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Mineral Pigments in the Historical and Archaeological Context: from Invasive to Non-invasive Analyses

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A special issue of Minerals (ISSN 2075-163X). This special issue belongs to the section "Crystallography and Physical Chemistry of Minerals & Nanominerals".

Deadline for manuscript submissions: closed (31 March 2021) | Viewed by 30456

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Special Issue Editors

Prof. Dr. Domenico Miriello

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Guest Editor

Department of Biology, Ecology and Earth Sciences, University of Calabria, Via Pietro Bucci, 87036 Rende, Italy
Interests: archaeometry; mortars; plasters; pottery; ancient stones; petrography and mineralogy applied to the cultural heritage

Dr. Raffaella De Luca

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Guest Editor

Department of Biology, Ecology and Earth Sciences, University of Calabria, Via Pietro Bucci, 87036 Rende, CS, Italy
Interests: materials characterization; archaeometry; technologies applied to cultural heritage; ancient mortars and plasters, pigments

Dr. Michele Secco

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Guest Editor

Department of Cultural Heritage (DBC), University of Padova, 35139 Padova, Italy
Interests: cultural heritage; archaeometry; materials science; applied mineralogy; ancient and modern binding materials (lime, cement, mortars, plasters, renders, concretes); characterization of ancient masonry; pigments; characterization and conservation of decorated surfaces

Special Issue Information

Dear Colleagues,

The use of mineral pigments, present in nature inside rocks and soils, dates back to ancient times, starting from the Palaeolithic cave paintings, until today, with the introduction of mineral pigments of synthesis.

Their use has always been widespread in the field of cultural heritage for the decoration of several objects and artefacts with historical, archaeological and artistic value, such as frescoes, mural paintings, and paintings on canvas, wood, paper (e.g., manuscripts), ceramic materials, glass, and many other supports.

The study of mineral pigments can be performed with invasive or non-invasive analyses that can be carried out in situ, with a portable instrumentation, or in a laboratory setting. The most common techniques used for their compositional characterization are optical microscopy (OM), colorimetry, X-ray diffractometry (XRPD), X-ray fluorescence (XRF), Raman spectroscopy, FT-IR spectroscopy, multispectral and hyperspectral imaging, EPR spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), laser ablation with inductively coupled plasma mass spectrometry (LA-ICP-MS), but also other several methodologies can be applied.

This Special Issue will publish works concerning the use of mineral pigments in the field of cultural heritage and, in particular, in historical and archaeological contexts. Studies carried out on natural and synthetic pigments will be considered, performed through invasive or non-invasive analyses (mentioned above), applied in situ and/or in a laboratory setting, but also through specifically developed innovative technologies.

The Special Issue will include studies in the archaeometry field that highlight particular aspects of the production technology and/or concern historical and archaeological issues (e.g., provenance of the mineral pigments, supply of raw material, trade routes, etc.) and works finalized to the characterization of the mineral pigments and to the evaluation of their state of conservation, in order to solve restoration problems. Works concerning the conservation field will be also considered, with a focus on the use and the introduction of new consolidants and protective products aimed at preserving the pigmented surfaces.

Prof. Domenico Miriello
Dr. Raffaella De Luca
Dr. Michele Secco
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Minerals is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2400 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

archaeometry
characterization
production technology
provenance
conservation
restoration
consolidant and protective products
geochemistry
cultural heritage

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Published Papers (8 papers)

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Research

27 pages, 15707 KiB

Open AccessArticle

Methodological Approach (In Situ and Laboratory) for the Characterisation of Late Prehistoric Rock Paintings—Penedo Gordo (NW Spain)

by Jose Santiago Pozo-Antonio, Beatriz Comendador Rey, Lara Alves Bacelar and Pablo Barreiro

