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Advances in Analytical Strategies to Study Cultural Heritage Samples
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Advances in Analytical Strategies to Study Cultural Heritage Samples

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (30 April 2023) | Viewed by 41384

Printed Edition Available!
A printed edition of this Special Issue is available here.

Special Issue Editors

Dr. Maria Luisa Astolfi

E-Mail Website
Guest Editor
Department of Chemistry, Sapienza University of Rome, Rome, Italy
Interests: analytical and bioanalytical chemistry; environmental chemistry and monitoring; elemental analysis; atomic spectroscopic techniques (ICP-MS, ICP-OES, CV-AFS, AMA, GF-AAS); sample treatment; determination of trace elements in foods
Special Issues, Collections and Topics in MDPI journals
Dr. Maria Pia Sammartino

E-Mail Website
Co-Guest Editor
Department of Chemistry, Sapienza University of Rome, Rome, Italy
Interests: stones; metals; painting; modelling of degradation; microclimate; sensors; biosensors; organic phase enzime electrodes
Special Issues, Collections and Topics in MDPI journals
Dr. Emanuele Dell'Aglio

E-Mail Website
Co-Guest Editor
Department of Chemistry, Sapienza University of Rome, Rome, Italy
Interests: conservation and restoration of cultural heritage; green chemistry; analytical chemistry; stone materials; colorimetry

Special Issue Information

Dear Colleagues,

This Special Issue highlights the most recent advancements and trends in cultural heritage samples' analysis, including archeological and bio-archeological samples.

Cultural heritage samples are complex matrices that are made up of many chemical species of natural origin or due to transformation by humans or the environment. Analytical chemistry in the recent past also required samples of excessive size, and its methods were not sufficiently sensitive. Today, on the other hand, it is possible to optimize analytical methods that are capable of analyzing ever-smaller samples and analytes at ever-lower concentrations. The chemical investigation can help to ascertain the processing techniques and the destinations and uses of archaeological objects, including all human interests and activities (food, art, worship, ornament, use herbal medicines, or drug remedies). Furthermore, the study of organic remains from archaeological sites addresses questions about evolution, past human activities, subsistence, health, medical and care practices, nutrition, and how humans have interacted with or modified their natural environments. In addition, knowledge of the materials used in works of art allows for implementing preventive measures for their optimal conservation and protection. Finally, the analysis of the materials and microelements in the cultural heritage samples can make it possible to establish the geographical origin and authenticity of the find. We invite our colleagues to submit their original contributions as research articles, review articles, as well as short communications, to this Special Issue in order to provide recent updates regarding analytical strategies for all of the above-mentioned aspects.

Dr. Maria Luisa Astolfi
Guest Editor

Dr. Maria Pia Sammartino  
Dr. Emanuele Dell'Aglio
Co-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. Molecules is an international peer-reviewed open access semimonthly 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 2700 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

  • Sample preparation
  • Toxic metals
  • Trace elements
  • Multi-element analysis
  • Spectrometric techniques
  • Organic compounds
  • Authenticity
  • Chemical fingerprinting
  • Biological remains
  • Pigments

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Published Papers (20 papers)

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Editorial

Jump to: Research, Review

5 pages, 199 KiB  
Editorial
Advances in Analytical Strategies to Study Cultural Heritage Samples
by Maria Luisa Astolfi
Molecules 2023, 28(17), 6423; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28176423 - 04 Sep 2023
Viewed by 755
Abstract
The advancements of civilization are based on our ability to pass on the events and knowledge of the past so that the next generations can start from an ever-higher level of expertise [...] Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)

