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Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement

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

Deadline for manuscript submissions: closed (30 June 2023) | Viewed by 18708

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Dr. Lorena Carla Giannossa

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Department of Chemistry, University of Bari Aldo Moro, Bari, Italy
Interests: analytical chemistry; archaeometry; ceramics; cultural heritage; spectroscopy techniques; statistical treatments
Special Issues, Collections and Topics in MDPI journals

Prof. Dr. Annarosa Mangone

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Guest Editor

Department of Chemistry, University of Bari “Aldo Moro”, Bari, Italy
Interests: analytical chemistry; archaeometry; ceramics; cultural heritage; spectroscopy techniques; statistical treatments

Special Issue Information

Dear Colleagues,

It is our great pleasure to invite you to submit a manuscript to this themed Special Issue in honor of Professor Luigia Sabbatini's retirement.

Luigia Sabbatini (retired) was full professor of Analytical Chemistry at the University of Bari Aldo Moro 1986–2021. Among their academic and scientific duties: Representative of Italian Chemical Society in the European Analytical Chemistry Division of EuCheMS 2010–2021; President of the Analytical Chemistry Division of Italian Chemical Society (1998–2000); Member of the Senate of the University of Bari (1997–2002); Head of Chemistry Department of the University of Bari Aldo Moro (2005–2010); Coordinator of the Heads of Departments Committee at University of Bari (2005–2008); Director of the Research Center "Laboratory for Diagnostics in Cultural Heritage" (2005–2007; 2014–2019).

At present Associate Editor of Journal VACUUM (Elsevier), served in the past for many years as member of the Advisory Board of Analytical and Bioanalytical Chemistry (Springer), Nanomaterials (MDPI) and as member of the Editorial Board of Journal Electron Spectroscopy and Related Phenomena (Elsevier)

Scientific Coordinator of many Research Projects financed by Italian Minister for University and Research (MIUR) and National Council of Research (CNR), Puglia Region, EC, Interreg – IPA Cross-Border Cooperation Program.

Author of about 180 ISI papers, 4 books, co-inventor of several patents, guest editor of three Special Issues (Analytical and Bioanalytical Chemistry, Nanomaterials). About 150 communications at national and international congresses (49 invited).

She was awarded the “Canneri Medal” of the Analytical Chemistry Division of Italian Chemical Society (2017) and the "Career recognition Plaque" of the Analytical Chemistry Division of Italian Chemical Society (2021).

Her main scientific interests focus on:

(a) Development of non-invasive and micro-destructive analytical methodologies for the diagnosis of works of art (particular attention in recent years has been devoted to the study of composition and chemical ageing of: i) surface decoration by XPS, ii) lipids and proteins in paintings by MALDI-TOF, iii) pigments by micro-Raman, iv) synthetic materials (acrylic-, alchidic-, vinylic-based polymers/copolymers) of use in modern paintings, as well as in restoration by XPS, MALDI-TOF, and Py-GC/MS);

(b) Synthesis and characterization of nanostructured materials endowed with biocide and antifouling properties for application mainly in biomedical devices and cultural heritage conservation.

With the spirit to promote an inclusive Special Issue bringing together researchers engaged in CH investigations, we renew our invitation. Papers dealing with all aspects relating with chemical characterization in the field of cultural heritage are welcome: regular articles, communications, as well as reviews. Papers emphasizing a multidisciplinary approach will be very welcome.

Topics can range from the development of new strategies (including sample preparation, new materials, use of non-destructive instrumentation, or innovative multivariate statistical treatments) to their applications in case studies.

Chemical methods devoted to deepening knowledge about conservation, ageing, alteration, deterioration, dating, and authenticity processes are all warmly appreciated as well as research papers focused on emerging solutions towards sustainable practices in CH.

Best regards,

Dr. Lorena Carla Giannossa
Prof. Dr. Annarosa Mangone
Guest Editors

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Keywords

cultural heritage
archaeometry
spectroscopy techniques
spectrometry techniques
statistical treatments
conservation materials
degradation phenomena
cultural heritage monitoring

Published Papers (11 papers)

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Research

17 pages, 4938 KiB

Open AccessArticle

Tracking the Progression of the Simulated Bronze Disease—A Laboratory X-ray Microtomography Study

by Zedong Wang, Xiaoqi Xi, Lei Li, Zhicun Zhang, Yu Han, Xinguang Wang, Zhaoying Sun, Hongfeng Zhao, Ning Yuan, Huimin Li, Bin Yan and Jiachang Chen

Molecules 2023, 28(13), 4933; https://doi.org/10.3390/molecules28134933 - 23 Jun 2023

