Badania składu pierwiastkowego zapraw dziewiętnastowiecznych obrazów – nowe możliwości wspomagania datowania i atrybucji na podstawie nieinwazyjnych badań in situ z wykorzystaniem przenośnego spektrometru XRF

Till present the main tool among physical-chemical analyses of the 19th century paintings supporting dating and authentication was the pigment identification. The paper presents results of research enabling preliminary chronological assessment of the evolution of chemical composition of primings, basing on non-invasive examination by means of XRF with measurements executed from the backside through the canvas and parallel on tacking margins, with possibility of non-invasive identification of two layered grounds in this way. Non-invasiveness and easy applicability of the method as well as broadening the statistical sources makes the portable XRF primings recognition promising tool for material-chronological examination of the 19th century paintings.Dotychczas wśród analiz fizykochemicznych malarstwa XIX‐wiecznego jako narzędzie wspomagające datowanie i atrybucję wskazywano głównie identyfikację pigmentów. Tekst prezentuje rezultaty badań pozwalające na wstępne odniesienie chronologiczne do zarysowanej ewolucji składu zapraw w tym okresie, w oparciu o nieinwazyjne badania XRF nowatorską analizą od odwrocie przez płótno i na krajkach z umożliwieniem identyfikacji także zapraw dwuwarstwowych. Nieinwazyjność i łatwość aplikacji metody oraz ciągłe poszerzanie próby statystycznej czyni z badania obiecujące narzędzie znacząco pogłębiające dotychczas dostępne odniesienia chronologicznomateriałoznawcze dla XIX wieku

Przykłady wykorzystania analizy SEM-EDX do badań zabytkowych skór garbowanych związkami metali

Application of the SEM-EDX technique for determination of elements in alum as well as chrome tanner leathers discussed in the article. These leathers are found in museum, library and archival collections. Alum tanner leathers are known since ancient period while chrome tanner leathers for 19th c. Examples of the use of leather samples examination and range possibilities created by the technique presented. Additional substances (not being tannins) to be found in leather structure ad surface such as auxiliary agents, decorative layers, contaminations, focused on. The SEM-EDX technique is useful not only for characterization of elements composition of leathers, but also contributes to preservation of cultural heritage by giving possibilities of planning conservation treatments and examining influence of conservation chemicals on leathers

Żółte barwniki organiczne w XIX-wiecznych farbach Jana Matejki – identyfikacja substancji barwiących, nośników oraz wypełniaczy

Natural organic dyes can be found in many objects of cultural heritage. Identification of coloring substances present in historical paints provides relevant information for a wide range of specialists involved in art science. Determination of the composition of paints allows application of appropriate procedures for restoration and conservation of historical works of art. This information enables treatment in accordance with the ideological and esthetic decisions of the authors. The complexity of the chemical composition of art paints, which, apart from organic dyes can also include inorganic pigments, binders and other additives, hinders isolation and identification of its individual components. Nowadays, there are several analytical techniques and methods for extraction and identification of organic dyes, each of them has its limitations, however. For that reason, the development of the universal methodology for the analysis of colorant composition in art paints remains a challenge for chemists. In present work, an analytical protocol for identification of yellow dyes using reversed phase liquid chromatographymass spectrometry with atmospheric pressure electrospray ionization (LC-ESI/ /MS) is presented. The developed method was successfully applied to identification of the main components of Indian Yellow, weld (Reseda luteola L.), buckthorn berries (Rhamnus) and madder lake (madder plant’s root) extracts, in the historical oil paints from tubes of Richard Ainès company, formerly Mulard, owned before him by recognizable French art materials supplier Eduard. The recognition of paints composition was broadened by identification of non organic compounds – carriers of the dye: aluminum hydroxide, tin chloride, chalk, as well as filler like silica and or lead white. Researched samples of painting materials belonged to 19th century famous Polish painter Jan Matejko (1839–1893) and will be very helpful in understanding paintings of him and of his contemporaries

An Easy and Ecological Method of Obtaining Hydrated and Non-Crystalline WO3−x for Application in Supercapacitors

