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13 pages, 7321 KiB

Open AccessArticle

Experimental Development of Transport Percussion Marks on Obsidian Clasts, Pilauco Site, Chilean Northwestern Patagonia

by Catalina Madrigal, Haroldo Lledó, Daniel Fritte and Mario Pino

Minerals 2022, 12(3), 343; https://doi.org/10.3390/min12030343 - 11 Mar 2022

Viewed by 2400

Abstract

In the Pilauco site (40°34′11″ S, 73°06′17″ W; 13,570 ± 70–12,540 ± 90 14C year BP), a previous geochemical trace analysis suggested that the Puyehue-Cordón Caulle Volcanic Complex is the most likely source for obsidian and dacitic glass artifacts at Pilauco. It was [...] Read more.

In the Pilauco site (40°34′11″ S, 73°06′17″ W; 13,570 ± 70–12,540 ± 90 14C year BP), a previous geochemical trace analysis suggested that the Puyehue-Cordón Caulle Volcanic Complex is the most likely source for obsidian and dacitic glass artifacts at Pilauco. It was hypothesized that the glassy rocks were probably collected from a pebble beach deposit, as deduced by the presence of crescentic percussion marks on the artefact cortexes. An experimental study was designed using pebble obsidian clasts. Bidirectional transport produced by the waves on a beach was imitated by an oscillating table, using time lapses equivalent to a transport of 0.7 to 20 km. One hundred clasts were randomly selected and marked. The morphological changes were registered, measured and photographed after seven sequential runs. At the end of the experiment at 20 km, the mass loss of rounded and fractured clasts was 5% and 11%, respectively. Crescent, circular, pseudo-circular and irregular percussion marks occurred in both types of clasts. In all cases, the crescent marks developed a pseudo-frosted surface appearance, giving a whiter tone that masks the black color of the obsidian, exactly as observed in the cortex of the artifacts knapped in dacitic glass at the Pilauco site. Thus, it is highly probable that the vitreous material was obtained from a beach sourced by the Puyehue-Cordón Caulle Volcanic Complex. Full article

(This article belongs to the Special Issue Characterization of Archaeological and Historic Vitreous Materials)

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29 pages, 25606 KiB

Open AccessArticle

Microscopic-Scale Examination of the Black and Orange–Yellow Colours of Architectural Glazes from Aššur, Khorsabad and Babylon in Ancient Mesopotamia

by Fanny Alloteau, Odile Majérus, Floriane Gerony, Anne Bouquillon, Christel Doublet, Helen Gries, Anja Fügert, Ariane Thomas and Gilles Wallez

Minerals 2022, 12(3), 311; https://doi.org/10.3390/min12030311 - 28 Feb 2022

Cited by 8 | Viewed by 3744

Abstract

Three major corpora of architectural glazed bricks from Ancient Mesopotamia dating to the Neo-Assyrian (Aššur and Khorsabad sites) and the Neo-Babylonian (Babylon site) Periods have been submitted to an in-depth comparative study of the orange–yellow and black glazes. Distinct hues in the orange–yellow [...] Read more.

Three major corpora of architectural glazed bricks from Ancient Mesopotamia dating to the Neo-Assyrian (Aššur and Khorsabad sites) and the Neo-Babylonian (Babylon site) Periods have been submitted to an in-depth comparative study of the orange–yellow and black glazes. Distinct hues in the orange–yellow range were observed according to the archaeological site. They appear to have been well mastered by the glassmakers, consisting in the ex situ preparation of the antique lead antimonate pigment and its mixing with transparent soda-lime glass frit or with the glass-forming components. The intentional addition of hematite or of Cu²⁺ colouring ions in a controlled amount is suggested in two cases. SEM-EDX and Raman analysis of the lead antimonate pigments have pointed out different chemical substitutions in their pyrochlore structure, mainly Fe³⁺ in the Sb⁵⁺ site and Ca²⁺ in the Pb²⁺ site, the proportion of which being correlated to the pigment shade (from pale yellow to orange–red). Part of these substitutions arises from the chemical reaction of the pigment with the hematite and glass melt during firing. Regarding the black glazes, an unexpected colouring technique involving copper sulphide nanoparticles together with the chromophore Fe³⁺-S²⁻ is highlighted for Khorsabad (8th century BC) and for Babylon (6th century BC). For Aššur blacks, the study reveals a change in their colouring technique between the 9th and 8th centuries BC, from a colouration with Mn oxides to an enigmatic one that could also have involved copper sulphide nanoparticles. Full article

