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Beads from graves of the Samad Culture. Sultanate of Oman, and from an ancient craftsmen quarter of the old kingdom of Ruhuna. excavated in Sri Lanka, were investigated using electron microprobe analysis and X-ray powder diffraction. Both experimental methods were optimized towards a non-destructive analysis of archaeo­ logical finds. Based on thei...

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... metal beads investigated are hollow Table 2. ...
Context 2
... analysis of one of these beads shows that the spheres were made from pure Ag, Table 2). ...
Context 3
... (1990) describes the variation of colour of different alloys in the Au-Ag-Cu system, using an Au-Ag- Cu compositional triangle diagram. From this tri- angle, the original colour of the spheres is esti- mated as whitish, whereas the bond was whitish Table 2). The compositional variation of these added elements ranges from 5.5 to 31.5 ...

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... A CaO/MgO arány alapján a négy gránát a Srí Lanka-i torlatos lelőhelyekhez kötött heterogén X csoporton belül önálló halmazba tartozik (Rösch et al. 1997;Schüssler et al. 2001) (11. ábra), ami újabb típust feltételez a gránátok osztályozásában (Cluster H, Hans Albert Gilg szóbeli közlése alapján). ...
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... Intensive quarrying is attested in all these regions, and a synthesis of stylistic groups and technological traditions exist for the vessels (Phillips and Simpson 2018). What is still missing, however, is a petrographic synthesis of the quarried raw material, even though several case studies provide initial valuable insights (Rosch et al. 1997;Magee et al. 2005;Namdar et al. 2011). Additionally, there are also other, smaller UMS sources along the East African coast, namely the quarries around Masvingo, Zimbabwe, that provided the raw material for the famous soapstone birds and decorated bowls (Matenga 2011), as well as some isolated occurrences in South Africa (Rudner 1971;Evers 1979). ...
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... Jadeitite and mixed jades have been the subject of many analytical studies, including geological and physicochemical (Cameron et al. 1973;Cisowski et al. 2004;Clark et al. 1969;Compagnoni et al. 2007;D'Amico et al. 1995;Delaitte et al. 2010Delaitte et al. -2011Errera et al. 2012;Franz et al. 2014;Gil Ibarguchi 1995;Harlow 1993;Harlow et al. 1994Harlow et al. , 2011Harlow et al. , 2012aHarlow et al. , 2012bHarlow et al. , 2014Harlow et al. , 2015Hirajima & Compagnoni 1993;Kempe & Harvey 1983;Knaf et al. 2017;Lü et al. 2014;Macke et al. 2010;McClure 2012;Medaris et al. 1995;Mendoza et al. 2015;Morimoto et al. 1988;Ou Yang et al. 2011;Pétrequin et al. 2012aPétrequin et al. , 2017aPétrequin et al. , 2017cSeitz et al. 2001;Taube et al. 2004;Theye & Seidel 1991), archaeological Harrison & Orozco 2001;Pétrequin et al. 2012a;Rodríguez Ramos 2011;Rodríguez Ramos & Pagán Jiménez 2006;Surmely et al. 2001) and archaeometric, on Asian (Bishop et al. 1985, Chang et al. 2010Cook, 2013;Franz et al. 2014;Harlow et al. 2012b;Ou Yang et al. 2011;Rösch et al. 1997;Wang 2011;Wen & Jing 1992;Yang et al. 2004), American (Foshag & Leslie 1955;García-Casco et al. 2013;Harlow et al. 2006;Lange 1993;Ruvalcaba-Sil et al. 2008) and European samples (Coccato et al. 2014;Compagnoni et al. 2007Compagnoni et al. , 2012D´Amico 2005D´Amico , 2012D´Amico et al. 1995D´Amico et al. , 2003Domínguez-Bella et al. 2004;Domínguez-Bella et al. 2012Errera et al. 2012;Giustetto et al. 2018;Giustetto & Compagnoni 2014;Lozano et al., 2018;Odriozola et al. 2015;Pétrequin 2017;Pétrequin et al. 2012c;Querré et al. 2008;Rapp 2001;Ricq-de Bouard & Fedele 1993;Spišiak & Hovorka 2005). In all these approaches, information is provided regarding the nomenclature, the main and accessory minerals of jadeitite and mixed jades, the techniques used for their analysis and archaeometric information such as the identification of the source areas and the evidence of circulation of the artefacts made of this raw material. ...
