Powder diffraction software pattern

Powder diffraction studies with neutrons are perfonned both at nuclear reactors and at spallation sources. In both cases a cylindrical sample is observed by multiple detectors or, in some cases, by a curved, position-sensitive detector. In a powder diffractometer at a reactor, collimators and detectors at many different 20 angles are scaimed over small angular ranges to fill in the pattern. At a spallation source, pulses of neutrons of different wavelengdis strike the sample at different times and detectors at different angles see the entire powder pattern, also at different times. These slightly displaced patterns are then time focused , either by electronic hardware or by software in the subsequent data analysis. 

The X-ray powder diffraction (XRPD) pattern of a sample of atorvastatin calcium, Form-I, was recorded at room temperature on Bruker D8 Advance diffractometer (Karlsruhe, Germany), using nickel-filtered Cu Ka radiation. The sample was mounted in a polymethylmethacrylate sample holder, and analyzed in a continuous mode with a step size of 0.01° and a step time of 1 s over an angular range of 3-40° 26. The XRPD results are found in Fig. 1.18 and in Table 1.3, being evaluated with the DIFFRACplus EVA (version 9.0) diffraction software. 

Data collection software is generally supplied by the instrument manufacturers. This data collection software would also normally be equipped to perform preliminary analysis including peak finding routines and search/match of powder diffraction patterns from a database. The most popular database for powder diffraction data is maintained by the International Centre for Diffraction Data. ... 

Qualitative and quantitative analytical applications of X-ray diffraction both require reference diffraction patterns to identify and quantify the different polymorphic modifications. Experimental powder patterns may be suspect for their use as standards as a result of experimentally induced errors or aberrations or the lack of polymorphic purity in the sample itself (which may even result from the sample preparation). The availability of full crystal structure determinations for any or all of the polymorphic modifications can considerably facilitate generation of standard powder patterns. A variety of public domain software is now available for calculating powder diffraction patterns from single crystal data (ICDD 2001, lUCr 2001)." ... 

There is a variety of freely available software, which enables one to deconvolute a powder diffraction pattern and determine either or all individual intensities, lattice and peak shape function parameters, and observed structure factors of all possible Bragg reflections. Freeware codes include EXPO, FullProf, GSAS, LHPM-Rietica, and others. In addition to free programs, nearly all manufacturers of commercial powder diffractometers offer software for sale either as a package with the sale of the equipment or as stand-alone products. ... 

Most powder diffraction databases only serve angular dispersive X-ray diffraction. Energy dispersive X-ray diffraction data can be transformed into an angular dispersive equivalent that can then be used in conventional search-match software. Users of neutron diffraction data are currently limited to performing phase identification using a list of crystal structures imported into a Rietveld program. It is wise to first run samples destined for neutron diffraction sample in a powder XRD prior to confirm phase purity, and to use calculated patterns to assist in phase identification of possible undesired phases due to ancillary equipment or sample environment. 

Table 17.9 Available powder diffraction pattern viewing and processing software.

Although, the powder method was developed as early as 1916 by Debye and Scherrer, for more than 50 years its use was almost exclusively limited to qualitative and semi-quantitative phase analysis and macroscopic stress measurements. The main reason for this can be found in what is known as the principal problem of powder diffraction accidental and systematic peak overlap caused by a projection of three-dimensional reciprocal space on to the one-dimensional 26 axis, leading to a strongly reduced information content compared to a single crystal data set. However, despite the loss of angular information, often sufficient information resides in the ID dataset to reconstruct the 3D structure. Indeed, quantitative analysis of the pattern using modern computers and software yields the wealth of additional information about the sample structure that is illustrated in Figure 1. Modern... 

The powder X-ray diffraction patterns of the samples were recorded on a Philips PW 1820 diffractometer using nickel filtered Cu Ka radiation. The crystallinity of the samples was calculated by measuring the area under the (5 3 3) peak taking original NaY sample as reference. The unit cell size (So) of the samples were determined from XRD patterns using PDPll software. 

X-ray diffraction patterns were obtained with a Bruker D5005 Theta-Theta diffractometer equipped with a diffracted-beam graphite monochromator using Cu Ka radiation (1.54184 A). The data were collected by continuous scanning between 15 and 73° (20) with a counting time of 8 s per 0.02°. The recorded patterns were referred to the powder diffraction file PDF-2 Database (International Centre for Diffraction Data) for the identification of phases, using the software package DiffracPlus (Socabim-Bruker). 

IR and Raman may be used to confirm results obtained from structure prediction software. In a study on eniluracil [35], the crystal structure was predicted from the X-ray powder diffraction pattern. Two feasible crystal sttuctures were identified in which the hydrogen bonding pattern was very similar with only the orientation of the non-bonded carbonyl differing between the two. The IR and Raman spectra of eniluracil support the presence of such a... 

X-Ray Powder Diffraction. X-ray powder diffraction patterns were recorded with a Philips X-ray diffractometer PW1800 using the Cuk(x radiation (LFF tube, 40kV, 50 mA), a graphic back monochromator with automatic divergence slit (irradiated sample length 10 mm) and APD 1700 version 4.0 software. X-ray diffraction patterns, JCPDS files, and data from the literature were used to identify the crystallized phases obtained for randomly oriented samples. 

Powder X-ray diffraction patterns are the fingerprint of all crystalline substances. The technique is a rapid and powerful tool for identification of all crystalline compounds, and it is especially valuable in the presence of polymorphs or quasi-isochemical compounds, where chemical techniques cannot be applied. The data collection time of a medium-resolution powder diffraction pattern for identification purposes is typically of the order of 20-30 min. Identification of the unknowns in a compound composed of a few phases is a straight-forward automatic procedure in which the Bragg diffraction peaks in the observed pattern are matched against the reported powder diffraction patterns of all known crystalline substances in the powder diffraction file. Advanced computer software is available for such applications. 

H.M. Rietveld developed a practical method to analyze powder diffraction data. The Rietveld refinement method [6] is based on modeling a diffraction pattern according to structural information available for the phases previously identified in the pattern. This model is calculated by computer software after introduction of some crystallographic data space group symmetry, atomic species and positions within the cell, occupancies, lattice parameters, line broadening parameters, and experimental conditions. The term refinement refers to the cyclic improvement process used in the estimation of the set of parameters that can model the diffraction pattern as close as possible to the observed pattern. Usually, the Rietveld refinement is accomplished by minimizing the sum of the differences of calculated and observed intensities for each angular step of the diffraction pattern and by a... 

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