bluuebunny/crossref_metadata_2025 huggingface dataset:
Interactive Dialog for Phase Identification by the Johnson/Vand Program for X-Ray Diffraction Data
Authors: Wims Andrew M. , Johnson Gerald G.
Published: January 2013

A new, convenient program has been designed and implemented on a VAX computer to facilitate the use of the Johnson/Vand program (Version 21) for identifying components in crystalline mixtures by X-ray diffraction. (The data base of references is distributed solely by the JCPDS – International Centre for Diffraction Data.) This new program uses an easy-to-follow conversational mode of communication for setting up the input file for the identification program from a remote terminal. The program is menu driven with screens for input of sample information, for change of default computational parameters, and for handling the experimental diffraction data. Many of the input screens can be readily bypassed when the default parameters are acceptable. An editor feature is provided for viewing the final input file and for correcting the diffraction data.
Crystal Data for RuIn3
Authors: Roof R. B. , Fisk Z. , Smith J. L.
Published: January 2013

Crystal data for RuIn3 are reported. The material is tetragonal, , with a = 6.9983 (3), c = 7.2440 (4) Å, Vol = 354.78 Å3, Z = 4, Dc = 8.34 gm/cm3. It is isostructural with the compound CoGa3. The crystals of RuIn3, which form long needles, display electrical resistivity characteristics of a typical metal.

Intensity data were obtained from a diffractometer trace taken with CuKα radiation, λ = 1.54178 Å. The structure was refined by least-squares calculations to R1 = 0.116 with 53 observed reflections. Powder pattern data are also given.
Towards Improved Alignment of Powder Diffractometers
Authors: Schreiner Walter N.
Published: January 2013

An improved method of alignment of a Philips diffractometer equipped with a theta-compensating slit is described. The method employs a special fluorescent screen which is flat to better than 10 microns. The procedure results in accurate alignment of the theta-compensating slit at low angles and assures reliable intensity data down to one degree two theta or less.
μPDSM: Mainframe Search/Match on an IBM PC
Authors: Marquart R. G.
Published: January 2013

μPDSM, a powder diffraction search/match system, is derived from the original interactive time-sharing system written for the NIH/EPA Chemical Information System. Transformed and essentially rewritten, it still searches the entire JCPDS database, but on an inexpensive IBM PC microcomputer. In the transition from mainframe to micro, μPDSM has lost none of its speed or performance. Indeed, the basic discriminating power of the search/match algorithms had to be improved, since the Powder Diffraction File is some 50% larger than it was when The CIS version was in operation. While μPDSM will solve typical problems on a “push-button” mode, it provides an environment that promotes optimization of search parameters by the diffractionist, and provides all of the subfile and chemistry functions associated with larger systems.
Identification of the Polytype-like Modifications of Ca3GeO5 by Powder Diffraction
Authors: Takeuchi Yoshio , Nishi Fumito
Published: January 2013

Features of the powder diffraction patterns of known polytype-like modifications of Ca3GeO5, such as 2H, 9R and 24R types, and a monoclinic polymorph have been studied by means of the patterns calculated based on their crystal structures. The result has provided keys to identify them when they coexist in the same synthetic product. Accounts have been given on the crystallographic features of the building layer and rules for layer stackings of the modifications in general. Any modification may then be constructed to predict its powder diffraction pattern.
The Measurement of Stresses in Composites
Authors: Cohen J. B.
Published: January 2013

Although there is mounting interest in the measurement of stresses in composite materials after fabrication and/or use, few measurements to date have not taken into account the three dimensional nature of the stress system in such materials. Most data give only the net stress, that is, the difference between principal stresses. A procedure for a more complete measurement (in a reasonable time) is developed here, including the separation of macrostresses and microstresses. If time does not permit a full investigation, measurements of the lattice parameters of the component phases provide a simple way to sample the hydrostatic component due to differential thermal contraction. The Barrett-Predecki method of adding filler is particularly promising for stress measurements in those composites whose component phases do not give appropriate diffraction peaks. This procedure could also be used for monitoring stresses during the useful life of such materials.
An XRPD Investigation of a Face-Centered Cubic Metallic Plating
Authors: Ruud Clay Olaf , McDowell Robin J. , Snoha Daniel J.
Published: January 2013

Internal elastic strain (i.e., residual stress) and the diffracted X-ray intensity variation over several orientations of crystallites with respect to the specimen surface were investigated as a means of differentiating two qualities of polycrystalline nickel plating. A unique instrument based upon a position-sensitive scintillation X-ray detector was used to apply all of the techniques commonly applied to X-ray stress analysis in this investigation. It was concluded that residual stress measurements did not provide a clear distinction between the two specimens, but comparison of the relative intensities diffracted from crystallographic planes at certain orientations with the surface did provide a distinction.
Standard X-Ray Diffraction Powder Patterns from the JCPDS Research Associateship
Authors: McMurdie Howard F. , Morris Marlene C. , Evans Eloise H. , Paretzkin Boris , Wong-Ng Winnie , Ettlinger Lisa , Hubbard Camden R.
Published: January 2013

The following new or updated patterns are submitted by the JCPDS Research Associateship at the National Bureau of Standards. The patterns are a continuation of the series of standard X-ray diffraction powder patterns published previously in the NBS Circular 539, the NBS Monograph 25, and in this journal. The methods of producing these reference patterns are described in this journal, Vol. 1, No. 1, p. 40 (1986).

