This work presents a comparative osteological, material, and technical investigation of three 18th-century simulacra preserved in Portugal, aiming to clarify their origin, circulation, assembly, and shared workshop practices. Archival documentation and authentication seals confirmed their Roman origin and circulation during the 1770s. Radiocarbon dating places the skeletal remains between the 3rd and 5th centuries, spanning both periods of Christian persecution and subsequent imperial consolidation. Osteological, radiographic, and endoscopic analyses revealed differing anatomical configurations: St Semuc and St Fortunato incorporate remains from multiple non-adult individuals, assembled through deliberate substitution and consolidation practices, whereas St Clemente preserves a largely complete and anatomically coherent skeleton of a probable young adult male. Nevertheless, a similar assemblage for the body was uncovered for all simulacra . Facial modelling relied on silk gauze tiers, stiffened with various organic materials, alone or mixed, including proteinaceous and resin binders, such as collagen-based glues and conifer colophony-type. Imaging-based morphometric analysis was used to explore the weave type, and similar morphometric parameters were estimated, indicating a deliberate and coherent choice of gauze type. Ultimately, SEM-EDS showed that "false gold" strips (gilt-silvered-copper strips) were used in the simulacra's helmets. Overall, the interdisciplinary approach evidenced that simulacra were assembled as devotional reliquaries likely in Rome, and that they shared the same workshop or similar workshop practices. (c) 2026 The Author(s). Published by Elsevier Masson SAS. This is an open access article under the CC BY license ( http://creativecommons.org/licenses/by/4.0/ )

The Orthographia Pratica de Varias Letras is a unique 17th-century Portuguese codex, notable for its exceptional significance in the history of Latin calligraphy during the Modern period. Unfortunately, it faces complex conservation challenges due to the presence of iron gall ink (IGI). This work aimed to thoroughly characterise the inks and their impact on the manuscript using an integrated analytical approach. Extensive micro-XRF analysis revealed two distinct groups of IGIs based on their transition metal content. Zn-rich IGIs were found in half of the manuscript, suggesting the use of Zn-bearing green vitriol. In contrast, a more refined form of green vitriol was identified in the IGIs on the other half, suggesting that different types of vitriol were used. Variations in the binder-to-vitriol ratios were proposed, indicating distinct IGI formulations throughout the codex. The poor condition observed in some folios was primarily associated with greater ink coverage per surface area and lower binder content. FIB-SEM and PIXE analysis provided insights into the behaviour of Fe within the cellulose structure, including penetration and lateral migration. The IGI chromophore was further investigated by M & ouml;ssbauer and XPS, which confirmed an Fe(III)-polyphenol mono-complex with a catecholate binding mode and Fe(III) in an octahedral arrangement. (c) 2026 The Author(s). Published by Elsevier Masson SAS. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/)

Iron gall inks (IGIs) played a central role as a writing medium in Western countries, leaving behind a vast legacy and significant conservation challenges. This study presents a twofold methodological approach to investigate the physicochemical behaviour of IGI-based formulations found in historical Portuguese sources. Fresh and 6-month naturally aged precipitates and supernatant solutions (dried inks) were characterised, and the impact of IGIs on Whatman paper over ageing was studied using attenuated total reflectance Fourier-transform infrared (ATR-FT-IR) spectroscopy, Raman and Mössbauer spectroscopies and X-ray diffraction (XRD). Iron(II) sulphates comprised the primary crystalline phase in the precipitates, while the dried inks consisted of distinct Fe(III)-polyphenol (PPh) complexes. Over time, Fe(III) Mössbauer parameters supported complex structural alterations. IGI-induced degradation on aged mockups was attested by Fe(II) oxalate formation until total depletion of the Fe(III)-PPh fraction. pH, ATR-FT-IR and degree of polymerisation analyses suggested that cellulose oxidation is the primary degradation mechanism, and the physical properties and XRD corroborated that the cellulose structure became disordered over ageing. The ink with the higher weight ratio of Fe(II) sulphate:gallnuts (unbalanced) exhibited the most aggressive action on the support. The results confirm that the more unbalanced the ink composition, the more severe its impact, with ink concentration per surface area also being a critical factor in paper decay.

