Experimental Heating of Moravian Cherts and its Implication for Palaeolithic Chipped Stone Assemblages

The applicability of colour, magnetic susceptibility and remanent magnetization measurements for the identification of heated or accidentally burned Palaeolithic cherts from Moravia (Czech Republic) is tested in this study. We conclude that all these methods are usable. Colour changes are best detectable in materials heated at between 250–350°C, while magnetic susceptibility and remanent magnetization change at higher temperatures, closer to 600°C. This latter temperature, however, is usually destructive for cherts and is probably evidenced by accidentally burned artefacts. With the use of the three methods, we managed to identify three probably heated chert artefacts from two early Upper Palaeolithic assemblages from Moravia.     

Palaeomagnetic dating of fluid-flow events in dolomitized rocks along the Highland Boundary Fault, central Scotland

Palaeomagnetic and geochemical studies of Cambrian–Ordovician serpentinite in the Highland Border Complex (HBC), a tectonic terrane along the Highland Boundary Fault (HBF) in Scotland, indicate that the HBF was a conduit for fluids in the Carboniferous–Permian. The fluids caused dolomitization, silicification, and haematite authigenesis. Both red dolomitized serpentinite and relatively unaltered serpentinite were sampled at multiple localities. The unaltered serpentinite contains a poorly defined magnetization with westerly declinations that resides in magnetite and has a pole which plots well off the apparent polar wander path. Most specimens of the red dolomitized serpentinite contain a magnetization with southerly declinations and negative inclinations that resides in haematite. A regional fold test suggests that this magnetization post‐dates tilting and the pole positions for the different locations fall on the Carboniferous to Permian part of the apparent polar wander path. In some specimens of red dolomitized serpentinite, alternating field (AF) demagnetization prior to thermal treatment removes a component with a similar direction. Dolomitized basement rocks along the fault contain a similar although apparently slightly older magnetization. Fluid inclusion and geochemical studies indicate that the fluids were hydrothermal in origin (110–240°C) and had a range of sources. The Carboniferous–Permian magnetization in haematite is interpreted as a chemical remanent magnetization that formed when warm fluids moved along the fault zone and caused haematite authigenesis. The component removed by AF treatment is interpreted as a thermal resetting of primary magnetite by the fluids. The variability of the palaeomagnetic, fluid inclusion, and stable isotope results suggests that there were probably multiple flow events that caused the alteration. The origin of the fluids could be related to the intrusion of late Carboniferous dikes in central Scotland and/or to reactivation of the HBF in the Carboniferous–Permian.     

Cemented ash as a receptacle or work surface for ochre powder production at Sibudu,South Africa, 58,000 years ago

The white ash of Sibudu hearths sometimes became cemented and, when this was the case, some of these crusts were used as work surfaces or receptacles, particularly in occupations dating about 58,000 years ago. Substantial deposits of red and yellow ochre powder have been found on these crusts. This suggests that the ochre was not associated with hearths for heat treatment because yellow ochre readily transforms to red even at low temperatures. XRF readings suggest that the ochre used at the site derives from different geological sources. Micromorphological studies imply that phosphatization caused the cementation of the ashes in some hearths, while gypsum growth hardened one of the hearths described here.     

Heat Treatment of Mineral Pigment During the Upper Palaeolithic in North‐East Italy

The use of red ochre for utilitarian, symbolic and artistic purposes is widely documented in prehistoric contexts. The absence of adequate red‐coloured raw materials influenced the development of technological activities aimed at modifying the original physiochemical properties of yellow ochre. The heat treatment of goethite to obtain hematite was investigated in the western sector of the Lessini Mountains in north‐east Italy, where red ochre was found in the (Proto)Aurignacian levels at Fumane cave and in the Late Epigravettian sequence at Tagliente rockshelter. The combination of X‐ray powder diffraction (XRPD) and transmission electron microscopy (TEM) proved that heat treatment was a common practice in the studied archaeological sites due to the scarce availability of suitable hematite‐based material in the region.     

