Characterization of the glaze and in-glaze pigments of the nineteenth-century relief tiles from the Pena National Palace, Sintra, Portugal

Veiga, João Pedro; Alves, L.C.; Mirão, José; Dias, Luís; Lima, Augusta; Muralha, Vânia S. F.; Macedo, Maria Filomena

doi:10.1007/s00339-016-0214-5

Cited by 12 publications

(23 citation statements)

References 35 publications

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“…Green and amber glazes owe their colors to the presence of copper and iron, respectively, as identified in a previous study (Coentro et al, 2017). The Cu 2+ ion in a lead glaze is known to yield a “bottle-green” shade, whereas the Fe 3+ is responsible for the amber color (Molera et al, 1997; Navarro, 2003).…”

Section: Resultssupporting

confidence: 67%

“…In the present paper, we aim to discuss in more detail the mineral inclusions observed and identified in the glazes. Besides complementing the already-published µ -Raman analysis of Hispano-Moresque ceramics (Coentro et al, 2014, 2017; Zuluaga et al, 2012; Vieira Ferreira et al, 2014), new results are presented and discussed with the aim of achieving a better understanding of the technology behind these glazes.…”

Section: Introductionmentioning

confidence: 83%

“…Table 1 contains a list of the glaze samples included in this study and Table 2 contains their average chemical composition, as obtained by µ -PIXE in Coentro et al (2017). Figure 1 illustrates some of the analyzed cuerda seca and arista tile fragments.…”

Section: Methodsmentioning

confidence: 99%

“…In a previous work, the authors studied and compared several collections of Hispano-Moresque tiles (Coentro et al, 2017). The results suggested a widespread technology with glaze composition showing small differences among collections.…”

Section: Introductionmentioning

confidence: 99%

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Mineralogical Characterization of Hispano-Moresque Glazes: A µ-Raman and Scanning Electron Microscopy with X-Ray Energy Dispersive Spectrometry (SEM-EDS) Study

et al. 2018

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This work explores the combination of µ-Raman spectroscopy and scanning electron microscopy with X-ray energy dispersive spectrometry (SEM-EDS) for the study of the glazes in 15th-16th century Hispano-Moresque architectural tiles. These are high lead glazes that can be tin-opacified or transparent, and present five colors: tin-white, cobalt-blue, copper-green, iron-amber, and manganese-brown. They are generally homogenous and mineral inclusions are mostly concentrated in the glaze-ceramic interface. Through SEM-EDS, these inclusions were observed and chemically analyzed, whereas µ-Raman allowed their identification on a molecular level. K-feldspars, wollastonite and diopside were the most common compounds, as well as cassiterite agglomerates that render the glaze opaque. Malayaite was identified in green glazes, and andradite and magnesioferrite in amber glazes. Co-Ni-ferrites were identified in blue glazes, as well as Ni-Fe-olivines. Manganese-brown is the color where most compounds were identified: bustamite, jacobsite, hausmannite, braunite, and kentrolite. Through the µ-Raman analysis of different areas in large inclusions previously observed by SEM, it was possible to identify intermediate phases that illustrate the reaction process that occurs between the color-conferring compounds and the surrounding lead glaze. Furthermore, the obtained results allowed inference of the raw materials and firing temperatures used on the manufacture of these tiles.

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Section: Resultssupporting

confidence: 67%

Section: Introductionmentioning

confidence: 83%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Mineralogical Characterization of Hispano-Moresque Glazes: A µ-Raman and Scanning Electron Microscopy with X-Ray Energy Dispersive Spectrometry (SEM-EDS) Study

et al. 2018

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“…Among these methods, the most frequently applied analytical techniques are proton-induced X-ray emission (PIXE) and proton-induced γ-ray emission (PIGE). Many researchers apply them to detect historic building samples as the first step, which provide the chemical composition of various materials such as pigments [288][289][290], glasses [291,292], mortars [293,294], etc. Because Fig.…”