Research

Jump to: Editorial, Review

17 pages, 4457 KiB  
Article
Study of Micro-Samples from the Open-Air Rock Art Site of Cueva de la Vieja (Alpera, Albacete, Spain) for Assessing the Performance of a Desalination Treatment
by Ilaria Costantini, Julene Aramendia, Nagore Prieto-Taboada, Gorka Arana, Juan Manuel Madariaga and Juan Francisco Ruiz
Molecules 2023, 28(15), 5854; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28155854 - 03 Aug 2023
Cited by 1 | Viewed by 846
Abstract
In this work, some micro-samples belonging to the open-air rock art site of Cueva de la Vieja (Alpera, Albacete, Spain) were analysed. These samples were collected after and before a desalination treatment was carried out, with the aim of removing a whitish layer [...] Read more.
In this work, some micro-samples belonging to the open-air rock art site of Cueva de la Vieja (Alpera, Albacete, Spain) were analysed. These samples were collected after and before a desalination treatment was carried out, with the aim of removing a whitish layer of concretion that affected the painted panel. The diagnostic study was performed to study the conservation state of the panel, and to then confirm the effectiveness of the treatment. Micro energy dispersive X-ray fluorescence spectrometry, Raman spectroscopy, and X-ray diffraction were employed for the characterization of the degradation product as well as that of the mineral substrate and pigments. The micro-samples analysis demonstrated that the painted layer was settled on a dolomitic limestone with silicon aggregates and aluminosilicates as well as iron oxides. The whitish crust was composed by sulfate compounds such as gypsum (CaSO4·2H2O) with a minor amount of epsomite (MgSO4·7H2O). An extensive phenomenon of biological activity has been demonstrated since then in almost all of the samples that have been analysed, and the presence of calcium oxalates monohydrate (CaC2O4·H2O) and dehydrate (CaC2O4·2H2O) were found. The presence of both calcium oxalates probably favoured the conservation of the pictographs. In addition, some carotenoids pigments, scytonemin (C36H20N2O4), and astaxanthin (C40H52O4) were characterized both by Raman spectroscopy and by X-ray diffraction. Hematite was found as a pigment voluntarily used for the painting of the panels used in a mixture with hydroxyapatite and amorphous carbon. The results of the analyses of the samples taken after the cleaning treatment confirmed a substantial decrease in sulphate formation on the panel surface. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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21 pages, 2781 KiB  
Article
Inside the History of Italian Coloring Industries: An Investigation of ACNA Dyes through a Novel Analytical Protocol for Synthetic Dye Extraction and Characterization
by Ilaria Serafini, Kathryn Raeburn McClure, Alessandro Ciccola, Flaminia Vincenti, Adele Bosi, Greta Peruzzi, Camilla Montesano, Manuel Sergi, Gabriele Favero and Roberta Curini
Molecules 2023, 28(14), 5331; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28145331 - 11 Jul 2023
Cited by 3 | Viewed by 951
Abstract
The introduction of synthetic dyes completely changed the industrial production and use of colorants for art materials. From the synthesis of the first synthetic dye, mauveine, in 1856 until today, artists have enjoyed a wider range of colors and selection of chemical properties [...] Read more.
The introduction of synthetic dyes completely changed the industrial production and use of colorants for art materials. From the synthesis of the first synthetic dye, mauveine, in 1856 until today, artists have enjoyed a wider range of colors and selection of chemical properties than was ever available before. However, the introduction of synthetic dyes introduced a wider variety and increased the complexity of the chemical structures of marketed dyes. This work looks towards the analysis of synthetically dyed objects in heritage collections, applying an extraction protocol based on the use of ammonia, which is considered favorable for natural anthraquinone dyes but has never before been applied to acid synthetic dyes. This work also presents an innovative cleanup step based on the use of an ion pair dispersive liquid–liquid microextraction for the purification and preconcentration of historical synthetic dyes before analysis. This approach was adapted from food science analysis and is applied to synthetic dyes in heritage science for the first time in this paper. The results showed adequate recovery of analytes and allowed for the ammonia-based extraction method to be applied successfully to 15 samples of suspected azo dyes from the Azienda Coloranti Nazionali e Affini (ACNA) synthetic dye collection, identified through untargeted HPLC-HRMS analyses. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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16 pages, 6022 KiB  
Article
New Advances in Dye Analyses: In Situ Gel-Supported Liquid Extraction from Paint Layers and Textiles for SERS and HPLC-MS/MS Identification
by Adele Bosi, Greta Peruzzi, Alessandro Ciccola, Ilaria Serafini, Flaminia Vincenti, Camilla Montesano, Paolo Postorino, Manuel Sergi, Gabriele Favero and Roberta Curini
Molecules 2023, 28(14), 5290; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28145290 - 08 Jul 2023
Cited by 2 | Viewed by 1029
Abstract
To date, it is still not possible to obtain exhaustive information about organic materials in cultural heritage without sampling. Nonetheless, when studying unique objects with invaluable artistic or historical significance, preserving their integrity is a priority. In particular, organic dye identification is of [...] Read more.