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... The use of X-Ray diffraction for the study of historical/archaeological glasses is still sporadically attested, especially for non-invasive investigation purposes. Previous studies have focused on beads from the Sultanate of Oman and Sri Lanka (Rösh et al., 1997;Welter et al., 2007), Mosaic Tesserae from the monasteries of Daphi and Hosios Loukas in Greece (Arletti et al., 2010a), Iron Age beads from Northern Italy (Arletti et al., 2010b), Ca-antimonate in Roman glasses (Lahlil et al., 2010), mosaic Tesserae from St. Peter in Rome (Arletti et al., 2011b), archaeological red glasses from China (Zhu et al., 2012) and Iron-age findings from the Treviso province (Olmeda et al., 2015). X-ray Fig. 1. ...
Article
A totally non-destructive approach was employed to characterize beads from two Picene necropolises (Novilara-PU and Crocefisso-Matelica-MC) dating back to between 9th and 6th centuries B.C. Investigations were carried out principally by means of Reflectance Spectroscopy determining Co2+, Cu2+ and Fe3+ as the main chromophores, and by Raman Spectroscopy to distinguish samples realized with other materials, in particular bones and shells were recognized. Furthermore, Raman spectroscopy identified hematite as a coloring phase in the unique red bead discovered as unmelt crystals in blue and yellow beads. Additionally, X-Ray Diffractometry investigations indicated Ca-phosphates, bindhemite and the less common brizzite, as opacifiers in white and yellow beads, while chemical data collected through X-Ray Fluorescence evidenced differences between findings from the two localities and/or within the same site. Beads were found to belong to the Low Magnesium Glass (LMG) and High Magnesium Low Potassium (HMLK) classes with most blue beads being comprised of cobaltiferous alum salts and a relatively impure sand, and a calcareous sand having been used for all other analyzed beads. Finally, differentiations performed on the basis of MgO amounts tended to indicate the samples from Crocefisso as being more similar to Bronze Age compositions than the Novilara ones which are closer to typical Iron Age proportions. In addition, high amounts of lead have been detected in all the yellow beads, but they could be positively correlated to Sb2O3 only for samples recovered in the Novilara necropolis, thus indicating the use of lead antimonates as coloring agents.
... Further down the Oman peninsula glass finds from the Samad-period mostly include beads, which are characterised by high alumina and potassium contents and low manganese; a number of lead-silicate beads were also found. There is no evidence of local glass working (Rösch et al., 1997). ...
Thesis
The aim of this PhD was to develop non-destructive methods for the elemental and isotopic analysis of archaeological objects. Non-destructive or non-invasive chemical and isotopic analysis of archaeological objects is at the centre of current developments in archaeological science. The search for such methods is fed by both curiosity on the analytical limits of these methods and the possibilities they promise. Especially the possibility to analyse rare or precious objects, as well as the possibility to obtain both elemental and isotopic information using the same sample (hence reducing the amount of sampled material) are appealing. Developments achieved in this study were tested on case-studies and further refined if needed. Two material categories were investigated: glass and metal (here only lead). The case-studies were chosen for their archaeological interest, for their ability to answer specific questions regarding transitions in technology (for both glass studies) and the nature and use of coin-like lead objects during the Sasanian period. The case-studies were always elaborated in collaboration with archaeologists specialist of the sites, era, area and/or material category. This work in structured is two large sections: (i) method development, (ii) archaeological applications. The specific research questions on method development were: - Is it possible to obtain accurate and precise Sr, Nd and Pb isotopic ratios for glass objects non-invasively using laser ablation-multi-collector-mass spectrometry (LA-MC-ICP-MS)? If so, how can this be achieved? - Given that laser ablating metallic objects would lead to fouling of the instrument, is there an alternative solution for metallic objects? - What are the best measurement conditions to obtain accurate and precise chemical composition using micro-X-ray Fluorescence? - How useful is the obtained chemical and isotopic data to answer archaeological questions? It is shown that it is possible to obtain accurate and precise Sr and Pb isotopic compositions for archaeological glass through LA-MC-ICP-MS. Findings from the case-study on medieval glass restricted this conclusion to soda-lime silicate glasses. Sr isotopic analysis of soda-lime glass performed in medium-resolution (to avoid potential bias induced by rare earth elements), mass bias correction using 88Sr/86Sr as internal correction and relying on Russell's law provided the most accurate results. The precision is one order of magnitude lower than in solution analysis. Pb isotopic analysis was possible using a combination of internal (using 205Tl/203Tl) and external correction relying on Russell's law and Corning D for mass bias correction. As for Sr isotopic analysis, the precision is one order of magnitude below solution analysis. It was impossible to measure Nd isotopic compositions using laser ablation due to the low concentration of Nd in the glass (4 to 10ppm), leading to insufficient signals in the spectrometer. An alternative sampling technique for lead isotopic analysis of lead objects is explored by studying Sasanian coins. This alternative consists of passing a slightly acidified cotton swab over the coins. Comparison