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Powder Diffractometer (powder + diffractometer)
Selected AbstractsIn-house characterization of protein powderJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 4 2010Christian Grundahl Hartmann X-ray powder diffraction patterns of lysozyme and insulin were recorded on a standard in-house powder diffractometer. The experimental powder diffraction patterns were compared with patterns calculated from Protein Data Bank coordinate data. Good agreement was obtained by including straightforward corrections for background, unit-cell parameters, disordered bulk solvent and geometric factors. In particular the solvent correction was found crucial for a good agreement. A revised Lorentz factor was derived, which gave a minor, but significant, improvement to the fit in the low-angle region. An attempt to include calculated H-atom positions did not improve the overall fit and was abandoned. The method devised was shown to be a quick and convenient tool for distinguishing precipitates and polymorphs of proteins. [source] A 100-position robotic sample changer for powder diffraction with low-background vacuum chamberJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 2 2010S. R. Olsen At the new Australian OPAL research reactor, experiments carried out at room temperature use a substantial fraction of beam time on the high-resolution powder diffractometer, Echidna. With an average data collection time of 2,h and a complicated safety interlock system to protect users, the need for a fully automated and remotely controlled system was quickly realized. This report presents a solution based on a commercial four-axis robot capable of loading samples from two 50-position sample trays, in any order, into an automatically evacuated chamber. This chamber significantly reduced background signal arising from air scattering, with the effect being especially pronounced at low and high 2, angles. In the case of textured or inhomogeneous samples, the system may be re-configured so that the robot rotates the sample in the beam or translates it vertically through the beam. [source] Management of metadata and automation for mail-in measurements with the APS 11-BM high-throughput, high-resolution synchrotron powder diffractometerJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 6 2009Brian H. Toby A high-resolution and high-throughput synchrotron powder diffractometer has been automated for use with samples that are mailed in by Advanced Photon Source users. Implementation of a relational database with web interfaces for both outside users and beamline staff, which is integrated into the facility-wide proposal and safety system, allows all aspects of beamline management to be integrated. This system permits users to request kits for mounting samples, to provide sample safety information, to obtain their collected data and to provide usage information upon project completion in a quick and simple manner. Beamline staff use a separate interface to note receipt of samples, schedule and collect diffraction data, post-process and quality-check data, and dispose of samples. The design of the software and database are discussed in detail. [source] POWTEX , the high-intensity time-of-flight diffractometer at FRM II for structure analysis of polycrystalline materialsJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 5 2008Harald Conrad In order to provide the large chemistry and materials science as well as the geosciences communities with a powerful tool for rapid data acquisition, a time-of-flight powder diffractometer to be installed at the new Munich reactor has been designed. The time-of-flight technique is expected to outperform a monochromator instrument by at least an order of magnitude in data acquisition time, particularly on small samples of less than a cubic centimetre. The construction of this innovative type of diffractometer utilizes modern components such as focusing super-mirror neutron guides, a four-unit high-speed disk chopper system and linear position-sensitive detectors covering a solid angle of about 2, steradian. The diffractometer design enables an easy enlargement of the focal spot size and is therefore equally well suited for the texture analysis of large geological and archaeological samples. [source] Symmetrization of diffraction peak profiles measured with a high-resolution synchrotron X-ray powder diffractometerJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 1 2006H. Hibino The asymmetry of diffraction peak profiles observed with a high-resolution synchrotron powder X-ray diffractometer has been successfully removed by a double deconvolution method. In the first step, the asymmetry caused by the axial divergence aberration of the diffractometer is removed by a whole-pattern deconvolution method based on an a priori theoretical model for the aberration. In the second step, the residual asymmetry, the origin of which can be ascribed to the aberrations of the beamline optics, is also removed by a whole-pattern deconvolution method, based on an empirical model derived from the analysis of experimental diffraction peak profiles of a standard Si powder (NIST SRM640b). The beamline aberration has been modelled by the convolution of a pseudo-Voigt or Voigt function with an exponential distribution function. It has been found that the angular dependence of the asymmetry parameter in the exponential function is almost proportional to tan,, which supports the idea that the residual asymmetry should be ascribed mainly to the intrinsic asymmetry in the spectroscopic distribution of the source X-ray supplied by the beamline optics of the synchrotron facility. Recently developed procedures of whole-pattern deconvolution have been improved to treat the singularity of the instrumental function in the measured angular range. Formulae for the whole-pattern deconvolution based on the Williamson,Hall-type