Analytical Techniques Applied to the Study of Industrial Archaeology Heritage: The Case of Plaiko Zubixe Footbridge.

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.

Non-Destructive Analytical Investigation of Decorative Wallpapers Samples of the Nineteenth Century before Their Restoration.

In this work, decorative wallpapers (19th century) from an historical palace located in Oiartzun (Basque Country, Spain) were analyzed before their restoration. Micro-energy dispersive X-ray fluorescence spectroscopy, Raman spectroscopy, and attenuated total reflectance infrared spectroscopy were used to investigate the elemental and molecular composition of pigments, the presence of binders, and the state of conservation of the paper support. The aim of the investigation was trying to understand the possible degradation pathways and identify the raw materials in order to choose the best restoration protocol according to the original aspect of wallpapers. As stated from both the elemental distribution and the identification of mineral phases by Raman spectroscopy, the most used pigment was lead chromate. It was mixed with other pigments such as ultramarine blue, zinc chromate, hematite, and atacamite among others to obtain different shades and they were applied mixed with an animal glue. Brass, identified thanks to elemental micro-EDXRF maps, was employed as a shiny decorative element. In addition, a partial degradation of cellulose was detected due to its natural ageing, the acidic nature of lignin, and to a phenomenon of humidity of the walls. Probably the deposition of black particulate matter was the cause of the darkening of the painting surfaces.

Analytical methodology to evaluate the Terrestrial Weathering of Libyan Desert Glasses and Darwin Glasses after their formation.

Libyan Desert Glasses (LDGs) and Darwin Glasses (DGs) are impact glasses produced by the impact of an extraterrestrial body into the Earth million years ago. LDGs were formed in the Libyan Desert (Africa) and DGs in Tasmania (Australia). From their formation, they have suffered terrestrial weathering processes due to their interaction with the environment. This is the first work that has evaluated their weathering processes according to their composition, the surrounding environment, and the climate. An innovative methodology based on the leaching of organic and inorganic ions and chemical modeling simulations was employed. Inductively coupled plasma-mass spectrometry (ICP-MS), ionic chromatography (IC), and solid-phase microextraction (SPME), and head space (HS) injections coupled to gas chromatography and mass spectrometry (GC-MS) detection were used. As a result, soluble organic compounds such as oxalates, n-hexadecanoic acid, and 4-chlorobenzalacetone were detected. The inorganic ions suffered a similar process, going inside the body of glasses and precipitating the corresponding salts when water evaporated. As these compounds are polar, they were probably transported by infiltration waters from outside the glasses, remaining inside in the pores, cavities, or cracks of the glasses during thousands of years. In the case of the DGs, it could be observed that under the oxidizing conditions of the terrestrial atmosphere, sulfides present in some samples transformed into sulfates. Finally, this methodology could be applied in other extraterrestrial materials discovered in deserts, ice fields, or in locations with great living activity like those of Tasmania.

Wine markers in archeological potteries: detection by GC-MS at ultratrace levels.

The detection of organic residues that remain absorbed into the pores of ceramic artifacts constitutes a source of information regarding their management. Taking into account the poor conservation state of the potteries and the low amount of the organic tracers together with the main drawbacks to get the relevant information concerning different aspects of past societies, the detection of organic biomarkers is still an analytical challenge. In this work, an improved analytical methodology to maximize the recovery of organic markers related to wine in archeological ceramics is presented. The developed method consists on the extraction of wine-related organic compounds including tartaric acid, malic acid, fumaric acid, succinic acid, citric acid, and syringic acid by means of ultrasonic probe-assisted extraction (UPAE) followed by a preconcentration step by mixed-mode strong anion exchange and reversed-phase solid-phase extraction (SPE) and a derivatization step prior to analysis by means of gas chromatography-mass spectrometry (GC-MS). Finally, the method was applied to real archeological ceramic fragments (two dolia), suspected to have been used to store wine, together with organic residues found inside two amphorae from Zaragoza (Spain). Graphical abstract.

Detection of organic compounds in impact glasses formed by the collision of an extraterrestrial material with the Libyan Desert (Africa) and Tasmania (Australia).

