61 research outputs found

    What about Phenol Formaldehyde (PF) Foam in Modern-Contemporary Art? Insights into the Unaged and Naturally Aged Material by a Multi-Analytical Approach

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    The ageing behavior of phenol formaldehyde (PF) foam, a material increasingly used in modern‐contemporary art, was investigated by a multi‐analytical approach. PF foams with open and closed‐cell structures were selected and analyzed in their unaged and naturally indoor‐aged state by employing optical microscopy (OM) and fiber optical reflectance spectroscopy (FORS) for assessing their morphology and color alteration. Micro‐Fourier transform infrared spectroscopy (Ό‐ FTIR) was used for determining chemical changes and oxidation processes, and the acidity was monitored by pH measurements. The results clearly showed the extreme sensitivity of both open and closed‐cell PF foams to conditions typically found in indoor museums. OM indicated that the cells of the foams are prone to disrupt, and a tendency towards a red color shift was observed with FORS. Ό‐FTIR revealed the formation of quinone groups resulting from oxidation reactions. Finally, a slight decrease in the acidity was found by pH measurements.The ageing behavior of phenol formaldehyde (PF) foam, a material increasingly used in modern‐contemporary art, was investigated by a multi‐analytical approach. PF foams with open-and closed‐cell structures were selected and analyzed in their unaged and naturally indoor‐aged state by employing optical microscopy (OM) and fiber optical reflectance spectroscopy (FORS) for assessing their morphology and color alteration. Micro‐Fourier transform infrared spectroscopy (Ό‐ FTIR) was used for determining chemical changes and oxidation processes, and the acidity was monitored by pH measurements. The results clearly showed the extreme sensitivity of both open-and closed‐cell PF foams to conditions typically found in indoor museums. OM indicated that the cells of the foams are prone to disrupt, and a tendency towards a red color shift was observed with FORS. Ό‐FTIR revealed the formation of quinone groups resulting from oxidation reactions. Finally, a slight decrease in the acidity was found by pH measurements

    Electrochemical Immunosensor for Detection of IgY in Food and Food Supplements

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    Immunoglobulin Y is a water-soluble protein present in high concentration in hen serum and egg yolk. IgY has applications in many fields, e.g., from food stuff to the mass production of antibodies. In this work, we have implemented an electrochemical immunosensor for IgY based on templated nanoelectrodes ensembles. IgY is captured by the templating polycarbonate and reacted with anti-IgY labeled with horseradish peroxidase. In the presence of H2O2 and methylene blue as the redox mediator, an electrocatalytic current is generated which scales with IgY concentration in the sample. After optimizing the extracting procedure, the immunosensor was applied for analysis of fresh eggs and food integrators. The data obtained with the biosensor were validated by SDS-PAGE and Western blot measurements

    Redesigning an Electrochemical MIP Sensor for PFOS: Practicalities and Pitfalls

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    There is a growing interest in the technological transfer of highly performing electrochemical sensors within portable analytical devices for the in situ monitoring of environmental contaminants, such as perfluorooctanesulfonic acid (PFOS). In the redesign of biomimetic sensors, many parameters should be taken into account from the working conditions to the electrode surface roughness. A complete characterization of the surface modifiers can help to avoid time-consuming optimizations and better interpret the sensor responses. In the present study, a molecularly imprinted polymer electrochemical sensor (MIP) for PFOS optimized on gold disk electrodes was redesigned on commercial gold screen-printed electrodes. However, its performance investigated by dierential pulse voltammetry was found to be poor. Before proceeding with further optimization, a morphological study of the bare and modified electrode surfaces was carried out by scanning electron microscopy–energy-dispersive X-ray spectrometry (SEM–EDS), atomic force microscopy (AFM) and profilometry revealing an heterogeneous distribution of the polymer strongly influenced by the electrode roughness. The high content of fluorine of the target-template molecule allowed to map the distribution of the molecularly imprinted polymer before the template removal and to define a characterization protocol. This case study shows the importance of a multi-analytical characterization approach and identify significant parameters to be considered in similar redesigning studies

