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It is widely known that the vivid hue of red cinnabar can darken or turn black. Many authors have studied this transformation, but only a few in the context of the archeological site of Pompeii. In this work, the co-occurrence of different degradation patterns associated with Pompeian cinnabar-containing fresco paintings (alone or in combination with red/yellow ocher pigments) exposed to different types of environments (pre- and post-79 AD atmosphere) is reported. Results obtained from the in situ and laboratory multianalytical methodology revealed the existence of diverse transformation products in the Pompeian cinnabar, consistent with the impact of the environment. The effect of hydrogen sulfide and sulfur dioxide emitted during the 79 AD eruption on the cinnabar transformation was also evaluated by comparing the experimental evidence found on paintings exposed and not exposed to the post-79 AD atmosphere. Our results highlight that not all the darkened areas on the Pompeian cinnabar paintings are related to the transformation of the pigment itself, as clear evidence of darkening associated with the presence of manganese and iron oxide formation (rock varnish) on fragments buried before the 79 AD eruption has also been found. The research leading to these results has received funding from “la Caixa” Foundation (Silvia Pérez-Diez, ID 100010434, Fellowship code LCF/BQ/ES18/11670017). A.P.M. is a Serra Húnter fellow. A.P.M’s research was supported by a Beatriu de Pinós postdoctoral grant (2017 BP-A 00046) of the Government of Catalonia’s Secretariat for Universities & Research of the Ministry of Economy and Knowledge. This work has been supported by the project MADyLIN (BIA2017-87063-P) funded by the Spanish Agency for Research AEI (MINECO-FEDER/UE). The authors thank for the funding provided by University of the Basque Country through the Institutionally Sponsored Open Access.

In this work, an innovative non-destructive monitoring methodology based on the analysis over time of open-air rock art sites is presented. This approach is based on the combination of in situ spectroscopic and chemometric studies to diagnose and monitor the state of conservation of rock art sites. Data acquired over a period of time by non-invasive analytical techniques such as portable Raman spectrometry (RS) and handheld energy-dispersive X-ray fluorescence (HH-EDXRF) spectrometry are compared to detect physicochemical changes that could affect the rock painting integrity. To demonstrate the applicability of the proposed procedure, three analysis campaigns (between 2013 and 2016) were carried out, analyzing Levantine rock pictographs preserved in the rock shelter of Solana de las Covachas VI (Albacete, Spain; see Electronic Supplementary Material (ESM) Fig. S1). The analyzed areas showed different types of active weathering processes such as gypsum and calcium oxalate formation, giving rise to conservation issues such as painting fading, surface loss, microbial colonizations, and formation of crusts. Results evidence that the proposed methodology can be very useful to monitor chemical changes in the surface of the walls where the rock art is located, thus obtaining crucial information for its preservation and management.

Personal ornaments have become a key cultural proxy to investigate cognitive evolution, modern human dispersal, and population dynamics. Here, we reassess personal ornaments found at Zhoukoudian Upper Cave and compare them with those from other Late Paleolithic Northern Chinese sites. We reappraise the information provided by Pei Wen Chung on Upper Cave personal ornaments lost during World War II and analyze casts of 17 of them, along with two unpublished objects displayed at the Zhoukoudian Site Museum and three original perforated teeth rediscovered at the Zhoukoudian Site Museum. We apply archeozoological, technological and use-wear analyses to document variation in ornamental practices and their change throughout the site stratigraphy. Badger, fox, red deer, sika deer, marten, and tiger teeth as well as carp bone, bird bone, Anadara shell, limestone beads, and perforated pebble appear to have been the preferred objects used as ornaments by Upper Cave visitors. Multivariate analysis of technological data highlights a correspondence between cultural layers and perforation techniques, with radial incising being typical of layer L2 and bidirectional incising of L4. The three rediscovered badger canines display features suggesting they were sewed on clothing rather than suspended from necklaces or bracelets. Elemental scanning electron microscopy coupled with energy dispersive X-ray spectromety and mineralogical (μ-Raman) analyses of red residues adhering to the rediscovered teeth indicate these objects were originally coated with ochre and identify variations that match differences in technology. The two ornaments exhibited at the Zhoukoudian Site Museum are ancient teeth that were recently perforated and should be excluded from the Upper Cave assemblage. A seriation of Late Paleolithic ornaments found at Northern Chinese sites identifies a clear-cut difference in preferred ornament types between western and eastern sites, interpreted as reflecting two long-lasting traditions in garment symbolic codes. acceptedVersion

Cueva de Ardales in Málaga, Spain, is one of the richest and best-preserved Paleolithic painted caves of southwestern Europe, containing over a thousand graphic representations. Here, we study the red pigment in panel II.A.3 of “Sala de las Estrellas,” dated by U-Th to the Middle Paleolithic, to determine its composition, verify its anthropogenic nature, infer the associated behaviors, and discuss their implications. Using optical microscopy, scanning electron microscopy coupled with energy dispersive X-ray spectroscopy, micro-Raman spectroscopy, and X-ray diffraction, we analyzed a set of samples from the panel and compared them to natural coloring materials collected from the floor and walls of the cave. The conspicuously different texture and composition of the geological samples indicates that the pigments used in the paintings do not come from the outcrops of colorant material known in the cave. We confirm that the paintings are not the result of natural processes and show that the composition of the paint is consistent with the artistic activity being recurrent. Our results strengthen the hypothesis that Neanderthals symbolically used these paintings and the large stalagmitic dome harboring them over an extended time span.

