A system for collection and on-line integration of X-ray diffraction data from a multiwire area detector

1987 ◽  
Vol 20 (3) ◽  
pp. 235-242 ◽  
Author(s):  
M. Blum ◽  
P. Metcalf ◽  
S. C. Harrison ◽  
D. C. Wiley
Keyword(s):  
Diffraction Data ◽  
High Speed ◽  
X Ray Diffraction ◽  
Quality Of Data ◽  
X Ray ◽  
Camera Control ◽  
Area Detector ◽  
C Programming ◽  
On Line ◽  
Integrated Intensities

A system for collecting and measuring X-ray diffraction data from protein crystals has been developed for a multiwire area detector. Computer programs run concurrently on two microcomputers, which collect and reduce detector data to integrated intensities. The self-contained system consists of an X-ray area detector, a rotation/oscillation camera, and two microcomputers connected by a high-speed Ethernet network. One microcomputer is dedicated to operation of the detector, control of the camera, and storage of the raw data. The second microcomputer automatically integrates the data as they are collected and allows the user to monitor the quality of data as they are processed. The integration programs are written in Fortran 77 and have been designed to be portable. Additional programs for crystal alignment, detector and camera control, and graphics are written in the C programming language. A description of the system, some characteristics of the detector, and the results of data collection are presented.

scholarly journals HiSPoD: a program for high-speed polychromatic X-ray diffraction experiments and data analysis on polycrystalline samples

2016 ◽  
Vol 23 (4) ◽  
pp. 1046-1053 ◽  
Author(s):  
Tao Sun ◽  
Kamel Fezzaa
Keyword(s):  
Diffraction Data ◽  
High Speed ◽  
Short Pulse ◽  
Frame Rate ◽  
Short Exposure ◽  
X Rays ◽  
X Ray Diffraction ◽  
Short Exposure Time ◽  
X Ray ◽  
Structure Information

A high-speed X-ray diffraction technique was recently developed at the 32-ID-B beamline of the Advanced Photon Source for studying highly dynamic, yet non-repeatable and irreversible, materials processes. In experiments, the microstructure evolution in a single material event is probed by recording a series of diffraction patterns with extremely short exposure time and high frame rate. Owing to the limited flux in a short pulse and the polychromatic nature of the incident X-rays, analysis of the diffraction data is challenging. Here,HiSPoD, a stand-alone Matlab-based software for analyzing the polychromatic X-ray diffraction data from polycrystalline samples, is described. WithHiSPoD, researchers are able to perform diffraction peak indexing, extraction of one-dimensional intensity profiles by integrating a two-dimensional diffraction pattern, and, more importantly, quantitative numerical simulations to obtain precise sample structure information.

scholarly journals Automatic processing of macromolecular crystallography X-ray diffraction data at the ESRF

2013 ◽  
Vol 46 (3) ◽  
pp. 804-810 ◽  
Author(s):  
Stéphanie Monaco ◽  
Elspeth Gordon ◽  
Matthew W. Bowler ◽  
Solange Delagenière ◽  
Matias Guijarro ◽  
...  
Keyword(s):  
Diffraction Data ◽  
High Speed ◽  
Automatic Processing ◽  
European Synchrotron Radiation Facility ◽  
Macromolecular Crystallography ◽  
X Ray Diffraction ◽  
Computing Environment ◽  
X Ray ◽  
Standard Integration ◽  
Intuitive Manner

The development of automated high-intensity macromolecular crystallography (MX) beamlines at synchrotron facilities has resulted in a remarkable increase in sample throughput. Developments in X-ray detector technology now mean that complete X-ray diffraction datasets can be collected in less than one minute. Such high-speed collection, and the volumes of data that it produces, often make it difficult for even the most experienced users to cope with the deluge. However, the careful reduction of data during experimental sessions is often necessary for the success of a particular project or as an aid in decision making for subsequent experiments. Automated data reduction pipelines provide a fast and reliable alternative to user-initiated processing at the beamline. In order to provide such a pipeline for the MX user community of the European Synchrotron Radiation Facility (ESRF), a system for the rapid automatic processing of MX diffraction data from single and multiple positions on a single or multiple crystals has been developed. Standard integration and data analysis programs have been incorporated into the ESRF data collection, storage and computing environment, with the final results stored and displayed in an intuitive manner in the ISPyB (information system for protein crystallography beamlines) database, from which they are also available for download. In some cases, experimental phase information can be automatically determined from the processed data. Here, the system is described in detail.