of the lead isotope composition determined through this method and using conventional sampling proved it to be a reliable, accurate and precise method, with results indistinguishable, within measurement error, between both sampling techniques. Leaving no visible stain on the coins, this method allows more objects to be analysed for their lead isotopic composition. The element composition, determined by micro-XRF, of soda-lime glass is best obtained using measurements performed at 40kV and 700micro-A with the Rh-tube as excitation source. The quantification was achieved by a combination of fundamental parameters and external calibration based on reference materials. The accuracy and precision is not as good as using other methods but sufficient to answer some archaeological questions such as the type of glass (mineral soda, plant ash, wood ash) and the nature of the colourant. For glass objects the elemental composition was also determined using ICP-OES and LA-ICP-MS. The merits and limitations of micro-XRF and LA-ICP-MS are discussed. For the lead objects micro-XRF measurements were performed using a W-tube at 50kV and 700micro-A and the quantification relied on fundamental parameters. Invasive (LA) or destructive (ICP-OES) analysis was not allowed for these objects. The thus developed methods were applied to three archaeological case-studies: - Glass of first century CE Dibba, UAE - Sasanian lead coins - Medieval stained glass windows from Stavelot and Baume-Les-Messieurs Precious little is known on glass manufacture, trade and consumption on the Oman peninsula in pre-Islamic times. Glass is found in the archaeological record, but often not discussed in detail (though it is recorded and sometimes described). An exception is the site of Ed-dur, on the northern part of the Oman peninsula in the present-day UAE. Dibba, is a city on the southern part of the peninsula with a large assemblage of broken glass. A Roman origin was expected similar to the results of the contemporary site of Ed-dur. However, the glass proved to be neither Roman nor Indian and comparison with local sands makes a local origin also highly unlikely. Given the recipe, it is more probable the glass was made somewhere in Mesopotamia. The study also showed that these objects were early examples of mould-blown glass and that the craftsmen were able to control the oxidation conditions in the furnace to obtain amber glass. This assemblage leaves us with the question why there was this import of Mesopotamian glass alongside the ubiquitous Roman glass in circulation on the Oman Peninsula. In the second case-study, a range of Sasanian coin-like objects were investigated. Here, the question is whether these were coins used for everyday transactions, votive objects or rather some emergency currency minted by local rulers in times of need. The overall continuity in chemical composition in time and uniformity in space of the isotopic and elemental composition leads to the conclusion that most of these were indeed coins used for everyday transactions whose composition was controlled by the central government. The only exception are a set of later coins, struck under Husraw II using raw materials from the newly conquered Caucasus region. These coins look like drachme and were probably struck to commemorate this conquest. The glass assemblages from Baume-Les-Messieurs and Stavelot are two contemporary examples of the transition from natron-based to wood ash-based glass recipes. This is a transition in glass making tradition occurring in the medieval period in (North)-Western Europe. Examples of sites documenting this transition are scarce, and no isotopic analysis has been performed on such assemblages before. These samples are a unique chance to obtain an insight into this transition. We wanted to know whether the craftsmen, the raw materials or finished products travelled between those sites, or whether it was simply knowledge or information that was shared. This case-study showed that the method developed for the Sr isotope analysis did not allow for correct determination of the isotopic ratio. However, it was still possible to answer the question satisfactorily. The material from both sites has a different provenance. Nevertheless, we suggest there must be a link between both, as they are the only sites switching to wood ash based recipes in that period and both are monasteries of the Benedictine order.
... This is due to the fact that the natural mineral talc (Mg 3 Si 4 O 10 (OH) 2 ) is transformed into enstatite and SiO 2 while being heated to a temperature between 800 to 1100°C (Aglietti 1994;Balek et al. 2008). The know-how and required technology for heat-induced enstatite manufacturing out of talc were already available at ancient times, starting in the fifth and fourth millennia BCE (Panei et al. 2005;Rösch et al. 1997;Hegde 1983;Pickard and Schoop 2013). ...
... The formation of distinguishable phases depending on the firing temperature during manufacture of archaeological objects is an important source of information to deduce the manufacturing process and get a deeper insight into the technology used in ancient times (Rösch et al. 1997). ...
... The use of X-Ray diffraction for the study of historical/archaeological glasses is still sporadically attested, especially for non-invasive investigation purposes. Previous studies have focused on beads from the Sultanate of Oman and Sri Lanka (Rösh et al., 1997;Welter et al., 2007), Mosaic Tesserae from the monasteries of Daphi and Hosios Loukas in Greece (Arletti et al., 2010a), Iron Age beads from Northern Italy (Arletti et al., 2010b), Ca-antimonate in Roman glasses (Lahlil et al., 2010), mosaic Tesserae from St. Peter in Rome (Arletti et al., 2011b), archaeological red glasses from China (Zhu et al., 2012) and Iron-age findings from the Treviso province (Olmeda et al., 2015). X-ray Fig. 1. ...
