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X-ray Fluorescence Spectroscopy (x-ray + fluorescence_spectroscopy)
Selected AbstractsRevealing the sfumato Technique of Leonardo da Vinci by X-Ray Fluorescence Spectroscopy,ANGEWANDTE CHEMIE, Issue 35 2010Laurence de, Viguerie Dr. Mehr als nur ein hübsches Gesicht: Nichtinvasive Röntgenfluoreszenzspektroskopie gibt eine Antwort auf die Frage, wie das Auftragen mehrerer Farbschichten übereinander mithilfe der sfumato -Technik funktioniert. Diese Technik wurde von Leonardo da,Vinci für die Gesichter in sieben seiner Bilder verwendet. Mit der neuen Methode lässt sich ganz klar eine große Vielfalt in da,Vincis Technik erkennen. [source] Synthesis of silicon nitride based ceramic nanoparticles by the pyrolysis of silazane block copolymer micellesJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 15 2006Kozo Matsumoto Abstract Diblock copolymer poly(1,1,3,N,N,-pentamethyl-3-vinylcyclodisilazane)- block- polystyrene (polyVSA- b -polySt) and triblock copolymer poly(1,1,3,N,N,-pentamethyl-3-vinylcyclodisilazane)- block- polystyrene- block -poly(1,1,3,N,N,-pentamethyl-3-vinylcyclodisilazane) (polyVSA- b -polySt- b -polyVSA), consisting of silazane and nonsilazane segments, were prepared by the living anionic polymerization of 1,1,3,N,N,-pentamethyl-3-vinylcyclodisilazane and styrene. PolyVSA- b -polySt formed micelles having a poly(1,1,3,N,N,-pentamethyl-3-vinylcyclodisilazane) (polyVSA) core in N,N -dimethylformamide, whereas polyVSA- b -polySt and polyVSA- b -polySt- b -polyVSA formed micelles having a polyVSA shell in n -heptane. The micelles with a polyVSA core were core-crosslinked by UV irradiation in the presence of diethoxyacetophenone as a photosensitizer, and the micelles with a polyVSA shell were shell-crosslinked by UV irradiation in the presence of diethoxyacetophenone and 1,6-hexanedithiol. These crosslinked micelles were pyrolyzed at 600 °C in N2 to give spherical ceramic particles. The pyrolysis process was examined by thermogravimetry and thermogravimetry/mass spectrometry. The morphologies of the particles were analyzed by atomic force microscopy and transmission electron microscopy. The chemical composition of the pyrolysis products was analyzed by X-ray fluorescence spectroscopy and Raman scattering spectroscopy. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 4696,4707, 2006 [source] A high-throughput determination of metal concentrations in whole intact Arabidopsis thaliana seeds using synchrotron-based X-ray fluorescence spectroscopyJOURNAL OF SYNCHROTRON RADIATION, Issue 4 2006Lester W. Young The identification of genes involved in metal metabolism in plants requires the `screening' of thousands of genetic variants. While inductively coupled plasma mass-spectroscopy has been used to identify variants with an altered total metal concentration, a more convenient high-throughput technique capable of examining individual seeds (or other tissues) would be useful. Here, the high brightness of synchrotron radiation has been utilised to examine relative metal concentrations in seeds of the genetically well characterised plant Arabidopsis thaliana. The relative concentrations of Mn, Fe, Ni, Cu and Zn in individual seeds were determined using a 500,µm × 500,µm beam. Metal concentrations were normally distributed, except where metal-containing dust contaminated the samples. Neither seed orientation nor genetic background (from three `wild type' variants with different genetic lineages) had a significant affect on the Zn-normalised metal concentration. No advantages, such as the observation of tissue-specific metal accumulation, were obtained by using a 50,µm × 50,µm beam. A high-throughput proof-of-concept experiment was demonstrated that could be used to screen libraries of genetic variants for individuals with altered metal concentrations. Further work is required to standardise the technique before screening of libraries is possible. [source] Excitons in AgI,oxide particle composites: AgI,SrTiO3PHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 10 2006Fumito Fujishiro Abstract We fabricated (x)AgI,(1,x)SrTiO3 fine particle composites over a wide composition range of 0,100 mol% AgI. It is found that the dispersion of SrTiO3 fine particles enhances the ionic conductivity and (0.6)AgI,(0.4)SrTiO3 has the highest ionic conductivity (1.68 × 10,4 S/cm which is two hundreds times in comparison with that of pristine AgI), for the first time. In order to clarify such ionic conductivity enhanced by dispersing SrTiO3 fine particles into AgI, the