Revision of the crystal structure of ulrichite, CaCu2+(UO2)(PO4)2·4H2O

2001 ◽  
Vol 65 (6) ◽  
pp. 717-724 ◽  
Author(s):  
U. Kolitsch ◽  
G. Giester
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Diffraction Data ◽  
X Ray Diffraction ◽  
Coordination Polyhedra ◽  
Space Group ◽  
X Ray ◽  
Bond Angles ◽  
Area Detector

AbstractThe crystal structure of ulrichite, CaCu2+(UO2)(PO4)2·4H2O (space group P21/c, a = 12.784(3), b = 6.996(1), c = 13.007(3)Å, β = 91.92(1)°, V = 1162.7(4)Å3, Z = 4) was redetermined using X-ray diffraction data measured from a twinned crystal with Mo-Kα radiation and a CCD area detector (2510 unique reflections with Fo > 4σ(Fo), R1 = 8.8%). Ulrichite crystallizes in space group P21/c rather than C2/m reported previously. The newly determined atomic positions give reasonable coordination polyhedra. One unique Ca atom is irregularly coordinated by eight O atoms (<Ca–O> = 2.46 Å). One unique U atom shows a {2+5} coordination with characteristic bond angles and lengths (1.806(11)Å, 1.842(12)Å and five bonds between 2.252(15) and 2.441(11)Å). Furthermore, the structure contains groups in which strongly elongated CuO6 ‘octahedra’ (also describable as CuO4 squares) are corner-linked to two PO4 tetrahedra via two opposite, equatorial O atoms. Edge- and corner-sharing UO7, CaO8 and PO4 polyhedra form heteropolyhedral sheets parallel to (001) that are linked to adjacent sheets via the CuO6 ‘octahedra’ and hydrogen bonds.

A new position sensitive area detector for high-speed and high-sensitivity X-ray diffraction analysis

2006 ◽  
Vol 21 (2) ◽  
pp. 97-101 ◽  
Author(s):  
Takeyoshi Taguchi
Keyword(s):  
High Speed ◽  
Scintillation Counter ◽  
High Sensitivity ◽  
Dislocation Network ◽  
Sensitive Area ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Area Detector ◽  
Position Sensitive

A state-of-art semiconductor technology-based position sensitive area detector, namely D/teX-25, has recently been developed for high-speed and high-sensitivity X-ray diffraction (XRD) analysis of materials. X-ray powder diffraction intensities obtained by a D/teX-25 detector were found to over 50 times higher than those by a conventional scintillation counter. A D/teX-25 detector mounted on a conventional 2 kW XRD system has been used to collect ultrafast XRD data with scanning speeds up to 160°2θ per minute. Ultrahigh-speed XRD is particularly useful for time-resolved dynamical and in-situ studies. A D/teX-25 detector was successfully used on a Rigaku XRD differential scanning calorimetry (DSC) system for simultaneous measurements of XRD and DSC data under controlled temperature and humidity conditions. This has made possible the study of complex and rapid phase transformations of pharmaceutical terfenadine. The D/teX-25 area detector has also been used for recording two-dimensional XRD patterns showing the particle-size effects on α-quartz powder intensities and to obtain digital X-ray topographic images of a complex dislocation network in a Si wafer.

scholarly journals X-ray Determination of Compressive Residual Stresses in Spring Steel Generated by High-Speed Water Quenching