The origin and evolution of hominin mortuary practices are topics of intense interest and debate1–3. Human burials dated to the Middle Stone Age (MSA) are exceedingly rare in Africa and unknown in East Africa1–6. Here we describe the partial skeleton of a roughly 2.5- to 3.0-year-old child dating to 78.3 ± 4.1 thousand years ago, which was recovered in the MSA layers of Panga ya Saidi (PYS), a cave site in the tropical upland coast of Kenya7,8. Recent excavations have revealed a pit feature containing a child in a flexed position. Geochemical, granulometric and micromorphological analyses of the burial pit content and encasing archaeological layers indicate that the pit was deliberately excavated. Taphonomical evidence, such as the strict articulation or good anatomical association of the skeletal elements and histological evidence of putrefaction, support the in-place decomposition of the fresh body. The presence of little or no displacement of the unstable joints during decomposition points to an interment in a filled space (grave earth), making the PYS finding the oldest known human burial in Africa. The morphological assessment of the partial skeleton is consistent with its assignment to Homo sapiens, although the preservation of some primitive features in the dentition supports increasing evidence for non-gradual assembly of modern traits during the emergence of our species. The PYS burial sheds light on how MSA populations interacted with the dead. Primary and intentional deposit Burial versus funerary caching Taxonomic assessment Implications for human cultural evolution Online content

The aqueduct of Les Ferreres is a major element of the Archaeological Ensemble of Tarraco. Although the ashlars of the aqueduct are stacked without mortar, lime was used in some parts and lime was certainly used in later repairs. Worthy of note is a coating mortar used in a well-documented restoration (1854–1856). In this study, a limekiln found near the Roman aqueduct has been archaeomagnetically dated to determine if it was used for the construction of the aqueduct or in later repairs. The mean values for the measured archaeomagnetic direction from the limekiln were compared with two different archaeomagnetic models (SCHA.DIF.3k and GUMF1), and both indicate that the limekiln is modern with ages only slightly older than the well-documented restoration. The extensive use of the coating mortar in that restoration is consistent with the need of onsite lime production. Additional archaeomagnetic intensity has not contributed to constrain further the obtained archaeomagnetic age but the intensity datum can be added to archaeomagnetic intensity datasets to enhance geomagnetic intensity field models. The paper illustrates how archaeomagnetic dating can be useful to characterize secondary structures of major cultural heritage monuments. © 2020, Springer-Verlag GmbH Germany, part of Springer Nature.

African Middle Stone Age (MSA) populations used pigments, manufactured and wore personal ornaments, made abstract engravings, and produced fully shaped bone tools. However, ongoing research across Africa reveals variability in the emergence of cultural innovations in the MSA and their subsequent development through the Later Stone Age (LSA). When present, it appears that cultural innovations manifest regional variability, suggestive of distinct cultural traditions. In eastern Africa, several Late Pleistocene sites have produced evidence for novel activities, but the chronologies of key behavioral innovations remain unclear. The 3 m deep, well-dated, Panga ya Saidi sequence in eastern Kenya, encompassing 19 layers covering a time span of 78 kyr beginning in late Marine Isotope Stage 5, is the only known African site recording the interplay between cultural and ecological diversity in a coastal forested environment. Excavations have yielded worked and incised bones, ostrich eggshell beads (OES), beads made from seashells, worked and engraved ocher pieces, fragments of coral, and a belemnite fossil. Here, we provide, for the first time, a detailed analysis of this material. This includes a taphonomic, archeozoological, technological, and functional study of bone artifacts; a technological and morphometric analysis of personal ornaments; and a technological and geochemical analysis of ocher pieces. The interpretation of the results stemming from the analysis of OES beads is guided by an ethnoarcheological perspective and field observations. We demonstrate that key cultural innovations on the eastern African coast are evident by 67 ka and exhibit remarkable diversity through the LSA and Iron Age. We suggest the cultural trajectories evident at Panga ya Saidi were shaped by both regional traditions and cultural/demic diffusion. acceptedVersion

Lumps of mineral pigments are the more widespread archaeological remains found at Mousterian sites that may have been used by Neanderthals for symbolic activities. The characterisation of their chemical composition is essential to identify behavioural consistencies in their selection, transformation, and use, reconstruct changes through time in Neanderthals cultural practices, and discuss the emergence of symbolic cultures. In the Dordogne department of France, hundreds of black lumps, often bearing traces of intentional modification, were recovered at Middle (MP) and Upper Palaeolithic (UP) sites. In this paper we apply particle-induced X-ray emission (PIXE) to a representative sample of black lumps recovered at three MP and four UP sites as well as eight geological outcrops from this region with the aim of using major, minor, and trace elements content to identify potential sources and explore intra- and inter-site variability in the use of black colouring matter. Results suggest that MP and UP communities systematically searched for and surveyed Mn-rich formations to collect Mn-rich lumps. Differences in composition indicate that archaeological lumps were collected at a number of different outcrops, not sampled in the present study. A higher compositional variability is observed at UP compared to MP sites with single cultural layers. This suggests that UP modern humans may have, in some cases, exploited a wider range of Mn-rich sources than Mousterian Neanderthals.