To date, it is still not possible to obtain exhaustive information about organic materials in cultural heritage without sampling. Nonetheless, when studying unique objects with invaluable artistic or historical significance, preserving their integrity is a priority. In particular, organic dye identification is of significant interest for history and conservation research, but it is still hindered by analytes’ low concentration and poor fastness. In this work, a minimally invasive approach for dye identification is presented. The procedure is designed to accompany noninvasive analyses of inorganic substances for comprehensive studies of complex cultural heritage matrices, in compliance with their soundness. Liquid extraction of madder, turmeric, and indigo dyes was performed directly from paint layers and textiles. The extraction was supported by hydrogels, which themselves can undergo multitechnique analyses in the place of samples. After extraction, Ag colloid pastes were applied on the gels for SERS analyses, allowing for the identification of the three dyes. For the HPLC-MS/MS analyses, re-extraction of the dyes was followed by a clean-up step that was successfully applied on madder and turmeric. The colour change perceptivity after extraction was measured with colorimetry. The results showed ΔE values mostly below the upper limit of rigorous colour change, confirming the gentleness of the procedure. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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17 pages, 5263 KiB  
Article
Reflectance Spectroscopy as a Novel Tool for Thickness Measurements of Paint Layers
by Alice Dal Fovo, Marina Martínez-Weinbaum, Mohamed Oujja, Marta Castillejo and Raffaella Fontana
Molecules 2023, 28(12), 4683; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28124683 - 09 Jun 2023
Cited by 3 | Viewed by 1689
Abstract
A major challenge in heritage science is the non-invasive cross-sectional analysis of paintings. When low-energy probes are used, the presence of opaque media can significantly hinder the penetration of incident radiation, as well as the collection of the backscattered signal. Currently, no technique [...] Read more.
A major challenge in heritage science is the non-invasive cross-sectional analysis of paintings. When low-energy probes are used, the presence of opaque media can significantly hinder the penetration of incident radiation, as well as the collection of the backscattered signal. Currently, no technique is capable of uniquely and noninvasively measuring the micrometric thickness of heterogeneous materials, such as pictorial layers, for any painting material. The aim of this work was to explore the possibility of extracting stratigraphic information from reflectance spectra obtained by diffuse reflectance spectroscopy (DRS). We tested the proposed approach on single layers of ten pure acrylic paints. The chemical composition of each paint was first characterised by micro-Raman and laser-induced breakdown spectroscopies. The spectral behaviour was analysed by both Fibre Optics Reflectance Spectroscopy (FORS) and Vis-NIR multispectral reflectance imaging. We showed that there is a clear correlation between the spectral response of acrylic paint layers and their micrometric thickness, which was previously measured by Optical Coherence Tomography (OCT). Based on significant spectral features, exponential functions of reflectance vs. thickness were obtained for each paint, which can be used as calibration curves for thickness measurements. To the best of our knowledge, similar approaches for cross-sectional measurements of paint layers have never been tested. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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23 pages, 52214 KiB  
Article
Analytical Investigations of XIX–XX Century Paints: The Study of Two Vehicles from the Museum for Communications of Frankfurt
by Andrea Macchia, Lisa Maria Schuberthan, Daniela Ferro, Irene Angela Colasanti, Stefania Montorsi, Chiara Biribicchi, Francesca Irene Barbaccia and Mauro Francesco La Russa
Molecules 2023, 28(5), 2197; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28052197 - 27 Feb 2023
Cited by 2 | Viewed by 1320
Abstract
Over the centuries, humans have developed different systems to protect surfaces from the influence of environmental factors. Protective paints are the most used ones. They have undergone considerable development over the years, especially at the turn of the 19th and 20th centuries. Indeed, [...] Read more.
Over the centuries, humans have developed different systems to protect surfaces from the influence of environmental factors. Protective paints are the most used ones. They have undergone considerable development over the years, especially at the turn of the 19th and 20th centuries. Indeed, between the two centuries, new binders and pigments have been introduced in the constituent materials of paints. The years in which these compounds have been introduced and spread in the paint market allow them to be defined as markers for the dating of paints and painted artifacts. The present work is focused on the study of the paints of two vehicles of the Frankfurt Museum of Communication, i.e., a carriage and a cart, that was designed for the German Postal and Telecommunications Service roughly between 1880 and 1920. The characterization of the paints was performed through in situ non-invasive techniques, i.e., portable optical microscopy and multispectral imaging, and laboratory non-destructive techniques, i.e., FT-IR ATR spectroscopy and SEM-EDS. The analytical investigation and the comparison with the data reported in the literature allowed us to determine the historicity of the paints, which are all dated before the 1950s. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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16 pages, 4727 KiB  
Article
Analytical Investigation of Iron-Based Stains on Carbonate Stones: Rust Formation, Diffusion Mechanisms, and Speciation