The data for each phase apply to the specific sample described. A sample was mixed with 1 or 2 internal standards: silicon (SRM640a), silver, tungsten, or fluorophlogopite (SRM675). Expected 2-theta values for these standards are specified in the methods described (ibid.). Data from which the reported 2-theta values were determined, were measured with a computer controlled diffractometer. Computer programs were used to locate peak positions and calibrate the patterns as well as to perform variable indexing and least squares cell refinement. A check on the overall internal consistency of the data was also provided by a computer program.
A Search/Match Procedure for Electron Diffraction Data Based on Pattern Matching in Binary Bit Maps
Authors: Carr Martin J. , Chambers William F. , Melgaard David
Published: January 2013

A unique file structure and search algorithm have been developed for the purpose of obtaining matches between experimental electron diffraction and qualitative energy dispersive X-ray compositional data from an unknown crystalline phase and the reference data in the JCPDS Powder Diffraction File. The reference data for over 32,000 inorganic compounds from sets 1–33 were compressed and stored in binary format as bit pattern maps. The entire data set and searching programs require less than 4 Mbyte and retain the precision appropriate for electron diffraction analysis. The search algorithm, written in both RT-11 FORTRAN and Flextran, is based on pattern matching between bit maps obtained for the unknown and reference compounds for both composition and diffraction data. Special attention is given to double diffraction effects commonly encountered in electron diffraction analysis. The programs run on an interactive basis on a microcomputer dedicated to the X-ray energy dispersive spectrometer on an analytical electron microscope. A typical search takes about 15 seconds to run and extracts about 10–15 different compounds.
A Tubular Aerosol Suspension Chamber for the Preparation of Powder Samples for X-Ray Diffraction Analysis
Authors: Davis Briant L.
Published: January 2013

Highly uniform fine powder sample layers may be prepared for X-ray diffractometry by aerosol suspension and collection on glass fiber filter substrates. A tubular aerosol suspension chamber (TASC) has been fabricated for this purpose. Essential components include a 500 ml gas buret, 4.7-cm filter cassette, rotameter, and rotary pump. Aerosol particles are generated within the TASC buret by convection within a fluidized bed of glass beads mixed with the sample. Exceptional uniformity of load and randomness of particle orientation has been demonstrated for samples prepared with this system. For quantitative analytical work accurate intensities may be obtained using corrections to raw intensities based on fundamental sample and filter properties.
X-ray Powder Data for Sodium tri-aqua-hexa-(nicotinato-tri-μ-oxo- tri-chromium (III) perchlorate) hexahydrate {Na [Cr3O(C6H5NO2)6 (H2O)3] [ClO4]8·C6H5NO2·6H2O}
Authors: Mullica D. F. , Sappenfield E. L. , Bradshaw J. E.
Published: January 2013

The indexed X-ray diffraction powder data of sodium triaqua-hexa-(nicotinato-tri-μ-oxo-tri-chromium(III) perchlorate) hexahydrate {Na [Cr3 O(C6H5NO2)6(H2 O)3] [ClO4]8·C6H5NO2·6H2O, NICCR} is reported. NICCR crystallizes in the hexagonal space group P63/m. The refined cell parameters were determined by employing a Siemens Debye-Scherrer camera (Fe Kā radiation, λmean= 1.93736 Å). The cell constants are a = 13.573(2), c = 24.901(5) Å, V = 3972.8 Å3 and Dx =1.68 Mg m-3 (Dm =1.67 Mg m-3). The quantitative figure of merit (FN) for NICCR is F27 = 32(0.010,81). The JCPDS Diffraction File No. is 36–1978.
Standard Reference Materials for X-Ray Diffraction Part I. Overview of Current and Future Standard Reference Materials
Authors: Dragoo A. L.
Published: January 2013

Standard Reference Materials (SRM) are stable materials which have one or more properties certified by the National Bureau of Standards. A general introduction is given to the types of SRM's and their certification. SRM's for X-ray diffraction are described in detail, including their intended use and their certified and other properties. New SRM's are under consideration as quantitative standards, intensity and line shape standards, and materials properties standards.
Synthesis and Cell Refinement of Ba5 LiTiNb9 O30 and Ba2 Na3 GdNb10 O30 Ferroelectrics
Authors: Zellmer Lauren , Smith Deane K. , Scheetz Barry E.
Published: January 2013

The synthesis and unit cell refinement of two industrially important ferroelectric compounds with the tungsten-bronze structure are reported.
The CaIn2-Type Structure in YAg0.4Ga1.6
Authors: Dwight A. E.
Published: January 2013

The ternary compound YAg0.4Ga1.6 has the CaIn2-type structure. The only variable positional parameter z was determined by graphical methods from visual observations of intensities on a Debye-Scherrer pattern. Cu or Ni substitutions for Ag also result in a ternary CaIn2-type structure.
Standard X-Ray Diffraction Powder Patterns from the JCPDS Research Associateship
Authors: McMurdie Howard F. , Morris Marlene C. , Evans Eloise H. , Paretzkin Boris , Wong-Ng Winnie , Zhang Yuming , Hubbard Camden R.
Published: January 2013

The following new or updated patterns are submitted by the JCPDS Research Associateship at the National Bureau of Standards. The patterns are a continuation of the series of standard X-ray diffraction powder patterns published previously in the NBS Circular 539, the NBS Monograph 25, and in this journal. The methods of producing these reference patterns are described in this journal, Vol. 1, No. 1, p. 40 (1986).

The data for each phase apply to the specific sample described. A sample was mixed with one or two internal standards: silicon (SRM640a), silver, tungsten, or fluorophlogopite (SRM675). Expected 2-theta values for these standards are specified in the methods described (ibid.). Data, from which the reported 2-theta values were determined, were measured with a computer controlled diffractometer. Computer programs were used to locate peak positions and calibrate the patterns as well as to perform variable indexing and least squares cell refinement. A check on the overall internal consistency of the data was also provided by a computer program.
Charles S. Barrett: X-Ray Metallurgist — An Informal Portrait
Authors: Rose R. N.
Published: January 2013

Charles Barrett's work in phase transformation at the atomic level helped redefine the underpinnings of the science and practice of metallurgy. His work in low temperature physical chemistry has extended its range. And, perhaps more than anyone else, as a teacher and author, he has helped introduce the technique of X-ray diffraction to the present generations of practicing metallurgists.