Materials ◽  
2019 ◽  
Vol 12 (7) ◽  
pp. 1154
Author(s):  
Diego E. Lozano ◽  
George E. Totten ◽  
Yaneth Bedolla-Gil ◽  
Martha Guerrero-Mata ◽  
Marcel Carpio ◽  
...  
Keyword(s):  
Heat Treatment ◽  
Residual Stresses ◽  
High Speed ◽  
Spring Steel ◽  
X Ray Diffraction ◽  
Laboratory Equipment ◽  
X Ray ◽  
Water Chamber ◽  
Hardened Case ◽  
Compressive Residual Stresses

Automotive components manufacturers use the 5160 steel in leaf and coil springs. The industrial heat treatment process consists in austenitizing followed by the oil quenching and tempering process. Typically, compressive residual stresses are induced by shot peening on the surface of automotive springs to bestow compressive residual stresses that improve the fatigue resistance and increase the service life of the parts after heat treatment. In this work, a high-speed quenching was used to achieve compressive residual stresses on the surface of AISI/SAE 5160 steel samples by producing high thermal gradients and interrupting the cooling in order to generate a case-core microstructure. A special laboratory equipment was designed and built, which uses water as the quenching media in a high-speed water chamber. The severity of the cooling was characterized with embedded thermocouples to obtain the cooling curves at different depths from the surface. Samples were cooled for various times to produce different hardened case depths. The microstructure of specimens was observed with a scanning electron microscope (SEM). X-ray diffraction (XRD) was used to estimate the magnitude of residual stresses on the surface of the specimens. Compressive residual stresses at the surface and sub-surface of about −700 MPa were obtained.

scholarly journals High-pressure synthesis and crystal structure of the mixed-cation borate Ga4In4B15O33(OH)3

2019 ◽  
Vol 74 (4) ◽  
pp. 357-363
Author(s):  
Daniela Vitzthum ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
High Temperature ◽  
Diffraction Data ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Mixed Cation ◽  
High Pressure High Temperature ◽  
Pressure Synthesis

AbstractThe mixed cation triel borate Ga4In4B15O33(OH)3 was synthesized in a Walker-type multianvil apparatus at high-pressure/high-temperature conditions of 12.5 GPa and 1300°C. Although the product could not be reproduced in further experiments, its crystal structure could be reliably determined via single-crystal X-ray diffraction data. Ga4In4B15O33(OH)3 crystallizes in the tetragonal space group I41/a (origin choice 2) with the lattice parameters a = 11.382(2), c = 15.244(2) Å, and V = 1974.9(4) Å3. The structure of the quaternary triel borate consists of a complex network of BO4 tetrahedra, edge-sharing InO6 octahedra in dinuclear units, and very dense edge-sharing GaO6 octahedra in tetranuclear units.

Crystallization and preliminary x-ray diffraction data of the cryptomonad biliprotein phycocyanin-645 from a Chroomonas spec.

1984 ◽  
Vol 140 (2-3) ◽  
pp. 202-205 ◽  
Author(s):  
Walter Morisset ◽  
Werner Wehrmeyer ◽  
Tilman Schirmer ◽  
Wolfram Bode
Keyword(s):  
Diffraction Data ◽  
X Ray Diffraction ◽  
X Ray

Theoretically derived thermodynamic properties can be improved by the refinement of low-frequency modes against X-ray diffraction data

2021 ◽  
Author(s):  
Anna Agnieszka Hoser ◽  
Marcin Sztylko ◽  
Damian Trzybiński ◽  
Anders Østergaard Madsen
Keyword(s):  
Thermodynamic Properties ◽  
Dft Calculations ◽  
Diffraction Data ◽  
Molecular Crystals ◽  
Low Frequency ◽  
X Ray Diffraction ◽  
X Ray ◽  
Efficient Approach

A framework for estimation of thermodynamic properties for molecular crystals via refinement of frequencies from DFT calculations against X-ray diffraction data is presented. The framework provides an efficient approach to...

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