Viewed by 1142

Abstract

The internal three-dimensional characteristics of X-ray microtomography (micro-CT) has great application potential in the field of bronze corrosion. This work presents a method of simulating bronze disease based on an in situ micro-CT image to study the characteristics of the oxidative hydrolysis reactions of copper(I) chloride and copper(II) chloride dihydrate. A series of high-resolution reconstruction images were obtained by carrying out micro-CT at three key points throughout the experiment. We found that the reactions of copper(I) chloride and copper(II) chloride dihydrate showed different characteristics at different stages of the simulation in the micro-CT view. The method proposed in this work specifically simulated one single type of bronze corrosion and characterized the evolution characteristics of simulated bronze disease. It provides a new perspective to investigate bronze disease and can help improve the subsequent use of micro-CT to distinguish real bronze corrosions. Full article

(This article belongs to the Special Issue Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement)

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20 pages, 5727 KiB

Open AccessArticle

Spectral Features Differentiate Aging-Induced Changes in Parchment—A Combined Approach of UV/VIS, µ-ATR/FTIR and µ-Raman Spectroscopy with Multivariate Data Analysis

by Antonia Malissa, Federica Cappa, Manfred Schreiner and Martina Marchetti-Deschmann

Molecules 2023, 28(12), 4584; https://doi.org/10.3390/molecules28124584 - 06 Jun 2023

Cited by 2 | Viewed by 1362

Abstract

From the moment of production, artworks are constantly exposed to changing environmental factors potentially inducing degradation. Therefore, detailed knowledge of natural degradation phenomena is essential for proper damage assessment and preservation. With special focus on written cultural heritage, we present a study on the degradation of sheep parchment employing accelerated aging with light (295–3000 nm) for one month, 30/50/80% relative humidity (RH) and 50 ppm sulfur dioxide with 30/50/80%RH for one week. UV/VIS spectroscopy detected changes in the sample surface appearance, showing browning after light-aging and increased brightness after SO₂-aging. Band deconvolution of ATR/FTIR and Raman spectra and factor analysis of mixed data (FAMD) revealed characteristic changes of the main parchment components. Spectral features for degradation-induced structural changes of collagen and lipids turned out to be different for the employed aging parameters. All aging conditions induced denaturation (of different degrees) indicated by changes in the secondary structure of collagen. Light treatment resulted in the most pronounced changes for collagen fibrils in addition to backbone cleavage and side chain oxidations. Additional increased disorder for lipids was observed. Despite shorter exposure times, SO₂-aging led to a weakening of protein structures induced by transitions of stabilizing disulfide bonds and side chain oxidations. Full article

(This article belongs to the Special Issue Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement)

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12 pages, 7407 KiB

Open AccessArticle

New Insight on Archaeological Metal Finds, Nails and Lead Sheathings of the Punic Ship from Battle of the Egadi Islands

by Francesco Armetta, Rosina Celeste Ponterio, Ivana Pibiri and Maria Luisa Saladino

Molecules 2023, 28(4), 1968; https://doi.org/10.3390/molecules28041968 - 19 Feb 2023

Cited by 1 | Viewed by 2116

Abstract

The wreck of the Punic ship exhibited at the Archaeological Park of Lilybaeum (Marsala, Italy) is a unique example in the world. In this paper, the investigation of some metal finds (30 nails and 3 fragments of sheathings) belonging to the wreck of the Punic ship is reported. Portable X-ray fluorescence and Raman spectroscopy allowed us to identify the elements and compounds constituting them and make some deductions about their composition. X-ray diffractometry, polarised optical microscopy and scanning electron microscopy of the collected micro-samples allowed us to explain the degradation that occurred in the underwater environment. Full article

(This article belongs to the Special Issue Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement)

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13 pages, 1671 KiB

Open AccessArticle

New Evidence on the Reliable Use of Stable Isotopes of Bitumen Fractions in Archaeological Research

by Antonio Pennetta and Giuseppe E. De Benedetto

Molecules 2023, 28(4), 1962; https://doi.org/10.3390/molecules28041962 - 18 Feb 2023

