http://journals.iucr.org/j/issues/2012/01/00/isscontsbdy.html Journal of Applied Crystallography covers a wide range of crystallographic topics from the viewpoints of both techniques and theory. The journal presents papers on the application of crystallographic techniques and on the related apparatus and computer software. For many years, the Journal of Applied Crystallography has been the main vehicle for the publication of small-angle scattering papers and powder diffraction techniques. The journal is the primary place where crystallographic computer program information is published. en Copyright (c) 2012 International Union of Crystallography 2012-02-01 International Union of Crystallography International Union of Crystallography http://journals.iucr.org urn:issn:0021-8898 Journal of Applied Crystallography covers a wide range of crystallographic topics from the viewpoints of both techniques and theory. The journal presents papers on the application of crystallographic techniques and on the related apparatus and computer software. For many years, the Journal of Applied Crystallography has been the main vehicle for the publication of small-angle scattering papers and powder diffraction techniques. The journal is the primary place where crystallographic computer program information is published. text/html Journal of Applied Crystallography, Volume 45, Part 1, 2012 text yearly 6 2002-02-01T00:00+00:00 1 45 2012-02-01 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography 1 urn:issn:0021-8898 med@iucr.org February 2012 2012-02-01 http://journals.iucr.org/logos/rss10j.gif http://journals.iucr.org/j/issues/2012/01/00/isscontsbdy.html Still image http://scripts.iucr.org/cgi-bin/paper?cg5193 The recently developed GEO-MIX-SELF approximation (GMS) is applied to interpret the pressure dependence of the longitudinal ultrasonic wave velocities in a polycrystalline graphite sample that has already been investigated in a wide range of experimental contexts. Graphite single crystals have extremely anisotropic elastic properties, making this sample a challenging test to demonstrate the potential of the GMS method. GMS combines elements of well known self-consistent algorithms and of the geometric mean approximation. It is able to consider mixtures of different polycrystalline phases, each with its own nonspherical grain shape and preferred orientation (texture). Pores and `cracks', typical for bulk graphite, are modeled as phases with `empty' grains. The pressure dependence (up to 150 MPa) of the experimental wave velocities can be well explained using the known texture of the sample by fitting the shape parameters and volume fractions of the graphite grains, cracks and spherical pores. The pressure dependence of these parameters describes a reasonable scenario for the closing of the cracks and pores with increasing pressure. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Matthies, S. 2011-12-13 doi:10.1107/S002188981104338X International Union of Crystallography A combination of self-consistent and geometric mean algorithms is applied to describe the pressure-dependent anisotropic elastic properties of a textured reactor graphite sample. The experimental sound velocities can reasonably be explained by a system of differently oriented extremely anisotropic flat grains, flat micropores (cracks) and spherical macropores with comparable volume fractions in the porous (∼20%) sample. EN GEO-MIX-SELF polycrystalline materials elastic properties pressure dependence The recently developed GEO-MIX-SELF approximation (GMS) is applied to interpret the pressure dependence of the longitudinal ultrasonic wave velocities in a polycrystalline graphite sample that has already been investigated in a wide range of experimental contexts. Graphite single crystals have extremely anisotropic elastic properties, making this sample a challenging test to demonstrate the potential of the GMS method. GMS combines elements of well known self-consistent algorithms and of the geometric mean approximation. It is able to consider mixtures of different polycrystalline phases, each with its own nonspherical grain shape and preferred orientation (texture). Pores and `cracks', typical for bulk graphite, are modeled as phases with `empty' grains. The pressure dependence (up to 150 MPa) of the experimental wave velocities can be well explained using the known texture of the sample by fitting the shape parameters and volume fractions of the graphite grains, cracks and spherical pores. The pressure dependence of these parameters describes a reasonable scenario for the closing of the cracks and pores with increasing pressure. text/html GEO-MIX-SELF calculations of the elastic properties of a textured graphite sample at different hydrostatic pressures text 1 45 2011-12-13 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 1 16 http://scripts.iucr.org/cgi-bin/paper?rw5007 An unexpected precipitate phase was observed in Mg–20 wt% Dy alloy, with a cuboid morphology not compatible with any shown in the Mg–Dy binary phase diagram. As observed by scanning electron microscopy and energy-dispersive X-ray analysis, the ratio of atomic percent of Dy to Mg is very high in these particles, probably largely because of the poor spatial resolution of that technique but already showing the mismatch with any previously characterized Mg–Dy compound. High-brilliance synchrotron diffraction and transmission electron microscopy experiments confirmed that these particles are composed of DyH2. They are formed during sample preparation at room temperature when hydrogen-containing sources such as water are used. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Gan, W. Huang, Y. Yang, L. Kainer, K.U. Jiang, M. Brokmeier, H.-G. Hort, N. 2011-12-22 doi:10.1107/S0021889811053088 International Union of Crystallography High-brilliance synchrotron radiation was used to indentify an unexpected DyH2 precipitate in Mg–20 wt% Dy alloy. This precipitate can be formed at room temperature, and its formation mechanism was further clarified. EN magnesium alloys hydrogen intermetallic compounds synchrotron diffraction An unexpected precipitate phase was observed in Mg–20 wt% Dy alloy, with a cuboid morphology not compatible with any shown in the Mg–Dy binary phase diagram. As observed by scanning electron microscopy and energy-dispersive X-ray analysis, the ratio of atomic percent of Dy to Mg is very high in these particles, probably largely because of the poor spatial resolution of that technique but already showing the mismatch with any previously characterized Mg–Dy compound. High-brilliance synchrotron diffraction and transmission electron microscopy experiments confirmed that these particles are composed of DyH2. They are formed during sample preparation at room temperature when hydrogen-containing sources such as water are used. text/html Identification of unexpected hydrides in Mg–20 wt% Dy alloy by high-brilliance synchrotron radiation text 1 45 2011-12-22 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 17 21 http://scripts.iucr.org/cgi-bin/paper?ks5301 Anisotropic broadening correction in X-ray powder diffraction by an ellipsoidal formula is applied on samples with nanosized crystals. Two cases of minerals with largely anisotropic crystallite shapes are presented. The properly applied formalism not only improves the fitting of the theoretical and observed diffraction diagrams but also gives direct information about realistic crystallite shapes and sizes. The approach is demonstrated using the Rietveld refinement program TOPAS and it is easily adaptable to other similar software. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Katerinopoulou, A. Balic-Zunic, T. Lundegaard, L.F. 2012-01-14 doi:10.1107/S0021889811055075 International Union of Crystallography An ellipsoidal formula for the correction of anisotropic broadening in X-ray powder diffraction on samples with nanosized crystals has been applied. Information about crystallite shapes and sizes provided by the method is verified by imaging techniques. EN anisotropic line broadening ellipsoidal formula crystallite size crystallite shape X-ray powder diffraction Anisotropic broadening correction in X-ray powder diffraction by an ellipsoidal formula is applied on samples with nanosized crystals. Two cases of minerals with largely anisotropic crystallite shapes are presented. The properly applied formalism not only improves the fitting of the theoretical and observed diffraction diagrams but also gives direct information about realistic crystallite shapes and sizes. The approach is demonstrated using the Rietveld refinement program TOPAS and it is easily adaptable to other similar software. text/html Application of the ellipsoid modeling of the average shape of nanosized crystallites in powder diffraction text 1 45 2012-01-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 22 27 http://scripts.iucr.org/cgi-bin/paper?to5004 An in situ energy-dispersive X-ray diffraction experiment was undertaken on operational titanium electrowinning cells to observe the formation of rutile (TiO2) passivation layers on Magnéli-phase (TinO2n−1; n = 4–6) anodes and thus determine the relationship between passivation layer formation and electrolysis time. Quantitative phase analysis of the energy-dispersive data was undertaken using a crystal-structure-based Rietveld refinement. Layer formation was successfully observed and it was found that the rate of increase in layer thickness decreased with time, rather than remaining constant as observed in previous studies. The limiting step in rutile formation is thought to be the rate of solid-state diffusion of oxygen within the anode structure. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Rowles, M.R. Styles, M.J. Madsen, I.C. Scarlett, N.V.Y. McGregor, K. Riley, D.P. Snook, G.A. Urban, A.J. Connolley, T. Reinhard, C. 2011-12-13 doi:10.1107/S0021889811044104 International Union of Crystallography The formation of rutile passivation layers on Magnéli-phase anodes in an operational titanium electrowinning cell was observed by energy-dispersive X-ray diffraction. Quantitative phase analysis of the energy-dispersive data was undertaken using a crystal-structure-based Rietveld refinement and layer thicknesses were calculated. EN Rietveld refinement in situ energy-dispersive diffraction electrolysis An in situ energy-dispersive X-ray diffraction experiment was undertaken on operational titanium electrowinning cells to observe the formation of rutile (TiO2) passivation layers on Magnéli-phase (TinO2n−1; n = 4–6) anodes and thus determine the relationship between passivation layer formation and electrolysis time. Quantitative phase analysis of the energy-dispersive data was undertaken using a crystal-structure-based Rietveld refinement. Layer formation was successfully observed and it was found that the rate of increase in layer thickness decreased with time, rather than remaining constant as observed in previous studies. The limiting step in rutile formation is thought to be the rate of solid-state diffusion of oxygen within the anode structure. text/html Quantification of passivation layer growth in inert anodes for molten salt electrochemistry by in situ energy-dispersive diffraction text 1 45 2011-12-13 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 28 37 http://scripts.iucr.org/cgi-bin/paper?cg5198 A prototype X-ray pixel area detector (XPAD3.1) has been used for X-ray diffraction experiments with synchrotron radiation. The characteristics of this detector are very attractive in terms of fast readout time, high dynamic range and high signal-to-noise ratio. The prototype XPAD3.1 enabled various diffraction experiments to be performed at different energies, sample-to-detector distances and detector angles with respect to the direct beam, yet it was necessary to perform corrections on the diffraction images according to the type of experiment. This paper is focused on calibration and correction procedures to obtain high-quality scientific results specifically developed in the context of three different experiments, namely mechanical characterization of nanostructured multilayers, elastic–plastic deformation of duplex steel and growth of carbon nanotubes. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Le Bourlot, C. Landois, P. Djaziri, S. Renault, P.-O. Le Bourhis, E. Goudeau, P. Pinault, M. Mayne-L'Hermite, M. Bacroix, B. Faurie, D. Castelnau, O. Launois, P. Rouzière, S. 2011-12-13 doi:10.1107/S0021889811049107 International Union of Crystallography Corrections and image processing algorithms for data analysis with a prototype hybrid pixel detector are reported in the context of three different X-ray diffraction experiments with synchrotron radiation. EN synchrotron X-ray diffraction pixel area detectors calibration A prototype X-ray pixel area detector (XPAD3.1) has been used for X-ray diffraction experiments with synchrotron radiation. The characteristics of this detector are very attractive in terms of fast readout time, high dynamic range and high signal-to-noise ratio. The prototype XPAD3.1 enabled various diffraction experiments to be performed at different energies, sample-to-detector distances and detector angles with respect to the direct beam, yet it was necessary to perform corrections on the diffraction images according to the type of experiment. This paper is focused on calibration and correction procedures to obtain high-quality scientific results specifically developed in the context of three different experiments, namely mechanical characterization of nanostructured multilayers, elastic–plastic deformation of duplex steel and growth of carbon nanotubes. text/html Synchrotron X-ray diffraction experiments with a prototype hybrid pixel detector text 1 45 2011-12-13 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 38 47 http://scripts.iucr.org/cgi-bin/paper?to5009 Two static high-pressure X-ray diffraction (XRD) studies of potassium chlorate have been performed at pressures of up to ∼14.3 GPa in a diamond anvil cell at ambient temperature using the 16 ID-B undulator beamline at the Advanced Photon Source for the X-ray source. The first experiment was