by Rita Reale, Giovanni Battista Andreozzi, Maria Pia Sammartino and Anna Maria Salvi
Molecules 2023, 28(4), 1582; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28041582 - 07 Feb 2023
Cited by 3 | Viewed by 1266
Abstract
In cultural heritage, unaesthetic stains on carbonate stones due to their close contacts with metals are of concern for the preservation of sculptures, monumental facades and archeological finds of various origin and antiquities. Rust stains made up of various oxidized iron compounds are [...] Read more.
In cultural heritage, unaesthetic stains on carbonate stones due to their close contacts with metals are of concern for the preservation of sculptures, monumental facades and archeological finds of various origin and antiquities. Rust stains made up of various oxidized iron compounds are the most frequent forms of alteration. The presence of ferric iron on rust-stained marble surfaces was confirmed in previous studies and oriented the choice of the best cleaning method (based on complexing agents specific for ferric ions). However, the composition of rust stains may vary along their extension. As the corrosion of the metallic iron proceeds, if the oxygen levels in the surroundings are low and there are no conditions to favor the oxidation, ferrous ions can also diffuse within the carbonate structure and form a variety of intermediate compounds. In this study, the iron stains on archeological marbles were compared with those artificially produced on Carrara marbles and Travertine samples. The use of integrated techniques (optical and scanning electron microscopy as well as Mössbauer and XPS spectroscopy) with complementary analytical depths, has provided the overall information. Rust formation and diffusion mechanisms in carbonates were revealed together with the evolution of iron speciation and identification of phases such as ferrihydrite, goethite, maghemite, nanomagnetite, and hematite. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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14 pages, 7500 KiB  
Article
Microanalytical Characterization of an Innovative Modern Mural Painting Technique by SEM-EDS, NMR and Micro-ATR-FTIR among Others
by Pablo Aguilar-Rodríguez, Sandra Zetina, Adrián Mejía-González and Nuria Esturau-Escofet
Molecules 2023, 28(2), 564; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28020564 - 05 Jan 2023
Cited by 2 | Viewed by 1579
Abstract
During the 20th century, modern painters experimented with different mediums and painting techniques, one of them was Rafael Coronel in his mural painting, Paisaje Abstracto (Abstract landscape). The painting was created with a peculiar pouring technique and an unknown binding medium; [...] Read more.
During the 20th century, modern painters experimented with different mediums and painting techniques, one of them was Rafael Coronel in his mural painting, Paisaje Abstracto (Abstract landscape). The painting was created with a peculiar pouring technique and an unknown binding medium; ageing produced fractures and severe conservation problems. Therefore, the characterization of the painting medium became an urgent matter in order to understand the current condition of the painting and to develop a proper treatment. The aim of this research was to characterize the chemical composition and painting technique of Paisaje Abstracto. To approach this goal two microsamples were taken and analyzed by optical microscopy (OM), scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), nuclear magnetic resonance (NMR) spectroscopy, attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR), micro attenuated total reflection Fourier transform infrared spectroscopy (micro-ATR-FTIR) and gas chromatography/mass spectrometry (GC/MS). The analysis allowed for the identification of cadmium sulfide (CdS) and titanium dioxide (TiO2) as inorganic pigments; aluminosilicate fillers; poly(methyl methacrylate) (pMMA) as a binder; MMA monomer, red organic pigment PR181; benzoyl peroxide, dibutyl phthalate and 1-octadecanol as organic additives. This study presents an innovative painting technique with pMMA, a medium not commonly used by artists, which was probably polymerized onto the painting support. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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16 pages, 8860 KiB  
Article
The Bio-Patina on a Hypogeum Wall of the Matera-Sassi Rupestrian Church “San Pietro Barisano” before and after Treatment with Glycoalkaloids
by Francesco Cardellicchio, Sabino Aurelio Bufo, Stefania Mirela Mang, Ippolito Camele, Anna Maria Salvi and Laura Scrano
Molecules 2023, 28(1), 330; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28010330 - 31 Dec 2022
Cited by 2 | Viewed by 1160
Abstract
The investigation focused on the deterioration of the walls in the hypogeum of “San Pietro Barisano” rupestrian church, located in the Matera-Sassi (Southern Italy), one of the UNESCO World Heritage sites. The study evaluated the biocide activity of a mixture of natural glycoalkaloids [...] Read more.
The investigation focused on the deterioration of the walls in the hypogeum of “San Pietro Barisano” rupestrian church, located in the Matera-Sassi (Southern Italy), one of the UNESCO World Heritage sites. The study evaluated the biocide activity of a mixture of natural glycoalkaloids (GAs) extracted from the unripe fruit of Solanum nigrum and applied to clean a hypogeum wall surface in the church affected by bio-patinas. The analyzed bio-patina, collected before treatment and, at pre-established times, after treatment, showed changes in chemical composition detected by XPS, accompanied by visible discoloration and biological activity variation. The biocidal action of the glycoalkaloids mixture, directly employed on the wall surface, was effective after about four weeks for most bio-patina colonizers but not for the fungal species that can migrate and survive in the porosities of the calcarenite. Consequently, the cleaning procedure requires the integration of fungicidal actions, combined with the consolidation of the surfaces, to obtain complete bioremediation and avoid subsequent biological recolonization. SEM images and associated microanalysis of pretreated bio-patina have revealed the biocalcogenity of some autochthonous microorganisms, thus preluding to their eventual isolation and reintroduction on the wall surface to act as consolidants once the bio-cleaning phase has been completed. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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18 pages, 3885 KiB  