Cited by 1 | Viewed by 1209

Abstract

One of the goals of archaeological studies is to determine how material goods and ideas moved among human populations, and bitumen is a worthy proxy because it has been used since prehistory. As a result, when bitumen is excavated from archaeological sites, determining its provenance is important because it sheds light on the trade and communication of populations at a given time. During the study of archaeological bitumen from coastal sites in central and southern Puglia (Italy), we observed that stable isotope ratios of saturated and aromatic fractions were incompatible with those obtained from asphaltenes, supporting the absorption of a foreign substance. Experiments showed that lipids are absorbed by bitumen and, in the case of oils, are distributed mainly in the saturated and aromatic fractions as their isotopic ratios change. The same experiments showed that the isotopic ratios of the asphaltenes do not change. Lipid absorption on the archaeological bitumen may have occurred before the bitumen was applied to the pottery, during the use of the pottery or while underground, before being excavated. These hypotheses are discussed, and it is concluded that the isotopic ratio of asphaltenes is a reliable proxy for provenance, whereas those of the saturated and aromatic fractions should be considered with caution due to possible lipid absorption. Nevertheless, they provide new information on pottery use that can be used in archaeological chemistry. Full article

(This article belongs to the Special Issue Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement)

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20 pages, 5224 KiB

Open AccessArticle

Preliminary Air Quality and Microclimatic Conditions Study in the Santuario della Beata Vergine dei Miracoli in Saronno (VA)

by Andrea Bergomi, Valeria Comite, Vittoria Guglielmi, Mattia Borelli, Chiara Andrea Lombardi, Roberto Bonomi, Concetta Pironti, Maria Ricciardi, Antonio Proto, Carlo Mariani and Paola Fermo

Molecules 2023, 28(4), 1615; https://doi.org/10.3390/molecules28041615 - 07 Feb 2023

Cited by 4 | Viewed by 1293

Abstract

In the present work, the microclimatic conditions (temperature (T), relative humidity (RH), and illuminance (I)), together with the air quality (both aerosol particulate matter (PM) and gaseous pollutants), were monitored to evaluate the environmental conditions inside the Santuario della Beata Vergine dei Miracoli in Saronno (VA), a masterpiece of the Italian Renaissance. For this purpose, dataloggers were used to carry out the T, RH, and I measurements, whereas an optical particle counter (OPC) was employed to perform the particle count and determine the concentration of the aerosol PM. Finally, diffusive passive samplers were used to determine the concentration of nitrogen dioxide (NO₂) and BTEX (benzene, toluene, ethylbenzene, and xylenes). To identify possible spatial variations, the studies were conducted at different sites and different heights in the Sanctuary. Particular focus was given to the Easter week during which liturgical services attracting large numbers of people were carried out. Additionally, a comparison with the outdoor values was performed to highlight the accumulation phenomena and other variations in the concentrations of the species. Despite the indoor concentrations of pollutants and variations in the thermohygrometric parameters being generally lower compared to the outdoors (e.g., 5.2–15.0 µg m⁻³ versus 17.7–45.3 µg m⁻³ for NO₂), the microclimatic conditions were often not in line with the Italian legislation and technical standards. Full article

(This article belongs to the Special Issue Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement)

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13 pages, 7936 KiB

Open AccessArticle

A Possible Natural and Inexpensive Substitute for Lapis Lazuli in the Frederick II Era: The Finding of Haüyne in Blue Lead-Tin Glazed Pottery from Melfi Castle (Italy)

by Annarosa Mangone, Maria Cristina Caggiani, Tiziana Forleo, Lorena Carla Giannossa and Pasquale Acquafredda

Molecules 2023, 28(4), 1546; https://doi.org/10.3390/molecules28041546 - 06 Feb 2023

Cited by 1 | Viewed by 1454

Abstract

The blue color of glass and ceramic glazes produced in Apulia and Basilicata (Southern Italy) between the 13th and 14th centuries and connected to the Norman-Swabian Emperor Frederick II, has been, for a long time, under archaeometric investigation. On the one hand, it has usually been associated with lapis lazuli, due to the finding of the polysulphide blue chromophores typical of lazurite. Moreover, the observation that the mineral haüyne, which belongs to the sodalite group as well as lazurite, can be blue and/or can gain a blue color after heating, due to the same chromophores, has caused this automatic attribution to be questioned, and also considering that the mineral is characteristic of the rock haüynophyre of Melfi (Potenza, Southern Italy), a location of interest for glass and pottery findings. In this paper, for the first time, several haüyne crystals were found in the blue glaze of a ceramic dish found at Melfi Castle, leading to the hypothesis that, in this case, the local haüyne-bearing source could have been used as the coloring raw material. The discovery was possible thanks to SEM-EDS and Raman analyses that, respectively, highlighted the typical numerous presence of very fine sulphur-based inclusions in the crystals and the characteristic Raman signal of blue haüyne. This study was also focused on the composition of the crystals inclusions, aided by SEM-EDS and Raman maps, since the original very fine pyrrhotite was transformed into Cu and Pb phases (copper sulphates, copper sulphides, and lead oxide) due to reactions with cations that had mobilized from the glaze, while the migration of Si from the glass allowed the transformation of the rim of the haüyne, a silica-undersaturated mineral, into a corona of small euhedral and neomorphic Pb-rich feldspars, a silica-saturated phase. Full article