conducted to ascertain decomposition rates of potassium chlorate as a function of pressure. Below 2 GPa, the sample was observed to decompose rapidly in the presence of the X-ray beam and release oxygen. Above 2 GPa (near the phase I → phase II transition), the decomposition rate dramatically slowed so that good quality XRD patterns could be acquired. This suggests a phase-dependent decomposition rate. In the second study, X-ray diffraction spectra were collected at pressures from 2 to 14.3 GPa by aligning virgin portions of the sample into the focused X-ray beam at each pressure. The results suggest the co-existence of mixed monoclinic (I) and rhombohedral (II) phases of potassium chlorate near 2 GPa. At pressures beyond 4 GPa, the XRD patterns show a very good fit to KClO3 in the rhombohedral phase with space group R3m, in agreement with earlier studies. No further phase transitions were observed with pressure. Decompression of the sample to ambient pressure indicated mixed phases I and II coupled with a small amount of synchrotron X-ray-induced decomposition product. The equation of state within this pressure regime has been determined. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Pravica, M. Bai, L. Bhattacharya, N. 2011-12-22 doi:10.1107/S0021889811053957 International Union of Crystallography Two high-pressure X-ray diffraction studies were conducted on the important oxidizer potassium chlorate (KClO3) at 300 K. In the first study, the radiation-induced decomposition rate was observed to significantly diminish with pressure as the sample transformed from the monoclinic to the high-pressure rhombohedral phase, suggesting a phase-dependent decomposition rate, and in the second study, the equation of state was determined up to 14.3 GPa. EN high-pressure X-ray diffraction potassium chlorate decomposition Two static high-pressure X-ray diffraction (XRD) studies of potassium chlorate have been performed at pressures of up to ∼14.3 GPa in a diamond anvil cell at ambient temperature using the 16 ID-B undulator beamline at the Advanced Photon Source for the X-ray source. The first experiment was conducted to ascertain decomposition rates of potassium chlorate as a function of pressure. Below 2 GPa, the sample was observed to decompose rapidly in the presence of the X-ray beam and release oxygen. Above 2 GPa (near the phase I → phase II transition), the decomposition rate dramatically slowed so that good quality XRD patterns could be acquired. This suggests a phase-dependent decomposition rate. In the second study, X-ray diffraction spectra were collected at pressures from 2 to 14.3 GPa by aligning virgin portions of the sample into the focused X-ray beam at each pressure. The results suggest the co-existence of mixed monoclinic (I) and rhombohedral (II) phases of potassium chlorate near 2 GPa. At pressures beyond 4 GPa, the XRD patterns show a very good fit to KClO3 in the rhombohedral phase with space group R3m, in agreement with earlier studies. No further phase transitions were observed with pressure. Decompression of the sample to ambient pressure indicated mixed phases I and II coupled with a small amount of synchrotron X-ray-induced decomposition product. The equation of state within this pressure regime has been determined. text/html High-pressure X-ray diffraction studies of potassium chlorate text 1 45 2011-12-22 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 48 52 http://scripts.iucr.org/cgi-bin/paper?ks5294 A new crystallization system is described, which makes it possible to use an evaporation-based microfluidic crystallization technique for protein crystallization. The gas and water permeability of the used polydimethylsiloxane (PDMS) material enables evaporation of the protein solution in the microfluidic device. The rates of evaporation are controlled by the relative humidity conditions, which are adjusted in a precise and stable way by using saturated solutions of different reagents. The protein crystals could nucleate and grow under different relative humidity conditions. Using this method, crystal growth could be improved so that approximately 1 mm-sized lysozyme crystals were obtained more successfully than using standard methods. The largest lysozyme crystal obtained reached 1.57 mm in size. The disadvantage of the good gas permeability in PDMS microfluidic devices becomes an advantage for protein crystallization. The radius distributions of aggregrates in the solutions inside the described microfluidic devices were derived from in situ dynamic light scattering measurements. The experiments showed that the environment inside of the microfluidic device is more stable than that of conventional crystallization techniques. However, the morphological results showed that the protein crystals grown in the microfluidic device could lose their morphological stability. Air bubbles in microfluidic devices play an important role in the evaporation progress. A model was constructed to analyze the relationship of the rates of evaporation and the growth of air bubbles to the relative humidity. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Yu, Y. Wang, X. Oberthür, D. Meyer, A. Perbandt, M. Duan, L. Kang, Q. 2011-12-13 doi:10.1107/S0021889811048047 International Union of Crystallography A new crystallization system is described, which makes it possible to use an evaporation-based microfluidic crystallization technique for protein crystallization. Using this method, crystal growth could be improved so that approximately 1 mm-sized lysozyme crystals were obtained more successfully than using standard methods. EN microfluidics protein crystallization A new crystallization system is described, which makes it possible to use an evaporation-based microfluidic crystallization technique for protein crystallization. The gas and water permeability of the used polydimethylsiloxane (PDMS) material enables evaporation of the protein solution in the microfluidic device. The rates of evaporation are controlled by the relative humidity conditions, which are adjusted in a precise and stable way by using saturated solutions of different reagents. The protein crystals could nucleate and grow under different relative humidity conditions. Using this method, crystal growth could be improved so that approximately 1 mm-sized lysozyme crystals were obtained more successfully than using standard methods. The largest lysozyme crystal obtained reached 1.57 mm in size. The disadvantage of the good gas permeability in PDMS microfluidic devices becomes an advantage for protein crystallization. The radius distributions of aggregrates in the solutions inside the described microfluidic devices were derived from in situ dynamic light scattering measurements. The experiments showed that the environment inside of the microfluidic device is more stable than that of conventional crystallization techniques. However, the morphological results showed that the protein crystals grown in the microfluidic device could lose their morphological stability. Air bubbles in microfluidic devices play an important role in the evaporation