dependence of the width parameter of the instrumental function have also been developed. The method was applied to the diffraction intensity data of a standard ZnO powder sample (NIST SRM674) measured with a high-resolution powder diffractometer on beamline BL4B2 at the Photon Factory. The structure parameters of ZnO were refined from the integrated peak intensities, which were extracted by an individual profile fitting method applying symmetric profile models. The refined structure parameters coincide fairly well with those obtained from single-crystal data. [source] Deconvolution of instrumental aberrations for synchrotron powder X-ray diffractometryJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 2 2003T. Ida A method to remove the effects of instrumental aberrations from the whole powder diffraction pattern measured with a high-resolution synchrotron powder diffractometer is presented. Two types of asymmetry in the peak profiles caused by (i) the axial-divergence aberration of the diffractometer (diffractometer aberration) and (ii) the aberration of the monochromator and focusing optics on the beamline (beamline aberration) are both taken into account. The method is based on the whole-pattern deconvolution by Fourier technique combined with the abscissa-scale transformation appropriate for each instrumental aberration. The experimental powder diffraction data of LaB6 (NIST SRM660) measured on beamline BL-4B2 at the Photon Factory in Tsukuba have been analysed by the method. The formula of the scale transformation for the diffractometer aberration has a priori been derived from the instrumental function with geometric parameters of the optics. The strongly deformed experimental peak profiles at low diffraction angles have been transformed to sharp peak profiles with less asymmetry by the deconvolution of the diffractometer aberration. The peak profiles obtained by the deconvolution of the diffractometer aberration were modelled by an asymmetric model profile function synthesized by the convolution of the extended pseudo-Voigt function and an asymmetric component function with an empirical asymmetry parameter, which were linearly dependent on the diffraction angle. Fairly symmetric peak profiles have been obtained by further deconvolution of the empirically determined asymmetric component of the beamline aberration. [source] A twelve-analyzer detector system for high-resolution powder diffractionJOURNAL OF SYNCHROTRON RADIATION, Issue 5 2008Peter L. Lee A dedicated high-resolution high-throughput X-ray powder diffraction beamline has been constructed at the Advanced Photon Source (APS). In order to achieve the goals of both high resolution and high throughput in a powder instrument, a multi-analyzer detector system is required. The design and performance of the 12-analyzer detector system installed on the powder diffractometer at the 11-BM beamline of APS are presented. [source] Preparation, Characterization, and Photocatalytic Properties of CaNb2O6 NanoparticlesJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 2 2009In-Sun Cho CaNb2O6 nanoparticles with a size range of 30,50 nm were synthesized by heat treatment at 600°C after a solvothermal process and their optical and photocatalytic properties were investigated. The prepared powders were characterized by X-ray powder diffractometer, field-emission scanning electron microscope, transmission electron microscope, UV-Vis diffuse reflectance spectroscopy, Fluorescence spectroscopy, and Raman spectroscopy. Compared with a powder of the same material prepared by a solid-state reaction (SS) method, the nanoparticles exhibited a higher Brunauer,Emmett,Teller (BET) surface area, more efficient light absorption, and enhanced photocatalytic activity for producing H2 from pure water under UV irradiation. The photoluminescence spectra revealed that a radiative recombination process is dominant in the powder prepared by the SS method (strong blue emission at 300 K) under UV light irradiation, while no obvious emission was observed in the nanoparticles. This decrease of the radiative recombination as well as the higher optical absorption ability and higher BET surface area resulting from the reduced dimensionality led to enhanced photocatalytic activity of the nanoparticles. [source] An in situ method for the study of strain broadening using synchrotron X-ray diffractionJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 4 2007C. C. Tang A tensonometer for stretching metal foils has been constructed for the study of strain broadening in X-ray diffraction line profiles. This device, which is designed for use on powder diffractometers and was tested on Station 2.3 at Daresbury Laboratory, allows in situ measurements to be performed on samples under stress. It can be used for data collection in either transmission or reflection modes using either symmetric or asymmetric diffraction geometries. As a test case, measurements were carried out on an 18,µm-thick copper foil experiencing strain levels of up to 5% using both symmetric reflection and symmetric transmission diffraction. All the diffraction profiles displayed peak broadening and asymmetry which increased with strain. The measured profiles were analysed by the fundamental-parameters approach using the TOPAS peak-fitting software. All the observed broadened profiles were modelled by convoluting a refineable diffraction profile, representing the dislocation and crystallite size broadening, with a fixed instrumental profile predetermined using high-quality LaB6 reference powder. The deconvolution process yielded `pure' sample integral breadths and asymmetry results which displayed a strong dependence on applied strain and increased almost linearly with applied strain. Assuming crystallite size broadening in combination with dislocation broadening arising from f.c.c. a/2,110,{111} dislocations, the variation of mechanical property with strain has been