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1.
Riekel C García Gutiérrez MC Gourrier A Roth S 《Analytical and bioanalytical chemistry》2003,376(5):594-601
The status of synchrotron radiation (SR) microdiffraction techniques developed at the ID13 beamline of the European Synchrotron Radiation Facility (ESRF) is reviewed for polymer and biopolymer fiber applications. Beam sizes in the micrometer-range have been used to study the local structure of whole fibers such as viscose-rayon or poly(p-phenylene terephthalamide). The possibilities for in situ studies during stretching, extrusion, or indentation will be discussed. 相似文献
2.
Synchrotron radiation sources have proven to be highly beneficial in many fields of research for the characterization of materials. However, only a very limited proportion of studies have been conducted by the forensic science community. This is an area in which the analytical benefits provided by synchrotron sources could prove to be very important. This review summarises the applications found for synchrotron radiation in a forensic trace evidence context as well as other areas of research that strive for similar analytical scrutiny and/or are applied to similar sample materials. The benefits of synchrotron radiation are discussed in relation to common infrared, X-ray fluorescence, tomographic and briefly, X-ray diffraction and scattering techniques. In addition, X-ray absorption fine structure analysis (incorporating XANES and EXAFS) is highlighted as an area in which significant contributions into the characterization of materials can be obtained. The implications of increased spatial resolution on microheterogeneity are also considered and discussed. 相似文献
3.
Bruno Lengeler 《Mikrochimica acta》1987,91(1-6):455-475
The synchrotron radiation (SR) emitted by circulating high-energy electrons has extraordinary properties: The light is intensive and bright, it is tunable and highly collimated, and finally, it is linearly polarized. These exceptional properties have initiated a unique revival of many spectroscopies using electromagnetic radiation. The techniques of special concern for materials analysis which are treated in this article are: X-ray absorption, reflection, fluorescence, diffraction and topography. A number of examples will be given in order to illustrate the possibilities of these techniques when SR is used.On leave of absence from Institut für Festkörperforschung, KFA Jülich, D-5170 Jülich, Federal Republic of Germany 相似文献
4.
M.L. Carvalho T. Magalhães M. Becker A. von Bohlen 《Spectrochimica Acta Part B: Atomic Spectroscopy》2007
It is known that trace elements play an important role in a number of biological processes. These include the activation or inhibition of enzymatic reactions, competition between elements and metal proteins for binding positions and modifications in the permeability of cellular membranes. These elements may also influence carcinogenic processes, thus the knowledge of trace element concentrations in healthy and neoplastic tissues might help in diagnostic and in the etiology and development of cancer. 相似文献
5.
Transition rates were obtained from spectra for pure metallic samples of atomic number ranging from 22 to 27, measured with monochromatic incident X-ray beams from a synchrotron source. The experimental setup for this consisted of an energy dispersive spectrometer in a conventional 45–45° geometry, mounted in an evacuated chamber. Absorption, detector efficiency and multiple scattering were taken into account. The results obtained are compared with recent theoretical and experimental data as well as with the well-known theoretical predictions from Scofield. 相似文献
6.
Jianling Zhang Dongxia Liu Guanying Yang Buxing Han Zhonghua Wu 《Colloid and polymer science》2007,285(11):1275-1279
Synchrotron small-angle X-ray scattering technique has been used to study the effect of ultrasound on the microstructure of
polystyrene (PS) in cyclohexane solutions. The results show that the intramolecular radius of gyration (R
g) decreases with ultrasound, indicating the shrinkage and collapse of PS chains. There is an exponential relationship between
R
g and the molecular weight of PS (M
w), and the exponent changes from 0.5 to 0.417, as the ultrasound time is increased. This means that the shape of PS chain
changes from random coil to shrunken form. The Kratky plots also confirm the shape transformation of PS chains induced by
ultrasound. Moreover, the intermolecular correlation length increases with the ultrasound time, which is indicative of the
entanglement of PS chains. 相似文献
7.
Stribeck N 《Analytical and bioanalytical chemistry》2003,376(5):608-617
The prospects of a modern analysis of nanostructure evolution during the processing of polymer materials by means of scattering from synchrotron radiation are demonstrated in examples. The beam sources have gained stability, shortages are located in beamline setups and in method development for the quantitative analysis of voluminous data sets.By using the proposed multidimensional chord distribution function (CDF) analysis method, nanostructure information from small-angle X-ray scattering (SAXS) data are extracted and visualised. The method can be automated if the beamline setup is able to deliver a full data set with simple constraints. In this case even a simultaneous data evaluation is possible (while one pattern is accumulated, the previous one is analysed). The advantages of the method are demonstrated in a study of the straining of a thermoplastic elastomer. The possibilities of an automated analysis are demonstrated in an investigation of the crystallisation behaviour of high-pressure injection-moulded polyethylene (HPIM-PE). The achievable results of nanostructure analysis of polymer materials are discussed. It is shown that the time-resolved SAXS of polymer materials studied during a transformation and analysed by the CDF method is not just a powerful tool to investigate the relationship between structure and properties of materials; the information that can be gained concerning the processes that control nanostructure evolution is equally important. In the future the enlightenment of such relationships may help to tailor polymer materials with respect to their properties and, beyond that, to improve assessments concerning their aging. 相似文献
8.