Impact glasses are rich silica melted formed at high temperature and pressure by the impact of an extraterrestrial body on Earth. Here, Libyan Desert glasses (LDGs) and Darwin glasses (DGs) were studied. Two non-destructive analytical techniques were used to detect and characterize organic compounds present in their inclusions: Raman spectroscopy and scanning electron microscopy coupled to energy-dispersive X-ray spectroscopy (SEM-EDS). Phytoliths, humboldtine, palmitic acid, myristic acid, oleic acid, 4-methyl phthalic acid, and S-H stretching vibrations of amino acids were identified. The presence of these particular organic compounds in such materials has not been reported so far, providing information about (a) the ancient matter of the area where the impact glasses were formed, (b) organic matter belonging to the extraterrestrial body which impacted on the Earth, or (c) even to current plant or bacterial life, which could indicate an active interaction of the LDG and DG with the surrounding environment. Moreover, the identification of fullerene allowed us to know a pressure (15 GPa) and temperatures (670 K or 1800-1900 K) at which samples could be subjected.

Non-destructive characterisation of the Elephant Moraine 83227 meteorite using confocal Raman, micro-energy-dispersive X-ray fluorescence and Raman-scanning electron microscope-energy-dispersive X-ray microscopies.

The application of a non-destructive analytical procedure to characterise the mineral phases in meteorites is a key issue in order to preserve this type of scarce materials. In the present work, the Elephant Moraine 83227 meteorite, found in Antarctica in 1983 and originated from 4 Vesta asteroid, was analysed by micro-Raman spectroscopy, micro-energy-dispersive X-ray fluorescence and the structural and chemical analyser (Raman spectroscopy coupled with scanning electron microscopy-energy-dispersive spectroscopy) working in both point-by-point and image modes. The combination of all these techniques allows the extraction of, at the same time, elemental, molecular and structural data of the studied microscopic area of the meteorite. The most relevant results of the Elephant Moraine 83227 were the finding of tridymite for the first time in a 4 Vesta meteorite, along with quartz, which means that the meteorite suffered high temperatures at a certain point. Moreover, both feldspar and pyroxene were found as the main mineral phases in the sample. Ilmenite, apatite, chromite and elemental sulphur were also detected as secondary minerals. Finally, calcite was found as a weathering product, which was probably formed in terrestrial weathering processes of the pyroxene present in the sample. Besides, Raman spectroscopy provided information about the conditions that the meteorite experienced; the displacements in some feldspar Raman bands were used to estimate the temperature and pressure conditions to which the Elephant Moraine 83227 was subjected, because we obtained both low and high formation temperature feldspar.

Comparison between non-invasive methods used on paintings by Goya and his contemporaries: hyperspectral imaging vs. point-by-point spectroscopic analysis.

The development of non-invasive techniques for the characterization of pigments is crucial in order to preserve the integrity of the artwork. In this sense, the usefulness of hyperspectral imaging was demonstrated. It allows pigment characterization of the whole painting. However, it also sometimes requires the complementation of other point-by-point techniques. In the present article, the advantages of hyperspectral imaging over point-by-point spectroscopic analysis were evaluated. For that purpose, three paintings were analysed by hyperspectral imaging, handheld X-ray fluorescence and handheld Raman spectroscopy in order to determine the best non-invasive technique for pigment identifications. Thanks to this work, the main pigments used in Aragonese artworks, and especially in Goya's paintings, were identified and mapped by imaging reflection spectroscopy. All the analysed pigments corresponded to those used at the time of Goya. Regarding the techniques used, the information obtained by the hyperspectral imaging and point-by-point analysis has been, in general, different and complementary. Given this fact, selecting only one technique is not recommended, and the present work demonstrates the usefulness of the combination of all the techniques used as the best non-invasive methodology for the pigments' characterization. Moreover, the proposed methodology is a relatively quick procedure that allows a larger number of Goya's paintings in the museum to be surveyed, increasing the possibility of obtaining significant results and providing a chance for extensive comparisons, which are relevant from the point of view of art history issues.

Multispectroscopic methodology to study Libyan desert glass and its formation conditions.