Article
Visual and Physical Degradation of the Black and White Mosaic of a Roman Domus under Palazzo Valentini in Rome: A Preliminary Study
by Claudia Colantonio, Paola Baldassarri, Pasquale Avino, Maria Luisa Astolfi and Giovanni Visco
Molecules 2022, 27(22), 7765; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27227765 - 11 Nov 2022
Cited by 2 | Viewed by 1280
Abstract
Palazzo Valentini, the institutional head office of Città Metropolitana di Roma Capitale, stands in in a crucial position in the Roman archaeological and urban contexts, exactly between the Fora valley, Quirinal Hill slopes, and Campus Martius. It stands on a second-century A.D. complex [...] Read more.
Palazzo Valentini, the institutional head office of Città Metropolitana di Roma Capitale, stands in in a crucial position in the Roman archaeological and urban contexts, exactly between the Fora valley, Quirinal Hill slopes, and Campus Martius. It stands on a second-century A.D. complex to which belong, between other archeological remains, two richly decorated aristocratic domus. One of these buildings, the domus A, presents an outward porticoed room with a fourth-century AD central impluvium (open air part of the atrium designed to carry away rainwater) with a black/white tiled mosaic pavement, the preservation status of which is compromised by an incoherent degradation product that has caused gradual detachment of the mosaic tiles. To identify the product and determine the causes of degradation, samples of the product were taken and subjected to SEM-EDS, XRF, NMR, FT-IR and GC-MS analyses. The findings reported in this study can help restorers, archaeologists and conservation scientists in order to improve knowledge about the Roman mosaic, its construction phases, conservation problems and proper solutions. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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12 pages, 1206 KiB  
Article
Non-Invasive Paleo-Metabolomics and Paleo-Proteomics Analyses Reveal the Complex Funerary Treatment of the Early 18th Dynasty Dignitary NEBIRI (QV30)
by Elettra Barberis, Marcello Manfredi, Enrico Ferraris, Raffaella Bianucci and Emilio Marengo
Molecules 2022, 27(21), 7208; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27217208 - 25 Oct 2022
Cited by 3 | Viewed by 1783
Abstract
Biochemical investigations were carried out on the embalmed head of Nebiri (Museo Egizio, Turin; S-5109)—an 18th Dynasty Ancient Egyptian dignitary—and on the canopic jar containing his lungs (Museo Egizio, Turin; S. 5111/02) with the aim of characterizing the organ’s (lung) specific paleo-proteins and [...] Read more.
Biochemical investigations were carried out on the embalmed head of Nebiri (Museo Egizio, Turin; S-5109)—an 18th Dynasty Ancient Egyptian dignitary—and on the canopic jar containing his lungs (Museo Egizio, Turin; S. 5111/02) with the aim of characterizing the organ’s (lung) specific paleo-proteins and of identifying the compounds used in his embalming “recipe”. The application of a functionalized film method allowed us to perform a non-invasive sampling. Paleo-proteomics confirmed the presence of lung tissue-specific proteins (organ specific) as well as the presence of proteins linked to severe inflammation. Paleoproteomics and paleometabolomics further allowed the identification of the main components of Nebiri’s embalming recipe: animal fats and glue, balms, essential oils, aromatic plants, heated Pistacia, and coniferous resins. Both the use of Pistacia and coniferous resins in an early 18th Dynasty individual confirm Nebiri’s high social status. The technique applied offers a targeted approach to the chemical characterization of human tissues, embalming compounds, and organic materials layering in pottery. The ability of the functionalized film method to harvest all types of compounds, from macromolecules (i.e., proteins) to small molecules (i.e., organic acids) opens a new path in the study of ancient material culture; furthermore, it allows to perform untargeted analysis, which is necessary when no a priori information is available. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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16 pages, 3074 KiB  
Article
Photons for Photography: A First Diagnostic Approach to Polaroid Emulsion Transfer on Paper in Paolo Gioli’s Artworks
by Zeynep Alp, Alessandro Ciccola, Ilaria Serafini, Alessandro Nucara, Paolo Postorino, Alessandra Gentili, Roberta Curini and Gabriele Favero
Molecules 2022, 27(20), 7023; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27207023 - 18 Oct 2022
Cited by 3 | Viewed by 1501
Abstract
The aim of this research is to study and diagnose for the first time the Polaroid emulsion transfer in the contemporary artist Paolo Gioli’s artworks to provide preliminary knowledge about the materials of his artworks and the appropriate protocols which can be applied [...] Read more.