This paper addresses corrosion risk management for pewter objects from the Belinho I shipwreck (Esposende, Portugal). A collaborative framework was established, involving community stakeholders during the critical post-recovery phase, leading to the development of both field community and laboratory preventive conservation protocols. During the second phase of the laboratory protocol, a crowned-hammer hallmark was identified, consistent with others in the assemblage. The third phase of the laboratory protocol implemented a progressive sequence of passivation baths guided by Pourbaix diagrams and systematic monitoring of physicochemical parameters (Eh, pH, conductivity, and temperature). Characterization of primary corrosion products and precipitates from the baths, using 3D digital microscopy, SEM/EDS, & micro;-Raman, and XRD, identified basic tin chlorides with abhurite and hydroromarchite structures. Collectively, results demonstrate that immediate preventive conservation is an effective strategy for controlling corrosion risk, underscoring the necessity of collaborative frameworks for the long-term safeguarding of underwater pewter heritage.

Simulacra, or full-body reliquaries of corpi santi , have largely been overlooked in the discourse of the past century by the Church, the general public, and scholars. This work investigates two noteworthy cases among simulacra—two young individuals, St. Primogenita and St. Theodore—from Santa Casa da Misericórdia de Almada in Portugal. Based on a historical and analytical approach, the study examines the simulacra context, assembly methods, materials, symbols of martyrdom, and adornments. Their possible arrival in Portugal in the late eighteenth century is supported by the Bishop's seal and textile features that reflect the fashion of that period. Radiographic imaging and particularly borescope inspections revealed distinct assembly techniques, with St. Theodore displaying meticulous anatomical assembly, while St. Primogenita's construction is less precise. However, access to the cranium fragments of St. Primogenita revealed an elaborate consolidation method. SEM–EDS, FT-IR, and Py-GC–MS analyses identified a fibrous material coated with a dark brown paste, likely used to bond the unfused parts of the ectocranium fragments of a young individual, as well as a paste applied to reinforce the endocranium. Martyrdom symbols further distinguished the simulacra , with St. Primogenita adorned with a silk petal crown attached using animal glue, whereas St. Theodore's crown was crafted from pigment-dyed cellulosic materials. LC-DAD-MS analysis revealed the natural dyes used in coloured threads. Only St. Primogenita retained fragments from a phial of blood, where a creative method may have been employed to emphasise the blood content. This investigation highlighted the complexity and artistry behind these simulacra . Graphical abstract

The simulacrum of Saint Vincent Martyr, one of four corpi santi at the Major Seminary of Coimbra, Portugal, features Roman-origin bones mounted in metallic frameworks and covered with intricate Baroque garments. Enshrined within the urn-altar in Saint Michael's Chapel, its remains were exhumed from the Catacomb of Priscila and brought to Portugal in 1760 by Bishop Count D. Miguel da Anunciação. This study employs a multianalytical approach to examine the simulacrum's materiality, construction, and state of conservation. Non-invasive techniques, including digital radiography and borescope inspection, assessed structural integrity and skeletal arrangement. When feasible, micro-samples were collected for laboratory analysis. Optical microscopy and scanning electron microscopy with chemical analysis were used to analyse paper, textile fibres, and metal threads, revealing evidence of both craftsmanship and deterioration patterns. Additionally, Fourier-transform infrared spectroscopy characterised adhesives, coatings, and pigments, while chromatographic techniques identified dyes in garments and wax components on the face. Results corroborated photochemical damage, textile decay, and structural alterations, with in situ radiographic analyses revealing misaligned skeletal remains. Notably, softwood pulp paper with kaolin and an emerald green pigment in the flower crown points to a 19th-century local intervention after the French invasions of 1810. Furthermore, calcium carbonate in wax and lead-based pigments with iron oxides on the simulacrum's face indicate intentional methods to enhance durability and mimic human features. This study integrates material analysis with historical context to deepen understanding of Saint Vincent's simulacrum, tracing its material transformations and informing future conservation strategies for similar artefacts.

Com a investigação desenvolvida por esta equipa interdisciplinar, confirma-se a existência de uma areia processada para secar os textos nos séculos xvi–xix, em Portugal. Embora semelhante ao que aparecia em outros pontos da Europa, tinha as suas especificidades. Era a «areia de escrever», que muitos conventos e casas religiosas da época adquiriam. A sua composição podia variar, sendo constituída essencialmente por minerais (sobretudo ilmenite), a que se podiam juntar resíduos orgânicos.Estas areias representam hoje uma importante fonte histórica que tem sido negligenciada. Retirá-las pode implicar danos na mancha de texto e coloca sérios problemas éticos.

