NMR and other molecular and elemental spectroscopies for the characterization of samples from an outdoor mural painting by Siqueiros

• Published in: Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy Vol. 274; p. 121073
• Main Authors: Mejía-González, Adrián, Jáidar, Yareli, Zetina, Sandra, Aguilar-Rodríguez, Pablo, Ruvalcaba-Sil, J.L., Esturau-Escofet, Nuria
• Format: Journal Article
• Language: English
• Published: England Elsevier B.V 05.06.2022
• Subjects: Acrylic paints; FORS; FTIR-ATR; Nitrocellulose paint; Nuclear Magnetic Resonance; Py-CG/MS; Nitrocellulose paint; Nuclear Magnetic Resonance; FTIR-ATR; FORS; Py-CG/MS; Acrylic paints
• ISSN: 1386-1425; 1873-3557
• DOI: 10.1016/j.saa.2022.121073

[Display omitted] •High resolution NMR as a novel technique in heritage material characterization.•Identification of acrylic and nitrocellulose binders in Siqueiros mural.•Chemical identification by the combination of FORS, FTIR-ATR, Py-GC/MS and NMR.•Analysis of stratigraphic heritage samples by optical microscopy and SEM-EDS.•Characterization of Siqueiros outdoor mural painting technique in 1960–1970́s. This study presents the use of high resolution Nuclear Magnetic Resonance (NMR) as an outstanding tool for identifying with accuracy the structure of the polymers used as binders and the additives used as plasticizers in samples from a mural painted by David Alfaro Siqueiros between 1964 and 1972, an important period in which his artistic production has not been previously studied. Additionally, the presence of some organic pigments was detected. The mural Trazos de composición piramidal currently located outside of Siqueiros' studio La Tallera, in Cuernavaca Morelos (Mexico) was an artistic experiment done by Siqueiros to test outdoor painting. Eight micro-samples of paint were thoroughly analyzed by Optical Microscopy (OM), Scanning Electron Microscopy – Energy Dispersive X-Ray Spectroscopy (SEM-EDS), Fiber Optics Reflectance Spectra (FORS), Transmission Fourier Transform Infrared Spectroscopy with Attenuated Total Reflectance mode (FTIR-ATR) and Pyrolysis-Gas Chromatography/Mass Spectrometry (Py-GC/MS). Through these studies, contrasted with an historical investigation, we demonstrate that the samples present a multi-layered and complex painting system because Siqueiros made at least two versions of the painting. The multi-layered structure and the variable composition of each layer challenged the application of several analytical methodologies traditionally used for cultural heritage materials. In one sample, each layer was separated and they were studied in detail by FTIR-ATR, Py-GC/MS and NMR. This study revealed the presence of two main binders: acrylics in the first layers and nitrocellulose in the last one, also some phthalates and fatty acids were detected as additives. Inorganic pigments and fillers were identified as titanium dioxide and iron red oxide as well as diatoms and carbonates. The main contribution of this study, where NMR spectroscopy was applied for the first time in modern mural painting analysis, is the characterization of the materials used by Siqueiros during the last years of his artistic production.