(This article belongs to the Special Issue Characterization of Archaeological and Historic Vitreous Materials)

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19 pages, 8287 KiB

Open AccessArticle

Sand and Pebbles: The Study of Portuguese Raw Materials for Provenance Archaeological Glass

by Inês Coutinho, Teresa Medici, Bernard Gratuze, Andreia Ruivo, Pedro Dinis, Augusta Lima and Márcia Vilarigues

Minerals 2022, 12(2), 193; https://doi.org/10.3390/min12020193 - 2 Feb 2022

Cited by 4 | Viewed by 2185

Abstract

Portuguese archaeological excavations dated to the 17th century onwards are extremely rich in glass artefacts, with this being a reality from the north to the south of the territory. Contrasting with this reality, no glass production locations from this period have been discovered [...] Read more.

Portuguese archaeological excavations dated to the 17th century onwards are extremely rich in glass artefacts, with this being a reality from the north to the south of the territory. Contrasting with this reality, no glass production locations from this period have been discovered or excavated so far, which makes the provenance attribution a challenging endeavour. One specific archaeological location, the Monastery of Santa Clara-a-Velha in Coimbra, held one of the largest glass archaeological assemblages dated to the 17th century unearthed in Portugal so far. Due to the large variety of objects’ shapes, glass colours and decorative features, this assemblage is a valuable candidate to hold glass artefacts produced in Portugal. Lacking archaeological excavation on glass furnaces in Portugal, the study of glassmaking raw materials is the most promising research line to investigate the provenance of glass circulating in Portugal. In this study, sand and pebbles from six different locations in the north/centre of Portugal were collected and melted to produce glass samples. The resulting glass samples were chemically characterised using LA-ICP-MS, to obtain the composition of the samples in major, minor and trace elements. The obtained results were compared with the composition of 37 historical samples from the Monastery of Santa Clara-a-Velha previously studied. Additionally, the thermal properties of selected synthesised glasses were analysed by Differential Scanning Calorimetry, allowing new insights on melting temperatures and glass workability. Results indicate that three artefacts with stylistic features attributed to a Portuguese production were locally made with sands collected in Coimbra. Full article

(This article belongs to the Special Issue Characterization of Archaeological and Historic Vitreous Materials)

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17 pages, 5826 KiB

Open AccessArticle

Bodies and Glazes of Architectural Ceramics from the Ilkhanid Period at Takht-e Soleyman (North-Western Iran)

by Stefan Röhrs, Alexandra Dumazet, Katharina Kuntz and Ute Franke

Minerals 2022, 12(2), 158; https://doi.org/10.3390/min12020158 - 27 Jan 2022

Cited by 7 | Viewed by 2928

Abstract

Bodies and glazes of tiles from the Ilkhanid period found at the UNESCO World Heritage site of Takht-e Soleyman were studied to identify materials and certain technical characteristics of the architectural ceramics as part of a larger project to establish different productions. In [...] Read more.

Bodies and glazes of tiles from the Ilkhanid period found at the UNESCO World Heritage site of Takht-e Soleyman were studied to identify materials and certain technical characteristics of the architectural ceramics as part of a larger project to establish different productions. In addition, ceramic vessels and technical ceramics excavated at the site were analysed for comparison. µXRF, SEM/EDX, and Raman spectroscopy were used for the material investigations. Qualitative non-invasive µXRF results allowed for categorisation of the glazes and ceramic bodies based on their overall composition. Quantitative analysis by SEM/EDX on a subset of the samples delivered detailed results on the bodies and glazes. Tiles, made from clay or stonepaste, were almost exclusively decorated with a mixed alkaline lead glaze. The PbO content of this type of glaze ranged from 8 wt% to 25 wt%. The clay bodies of some tiles corresponded to the material of the locally used kiln furniture. Moreover, glaze residues preserved on the kiln furniture proved to be from a mixed lead alkaline glaze with a PbO content of 15 wt% to 25 wt%, a composition that is comparable to the tiles’ glazes. For more insights into the local or regional production of the tiles, supplementary in-depth studies including petrographic analysis would be needed to confirm and further specify the results. Full article