The relevance of his contributions is demonstrated by the continuing utility of his widely translated metallurgical text, Structure of Metals, which, when it first appeared, made the understanding of metallurgy at the atomic level accessible to a wide audience. Today this book has become a compendium of first principles.
Use of X-Ray Diffraction as an Analytical Technique for the Synthesis of Inorganic Catalysts
Authors: Straguzzi G. I. , Dismore Paden F.
Published: January 2013

X-ray powder diffraction was used as an analytical technique for the solid state synthesis of selective oxidation catalysts with large surface area. Qualitative analysis was used to determine the minimum temperature at which the synthesis was complete. Quantitative diffraction was used to analyze mixtures of isomorphous antimonates. Results indicated that the final mixtures are independent of the method of preparation, i.e., mixing or impregnation.
Statistical Inference, Size Distributions and Peak Broadening in Finite Crystals
Authors: Alvarez A. G. , Bonetto R. D. , Guérin D. M. A. , Plastino A. , Neira L. Rebollo
Published: January 2013

Calculations of crystal size distributions in oriented clays (montmorillonite and kaolinite) are carried out utilizing X-ray diffraction data together with a method based on information theory. Two different procedures for dealing with the available data are compared. One of them involves some points of the corresponding spectrum, the other correlates the data by means of their moments.
X-Ray Powder Diffraction Data for β-Lead Telluride
Authors: Peck Charles A. , Ruokolainen Robert B.
Published: January 2013

50-50 atomic percent lead telluride (Altaite), grown by the vapor transport method, was examined with a well aligned Rigaku horizontal beam diffractometer. PbTe is cubic (precise lattice parameter ao = 6.4591(5)Å) with an space group and a calculated density of 8.253 g/cm3. Fully indexed powder diffraction data are presented.
Powder Diffraction Data of Potassium Calcium Phosphate KCa PO4.H2O
Authors: Louër D. , Deneuve F. , Ouillon N.
Published: January 2013

Potassium calcium phosphate, KCa PO4.H2O, has been investigated by means of X-ray powder diffraction. Unit cell dimensions were determined from diffractometer data obtained with strictly monochromatized Cu Kα1 radiation, by indexing programs. A C-centered monoclinic cell was found: a =7.5834(9) Å, b = 8.1568(11) Å, c = 7.6541(8) Å, β= 102.975 (9)°.
Computer Program for Analysing Interstratified Structures by Fourier Transform Methods
Authors: Vila E. , Ruiz-Amil A.
Published: January 2013

A computer program for analysing two-component interstratified structures by two different Fourier transform methods is described. The first method consists of the calculation of the X-ray diffraction intensity function, and in the second one (direct method) the distribution function of interlayer distances is calculated. The programs have been written in compiled GWBASIC for an Olivetti M-24 microcomputer (MS-DOS operating system), and they may also be run on any IBM compatible personal computer. As an example, this program is applied for the analysis of a chlorite-smectite interstratified mineral.
Lattice Thermal Expansion of Lead Zirconate Titanate Piezoelectrics
Authors: Amin A. , Newnham R.E.
Published: January 2013

Lattice thermal expansion of a number of compositions in the tetragonal (P4mm) single cell region of the lead zirconate titanate Pb(ZrxTi1−x)O3 system have been measured by high temperature X-ray diffraction. Polynomial coefficients which describe the temperature dependence of the lattice constants of each composition below and above the ferroelectric-paraelectric transition temperature are given.
Crystal Data for CuInTe2
Authors: Haworth L. I. , Tomlinson R. D.
Published: January 2013

The Debye-Scherrer technique and filtered Cu Kα, radiation were used to obtain powder data for reflections to an angle of 2θ = 155°; a vertical scanning diffractometer was used to obtain intensity data to an angle of 2θ = 99°. The space group is with Z = 4. The lattice parameters of the tetragonal unit cell were measured to be a = 6.189 (1) Å and c = 12.391 (1) Å with c/a = 2.002 The unit cell volume was calculated as U = 474.6 (2) Å3 and the X-ray density as Dx = 6.07 ± 0.003 gm cm−3. By comparing measured and theoretical intensity values, the sublattice distortion parameter x was estimated to be x = 0.227 (12).
RIR - Measurement and Use in Quantitative XRD
Authors: Hubbard Camden R. , Snyder Robert L.
Published: January 2013

The Reference Intensity Ratio (RIR) is a general, instrument-independent constant for use in quantitative phase analysis by the X-ray powder diffraction internal standard method. When the reference standard is corundum, RIR is known as I/Ic; These constants are collected in the Powder Diffraction File (1987), can be calculated, and can be measured. Recommended methods for accurate measurement of RIR constants are presented, and methods of using these constants for quantitative analysis are discussed. The numerous, complex constants in Copeland and Bragg's method introduced to account for superimposed lines can be simply expressed in terms of RIR constants and relative intensities. This formalism also permits introduction of constraints and supplemental equations based on elemental analysis.
X-Ray Powder Diffraction Analysis of a Nonlinear Optical Material 4-(N,N-dimethylamino)-3-acetamidonitrobenzene
Authors: Huang T. C. , Karimi R. , Baumert J.-C. , Bjorklund G. C.
Published: January 2013

A nonlinear optical material 4-(N,N-dimethylamino)-3-acetamidonitrobenzene, (CH3)2NC6H3NO2NHCOCH3, has been characterized by X-ray powder diffractometer method. The experimental 2θ values corrected for systematic errors, the relative intensities, values of dexp and the Miller indices of the 46 peaks observed in the 5° to 51° 2θ range are reported. The powder diffraction data have been evaluated, and the figure of merit is F30 = 36.6 (0.016, 51). The unit cell parameter least-squares refined from 38 non-overlapping peaks of the monoclinic compound with a P21 space group are: a = 4.792(1)Å, b = 13.055(2)Å, c = 8.735(1)Å, β = 94.43(2)°, V = 544.8(1)Å3, Z = 2, and Dx = 1.36 gm/cm3. The powder diffraction results are in a good agreement with those obtained from single-crystal structure data.
A Practical Method for the Determination of the Instrumental Full Width at Half Maximum
Authors: Guérin D.M.A. , Bonetto R.D. , Alvarez A.G.
Published: January 2013

X-ray diffraction and neutron spectra present a peak assembly whose maxima are centered at angles corresponding to Bragg's law.

