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Minerals
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Historical Mineral Pigments
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Historical Mineral Pigments

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 (10 August 2020) | Viewed by 24839

Special Issue Editors

Prof. Dr. Carolina Cardell

E-Mail Website1 Website2
Guest Editor
Department of Mineralogy and Petrology, University of Granada, Granada, Spain
Interests: heritage science; archeometry; physical–chemical characterization of historical pigments; pigment–binder interactions; pigment degradation due to urban and marine air pollution; scanning electron microscopy–energy dispersive X-ray (SEM–EDX); Raman microscopy (RM); hyphenated SEM–EDX–RM; X-ray diffraction; nanominerals; chemometric analyses
Dr. Santiago Pozo-Antonio

E-Mail Website
Co-Guest Editor
Department of Natural Resources Engineering and Environment, University of Vigo, 36310 Vigo, Spain
Interests: cultural heritage; cleaning; consolidation; water-repelling; tempera paints; non-invasive techniques
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

In recent decades, a great body of scientific articles has emerged in specialized literature addressing the chemical–mineralogical composition, and morphological and physical characterization of natural and (premodern) synthetic historical mineral pigments. These include metallic pigments and clay-based pigments, embedded in artistic paintings, glass, painted enamel, ceramics, textiles, beads, etc. Often, these studies are performed by interdisciplinary research teams with crucial contributions by experts from the areas of mineralogy, crystallography, and geochemistry to correctly address questions arising with regard to pigment source, pigment manufacturing process, interactions between pigments, and weathering mechanisms or lightfastness, among other inquiries, since formation and transformation of mineral phases are processes involved in the research. Such investigations will provide essential clues to unravel pigment technological achievements, dating, trade routes, or pigment fingerprints for author/region adscriptions, as well as offering information to optimize conservation and/or restoration strategies of painted or colored artworks.

However, more light needs to be shed on specific issues. Particularly in historic paintings, in-depth studies are required to focus on pigment–(organic) binder interaction under diverse exposure scenarios; (urban and marine) air pollution-induced weathering; mitigation protocols so as to retard the photodegradation of pigments contained in paintings; biodeterioration due to microorganisms or insect debris, as well as the impact of airborne organic particles; pigment susceptibility to weathering considering its morphology, associated impurities, and particle size, with special attention to the presence of nanoparticles; detailed characterization of carbon-, clay- and earth-pigments; radiation damage during analysis; effects of surface cleaning and protection treatments; and application of novel analytical methodologies based on hyphenated techniques that offer remarkable advantages in the analysis of complex paintings (hybrid composite materials). All of these topics are welcome to be tackled in this Special Issue.

Prof. Dr. Carolina Cardell
Dr. Jose Santiago Pozo-Antonio
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

  • heritage science
  • mineral pigments
  • characterization
  • physical–chemical degradation
  • biodeterioration
  • protection treatments
  • hyphenated analytical techniques
  • chemometrics

Related Special Issue

Published Papers (7 papers)

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Editorial

Jump to: Research, Review

4 pages, 179 KiB  
Editorial
Editorial for Special Issue “Historical Mineral Pigments”
by Carolina Cardell and Jose Santiago Pozo-Antonio
Minerals 2021, 11(3), 237; https://doi.org/10.3390/min11030237 - 25 Feb 2021
Viewed by 1307
Abstract
The physical–chemical characterization of natural and synthetic historical inorganic and mineral pigments, which may be found embedded in paintings (real or mock-ups), glass, enamel, ceramics, beads, tesserae, etc [...] Full article
(This article belongs to the Special Issue Historical Mineral Pigments)