Poster
Studies carried out in the last decades defined that two main ethnic groups existed along the Italian Adriatic coast from the beginning of the Iron Age to the Romans conquest: Japigi and Sabelli, which were in turn divided into various tribes, including Picenes, living in the current coastal area of the Marche and of the northern Abruzzo regions between the 1st millennium B.C. and the 3rd century A.D. The excavations of two Picene necropolises in Novilara (9th-7th century B.C, PU) and Matelica (9th-6th century B.C., MC) uncovered various grave goods including many colored glass, shell and bone-based beads. A non-invasive characterization these beads has been performed by means of analytical techniques such as Reflectance and Raman spectroscopy and X-Ray diffraction. Raman spectroscopy resulted particularly useful in the characterization of shell and bone based beads, displaying the typical spectra of calcite and Ca-phosphate, respectively, parallel reflectance spectroscopy gave information about the use of different chromophores in blue glass beads: as expected spectra of the darker samples contain the typical features of tetrahedral Co2+ ions, while data obtained from the two light blue beads available, coming from the Matelica necropolis, showed no traces of this metal but only the spectral profile deriving from the presence of Cu2+ ions. As known from literature, turquoise glass was commonly used during the Bronze Age, while cobalt started to be employed as a colorant during the Final Bronze Age in association with copper and then became the dominant metal to obtain dark hues due to its high colouring efficiency. Both Reflectance and Raman Spectroscopy allowed the identification of hematite as the colouring agent of the only red bead available, coming from the Novilara necropolis. This is a very peculiar result, since no literature data have been reported so far, to the best of our knowledge, about the use of hematite in glassy beads dated to the Iron Age. White and yellow samples were mainly studied by XRD: in both cases the use of traditional opacifiers such as Ca and Pb antimonates was demonstrated. Yellow samples in particular displayed the presence of lead pyroantimonate (Pb2Sb2O7), whose diffraction peaks could be well distinguished over the broad glass structure; on the contrary, the collection of patterns from white samples, exhibiting a black surface decorative coating, gave results that were more difficult to interpret.
... Moreover, such results could then be compared with data obtained for garnets from modern sources (e.g. Löfgren, 1973;Rösch et al., 1997;Farges, 1998;Greiff, 1998;Quast and Schüssler, 2000;Calligaro et al., 2002). ...
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The archaeological site of Arikamedu, located in Tamil Nadu State on the east coast of India, was the centre for many centuries of a significant bead-producing industry. Beads were made of both glass and stone, including garnet, but the source of the garnet rough material has not been confirmed. To probe this question, garnet beads found at Arikamedu were compared with rough material from the Garibpet deposit, located approximately 640 km away in Telangana State, east of the city of Hyderabad, India. Samples from the two localities exhibited substantial correlation with respect to average composition, trace-element contents, chemical zoning of major and minor elements, inclusion assemblages and zoning of inclusions between the rims and cores of the crystals. Chemically, the stones were almandine rich (averaging 81.0% almandine, 11.5% pyrope, 3.3% spessartine and 1.5% grossular), with pronounced zoning for Mn and Mg. Zoning of trace elements also was observed, especially for Y, P and Zn. The most characteristic aspects of the inclusion pattern were sillimanite fibres that were concentrated in a zone between an inclusion-rich core and an inclusion-poor rim. In combination, the microscopic observations, identification of the inclusion assemblage, and chemical analyses established that the rough material used historically in the Arikamedu area to produce garnet beads originated from the Garibpet deposit. Furthermore, the results suggest that existing schemes for classifying historical garnets require additional refinement.
... Da notare inoltre anche la presenza di una perla in pasta bianca, probabilmente enstatite 24 , appartenente al tipo B (perle a disco cilindriche) confrontabile con le numerose perle rinvenute nel sito di Ra>s al-Hadd, nell'Oman settentrionale 25 . ...
... The predominant characteristic of this glass is the large amount of copper that was added to produce the orange and red colours (Dussubieux 2001;Dussubieux and Gratuze 2003a;Lankton and Dussubieux 2006). The concentration of copper in this glass is generally more than 10 wt% and the colour is produced by the dispersion of cuprite in the glass matrix (Rösch et al. 1997;Welter et al. 2007). Iron is also generally relatively high in this glass. ...
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This volume represents a comprehensive and essential collection of essays by Southeast Asia's leading archaeologists actively researching in the field