Libyan desert glass (LDG) is a melt product whose origin is still a matter of controversy. With the purpose of adding new information about this enigma, the present paper analyzes the inner part of LDG specimens and compares them with the results of LDG surfaces. An integrated analytical methodology was used combining different techniques such as Raman spectroscopy, in point-by-point and imaging modes, scanning electron microscopy with X-ray microanalysis (SEM-EDS), energy-dispersive micro X-ray fluorescence spectrometry (µ-EDXRF), electron probe micro analyzer (EPMA), and optical cathodoluminescence (Optical-CL). According to our results, flow structures of the melt and the amorphous nature of the matrix could be discerned. Moreover, the observed displacement of Raman bands, such as in the cases of quartz and zircon, and the identification of certain compounds such as coesite (the most clarifying phase of high pressures), α-cristobalite, gypsum, anhydrite, corundum, rutile, amorphous calcite, aragonite, and calcite allowed us to know that LDGs could be subjected to shock pressures between 6 and more than 30 GPa, and temperatures between 300 and 1470 °C. The differences of temperature and pressure would be provoked by different cooling processes during the impact. Besides, in most cases the minerals corresponding to high pressure and temperatures were located in the inner part of the LDGs, with some exceptions that could be explained because they were trapped subsequently to the impact; there was more than one impact or heterogeneous cooling.Furthermore, nitrogen and oxygen gases were identified inside bubbles, which could have been introduced from the terrestrial atmosphere during the meteorite impact.These data helped us to clarify some clues about the origin of these enigmatic samples.

In situ X-ray fluorescence-based method to differentiate among red ochre pigments and yellow ochre pigments thermally transformed to red pigments of wall paintings from Pompeii.

Most of the magnificent wall paintings from the ancient city of Pompeii are decorated with red and yellow colors coming from the ochre pigments used. The thermal impact of the pyroclastic flow from the eruption of Vesuvius, in AD 79, promoted the transformation of some yellow painted areas to red. In this work, original red ochre, original yellow ochre, and transformed yellow ochre (nowadays showing a red color) of wall paintings from Pompeian houses (House of Marcus Lucretius and House of Gilded Cupids) were analyzed by means of a handheld energy-dispersive X-ray fluorescence spectrometer to develop a fast method that allows chemical differentiation of the original red ochre and the transformed yellow ochre. Principal component analysis of the multivariate obtained data showed that arsenic is the tracer element to distinguish between both red colored ochres. Moreover, Pompeian raw red and yellow ochre pigments recovered from the burial were analyzed in the laboratory with use of a benchtop energy-dispersive X-ray fluorescence spectrometer to confirm the elemental composition and the conclusions drawn from the in situ analysis according to the yellow ochre pigment transformation in real Pompeian wall paintings.

Multispectroscopic and Isotopic Ratio Analysis To Characterize the Inorganic Binder Used on Pompeian Pink and Purple Lake Pigments.

Because of the fact that pigments are not ubiquitous in the archeological record, the application of noninvasive analytical methods is a necessity. In this work, pink and purple lake pigments recovered from the excavations of the ancient city of Pompeii (Campania, Italy) and preserved in their original bowls at the Naples National Archaeological Museum (Italy) were analyzed to characterize the composition of their inorganic binders (mordants). In situ preliminary analyses using a hand-held energy dispersive X-ray fluorescence spectrometer (HH-ED-XRF) allowed us to determine the use of an aluminosilicate enriched in Cu and Pb. Scanning electron microscopy coupled to energy dispersive X-ray spectrometry (SEM-EDS) and benchtop ED-XRF analyses confirmed these results, while inductively coupled plasma mass spectrometry (ICPMS) allowed one to determine the concentration of major, minor, and trace elements. The use of other techniques such as X-ray diffraction (XRD), and micro-Raman and infrared spectroscopies allowed one to characterize the pigments at the molecular level. The high concentration of Cu detected in the pigments (1228-12937 µg g(-1)) could be related to the addition of Cu salts to obtain the desired final hue. The concentrations of Pb (987-2083 µg g(-1)) was also remarkable. Lead isotopic ratio analysis ((206)Pb/(207)Pb) suggested a possible origin related to the leaching of the ancient lead pipes from Pompeii and the subsequent transfer to the buried pigments or to the inorganic binder. Molecular analysis also showed that the binder is composed of an allophane-like clay. Moreover, it was possible to determine that to obtain the final purple hue of a specific pigment, Pompeian blue pigment was also mixed into the dyed clay.