Bedding, hearths, and site maintenance in the Middle Stone Age of Sibudu Cave, KwaZulu-Natal, South Africa

Micromorphological analysis of sediments from the Middle Stone Age site of Sibudu Cave, KwaZulu-Natal, South Africa, provides a high-resolution sequence and evidence of site formation processes of predominantly anthropogenic deposits. This methodology allows for a detailed interpretation of individual anthropogenic activities, including the construction of hearths and bedding and the maintenance of occupational surfaces through the sweep out of hearths and the repeated burning of bedding. This analysis also provides a context for evaluating other studies at the site relating to magnetic susceptibility, paleobotany, paleozoology, anthracology, and studies of ochre.     

First large‐scale provenance study of pigments reveals new complex behavioural patterns during the Upper Palaeolithic of south‐western Germany

The use of red iron‐based earth pigments, or ochre, is a key component of early symbolic behaviours for anatomically modern humans and possibly Neanderthals. We present the first ochre provenance study in Central Europe showing long‐term selection strategies by inhabitants of cave sites in south‐western Germany during the Upper Palaeolithic (43–14.5 ka). Ochre artefacts from Hohle Fels, Geißenklösterle and Vogelherd, and local and extra‐local sources, were investigated using neutron activation analysis (NAA), X‐ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that local ochre sources were continuously and systematically accessed for c.29 500 years, with periodic events of long‐distance (about > 300 km) ochre acquisition during the Aurignacian (c.35–43 ka), suggesting higher mobility than previously suspected. The results reveal previously unknown long‐term, complex spatio‐temporal behavioural patterns during the earliest presence of Homo sapiens in Europe.     

ARTIFICIAL OR NATURAL ORIGIN OF HEMATITE‐BASED RED PIGMENTS IN ARCHAEOLOGICAL CONTEXTS: THE CASE OF RIPARO DALMERI (TRENTO,ITALY)

This study concerns those crystallographic and microstructural features that can provide indications on the actual origin of red pigments based on hematite (Fe₂O₃). The main features of natural and artificial hematite are recalled and used to discuss the results obtained from the characterization of red‐ochre samples coming from the Palaeolithic site of Riparo Dalmeri, a rock‐shelter located in northeastern Italy, dated to 13 000 cal. bp , and notorious for the presence, among the other finds, of red‐painted calcareous stones. Painting and the treatment of leather and hides obtained from the intensive hunting activity were the main uses of the hematite‐based red‐ochres at Riparo Dalmeri. It turns out that hematite was mostly obtained from the thermal treatment of goethite, which, unlike hematite, was and still is widely available in the neighbourhood of the site.     

Raman Spectroscopic Analysis of Ancient Egyptian Pigments

The application of FT‐Raman spectroscopy and visible Raman microscopy to the non‐destructive analysis of pigment specimens excavated from Tell el Amarna by Flinders Petrie in the 1890s has provided information about the chemical composition of the materials used by XVIIIth Dynasty artists in the New Kingdom at the time of King Akhenaten, c. 1340 bc. Comparison of the Raman spectra of the samples labelled ‘red and yellow ochre’ with documented, archival material from geological collections provided a clear indication of the materials used in the iron(III) oxide/hydroxide system, including α‐hematite, goethite, maghemite, magnetite and lepidocrocite. The yellow–orange specimen labelled ‘realgar’ proved to be a mixture of realgar and pararealgar; since the specimen had been sheltered from light since its excavation, this could indicate that the ancient Egyptian artists recognized the colour variation and may have used this to effect in their decorations. A specimen of yellow ochre contained goethite, α‐FeO.OH, with particles of crystalline, highly ordered graphite; in contrast, the red ochre specimens contained amorphous carbon particles.     