Analysis of diffracted intensity profiles in each peak can be used to estimate such morphologic characteristics of the samples as preferred orientation (Brindley and Kurtosy, 1961; Martin, 1966); crystallite sizes (Scherrer, 1919; Warren and Averbach, 1950; Wilson, 1962; and Guérin et al., 1986); and crystal shapes (Wilson, 1949). Such analysis can also be used to estimate the determination of residual stress and lattice defects (Warren and Averbach, 1950; Wilson, 1963). In such studies, a detailed analysis of the diffraction distribution is required and consequently adjustment of intensity values must be carried out, as they are affected by systematic errors in the measuring apparatus (for detailed description, see Klug and Alexander, 1974 and Wilson 1967).
Quantitative Determination by X-Ray Diffractometry of Calcium Sulfate and Calcium Carbonate in Airborne Dusts
Authors: Nakamura Toshihiro
Published: January 2013

A quantitative simultaneous determination method by X-ray powder diffractometry is described for calcium sulfate and calcium carbonate in airborne dusts. In order to eliminate the mutual interference among diffraction peaks, and to avoid the presence of the hydration isomers of calcium sulfate, dust samples were heated at 350°C for 2 h. To reduce the errors due to the difference-in crystallinity between the standard materials and the samples, the synthesized calcium sulfate anhydrate (anhydrite) was heated to such an extent that the half-width of the 002,020 peak was identical with that of the anhydrite in pretreated dust samples. Standard calcium carbonate (calcite) was ground until the half-width and the orientation index of the 104 peak of calcite was identical with that of the calcite in dust samples. Linear calibration curves were obtained throughout the range of 0 ∼ 30 wt% for anhydrite and the range of 0 ∼ 10 wt% for calcite, respectively. The determination limits were 0.2 wt% for anhydrite and 0.3 wt% for calcite. Relative standard deviations were 3.4 % for 8.0 wt% of anhydrite and 1.8% for 5.4 wt% of calcite. The present method is applicable to determination of calcium sulfate and calcium carbonate in actual dust samples.
Standard X-Ray Diffraction Powder Patterns of Fourteen Ceramic Phases
Authors: Wong-Ng Winnie , McMurdie Howard F. , Paretzkin Boris , Hubbard Camden R. , Dragoo Alan L.
Published: January 2013

The following fourteen reference patterns of carbide, nitride, telluride, and oxide ceramics are reported. Included in the fourteen reference patterns are data for three high Tc superconducting oxide related phases (Ba2CuO3, CuSrO2, and Ba2Cu3YO6). The general methods of producing these X-ray powder diffraction reference patterns are described in this journal, Vol. 1, No. 1, pg. 40 (1986).

Samples were mixed with one or two internal standards: silicon (SRM640a), silver, tungsten, or fluorophlogopite (SRM675). Expected 2θ values for these internal standards are specified in the methods described (ibid.). Data were measured with a computer controlled diffractometer. The POWDER-PATTERN system of computer programs was used to locate peak positions, to calibrate the patterns, and to perform variable indexing and least-squares cell refinement. A check on the overall internal consistency of the data was also provided by a computer program.
X-Ray Powder Data for CaWO4, Synthetic Scheelite
Authors: Blanchard Frank N.
Published: January 2013

New X-ray powder data for CaWO4 (synthetic scheelite) are presented and compared with the current PDF patterns and with a calculated pattern.
New X-Ray Powder Data for Gorceixite, BaAl3(PO4)2(OH)5·H2O, an Evaluation of d-Spacings and Intensities, Pseudosymmetry and Its Influence on the Figure of Merit
Authors: Blanchard Frank N.
Published: January 2013

New powder and crystallographic data for gorceixite, a mineral of the crandallite subgroup of the alunite group, are reported and compared with current Powder Data File (PDF) patterns and with calculated patterns. Both d-spacings and intensities have been evaluated, and the results indicate a significant improvement over existing patterns. Indexing of the reflections is given for the true monoclinic symmetry, Cm (8), the pseudorhombohedral symmetry, (166) (to compare with structurally analogous minerals), and the pseudocubic symmetry, Fm3m (225). Because of the strong pseudosymmetry, the overall figure of merit is lower than would be the case for indexing in one of the pseudospace groups.
Crystal data of the low-temperature solid form of 2-methyl-2-nitro-propanol(MNP)
Authors: Tamarit J. Ll. , Chanh N. B. , Négrier P. , López D. O. , Barrio M. , Haget Y.
Published: January 2013

By means of X-ray single crystal Weissenberg photographs, the crystal of the low-temperature solid form of 2-methyl-2-nitro-propanol, (CH3)2C(NO2)(CH2OH), has been determined and found to be of the monoclinic type, space group P21/c. The cell constants were refined from X-ray powder diffraction data: a=6.195(3) Å, b=19.116(7) Å, c=16.598(7) Å, and β = 90.12(2)° with Z = 12. The indexed pattern at 293 K is given.
Synthesis and crystal data for K3Nb3O6Si2O7
Authors: Launay S. , Mahé P. , Quarton M.
Published: January 2013

The silicate compound, K3Nb3O6Si2O7, has been synthesized by solid-state reaction. Single crystals were obtained; they crystallized with the hexagonal space group P2c. Refined unit-cell parameters are: a = 9.0377(3), c=8.0465(7)Å, V=569.18(5)Å3, Z=2, Dm = 3.84(4), Dx=3.851. Powder diffraction data are reported.
Powder Data for LaCo0.4Fe0.6O3
Authors: McCready D. E. , Kingsley J. J.
Published: January 2013