In this work, we report the synthesis of hydrated and non-crystalline WO3 flakes (WO3−x) via an environmentally friendly and facile water-based strategy. This method is described, in the literature, as exfoliation, however, based on the results obtained, we cannot say unequivocally that we have obtained an exfoliated material. Nevertheless, the proposed modification procedure clearly affects the morphology of WO3 and leads to loss of crystallinity of the material. TEM techniques confirmed that the process leads to the formation of WO3 flakes of a few nanometers in thickness. X-ray diffractograms affirmed the poor crystallinity of the flakes, while spectroscopic methods showed that the materials after exfoliation were abundant with the surface groups. The thin film of hydrated and non-crystalline WO3 exhibits a seven times higher specific capacitance (Cs) in an aqueous electrolyte than bulk WO3 and shows an outstanding long-term cycling stability with a capacitance retention of 92% after 1000 chronopotentiometric cycles in the three-electrode system. In the two-electrode system, hydrated WO3−x shows a Cs of 122 F g−1 at a current density of 0.5 A g−1. The developed supercapacitor shows an energy density of 60 Whkg−1 and power density of 803 Wkg−1 with a decrease of 16% in Csp after 10,000 cycles. On the other hand, WO3−x is characterized by inferior properties as an anode material in lithium-ion batteries compared to bulk WO3. Lithium ions intercalate into a WO3 crystal framework and occupy trigonal cavity sites during the electrochemical polarization. If there is no regular layer structure, as in the case of the hydrated and non-crystalline WO3, the insertion of lithium ions between WO3 layers is not possible. Thus, in the case of a non-aqueous electrolyte, the specific capacity of the hydrated and non-crystalline WO3 electrode material is much lower in comparison with the specific capacity of the bulk WO3-based anode material

Silicon Oxycarbide-Graphite Electrodes for High-Power Energy Storage Devices

Herein we present a study on polymer-derived silicon oxycarbide (SiOC)/graphite composites for a potential application as an electrode in high power energy storage devices, such as Lithium-Ion Capacitor (LIC). The composites were processed using high power ultrasound-assisted sol-gel synthesis followed by pyrolysis. The intensive sonication enhances gelation and drying process, improving the homogenous distribution of the graphitic flakes in the preceramic blends. The physicochemical investigation of SiOC/graphite composites using X-ray diffraction, 29Si solid state NMR and Raman spectroscopy indicated no reaction occurring between the components. The electrochemical measurements revealed enhanced capacity (by up to 63%) at high current rates (1.86 A g−1) recorded for SiOC/graphite composite compared to the pure components. Moreover, the addition of graphite to the SiOC matrix decreased the value of delithiation potential, which is a desirable feature for anodes in LIC

Silicon Oxycarbide-Graphite Electrodes for High-Power Energy Storage Devices

Herein we present a study on polymer-derived silicon oxycarbide (SiOC)/graphite composites for a potential application as an electrode in high power energy storage devices, such as Lithium-Ion Capacitor (LIC). The composites were processed using high power ultrasound-assisted sol-gel synthesis followed by pyrolysis. The intensive sonication enhances gelation and drying process, improving the homogenous distribution of the graphitic flakes in the preceramic blends. The physicochemical investigation of SiOC/graphite composites using X-ray diffraction, ²⁹Si solid state NMR and Raman spectroscopy indicated no reaction occurring between the components. The electrochemical measurements revealed enhanced capacity (by up to 63%) at high current rates (1.86 A g⁻¹) recorded for SiOC/graphite composite compared to the pure components. Moreover, the addition of graphite to the SiOC matrix decreased the value of delithiation potential, which is a desirable feature for anodes in LIC

Effects of Ozone Dissolved in Water on the Physicochemical Properties of Activated Carbons Applied in Drinking Water Treatment

The results of treating commercial granulated activated carbons with ozone, both gaseous and dissolved in water, were analyzed. The original carbons (Filtrasorb-300 and Carbsorb-38) were carefully flushed with distilled water to remove any water-soluble impurities. For comparison, each of the washed activated carbons was treated separately with aqueous hydrogen peroxide. The following procedures were applied to assess the effects of contact between each carbon and the oxidizing agents: thermogravimetry, alkalimetry, voltammetry, EDX and FT-IR methods to illustrate changes in the surface chemistry, and nitrogen low-temperature adsorption to show up any possible changes in the porous structure. Ozone dissolved in water exhibited the lowest oxidative strength — EDX and FT-IR spectroscopy revealed only a slight oxidation of the Filtrasorb-300 surface layer. Despite its smaller specific area, this carbon surface exhibited greater roughness and was more susceptible to oxidation. The liquid-phase adsorption isotherms of p -chlorophenol from aqueous solution onto this carbon showed that surface oxygen reduced the extent of adsorption. The experimental data were best fitted by the Langmuir isotherm model