The aim of this research is to study and diagnose for the first time the Polaroid emulsion transfer in the contemporary artist Paolo Gioli’s artworks to provide preliminary knowledge about the materials of his artworks and the appropriate protocols which can be applied for future studies. The spectral analysis performed followed a multi-technical approach first on the mock-up samples created following Gioli’s technique and on one original artwork of Gioli, composed by: FORS (Fiber Optics Reflectance), Raman, and FTIR (Fourier-Transform InfraRed) spectroscopies. These techniques were chosen according to their completely non-invasiveness and no requirement for sample collection. The obtained spectra from FTIR were not sufficient to assign the dyes found in the transferred Polaroid emulsion. However, they provided significant information about the cellulose-based materials. The most diagnostic results were obtained from FORS for the determination of the dye developers present in the mock-up sample which was obtained from Polacolor Type 88 and from Paolo Gioli’s original artwork created with Polacolor type 89. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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24 pages, 4998 KiB  
Article
The Use of UV-Visible Diffuse Reflectance Spectrophotometry for a Fast, Preliminary Authentication of Gemstones
by Maurizio Aceto, Elisa Calà, Federica Gulino, Francesca Gullo, Maria Labate, Angelo Agostino and Marcello Picollo
Molecules 2022, 27(15), 4716; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27154716 - 23 Jul 2022
Cited by 3 | Viewed by 2647
Abstract
The identification of gemstones is an important topic in the field of cultural heritage, given their enormous value. Particularly, the most important precious stones, namely diamond, emerald, ruby and sapphire, are frequently subjected to counterfeit by substitution with objects of lesser value with [...] Read more.
The identification of gemstones is an important topic in the field of cultural heritage, given their enormous value. Particularly, the most important precious stones, namely diamond, emerald, ruby and sapphire, are frequently subjected to counterfeit by substitution with objects of lesser value with similar appearance, colour or shape. While a gemmologist is able to recognise a counterfeit in most instances, more generally, it is not easy to do this without resorting to instrumental methods. In this work, the use of UV-visible diffuse reflectance spectrophotometry with optic fibres (FORS) is proposed as a fast and easy method for the preliminary identification of gemstones, alternative to the classical methods used by gemmologists or to Raman spectroscopy, which is by far the instrumental method with the best diagnostic potential, but it cannot be used in situations of problematic geometric hindrance. The possibilities and the limitations given by the FORS technique are critically discussed together with the spectral features of the most important gemstones. Finally, the application of chemometric pattern recognition methods is described for the treatment of large sets of spectral data deriving from gemstones identification. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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12 pages, 2589 KiB  
Article
A Silver Monochrome “Concetto spaziale” by Lucio Fontana: A Spectroscopic Non- and Micro-Invasive Investigation of Materials
by Margherita Longoni, Carlotta Beccaria, Letizia Bonizzoni and Silvia Bruni
Molecules 2022, 27(14), 4442; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27144442 - 11 Jul 2022
Cited by 1 | Viewed by 1255
Abstract
In several of his artworks, for instance the Venezie cycle, Fontana employed metallic paints; previous investigations on such materials highlighted the use of different synthetic binders and of thick paint layers below the metal one, having different colours to change the visual perception [...] Read more.
In several of his artworks, for instance the Venezie cycle, Fontana employed metallic paints; previous investigations on such materials highlighted the use of different synthetic binders and of thick paint layers below the metal one, having different colours to change the visual perception of the metallic surface. In the present work, a monochrome silver “Concetto spaziale” by the Italo–Argentine artist belonging to a private collection recently gifted to the museum of the Church of San Fedele in Milano, Italy, was investigated to deepen the knowledge of this particular group of Fontana’s paintings. The artwork was initially visually inspected in visible and ultraviolet (UV) light. Subsequently, a non-invasive spectroscopic investigation was performed by X-ray fluorescence (XRF), reflection Fourier-transform infrared (FTIR) and Raman spectroscopy. A minute fragment of silver-coloured paint was taken from the reverse of the painting, near the cut edge, and examined by scanning electron microscopy coupled with energy dispersive X-ray analysis (SEM-EDX) and micro-Fourier-transform Raman (FT-Raman) spectroscopy. The analytical data made it possible to identify the composition of the metallic paint layer and of the underlying dark one, both from the point of view of the pigments and of the binders used, also highlighting the potential of the non-invasive and micro-invasive methods adopted in the investigation. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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15 pages, 2932 KiB  
Article
Analytical Techniques Applied to the Study of Industrial Archaeology Heritage: The Case of Plaiko Zubixe Footbridge
by Ilaria Costantini, Kepa Castro, Juan Manuel Madariaga and Gorka Arana
Molecules 2022, 27(11), 3609; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27113609 - 04 Jun 2022
Cited by 2 | Viewed by 1322
Abstract
In this work, micro-Raman spectroscopy and micro-energy-dispersive X-ray fluorescence spectroscopy (µ-EDXRF) were applied on microsamples taken from the Plaiko Zubixe footbridge (1927) located in Ondarroa (Basque Country, Spain) in order to investigate the original paint coating and make an evaluation of the conservation [...] Read more.