An alternative analytical method based on ultrasound micro bath hydrolysis and GC-MS analysis for the characterization of organic biomarkers in archaeological ceramics.

The analysis of organic biomarkers in ancient and valuable archaeological remains provides a worthwhile source of information regarding their management. This work was focused on the development of an analytical procedure to characterize organic residues that have remained in archaeological ceramic samples. A novel analytical approach based on an alkaline hydrolysis by means of an ultrasound micro bath followed by liquid extraction was proposed to isolate saturated and unsaturated fatty acids, degradation products such as dihydroxy acids or dienoic fatty acids, isoprenoid fatty acids, and many other biomarkers from archaeological remains. This main goal has been achieved after the optimization of the main parameters affecting the hydrolysis step, the extraction procedure, and the derivatization step prior to the gas chromatography-mass spectrometry analysis. In this work, archaeological ceramic remains suspected to have been used by Basque Whalers to store whale oil in the period from the sixteenth to the seventeenth century were studied. Nevertheless, the proposed method is useful to determine the organic remains preserved in many other archaeological ceramic remains. Moreover, this methodology can be used to determine organic remains in any porous ceramic, archaeological or not. The preliminary results of the analysis of ceramic vessels led to the determination of some interesting unsaturated compounds such as 11-eicosenoic acid, an important biomarker of marine commodities, and several saturated fatty acids, which could be indicative of having used the vessels to store whale oil. Graphical abstract ᅟ.

Evidence of internalized microplastics in mussel tissues detected by volumetric Raman imaging.

Microplastics are a global ecological concern due to their potential risk to wildlife and human health. Animals ingest microplastics, which can enter the trophic chain and ultimately impact human well-being. The ingestion of microplastics can cause physical and chemical damage to the animals' digestive systems, affecting their health. To estimate the risk to ecosystems and human health, it is crucial to understand the accumulation and localization of ingested microplastics within the cells and tissues of living organisms. However, analyzing this issue is challenging due to the risk of sample contamination, given the ubiquity of microplastics. Here, an analytical approach is employed to confirm the internalization of microplastics in cryogenic cross-sections of mussel tissue. Using 3D Raman confocal microscopy in combination with chemometrics, microplastics measuring 1 µm in size were detected. The results were further validated using optical and fluorescence microscopy. The findings revealed evidence of microplastics being internalized in the digestive epithelial tissues of exposed mussels (Mytilus galloprovincialis), specifically within the digestive cells forming digestive alveoli. This study highlights the need to investigate the internalization of microplastics in organisms like mussels, as it helps us understand the potential risks they pose to aquatic biota and ultimately to human health. By employing advanced imaging techniques, challenges associated with sample contamination can be overcome and valuable insights into the impact of microplastics on marine ecosystems and human consumers are provided.

Time-course distribution of fluorescent microplastics in target tissues of mussels and polychaetes.

