DSC investigations of amalgam formation in Bi-Sn-Hg system doped with indium

Differential scanning calorimetric (DSC) measurements have been carried out on Bi-Sn based amalgam precursors to be used in compact fluorescent lamps (CFLs) to study the changes in melting and solidifying behaviour caused by In dopant. The phase and elemental compositions of the samples have been characterized by using X-ray diffraction (XRD) and scanning electron microscopy-energy dispersive X-ray analysis (SEM-EDX), respectively. One of the endothermic peaks of the liquid amalgam formation shifted from 121°C to 112 and 105°C, with increasing content of 2.5 and 4.8 mass% In of samples, respectively.     

Chemical characterization of density separated submicrometer coal fly ash

A new geometrical particle size separation method in the range of submicrometer has been developed for coal fly ash. Coal fly ash particles prefractionated less than 5m in geometrical diameter were fractionated with a coupling of supersonical dispersion in methyl alcohol and filtration through antistatic Nucleopore filter into >1.0, 1.0–0.8, 0.8–0.6m.Submicrometer (1.0–0.6m) and micrometer coal fly ash (25–20m) were separated into six density fractions and their compositions measured by SEM-EDX were compared. For the both size fractions, for the low density fractions (<2.8 g/cm³) consisted mainly of aluminosilicates and the fractions of 2.8–3.2 g/cm³ consisted of oxides of aluminum, silicon and calcium, and in the fraction above 3.2 g/cm³ iron was rich. In submicrometer fly ash, phosphor and sulfur concentrated to the particles rich in calcium. In the heaviest fraction, the particles containing over 30 wt% titanium as oxide observed among the particles rich in iron. These fractions were revealed not as a single component, but as mixtures of several components.     

Determination of fluorine in uranium oxyfluoride particles as an indicator of particle age

As swipe samples from enrichment activities typically contain uranium particles with a detectable amount of fluorine, the question was raised whether the analysis of fluorine in particles could complement the information on the uranium isotope ratios.     

Nanotopography and electrochemical impedance spectroscopy of palladium deposited on different electrode materials

The objective of this work was to describe the characteristics of chemically and electrochemically deposited Pd surface layers on HOPG and polycrystalline gold electrode, using in situ ECSTM and EIS measurements, and SEM-EDX element analysis. Pd surface layers were deposited, in successive voltammetric cycles, and anodically dissolved in 0.01 M HCl+0.01 M (NH₄)₂PdCl₄ aqueous electrolyte. Both of the electrode materials used in the study were treated as standard testing electrodes: (i) HOPG for STM/ECSTM measurements, and (ii) polycrystalline Au as the well known working electrode in various electro-analytical applications. The elements surface analysis and nano-surface pictures were used to interpret the EIS diagrams and electrical equivalent circuits. Pd chemical and electrochemical deposition on the HOPG surface was compared with the same process on the polycrystalline gold electrode, on which palladium can be electrodeposited only by means of electrochemical cathodic deposition. Surface topographies of the electrodeposited palladium layers on HOPG and Au were completely different. The equivalent electrical circuits were fitted and the surface roughness of the investigated electrodes calculated. Relations between the surface topography, EIS and SEM-EDX, and interface model of the electrolyte solution electrodeposited Pd layer matrix electrode were proposed.     

Evaluating the use of laser radiation in cleaning of copper embroidery threads on archaeological Egyptian textiles

Cleaning of copper embroidery threads on archaeological textiles is still a complicated conservation process, as most textile conservators believe that the advantages of using traditional cleaning techniques are less than their disadvantages. In this study, the uses of laser cleaning method and two modified recipes of wet cleaning methods were evaluated for cleaning of the corroded archaeological Egyptian copper embroidery threads on an archaeological Egyptian textile fabric. Some corroded copper thread samples were cleaned using modified recipes of wet cleaning method; other corroded copper thread samples were cleaned with Q-switched Nd:YAG laser radiation of wavelength 532 nm. All tested metal thread samples before and after cleaning were investigated using a light microscope and a scanning electron microscope with an energy dispersive X-ray analysis unit. Also the laser-induced breakdown spectroscopy (LIBS) technique was used for the elemental analysis of laser-cleaned samples to follow up the laser cleaning procedure. The results show that laser cleaning is the most effective method among all tested methods in the cleaning of corroded copper threads. It can be used safely in removing the corrosion products without any damage to both metal strips and fibrous core. The tested laser cleaning technique has solved the problems caused by other traditional cleaning techniques that are commonly used in the cleaning of metal threads on museum textiles.     

Green Synthesis,Characterization, and Antibacterial Properties of Silver Nanoparticles Obtained by Using Diverse Varieties of Cannabis sativa Leaf Extracts