extracted. The observation of both peak asymmetry and broadening has been interpreted as a manifestation of a cellular structure with cell walls and cell interiors possessing high and low dislocation densities. [source] A simple and low-cost solution for the automation of X-ray powder diffractometers with chart recorder outputJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 4 2006M. Jayaprakasan X-ray powder diffraction is an established method for the qualitative identification of crystalline materials and their quantitative analysis. The new generation of X-ray diffraction systems are based on expensive digital/embedded control technology and computer interfaces. Yet many laboratories use conventional manual-controlled systems with XY strip-chart recorders. Since the output spectrum is a strip chart (hard copy), raw data, essential for structural and qualitative analysis, are not readily available for further analysis. Upgrading to modern computerized diffractometers is very expensive. The proposed automation design described here is intended to enable the conventional diffractometer user to collect, store and analyze data quickly. The design also improves the resolution by five times compared with the conventional setup. For the automation, a PC add-on card has been designed to control and collect the timing and intensity counts from the conventional X-ray diffractometer, and suitable software has been developed to collect, process and present the X-ray diffraction data for both qualitative and quantitative analysis. Moreover, a major advantage of this design is that it does not warrant any physical modification of the hardware of the conventional setup; it is simply an extension to enhance the performance of collecting raw data with a higher resolution at desired intervals/timings. [source] Divergence-slit intensity corrections for Bragg,Brentano diffractometers with circular sample surfaces and known beam intensity distributionJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 3 2004H. Krüger Bragg,Brentano powder diffractometers equipped with fixed-divergence slits show a loss of intensity at small 2, angles as a result of the overflow of the beam exceeding the sample surface. To correct this effect, geometrically derived algorithms are presented to calculate correction factors for circular sample surfaces. It is shown that the algorithms for rectangular samples can be applied to circular samples with sufficient accuracy if the value for the length of the sample is replaced by a value intermediate between the diameter of the circular sample and the length of the corresponding rectangular sample. Inhomogeneous beam intensity distribution also has serious effects on the correction factors, especially for wide divergence-slit apertures. [source] Scan profiles for neutron spectrometers.JOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 5 2003`Acceptance diagrams' are a powerful graphical method of describing beam characteristics on neutron scattering instruments. Recent examples of the technique have used hypothetical rectangular-profile beam elements, not the conventional Gaussian profiles, to clarify the description. This article develops the method for Gaussian-profile beam elements and shows that it gives identical results to accepted techniques. Direct expressions are presented for scan profiles, their widths and intensities for both powder diffractometers and three-axis spectrometers. This work gives some necessary background and therefore forms the first part of a discussion of the resolution effects of the new reflecting Soller collimators for neutrons. [source] Scan profiles for neutron spectrometers.JOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 5 2003The recent development of neutron collimators with rectangular transmission profiles (intensity versus angular divergence) extends hope of improved count rates on neutron scattering instruments. It is usually assumed that a more effective use of beam angular spread in these devices should increase count rates by about a factor of two. However, real beams have both angular and wavevector spread and both these spreads are governed by the allowed collimation. In this extended view, the gains from ideal rectangular-profile elements (angle filters) are shown to be much larger (about a factor of four). The mirror reflections used to achieve the rectangular profiles in real devices complicate the resolution effects. Specifically, the reflections disturb the wavevector,angular divergence correlation in the beams, leading to unusual peak shapes characterized by triple peaks on powder diffractometers. Thus, these reflecting collimators are likely to be universally useful only before the monochromator and immediately preceding the detector, where wavevector,angle correlations have no effect. This reduces the potential gains to a factor of two or so. Note that the gains are as previously expected but for quite different reasons than imagined. This remains a very significant gain in a field where most work is intensity-limited. [source] Scan profiles for neutron spectrometers.JOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 5 2003Newly developed reflecting neutron collimators promise increased detector count rates in a field where most work is intensity-limited. The effects of such elements on instrument resolution are complicated and appear to be even more subtle than previously imagined. Numerical tests using the McSTAS ray-tracing program (http://neutron.risoe.dk/mcstas) are reported which support and extend the recent analysis of these effects. If reflecting collimators are used in all instrument positions they give unusual scan profiles. Using reflecting collimators only before the monochromator and immediately before the detector has no deleterious resolution effects and increases count rates by a factor of more than two on powder diffractometers. [source] | ||||||||||