COLOUR SYMBOLISM IN THE PREHISTORIC ARCHITECTURE OF CENTRAL ANATOLIA AND RAMAN SPECTROSCOPIC INVESTIGATION OF RED OCHRE IN CHALCOLITHIC ÇATALHÖYÜK

The use of red ochre in the prehistoric architecture of Central Anatolia has long been recognized. Scholars have often argued that its use in architecture has a symbolic role, and that it has been used in sacred parts of ritual buildings. This paper examines red‐painted buildings in the prehistoric settlements of Central Anatolia. Recently, a building with red‐coloured plastered walls and floors was found in Chalcolithic Çatalhöyük West. The technique of Raman Spectroscopy has been applied to identify the red pigment and results show that it is red ochre, which contains predominantly hematite, Fe₂O₃.     

Ochre fingerprints: Distinguishing among Malawian mineral pigment sources with Homogenized Ochre Chip LA–ICPMS

In this study, we compared the effectiveness of instrumental neutron activation analysis (INAA) of bulk ochre to laser ablation‐inductively coupled plasma mass spectrometry of homogenized ochre chips (HOC LA–ICPMS) at distinguishing among three ochre sources in northern Malawi. Both techniques upheld the Provenance Postulate; however, HOC LA–ICPMS required less sample material than INAA and facilitated fast, inexpensive replicate observations that allowed for more robust statistical analysis. Our results indicated that HOC LA–ICPMS is a maturing technique that will be a valuable option for analysing artefacts that require minimally destructive sampling but are too large to fit into the laser cell for direct ablation. With regard to the statistical procedures used, stepwise canonical discriminant analysis was demonstrated to be a highly effective method for distinguishing among ochre sources, even in the presence of significant intra‐source and intra‐sample heterogeneity. Continued development of the HOC sample preparation technique will expand the range of archaeological ochre artefacts that can be included in provenance studies and prevent bias towards artefacts of convenient‐to‐analyse dimensions.     

A SCIENTIFIC INVESTIGATION ON THE PROVENANCE AND TECHNOLOGY OF A BLACK‐FIGURE AMPHORA ATTRIBUTED TO THE PRIAM GROUP*

The restoration of a Greek black‐figure amphora provided an opportunity to study the provenance and production technology of the vase. The composition of the ceramic body, determined by inductively coupled plasma optical emission spectroscopy (ICP–OES), matches that of Attic products. Investigation by X‐ray diffraction and reflectance spectroscopy suggests a maximum firing temperature around 900°C and a body re‐oxidation temperature around 800°C, respectively. The morphology and composition of black, red and dark red surface areas were studied by scanning electron microscopy and X‐ray energy‐dispersive analysis; the black areas show the features of a typical well‐vitrified black gloss, while the red areas were most probably obtained by simple burnishing of the body; the dark red additions, on the other hand, are the likely result of a partial re‐oxidation of a clay–ochre mixture.     

Ochre Provenance and Procurement Strategies During The Middle Stone Age at Diepkloof Rock Shelter,South Africa

Usually referred to in archaeological contexts simply as ‘ochre’, ferruginous rocks were commonly used during the Middle Stone Age (MSA) in South Africa. While ochre use by early modern humans has often been interpreted as reflecting complex behaviours, related procurement strategies and selection criteria remain poorly documented. Eight ochre sources from the surroundings of Diepkloof rock shelter in South Africa and 28 ochre pieces from the site's MSA levels were studied by XRD, ICP–OES and ICP–MS. Mineralogical and geochemical data demonstrate that ochre was both locally procured and transported to the site from more distant sources. Here, we investigate the reasons underlying the choice of particular local and non‐local ochre sources exploited at Diepkloof, emphasizing differences in their physico‐chemical properties. Regardless of the motivations behind ochre selection, our data shed new light on the behavioural complexity of MSA societies and suggest that ochre procurement strategies may be independent of subsistence concerns.     

