THERMOLUMINESCENCE DATING OF MATERIALS WHICH EXHIBIT ANOMALOUS FADING

This article reports a generalised and systematic approach to the thermoluminescence (TL) dating of samples which suffer from anomalous fading. We hypothesise that the TL signal from each mineral phase is composed of a stable and an unstable portion. The decay of the unstable TL is accelerated thermally, until only stable TL remains. The dating is then carried out on this stable signal. The results, on four known-age, coeval samples, exhibiting gross anomalous fading (25-50% loss over a few days), indicate that many, if not all, samples may successfully be dated with this approach.     

LES VERRES ANCIENS: LA QUESTION DE LA DATABILITÉ PAR THERMOLUMINESCENCE

La plupart des échantillons de verres archéologiques ne sont pas datables par thermoluminescence. Une analyse des causes limitant l'extension de la datation par thermoluminescence aux verres anciens montre que celles-ci sont directement issues de caracteristiques de l'etat vitreux. Toutefois. dans certains cas particuliers, la datation est possible. Most archaeological glass samples cannot be dated using thermoluminescence (TL). An analysis of the causes which limit the extension of the TL dating method to ancient glass shows that these causes come from the vitreous state characteristics. Nevertheless in some cases, dating is still possible.     

X荧光成分分析实验对测量陶瓷器热释光年代的影响研究

为了考察对一件已经经过X荧光分析实验的陶瓷样品进行热释光年代测定时,年代结果是否会受到X荧光分析实验的影响及其影响程度,本工作选取了古代与现代的陶器、瓷器及三彩样品共26件,在常规、经过胎体成分分析、经过釉层成分分析三种实验条件下测量比较热释光年代的变化.研究发现,对不同时代不同类型的样品,X荧光成分分析实验对热释光测年的影响程度不同;对部分样品的测年结果无影响,对部分样品的年代有增大的影响,但增大的程度不会使热释光测年结果产生真假颠倒的结论.     

A NEW THERMOLUMINESCENCE DATING TECHNIQUE FOR HEATED FLINT*

A new thermoluminescence (TL) technique for determining the age of heated flint artefacts from archaeological sites is presented. It is a variant of the SAR protocol, which is usually used for OSL dating of sediment, but it is not based on a presumed model for fitting the dose–response curve. Dose recovery tests as well as comparisons with standard protocols show the accuracy of the new technique. It is found that the sensitivity of the thermoluminescence (TL) signal of flint in the orange–red waveband does not show severe changes due to the heating process while measuring the TL. This allows the application of a short SAR procedure, which requires only two dose points. The technique does not require as much instrument time as other SAR techniques, and thus is advantageous for dating very old samples. The major advantage of this new technique is the small amount of sample material required, which allows the dating of samples that are too small for standard TL dating techniques.     

THERMOLUMINESCENCE DATING OF STALAGMITIC CALCITE

The thermoluminescence (TL) method of dating stalagmitic calcite has been applied to twenty-seven samples from two paleolithic cave sites; Pontnewydd, Wales, and Caune de l'Arago, Tautavel, France. Environmental dose-rates were evaluated mainly by means of CaF₂ capsule burials. The ages of the stalagmitic samples were independently determined by means of the uranium series disequilibrium method. In general, good agreement is found between the TL and uranium series dates, which cover a range from approximately 15 000 to 300 000 years B.P. It is estimated that the TL method should extend to the order of a million years in good circumstances.     

Mesopleistocene loess deposits in the Mamalyha 2 profile of Ukraine — interlaboratory comparison of the thermoluminescence dating results

The history of the interlaboratory comparison of TL dating results in Poland started in the 1980s. At that time the Lublin, Warsaw and Silesian laboratories made the first attempts at TL dating of the same loess samples from the Odonów profile. However, the cooperation ceased for many years due to great differences in the obtained TL age estimates. The next interlaboratory comparisons were made in the years 2000–2009 for the loess samples from several Polish (Dybawka, Tarnawce, Dankowice, Biały Kościół) and Ukrainian (Boyanychi, Halych, Velykyj Hlybochok, Yezupil) profiles. Most of the compared dates, obtained for the loess deposits from the Upper Pleistocene and younger part of the Middle Pleistocene, were consistent. This encouraged us to undertake the Gdańsk-Lublin interlaboratory cooperation in dating of 200-700 ka old loess deposits. Nine samples were taken from the Ukrainian profile Mamalyha 2 in 2009 for this purpose. The TL dating results indicate that comparable dates are obtained in two laboratories for loess deposits younger than 300 ka BP. The TL signal obtained in the Gdańsk laboratory for the samples older than 300 ka BP was saturated so such samples should not be dated by the multi-aliquot regeneration method. The results obtained in the Lublin laboratory for these deposits (489–682 ka) confirm that it is possible to date loess deposits older than 500 ka. It probably results from the use of total-bleach method with preheating at 160°C for the equivalent dose determination.     