In the present paper, lithium was determined in river sediment using slurry sampling and electrothermal atomic absorption spectrometry (ET AAS) after L’vov platform coating with zirconium (as a permanent chemical modifier). The performance of this modifier and its distribution on the L’vov platform after different heating cycles were evaluated using synchrotron radiation X-ray fluorescence (SRXRF) and imaging scanning electron microscopy (SEM) techniques. The analytical conditions for lithium determination in river sediment slurries were also investigated and the best conditions were obtained employing 1300 and 2300 °C for pyrolysis and atomization temperatures, respectively. In addition, 100 mg of sediment samples were prepared using 4.0 mol l−1 HNO3. The Zr-coating permitted lithium determination with good precision and accuracy after 480 heating cycles using the same platform for slurry samples. The sediment samples were collected from five different points of the Cachoeira river, São Paulo, Brazil. The detection and quantification limits were, respectively, 0.07 and 0.23 μg l−1. 相似文献
9.
An exemplary system suitable for optoelectronics applications, i.e. poly(3-hexylthiophene), hereinafter P3HT, deposited by spin casting onto silicon substrates functionalised by three selected molecules and then properly annealed, has been examined. Grazing Incidence X-ray Scattering (GIXS) measurements have been performed with 4-circle diffractometer, allowing for a fine control of sample axes movement.By choosing different grazing incident angles, diffraction patterns from different layers of polymeric thin films have been recorded. Both in-plane and out-of-plane geometries have been combined in order to obtain complementary structural information. In this way structural and orientational differences of the polymer along with the film thickness (?50 nm) have been highlighted. For all P3HT films spun on functionalized Si wafer, macromolecular layers close to the substrate surface give some evidence of higher order and orientation than those outmost the surface, and this behaviour is pronounced to a different extent depending on the functionalized molecules used. Contrariwise P3HT layers deposited onto bare Si wafer display reduced orientation and decreased crystallite size, especially at buried interface. 相似文献
10.
Katja Kavkler ?iga Šmit David JezeršekDiane Eichert Andrej Demšar 《Polymer Degradation and Stability》2011,96(6):1081-1086
We have examined specimens of historical biodeteriorated cellulose textiles using synchrotron radiation and conventional source FTIR spectroscopy. The main aim of our research was to investigate structural changes caused by ageing and biodeterioration in different types of cellulose fibres. We compared the results, obtained with both methods regarding spectral quality and information obtained with each method. Additionally, we obtained mapping images of the cross sections of the investigated specimens using synchrotron FTIR in order to analyze structural changes in cross sections, caused due to biodeterioration. 相似文献
11.
Characterization of polymer materials by scattering techniques,with applications to block copolymers
Tim Lodge 《Mikrochimica acta》1994,116(1-3):1-31
The application of six techniques—static and dynamic light scattering, small-angle neutron and X-ray scattering, neutron and X-ray reflectivity—to the characterization of polymer materials is summarized. Emphasis is placed on the similarities and differences among the various techniques, and on recent advances in experimental practice. Twelve examples from the recent literature are described, most of which concern block copolymers. A brief introduction to block copolymer properties is also provided. 相似文献
12.
A. C. M. Costa M. J. Anjos S. Moreira R. T. Lopes E. F. O. de Jesus 《Spectrochimica Acta Part B: Atomic Spectroscopy》2003,58(12):2199-2204
The total reflection X-ray fluorescence using synchrotron radiation (SRTXRF) has become a competitive technique for the determination of trace elements in samples that the concentrations are lower than 100 ng ml−1. In this work, thirty-seven mineral waters commonly available in supermarkets of Rio de Janeiro, Brazil, were analyzed by SRTXRF. The measurements were performed at the X-Ray Fluorescence Beamline at Brazilian National Synchrotron Light Laboratory (LNLS), in Campinas, São Paulo, using a polychromatic beam with maximum energy of 20 keV for the excitation. Standard solutions with gallium as internal standard were prepared for calibration of the system. Mineral water samples of 10 μl were added to Perspex sample carrier, dried under infrared lamp and analyzed for 200 s measuring time. It was possible to determine the concentrations of the following elements: Si, S, K, Ca, Ti, Cr, Mn, Ni, Cu, Zn, Ge, Rb, Sr, Ba and Pb. The elemental concentration values were compared with the limits established by the Brazilian legislation. 相似文献
13.