Standardized X-ray powder diffraction data for orthorhombic LaCo0.4Fe0.6O3 prepared by calcination of a glycine-nitrate combustion-synthesized precursor are reported. Orthorhombic unit cell parameters: a = 5.4688 (2), b = 5.5100 (2), c = 7.7462 (3) Å. The reference intensity ratio, I/Icor,= 6.12.
An X-ray powder diffraction study of amine zinc hydroxide nitrate
Authors: Bénard Patricia , Auffrédic Jean Paul , Louër Daniel
Published: January 2013

A new amine zinc hydroxide nitrate has been synthesized and investigated by means of X-ray powder diffraction. The monoclinic unit cell dimensions are a = 20.781(3) Å, b = 6.2151(9) Å, c = 5.4952(6) Å, β = 92.24(1)° (space group C2/m with Z = 2). The crystal structure has been refined by the Rietveld method using the structure of the related dihydrated phase as a starting model (Rp = 0.092 and RF = 0.068 for 372 reflections). The structure is characterized by octahedra [Zn(OH)6] describing a brucite-type layer, with one-quarter of the metal atoms missing, and by tetrahedra [Zn(OH)3(NH3)] located above and below the empty octahedra. The complex positive sheet has the formula [Zn3octa(OH)8Zn2tetra(NH3)2]2+ and the cohesion of the structure is realized through hydrogen bonding.
Characterization of new solid solution phases in (Y,Ca)(Cr,Co)O3 system
Authors: Basceri Cem , Tas A. Cuneyt , Timucin Muharrem
Published: January 2013

New solid solution phases in the (Y,Ca)(Cr,Co)O3 system have been synthesized and characterized by powder X-ray diffraction. The selected compositions in this system were prepared by the modified Pechini method. Powder-diffraction patterns were prepared.
Rietveld refinement of the crystal structures of hexagonal Y6Cr4+xAl43−x (x=2.57) and tetragonal YCr4−xAl8+x (x=1.22)
Authors: Černý R. , Yvon K. , Yanson T. I. , Manyako M. B. , Bodak O. I.
Published: January 2013

Y6Cr4+xAl43−x (x = 2.57); space group P63/mcm, a = 10.8601(1) Å, c = 17.6783(3) Å, V= 1805.7(1) Å3, Z=2; isostructural to Yb6Cr4+xAl43−x, (x=1.76) with two aluminium sites partially occupied by chromium (44% and 27% Cr). YCr4−xAl8+x (x=1.22); space group I4/mmm, a = 9.0299(2) Å, c = 5.1208(2) Å, V=417.55(3) Å3, Z=2, disordered variant of CeMn4Al8 with one chromium site (8f) partially occupied by aluminium (33% Al); X-ray powder diffraction data were collected on a well-crystallized multiphase sample containing 43 wt.% of Y6Cr4+xAl43−x, 27 wt.% of Y2Cr8−xAl16+x, 16 wt.% of Al, 13 wt.% of YAl3, and traces of Y2O3. Structure refinement converged at Rwp = 2.0% and RB = 3.5, 3.6% resp. for a total of 78 parameters and 1190 reflections.
DISVAR93: A software package for determining systematic effects in X-ray powder diffractometry
Authors: Berti G. , Giubbili S. , Tognoni E.
Published: January 2013

DISVAR93 is a collection of programs devised to process XRPD patterns with the aim of determining the parameters of systematic instrumentation and sample effects. These effects have an influence on data uncertainty and also accuracy of the adopted models describing diffraction phenomena. Such modeling is carried out through the mathematical X-ray powder-diffraction theory, while parameter optimization is achieved by using the additive property of X2 and constraining the models to converge simultaneously to the same minimum in a restrained Hilbert's space. The package has been designed to allow both user interaction as well as automatic linking of programs managed by one main menu and offer several options to satisfy individual user requirements.
Preparation and structural characterization of the rare-earth oxides BaR2O4, R=Pr, Tb
Authors: Cascales C. , Rasines I.
Published: January 2013

The compounds BaR2O4, (R = Pr, Tb), where R are two of the less frequent trivalent lanthanides, have been prepared under reducing atmosphere from mixtures of BaO2, the R metals, and the oxides Pr2O3 and Tb4O7, respectively. The crystal structure of BaR2O4 have been refined from X-ray powder diffraction data by the Rietveld method of profile analysis using 31 parameters in each case. Both oxides are orthorhombic, isotypic with SrY2O4, of the perovskite-related CaFe2O4 structure type, S.G. Pnma (No. 62), Z = 4, a = 10.6113(8), b = 3.6303(3), c = 12.485(1) Å, and V = 480.93(5) Å3 for R = Pr; and a = 10.4282(8), b = 3.4893(3), c = 12.1809(6) Å, and V = 443.22(3) Å3 for R = Tb. The R–O distances vary between 2.15(6) to 3.40(6) Å for R = Pr, and between 2.15(3) to 2.91(5) Å for R = Tb.
Powder X-ray crystallography of gallium 3-hydroxy-4-pyronates
Authors: Bernstein Lawrence R.
Published: January 2013