FIFTY YEARS OF LUMINESCENCE DATING*

Luminescence techniques for dating both heated materials (e.g., pottery and burnt stone) and sediments have gone through three phases in the past 50 years. The first 22 years, from 1957 to 1979, were devoted to thermoluminescence (TL) techniques applied to heated material. In the next six years, from 1979 to 1985, it was found that TL dating could be applied to sediments. However, the TL signals of both quartz and feldspar grains observed for modern sediments were small, but were not zero, thus making them useful only for older sediments. A new luminescence signal that was totally zeroed by exposure to sunlight for a relatively short period of time, a few hours or less, was found; this led to the development of optically stimulated luminescence (OSL) dating techniques in 1985. Further developments have continued to the present day. Within the past 22 years, 1999 was also a year with major developments. A reliable procedure for single aliquots of quartz that have a rapidly bleached (‘fast’) OSL component was formalized and an instrument that allowed rapid measurement of equivalent doses for single grains was constructed. These developments have led to OSL becoming a major dating tool in Quaternary geology, at least for the past 100 000 years, and in archaeology, particularly as related to the dispersal of modern humans.     

Thermoluminescence dating

Over the last few years the Nordic Laboratory for Thermoluminescence (TL) Dating has obtained TL dates for a considerable number of archaeological samples, ceramics, bricks, burnt clay and burnt stones from the Nordic countries. The majority of TL dates have been consistent and in agreement with other dating evidence. Discrepancies caused primarily by excessive short‐term fading of the latent TL signal were encountered in a few cases. A procedure for eliminating errors caused by short‐term fading is described. A brief discussion of the sources of error in TL dating is given. Finally, results obtained by TL are compared with those obtained by radiocarbon for a number of sites.     

Attempts at thermoluminescence dating of fired materials from the Przeworsk Culture settlements

The thermoluminescence (TL) dating method has a significant measurement error margin reaching almost 10%. Due to this fact it could be considered as little effective in case of such sites from the Roman period as burial grounds with many artefacts useful for archaeological dating. However, for many settlements from this period, where pottery is the only kind of artefacts, the TL method can give notable results. The main purpose of the study was to make an attempt at TL dating of pottery and clay daub samples from the Nieszawa Kolonia and Kręcieszki sites and to compare the obtained dates with the results of archaeological dating of selected features from the Przeworsk Culture settlements. In the Kręcieszki site the fragments of burnt clay daub were dated by the TL method for the first time in the Lublin laboratory. It turned out that clay daub is an equally good dating material as pottery. It can be found that the TL dating of pottery from Nieszawa Kolonia confirms two stages of settlement. The first settlement stage is related to the phases B2-B2/C1-C1a of the Roman period, i.e. from the beginning of the 2^nd to the beginning of the 3^rd century. The second group of TL dates corresponds to the phases C2D that is to the second stage of settlement, from the second half of the 3^rd century to the half of the 5^th century AD. The results of TL dating of pottery and clay daub in the Kręcieszki site are rather similar and correspond to the phase B1/B2 of the period of Roman influence, determined from pottery style, but can also indicate the phase B2/C1.     

Thermoluminescent dating in its application to archaeology: A review

This paper sets out to describe the fundamentals of thermoluminescent (TL) dating and to explain the principles of operation of the different methods at present in use. The various complicating factors associated with TL dating are discussed, together with the measures which can be taken to recognize and as far as possible to correct them. Those materials from archaeological contexts which are suitable for dating by the TL technique are described and the criteria for the selection of suitable samples, and the methods of obtaining the desired ancilliary information relating to the environment of the site, are discussed.     

