertebra AG 3.3 -20.9 AF 3.2 -20.6Ash Tree Cave, Derbyshire (clay)Bison priscus, metatarsal AF 3.3 -20.4Bone fragment AF 3.3 -20.4Bone fragment AF 3.3 -20.2Banwell Bone Cave, north SomersetBison priscus, calcaneum AF 3.2 -20.3Bison priscus, calcaneum AF 3.2 -20.6 AF 3.1 -20.7Hunter's Lodge Inn Sink, SomersetBison priscus, scapula AF 3.2 -20.6 [delta][sup.15]NElement/species ([per thousand]) Wt.% coll.Windy Knoll, DerbyshireBison priscus, radius 1.4 4.6 10.1Steetley Quarry, NottinghamshireBison priscus, metacarpal 8.3 9.4 2.7Brean Down, north SomersetCanis lupus, humerus 1.5 10.5 1.7Ash Tree Cave, Derbyshire (clay)Bison priscus, cervical vertebra 5.6 6.2 6.6 2.6Ash Tree Cave, Derbyshire (clay)Bison priscus, metatarsal 8.8 3.7Bone fragment 9.9 6.4Bone fragment 10.0 2.4Banwell Bone Cave, north SomersetBison priscus, calcaneum 10.8 14.8Bison priscus, calcaneum 11.1 6.0 10.6 3.5Hunter's Lodge Inn Sink, SomersetBison priscus, scapula 8.8 3.6 Pretreat.Element/species yield (mg) %CWindy Knoll, DerbyshireBison priscus, radius 6.8 61.8 94.5 42.6Steetley Quarry, NottinghamshireBison priscus, metacarpal 25 44.1 14 43.3Brean Down, north SomersetCanis lupus, humerus 5.0 48.0 12.1 41.8Ash Tree Cave, Derbyshire (clay)Bison priscus, cervical vertebra 75.6 31.2 25.6 42.1Ash Tree Cave, Derbyshire (clay)Bison priscus, metatarsal 30.0 46.8Bone fragment 47.7 47.1Bone fragment 17.0 43.3Banwell Bone Cave, north SomersetBison priscus, calcaneum 59.0 41.2Bison priscus, calcaneum 35.0 41.7 14.6 41.1Hunter's Lodge Inn Sink, SomersetBison priscus, scapula 17.9 43.2Table 4. Radiocarbon ages of charcoal from the site of Grotta diFumane, Italy. The dates are divided into two columns, one ABA agestreated with the routine acid-base-acid preparation, the other ABOx-SC ages, treated using that method. Determinations in each level comefrom the same homogeneous sample of charcoal. The differences areattributed to the different pre-treatment chemistry applied. The OxA-X prefix is given for the sample from Layer A5 that produced a verylow %C value which is not usually expected for this type of material. [delta][sup.13]C ABA ages %C ([per thousand])Proto AurignacianLyr A2, sq. 97d 30 650 [+ or -] 260 58.5 -25.2 (OxA-11347)Lyr A2/struc. 18 33 380 [+ or -] 210 64.4 -24.7 (OxA-19525)Lyr A2/struc. 16/ 32 120 [+ or -] 240 44.2 -24.5lev. B (OxA-19413)Lyr A2/struc. 17 32 530 [+ or -] 240 60.7 -25.6 (OxA-19411)Lyr A2, sq. 107i 31830 [+ or -] 260 44.3 -23.3 (OxA-11360)MousterianLyr A5, sqs. 85, 86, 33 700 [+ or -] 600 62.3 -22.195, 96 (OxA-6463) 36 860 [+ or -] 700 60.7 -21.2 (OxA-18199)Lyr A5 sq. 88i, 34 500 [+ or -] 270 58.8 -24.63789/struc. III (OxA-19410)Lyr A5 + A6, sq. 90 38 800 [+ or -] 750 42.1 -23.8 (OxA-8022) 38 250 [+ or -] 700 66.3 -24.2 (Ox-A-8023) 39 500 [+ or -] 330 60.4 -24.2 (OxA-17567) 39 490 [+ or -] 350 57.8 -24.5 (OxA-17568) [delta][sup.13]C ABOx-SC ages %C ([per thousand])Proto AurignacianLyr A2, sq. 97d 35640 [+ or -] 220 80.6 -22.5 (OxA-17569)Lyr A2/struc. 18 35850 [+ or -] 310 40.5 -23.8 (OxA-19584)Lyr A2/struc. 16/ 34180 [+ or -] 270 48.6 -24.7lev. B (OxA-19414)Lyr A2/struc. 17 34940 [+ or -] 280 61.8 -24.2 (OxA-19412)Lyr A2, sq. 107i 35 180 [+ or -] 220 74.5 -21.7 (OxA-17570)MousterianLyr A5, sqs. 85, 86, 40150 [+ or -] 350 74.4 -21.195, 96 (OxA-17980)Lyr A5 sq. 88i, 41650 [+ or -] 650 24.4 -23.03789/struc. III (OxA-X-2275-45)Lyr A5 + A6, sq. 90 40460 [+ or -] 360 62.1 -24.4 (OxA-17566)