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In this work, colloidal gold nanoparticles (AuNPs) stabilized into a chitosan matrix were prepared using a green route. The synthesis was carried out by reducing Au(III) to Au(0) in an aqueous solution of chitosan and different organic acids (i.e., acetic, malonic, or oxalic acid). We have demonstrated that by varying the nature of the acid it is possible to tune the reduction rate of the gold precursor (HAuCl(4)) and to modify the morphology of the resulting metal nanoparticles. The use of chitosan, a biocompatible and biodegradable polymer with a large number of amino and hydroxyl functional groups, enables the simultaneous synthesis and surface modification of AuNPs in one pot. Because of the excellent film-forming capability of this polymer, AuNPs-chitosan solutions were used to obtain hybrid nanocomposite films that combine highly conductive AuNPs with a large number of organic functional groups. Herein, Au-chitosan nanocomposites are successfully proposed as sensitive and selective electrochemical sensors for the determination of caffeic acid, an antioxidant that has recently attracted much attention because of its benefits to human health. A linear response was obtained over a wide range of concentration from 5.00 × 10(-8) M to 2.00 × 10(-3) M, and the limit of detection (LOD) was estimated to be 2.50 × 10(-8) M. Moreover, further analyses have demonstrated that a high selectivity toward caffeic acid can be achieved without interference from catechin or ascorbic acid (flavonoid and nonphenolic antioxidants, respectively). This novel synthesis approach and the high performances of Au-chitosan hybrid materials in the determination of caffeic acid open up new routes in the design of highly efficient sensors, which are of great interest for the analysis of complex matrices such as wine, soft drinks, and fruit beverages.

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Since the 18th century many analytical methods have been used to identify the chemical composition of archaeological artefacts, the provenance of the raw materials and the technical aspects of the manufacturing process. These techniques generally probe the bulk chemical and structural features of the objects and overlook surface characteristics often essential for understanding the manufacturing techniques and the ageing processes. This work describes the contribution of x-ray photoelectron spectroscopy (XPS) combined with bulk analytical techniques such as scanning electron microscopy + energy − dispersive spectrometry (SEM + EDS), inductively coupled plasma mass spectrometry (ICPMS) and x-ray diffraction (XRD) by discussing the origin of the embrittlement of some selected series of silver Republican Roman coins and the study of the microchemical nature of black and coral red glosses on Attic figured vases. The results show that XPS, if allowance is made for contamination or unrepresentative or non-homogeneous samples, complements the existing bulk analytical techniques and can provide detailed information about the surface chemical nature of the archaeological objects, as well as about their present state, and lead to recommendations for restoration and preservation.