    Chemical analysis and computed tomography of metallic inclusions in Roman glass to unveil ancient coloring methods

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    This paper describes the analysis of two near-spherical metallic inclusions partially incorporated within two Roman raw glass slags in order to elucidate the process that induced their formation and to determine whether their presence was related to ancient glass colouring processes. The theory of metallic scraps or powder being used in Roman times for glass-making and colouring purposes is widely accepted by the archaeological scientific community, although the assumption has been mainly based on oral traditions and documented medieval practices of glass processing. The analysis of the two inclusions, carried out by X-ray computed tomography, electrochemical analyses, and scanning electron microscopy, revealed their material composition, corrosion and internal structure. Results indicate that the two metallic bodies originated when, during the melting phase of glass, metal scraps were added to colour the material: the colloidal metal–glass system reached then a supersaturation condition and the latter ultimately induced metal expulsion and agglomeration. According to the authors’ knowledge, these two inclusions represent the first documented and studied finds directly associated with the ancient practise of adding metallic agents to colour glass, and their analysis provides clear insights into the use of metallic waste in the glass colouring process.This paper describes the analysis of two near-spherical metallic inclusions partially incorporated within two Roman raw glass slags in order to elucidate the process that induced their formation and to determine whether their presence was related to ancient glass colouring processes. The theory of metallic scraps or powder being used in Roman times for glass-making and colouring purposes is widely accepted by the archaeological scientific community, although the assumption has been mainly based on oral traditions and documented medieval practices of glass processing. The analysis of the two inclusions, carried out by X-ray computed tomography, electrochemical analyses, and scanning electron microscopy, revealed their material composition, corrosion and internal structure. Results indicate that the two metallic bodies originated when, during the melting phase of glass, metal scraps were added to colour the material: the colloidal metal-glass system reached then a supersaturation condition and the latter ultimately induced metal expulsion and agglomeration. According to the authors' knowledge, these two inclusions represent the first documented and studied finds directly associated with the ancient practise of adding metallic agents to colour glass, and their analysis provides clear insights into the use of metallic waste in the glass colouring process

    Covalent immobilization of delipidated human serum albumin on poly(pyrrole-2-carboxylic) acid film for the impedimetric detection of perfluorooctanoic acid

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    The immobilization of biomolecules at screen printed electrodes for biosensing applications is still an open challenge. To enrich the toolbox of bioelectrochemists, graphite screen printed electrodes (G-SPE) were modified with an electropolymerized film of pyrrole-2-carboxilic acid (Py-2-COOH), a pyrrole derivative rich in carboxylic acid functional groups. These functionalities are suitable for the covalent immobilization of biomolecular recognition layers. The electropolymerization was first optimized to obtain stable and conductive polymeric films, comparing two different electrolytes: sodium dodecyl sulphate (SDS) and sodium perchlorate. The G-SPE modified with Py-2-COOH in 0.1 M SDS solution showed the required properties and were further tested. A proof-of-concept study for the development of an impedimetric sensor for perfluorooctanoic acid (PFOA) was carried out using the delipidated human serum albumin (hSA) as bioreceptor. The data interpretation was supported by size exclusion chromatography and small-angle X-ray scattering (SEC-SAXS) analysis of the bioreceptor-target complex and the preliminary results suggest the possibility to further develop this biosensing strategy for toxicological and analytical studies

    Plasma Activation of Copper Nanowires Arrays for Electrocatalytic Sensing of Nitrate in Food and Water

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    Electrochemical methods for nitrate detection are very attractive since they are suitable for in-field and decentralized monitoring. Copper electrodes are often used to this aim as this metal presents interesting electrocatalytic properties towards nitrate reduction. In this research, we study improvements in the electrochemical analysis of nitrate in natural water and food by taking advantage of the detection capabilities of ensembles of copper nanowire electrodes (CuWNEEs). These electrodes are prepared via template electrodeposition of copper within the nanopores of track-etched polycarbonate (PC) membranes. A critical step in the preparation of these sensors is the removal of the template. Here, we applied the combination of chemical etching with atmospheric plasma cleaning which proved suitable for improving the performance of the nanostructured copper electrode. Analytical results obtained with the CuWNEE sensor for nitrate analyses in river water samples compare satisfactorily with those achieved by standard chromatographic or spectroscopic methods. Experimental results concerning the application of the CuWNEEs for nitrate analysis in food samples are also presented and discussed, with focus on nitrate detection in leafy vegetables