Understanding the capacitance of thin composite films based on conducting polymer and carbon nanostructures in aqueous electrolytes

In this work electrochemical performance of thin composite films consisted of poly(3,4-ethylenedioxythiophene) (PEDOT), graphene oxide (G0x) and oxidized multiwalled carbon nanotubes (oxMWCNTs) is investigated in various sulphates (Li2SO4, Na2SO4, K2SO4, MgSO4) and acidic (H2SO4) electrolytes. Capacitance values, rate capability and cycling stability achieved for the composite layers are correlated with the electrolytes' properties such as the conductivity, viscosity, cation size and pH. The highest capacitance values are achieved in acidic solution (98.6 mF cm(-2) at 1 mA cm(-2)), whereas cycling stability is better in neutral electrolytes (88.4% of initial capacitance value after 10'000 cycles recorded for symmetric supercapacitor in 0.5 M MgSO4 solution). Diffusion controlled and non-diffusion controlled capacitance contributions are calculated and the results are discussed considering various ranges of sweep rates taken into account in the linear fitting and extrapolation of parameters

Pyrolized Diatomaceous Biomass Doped with Epitaxially Growing Hybrid Ag/TiO₂ Nanoparticles: Synthesis, Characterisation and Antibacterial Application

In the pursuit of innovative solutions for modern technologies, particularly in the design and production of new micro/nanostructured materials, microorganisms acting as “natural microtechnologists” can serve as a valuable source of inspiration. This research focuses on harnessing the capabilities of unicellular algae (diatoms) to synthesize hybrid composites composed of AgNPs/TiO2NPs/pyrolyzed diatomaceous biomass (AgNPs/TiO2NPs/DBP). The composites were consistently fabricated through metabolic (biosynthesis) doping of diatom cells with titanium, pyrolysis of the doped diatomaceous biomass, and chemical doping of the pyrolyzed biomass with silver. To characterize the synthesized composites, their elemental and mineral composition, structure, morphology, and photoluminescent properties were analysed using techniques such as X-ray diffraction, scanning and transmission electron microscopy, and fluorescence spectroscopy. The study revealed the epitaxial growth of Ag/TiO2 nanoparticles on the surface of pyrolyzed diatom cells. The antimicrobial potential of the synthesized composites was evaluated using the minimum inhibitory concentration (MIC) method against prevalent drug-resistant microorganisms, including Staphylococcus aureus, Klebsiella pneumonia, and Escherichia coli, both from laboratory cultures and clinical isolates

Electrochemically Obtained TiO2/CuxOy Nanotube Arrays Presenting a Photocatalytic Response in Processes of Pollutants Degradation and Bacteria Inactivation in Aqueous Phase

TiO2/CuxOy nanotube (NT) arrays were synthesized using the anodization method in the presence of ethylene glycol and different parameters applied. The presence, morphology, and chemical character of the obtained structures was characterized using a variety of methods—SEM (scanning electron microscopy), XPS (X-ray photoelectron spectroscopy), XRD (X-ray crystallography), PL (photoluminescence), and EDX (energy-dispersive X-ray spectroscopy). A p-n mixed oxide heterojunction of Ti-Cu was created with a proved response to the visible light range and the stable form that were in contact with Ti. TiO2/CuxOy NTs presented the appearance of both Cu2O (mainly) and CuO components influencing the dimensions of the NTs (1.1–1.3 µm). Additionally, changes in voltage have been proven to affect the NTs’ length, which reached a value of 3.5 µm for Ti90Cu10_50V. Degradation of phenol in the aqueous phase was observed in 16% of Ti85Cu15_30V after 1 h of visible light irradiation (λ > 420 nm). Scavenger tests for phenol degradation process in presence of NT samples exposed the responsibility of superoxide radicals for degradation of organic compounds in Vis light region. Inactivation of bacteria strains Escherichia coli (E. coli), Bacillus subtilis (B. subtilis), and Clostridium sp. in presence of obtained TiO2/CuxOy NT photocatalysts, and Vis light has been studied showing a great improvement in inactivation efficiency with a response rate of 97% inactivation for E. coli and 98% for Clostridium sp. in 60 min. Evidently, TEM (transmission electron microscopy) images confirmed the bacteria cells’ damage