越窑青瓷的辐照熄灭测试研究

熄灭率是研究瓷器辐照熄灭特性的一个重要参数,也是衡量一件古瓷器能否用热释光前剂量技术测定的一个重要条件.如果一件瓷器的熄灭率太低,这件瓷器就不能用前剂量技术测定年代,或测定得到的年代结果误差会很大.为此,本工作对中国最早的青瓷——浙江慈溪上林湖唐代、五代及宋代的10个越窑古窑址的78件青瓷样品进行了辐照熄灭率测试研究.测试结果分别获得了各测定样品的“辐照熄灭率”.越窑青瓷样品的平均熄灭率为11.38％,这样的熄灭率保证了热释光灵敏度曲线测量时有足够的分辨率,也保证了应用热释光前剂量熄灭法测定越窑瓷器样品年代结果的准确性.     

A COMPARATIVE STUDY OF THE SPATIAL DISTRIBUTION OF URANIUM AND OF TL-PRODUCING MINERALS IN ARCHAEOLOGICAL MATERIALS

A technique is described by which the spatial distribution of uranium as well as of thermoluminescent minerals can be examined in the same archaeological sample. The uranium distribution is replicated on an aluminized plastic film with the help of a ‘spark counter’following reactor-irradiation of the sample, while the TL pattern is photographed directly from a γ-irradiated sample. Implications for dating from such a comparative examination are discussed for certain pottery and flint samples.     

Thermoluminescence dates for the Middle Palaeolithic site of Chez-Pinaud Jonzac (France)

Thermoluminescence dating of heated flint artefacts from the Middle Palaeolithic sequence of Chez-Pinaud Jonzac (France) places an assemblage of Quina type Mousterian into MIS 4, while the overlying assemblage of Denticulate Mousterian which is followed by two layers with Mousterian of Acheulean Tradition are all assigned to MIS 3. TL dating is used to verify the mixed nature of deposits from which diagnostic Middle as well as Upper Palaeolithic tools were recovered. The TL ages are significantly different for samples from this layer and broadly agree with the archaeological attributions. While the study is generally limited by the low number of heated samples available, a correlation with a generalized chronostratigraphic sequence is possible by including proxy data from the faunal remains associated with the lithic assemblages in question. The Quina Mousterian in southwestern France, therefore, can be placed by chronometric dating methods in MIS 4 to MIS 3.     

Optically stimulated luminescence dating of heated materials using single-aliquot regenerative-dose procedure: a feasibility study using archaeological artefacts from India

Optically stimulated luminescence (OSL) dating of heated/fired materials of archaeological importance from various parts of India was attempted. A single-aliquot regenerative-dose (SAR) procedure was used for palaeodose determination in the quartz grains extracted from the heated materials using the luminescence produced by blue light stimulation. In most pottery samples, the palaeodose obtained using SAR-OSL is ∼6% lower than the palaeodose measured using thermoluminescence (TL) method. Broadly, there is good agreement between the SAR-OSL and TL ages of the artefacts and their archaeologically expected ages. The results suggest that routine dating of heated/fired materials using the SAR-OSL procedure is more practicable, especially when the TL sensitivity of the quartz grains is poor and availability of datable material is limited.     

Thermoluminescent dating of the Late Bronze and Early Iron Age pottery on sites in Kłyżów and Jarosław (SE Poland)

The absolute chronology of Late Bronze and Early Iron Ages in Polish territories is a result of long-term and complex research. Here, we have investigated the absolute dating of two sites, namely K?y?ów, a cemetery of the Tarnobrzeg Lusatian culture, and Jaros?aw, a settlement spanning from the late phase of the former to Pomeranian culture, possibly with Jastorf elements. Having been spurred by promising results of thermoluminescence (TL) dating of medieval and Przeworsk materials, we have employed it in those situations, where no other chronometric methods seem to be efficient. TL dating has been combined with typological analysis of the dated pottery and, partially, with radiocarbon method. Albeit the produced TL dates do not represent the level of sought-for fine chronological resolution, they indicate the temporal trends and corroborate the typological research. Our study has shown the potential of TL dating for periods with plateaus on ¹⁴C calibration curve. We also have dealt with unexpected TL ages and suggested some solutions of the problem. Finally, we have demonstrated that the condition sine qua non for archaeological interpretation of TL dates is a thorough stylistic-chronological analysis of dated pottery and clear understanding of relations between chronometric dates and the archaeological event to be dated.     