Research

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17 pages, 4759 KiB  
Article
Monte Carlo SEM-EDS Nano-Microanalysis Strategy of Historical Mineral Pigments: The Simulation of the Egyptian Blue from Pompeii (Italy) as an Example
by Domingo Martín, Daniele Moro, Gianfranco Ulian and Giovanni Valdrè
Minerals 2020, 10(9), 807; https://doi.org/10.3390/min10090807 - 13 Sep 2020
Cited by 3 | Viewed by 2899
Abstract
A correct determination of the mineral and chemical composition of specimens is of the utmost importance to answer questions regarding the Cultural Heritage field. Because of the preciousness and often very low quantity of sample available, with textures and sizes in the nano-to-micrometric [...] Read more.
A correct determination of the mineral and chemical composition of specimens is of the utmost importance to answer questions regarding the Cultural Heritage field. Because of the preciousness and often very low quantity of sample available, with textures and sizes in the nano-to-micrometric range, scanning electron microscopy (SEM) combined with energy-dispersive X-ray spectroscopy (EDS) is one of the most suited and exploited nano-microanalytical techniques. In these cases, to avoid severe mistakes and quantification errors in SEM-EDS, it is mandatory to consider several effects related to the transport of electrons and X-rays in the material, which in turn are dependent on the SEM-EDS setup. In the present work, a Monte Carlo SEM-EDS nano-microanalytical simulation strategy is proposed and applied to a practical selected case. The Egyptian blue mineral pigment, which is found in Pompeian murals, is used here as an example and model system to show the effects of real size variations (0.1–10 µm), basic geometrical shapes of the pigment (prismatic and spherical) and typical SEM setups, sample holders and substrates. The simulations showed a great—sometimes not intuitive—dependence of the X-ray intensity on the thickness and shape of the samples and SEM-EDS parameters, thereby influencing the analysis and quantification. The critical overview of the results allowed the determination of the correct procedure and technical SEM-EDS parameters and indicated how to apply the Monte Carlo simulation strategy to other Cultural Heritage cases. Full article
(This article belongs to the Special Issue Historical Mineral Pigments)
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19 pages, 1698 KiB  
Article
Use of Temperature Controlled Stage Confocal Raman Microscopy to Study Phase Transition of Lead Dioxide (Plattnerite)
by Ilaria Costantini, Pier Paolo Lottici, Kepa Castro and Juan Manuel Madariaga
Minerals 2020, 10(5), 468; https://doi.org/10.3390/min10050468 - 21 May 2020
Cited by 10 | Viewed by 3873
Abstract
The present work concerns the study of the phase transition of plattnerite [β-PbO2 lead (IV) oxide]-based samples when they are analysed by Raman spectroscopy. The laser-induced degradation process was carried out either on historical painting samples, where plattnerite was present as a [...] Read more.
The present work concerns the study of the phase transition of plattnerite [β-PbO2 lead (IV) oxide]-based samples when they are analysed by Raman spectroscopy. The laser-induced degradation process was carried out either on historical painting samples, where plattnerite was present as a degradation product of lead-based pigments, or commercial plattnerite samples as powder and pellets. The Raman spectra of plattnerite taken at low excitation power, to avoid phase transformations, are reported up to low wavenumbers, and they were characterized by the features at 159, 380, 515 and 653 cm−1 and a shoulder at 540 cm−1. The degradation of plattnerite was induced by increasing the laser power on the sample, and the formation of its secondary products red lead (Pb3O4), litharge (α-PbO) and massicot (β-PbO), when varying the laser power, is discussed. The analyses were performed in a controlled condition by coupling the Raman spectrometer to a temperature-controlled stage (Linkam THMS600- Renishaw), which allows for varying the sample temperature (from room temperature up to 600 °C) and keeping it constant inside the stage during the analysis. In this way, commercial plattnerite samples were heated by increasing the cell temperature to verify the temperature range at which the phase transitions of lead dioxide occur. In addition, thanks to the construction of temperature ramps, all the degradation pathways were shown, and other lead compounds were identified, generated by the laser power contribution. A different behaviour was found between pigments from historical painting samples and commercial samples under the effect of the laser. This information could be useful in order to recognize their nature when they are found in cultural heritage materials. Full article
(This article belongs to the Special Issue Historical Mineral Pigments)
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24 pages, 3881 KiB  
Article
Effect of a SO2 Rich Atmosphere on Tempera Paint Mock-Ups. Part 1: Accelerated Aging of Smalt and Lapis Lazuli-Based Paints
by José Santiago Pozo-Antonio, Teresa Rivas, Amelia Dionísio, Diana Barral and Carolina Cardell
Minerals 2020, 10(5), 427; https://doi.org/10.3390/min10050427 - 10 May 2020
Cited by 8 | Viewed by 3343
Abstract
The behavior of historic tempera paints exposed to pollutant gases is an important issue when developing conservation strategies. In this work, binary tempera paint mock-ups that were made with either smalt or lapis lazuli pigments mixed with either rabbit glue or egg yolk [...] Read more.
