This study presents the analysis of seven microsamples from Untitled Mural 3, painted by David Alfaro Siqueiros between 1964 and 1972. The mural has never been restored, therefore preserving the materials used by the artist. The microsamples were analyzed using a combination of techniques: optical microscopy (OM), scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS), attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR), micro-Fourier transform infrared spectroscopy (micro-FTIR) with reflection mode, and high-resolution nuclear magnetic resonance (NMR) spectroscopy. In this work, compounds common to those identified in the analysis of the contemporary mural Trazos de composición piramidal composition were identified, such as acrylic and nitrocellulose binders, titanium white and iron red oxide as pigments, and DEHP as a plasticizer. Unexpectedly, polyvinyl acetate (PVAc) and different nitrocellulose monomers were identified, in addition to chrome yellow instead of ochre, and a predominance of quartz, asbestos, and talc as fillers, instead of carbonates. The study confirmed that Siqueiros used multiple binders in successive layers in no apparent order, providing valuable insights into his artistic techniques. The research also proved an efficient methodology for studying very small and complex samples.
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