Section: Ion Beam Analysis Techniquesmentioning

confidence: 99%

Recent progress in instrumental techniques for architectural heritage materials

et al. 2019

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Both conservation and intervention methods must be compatible with each other and appropriate for the original building materials. Therefore, the characterization of historic building materials is indispensable for investigating chemical composition, micro-structure and morphological features to study the current condition, environmental influence and change mechanism due to natural aging or man-made decay processes. Given the great variety of chemicals which can be analyzed, complex problems related to architectural heritage materials are investigated via optimized methodologies. Among the existing techniques, optical microscopy (OM) is an inexpensive and dominating tool to obtain preliminary information on complex samples. Atomic force microscopy (AFM) can provide real three-dimensional topographies showing sample surface properties. Electron microscopes combined with energy dispersion X-ray analysis (EM-EDX) are the instruments specifically developed to acquire images of target materials at high magnification. Infrared and Raman spectroscopies are frequently used to characterize inorganic and organic compounds. Thermal analysis can rapidly and accurately measure changes in crystalline structure, dehydration and decomposition. X-ray based technologies have a wide range of applications as follows. X-ray fluorescence (XRF) is one of the most frequently used techniques for elemental analysis. X-ray diffraction (XRD) is a fast and inexpensive technique for the characterization of man-made and natural materials. X-ray photoelectron spectroscopy (XPS) is applied to quantify the valence and electronic levels of specific elements. X-ray absorption spectroscopy (XAS) is a powerful technique for detecting the electronic structure of matter. UV-visible (UV-vis) spectroscopy is also of great importance in architectural heritage, which can reveal different physicochemical mechanisms causing color. Laserinduced breakdown spectroscopy (LIBS) can effectively eliminate the pollution on the surface and detect the internal elements of the target material. Ion beam analysis can quantify trace elements with high sensitivity. Mass-based techniques are mainly applied to identify unknown organic substances at the molecular level. This review describes some classical applications of individual techniques and provides scientific support for scientists and engineers to make decisions in the context of architectural heritage.

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Raman identification of pigments and opacifiers: Interest and limitation of multivariate analysis by comparison with solid state spectroscopical approach—II. Arsenic‐based opacifiers and relation with cobalt ores

Burlot,

Vangu,

Bellot‐Gurlet

et al. 2023

J Raman Spectroscopy

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Raman analysis is a noninvasive technique that can be conducted on‐site via a mobile system. However, the presence in variable quantity of different crystalline or amorphous phases (glassy matrix, opacifiers and pigments) in the enamel leads to the partial observation of Raman signatures, signatures often not being characterized in the literature. We study here the phases observed in the white, blue and yellow/green enamels of French and Chinese objects from the 18th century and compare the effectiveness of a solid‐state spectroscopic approach (identification of the parameters determining the vibrational modes in relation to the structures) and the multivariate chemometric approach (PCA and Hierarchical Clustering), carried out on the global or partial spectra, or on the parameters extracted from the first approach. The incorporation of the spectra of neighbouring or similar phases from the literature into the corpus of processed data, in particular those obtained for phases that are not initially structurally characterized, is decisive for the quality of the results. At least four different lead arsenates are identified. The combination of visual observation of the peaks and multivariate analysis shows that the shape, position and area of the band associated with the main As‐O stretching vibration around 820 cm−1 vary according to several criteria related to production techniques specific to certain workshops. The contribution of multivariate analysis based on spectra alone appears to be very limited compared to the examination of spectroscopic parameters.

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Characterization of the glaze and in-glaze pigments of the nineteenth-century relief tiles from the Pena National Palace, Sintra, Portugal

Cited by 12 publications

References 35 publications

Mineralogical Characterization of Hispano-Moresque Glazes: A µ-Raman and Scanning Electron Microscopy with X-Ray Energy Dispersive Spectrometry (SEM-EDS) Study

Mineralogical Characterization of Hispano-Moresque Glazes: A µ-Raman and Scanning Electron Microscopy with X-Ray Energy Dispersive Spectrometry (SEM-EDS) Study

Recent progress in instrumental techniques for architectural heritage materials

Raman identification of pigments and opacifiers: Interest and limitation of multivariate analysis by comparison with solid state spectroscopical approach—II. Arsenic‐based opacifiers and relation with cobalt ores

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