Cannabis sativa L. (hemp) is a plant used in the textile industry and green building material industry, as well as for the phytoremediation of soil, medical treatments, and supplementary food products. The synergistic effect of terpenes, flavonoids, and cannabinoids in hemp extracts may mediate the biogenic synthesis of metal nanoparticles. In this study, the chemical composition of aqueous leaf extracts of three varieties of Romanian hemp (two monoecious, and one dioecious) have been determined by Fourier-Transformed Infrared spectroscopy (FT-IR), high-performance liquid chromatography, and mass spectrometry (UHPLC-DAD-MS). Then, their capability to mediate the green synthesis of silver nanoparticles (AgNPs) and their pottential antibacterial applications were evaluated. The average antioxidant capacity of the extracts had 18.4 ± 3.9% inhibition determined by 2,2-diphenyl-1-picrylhydrazyl (DPPH^•) and 78.2 ± 4.1% determined by 2,2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt (ABTS™) assays. The total polyphenolic content of the extracts was 1642 ± 32 mg gallic acid equivalent (GAE) L⁻¹. After this, these extracts were reacted with an aqueous solution of AgNO₃ resulting in AgNPs, which were characterized by UV−VIS spectroscopy, FT-IR, scanning electron microscopy (SEM-EDX), and dynamic light scattering (DLS). The results demonstrated obtaining spherical, stable AgNPs with a diameter of less than 69 nm and an absorbance peak at 435 nm. The mixture of extracts and AgNPs showed a superior antioxidant capacity of 2.3 ± 0.4% inhibition determined by the DPPH^• assay, 88.5 ± 0.9% inhibition as determined by the ABTS^•+ assay, and a good antibacterial activity against several human pathogens: Escherichia coli, Klebsiella pneumoniae, Pseudomonas fluorescens, and Staphylococcus aureus.     

New insight on the underdrawing of 16th Flemish-Portuguese easel paintings by combined surface analysis and microanalytical techniques

This paper focusses on the study of the underdrawings of 16th century easel paintings attributed to the workshop of the Portuguese-Flemish Master Frei Carlos. This investigation encompasses multidisciplinary research that relates the results of surface exams (infrared reflectography, standard light photography and infrared photography) with analytical investigations.The surface analysis of Frei Carlos’ underdrawings by infrared reflectography has shown heterogeneous work, revealing two different situations: (1) an abundant and expressive underdrawing, revealing a Flemish influence and (2) a simple and outlined underdrawing. This preliminary research raised an important question related to this Portuguese-Flemish workshop and to the analytical approach: Is the underdrawing's heterogeneity, as observed in the reflectograms, related to different artists or is this rather an effect that is produced due to the use of different materials in the underdrawing's execution? Consequently, if different materials were used, how can we have access to the hidden underdrawings? In order to understand the reasons for this dissemblance, chemical analysis of micro-samples collected in underdrawing areas and representing both situations were carried out by optical microscopy, micro Fourier transform infrared spectroscopy (μ-FTIR), scanning electron microscopy coupled with energy dispersive X-ray spectrometry (SEM-EDX) and micro-Raman spectroscopy (μ-Raman). Taking into account the different possibilities and practical and theoretical limitations of surface and punctual examinations in the study of easel painting underdrawings, the methodology of research was adjusted, sometimes resulting in a re-analysis of experimental results. This research shows the importance of combining multispectral surface exams and chemical analysis in the understanding of the artistic creative processes of 16th century easel paintings.     

Micro-Raman Spectroscopy and X-ray Diffraction Analyses of the Core and Shell Compartments of an Iron-Rich Fulgurite

Fulgurites are naturally occurring structures that are formed when lightning discharges reach the ground. In this investigation, the mineralogical compositions of core and shell compartments of a rare, iron-rich fulgurite from the Mongolian Gobi Desert were investigated by X-ray diffraction and micro-Raman spectroscopy. The interpretation of the Raman data was helped by chemometric analysis, using both multivariate curve resolution (MCR) and principal component analysis (PCA), which allowed for the fast identification of the minerals present in each region of the fulgurite. In the core of the fulgurite, quartz, microcline, albite, hematite, and barite were first identified based on the Raman spectroscopy and chemometrics analyses. In contrast, in the shell compartment of the fulgurite, the detected minerals were quartz, a mixture of the K-feldspars orthoclase and microcline, albite, hematite, and goethite. The Raman spectroscopy results were confirmed by X-ray diffraction analysis of powdered samples of the two fulgurite regions, and are consistent with infrared spectroscopy data, being also in agreement with the petrographic analysis of the fulgurite, including scanning electron microscopy with backscattering electrons (SEM-BSE) and scanning electron microscopy with energy dispersive X-ray (SEM-EDX) data. The observed differences in the mineralogical composition of the core and shell regions of the studied fulgurite can be explained by taking into account the effects of both the diffusion of the melted material to the periphery of the fulgurite following the lightning and the faster cooling at the external shell region, together with the differential properties of the various minerals. The heavier materials diffused slower, leading to the concentration in the core of the fulgurite of the iron and barium containing minerals, hematite, and barite. They first underwent subsequent partial transformation into goethite due to meteoric water within the shell of the fulgurite. The faster cooling of the shell region kinetically trapped orthoclase, while the slower cooling in the core area allowed for the extensive formation of microcline, a lower temperature polymorph of orthoclase, thus justifying the prevalence of microcline in the core and a mixture of the two polymorphs in the shell. The total amount of the K-feldspars decreases only slightly in the shell, while quartz and albite appeared in somewhat larger amounts in this compartment of the fulgurite. On the other hand, at the surface of the fulgurite, barite could not be stabilized due to sulfate lost (in the form of SO₂ plus O₂ gaseous products). The conjugation of the performed Raman spectroscopy experiments with the chemometrics analysis (PCA and, in particular, MCR analyses) was shown to allow for the fast identification of the minerals present in the two compartments (shell and core) of the sample. This way, the XRD experiments could be done while knowing in advance the minerals that were present in the samples, strongly facilitating the data analysis, which for compositionally complex samples, such as that studied in the present investigation, would have been very much challenging, if possible.