Two complexes of gallium with 3-hydroxy-4-pyrones were synthesized as potential pharmaceutical compounds for oral administration. These compounds were analyzed by powder X-ray diffraction followed by computer indexing of the data. The first compound, tris(3-hydroxy-2-methyl-4-pyronato)gallium [Ga(C6H5O3)3], was found to be orthorhombic, a = 18.500(2), b = 16.948(2), c = 12.012(2) Å, V = 3766(1) Å3, Z = 8, Dm = 1.56(5), Dx = 1.570. The compound appears closely analogous to a similar compound containing Al instead of Ga, which crystallizes in space group Pbca. The second compound, tris(3-hydroxy-2-ethyl-4-pyronato)gallium [Ga(C7H7O3)3], was found to be monoclinic, a = 31.634(2), b = 8.7662(5), c = 7.8982(5) Å, β = 103.240(6)°, V = 2132.0(5) Å3, Z = 4, Dm = 1.50(5), Dx = 1.517, with a primitive space group.
X-ray powder diffraction data for RuCI2(TRIPHOS)(DMSO) dichloro [bis(2-diphenylphosphinoethyl) phenylphosphine] [dimethylsulfoxide] ruthenium (II)
Authors: Delgado Gerzon , Rivera A. Valentina , Suárez Trino , Fontal Bernardo
Published: January 2013

X-ray powder diffraction data for Dichloro [bis(2-diphenylphosphinoethyl) phenylphosphine] [dimethylsulfoxide] Ruthenium (II) is reported. The powder pattern was obtained using CuKα radiation. The lattice parameters determinated by least-squares refinement for the monoclinic space group P21/c are: a = 21.073(3) Å, b = 11.970(2) Å, c = 16.889(3) Å, and β = 107.72(1)°, with M20 = 10.67 and F30 = 15.4 (0.0145, 134), and are in good agreement with those obtained from the single crystal structure determination. Observed and calculated X-ray powder diffraction data are given for the titled compound.
A synchrotron X-ray powder diffraction study of CoAl2O4and CoGa2O4by PSD diffractometer technique
Authors: Christensen A. Nørlund , Norby P. , Hanson J. C.
Published: January 2013

X-ray powder diffraction data for the spinels CoAl2O4and CoGa2O4were measured with synchrotron radiation usingλ= 1.2033 Å, determined with Si as a standard (a= 5.4305 Å). The two blue compounds prepared hydrothermally are cubic with space groupFd3m. Profile refinements gave the results: CoAl2O4hada= 8.0968(1) Å and composition (Co0.71Al0.29]Al1.71Co0.29]O4and CoGa2O4hada= 8.3229(1) Å and composition Ga[CoGa]O4. The degree of inversion is thus 0.29 for CoAl2O4and one for CoGa2O4.
Synthesis and X-ray powder diffraction study of the elpasolite Cs2NaCeCl6
Authors: Acevedo R. , Poblete V.
Published: January 2013

The synthesis at 850 °C and the structural characterization of the elpasolite structure compound Cs2NaCeCl6 is reported space group Fm3m, a = 10.943(2) Å, V = 1310.4 (Å)3, Z = 4, M = 641.64, Dx = 3.252, and Dexp = 3.21. Powder diffraction data from a Rietveld structure refinement, are reported.
Powder X-ray characterisation of natrolite, Na2Al2Si3O10.2H2O
Authors: Finch A. A. , Fletcher J. G. , Kindness A. , Skakle J. M. S.
Published: January 2013

High-quality powder X-ray diffraction data for a well-characterised natural sample of natrolite (Na2Al2Si3O10.2H2O, space group Fdd2, Z = 8) are presented. Refined cell parameters were a = 18.2984±0.0007 Å, b = 18.6502±0.0008 Å, and c = 6.5589±0.0003 Å. The sample was characterised using thermogravimetric techniques (to determine water content), EPMA and ICP-MS (to determine composition). Available data suggest that the crystal matches the expected stoichiometry of natrolite. Our powder data show close similarity with the proposed structure of natrolite using the Rietveld method, giving R values of 8.54%, and suggest that preferred orientation is not present in the sample.
Powder diffraction of La0.3Sr0.7CoO3−δ
Authors: van Doorn René H. E. , Boeijsma Jaap , Burggraaf Anthonie J.
Published: January 2013

Powder X-ray diffraction data for cubic La0.3Sr0.7CoO3−δ, perovskite prepared by a combustion method, using metal-EDTA complexes are reported. The cubic cell parameter is: ac = 3.8323(9)Å.
Powder X-ray data for the ammonium dioxalatotitanyl (IV) monohydrate (NH4)2TiO(C2O4)2·H2O
Authors: Ezahri Mohamed , Coffy Georges , Mentzen Bernard F.
Published: January 2013

X-ray powder diffraction data are reported for the monohydrated ammonium dioxalatotitanyl (IV). The crystal system is monoclinic with space group P21/c. Refined unitcell parameters are a = 13.484(3), b = 11.325(2), c = 17.673(3) Å, and β = 126.613(8)°.
Crystal and powder XRD data of Mg3(PO4)2-III: High-temperature and high-pressure form
Authors: Brunet F. , Chopin C. , Elfakir A. , Quarton M.
Published: January 2013

A new diffraction pattern of the high-temperature and high-pressure polymorph Mg3(PO4)2-III (PDF 43-500) is given and indexed on the basis of a single-crystal structure refinement. It allows diffractogram indexing of the isostructural high-temperature and high-pressure form of Co3(PO4)2 (PDF 43-499).
The POWDER SUITE: Computer Programs for Searching and Accessing the JCPDS-ICDD Powder Diffraction Database
Authors: Toby B.H. , Harlow R. L. , Holomany M. A.
Published: January 2013

Two new VAX/VMS computer programs are presented for accessing and searching the Powder Diffraction File (PDF) (1989) of the JCPDS-International Centre for Diffraction Data (ICDD). The programs use binary mapped index files which affords rapid searches of the database. Program LOGIC permits entries in the database to be selected by chemistry, peak position or name constraints. The selected entries may be displayed, printed or graphed. The program can display or print entries from the full PDF-2 (1989) database, if on-line. Program SEARCH searches for patterns in the database which match an unknown set of peaks; the program may be optimized for a wide variety of applications including identification of component phases in mixtures. Commands may be entered to the programs in two modes. In the “novice-friendly” mode, users must answer questions to select options. However, experienced users may opt to use a concise one-line command syntax. The modes may be mixed.
Identification and Quantification of Unknown Component Phases in Powder Samples by X-Ray Diffractometry
Authors: Kato Masanao , Fujii Sinzo , Ui Takuji , Asada Eiichi
Published: January 2013

A method of analysis for X-ray diffractometry is proposed for determining the number and the concentrations of phases in a series of samples of the same multiphase system. This method can be used when n samples containing N phases, where N<n, with different concentrations are given or prepared from a given sample.