The majority of the plastic produced in the last century is accumulated in the environment, leading to an exacerbated contamination of marine environments due to transport from land to the ocean. In the ocean, mechanical abrasion, oxidation, and photodegradation degrade large plastics into microplastics (MPs) - 0.1 µm to 5 mm (EFSA, 2016) which are transported through water currents reaching the water surface, water column, and sediments. Further, they can be accumulated by aquatic and benthic species, entering the trophic chain and becoming a potential threat to humans. In the present research, we aimed to decipher the accumulation and distribution time-courses between different organs or target tissues of organisms inhabiting coastal areas such as mussels Mytilus galloprovincialis and polychaetes Hediste diversicolor. Both were exposed in microcosm experiments to fluorescent polystyrene MPs (1 µm) which were spiked at two doses (103 and 105 particles/mL) for 1, 4, 24, and 72 h. Mussels and polychaetes were digested with 10% KOH and filtered to quantify the number of MPs incorporated. Different anatomical parts of the body were selected and processed for cryosectioning and posterior microscopic localisation of MPs. Both species accumulate MPs spiked in water column, mainly after exposure to the highest dose. In mussels, particles were found in distinct parts of the digestive tract (stomach, digestive diverticula, ducts) and gills. Even if the majority of MPs were localised in the lumen of the digestive tract, in some cases, were inside the digestive epithelium. The identification of MPs and their internalization in the digestive system was studied using Raman spectroscopy. A decreasing trend with time regarding MPs number in the digestive tract (stomach) of mussels was observed while the opposite was recorded for polychaetes and sediments. The combination of microscopical observations of frozen sections and Raman, appeared to be accurate methodologies to address MPs abundances and to reveal their localisation in different organs. This work has enabled to understand the distribution and fate of MPs in different environmental compartments and it could contribute to gain knowledge about their impact after ingestion by coastal organisms.

Misinterpretation in microplastic detection in biological tissues: When 2D imaging is not enough.

The presence of microplastics in the food chain is a public concern worldwide, and its analysis is an analytical challenge. In our research, we apply Raman imaging to study the presence of 1 µm polystyrene microplastics in cryosections of Mytilus galloprovincialis due to its wide geographic distribution, widespread occurrence in the food web, and general high presence in the environment. Ingested microplastics are accumulated in the digestive tract, but a large number can also be rapidly eliminated. Some authors state that the translocation of microplastics to the epithelial cells is possible, increasing the risk of microplastics transmission along the food chain. However, as seen in our study, a surface imaging approach (2D) is probably not enough to confirm the internalization of particles and avoid misinterpretation. In fact, while some microplastic particles were detected in the epithelium by 2D Raman imaging, further 3D Raman imaging analysis demonstrated that those particles were dragged from the lumens to the epithelium during sample preparation due to the blade drag effect of the cryotome, and subsequently located on the surface of the analyzed cryosection, discarding the translocation to the epithelial cells. This effect can also happen when the samples are fortuitously contaminated during sample preparation. Several research articles that use similar analytical techniques have shown the presence of microplastics in different types of tissue. It is not our intention to put such results in doubt, but the present work points out the necessity of appropriate three-dimensional analytical methods including data interpretation and the need to go a step further than just surface imaging analysis.

Geochemical characterization of the Martian analogues Enekuri and Fruiz, located in the Basque-Cantabrian Basin, by spectroscopic techniques.

This work presents the geochemical characterization of two Martian analogues located in the Basque-Cantabrian Basin: Enekuri and Fruiz. In contrast to previous works carried out on the coastline analogues Meñakoz and Armintza (Biscay, Spain), these new outcrops are not in contact with sea-water nowadays. Hence, the weathering processes observed in Enekuri and Fruiz (inland) are different from those observed in Armintza and Meñakoz (coastline). In this way, among all the mineral phases found the only ones in common between inland and coastline outcrops are albite and chlorites, minerals that were formed in aqueous conditions. Understanding the differences presented in both types of outcrops could help to interpret the future results from the missions Mars2020 and the ExoMars2022, since coastline outcrops are affected by sea-water weathering and inland outcrops are altered by the high biological activity.

Compositionally and density stratified igneous terrain in Jezero crater, Mars.

Before Perseverance, Jezero crater's floor was variably hypothesized to have a lacustrine, lava, volcanic airfall, or aeolian origin. SuperCam observations in the first 286 Mars days on Mars revealed a volcanic and intrusive terrain with compositional and density stratification. The dominant lithology along the traverse is basaltic, with plagioclase enrichment in stratigraphically higher locations. Stratigraphically lower, layered rocks are richer in normative pyroxene. The lowest observed unit has the highest inferred density and is olivine-rich with coarse (1.5 millimeters) euhedral, relatively unweathered grains, suggesting a cumulate origin. This is the first martian cumulate and shows similarities to martian meteorites, which also express olivine disequilibrium. Alteration materials including carbonates, sulfates, perchlorates, hydrated silicates, and iron oxides are pervasive but low in abundance, suggesting relatively brief lacustrine conditions. Orbital observations link the Jezero floor lithology to the broader Nili-Syrtis region, suggesting that density-driven compositional stratification is a regional characteristic.