photoluminescence measurements were carried out at different temperatures between 10 K and room temperature under different photoexcitation intensities, together with the structural and morphological studies (X-ray diffractometry, scanning electron microscopy and energy dispersive X-ray fluorescence spectroscopy). The spectra consist of free exciton luminescence band and several broad luminescence bands due to the excitons trapped at crystal defects and residual impurities. The free exciton luminescence band almost disappears at x = 0.6, which may suggest the existence of considerable number of non-radiative traps (crystal defects) at the AgI/SrTiO3 particle interfaces. Such crystal defects may act as ionic pathways. The structural and morphological studies confirm the randomly-stacked ,AgI/,AgI heterostructures at the AgI/SrTiO3 particle interfaces. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Influence of supported vanadium catalyst on ethylene polymerization reactionsPOLYMER INTERNATIONAL, Issue 2 2008Sutapa Ghosh Abstract BACKGROUND: In the research area of homogeneous Ziegler,Natta olefin polymerization, classic vanadium catalyst systems have shown a number of favourable performances. These catalysts are useful for (i) the preparation of high molecular weight polymers with narrow molecular weight distributions, (ii) the preparation of ethylene/R -olefin copolymers with high R -olefin incorporation and (iii) the preparation of syndiotactic polypropylenes. In view of the above merits of vanadium-based catalysts for polymerization reactions, the development of well-defined single-site vanadium catalysts for polymerization reactions is presently an extremely important industrial goal. The main aim of this work was the synthesis and characterization of a heterogeneous low-coordinate non-metallocene (phenyl)imido vanadium catalyst, V(NAr)Cl3, and its utility for ethylene polymerization. RESULTS: Imido vanadium complex V(NAr)Cl3 was synthesized and immobilized onto a series of inorganic supports: SiO2, methylaluminoxane (MAO)-modified SiO2 (4.5 and 23 wt% Al/SiO2), SiO2 Al2O3, MgCl2, MCM-41 and MgO. Metal contents on the supported catalysts determined by X-ray fluorescence spectroscopy remained between 0.050 and 0.100 mmol V g,1 support. Thermal stability of the catalysts was determined by differential scanning calorimetry (DSC). Characterization of polyethylene was done by gel permeation chromatography and DSC. All catalyst systems were found to be active in ethylene polymerization in the presence of MAO or triisobutylaluminium/MAO mixture (Al/V = 1000). Catalyst activity was found to depend on the support nature, being between 7.5 and 80.0 kg PE (mol V),1 h,1. Finally, all catalyst systems were found to be reusable for up to three cycles. CONCLUSION: Best results were observed in the case of silica as support. Acid or basic supports afforded less active systems. In situ immobilization led to higher catalyst activity. The resulting polyethylenes in all experiments had ultrahigh molecular weight. Finally, this work explains the synthesis and characterization of reusable supported novel vanadium catalysts, which are useful in the synthesis of very high molecular weight ethylene polymers. Copyright © 2007 Society of Chemical Industry [source] Flame retardancy mechanisms of metal phosphinates and metal phosphinates in combination with melamine cyanurate in glass-fiber reinforced poly(1,4-butylene terephthalate): the influence of metal cationPOLYMERS FOR ADVANCED TECHNOLOGIES, Issue 6 2008Ulrike Braun Abstract The pyrolysis and fire behavior of glass-fiber reinforced poly(butylene terephthalate) (PBT/GF) with two different metal phosphinates as flame retardants in combination with and without melamine cyanurate (MC) were analyzed by means of thermogravimetry, thermogravimetry coupled with infrared spectroscopy, flammability, and cone calorimeter tests as well as scanning electron microscopy/energy dispersive X-ray spectroscopy and X-ray fluorescence spectroscopy. In PBT/GF, dosages of 13,20% of the halogen-free flame retardant aluminum phosphinate or aluminum phosphinate in combination with MC fulfill the requirements for electrical engineering and electronics applications (UL 94,=,V-0; LOI,>,42%), whereas the use of the same amount of zinc phosphinate or zinc phosphinate in combination with MC does not improve the fire behavior satisfactorily (UL 94,=,HB; LOI,=,27,28%). The performance under forced flaming conditions (cone calorimeter) is quite similar for both of the metal phosphinates. The use of