In this work, micro-Raman spectroscopy and micro-energy-dispersive X-ray fluorescence spectroscopy (µ-EDXRF) were applied on microsamples taken from the Plaiko Zubixe footbridge (1927) located in Ondarroa (Basque Country, Spain) in order to investigate the original paint coating and make an evaluation of the conservation state before its restoration. Elemental and molecular images were acquired for the study of the compounds distribution. Some modern pigments such as phthalocyanine blue and green pigments, minium, calcium carbonate, Prussian blue, and hematite were identified. Barium sulfate and titanium dioxide were recognized as opacifier agents. Thanks to the study of the stratigraphies, it has been possible to determine the original paint layer, which includes lead white, ultramarine blue, carbon black, and barium sulfate. In addition, colorimetric analyses made it possible to know the CIELab values of the original layer in order to reproduce the original colour during the planned restoration work. The massive presence of chlorine detected by µ-EDXRF and the corrosion products of the rust layer, in particular akaganeite and hematite, highlighted the atmospheric impact in the conservation of the bridge because they were due to the effect of both marine aerosol and to the presence of acidic components in the environment coming from anthropogenic activity. This work demonstrated the usefulness of a scientific approach for the study of industrial archaeology heritage with the aim to contribute to its conservation and restoration. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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21 pages, 3804 KiB  
Article
The “Historical Materials BAG”: A New Facilitated Access to Synchrotron X-ray Diffraction Analyses for Cultural Heritage Materials at the European Synchrotron Radiation Facility
by Marine Cotte, Victor Gonzalez, Frederik Vanmeert, Letizia Monico, Catherine Dejoie, Manfred Burghammer, Loïc Huder, Wout de Nolf, Stuart Fisher, Ida Fazlic, Christelle Chauffeton, Gilles Wallez, Núria Jiménez, Francesc Albert-Tortosa, Nati Salvadó, Elena Possenti, Chiara Colombo, Marta Ghirardello, Daniela Comelli, Ermanno Avranovich Clerici, Riccardo Vivani, Aldo Romani, Claudio Costantino, Koen Janssens, Yoko Taniguchi, Joanne McCarthy, Harald Reichert and Jean Susiniadd Show full author list remove Hide full author list
Molecules 2022, 27(6), 1997; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27061997 - 20 Mar 2022
Cited by 19 | Viewed by 3941
Abstract
The European Synchrotron Radiation Facility (ESRF) has recently commissioned the new Extremely Brilliant Source (EBS). The gain in brightness as well as the continuous development of beamline instruments boosts the beamline performances, in particular in terms of accelerated data acquisition. This has motivated [...] Read more.
The European Synchrotron Radiation Facility (ESRF) has recently commissioned the new Extremely Brilliant Source (EBS). The gain in brightness as well as the continuous development of beamline instruments boosts the beamline performances, in particular in terms of accelerated data acquisition. This has motivated the development of new access modes as an alternative to standard proposals for access to beamtime, in particular via the “block allocation group” (BAG) mode. Here, we present the recently implemented “historical materials BAG”: a community proposal giving to 10 European institutes the opportunity for guaranteed beamtime at two X-ray powder diffraction (XRPD) beamlines—ID13, for 2D high lateral resolution XRPD mapping, and ID22 for high angular resolution XRPD bulk analyses—with a particular focus on applications to cultural heritage. The capabilities offered by these instruments, the specific hardware and software developments to facilitate and speed-up data acquisition and data processing are detailed, and the first results from this new access are illustrated with recent applications to pigments, paintings, ceramics and wood. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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12 pages, 1848 KiB  
Article
Iron Forms Fe(II) and Fe(III) Determination in Pre-Roman Iron Age Archaeological Pottery as a New Tool in Archaeometry
by Lidia Kozak, Andrzej Michałowski, Jedrzej Proch, Michal Krueger, Octavian Munteanu and Przemyslaw Niedzielski
Molecules 2021, 26(18), 5617; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26185617 - 16 Sep 2021
Cited by 4 | Viewed by 2041
Abstract
This article presents studies on iron speciation in the pottery obtained from archaeological sites. The determination of iron forms Fe(II) and Fe(III) has been provided by a very simple test that is available for routine analysis involving the technique of molecular absorption spectrophotometry [...] Read more.
This article presents studies on iron speciation in the pottery obtained from archaeological sites. The determination of iron forms Fe(II) and Fe(III) has been provided by a very simple test that is available for routine analysis involving the technique of molecular absorption spectrophotometry (UV–Vis) in the acid leachable fraction of pottery. The elemental composition of the acid leachable fraction has been determined by inductively coupled plasma optical emission spectrometry (ICP-OES). Additionally, the total concentration of the selected elements has been determined by X-ray fluorescence spectrometry with energy dispersion (EDXRF). The results of the iron forms’ determinations in archaeological pottery samples have been applied in the archaeometric studies on the potential recognition of the pottery production technology, definitely going beyond the traditional analysis of the pottery colour. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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Review