Thermodynamic and spectroscopic speciation to explain the blackening process of hematite formed by atmospheric SO2 impact: the case of Marcus Lucretius House (Pompeii).

After many decades exposed to a polluted environment, in some areas of Marcus Lucretius House, there are clear signs that plasters and hematite pigments are suffering deterioration. In the exhaustive analysis of the black layer covering the red pigment hematite it was possible to identify magnetite (Fe(3)O(4)) as responsible for the black colour, which always appears in combination with gypsum. Thermodynamic modelling stated that the presence of gypsum as well as the transformation of hematite into magnetite is a consequence of the attack of atmospheric SO(2).

Are these liquids explosive? Forensic analysis of confiscated indoor fireworks.

Complete forensic analysis of several confiscated liquids and gels putatively used as firework components was achieved by combining Raman, FTIR spectroscopy, and scanning electron microscopy combined with energy-dispersive spectroscopy (SEM-EDS). The chemical composition of the liquids was consistent with their use as indoor fireworks. Alcohols (methanol and isopropyl alcohol) were used to solubilise compounds producing coloured flames. Boric acid, recently introduced in the list of Substances of Very High Concern (SVHC) for the REACH Regulation of the European Union, was found in one of the samples.

Spectroscopic-assisted archaeometric studies to determine the production technology of the VI BC Zeus Enthroned statue (Paestum, Italy) and Pre-Roman technology transfer.

This work summarizes the spectroscopic-assisted archaeometric study of the most important terracotta statue of Poseidonia-Paestum (Italy), the so-called Zeus Enthroned (VI sec. BC). The selected analytical strategy combines the mineralogical and molecular information provided by X-Ray diffraction (XRD) and Raman analysis with the elemental data obtained from X-Ray fluorescence (XRF) and Scanning Electron Microscopy coupled to Energy Dispersive Spectrometry (SEM/EDS). To shed light on the raw materials used to create and decorate this unique artwork, the analytical results gathered in this study helped disclosing the applied production technology. As suggested by the detected mineral assemblages, the body was prepared in two steps, using calcareous clay (CC) rich in Mg- and Fe- minerals as raw materials. The inner core and the outer depurated layers were both fired in oxidizing conditions but reaching different temperatures (≥900 °C and 850-900 °C respectively). The statue was decorated by firing manganese- (jacobsite MnFe2O4) and iron- (hematite Fe2O3) oxides in oxidizing conditions. Knowing that the decoration techniques based on the use of Mn-oxides were mastered by Etruscans rather than by Ancient Greeks, the obtained results suggest a transfer of production technology across borders, thus providing an additional clue about the flourishing commercial and cultural exchanges occurred between Greek colonies and Italic pre-Roman societies.

Development of a novel method for the in-situ dechlorination of immovable iron elements: optimization of Cl- extraction yield through experimental design.

The conservation of iron objects exposed to marine aerosol is threatened by the formation of akaganeite, a highly unstable Cl-bearing corrosion phase. As akaganeite formation is responsible of the exfoliation of the rust layer, chlorides trigger a cyclic alteration phenomenon that often ends with the total consumption of the iron core. To prevent this degradation process, movable iron elements (e.g. archaeometallurgical artefacts) are generally immersed in alkaline dechlorination baths. Aiming to transfer this successful method to the treatment of immovable iron objects, we propose the in-situ application of alkaline solutions through the use of highly absorbent wraps. As first step of this novel research line, the present work defines the best desalination solution to be used and optimizes its extraction yield. After literature review, a screening experimental design was performed to understand the single and synergic effects of common additives used for NaOH baths. Once the most effective variables were selected, an optimization design was carried out to determine the optimal conditions to be set during treatment. According to the experimental work here presented, the use of 0.7 M NaOH solutions applied at high temperatures (above 50 °C) is recommended. Indeed, these conditions enhance chloride extraction and iron leaching inhibition, while promoting corrosion stabilization.