The identification of archaeological biomarkers is one of the main objectives of analytical chemistry in the archaeological field. However, no information is currently available on biomarkers able to unambiguously indicate the presence of olive oil, a cornerstone of Mediterranean ancient societies lifestyle, in an organic residue. This study aims to bridge this gap by a thorough characterization of the degradation products of extra-virgin olive oils (EVOOs) resulting from in-lab thermal oxidative treatments, with the primary goal of revealing potential archaeological biomarkers for olive oil. Thirty-three EVOOs sourced from eleven different monocultivars across five Italian regions (Sicily, Apulia, Lazio, Tuscany, and Liguria) and Spain, were analyzed before and after thermal oxidation. In addition, an identical thermal treatment was employed on pure triglyceride standards (triolein, trilinolein, and tristearin), due to the high concentration of their fatty acids in EVOO discerning their degradation patterns. A combination of analytical strategies was employed, including HPLC-MS and HPLC-ELSD for the complete evaluation of the intact lipids (triglycerides, diglycerides, and their oxidative species) in olive oils before and after oxidation, and HS-SPME-GC-MS and GC-FID for the characterization of secondary oxidation products formed by the thermal treatment. In addition, to elucidate the fatty acid distribution in the oxidized EVOOs by GC-MS and GC-FID techniques a derivatization step was performed to convert lipid compounds into trimethylsilyl (TMS) derivatives. A chemometric approach was used to thoroughly interpret the data obtained from intact and oxidized samples. This comprehensive investigation sheds light on the chemical transformations of EVOOs under thermal oxidative conditions and indicates mono-carboxylic acids such as pentanoic, hexanoic, heptanoic, octanoic, nonanoic, and decanoic acids as potential archaeological biomarkers for the presence of lipid substances coming from olive oil in archaeological organic residues. Finally, lipid contents from twenty-four real archaeological samples, grouped in amphorae (10), unguentaria (5), and lamps (9), excavated from the Roman domus of Villa San Pancrazio in Taormina (Italy), were determined. The analytical results obtained from amphorae samples revealed the presence of the selected olive oil-specific archaeological biomarkers, an information extremely interesting considering that this type of amphorae have so far been solely associated with the storage of wine.

This study refers to the archaeometric analysis of ceramic fragments found in archaeological excavations around slave quarters of Colégio dos Jesuítas and São Bento plantations, both located in Campos dos Goytacazes - RJ. The question whether handmade ceramics were produced by the slaves themselves or acquired through local trade networks is an open and important question in the African diaspora. Samples of clay sources and the ceramic fragments, were analyzed using the EDXRF technique with the aid of multivariate statistical analysis.

Raman spectroscopic analysis of the pigments on an Italian painting described as a \"Full Length Portrait of a Gentleman\", known also as the \"Malatesta\", and attributed to the Renaissance period has established that these are consistent with the historical research provenance undertaken earlier. Evidence is found for the early 19th Century addition of chrome yellow to highlighted yellow ochre areas in comparison with a similar painting executed in 1801 by Sir Thomas Lawrence of John Kemble in the role of Hamlet, Prince of Denmark. The Raman data are novel in that no analytical studies have previously been made on this painting and reinforces the procedure whereby scientific analyses are accompanied by parallel historical research.

Prussian blue, a hydrated iron(III) hexacyanoferrate(II) complex, is a synthetic pigment discovered in Berlin in 1704. Because of both its highly intense color and its low cost, Prussian blue was widely used as a pigment in paintings until the 1970s. The early preparative methods were rapidly recognized as a contributory factor in the fading of the pigment, a fading already known by the mid-eighteenth century. Herein two typical eighteenth-century empirical recipes have been reproduced and the resulting pigment analyzed to better understand the reasons for this fading. X-ray absorption and Mössbauer spectroscopy indicated that the early syntheses lead to Prussian blue together with variable amounts of an undesirable iron(III) product. Pair distribution functional analysis confirmed the presence of nanocrystalline ferrihydrite, Fe10O14(OH)2, and also identified the presence of alumina hydrate, Al10O14(OH)2, with a particle size of ∼15 Å. Paint layers prepared from these pigments subjected to accelerated light exposure showed a tendency to turn green, a tendency that was often reported in eighteenth- and nineteenth-century books. The presence of particles of hydrous iron(III) oxides was also observed in a genuine eighteenth-century Prussian blue sample obtained from a polychrome sculpture.