Minerals 2021, 11(6), 551; https://doi.org/10.3390/min11060551 - 22 May 2021

Cited by 3 | Viewed by 2957

Abstract

This paper draws on the study of the prehistoric art site of Penedo Gordo (NW Spain) resulting from a collaborative interdisciplinary research. One of its primary goals was to design and put into practice a multi-analytical protocol for characterising prehistoric rock paintings, combining in situ and laboratory analytical techniques. Thus, following the archaeological assessment of the site, the panels exhibiting red paintings were analysed by colour spectrophotometry and portable Raman spectroscopy. Analytical techniques were applied to a collection of samples exhumed from the excavation that simultaneously took place on site. These included three red accretions on different substrates (compact soil, white quartzite and grey quartzite) and stone fragments representative of the outcrop’s petrographic variability, aiming to determine their mineralogical composition, texture and study the stone-paint boundaries. Moreover, colouring materials exhumed from the excavation and collected in the immediate surroundings of the rock outcrop were analysed in order to scrutinise the provenience rock art’s raw materials. Laboratory analysis consisted of stereomicroscopy, X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy. One of the major outcomes was the discovery of a drop of red pigment preserved in an archaeological layer associated with Late Neolithic/Copper Age material remains. Full article

(This article belongs to the Special Issue Mineral Pigments in the Historical and Archaeological Context: from Invasive to Non-invasive Analyses)

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21 pages, 9310 KiB

Open AccessArticle

Analytical Approach for the Study of Teotihuacan Mural Paintings from the Techinantitla Complex

by José Luis Ruvalcaba-Sil, Luis Barba, Edgar Casanova-González, Alejandro Mitrani, Margarita Muñoz, Isaac Rangel-Chavez, Miguel Ángel Maynez-Rojas and Jaqueline Cañetas

Minerals 2021, 11(5), 508; https://doi.org/10.3390/min11050508 - 11 May 2021

Cited by 4 | Viewed by 3282

Abstract

Techinantitla building complex, in the Amanalco neighborhood of the ancient city of Teotihuacan, is famous for the iconography and quality of the mural paintings found in this site. A significant part of this heritage has been lost due to looting. In recent years, an interdisciplinary research project was developed to study the limited patrimony that was left. As part of this study, we first employed geophysical techniques to reconstruct the architectural pattern of the compound’s remaining walls, where other paintings may still be found. Then, we applied a non-invasive methodology to characterize a large set of fragments recovered in the 1980s and to gain information on their pigments and manufacturing techniques. This methodology included False Color Infrared Imaging, X-ray Fluorescence and Fiber-Optics Reflectance Spectroscopy, and led to the identification of hematite, calcite, malachite, azurite and an unidentified blue pigment. The results were compared with a previous study performed on a set of Techinantitla mural paintings looted in the 1960s. A broader comparison with contemporary mural paintings from other Teotihuacan complexes shows good agreement in the materials used. These results may suggest a standardization in the making of Teotihuacan mural painting during the Xolapan period (350 to 550 AD). Full article

(This article belongs to the Special Issue Mineral Pigments in the Historical and Archaeological Context: from Invasive to Non-invasive Analyses)

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34 pages, 3379 KiB

Open AccessArticle

Invasive and Non-Invasive Analyses of Ochre and Iron-Based Pigment Raw Materials: A Methodological Perspective

by Laure Dayet

Minerals 2021, 11(2), 210; https://doi.org/10.3390/min11020210 - 17 Feb 2021

Cited by 17 | Viewed by 5229

Abstract

Naturally occurring and deeply coloured iron-bearing materials were exploited very early on by human populations. The characterization of these materials has proven useful for addressing several archaeological issues, such as the study of technical behaviors, group mobility, and the reconstruction of cultural dynamics. However, this work poses some critical methodological questions. In this paper, we will review ochre studies by focusing on the analytical methods employed, the limits of non-invasive methods, as well as examples of some quality research addressing specific issues (raw material selection and provenience, heat treatment). We will then present a methodological approach that aims to identify the instrumental limits and the post-depositional alterations that significantly impact the results of the non-invasive analysis of cohesive ochre fragments from Diepkloof rock Shelter, South Africa. We used ochre materials recuperated in both archaeological and geological contexts, and we compared non-invasive surface analyses by XRD, scanning electron microscopy coupled with dispersive X-ray spectrometry (SEM-EDXS), and particle-induced X-ray emission (PIXE) with invasive analysis of powder pellets and sections from the same samples. We conclude that non-invasive SEM-EDXS and PIXE analyses provide non-representative results when the number of measurements is too low and that post-depositional alterations cause significant changes in the mineralogical and major element composition at the surface of archaeological pieces. Such biases, now identified, must be taken into account in future studies in order to propose a rigorous framework for developing archaeological inferences. Full article

(This article belongs to the Special Issue Mineral Pigments in the Historical and Archaeological Context: from Invasive to Non-invasive Analyses)