(This article belongs to the Special Issue Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement)

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32 pages, 18300 KiB

Open AccessArticle

New Insights into the Medieval Hispano-Muslim Panel Painting: The Alfarje Found in a Balearic Casal (Spain)

by Carla Álvarez-Romero, Ana García-Bueno, Teresa López-Martínez, Rafael Turatti-Guerrero, Noemí Montoya and María Teresa Doménech-Carbó

Molecules 2023, 28(3), 1235; https://doi.org/10.3390/molecules28031235 - 27 Jan 2023

Viewed by 1702

Abstract

Hispano-Muslim culture flourished during the Middle Ages in the Iberian Peninsula and Balearic Islands. During the restoration of a Balearic nobiliary building (casal), several panels with polychrome decoration on the back side were found. They were part of an old Muslim wooden ceiling (alfarje). A multi-technique strategy including optical microscopy, infrared and μRaman spectroscopies, field emission scanning electron microscopy-X-ray microanalysis (FESEM-EDX), focused ion beam (FIB-FESEM-EDX), atomic force microscopy nanoindentation (AFM-NI), and gas chromatography-mass spectrometry (GC-MS) has been applied in the analysis of these panel paintings and has provided morphological and compositional data that have led to the identification of the materials and artistic technique as well as the alteration mechanisms due to the natural aging and the adverse conditions of conservation. As a novelty, this study has confirmed the use of indigo as a blue pigment, an unusual material in Hispano-Muslim panel painting. Apart from the notable change in the visual appearance observed in the paintings, the study has also confirmed a change in the mechanical resistance in the paint layers. These changes have been induced by the combination of the chemical and microbiological alteration mechanisms identified. Full article

(This article belongs to the Special Issue Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement)

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15 pages, 28402 KiB

Open AccessArticle

Study of the Materials and Techniques of a Rare Papier-Mâché Mushroom Model Crafted in H. Arnoldi Factory

by Maria J. Melo, Ana Freitas, Cristiana Vieira, Márcia Vilarigues, Márcia Vieira, Paula Nabais, Sílvia Sequeira, Mónica Lourenço, Gabriel Oliveira and Ana Rita Correia

Molecules 2023, 28(3), 1062; https://doi.org/10.3390/molecules28031062 - 20 Jan 2023

Viewed by 1779

Abstract

The Natural History and Science Museum of the University of Porto houses a collection of 45 models of fungi in papier-mâché from the 19th-century, which were used at the university until 2015 as didactic models. For the first time, the materials and techniques used in the production of a Boletus edulis model were studied (vernacular name: cep, porcini). These sculptures, made to life-size scale, are painted in colors similar to those of the represented species (white, brown, and light brown). They are fixed to a rectangular base, which is painted black, and to which moss has been pasted. To fully characterize each color, at the molecular level, a multi-analytical approach was used, combining energy-dispersive x-ray fluorescence spectroscopy (micro-XRF) with fingerprinting techniques of Raman microscopy (microRaman and handheld Raman) spectroscopy and microFourier transform infrared spectroscopy (microFTIR). The papier-mâché was prepared with a groundwood paper to which kaolin and a quartz-based material have been added to reinforce the structure. Raman microscopy also identified carbon black in it, which is possibly responsible for its grey color. The white color was unequivocally identified as lithopone by microRaman. This white paint was prepared in a proteinaceous tempera, with calcium carbonate having been identified as filler (by microFTIR). In the brown color, iron was identified by microXRF, pointing to the use of ocher, which was not possible to identify by microRaman and microFTIR. Regarding the black rectangular base, the moss was fixed using a collagen-based glue. The binding medium in this black is possibly a mixture of drying oil and protein. Again, XRF detected iron as the main element, but it was not possible to acquire a Raman spectrum due to the high fluorescence of the binder/varnish. Others, such as the writing inks, will also be discussed. The colors identified are in line with the best materials available for use by artists of that time. This new knowledge is fundamental to informing the choice of the best conservation strategies for the preservation of these extraordinary models. Full article

(This article belongs to the Special Issue Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement)

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23 pages, 15349 KiB

Open AccessArticle

Pigments and Techniques of Hellenistic Apulian Tomb Painting

by Annarosa Mangone, Camilla Colombi, Giacomo Eramo, Italo Maria Muntoni, Tiziana Forleo and Lorena Carla Giannossa