Several organo-modified montmorillonites were studied to prepare nanocomposites of polyoctamethylene suberate, a biodegradable polyester. Mixtures were analyzed by conventional powder X-ray diffraction and transmission electron microscopy techniques. C30B clay was effective in rendering an intercalated structure with rather variable silicate layer spacing. The hydroxyl groups of the organo-modifier may allow the establishment of good interactions with the polar carbonyl groups of the studied polyester. A slight decrease in thermal stability was detected when the modified clay was incorporated into the polymer matrix. Isothermal and nonisothermal crystallization kinetics were studied by DSC and results compared with those for the neat polyester. The overall crystallization rate determined by calorimetric methods depends on the nucleation density and the crystal growth rate, which were independently evaluated by means of optical microscopy. Crystallization and morphological features were also analyzed by simultaneous SAXS/WAXD measurements made at a selected crystallization temperature and cooling rate under both isothermal and nonisothermal conditions, respectively. 相似文献
14.
C. Streli G. Pepponi P. Wobrauschek N. Zger P. Pianetta K. Baur S. Pahlke L. Fabry C. Mantler B. Kanngießer W. Malzer 《Spectrochimica Acta Part B: Atomic Spectroscopy》2003,58(12):2105-2112
The unique properties of synchrotron radiation, such as high incident flux combined with low divergence, its linear polarization and energy tunability, make it an ideal excitation source for total reflection X-ray fluorescence (TXRF) spectroscopy in order to non-destructively detect trace impurities of transition metals on Si wafer surfaces. When used with a detector suitable for the determination of low energy radiation this technique can be extended to the detection of low-Z elements, such as Al, Na and Mg. Experiments have been performed at SSRL Beamline 3-3, a bending magnet beamline using monochromatic radiation from a double multilayer monochromator. The wafer was mounted vertically in front of the detector, which was aligned along the linear polarization vector of the incoming synchrotron radiation. This configuration allows the detector to accept a large solid angle as well as to take advantage of the reduced scattered X-ray intensity emitted in the direction of the linear polarization vector. A comparison between droplet samples and spin coated samples was done, in order to compare the capabilities of vapor phase decomposition (VPD-TXRF) with conventional SR-straight-TXRF. Detection limits in the range of 50 fg corresponding to 2E10 atoms/cm2 have been obtained for Na. The spin coated samples, prepared from solutions containing an equal amount of Na, Mg and Al showed an unexpected result when performing a scan of the angle of incidence of the incoming X-rays suggesting a different adsorption behavior of the elements in a multielement solution on the wafer surface. The observation of this behavior is important because the spin coating technique is the standard method for the preparation of surface standards in semiconductor quality control. This effect could be characteristic of the Na, Mg, Al solution used, but the angle dependence of the fluorescence signal of a standard should always be investigated before using the standard for calibration of the apparatus and quantification. 相似文献
15.
Kuroiwa Y. Aoyagi S. Sawada A. Ikawa H. Yamashita I. Inoue N. Atake T. 《Journal of Thermal Analysis and Calorimetry》2002,69(3):933-938
The crystal structures of BaTiO3 and PbTiO3 fine particles have been investigated by powder diffraction using synchrotron radiation high energy X-rays. It is revealed
that a BaTiO3 fine particle essentially consists of tetragonal and cubic structure components at 300 K, whereas a PbTiO3 fine particle consists of a tetragonal structure. Adopting a structure model for the BaTiO3 particle that a cubic shell covers a tetragonal core, the thickness of cubic BaTiO3 shell is estimated at almost constant irrespective of particle sizes. Successive phase transitions are detected in 100 nm
particles of BaTiO3 near the phase-transition temperatures of a bulk crystal. The changes in diffraction profiles are small, but they are apparent
for a most up-to-date powder diffractometry.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
16.
Thermoluminescence and synchrotron radiation studies on the persistent luminescence of BaAl2O4:Eu,Dy
L.C.V. Rodrigues R. Stefani M.C.F.C. Felinto M. Lastusaari T. Laamanen M. Malkamäki 《Journal of solid state chemistry》2010,183(10):2365-2371
The persistent luminescence materials, barium aluminates doped with Eu2+ and Dy3+ (BaAl2O4:Eu2+,Dy3+), were prepared with the combustion synthesis at temperatures between 400 and 600 °C as well as with the solid state reaction at 1500 °C. The concentrations of Eu2+/Dy3+ (in mol% of the Ba amount) ranged from 0.1/0.1 to 1.0/3.0. The electronic and defect energy level structures were studied with thermoluminescence (TL) and synchrotron radiation (SR) spectroscopies: UV-VUV excitation and emission, as well as with X-ray absorption near-edge structure (XANES) methods. Theoretical calculations using the density functional theory (DFT) were carried out in order to compare with the experimental data. 相似文献
17.