    Nanocoated fiber label-free biosensing for perfluorooctanoic acid detection by lossy mode resonance

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    The determination of per- and polyfluoroalkyl substances (PFAS) in environmental samples, such as drinking waters, requires the design of high performing and versatile sensing strategies. Label-free biosensing platforms based on specialty fiber optics are a valid option to face this challenge. Among them, lossy mode resonance (LMR) fiber optic biosensors are showing remarkable performance in terms of detection limit, selectivity, and reproducibility. The detection of small molecules, such as perfluorooctanoic acid (PFOA), can be achieved with the help of well-designed biological recognition layers. In this study, the biosensing potentialities of a label-free LMR-assisted optical platform based on nanocoated fibers are investigated. Delipidated human serum albumin (hSA) was used as biological recognition layer for PFOA in aqueous solution. Different fiber functionalization protocols based on the covalent immobilization of hSA were tested. The conformational changes related to the formation of hSA/PFOA complex were followed via optical monitoring of LMR spectral shift, showing a trend that can be modeled with Langmuir adsorption isotherm. These results confirmed the potentiality of LMR-based fiber biosensors for the detection of small molecules, such as PFOA, in synthetic samples

    Insights into the secondary glass production in Roman Aquileia: A preliminary study

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    A set of 29 glass shards, selected from numerous ones recovered in 2017 in Aquileia (NE Italy), was studied to provide evidence of local glass production for that specific area in antiquity. These shards can be dated between the 1st and the 4th century AD. The chemical composition of glass samples was obtained using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) that enables to quantify the concentration of major, minor, and trace elements needed to investigate provenance and compositional groups and sometimes to suggest a chronological frame of the samples. To ensure that the samples are homogeneous enough to perform accurate quantification, some of them were also analysed by instrumental neutron activation analysis (INAA). Most of the chunks, working wastes, and artefact shards considered in this work exhibited similarities among them in terms of composition, which likely indicates that glass working activities were practised at the site of recovery. The analyses demonstrated the presence of both recycled glass and primary glass. Interestingly, the compositional data of raw primary glass point to both Syro-Palestinian and Egyptian regions as sourcing areas, confirming the role of the Roman city of Aquileia as a network node for the trade of goods. In addition, some particularly coloured glass fragments showed a composition typical of glass produced starting from the 1st or 2nd century AD, requiring specific types of furnaces and procedures for its manufacture, and suggesting the possibility of local highly-specialised production. The preliminary results of this work strengthen the hypothesis that Aquileia was a thriving centre, either for working primary glass or for glass recycling and production of objects with particular colours

    Gold nanoelectrode ensembles for direct trace electroanalysis of iodide

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    A procedure for the standardization of ensembles of gold nanodisk electrodes (NEE) of 30 nm diameter is presented, which is based on the analytical comparison between experimental cyclic voltammograms (CV) obtained at the NEEs in diluted solutions of redox probes and CV patterns obtained by digital simulation. Possible origins of defects sometimes found in NEEs are discussed. Selected NEEs are then employed for the study of the electrochemical oxidation of iodide in acidic solutions. CV patterns display typical quasi-reversible behavior which involves associated chemical reactions between adsorbed and solution species. The main CV characteristics at the NEE compare with those observed at millimeter sized gold disk electrodes (Au-macro), apart a slight shift in E1/2 values and slightly higher peak to peak separation at the NEE. The detection limit (DL) at NEEs is 0.3 M, which is more than one order of magnitude lower than DL at the Au-macro (4 M). The mechanism of the electrochemical oxidation of iodide at NEEs is discussed. Finally, NEEs are applied to the direct determination of iodide at micromolar concentration levels in real samples, namely in some ophthalmic drugs and iodized table salt
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