Iron gall ink (IGI), renowned for its indelibility, was the most important writing ink in the Western world from the 15th to the late 19th century. However, it is now known that IGIs induce acid-catalyzed hydrolysis and iron-catalyzed oxidation of the cellulose in historical paper documents. These mechanisms of deterioration cause significant damage to the writing support materials, including color alteration and burn-through appearance, and in the worst scenarios, physical disintegration of the supports. Minimally invasive, long-term effective conservation treatments that tackle the underlying mechanisms of IGI degradation and their corrosion effects are yet to be developed. This study introduces the deployment of hydrophobic and anticorrosive polyoxometalate-ionic liquids (POM-ILs) as colorless coatings to counteract IGI-corrosion of cellulosic supports. Model IGI-containing papers (mockups) were prepared, coated with POM-ILs, and artificially aged to assess the compatibility of POM-ILs with IGI-containing documents. Comprehensive monitoring using colorimetric and scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM/EDS) analyses showed minimal interference with the aesthetic properties and morphology of the IGI mockups. In addition, polyoxometalates (POMs) with vacant metal atom sites in the cluster shell can be used to coordinate free transition metal ions. The ability of a monolacunary Keggin-type polyoxotungstate to coordinate free Fe(II) from IGI solution was demonstrated using UV-vis analysis. This led to the formation of a dimeric species, [(SiW11O39Fe)2O]K12·28H2O, which was characterized by single-crystal X-ray diffraction. Altogether, this study points to POM-ILs as promising protective coatings for effectively preserving historical IGI-written heritage.

A collection of relics from a regal donation of Queen Leonor (1458-1525) to the Madre de Deus Monastery, inserted in busts from the late 16th century and the first half of the 17th, is being studied from several perspectives. Through a multi-analytical methodology, this study aims to characterize the materials and techniques used in the sculptures’ production, searching for affinities and differences between them to shed light on possible origins and ordering processes. The analytical study includes the use of μ-FTIR, μ-XRD, μ-Raman spectroscopy, SEM-EDS, GC-MS and LC/DAD/MS. The results confirmed the use of materials and techniques well known and established in the 16th and 17th centuries in Portugal, such as gypsum and anhydrite in the white preparation, a predominantly kaolinitic clay used for the bole layer and highly pure gold alloys. The palette includes some of the most common pigments of the time (lead white, vermilion, red ochre, red lead, malachite, azurite, indigo, yellow ochre and carbon black). Nonetheless, there have been some less expected results, such as lead-tin yellow and realgar, all poorly documented in the Portuguese artistic production of this period, Prussian blue, and the use of a cochineal lake and lac dye in the relic’s containers.

A substantial part of our written heritage is threatened by the fact that much of it has been written using iron-gall ink (IGI). One such example is the documents of the Portuguese Inquisition Tribunals, held by the Arquivo Nacional da Torre do Tombo. Here we present the first systematic analytical approach, using SEM/EDS, µ-FT-IR-ATR and µ-Raman techniques, to characterise fragments from historical records of the Inquisition Tribunals of Évora, Lisboa and Coimbra from the 16th to 18th centuries. The writing ink was identified as IGI, providing complementary compositional data and establishing differences between various formulations of the ink. Additionally, the deleterious effects of the inks-associated degradation phenomena were highlighted. This work allowed understand the writing inks used by this Portuguese institution.

This paper reports the results of a multi analytical research undertaken on a mural and on a panel painting altarpiece authored by Jose de Escovar in 1603, one of the most productive and controversial painters working for Evora Archiepiscopate at the end of the 16th century and beginning of the 17th century. The two paintings are among his first documented artworks in the region and the only case where both are still in their original architectural location - the Chapel of the Souls in the main church of Vila Nova da Baronia (30 km away from the city of Evora). Jose de Escovar is a well-known mural painter but not much is still known about his other skills. To better define his craftsmanship, comparison of technical features and painting materials employed on both supports and paint layers was carried out using a multi-analytical setup for in situ analyses and laboratory characterization. The analytical campaign comprised technical photography (UVF-Vis-IR), portable EDXRF, OM, XRD, SEM/EDS, mu-Raman, mu-FT-IR and py-GC/MS. The results showed that although Jose de Escovar was considered a minor painter, he was clearly acquainted with both painting techniques and the use of different materials in accordance with the pictorial specifications and traditions at the time in Europe.