Thermoluminescence age of quartz xenocrysts in basaltic lava from Oninomi monogenetic volcano, northern Kyushu, Japan

We determined the eruption age of basaltic rocks by application of thermoluminescence (TL) method, which is often used for TL dating, to quartz. Mafic magma only rarely includes quartz because of their mutual disequilibration. The basaltic lavas reported herein include quartz as xenocrysts, as corroborated by their rounded or anhedral shape. The basaltic lava used for this study is from the Oninomi monogenetic volcano in northern Kyushu, Japan. The volcano eruption was estimated as occurring 7.3–29 ka because the lava exists between two widespread tephras: Aira-Tanzawa ash (26–29 ka) and Kikai-Akahoya ash (7.3 ka). We succeed-ed in collecting ca. 200 mg of quartz by decomposition of 30 kg of the lava samples. TL measurements for the lava indicate the eruption age as 15.8 ± 2.5 ka, which is fairly consistent with the stratigraphical estimation. Although the TL method has played a considerable part in constraining the timescale of Quaternary events, its application has been limited to silicic samples. The present result demonstrates the availability of quartz for dating even of mafic rock.     

THE EFFECT OF HF ACID ETCHING ON THE MORPHOLOGY OF QUARTZ INCLUSIONS FOR THERMOLUMINESCENCE DATING

The assumption of isotropic etching in hydrofluoric acid of quartz grains prepared for thermoluminescence dating has been tested by optical and scanning electron microscopy. We have found that the rate of etch is very irregular over the surface of many grains and that some grains are attacked much more severely than others. The uncertainty introduced into TL dating by this effect is discussed.     

THERMOLUMINESCENT AUTHENTICITY STUDY AND DATING OF RENAISSANCE TERRACOTTAS

A comparative study is made of the thermoluminescence (TL) of terracottas of the Renaissance era and some known limitations of such ware dating to the middle of the last century. The data shows that conclusions on authenticity of an unknown work can be reliably obtained using this scientific method. Also examples are presented of accurate dating of genuine terracottas despite a lack of knowledge about the environmental circumstances of each piece's archaeological past.     

Problems of TL dating of the Mesopleistocene loess deposits in the Podillya and Pokuttya regions (Ukraine)

In many papers different authors was described problem of systematic underestimation of TL ages for sediments older then 100 ka. We presented the results which probably are not significantly rejuvenated. This is another example of the TL dates made in Lublin laboratory which are likely in agreement with the stratigraphic interpretation. In 2002 Kusiak et al. published the TL ages ranging from 200 to 800 ka for the Zahvizdja loess profile in Ukraine. These first promising results of TL dating of so old deposits encouraged us to undertake further studies. In next years were discovered other Ukrainian loess profiles with the Middle and Lower Pleistocene deposits, among others in the Skala Podils’ka, Mamalyha and Vendychany sites. The thermoluminescence dating made for these profiles in the Lublin laboratory gave the next, after Zahvizdja, series of 15 TL ages ranging from 200 to 700 ka. This way we confirmed the possibility of TL dating of the deposits older than 400 ka BP.     

EMPLOYING TL METHODS FOR THE VERIFICATION OF MACROSCOPICALLY DETERMINED HEAT ALTERATION OF FLINT ARTEFACTS FROM PALAEOLITHIC CONTEXTS

The reconstruction of past human use of fire is often based on the presence of fire in archaeological sites as evidenced by alterations of lithic material. Here, a simple test based on thermoluminescence (TL) methods is used as a verification tool for the macroscopic identification of burning damage on flint microartefacts from the Early and early Middle Pleistocene site of Gesher Benot Ya‘aqov (Israel). The small dimensions of the microartefacts often prevented the removal of the outer surface, for which the TL signal might have been altered (bleached) by exposure to light during excavation. Bleaching of the TL signal by sunlight was found for fresh raw material, but appeared to be less problematic for the archaeological material, presumably due to patination. However, TL results for some samples are ambiguous and it is sometimes difficult to distinguish heating from post‐depositional bleaching, especially for samples that are macroscopically considered as not having been heated. A qualitative interpretation of the TL data is compared with the macroscopic assessment. The general agreement of the TL analyses with the macroscopic observations provides an independent verification of the observed burning and thus supports the assumption that fire was used and controlled throughout the long occupational sequence of Gesher Benot Ya‘aqov.