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Grisaille was the first paint applied on stained-glass panels, used in Europe since the twelfth century. Historical written sources described the use of iron and copper together with a high lead-silica base glass in the grisailles production. This project aims to study the evolution of the grisaille paint composition throughout time and the changes in the raw materials used in their production using non-destructive and non-invasive techniques. To achieve this objective, 23 grisaille samples dated from the 13th to the twentieth centuries from nine different countries (Portugal, Poland, United Kingdom, Sweden, Norway, Belgium, Low Countries, Germany, and France) were studied by means of micro particle-induced X-ray emission (μ-PIXE), micro energy dispersive X-ray fluorescence (μ-EDXRF), laser-induced breakdown spectroscopy (LIBS), laser-induced fluorescence (LIF), non-linear optical microscopy (NLOM) in the modality of multiphoton excitation fluorescence (MPEF) and optical microscopy (OM). The results showed that it was possible to identify compositional differences and patterns throughout the samples when compared with literature results. The preference for using copper in central and south-central European countries and the addition of new compounds (CoO, Cr2O3, MnO) as colouring agents since the nineteenth century was verified. The LIBS analyses allow the identification of boron on two samples, confirming the change of base glass components since the seventeenth century. The NLOM-MPEF showed the capability of this technique to measure the grisaille paint layers' thickness. This non-invasive multi-analytical and complementary approach proves itself efficient in identifying changes in the grisaille's composition throughout time, which can be interpreted as changes in the raw materials and manufacture used in the production of these paint materials. [ABSTRACT FROM AUTHOR]

The present work aims to study the glasses commonly named crystal glass produced in Portuguese factories from the 18th to the 20th centuries through their arcana or batch books. Recipes for colorless crystal glasses were selected, analyzed, and reproduced in the laboratory. Five recipes were chosen from the Marinha Grande arcanum, five recipes from the Gaivotas' Factory arcanum, and three recipes from the Castro and Oliveira Guerra arcanum. To characterize the composition and thermal‐physical properties of reproduced glasses, different analytical techniques were used such as micro‐energy dispersive X‐ray fluorescence, µ‐ Raman spectroscopy, differential scanning calorimetry, dilatometry, Vickers hardness, optical microscopy, and UV‐Vis absorbance spectroscopy. The selected recipes were proven viable for reproduction and the obtained glasses presented good thermal properties that allow the workability and creation of objects. It was also proven that there is a similarity in terms of chemical composition to some of the historical glasses attributed to Portuguese production in Portuguese museums. [ABSTRACT FROM AUTHOR]

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Tarnishing is produced by reaction of silver with gaseous reduced sulphur compounds from atmospheric pollution. It induces the formation of Ag 2 S crystals which produce a dark appearance. To remove sulphur tarnishing, different mechanical, chemical and electrochemical methods have been traditionally used. To assess the effect of different cleaning treatments on tarnished silver, coupons of pure and sterling silver (92% Ag/8% Cu) were subjected to six cycles of induced tarnishing and cleaning. The cleaning methods evaluated were mechanical (soft abrasives and rubber point mounted on a rotary tool); chemical (chelating and acid solutions) and electrochemical (potentiostatic reductions). Surface morphology, composition, weight, color and luminosity were evaluated by optical microscopy, scanning electron microscopy/energy dispersive X-ray spectroscopy, atomic force microscopy, X-ray photoelectron spectroscopy and colorimetry. The cleaning impact on tarnished silver depended on the cleaning procedure and the composition of silver. Mechanical treatments restored the original visual appearance of silver although they produced a significant mass loss and a fast re-tarnishing. Chemical cleaning methods were fast; nevertheless the surface appeared completely attacked. Electrochemical cleaning did not yield good result for sterling silver, but was an effective cleaning method for pure silver coupons. [ABSTRACT FROM AUTHOR]