The behavior of historic tempera paints exposed to pollutant gases is an important issue when developing conservation strategies. In this work, binary tempera paint mock-ups that were made with either smalt or lapis lazuli pigments mixed with either rabbit glue or egg yolk binders were exposed to an SO2 accelerated aging test in order to find out more about the forms and mechanisms of alteration resulting from pigment-binder interaction. To this end, spectrophotometry, hyperspectral image analysis, and profilometry were used to study macro-scale, physical changes taking place on the surface of the paints, affecting color, gloss, reflectance, and roughness. Likewise, chemical and mineralogical changes were evaluated by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (ATR-FTIR), polarized light microscopy (PLM), and scanning electron microscopy with micro-analysis (SEM-EDS), which was also used to visualize micro-texture changes in the paints. The smalt-based tempera showed a higher degree of deterioration than the lapis lazuli-based tempera, in particular a notable whitening related to the precipitation of sulfate-rich salts and to binder and pigment chemical alterations. Moreover, whereas aged egg yolk-based paints showed visible color change due to damage to the oily binder and the pigments, the most evident change in rabbit glue-based paints was binder loss. The alteration suffered by the pigments varied in line with their composition; thus, smalt (blue cobalt-containing glass) grains were more sensitive to SO2 exposure than lapis lazuli-(Na,Ca)8[(S,Cl,SO4,OH)2|(Al6Si6O24)]-crystals. In the smalt grains, the SO2 test caused K+ leaching from the glass matrix, which was detected by means of K/Co ratios, but the lazurite crystals (main component of lapis lazuli) were unaffected (regardless of the binder used in the tempera). The most likely source of the crystallized sulfate rich salts were the impurities that were detected in association with the natural lapis lazuli pigment, i.e., calcite and diopside. Indeed, the precipitation of efflorescences is the main cause of the optical changes found in the smalt- and lapis lazuli-based tempera, in addition to the physical-chemical damage to the binders. The information reported here would be useful for preventive conservation, as well as for art restorers, who are planning work on paintings in which paints of this kind were used. Full article
(This article belongs to the Special Issue Historical Mineral Pigments)
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24 pages, 7699 KiB  
Article
Effect of a SO2 Rich Atmosphere on Tempera Paint Mock-Ups. Part 2: Accelerated Aging of Azurite- and Malachite-Based Paints
by Jose Santiago Pozo-Antonio, Carolina Cardell, Diana Barral, Amelia Dionisio and Teresa Rivas
Minerals 2020, 10(5), 424; https://doi.org/10.3390/min10050424 - 10 May 2020
Cited by 4 | Viewed by 2434
Abstract
In order to improve our knowledge of the weathering response of tempera paints exposed to an industrial atmosphere, azurite- and malachite-based paint mock-ups prepared with either rabbit glue or egg yolk binders were artificially aged in an SO2 rich atmosphere. The aim [...] Read more.
In order to improve our knowledge of the weathering response of tempera paints exposed to an industrial atmosphere, azurite- and malachite-based paint mock-ups prepared with either rabbit glue or egg yolk binders were artificially aged in an SO2 rich atmosphere. The aim was to identify the different alteration mechanisms and forms of degradation in the paints by observing their physical (color, gloss, reflectance, and roughness), mineralogical, chemical, and micro-textural characteristics. Superficial physical changes were evaluated by stereomicroscopy, spectrophotometry, gloss measurement, hyperspectral imaging, and roughness measurements. Chemical and mineralogical changes were evaluated by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy with microanalysis (SEM-EDS), which was also used to evaluate the micro-texture of the paints. The differences between the fresh temperas were due mainly to the binder (egg yolk or rabbit glue) used in the paint mixture, which also played a crucial role in the different deterioration patterns in the artificially aged paint mock-ups. Thus, the egg yolk-based paints remained physically quite intact after SO2 exposure, although they suffered more significant chemical degradation, above all in the form of copious precipitation of Cu and Ca-rich sulfate salts and the subsequent yellowing of the egg yolk binder. The SO2 aged rabbit glue-based mock-ups showed microscopically important crack formation and binder loss and fewer sulfated salts precipitated on the surface of the paints. Full article
(This article belongs to the Special Issue Historical Mineral Pigments)
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21 pages, 4289 KiB  
Article
The Color Palette of the Mosaics in the Roman Villa of Noheda (Spain)
by Nadine Schibille, Cristina Boschetti, Miguel Ángel Valero Tévar, Emmanuel Veron and Jorge de Juan Ares
Minerals 2020, 10(3), 272; https://doi.org/10.3390/min10030272 - 18 Mar 2020
Cited by 18 | Viewed by 6025
Abstract
Excavations at the Roman villa of Noheda (Spain) revealed the remains of an exceptionally elaborate fourth-century floor mosaic that contains a surprisingly large number of glass tesserae, representing a broad spectrum of colors. This paper presents the results of the chemical (LA-ICP-MS) and [...] Read more.
Excavations at the Roman villa of Noheda (Spain) revealed the remains of an exceptionally elaborate fourth-century floor mosaic that contains a surprisingly large number of glass tesserae, representing a broad spectrum of colors. This paper presents the results of the chemical (LA-ICP-MS) and microstructural analyses (SEM-EDS, XRPD) of 420 glass tesserae from these mosaics. The high number of data allowed us to establish the compositional variability and to elucidate questions of supply in relation to a large-scale artistic campaign. The tesserae from Noheda were almost exclusively made from recycled mixed Roman Mn and Sb base glass, thus demonstrating that recycling of Roman base glasses was common practice in the fourth century, occurring on a near industrial scale. It also suggests that the workshops specializing in the production of mosaic tesserae might have been in the western Mediterranean. A limited number of coloring and opacifying additives (Mn, Co, Cu, Sb, Pb) were identified, which resulted in a wide range of hues. These were differentially associated with various trace elements, which implies the use of different raw materials. A sub-set of red, green, and orange tesserae reflect distinct base glass characteristics as well as coloring technologies that point to an Egyptian provenance. Full article
(This article belongs to the Special Issue Historical Mineral Pigments)
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Review

