Another beauty of analytical chemistry: chemical analysis of inorganic pigments of art and archaeological objects

[EN] This lecture text shows what fascinating tasks analytical chemists face in Art Conservation and Archaeology, and it is hoped that students reading it will realize that passions for science, arts or history are by no means mutually exclusive. This study describes the main analytical techniques used since the eighteenth century, and in particular, the instrumental techniques developed throughout the last century for analyzing pigments and inorganic materials, in general, which are found in cultural artefacts, such as artworks and archaeological remains. The lecture starts with a historical review on the use of analytical methods for the analysis of pigments from archaeological and art objects. Three different periods can be distinguished in the history of the application of the Analytical Chemistry in Archaeometrical and Art Conservation studies: (a) the "Formation'' period (eighteenth century1930), (b) the "Maturing'' period (1930-1970), and (c) the "Expansion'' period (1970-nowadays). A classification of analytical methods specifically established in the fields of Archaeometry and Conservation Science is also provided. After this, some sections are devoted to the description of a number of analytical techniques, which are most commonly used in routine analysis of pigments from cultural heritage. Each instrumental section gives the fundamentals of the instrumental technique, together with relevant analytical data and examples of applications.Financial support is gratefully acknowledged from Spanish ‘‘I+D+I MINECO’’ projects CTQ2011-28079-CO3-01 and CTQ2014-53736-C3-1-P supported by ERDEF funds.Domenech Carbo, MT.; Osete Cortina, L. (2016). 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Preparation and infrared spectroscopic characterization of reduced-charge montmorillonite with various Li contents

A series of reduced-charge montmorillonites (RCMs) was prepared from Li-montmorillonite from Jelšový Polok (Slovakia) by heating at various temperatures (105-210°C) for 24 h. The amount of fixed Li, 0.09-0.67 per O 20 (OH) 4 , increased with increasing temperature, confirming preparation of a set of samples of variable layer charge from the same parent Li-montmorillonite by varying only the preparation temperature. Infrared spectroscopy revealed that Li was trapped in the hexagonal cavities of the tetrahedral sheet at all temperatures. Partial deprotonation of the samples, reflected in the decrease of the intensities of the OH-bending bands, was observed after treatments above 120°C. Analysis of the OH-stretching region showed Li in the previously vacant octahedra in the samples heated above 150°C. Weak inflections near 660 and 720 cm -1 confirmed development of local trioctahedral character of octahedral cations coordinated with OH groups in the sample heated at 210°C. Gradual decrease of the layer charge due to Li fixation led to a shift of the Si-O stretching hand to higher frequencies and to the appearance of new, pyrophyllite-like bands at 1120 and 419 cm -1