The method of principal component analysis was applied to the determination of the number of individual phases in multiphase mixtures. A quantification method using the intensity ratio to an arbitrary chosen standard mixture, which is also one of the mixtures to be analyzed, is proposed.

In this study, we examined the validity of this method for X-ray diffractograms of two and three component systems. It is shown that the values determined by the present method are in good agreement with the prepared concentrations of the samples.
Mass Absorption Corrected X-Ray Powder Diffractograms. Part 1: Measuring Pyrite in Powdered Coals
Authors: Wertz David L.
Published: January 2013

An X-ray analysis method has been developed for the quantitative analysis of pyrite (FeS2) in coals and lignites. Requiring neither the use of external or internal references, the method linearly relates diffraction peak area in the absorption corrected X-ray diffractogram obtained from the finely powdered coal to the pyrite abundance. The [311] diffraction peak of pyrite (FeS2) has been used to develop the analysis protocol. The Argonne premium coals have been used as the experimental subjects. The abundance of pyrite in each coal has been measured from the absorption corrected diffractograms, which has been constructed from the experimentally measured diffraction intensities and the mass absorption coefficient of each coal sample. The accuracy (accessed from the figure-of-merit and the net count uncertainty associated with the 1.63 Å pyrite peak) as well as the lower limit of detection for pyrite in these coals is presented. The role of the mass absorption coefficient in the conversion of the measured intensity to the absorption corrected intensity is discussed.
Indexing of the Powder Diffraction Pattern of Yttrium Oxalate Dihydrate
Authors: Louër D. , Deneuve F. , Ecochard F.
Published: January 2013

Yttrium oxalate dihydrate, Y2(C2O4)3.2H2O, has been investigated by means of X-ray powder diffraction. Unit cell dimensions were determined by an indexing program based on the variation of parameters by successive dichotomies. The diffractometer data were collected with strictly monochromatic radiation. A monoclinic cell was found: a=9.3811(8)Å, b=11.6385(15)Å, c=5.9726(7)Å, β=96.079(8)°, which is characterized by the figures of merit M20=87 and F30=112 (0.0065,41). A preliminary analysis of the anisotropic line broadening has revealed some microstructural properties. It is shown that line broadening is mainly due to a micro-strain effect.
Determination of the Relative Amounts of α-carbamazepine and β-carbamazepine in a Mixture by Powder X-Ray Diffractometry
Authors: Suryanarayanan Raj
Published: January 2013

A powder X-ray diffraction technique has been developed to quantify the relative amounts of α-carbamazepine (A) and β-carbamazepine (B) when they occur as a mixture. The theoretical basis of this technique was developed in 1948 by Alexander and Klug (Anal. Chem., 20:886-889). The powder X-ray diffraction patterns of A and B revealed that the line with d-spacing of 10.1 Å was unique to A. The ratio of the integrated intensity of the 10.1 Å line in a mixture of A and B, to the intensity of the 10.1 Å line in a sample consisting of only A, was calculated as a function of weight fraction of A in the mixture. These ratios were also experimentally determined, and there was a good agreement between the theoretical and experimental intensity ratios. The particle size of the samples, the sample preparation technique and the experimental conditions were controlled so as to eliminate the major sources of error in powder X-ray diffractometry. In order to minimize preferred orientation of the particles, a sample holder was specially fabricated.
On The Harris Texture Index
Authors: Valvoda V. , Järvinen M.
Published: January 2013

The texture index introduced by Harris (1952) is reconsidered from the point of view of the orientation distribution of crystallites in a flat powder specimen. It is shown that the texture index can be used as an approximate measure of texture degree or as a texture correction factor in cases of a weak texture. Its failure in both these aspects for the strong textures is caused by an incorrect averaging of pole densities contained in the original definition of this quantity.
X-Ray Powder Structural Analysis of the Spinel Polymorph of Fe2SiO4
Authors: Ding Jianping , Li De-yu , Fu Ping-qiu
Published: January 2013

The crystal structure of the spinel polymorph of Fe2SiO4, synthesized at high temperature (900°C) and high pressure (70 kbar), was studied by the Rietveld analysis of X-ray powder diffraction data collected with a Guinier-Hägg camera. The compound is cubic, space group , with cell dimension: a= 8.2413(6) Å, V= 559.8(1) Å3, Z= 8, Cell Wt. = 1630.2, Dx= 4.835 g·cm−3, Do= 4.75 g·cm−3. The figure of merit is F10= 92(0.011, 10). The final R value is RF= 0.058. The crystal has a mixed normal-inverse spinel structure. The site occupancy refinement showed that 37.9% of the silicon was found in the octahedral site (M site), while 18.9% of the iron occupied the tetrahedral site (T site). Due to the larger displacement of Si4+ion by Fe2+ion, the positional parameter of oxygen atom (0.3689) is smaller than that of X-ray single crystal structure (0.3658), and the average Si-O bond (1.697(1)Å) is longer and Fe-O bond (2.112(1)Å) is shorter than those of X-ray single crystal structure.
X-Ray Powder Data for α-Si3N4
Authors: Norris D. A. , Rodriguez M. A. , Fukuda S. K. , Snyder R. L.
Published: January 2013

A new X-ray powder diffraction pattern for α-Si3N4is presented and compared with the current PDF pattern. The necessity for an updated pattern is discussed.
X-Ray Diffraction Analysis of Titanium Carbonitride 30/70 and 70/30 Solid Solutions
Authors: Guilemany J.M. , Sanchiz I. , Alcobé X.
Published: January 2013