Molecules 2023, 28(3), 1055; https://doi.org/10.3390/molecules28031055 - 20 Jan 2023

Cited by 2 | Viewed by 1456

Abstract

The wall paintings of five Hellenistic tombs in Apulia were analysed using a multi-technique approach to discern the painting techniques used and contextualise them within the phenomenon of Hellenistic tomb painting in Southern Italy. In particular, the question was asked whether technical knowledge played a role in the reception of Hellenistic artistic models and whether this knowledge was present locally. Raman and IR spectroscopies were used to identify pigments, colourants, and binders; light and electron microscopy were used to determine the structural characteristics of the paint layers and recognise the manufacturing technique. Analyses identified a fresco application for the Tomba dei Cavalieri (Arpi) and a dry application for the Canosian hypogea. The palette—typical for Hellenistic tomb painting in Southern Italy, Etruria and Macedonia—was composed of lime (white), charcoal (black), hematite (red), goethite (yellow), and Egyptian blue (blue). In the Tomba della Nike (Arpi), meanwhile, two particularly refined preparatory layers were observed. The palette was enriched with precious cinnabar and madder lake. The colouring components of the root were mixed with clay and K-alum applied on an additional layer of lime. The use of madder lake and a pink background link the painting to the polychrome Daunian pottery, and the contribution of a local workshop to the decoration of this tomb thus seems plausible. Full article

(This article belongs to the Special Issue Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement)

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18 pages, 10162 KiB

Open AccessArticle

Rust Conversion of Proanthocyanidins to Archaeological Steel: A Case Study of Lingzhao Xuan in the Forbidden City

by Minghao Jia, Pei Hu, Xiaogu Zhang and Gang Hu

Molecules 2022, 27(22), 7711; https://doi.org/10.3390/molecules27227711 - 09 Nov 2022

Cited by 1 | Viewed by 1329

Abstract

This work was focused on the rust conversion of proanthocyanidins (PC) for goethite (α-FeOOH), akaganeite (β-FeOOH) and lepidocrocite (γ-FeOOH), trying to show the potential of PC as an eco-friendly corrosion inhibitor and rust converter for archaeological steel conservation. The experiment used a rusted steel screw from Lingzhao Xuan of the Forbidden City in the Qing Dynasty and three kinds of pure iron oxyhydroxides as research samples. By means of micro-Raman, FTIR, XRD, XPS, SEM and EIS, PC had the ability to chemically react with iron oxyhydroxides in the rust, forming amorphous PC-FeOOH with a marked signal about 1384 cm⁻¹ as phenolic-Fe in infrared properties. The original relatively stable iron oxides were not induced to phase transformation and still remained. The converted rust layer could be more stable in the corrosive medium and increased the corrosion potential more effectively. Both the rust layer resistance and the charge transfer resistance of the archaeological samples were improved by at least 3 times with 5.0 g/L of PC, which could reasonably stabilize the archaeological rust and hindered external corrosive penetration into the core. It was a mild protection material that showed satisfactory performance for archaeological steel cultural heritage and has a good application prospect. Full article

(This article belongs to the Special Issue Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement)

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18 pages, 3880 KiB

Open AccessArticle

Data from Multiple Portable XRF Units and Their Significance for Ancient Glass Studies

by Oleh Yatsuk, Marco Ferretti, Astrik Gorghinian, Giacomo Fiocco, Marco Malagodi, Angelo Agostino and Monica Gulmini

Molecules 2022, 27(18), 6068; https://doi.org/10.3390/molecules27186068 - 17 Sep 2022

Cited by 11 | Viewed by 2615

Abstract

X-ray fluorescence spectroscopy is a non-destructive technique employed for elemental analysis of a wide range of materials. Its advantages are especially valued in archaeometry, where portable instruments are available. Considering ancient glass, such instruments allow for the detection of some major, minor, and trace elements linked to the deliberate addition of specific components or to impurities in the raw materials of the glass batch. Besides some undoubted advantages, portable XRF (p-XRF) has some limitations that are addressed in this study. The performance assessment of four different p-XRF units and the reconciling of their output were conducted. The results show the limitations in cross-referencing the data obtained from each unit and suggest procedures to overcome the issues. The p-XRF units were tested on the set of Corning reference glasses and on a small set of archaeological glasses with known composition. The compatibility of the output was assessed using multivariate statistical tools. Such a workflow allows us to consider data from multiple sources in the same frame of reference. Full article

(This article belongs to the Special Issue Chemical Analysis Strategies in the Cultural Heritage Field: A Themed Issue in Honor of Professor Luigia Sabbatini’s Retirement)

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