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35 pages, 1433 KiB  
Review
Artefact Profiling: Panomics Approaches for Understanding the Materiality of Written Artefacts
by Marina Creydt and Markus Fischer
Molecules 2023, 28(12), 4872; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules28124872 - 20 Jun 2023
Cited by 1 | Viewed by 1268
Abstract
This review explains the strategies behind genomics, proteomics, metabolomics, metallomics and isotopolomics approaches and their applicability to written artefacts. The respective sub-chapters give an insight into the analytical procedure and the conclusions drawn from such analyses. A distinction is made between information that [...] Read more.
This review explains the strategies behind genomics, proteomics, metabolomics, metallomics and isotopolomics approaches and their applicability to written artefacts. The respective sub-chapters give an insight into the analytical procedure and the conclusions drawn from such analyses. A distinction is made between information that can be obtained from the materials used in the respective manuscript and meta-information that cannot be obtained from the manuscript itself, but from residues of organisms such as bacteria or the authors and readers. In addition, various sampling techniques are discussed in particular, which pose a special challenge in manuscripts. The focus is on high-resolution, non-targeted strategies that can be used to extract the maximum amount of information about ancient objects. The combination of the various omics disciplines (panomics) especially offers potential added value in terms of the best possible interpretations of the data received. The information obtained can be used to understand the production of ancient artefacts, to gain impressions of former living conditions, to prove their authenticity, to assess whether there is a toxic hazard in handling the manuscripts, and to be able to determine appropriate measures for their conservation and restoration. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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23 pages, 1856 KiB  
Review
Lipids in Archaeological Pottery: A Review on Their Sampling and Extraction Techniques
by Anna Irto, Giuseppe Micalizzi, Clemente Bretti, Valentina Chiaia, Luigi Mondello and Paola Cardiano
Molecules 2022, 27(11), 3451; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27113451 - 26 May 2022
Cited by 8 | Viewed by 4661
Abstract
Several studies have been performed so far for the effective recovery, detection and quantification of specific compounds and their degradation products in archaeological materials. According to the literature, lipid molecules are the most durable and widespread biomarkers in ancient pottery. Artificial ageing studies [...] Read more.
Several studies have been performed so far for the effective recovery, detection and quantification of specific compounds and their degradation products in archaeological materials. According to the literature, lipid molecules are the most durable and widespread biomarkers in ancient pottery. Artificial ageing studies to simulate lipid alterations over time have been reported. In this review, specific lipid archaeological biomarkers and well-established sampling and extraction methodologies are discussed. Although suitable analytical techniques have unraveled archaeological questions, some issues remain open such as the need to introduce innovative and miniaturized protocols to avoid extractions with organic solvents, which are often laborious and non-environmentally friendly. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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26 pages, 11845 KiB  
Review
Fatty Acids and Their Metal Salts: A Review of Their Infrared Spectra in Light of Their Presence in Cultural Heritage
by Anna Filopoulou, Sophia Vlachou and Stamatis C. Boyatzis
Molecules 2021, 26(19), 6005; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26196005 - 03 Oct 2021
Cited by 32 | Viewed by 7053
Abstract
In a cultural heritage context, fatty acids are usually found as breakdown products of lipid-containing organic remains in archaeological findings, binders in aged oil paintings, and additives in modern art-related materials. They may further interact with the ionic environment transforming into metal soaps, [...] Read more.
In a cultural heritage context, fatty acids are usually found as breakdown products of lipid-containing organic remains in archaeological findings, binders in aged oil paintings, and additives in modern art-related materials. They may further interact with the ionic environment transforming into metal soaps, a process that has been recognized as a threat in aged paintings but has received less attention in archaeological objects. The investigation of the above related categories of materials with infrared spectroscopy can provide an overall picture of the organic components’ identity and demonstrate their condition and prehistory. The capability of investigating and distinguishing fatty acids and their metal soaps through their rich infrared features, such as the acidic carbonyl, the carboxylate shifts, the variable splits of alkyl chain stretching, bending, twisting, wagging, and rocking vibrations, as well as the hydroxyl peak envelopes and acid dimer bands, allows for their direct detailed characterization. This paper reviews the infrared spectra of selected saturated fatty monoacids and diacids, and their corresponding sodium, calcium, and zinc salts and, supported by newly recorded data, highlights the significance of their spectroscopic features. Full article
(This article belongs to the Special Issue Advances in Analytical Strategies to Study Cultural Heritage Samples)
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