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13. Advanced Spectroscopy for the Study of Colourants in Cultural Heritage

Author

Quintero Balbas, Diego Ivan <1988> and Mazzeo, Rocco

Subjects
CHIM/12 Chimica dell'ambiente e dei beni culturali
Abstract

Colourants are substances used to change the colour of something, and are classified in three typology of colorants: a) pigments, b) dyes, and c) lakes and hybrid pigments. Their identification is very important when studying cultural heritage; it gives information about the artistic technique, can help in dating, and offers insights on the condition of the object. Besides, the study of the degradation phenomena constitutes a framework for the preventive conservation strategies, provides evidence of the object's original appearance, and contributes to the authentication of works of art. However, the complexity of these systems makes it impossible to achieve a complete understanding using a single technique, making necessary a multi-analytical approach. This work focuses on the set-up and application of advanced spectroscopic methods for the study of colourants in cultural heritage. The first chapter presents the identification of modern synthetic organic pigments using Metal Underlayer-ATR (MU-ATR), and the characterization of synthetic dyes extracted from wool fibres using a combination of Thin Layer Chromatography (TLC) coupled to MU-ATR using AgI@Au plates. The second chapter presents the study of the effect of metallic Ag in the photo-oxidation process of orpiment, and the influence of the different factors, such as light and relative humidity. We used a combination of vibrational and synchrotron radiation-based X-ray microspectroscopy techniques: µ-ATR-FT-IR, µ-Raman, SR-µ-XRF, µ-XANES at S K-, Ag L3- and As K-edges and SR-µ-XRD. The third chapter presents the study of metal carboxylates in paintings, specifically on the formation of Zn and Pb carboxylates in three different binders: stand linseed oil, whole egg, and beeswax. We used micro-ATR-FT-IR, macro FT-IR in total reflection (rMA-FT-IR), portable Near-Infrared spectroscopy (NIR), macro X-ray Powder Diffraction (MA-XRPD), XRPD, and Gas Chromatography Mass-Spectrometry (GC-MS). For the data processing, we explored the data from rMA-FT-IR and NIR with the Principal Component Analysis (PCA).

Published
2021
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15. Noninvasive identification of turmeric and saffron dyes in proteinaceous textile fibres using Raman spectroscopy and multivariate analysis.

Author

Quintero Balbas, Diego, Lanterna, Giancarlo, Cirrincione, Claudia, Ricci, Marilena, Becucci, Maurizio, Fontana, Raffaella, and Striova, Jana

Subjects
*RAMAN spectroscopy, *WOOL, *MULTIVARIATE analysis, *FIBERS, *TURMERIC, *SAFFRON crocus, *DYES & dyeing
Abstract

We used Raman spectroscopy combined with multivariate analysis to study noninvasively naturally and artificially aged samples of silk and wool fibres dyed with turmeric and saffron dyes, following historical recipes. The Raman spectra obtained from all the samples using the two excitation lasers (785 and 1064 nm) showed the characteristic peaks of each dye and fibre. The 1064‐nm macro FT‐Raman offered more information regarding the degradation of the fibre substrate, whereas the μ‐Raman at 785‐nm spectra proved more suitable in the identification of dye characteristic peaks. We also performed colorimetric measurements to evaluate the colour change upon artificial ageing and compared them with the information obtained with Raman spectroscopy. The results suggest saffron has a higher lightfastness than turmeric and that silk fibres suffer higher fading and more evident degradation than wool. Raman spectroscopy informs about the chemical composition of the colourants and fibres and their changes upon ageing without sample pretreatment. Finally, we analysed a historical wool sample coming from a 19th‐century Persian carpet, and we identified turmeric. [ABSTRACT FROM AUTHOR]

Published
2022
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16. Fluorescence Lifetime Phasor Analysis and Raman Spectroscopy of Pigmented Organic Binders and Coatings Used in Artworks.

Author

Dal Fovo, Alice, Mattana, Sara, Chaban, Antonina, Quintero Balbas, Diego, Lagarto, João Luis, Striova, Jana, Cicchi, Riccardo, and Fontana, Raffaella

Subjects
RAMAN spectroscopy, ORGANIC coatings, FLUORIMETRY, FLUORESCENCE, BINDING agents, SURFACE coatings
Abstract

Fluorescence analysis of materials used as binders and coatings in artworks is often hampered by numerous factors, leading to uncertainties in data interpretation. Fluorescence lifetime (FL) measurements enable improvement of the specificity with respect to steady-state measurements by resolving the decay dynamics of the fluorophore emissions. In this work, layers of natural resin, oil, and wax—in pure form, pigmented, in mixtures, and spread on different substrates—were analyzed using a compact, portable, fiber-based FL instrument. FL data were processed via the phasor method and integrated with Raman spectroscopy to obtain complementary chemical information on the different substances. It was observed that the τ-phase of the mixtures is affected by both the pigments and the dispersing medium, and that the presence of the metal substrate contributes to changes in the FL of mixtures. The results obtained with our portable FL system combined with Raman spectroscopy pave the way for a systematic study of a larger number of materials for future in situ applications on works of art. [ABSTRACT FROM AUTHOR]

Published
2022
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18. Analytical studies on commercial artists’ colour charts from Das Deutsche Farbenbuch(1925)—identification of synthetic and natural organic colourants by Raman microscopy, surface-enhanced Raman spectroscopy and metal underlayer ATR-FTIR spectroscopy

Author

Sessa, Clarimma, Steuer, Christoph, Quintero Balbas, Diego, Sciutto, Giorgia, Prati, Silvia, and Stege, Heike

Abstract

Historical colour charts provide a rich and often well-dated reference materials source for studying the chemical composition of all kinds of commercial brands of artists’ paints. This article presents the results of an extensive analytical study of more than 80 paint hues from 11 colour charts that are included in the German standard book Das Deutsche Farbenbuchby H. Trillich (1925, Part II). Our research focused on the identification of synthetic organic pigments, whose quickly increasing significance for artists’ paints in the early twentieth century is impossible to evaluate by documentary source research alone. A stepwise procedure combining different non- or minimally invasive vibrational spectroscopy techniques—Normal Raman and Surface-Enhanced Raman spectroscopy as well as Metal Underlayer Attenuated Total Reflection Fourier-transform Infrared Spectroscopy—allowed the identification of 18 different organic colourants in artists’ watercolours, tempera and oil colours from six German manufacturers. In addition, micro-X-Ray Fluorescence spectroscopy was applied to determine the elemental pattern of substrates, fillers, and admixed inorganic pigments. In addition to a few traditional natural organic colourants (dark and rose madder lake, cochineal lake), most of the identified compounds comprised synthetic organic pigments or synthetic dyes from various chemical classes (indigo, anthraquinone, monoazo, ß-naphthol, xanthene, triarylcarbonium, nitroso, and azine compounds). Some of these have not or only rarely been reported in artists’ paints so far. Since the identified organic colourants have mainly poor to fair (only sometimes good) fastness to light according to modern standards and partially also to solvents typically used in conservation treatments, it is evident that works of art from this period should be treated keeping in mind the possible presence of such colourants, when planning both interventive treatments and preventive measures.

Published
2022
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