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21 pages, 5531 KiB  
Review
Clay Minerals in European Painting of the Mediaeval and Baroque Periods
by David Hradil, Janka Hradilová and Petr Bezdička
Minerals 2020, 10(3), 255; https://doi.org/10.3390/min10030255 - 11 Mar 2020
Cited by 12 | Viewed by 3955
Abstract
Clay-based pigments are among the most traditional. Unlike other mineral pigments, they have never been fully replaced by synthetic analogues and are still used in painting today. Since their analysis requires a specific approach, detailed distinction of clay pigments has never been a [...] Read more.
Clay-based pigments are among the most traditional. Unlike other mineral pigments, they have never been fully replaced by synthetic analogues and are still used in painting today. Since their analysis requires a specific approach, detailed distinction of clay pigments has never been a part of routine chemical-technological research in fine arts—regardless of a great potential of clay minerals for determining regional provenance of the material. This review article maps and summarizes research on clay pigments in historical paintings that has been systematically pursued by authors since the beginning of this millennium. This rallying and interconnection of knowledge was an opportunity for a new reflection on the common aspects of these research projects, either methodological or interdisciplinary, since these findings are closely related to art-historical evaluation of artworks. It offers a comprehensive insight into the microanalysis of clay pigments with using powder X-ray micro-diffraction and complementary methods. Significant new findings come, for example, from research on the Italian Baroque. It becomes clear that cheap availability of raw material, pottery clays, could have played an important role in the change in painting technology at the turn of the 16th and 17th centuries. Full article
(This article belongs to the Special Issue Historical Mineral Pigments)
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