(This article belongs to the Special Issue Characterization of Archaeological and Historic Vitreous Materials)

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14 pages, 4497 KiB

Open AccessArticle

On the Surface and Beyond. Degradation Morphologies Affecting Plant Ash-Based Archaeological Glass from Kafir Kala (Samarkand, Uzbekistan)

by Sara Fiorentino, Tania Chinni, Dagmar Galusková, Simone Mantellini, Alberta Silvestri, Amriddin E. Berdimuradov and Mariangela Vandini

Minerals 2021, 11(12), 1364; https://doi.org/10.3390/min11121364 - 2 Dec 2021

Cited by 7 | Viewed by 3367

Abstract

The study focuses on an assemblage of glass finds from the citadel of Kafir Kala, Uzbekistan, located along one of the major Eurasian branches of the “Silk Roads” with a consistent occupation between the 8th and 12th century CE. Glass fragments for this [...] Read more.

The study focuses on an assemblage of glass finds from the citadel of Kafir Kala, Uzbekistan, located along one of the major Eurasian branches of the “Silk Roads” with a consistent occupation between the 8th and 12th century CE. Glass fragments for this study were selected based on marked surface alterations they showed, with stratified deposits of different thickness and colours. Starting from a preliminary observation under Optical Microscope, fragments were clustered into four main groups based on the surface appearance of the alterations; Scanning Electron Microscopy investigations of the stratigraphy of the alteration products were then carried out, to evaluate micro-textural, morphological and compositional features. Data from the analyses allowed identifying preferential patterns of development of the various degradation morphologies, linkable to compositional alterations of the glass due to burial environment and the alkali leaching action of the water. Iridescence, opaque weathering (at times associated with black stains), and blackening were identified as recurring degradation morphologies; as all but one sample were made of plant ash-based glass, results show no specific correlation between glass composition and the occurrence of one or the other degradation pattern, often found together. Framed in a broad scenario, the paper aims to set the basis for the development of a study approach dedicated to the degradation morphologies affecting archaeological glasses, a topic still lacking systematisation and in-depth dedicated literature. Full article

(This article belongs to the Special Issue Characterization of Archaeological and Historic Vitreous Materials)

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15 pages, 1497 KiB

Open AccessArticle

Trends in Colouring Blue Glass in Central Europe in Relation to Changes in Chemical Composition of Glass from the Middle Ages to Modern Age

by Zuzana Zlámalová Cílová, Michal Gelnar and Simona Randáková

Minerals 2021, 11(9), 1001; https://doi.org/10.3390/min11091001 - 14 Sep 2021

Cited by 6 | Viewed by 3552

Abstract

The study deals with the development of the chemical composition of blue glass from the 13th to the 19th century in the region of Bohemia (Central Europe). Nearly 100 glass samples (colourless, greenish, and blue) were evaluated by an XRF method to distinguish [...] Read more.