A. von Bohlen M. Brücher B. Holland R. Wagner R. Hergenröder 《Spectrochimica Acta Part B: Atomic Spectroscopy》2010
A systematic characterization of mono-disperse nanoparticles with nominal diameters of 25 nm, 46 nm, 73 nm, 100 nm, 115 nm, and 250 nm was performed using X-ray standing waves (XSW). The samples were prepared on Si-wafer pieces and analyzed at DELTA synchrotron facility at beamline BL8 under grazing incidence geometry of the primary radiation. Additionally, SEM-EDX inspections of single particles as well as population-density checks were conducted. Particles with smaller diameters were able be characterized by XSW while the larger ones were not completely covered by the interference field produced by the provided 15 keV monochromatic radiation of BL8. The results of the measurements were compared with those of numerical simulations. The extension of the interference field perpendicular to the Si-wafer reflector was determined to be 83 nm ± 4 nm. 相似文献
18.
The high-pressure compression behaviour of 3 different cation forms of gallosilicate zeolite with CGS topology has been investigated using in situ synchrotron X-ray powder diffraction and a diamond-anvil cell technique. Under hydrostatic conditions mediated by a nominally penetrating pressure-transmitting medium, unit-cell lengths and volume compression is modulated by different degrees of pressure-induced hydration and accompanying channel distortion. In a Na-exchanged CGS (Na10Ga10Si22O64·16H2O), the unit-cell volume expands by ca. 0.6% upon applying hydrostatic pressure to 0.2 GPa, whereas, in an as-synthesized K-form (K10Ga10Si22O64·5H2O), this initial volume expansion is suppressed to ca. 0.1% at 0.16 GPa. In the early stage of hydrostatic compression below ∼1 GPa, relative decrease in the ellipticity of the non-planar 10-rings is observed, which is then reverted to a gradual increase in the ellipticity at higher pressures above ∼1 GPa, implying a change in the compression mechanism. In a Sr-exchanged sample (Sr5Ga10Si22O64·19H2O), on the other hand, no initial volume expansion is observed. Instead, a change in the slope of volume contraction is observed near 1.5 GPa, which leads to a 2-fold increase in the compressibility. This is interpreted as pressure-induced rearrangement of water molecules to facilitate further volume contraction at higher pressures. 相似文献
19.
Wout De Nolf Jakub Jaroszewicz Roberto Terzano Ole Christian Lind Brit Salbu Bart Vekemans Koen Janssens Gerald Falkenberg 《Spectrochimica Acta Part B: Atomic Spectroscopy》2009,64(8):775
The performance of a combined microbeam X-ray fluorescence/X-ray powder diffraction (XRF/XRPD) measurement station at Hamburger Synchrotronstrahlungslabor (HASYLAB) Beamline L is discussed in comparison to that at European Synchrotron Radiation Facility (ESRF) ID18F/ID22. The angular resolution in the X-ray diffractograms is documented when different combinations of X-ray source, optics and X-ray diffraction detectors are employed. Typical angular resolution values in the range 0.3–0.5° are obtained at the bending magnet source when a ‘pink’ beam form of excitation is employed. A similar setup at European Synchrotron Radiation Facility beamlines ID18F and ID22 allows to reach angular resolution values of 0.1–0.15°. In order to document the possibilities and limitations for speciation of metals in environmental materials by means of Hamburger Synchrotronstrahlungslabor Beamline L X-ray fluorescence/X-ray powder diffraction setup, two case studies are discussed, one involved in the identification of the crystal phases in which heavy metals such as chromium, iron, barium and lead are present in polluted soils of an industrial site (Val Basento, Italy) and another involved in the speciation of uranium in depleted uranium particles (Ceja Mountains, Kosovo). In the former case, the angular resolution is sufficient to allow identification of most crystalline phases present while in the latter case, it is necessary to dispose of an angular resolution of ca. 0.2° to distinguish between different forms of oxidized uranium. 相似文献
20.
D.C. Creagh 《Radiation Physics and Chemistry》2005,74(6):426-442
All societies attempt to preserve their cultural heritage because it is this that gives them their identity. How artefacts are identified as being of significance to society, and how to preserve these for posterity, depend on the sophistication of those societies, their wealth, and the determination of members of the societies to preserve their past. If conservation or restoration measures are being undertaken complex analytical experiments must be undertaken beforehand to ensure that the work is being undertaken in an appropriate manner. These investigations may employ electromagnetic (IR, VIS, UV, X-ray, γ-ray) or particulate (electron, proton, neutron, and ion beams) radiation. The use of many of these techniques is described in this paper in experiments on Australian Aboriginal bark paintings, a suit of armour belonging to a famous Australian outlaw, and the degradation of colour motion picture film. 相似文献