Beads are a communication technology used by humans to transmit information on the wearer identity to members of the same or neighbouring groups by means of a shared symbolic language. Here we focus on the earliest evidence from Eastern Asia of a communication technology – the production of artificially coloured beads – that has allowed humans to further complexify the messages conveyed by personal ornaments, and associate, to some extent, the performance characteristics of beads and pigment. We study six ochred ostrich eggshell beads (OESB) from Shuidonggou Locality 2 (SDG2), Cultural Layer (CL) 2, China, dated to c. 31 kyr cal BP. Analysis of the beads manufacturing technique, size, and wear, combined with SEM-EDS and µ-Raman spectroscopy (µ-RS) study of well-preserved red residues sampled on the beads and sediment from CL2 indicate that these beads come from body ornaments and that red residues are the remnant of a pigmented compound coating the beads at the time they were worn by the SDG Palaeolithic visitors. SDG2-CL2 red stained OESBs thus represent, with the red stained bone disk from Xiaogushan, the earliest consistent evidence of pigment use for symbolic activities from China. Results also identify variations in the composition of the pigmental compound used to colour the beads that closely match differences in bead technology, size, and style. We argue that such a hitherto unknown consistency in bead production and decoration may reflect technological, morphological, and pigment coating standardisation at the individual level, standardisation in technology associated with variation in morphology and pigment at the group level, and substantial differences in these three domains at inter-group level.

The originally published version of this Article contained an error in Fig. 3, whereby an additional unrelated graph was overlaid on top of the magnetic susceptibility plot. Furthermore, the Article title contained an error in the capitalisation of ‘Stone Age’. Both of these errors have now been corrected in both the PDF and HTML versions of the Article.

Because of the fact that pigments are not ubiquitous in the archeological record, the application of noninvasive analytical methods is a necessity. In this work, pink and purple lake pigments recovered from the excavations of the ancient city of Pompeii (Campania, Italy) and preserved in their original bowls at the Naples National Archaeological Museum (Italy) were analyzed to characterize the composition of their inorganic binders (mordants). In situ preliminary analyses using a hand-held energy dispersive X-ray fluorescence spectrometer (HH-ED-XRF) allowed us to determine the use of an aluminosilicate enriched in Cu and Pb. Scanning electron microscopy coupled to energy dispersive X-ray spectrometry (SEM-EDS) and benchtop ED-XRF analyses confirmed these results, while inductively coupled plasma mass spectrometry (ICPMS) allowed one to determine the concentration of major, minor, and trace elements. The use of other techniques such as X-ray diffraction (XRD), and micro-Raman and infrared spectroscopies allowed one to characterize the pigments at the molecular level. The high concentration of Cu detected in the pigments (1228–12937 μg g–1) could be related to the addition of Cu salts to obtain the desired final hue. The concentrations of Pb (987–2083 μg g–1) was also remarkable. Lead isotopic ratio analysis (206Pb/207Pb) suggested a possible origin related to the leaching of the ancient lead pipes from Pompeii and the subsequent transfer to the buried pigments or to the inorganic binder. Molecular analysis also showed that the binder is composed of an allophane-like clay. Moreover, it was possible to determine that to obtain the final purple hue of a specific pigment, Pompeian blue pigment was also mixed into the dyed clay. The authors would like to thank the Naples National Archaeological Museum for the permissions given to perform the in situ measurements of the raw lake pigments contained in the original bowls and deposited in this museum and also for the permissions given to extract samples from these pigment bowls. This work has been funded by the Ministry of Economy and Competitiveness (MINECO) and the European Regional Development Fund (FEDER) through the Project DISILICA-1930 (ref BIA2014-59124-P). Iker Marcaida is grateful to the Basque Government who funded his predoctoral fellowship. Technical support provided by the General X-ray Service of the SGIKer (UPV/EHU, MICINN, GV/EJ, ERDF, and ESF) for the X-ray diffraction analyses and also by the Raman-LASPEA Laboratory of the SGIker (UPV/EHU, MICINN, GV/EJ, ERDF, and ESF) is also gratefully acknowledged.

The red disks from El Castillo Cave are among the earliest known cave paintings. Here, we combine the morphometric and technological study of red disks from two areas located at the end of the cave with the microscopic, elemental, and mineralogical analysis of the pigment and compare the results obtained with observations derived from experimental replication. Ergonomic constraints imply that a number of disks were made by adults, and the differences in pigment texture and composition suggest that they correspond to an accumulation through time of panels made by different persons who shared neither the same technical know-how nor, very possibly, the same symbolic system.