Pyrophyllite formation in the thermal aureole of a hydrothermal system in the Lower Saxony Basin,Germany

A combined clay mineralogical, fluid inclusion, and K‐Ar study of Upper Jurassic metasediments at the Gehn (Lower Saxony Basin, Germany) provides evidence for a transient hydrothermal event during Upper Cretaceous basin inversion centered on a prominent gravimetric anomaly. Kaolinite and smectite in Oxfordian pelitic parent rocks that cap a deltaic sandstone unit were locally transformed into pyrophyllite, 2M₁ illite, R3 illite–smectite, chlorite, and berthierine at the Ueffeln quarry. The pyrophyllite‐bearing metapelites lack bedding‐parallel preferred orientation of sheet silicates and experienced peak temperatures of about 260–270°C consistent with microthermometric data on quartz veins in the underlying silicified sandstones. The presence of expandable layers in illite–smectite and high Kübler Index values indicate that the thermal event was rather short‐lived. K‐Ar dating of the <0.2 μm fraction of the pyrophyllite‐bearing Ueffeln metapelite yields a maximum illitization age of 117 ± 2 Ma. Lower trapping temperatures of aqueous fluid inclusions in quartz veins and the absence of pyrophyllite in metapelites of the Frettberg quarry in a distance of about 2.5 km from the Ueffeln quarry infer maximum paleotemperatures of only 220°C. The highly localized thermal anomaly at Ueffeln suggests fault‐controlled fluid migration and heat transfer that provided a thermal aureole for pyrophyllite formation in the metapelites rather than metamorphism due to deep burial. A pH neutral hydrothermal fluid that formed by devolatilization reactions or less likely by mixing of meteoric and marine waters that interacted at depth with shales is indicated by the low salinity (3–5 wt. % NaCl equiv.) of aqueous inclusions, their coexistence with methane–carbon dioxide‐dominated gas inclusions as well as carbon, hydrogen, and oxygen isotope data. The upwelling zone of hydrothermal fluids and the thermal maximum is centered on a gravimetric anomaly interpreted as an igneous intrusion (‘Bramsche Massif’) providing the heat source for the intrabasinal hydrothermal system.     

THE REMANENT MAGNETIZATION OF ANCIENT STRUCK COINS

Magnetic and other measurements are reported for the Guehenno II Gallo-Roman hoard (56-France) which, amongst several thousand Tetricus antoniniani, contains 275 coins struck with the same dies. The orientation of the remanent magnetization is systematically directed outwards from the obverse confirming the identity of the anvil die with the obverse. The magnetization vector is statistically distributed around the vertical axis giving no indication of the geomagnetic inclination at the time of striking. Consequently ancient struck coins cannot be used for dating. The origin of the remanent magnetization was also investigated.     

陕西安康紫阳北五省会馆壁画颜料分析研究

陕西安康紫阳北五省会馆壁画是目前陕西省境内发现的最大的一处建筑壁画,为了解其颜料组成,本工作采用X射线荧光、偏光显微镜、X射线衍射、激光显微拉曼光谱及扫描电镜能谱分析相结合的分析方法,对颜料样品进行了分析。结果表明,北五省会馆壁画除正殿发现一处红色染料外,其他均为无机颜料;红色颜料主要是铅丹、朱砂、铁红;绿色颜料为氯铜矿、石绿、斜氯铜矿;蓝色颜料的主要成分是普鲁士蓝、smalt、石青;黄色颜料为雌黄、铁黄;褐色颜料的主要成分是铁红及铅丹的变色产物二氧化铅;黑色为炭黑;白色颜料主要是铅白,且多使用铅白作为调色颜料。研究结果对于了解清代民间壁画的制作工艺,丰富对陕西建筑壁画的认识具有重要意义。     

The Source of Iron‐Oxide Pigments Used in Pecos River Style Rock Paints

The likely sources of iron‐oxide pigments used in prehistoric rock paintings in the Lower Pecos Archaeological Region were identified on the basis of chemical fingerprinting using LA–ICP–MS. The chemical signatures of 13 red rock paint samples collected from two south‐west Texas sites were compared with three potential source materials (ochre, siltstone and rhyolite), and two pigment cakes (crayons) that were excavated near the sampling sites. The significant chemical similarities between the paint and siltstones suggest that siltstone was used as the source of the colour. The overlapping chemical signatures for one of the pigment cakes and siltstone further suggests that some of the prehistoric people inhabiting the area 3000–4000 years ago had acquired the skills to extract iron oxide from siltstone and process it into paint pigments.     