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30 pages, 66849 KiB

Open AccessArticle

Ochre-Based Pigments in the Tablinum of the House of the Bicentenary (Herculaneum, Italy) between Decorative Technology and Natural Disasters

by Michele Secco, Leslie Rainer, Kiernan Graves, Arlen Heginbotham, Gilberto Artioli, Francesca Piqué and Ivana Angelini

Minerals 2021, 11(1), 67; https://doi.org/10.3390/min11010067 - 11 Jan 2021

Cited by 9 | Viewed by 3831

Abstract

Ochre-based pigments have been employed since the first artistic expressions of mankind, with widespread diffusion during the Roman civilization. Such prominent use influenced their technological development, focused on functional and aesthetic optimization through complex manufacturing procedures. Furthermore, their appearance is also influenced by degradation processes, sometimes driven by natural disasters such as the eruption of Mount Vesuvius in 79 AD, in which yellow ochres of Vesuvian sites were sometimes converted to red by thermal alteration. In this contribution, a multi-analytical approach was adopted based on preliminary non-invasive investigations complemented by laboratory analyses to characterize the painted surfaces of the tablinum of the House of the Bicentenary (Herculaneum) with a particular focus on the ochre-based monochrome backgrounds. The study was aimed at (a) reconstructing the original color scheme of the walls and (b) deciphering the complex decorative techniques adopted by Roman craftsmen. The analytical results allowed testing and defining analytical procedures for the discrimination between the original and converted red pigments. Furthermore, these studies indicated that specific decorative technologies were adopted according to aesthetic, functional, and economic purposes, including the utilization of various qualities of ochre with different compositional and textural properties, and the mixture of ochre pigments with other compounds. Full article

(This article belongs to the Special Issue Mineral Pigments in the Historical and Archaeological Context: from Invasive to Non-invasive Analyses)

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13 pages, 6674 KiB

Open AccessArticle

Sulfur Isotope Analysis to Examine the Provenance of Cinnabar Used in Wall Paintings in the Roman domus Avinyó (Barcelona)

by Evanthia Tsantini, Takeshi Minami, Miguel Ángel Cau Ontiveros, Kazuya Takahashi and Joan Carles Melgarejo

Minerals 2021, 11(1), 6; https://doi.org/10.3390/min11010006 - 23 Dec 2020

Cited by 4 | Viewed by 3170

Abstract

Wall paintings in the Roman period were used to decorate both public and private spaces; therefore, they reflect, on the one hand, ideas and convictions, and on the other, daily activities and socio-economic models. Characterizations of the pigments used in mural paintings are useful for determining the economic status of a specific settlement or the importance of a particular area or the buildings within it, since the cost of different pigments varied widely. Isotope analysis can be used to identify the provenance of pigments and to establish whether the raw materials are local, regional, or imported. This provides very important information, as it might be related to both the quality and the cost of the pigments, which, in turn, might be indicators of the socio-economic status of the area in question. The present study examines the sulfur isotope ratios of the cinnabar used in Roman wall paintings sampled from the high-status Roman Domus of Casa d’Avinyó and compares them with the ratios of the analyzed geological ores sampled at various Spanish cinnabar/mercury mines. The results exclude the possibility of the cinnabar being imported from outside the Iberian Peninsula. An isotopic analysis also suggested a few possible sources for the pigments. Full article

(This article belongs to the Special Issue Mineral Pigments in the Historical and Archaeological Context: from Invasive to Non-invasive Analyses)

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14 pages, 6018 KiB

Open AccessArticle

The Irreplaceable Contribution of Cross Sections Investigation: Painted Plasters from the Sphinx Room (Domus Aurea, Rome)

by Alessia Coccato, Maria Cristina Caggiani, Roberta Occhipinti, Paolo Mazzoleni, Alessandro D’Alessio, Alfonsina Russo and Germana Barone