The study deals with the development of the chemical composition of blue glass from the 13th to the 19th century in the region of Bohemia (Central Europe). Nearly 100 glass samples (colourless, greenish, and blue) were evaluated by an XRF method to distinguish the colouring components of blue glass. As early as in the 13th century, blue glass based on ash containing colouring ions of Co and Cu was produced here. To achieve the blue colour of glass, a copper-rich raw material was most likely applied. This information significantly complements the existing knowledge about glass colouring in the Middle Ages, as the glass of later periods was typically coloured with raw materials containing cobalt. Full article

(This article belongs to the Special Issue Characterization of Archaeological and Historic Vitreous Materials)

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13 pages, 4532 KiB

Open AccessArticle

Melting Process and Viscosity of Bohemian Historical Glasses Studied on Model Glasses

by Karolína Pánová, Kristýna Jílková, Dana Rohanová, František Lahodný, Dagmar Galusková and Martin Míka

Minerals 2021, 11(8), 829; https://doi.org/10.3390/min11080829 - 30 Jul 2021

Cited by 2 | Viewed by 2317

Abstract

Analyzing the chemical composition of archaeological glasses can provide an insight into their provenance and raw materials used in their making. However, to the authors’ knowledge, the historical production process itself and melting characteristics of the glasses have not yet been extensively investigated. [...] Read more.

Analyzing the chemical composition of archaeological glasses can provide an insight into their provenance and raw materials used in their making. However, to the authors’ knowledge, the historical production process itself and melting characteristics of the glasses have not yet been extensively investigated. The main focus of this paper is to describe the melting process of three main types of Bohemian historical glasses: Gothic (14th–1st half of 16th c.); Renaissance (16th–17th c.); and Baroque (end of 17th–18th c.). The model glasses were prepared from natural raw materials and processes that take place during melting were investigated using optical microscopy, SEM-EDS, XRD, and DTA-TG methods. Furthermore, the viscosity of model glasses and thermal dilatation was measured and used to calculate the reference viscosity points. The results illustrate the complexity of historical glass melting, as well as the technological progress between different periods. Full article

(This article belongs to the Special Issue Characterization of Archaeological and Historic Vitreous Materials)

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Review

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42 pages, 9584 KiB

Open AccessReview

Cobalt and Associated Impurities in Blue (and Green) Glass, Glaze and Enamel: Relationships between Raw Materials, Processing, Composition, Phases and International Trade

by Philippe Colomban, Burcu Kırmızı and Gulsu Simsek Franci

Minerals 2021, 11(6), 633; https://doi.org/10.3390/min11060633 - 15 Jun 2021

Cited by 42 | Viewed by 10152

Abstract

Minerals able to colour in blue (and green in combination with yellow pigments) are limited in number and geologically. After presenting a short history of the use of cobalt as a colouring agent of glass, glaze and enamel in the Western/Mediterranean, Islamic and [...] Read more.

Minerals able to colour in blue (and green in combination with yellow pigments) are limited in number and geologically. After presenting a short history of the use of cobalt as a colouring agent of glass, glaze and enamel in the Western/Mediterranean, Islamic and Asian worlds since Antiquity, we will present the different forms (dissolved ions, natural and synthetic crystalline phases/pigments) of cobalt and associated elements regarding primary (transition metals) and secondary geological deposits (transition metals and/or arsenic, bismuth, silver). Attempts to identify the origin of cobalt have been made by many authors considering the associated elements but without considering the important modifications due to different processing of the raw materials (extraction/purification/formulation). We review the information available in the ancient reports and present literature on the use of cobalt, its extraction and production from the ores, the different geological sources and their relationship with associated elements (transition metals, bismuth, arsenic, and silver) and with technological/aesthetic requirements. (Partial) substitution of cobalt with lapis lazuli is also addressed. The relative application of non-invasive mobile Raman and pXRF analytical instruments, to detect mineral phases and elements associated with/replacing cobalt is addressed, with emphasis on Mamluk, Ottoman, Chinese, Vietnamese and Japanese productions. The efficiency of Ni-Zn-As diagram proposed by Gratuze et al. as a classification tool is confirmed but additionally, CoO-Fe₂O₃₋MnO and CoO-NiO-Cr₂O₃ diagrams are also found as very efficient tools in this research. The relationship between the compositional data obtained from the artefacts and historical questions on the origin and date of their production are discussed in order to obtain a global historical view. The need of a better knowledge of (ancient) deposits of cobalt ores and the evolution of cobalt ore processing with time and place is obvious. Full article

(This article belongs to the Special Issue Characterization of Archaeological and Historic Vitreous Materials)

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