THE ROMANESQUE FRIEZE AT LINCOLN CATHEDRAL (ENGLAND)—PRIMARY OR SECONDARY INSERTION? MAGNETIC CONSIDERATIONS*

The current debate about the age of the Romanesque frieze of Lincoln Cathedral weighs archaeological evidence against art history. On the one hand, the panels appear to be an integral part of the original Norman structure built by the first bishop (AD 1072–92). However, on grounds of style and artistic comparisons, art historians argue for a later installation during the restoration of AD 1141–6. In order to determine when the panels were stabilized in the cathedral, we used a new method that measures their degree of remagnetization by the earth's magnetic field since they were quarried. The longer that masonry remains stabilized in a given orientation, the greater its viscous remagnetization. Viscous remanent magnetization dating has previously been successful with this particular type of limestone masonry. Our results lend support to the view that the panels were installed in the early 1140s.     

RESEARCH REPORT: MAGNETIC INVESTIGATIONS AND THE AGE OF A MEDIEVAL KILN AT KUNGAHÄLLA (SOUTH‐WEST SWEDEN)*

The results from a magnetic survey and archaeomagnetic investigation of a medieval brick kiln at Kungahälla in Bohuslän (south‐west Sweden) are reported. Detailed magnetic total field and magnetic gradient measurements over known traces of the kiln showed marked local magnetic anomalies of up to 200 nT, revealing the rectangular shape of the kiln remains. Palaeomagnetic investigations of the remanent magnetization of 12 bricks from the kiln floor gave precise definitions of both the direction of the archaeomagnetic field [(D_m, I_m) = (66.7°, 8.8°), k = 655, α₉₅= 1.7°] and the palaeointensity [B_m= 69.0 ± 3.6 µT]. An archaeomagnetic date is obtained by comparing the direction of the archaeomagnetic field found in the kiln with a geocentral dipole‐transformation of the British master‐curve for secular variation. Of two possible archaeomagnetic dates (ad 1280 ± 50 or ad 1480 ± 50), the ad 1280 ± 50 age is in good accordance with the C‐14 ages and archaeological dates as well as with direct historical evidence, whereas a c. 100 years younger TL date appears to be too young.     

The death and burial of sunghir 1

The Mid Upper Paleolithic Sunghir 1 burial of an older adult male is one of the most elaborate burials known, with red ochre, thousands of mammoth ivory beads, and other body ornaments. Reanalysis and cleaning of the skeletal remains revealed a perimortem incision in the ventral–lateral first thoracic vertebra (T1) body, most likely from a sharp blade or point and the probable cause of death. Context indicates that the trauma was most likely from a hunting accident or social altercation. The unusual cause of death may be correlated with the exceptional burial elaboration of Sunghir 1, adding to the high frequency of unusual individuals in the ‘red ochre’ burials of the Mid Upper Paleolithic. Copyright © 2010 John Wiley & Sons, Ltd.     

AN ARCHAEOMAGNETIC STUDY OF POTTERY KILNS FROM BRÜHL-PINGSDORF (GERMANY)*

Four pottery kilns from Brühl-Pingsdorf (Germany) were dated by comparing their characteristic remanent magnetization with a curve of the palaeo-secular variation of the geomagnetic field. Archaeomagnetic results suggest last heating events between AD 775 and 1020. The archaeological evidence generally supports the relative temporal succession and the duration of use, but indicates that the kilns are about 150 years younger on average. Hence, a systematic offset between these independently developed chronologies must be considered. Rock magnetic parameters display radial variations through the kiln walls. These variations are controlled by the maximum temperature the rock was exposed to. These parameters were used to identify specimen which acquired a thermoremanent magnetization.