Minerals 2021, 11(1), 4; https://doi.org/10.3390/min11010004 - 22 Dec 2020

Cited by 4 | Viewed by 2749

Abstract

Fragments and micro-fragments of painted plasters from the Sphinx Room, recently discovered in the Domus Aurea Esquiline wing (Rome, Italy), were studied. They were respectively taken from the debris in the vicinity of the walls and from already damaged edges of the decorated walls. A previous study, mainly based on non-destructive and non-invasive investigations, proved effective in giving a general overview of the employed palette, allowing the comparison with paintings from the same palace and other coeval contexts, and also providing some preliminary hints concerning the pictorial technique. Nevertheless, some issues remained unsolved, concerning the pigment mixtures (e.g., lead-/iron-based yellow to red colors; copper-/iron-based green/greyish areas), and the a fresco/a secco painting technique debate. Therefore, cross sections of the above-mentioned fragments were observed by means of Optical (OM) and Scanning Electron (SEM) Microscopy and analyzed with micro-Raman spectroscopy and Energy Dispersive X-Ray Spectroscopy (EDS), with the aims of: studying the paint layer composition through point analysis and mapping of the elemental distribution; comparing these in relation to what was observed with previously reported non-destructive analyses; studying the stratigraphy of the painted plaster, focusing on the contact between the plaster and the paint. Full article

(This article belongs to the Special Issue Mineral Pigments in the Historical and Archaeological Context: from Invasive to Non-invasive Analyses)

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31 pages, 23685 KiB

Open AccessArticle

Egyptian Blue Pellets from the First Century BCE Workshop of Kos (Greece): Microanalytical Investigation by Optical Microscopy, Scanning Electron Microscopy-X-ray Energy Dispersive Spectroscopy and Micro-Raman Spectroscopy

by Ariadne Kostomitsopoulou Marketou, Fabrizio Andriulo, Calin Steindal and Søren Handberg

Minerals 2020, 10(12), 1063; https://doi.org/10.3390/min10121063 - 27 Nov 2020

Cited by 19 | Viewed by 5390

Abstract

This paper aims to expand our understanding of the processes involved in the production of the artificial pigment Egyptian blue through the scientific examination of pigments found in the first century BCE workshop of the Greek island of Kos. There, 136 Egyptian blue pellets were brought to light, including successfully produced pellets, as well as partially successful and unsuccessful products. This study is based on the examination of eighteen samples obtained from pellets of various textures and tones of blue, including light and dark blue pigments, coarse and fine-grained materials, and one unsuccessful pellet of dark green/grey colour. The samples were examined by optical microscopy, scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDS), and micro-Raman spectroscopy. These complementary microanalytical techniques provide localised information about the chemical and mineralogical composition of this multicomponent material, at a single-grain level. The results shed light on the firing procedure and indicate possible sources for raw materials (beach sand, copper alloys), as well as demonstrating the use of a low-alkali starting mixture. Moreover, two different process for the production of light blue pigments were identified: (a) decreased firing time and (b) grinding of the initially produced pellet and mixing with cobalt-containing material. Full article

(This article belongs to the Special Issue Mineral Pigments in the Historical and Archaeological Context: from Invasive to Non-invasive Analyses)

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18 pages, 6158 KiB

Open AccessArticle

Vitreous Tesserae from the Four Seasons Mosaic of the S. Aloe Quarter in Vibo Valentia–Calabria, Italy: A Chemical Characterization

by Elia Fiorenza, Natalia Rovella, Maria D’Andrea, Marianna Musella, Fabrizio Sudano, Armando Taliano Grasso and Donatella Barca

Minerals 2020, 10(8), 658; https://doi.org/10.3390/min10080658 - 25 Jul 2020

Cited by 3 | Viewed by 2505

Abstract

This work reports the results of the archaeometrical investigation performed on twenty glass tesserae collected in 2018, during the restoration of the Four Seasons mosaic, which dates between the second and the third century AD, in the archaeological area of the S. Aloe quarter in Vibo Valentia (Calabria, Italy). The coloured glass tesserae were analysed through a micro-analytical approach using an Electron Probe Micro Analyser with Wavelength-Dispersive Spectroscopy (EPMA-WDS) and Laser Ablation with Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS). The aims of the study were (1) the determination of the chemical composition and the technology of glass mosaic tesserae production; (2) the individuation of colouring and opacifying agents used for the production of the glass tesserae. The glasses show the typical soda–lime–silica composition. EPMA-WDS results prove the use of Sn–Pb antimonates to create yellow glass, and of cuprite to obtain the red colour. Copper and cobalt were employed in both green and blue glasses to produce different shades of colour (grey, tints of green, dark and light blue). Full article

(This article belongs to the Special Issue Mineral Pigments in the Historical and Archaeological Context: from Invasive to Non-invasive Analyses)

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