Optimal Sample Preparation for the Analysis of Micrometric Heterogeneous Samples

Beltrán, Victoria; Salvadó, Nati; Butí, Salvador; Cinque, Gianfelice; Wehbe, Katia; Pradell, Trinitat

doi:10.1021/acs.analchem.5b01997

Cited by 11 publications

(10 citation statements)

References 26 publications

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“…The combination of these analytical techniques can overcome the analytical challenge and provide essential information about the old fungi activity leading to a better understanding of the relationship between fungi and the paint substratum. Infrared spectroscopy was used as a first step in the identification of the nature of those substances and the LMWOA anions were determined using the whole of a sample using GC-MS. Their distribution in the layers was resolved using the micro-analytical techniques 8,9 . Synchrotron radiation (SR) thanks to the high brilliance, energy selection and collimation of the beam enables obtaining spectra with a very high signal to noise ratio on areas as small as a few micrometres.…”

Section: Introductionmentioning

confidence: 99%

Low molecular weight organic acid salts, markers of old fungi activity in wall paintings

et al. 2016

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Micro Infrared Spectroscopy (µSR-FTIR) and X-Ray diffraction (µSR-XRD) with synchrotron light, Gas Chromatography/Mass Spectrometry (CG/MS), Optical Microscopy (OM) and Scanning Electron Microscopy (SEM/EDS) were used to identify and obtain the distribution of complex mixtures of calcium salts of low molecular weight organic acids (LMWOA) in micro-layered micro-samples. Filamentous fungi produce LMWOA that can react with metal cations producing stable salts. These substances were found in the dark spots covering the surfaces of Saint Michael's Chapel wall paintings of the Royal Monastery of Pedralbes in Barcelona linking them to old fungi activity. The presence of glycerol likewise related to the fungi activity is also identified in the layers.

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Section: Introductionmentioning

confidence: 99%

Low molecular weight organic acid salts, markers of old fungi activity in wall paintings

et al. 2016

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“…Finally, the spectra of the epoxy resin used to embed the sample can also be discriminated. It should be mentioned that the most intense bands (1512 cm −1 related to the C=C stretching of the aromatic groups and at 1247 cm −1 related to the C‐O deformation [38] ) are also noticeable in the other displayed μSR‐FTIR spectra: this is probably explained by the spot size of this technique, which is too big to select only regions inside of the sample. Consequently, the analyzed areas usually include regions outside the paint fragment, where there is only embedding medium, or regions close to the edge of the sample, where the embedding medium has been infiltrated.…”

Section: Resultsmentioning

confidence: 99%

Nanoscale Analysis of Historical Paintings by Means of O‐PTIR Spectroscopy: The Identification of the Organic Particles in L′Arlésienne (Portrait of Madame Ginoux) by Van Gogh

et al. 2021

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Optical‐photothermal infrared (O‐PTIR) spectroscopy is a recently developed technique that provides spectra comparable to traditional transmission FTIR spectroscopy with nanometric spatial resolution. Hence, O‐PTIR is a promising candidate for the analysis of historical paintings, as well as other cultural heritage objects, but its potential has not yet been evaluated. This work presents the first application of O‐PTIR to the analysis of cultural heritage, and in particular to an extremely small fragment from Van Gogh's painting L′Arlésienne (portrait of Madame Ginoux). The striking results obtained, including the detection of geranium lake pigments as well as the complete analysis of the stratigraphy, failed with other state‐of‐the‐art techniques, highlight the potential of this method. The integration of O‐PTIR to the study of cultural heritage opens to the possibility of decreasing the amount of sample extracted, therefore contributing to the preservation of the integrity of artworks while providing a complete characterization of the materials.

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“…Cross sections. Polished cross sections and thin cross sections of the samples were obtained for analysis [10,11]. Small fragments of the samples (a few hundred micrometers in size) were first embedded in epoxy resin and subsequently microtomed.…”

Section: Samples and Sample Preparationmentioning

confidence: 99%

“…Small fragments of the samples (a few hundred micrometers in size) were first embedded in epoxy resin and subsequently microtomed. In some samples, a thin gold protection layer was applied on the surface before embedding the sample to avoid the contamination of the sample by the epoxy resin [11]. 2 µm and 20 µm thick cross sections were cut for the infrared and X-ray diffraction measurements respectively.…”

Section: Samples and Sample Preparationmentioning

confidence: 99%

“…With regard to the identification of the nature of the compounds present Micro Infrared Spectroscopy (μ-FTIR), Micro Raman Spectroscopy (μ-Raman) and Micro X-ray Diffraction (μ-XRD) are among the most commonly employed. The use of synchrotron radiation (SR) adds micro-focusing capability and high quality data due to the brightness and high signal to noise ratio and may be critical for the success of the analysis [9][10][11][12].…”

Section: Introductionmentioning

confidence: 99%

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Microanalytical study of luster glazed gilding and silvering from Baroque altarpieces

Salvadó

Butí

Clemente

et al. 2017

Pure and Applied Chemistry

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Lustering, a technique which involved the application of coloured translucent glazes over gilding and silvering was widely used to enrich and decorate altarpieces in the Baroque period. The decorations consist of a micrometric multilayered structure including several color glazes, metallic leaves andboleapplied over a plaster ground. The collection of Baroque altarpieces, the oldest dating 1671 and the newest 1775 from the cathedral of Tortosa (Catalonia), is a perfect case of study of the materials used and the techniques employed throughout the period. Further information is obtained from the analysis of the reaction and aging compounds resulting from the interaction among the compounds present in the layers and between the different layers. A combination of sensitive analytical techniques, Synchrotron based μ-XRD and μ-IR and SEM-EDS which enabled the luster samples to undergo analysis without altering their original layered microstructure were selected. The nature of the compounds used to produce the yellow, green, red and blue glazes (pigments, pigment lakes and resins), metallic leaves and boles is presented. Relevant information from historical and conservation viewpoints about the origin and nature of the materials used, the making of the lusters and their reactivity and aging are also discussed.

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Optimal Sample Preparation for the Analysis of Micrometric Heterogeneous Samples

Cited by 11 publications

References 26 publications

Low molecular weight organic acid salts, markers of old fungi activity in wall paintings

Low molecular weight organic acid salts, markers of old fungi activity in wall paintings

Nanoscale Analysis of Historical Paintings by Means of O‐PTIR Spectroscopy: The Identification of the Organic Particles in L′Arlésienne (Portrait of Madame Ginoux) by Van Gogh

Microanalytical study of luster glazed gilding and silvering from Baroque altarpieces

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