progress. A model was constructed to analyze the relationship of the rates of evaporation and the growth of air bubbles to the relative humidity. text/html Design and application of a microfluidic device for protein crystallization using an evaporation-based crystallization technique text 1 45 2011-12-13 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 53 60 http://scripts.iucr.org/cgi-bin/paper?nb5006 Nanocrystalline Ni thin films have been produced by direct current electrodeposition with different additives and current density in order to obtain 〈100〉, 〈111〉 and 〈211〉 major fiber textures. The dislocation density, the Burgers vector population and the coherently scattering domain size distribution are determined by high-resolution X-ray diffraction line profile analysis. The substructure parameters are correlated with the strength of the films by using the combined Taylor and Hall–Petch relations. The convolutional multiple whole profile method is used to obtain the substructure parameters in the different coexisting texture components. A strong variation of the dislocation density is observed as a function of the deposition conditions. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Csiszár, G. Pantleon, K. Alimadadi, H. Ribárik, G. Ungár, T. 2012-01-14 doi:10.1107/S0021889811053234 International Union of Crystallography The method and software of extended convolutional multiple whole profile (eCMWP) line profile analysis is used to determine the substructure in different texture components in terms of dislocation densities, subgrain size and twin boundary densities in nanocrystalline Ni thin films with different fiber textures. The diffraction patterns are measured in a high-angular-resolution X-ray diffractometer with almost parallel beam geometry, where the specimens are stationarily oriented for the hkl peaks corresponding to the different texture components. EN nanocrystalline Ni films dislocation densities Burgers vector population X-ray line profile analysis Nanocrystalline Ni thin films have been produced by direct current electrodeposition with different additives and current density in order to obtain 〈100〉, 〈111〉 and 〈211〉 major fiber textures. The dislocation density, the Burgers vector population and the coherently scattering domain size distribution are determined by high-resolution X-ray diffraction line profile analysis. The substructure parameters are correlated with the strength of the films by using the combined Taylor and Hall–Petch relations. The convolutional multiple whole profile method is used to obtain the substructure parameters in the different coexisting texture components. A strong variation of the dislocation density is observed as a function of the deposition conditions. text/html Dislocation density and Burgers vector population in fiber-textured Ni thin films determined by high-resolution X-ray line profile analysis text 1 45 2012-01-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 61 70 http://scripts.iucr.org/cgi-bin/paper?cg5201 The formation of GeSi nanoparticles on an SiO2 matrix is studied here by synchrotron-based techniques. The shape, average diameter and size dispersion were obtained from grazing-incidence small-angle X-ray scattering data. X-ray diffraction measurements were used to obtain crystallite sizes and composition via resonant (anomalous) measurements. By using these techniques as input for extended X-ray absorption fine structure analysis, the local composition surrounding the Ge atoms is investigated. Although the results for each of the methods above are commonly analyzed separately, the combination of such techniques leads to an improved understanding of nanoparticle structural and chemical properties. Crucial indirect parameters that cannot be quantified by other means are accessed in this work, such as local strain, the possibility of forming core–shell structures, the fraction of Ge atoms diluted in the matrix (not forming nanoparticles), the amorphous and crystalline Ge fractions, and the relative population of nanoparticles with single and multiple crystalline domains. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Gasperini, A. Malachias, A. Fabbris, G. Kellermann, G. Gobbi, A. Avendaño, E. Azevedo, G. de M. 2011-12-13 doi:10.1107/S0021889811049302 International Union of Crystallography GeSi nanoparticles were characterized by grazing-incidence small-angle X-ray scattering, X-ray diffraction and extended X-ray absorption fine structure spectroscopy. Besides direct measurements, important indirect results only accessible by combining the results of the various techniques have been obtained. EN GeSi nanoparticles X-ray diffraction anomalous diffraction grazing-incidence small-angle X-ray scattering extended X-ray absorption fine structure The formation of GeSi nanoparticles on an SiO2 matrix is studied here by synchrotron-based techniques. The shape, average diameter and size dispersion were obtained from grazing-incidence small-angle X-ray scattering data. X-ray diffraction measurements were used to obtain crystallite sizes and composition via resonant (anomalous) measurements. By using these techniques as input for extended X-ray absorption fine structure analysis, the local composition surrounding the Ge atoms is investigated. Although the results for each of the methods above are commonly analyzed separately, the combination of such techniques leads to an improved understanding of nanoparticle structural and chemical properties. Crucial indirect parameters that cannot be quantified by other means are accessed in this work, such as local strain, the possibility of forming core–shell structures, the fraction of Ge atoms diluted in the matrix (not forming nanoparticles), the amorphous and crystalline Ge fractions, and the relative population of nanoparticles with single and multiple crystalline domains. text/html Investigation of indirect structural and chemical parameters of GeSi nanoparticles in a silica matrix by combined synchrotron radiation techniques text 1 45 2011-12-13 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 71 84 http://scripts.iucr.org/cgi-bin/paper?he5534 The micro- and nanofocus X-ray scattering (MINAXS) beamline of PETRA III is equipped with two consecutively arranged endstations, the last of which is the nanofocus endstation. The first in-beam commissioning of the experimental equipment was successfully performed at the end of 2010, using two-dimensionally confining hard X-ray silicon waveguides with cross sections of 50 nm × 50 µm to 50 nm × 2 µm for nanobeam generation. A full characterization of the waveguide-generated beams was performed, giving values for the beam geometries, the transmission efficiencies of the waveguides and absolute fluxes. Along with these results a detailed description of the setup is presented in this paper. A first high-resolution nanodiffraction experiment on a nanocrystalline TiN hard coating was performed to verify the resolution of the nanodiffraction setup and to reveal the local gradients across the blasted TiN coating. In conclusion, the main concern is the availability of the nanobeam, how it was generated and the fact that a beam out of a two-dimensionally confining waveguide was used for diffraction experiments for the first time. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Krywka, C. Neubauer, H. Priebe, M. Salditt, T. Keckes, J. Buffet, A. Roth, S.V. Doehrmann, R. Mueller, M. 2011-12-13 doi:10.1107/S0021889811049132 International Union of Crystallography A characterization of the X-ray beam generated from differently sized two-dimensional waveguides was performed, giving values for the beam geometry, the transmission efficiency and absolute fluxes. A first high-resolution nanodiffraction experiment using the beam out of a two-dimensionally confining waveguide was performed on a nanocrystalline TiN hard coating in order to reveal the local gradients across the blasted coating. EN waveguides nanodiffraction The micro- and nanofocus X-ray scattering (MINAXS) beamline of PETRA III is equipped with two consecutively arranged endstations, the last of which is the nanofocus endstation. The first in-beam commissioning of the experimental equipment was successfully performed at the end of 2010, using two-dimensionally confining hard X-ray silicon waveguides with cross sections of 50 nm × 50 µm to 50 nm × 2 µm for nanobeam generation. A full characterization of the waveguide-generated beams was performed, giving values for the beam geometries, the transmission efficiencies of the waveguides and absolute fluxes. Along with these results a detailed description of the setup is presented in this paper. A first high-resolution nanodiffraction experiment on a nanocrystalline TiN hard coating was performed to verify the resolution of the nanodiffraction setup and to reveal the local gradients across the blasted TiN coating. In conclusion, the main concern is the availability of the nanobeam, how it was generated and the fact that a beam out of a two-dimensionally confining waveguide was used for diffraction experiments for the first time. text/html A two-dimensional waveguide beam for X-ray nanodiffraction text 1 45 2011-12-13 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 85 92 http://scripts.iucr.org/cgi-bin/paper?rg5004 Specialized software has been developed to calculate the absorption factor for the infinite-cylinder transmission Debye–Scherrer geometry (including inclined beams) to be used with two-dimensional area powder pattern registration. The diffracted beams are defined by the direction cosines in the laboratory Cartesian coordinate system. Modern two-dimensional area detectors have a large number of pixels, so an interpolation is made by the triangulation procedure to save computer time. The absorption correction is allowed for so that the intensity in each pixel is reduced on the same scale and the final diffraction-angle-dependent intensity, I(2θ), does not require any further absorption correction. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Sulyanov, S. Gogin, A. Boysen, H. 2011-12-13 doi:10.1107/S0021889811048217 International Union of Crystallography A method and software to calculate the absorption factor for the infinite-cylinder transmission Debye–Scherrer geometry with two-dimensional area powder pattern registration are presented. EN powder diffraction absorption correction two-dimensional area detectors Specialized software has been developed to calculate the absorption factor for the infinite-cylinder transmission Debye–Scherrer geometry (including inclined beams) to be used with two-dimensional area powder pattern registration. The diffracted beams are defined by the direction cosines in the laboratory Cartesian coordinate system. Modern two-dimensional area detectors have a large number of pixels, so an interpolation is made by the triangulation procedure to save computer time. The absorption correction is allowed for so that the intensity in each pixel is reduced on the same scale and the final diffraction-angle-dependent intensity, I(2θ), does not require any further absorption correction. text/html Spatial distribution of the absorption factor for an infinite cylindrical sample used with a two-dimensional area detector text 1 45 2011-12-13 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 93 97 http://scripts.iucr.org/cgi-bin/paper?kk5086 Multiple Bragg reflections (MBRs), which can be realized in a bent perfect crystal (BPC) slab and are mutually in dispersive diffraction geometry, provide a monochromatic beam of excellent resolution. After identifying many MBR effects in a BPC Si crystal by using the method of θ–2θD scanning, we have turned our attention to the study of selected effects using the method of azimuthal rotation of the crystal lattice around the scattering vector of the primary reflection for a fixed chosen wavelength. In this paper, several azimuthal scans with the intention of possible practical exploitation for very high resolution diffractometry are presented. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Mikula, P. Vrána, M. Šaroun, J. Davydov, V. Em, V. Seong, B.-S. 2012-01-04 doi:10.1107/S0021889811054124 International Union of Crystallography Multiple reflection effects in perfect crystals can be strongly enhanced by elastic bending. They can be used for high-resolution monochromatization. EN multiple reflection bent perfect crystals Ge crystals Si crystals Multiple Bragg reflections (MBRs), which can be realized in a bent perfect crystal (BPC) slab and are mutually in dispersive diffraction geometry, provide a monochromatic beam of excellent resolution. After identifying many MBR effects in a BPC Si crystal by using the method of θ–2θD scanning, we have turned our attention to the study of selected effects using the method of azimuthal rotation of the crystal lattice around the scattering vector of the primary reflection for a fixed chosen wavelength. In this paper, several azimuthal scans with the intention of possible practical exploitation for very high resolution diffractometry are presented. text/html Experimental studies of dispersive double reflections excited in cylindrically bent perfect-crystal slabs at a constant neutron wavelength text 1 45 2012-01-04 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 98 105 http://scripts.iucr.org/cgi-bin/paper?to5007 Combined refinements of local atomic structure that involve simultaneous fitting of powder-averaged and single-crystal data were implemented as an extension to the publicly available RMCProfile software. The refinements employ the reverse Monte Carlo method to fit neutron total scattering data, the neutron Bragg profile, extended X-ray absorption fine structure (EXAFS) and structured diffuse scattering in electron diffraction. The procedure was tested using simulated data generated for a realistic model of perovskite-like KNbO3, which exhibits strongly correlated Nb and O displacements. The results indicated that fitting the powder data (i.e. total scattering or total scattering plus EXAFS) alone fails to reproduce the nanoscale range of displacement correlations. Simultaneous fitting of the powder data and the patterns of diffuse intensity in single-crystal electron diffraction patterns returns significantly more accurate correlation characteristics. The approach and the computer software described in this contribution are not limited to electron diffraction patterns as other types of single-crystal diffraction data (i.e. X-ray or neutron) can be included in the fit. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Krayzman, V. Levin, I. 2012-01-14 doi:10.1107/S0021889812000398 International Union of Crystallography Combined refinements of local atomic structure that involve simultaneous fitting of powder-averaged and single-crystal data were implemented as an extension to the publicly available RMCProfile software. The procedure was tested using simulated data generated for a realistic model of perovskite-like KNbO3, which exhibits strongly correlated Nb and O displacements. EN reverse Monte Carlo RMCProfile nanoscale atomic correlations Combined refinements of local atomic structure that involve simultaneous fitting of powder-averaged and single-crystal data were implemented as an extension to the publicly available RMCProfile software. The refinements employ the reverse Monte Carlo method to fit neutron total scattering data, the neutron Bragg profile, extended X-ray absorption fine structure (EXAFS) and structured diffuse scattering in electron diffraction. The procedure was tested using simulated data generated for a realistic model of perovskite-like KNbO3, which exhibits strongly correlated Nb and O displacements. The results indicated that fitting the powder data (i.e. total scattering or total scattering plus EXAFS) alone fails to reproduce the nanoscale range of displacement correlations. Simultaneous fitting of the powder data and the patterns of diffuse intensity in single-crystal electron diffraction patterns returns significantly more accurate correlation characteristics. The approach and the computer software described in this contribution are not limited to electron diffraction patterns as other types of single-crystal diffraction data (i.e. X-ray or neutron) can be included in the fit. text/html Reverse Monte Carlo refinements of nanoscale atomic correlations using powder and single-crystal diffraction data text 1 45 2012-01-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 106 112 http://scripts.iucr.org/cgi-bin/paper?he5525 In this study, the change in internal lattice strain in an iron plate during tensile deformation was investigated by performing in situ measurements under applied force. The lattice strain was evaluated by neutron diffraction and Bragg-edge transmission. The neutron diffraction results showed that the averaged 110 lattice strain along the direction perpendicular to the applied force was between −422 and −109 × 10−6. The position dependence of the lattice strain and the change in the distribution of elastic strain in an iron plate with notches during tensile deformation was obtained by Bragg-edge transmission. It was also observed that, when the load increased over 30 kN, the area of plastic deformation increased around the positions of the notches. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Iwase, K. Sato, H. Harjo, S. Kamiyama, T. Ito, T. Takata, S. Aizawa, K. Kiyanagi, Y. 2012-01-14 doi:10.1107/S0021889812000076 International Union of Crystallography Lattice strain was determined by neutron transmission and diffraction during tensile testing. The position dependence of the lattice strain was clearly observed by Bragg-edge transmission. EN Bragg-edge transmission neutron diffraction in situ measurement lattice strain strain scanning strain mapping In this study, the change in internal lattice strain in an iron plate during tensile deformation was investigated by performing in situ measurements under applied force. The lattice strain was evaluated by neutron diffraction and Bragg-edge transmission. The neutron diffraction results showed that the averaged 110 lattice strain along the direction perpendicular to the applied force was between −422 and −109 × 10−6. The position dependence of the lattice strain and the change in the distribution of elastic strain in an iron plate with notches during tensile deformation was obtained by Bragg-edge transmission. It was also observed that, when the load increased over 30 kN, the area of plastic deformation increased around the positions of the notches. text/html In situ lattice strain mapping during tensile loading using the neutron transmission and diffraction methods text 1 45 2012-01-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography research papers 113 118 http://scripts.iucr.org/cgi-bin/paper?rg5006 Anomalous dispersion at the Si K absorption edge has been used to control the reflection from the interface between a film and an Si substrate, which otherwise complicates the nanostructure analysis of such a film, particularly for the soft-matter case, in grazing-incidence small-angle scattering. Such a reflectionless condition has been chosen for a triblock copolymer thin film, and two-dimensional grazing-incidence small-angle scattering patterns were obtained without the effect of the reflection. The present approach is useful for analysing nanostructures without introducing complicated corrections arising from the reflection. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Okuda, H. Takeshita, K. Ochiai, S. Kitajima, Y. Sakurai, S. Ogawa, H. 2011-12-13 doi:10.1107/S002188981105206X International Union of Crystallography Anomalous dispersion at the Si K edge is used to control the refractive index of an Si substrate to match that of a polymer thin film on its surface. Diffuse scattering from the film/substrate interface disappears at a photon energy very close to the Si absorption edge. EN grazing-incidence small-angle X-ray scattering anomalous scattering block copolymers soft X-rays Anomalous dispersion at the Si K absorption edge has been used to control the reflection from the interface between a film and an Si substrate, which otherwise complicates the nanostructure analysis of such a film, particularly for the soft-matter case, in grazing-incidence small-angle scattering. Such a reflectionless condition has been chosen for a triblock copolymer thin film, and two-dimensional grazing-incidence small-angle scattering patterns were obtained without the effect of the reflection. The present approach is useful for analysing nanostructures without introducing complicated corrections arising from the reflection. text/html Contrast matching of an Si substrate with polymer films by anomalous dispersion at the Si K absorption edge text 1 45 2011-12-13 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography short communications 119 121 http://scripts.iucr.org/cgi-bin/paper?fs5008 A method is derived to calculate the attenuation correction factors for elastic or inelastic X-ray or neutron scattering experiments using a spherical sample. The method can be applied to a sphere that is either fully or partially illuminated by an incident beam of rectangular cross-sectional area. The required input parameters are the energy-dependent attenuation coefficients, the radius of the sphere and the dimensions of the incident beam. In-plane scattering is assumed. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Zeidler, A. 2011-12-13 doi:10.1107/S0021889811050370 International Union of Crystallography A method is derived to calculate the attenuation correction factors for elastic or inelastic X-ray or neutron scattering experiments using a spherical sample that is fully or partially illuminated by an incident beam of rectangular cross-sectional area. EN X-ray scattering neutron scattering attenuation correction factors A method is derived to calculate the attenuation correction factors for elastic or inelastic X-ray or neutron scattering experiments using a spherical sample. The method can be applied to a sphere that is either fully or partially illuminated by an incident beam of rectangular cross-sectional area. The required input parameters are the energy-dependent attenuation coefficients, the radius of the sphere and the dimensions of the incident beam. In-plane scattering is assumed. text/html X-ray and neutron attenuation correction factors for spherical samples text 1 45 2011-12-13 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography short communications 122 123 http://scripts.iucr.org/cgi-bin/paper?he5539 Gravity distorts the circular contours found for small-angle neutron scattering data from azimuthally symmetric scattering systems when taken at long wavelength and with large wavelength spreads. The resolution is calculated for a Debye–Scherrer ring and compared with results from measurements taken on a sample of opal. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Mildner, D.F.R. Cubitt, R. 2012-01-14 doi:10.1107/S0021889812000945 International Union of Crystallography The resolution calculated for a Debye–Scherrer ring that includes the effect of gravity is compared with results from measurements taken on a sample of opal. EN Debye–Scherrer rings gravity long wavelengths scattering vectors small-angle neutron scattering Gravity distorts the circular contours found for small-angle neutron scattering data from azimuthally symmetric scattering systems when taken at long wavelength and with large wavelength spreads. The resolution is calculated for a Debye–Scherrer ring and compared with results from measurements taken on a sample of opal. text/html The effect of gravity on the Debye–Scherrer ring in small-angle neutron scattering text 1 45 2012-01-14 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography short communications 124 126 http://scripts.iucr.org/cgi-bin/paper?aj5185 This article describes the development of a curated online protein block sequence database, PDB-2-PB. The protein block sequences for protein structures with complete backbone coordinates have been encoded using the encoding procedure of de Brevern, Etchebest & Hazout [Proteins (2000), 41, 271–287]. In the current release of the PDB-2-PB database (version 1.0), the protein entries from a recent release of the World Wide Protein Data Bank (wwPDB), which has 74 297 solved PDB entries as of 7 July 2011, have been used as a primary source. The PDB-2-PB database stores the protein block sequences for all the chains present in a protein structure. PDB-2-PB version 1.0 has the curated protein block sequences for 103 252 PDB chain entries (93 547 X-ray, 7033 NMR and 2672 other experimental chain entries). From the PDB-2-PB database, users can extract the curated protein block sequence and its corresponding amino acid sequence, which is extracted from the PDB ATOM records. Users can download these sequences either by using the PDB code or by using various parameters listed in the database. The PDB-2-PB database is freely available at http://bioinfo.bdu.ac.in/~pb/. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Suresh, V. Ganesan, K. Parthasarathy, S. 2011-12-22 doi:10.1107/S0021889811052356 International Union of Crystallography A curated online protein block sequence database, PDB-2-PB, with user-friendly sequence retrieval systems has been developed. The options available in PDB-2-PB are used to extract the protein block sequence of a chain along with its corresponding chain information and amino acid sequence. EN protein block sequences databases local protein structures Protein Data Bank This article describes the development of a curated online protein block sequence database, PDB-2-PB. The protein block sequences for protein structures with complete backbone coordinates have been encoded using the encoding procedure of de Brevern, Etchebest & Hazout [Proteins (2000), 41, 271–287]. In the current release of the PDB-2-PB database (version 1.0), the protein entries from a recent release of the World Wide Protein Data Bank (wwPDB), which has 74 297 solved PDB entries as of 7 July 2011, have been used as a primary source. The PDB-2-PB database stores the protein block sequences for all the chains present in a protein structure. PDB-2-PB version 1.0 has the curated protein block sequences for 103 252 PDB chain entries (93 547 X-ray, 7033 NMR and 2672 other experimental chain entries). From the PDB-2-PB database, users can extract the curated protein block sequence and its corresponding amino acid sequence, which is extracted from the PDB ATOM records. Users can download these sequences either by using the PDB code or by using various parameters listed in the database. The PDB-2-PB database is freely available at http://bioinfo.bdu.ac.in/~pb/. text/html PDB-2-PB: a curated online protein block sequence database text 1 45 2011-12-22 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography computer programs 127 129 http://scripts.iucr.org/cgi-bin/paper?aj5181 Stereographic projection is one of the most powerful research tools for crystallography in materials science. A new program for full operation of stereographic projections and in-depth exploration of crystallographic orientation relationships is described. It is specifically designed for materials researchers who are in need of tools for extensive crystallographic analysis. The difference from other popular commercial software for crystallography is that this program provides new options for users to plot and fully control stereographic projections of an arbitrary pole centre for an arbitrary crystal structure and to illustrate composite stereographic projections, which are necessary to explore the orientation relationships between two phases. The program is able to perform a range of essential crystallographic calculations. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Liu, H. Liu, J. 2011-12-13 doi:10.1107/S0021889811049582 International Union of Crystallography A computer program is reported for plotting stereographic projection and exploring crystallographic orientation relationships. It offers a user-friendly interface to fully control stereographic projections of an arbitrary pole centre for an arbitrary crystal structure and to illustrate composite stereographic projections. EN stereographic projection orientation relationships computer programs Stereographic projection is one of the most powerful research tools for crystallography in materials science. A new program for full operation of stereographic projections and in-depth exploration of crystallographic orientation relationships is described. It is specifically designed for materials researchers who are in need of tools for extensive crystallographic analysis. The difference from other popular commercial software for crystallography is that this program provides new options for users to plot and fully control stereographic projections of an arbitrary pole centre for an arbitrary crystal structure and to illustrate composite stereographic projections, which are necessary to explore the orientation relationships between two phases. The program is able to perform a range of essential crystallographic calculations. text/html SP2: a computer program for plotting stereographic projection and exploring crystallographic orientation relationships text 1 45 2011-12-13 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography computer programs 130 134 http://scripts.iucr.org/cgi-bin/paper?nb5007 A low-budget automatic sample changer that allows the rapid analysis of powder or polycrystalline samples using an X-ray single-crystal diffractometer equipped with an area detector is here described. It uses control software that synchronizes the movement of a linear stage with the collection of frames by the diffractometer. Small pieces of thin solid samples are directly attached to a 30 cm ruler, which is used as a disposable magazine, while loose powder samples are loaded into holes on an acetate strip covered on both sides with Kapton tape and attached to the ruler. The use of this type of diffractometer with a sample changer is a simple, low cost and effective solution for studies requiring the analysis of a large number of samples by X-ray powder diffraction. With the current design up to 30 samples can be measured in a single experiment. The current sample changer was designed so that it can be fitted into a Bruker SMART APEX X-ray single-crystal diffractometer. However, it can be easily adapted to diffractometers from other makers. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Rodriguez-Navarro, A.B. Kudlacz, K. Ortega-Huertas, M. 2011-12-13 doi:10.1107/S0021889811048321 International Union of Crystallography A low-cost automatic sample changer for powder or polycrystalline samples is here described. The sample changer was designed so that it can be fitted into a Bruker SMART APEX X-ray single-crystal diffractometer, but it can be easily adapted to diffractometers from other makers. EN X-ray diffraction combinatorial chemistry rapid screening area detectors mineral phase identification A low-budget automatic sample changer that allows the rapid analysis of powder or polycrystalline samples using an X-ray single-crystal diffractometer equipped with an area detector is here described. It uses control software that synchronizes the movement of a linear stage with the collection of frames by the diffractometer. Small pieces of thin solid samples are directly attached to a 30 cm ruler, which is used as a disposable magazine, while loose powder samples are loaded into holes on an acetate strip covered on both sides with Kapton tape and attached to the ruler. The use of this type of diffractometer with a sample changer is a simple, low cost and effective solution for studies requiring the analysis of a large number of samples by X-ray powder diffraction. With the current design up to 30 samples can be measured in a single experiment. The current sample changer was designed so that it can be fitted into a Bruker SMART APEX X-ray single-crystal diffractometer. However, it can be easily adapted to diffractometers from other makers. text/html Automatic sample changer for the analysis of powder samples on an X-ray single-crystal diffractometer equipped with an area detector text 1 45 2011-12-13 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography laboratory notes 135 137 http://scripts.iucr.org/cgi-bin/paper?fs5009 A prototype jig to attach a protein crystallization plate to a standard X-ray goniometer has been designed and constructed in partnership with an engineering firm. This allows a low-cost implementation of in situ diffraction using the available home-laboratory X-ray source. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Hargreaves, D. 2011-12-22 doi:10.1107/S0021889811052654 International Union of Crystallography A prototype jig to attach a protein crystallization plate to a standard X-ray goniometer has been designed and constructed. This allows a low-cost implementation of in situ diffraction using the available home-laboratory X-ray source. EN in situ diffraction screening crystallization plates crystal quality room-temperature diffraction A prototype jig to attach a protein crystallization plate to a standard X-ray goniometer has been designed and constructed in partnership with an engineering firm. This allows a low-cost implementation of in situ diffraction using the available home-laboratory X-ray source. text/html A manual low-cost protein-crystallization plate jig for in situ diffraction in the home laboratory text 1 45 2011-12-22 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography laboratory notes 138 140 http://scripts.iucr.org/cgi-bin/paper?ks5310 Errors in the paper by Liu, Waclawik & Luo [J. Appl. Cryst. (2010), 43, 448–454] are corrected. Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Liu, H. Waclawik, E.R. Luo, C. 2012-01-04 doi:10.1107/S0021889811055087 International Union of Crystallography Errors in the paper by Liu, Waclawik & Luo [J. Appl. Cryst. (2010), 43, 448–454] are corrected. EN transformations invariant line analysis precipitation habit planes orientation relationships Errors in the paper by Liu, Waclawik & Luo [J. Appl. Cryst. (2010), 43, 448–454] are corrected. text/html A simplified invariant line analysis for face-centred cubic/body-centred cubic precipitation systems. Erratum text 1 45 2012-01-04 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography addenda and errata 141 141 http://scripts.iucr.org/cgi-bin/paper?me0458 Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 IUCr Editorial Office 2012-01-04 doi:10.1107/S0021889811044621 International Union of Crystallography Notes for authors. EN Notes for authors text/html Notes for authors 2012 text 1 45 2012-01-04 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography international union of crystallography 142 147 http://scripts.iucr.org/cgi-bin/paper?pf0090 Copyright (c) 2012 International Union of Crystallography urn:issn:0021-8898 Vtyurin, A. 2012-01-04 doi:10.1107/S0021889811051429 International Union of Crystallography EN text/html Concepts and Methods of 2D Infrared Spectroscopy. By Peter Hamm and Martin Zanni. Pp. 296, 124 illustrations, 71 exercises. Cambridge University Press, 2011. Price (hardcover) 99.00 USD. ISBN 978-1-107-00005-6. text 1 45 2012-01-04 Copyright (c) 2012 International Union of Crystallography Journal of Applied Crystallography book reviews 148 149