aluminum and zinc salts results in similar flame inhibition predominantly due to the release of the phosphinate compounds in the gas phase. Both metal phosphinates and MC interact with the polymer changing the decomposition characteristics. However, part of the zinc phosphinate vaporizes as a complete molecule. Because of the different decomposition behavior of the metal salts, only the aluminum phosphinate results in a small amount of thermally stable carbonaceous char. In particular, the aluminum phosphinate-terephthalate formed is more stable than the zinc phosphinate-terephthalate. The small amount of char has a crucial effect on the thermal properties and mechanical stability of the residue and thus the flammability. Copyright © 2008 John Wiley & Sons, Ltd. [source] CYPRIOT BYZANTINE GLAZED POTTERY: A STUDY OF THE PAPHOS WORKSHOPSARCHAEOMETRY, Issue 4 2010A. C. CHARALAMBOUS Twenty-five samples of Byzantine glazed pottery from two archaeological sites between Limassol and Paphos region (Cyprus), dated between the 12th and 15th century ad were studied using micro X-ray fluorescence spectroscopy, scanning electron microscopy and X-ray diffraction analysis. It was found that all the glazes contain lead, following the main manufacturing process of medieval pottery in the Mediterranean territory, while some of them contain tin, possibly for better opacity. Furthermore, it is shown that copper, iron and cobalt with nickel are responsible for the decoration colours. Finally, the application of principal component analysis revealed significant differentiation for some of the samples. [source] Crystallization and preliminary X-ray analysis of the small subunit (R2F) of native ribonucleotide reductase from Corynebacterium ammoniagenesACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 9 2009Hideaki Ogata Ribonucleotide reduction, the unique step in DNA-precursor biosynthesis, involves radical-dependent redox chemistry and diverse metallo-cofactors. The metallo-cofactor (R2F) encoded by the nrdF (nucleotide reduction) gene in Corynebacterium ammoniagenes ATCC 6872 was isolated after homologous expression and a new crystal form of ribonucleotide reductase R2F was obtained. R2F was crystallized at 277,K using the vapour-diffusion method with PEG as the precipitating agent. A data set was collected to 1.36,Å resolution from a single crystal at 100,K using synchrotron radiation. The crystal belonged to space group C2, with unit-cell parameters a = 96.21, b = 87.68, c = 83.25,Å, , = 99.29°. The crystal contained two molecules per asymmetric unit, with a Matthews coefficient (VM) of 2.69,Å3,Da,1; the solvent content was estimated to be 54.3%. X-ray fluorescence spectroscopy and MAD diffraction data indicated the presence of manganese in the molecule and the absence of iron. [source] Heavy Metal Distribution in Soils near the Almalyk Mining and Smelting Industrial Area, UzbekistanACTA GEOLOGICA SINICA (ENGLISH EDITION), Issue 5 2009Obidjon KODIROV Abstract: The present study demonstrates distribution and chemical forms of heavy metals in soils of the Almalyk mining and smelting industrial area along five transects. The study area is located in Almalyk, Uzbekistan, where the intensification of industrial enterprises negatively impacts the environment. The distribution of 17 heavy metals (Cu, Zn, Pb, Sc, V, Cr, Co, Ni, Ga, Rb, Sr, Y, Zr, Nb, Ba, Th, and U) were studied in 21 sampling locations (21×3=63 soil samples) along five radial transects with a total length of 60 km downwind deposition gradient. Soil samples were collected from the upper layer (0,10 cm) at 4,6 km intervals. As a result of X-ray fluorescence spectrometry analyses by using X-ray fluorescence spectroscopy (XRF, Philips Analytical Ink, USA), a significant decrease in heavy metal (Cu, Zn, Pb) deposition was found going from the source in a downwind direction. Soil samples taken from the first location (near the pollution sources) showed higher concentrations of Cu, Zn and Pb, and lower concentrations with increasing distance from the source. Obtained data showed different impact of pollution sources to heavy metal deposition and distribution in soils. The Almalyk mining and smelting complex is the major source of Pb, Zn and Cu enrichment in soils. Distribution of other trace elements does not exceed background content and suggests lithogenic background. This allowed us to divide these elements into two groups: (1) technogenic (Cu, Zn and Pb); and (2) lithogenic (Sc, V, Cr, Co, Ni, Ga, Rb, Sr, Y, Zr, Nb, Ba, Th and U) origins. [source] | |||||||||||||