This work used a multi-analytical approach to characterize two 19th century ambrotypes and was motivated by the lack of insight on these historical objects. Photographic imaging and optical microscopy (OM) were used to identify abrasions, cracks related to reticulation, tarnishing, and other aspects associated to production and degradation processes. With variable pressure scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (EDS) these processes were seen with great detail and further characterized. Elemental point analysis and elemental mapping showed that the photosensitive material used was silver iodide. Degradation compounds were found as silver and chlorine-containing compounds. In one of the items, the tarnishing area also contained redeposited silver in a ring-shape surrounding a nucleus rich in silver, copper, and sulfur, in addition to copper-based salts. EDS analyses also identified that the supports were common soda-lime-silica glasses, refined with arsenic; and showed that a pigment rich in iron was used in both items to hand color the cheeks, extended with aluminum silicates alone or mixed with barium sulfate. The μ-Raman study pointed out that a synthetic Mars pigment was employed. μ-Fourier-transform infrared spectroscopy analyses identified collodion as the binder. Shellac was used as a protective varnish in one of the items and a gum was possibly employed on the other. Bitumen was used for the background in one ambrotype.

In this paper the object of study was to determine the chemical nature of foxing stains in paper.The purpose of our study was to deepen the knowledge on the paper with special emphasis on foxing stains, their chemical nature and morphological aspects of foxing stains in paper.The methods used are photography under different illuminations and optical microscopy. The presence of fibers disruption was observed with scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS), it was used Attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) was also used. Micro X-ray diffraction was used to evaluate the crystalline fillers in the sample. Mass Spectrometry was used for chemical analysis to identify the organic components and different classes of organic compounds.From this study we conclude: unfoxed areas and foxed areas of paper samples showed no differences from a morphological point of view. The unfoxed areas do not present disruption of fibers or accumulation of particles. The sample’ surface was structurally organized, paper fibers seem to be in good condition, without any visible disturbance. The combination of several non-destructive techniques allowed the characterization of paper composition and the evaluation of morphological aspects.

This article reports the preliminary results of a technical and material study carried out on a 17th century panel painting located at the Chapel of the Souls in the main church of Vila Nova da Baronia (30 km away from Evora city, in southern Portugal). This painting is attributed to Jose the Escovar, a painter that worked for Evora Archiepiscopate between 1583 and 1622. Jose the Escovar is known by his mural paintings all across the Alentejo region. This is the first time that a panel painting made by this artist was studied. Analytical methods used included in situ technical photography (visible (Vis), raking light (RAK), infrared (IR), and ultraviolet (UV)), optical microscopy of cross sections, scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDS), micro Raman spectroscopy, and micro Fourier transform infrared spectroscopy (-FT-IR). The goal was to ascertain the techniques and colored materials used by Escovar on this painting so that the data can be used in future comparisons with others works attributed to this painter based on stylistic aspects. (c) 2016 Wiley Periodicals, Inc. Col Res Appl, 41, 252-257, 2016

This work comprises the use of a multi-analytical approach combined with microbiological studies to characterize six paper samples, containing foxing stains, from the 20th century, regarding their cellulose matrix, fillers, and sizing materials, and to evaluate possible paper degradation that might have occurred during the foxing stains. Photography under different illuminations and optical microscopy were used for morphological characterization of the paper samples and foxing stains. Scanning electron microscopy coupled energy dispersive spectroscopy (SEM-EDS) was of particular importance for defining the presence of fiber disorder and disruption on the surface of some of the stains, and localized accumulations of mineral-like particles on the surface of others. SEM-EDS, attenuated total reflection Fourier transform infrared spectroscopy (ATR-FT-IR), and energy dispersive X-ray fluorescence (EDXRF) were used for the identification of mineral fillers, whereas sizing agents were analyzed using ATR-FT-IR. EDXRF results showed that no differences, within the standard deviation, were found in iron and copper contents between the foxed and unfoxed areas. Fungi belonging to the genus Penicillium spp. were found in all the paper samples. Unfoxed areas presented lower contamination than the foxed areas.

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