X-ray powder data and refined cell parameters for two titanium carbonitride solid solutions are presented. Some deviations from Vegard's law were observed.
Powder Diffraction Data for Synthetic Potassium-Richterite, Nickel-Potassium-Richterite and Cobalt-Potassium-Richterite
Authors: Raudsepp Mati , Ventura Giancarlo Della , Hawthorne Frank C. , Robert Jean-Louis
Published: January 2013

Indexed X-ray powder diffraction data derived from Rietveld crystal structure refinements are reported for synthetic potassium-richterite (KRC: K[CaNa]Mg5Si8O22(OH)2), nickel-potassium-richterite (NIKRC:K[CaNa] Ni5Si8O22(OH2) and cobalt-potassium-richterite (COKRC:K[CaNa]Co5Si8O22 (OH2). The following dimensions were obtained: KRC: a = 10.0547(8), b = 17.997(1), c = 5.2746(4)Å, β = 104.832(5)°; NIKRC: a = 10.0297(7), b = 17.942(1), c = 5.2576(4)Å, β = 104.982(5)°; COKRC: a = 10.1166(9), b = 18.066(1), c = 5.2752 (4)Å, β= 104.846(6)°.
Determination of Amorphous Phase in Quartz Powder by X-Ray Powder Diffractometry
Authors: Nakamura Toshihiro , Sameshima Katsumi , Okunaga Kiyoyuki , Sugiura Yoshitaka , Sato Jun
Published: January 2013

A powder diffraction method was applied to the quantitative analysis of amorphous silica in several quartz powders. Two calibration methods, i.e., direct analysis and the standard addition method were examined. Calibration mixtures were made by mixing a standard silica gel powder ground to under 5 μm particle size with a matrix quartz powder which was ground to 10 to 40 μm particle size and treated with NaOH solution to remove the amorphous phase caused by grinding. Intensity of the amorphous halo was measured at 23.0° 2θ, and the background intensity at 53.0° 2θ was subtracted. Linear calibration curves were obtained over the ranges of 0 to 50 wt% by direct analysis and 0 to 20 wt% by standard addition methods, respectively. The analytical results obtained by the two calibration methods were in good agreement with each other. The relative standard deviations for 4.3 wt% of amorphous silica were 4.6% by the direct analysis and 5.4% by the standard addition method. These methods were successfully applied to a correction of reference intensity ratios (RIR) for several quartz powders containing amorphous silica. After the correction for amorphous content, the relative standard deviations of the RIR values for quartz powders became smaller.
Standard X-Ray Diffraction Powder Patterns of Fourteen Ceramic Phases
Authors: Wong-Ng Winnie , McMurdie Howard F. , Paretzkin Boris , Kuchinski M.A. , Dragoo Alan L.
Published: January 2013

Fourteen reference patterns of oxide ceramics are reported. Included in the fourteen reference patterns are data for nine high critical temperature super-conducting oxide related phases: (BaCuEr2O5, Ba2Cu3EuO7, BaCuGd2O5, Ba2Cu3GdO7, Ba2.4Cu5La4O13, Ba1.9cu3La1.1O7, Ba2Cu3SmO7 and (Ba0.4Sr0.6)2Cu3 YO7). The general methods of producing these X-ray powder diffraction reference patterns were described previously in this journal (Vol. 1, No. 1, pg. 40 (1986)). The symbols used in this article are defined in the PDF cards.
X-Ray Diffraction Data for SnO2. An Illustration of the New Powder Data Evaluation Methods
Authors: McCarthy Gregory J. , Welton Jean M.
Published: January 2013

The Powder Diffraction File (PDF) X-ray diffraction pattern for SnO2 (cassiterite, syn), determined in the early 1950's at the National Bureau of Standards, was evaluated using the NBS*AIDS83 editorial review program and a calculated powder pattern. Systematic errors in d-spacings and relative intensities were attributed to the lack of an iterative least-squares refinement of unit cell parameters, to inadequate precision in reporting d-spacings, to poor sensitivity to high angle reflections, and to detector dead time. A new SnO2 pattern was prepared and used to illustrate criteria for evaluation of powder patterns. An R-Factor for quantifying agreement between observed and calculated relative intensities was utilized. The systematic errors in the earlier pattern occurred at higher angles and did not hinder its usefulness for identification purposes.
Crystal Data for [Cu(C15H11N3)X2]·nH2O [X−=NCO (n=1); NCSe and N3(n=ø)] Compounds
Authors: Vía J. , García A. , Mesa J. L. , Arriortua M. I. , Rojo T.
Published: January 2013

Three members of the family [CuC15H11N3)X2]·nH2O [X−=NCO (n=1), NCSe and N3 (n=ø)], C15H11N3=2,2′:6′,2″ – terpyridine (terpy), have been prepared by reaction in solution. Crystal data determined widi the aid of single crystal methods, powder diffraction data, and densities determined by flotation methods are presented.
Computer Programs for Standardless Quantitative Analysis of Minerals Using the Full Powder Diffraction Profile
Authors: Taylor J. C.
Published: January 2013

A Fortran 77 computer program has been developed for the quantitative analysis of minerals by multiphase profile analysis of the complete powder diffraction pattern. Featured are full-matrix least-squares refinement of 14 Rietveld “instrumental parameters” (phase scales, asymmetry, preferred orientations (March model), linewidths, instrument zero, lineshapes and unit cell dimensions), Brindley particle absorption contrast factors and amorphicity corrections. The program uses a crystal structure Databank, which contains information on absorption coefficients, unit cell data and crystal structures for some 90 common minerals. New minerals can be easily added. Structure parameters are also refinable by a profile decomposition method using a program called STRUCT. The sum of the calculated patterns, derived from the crystal structure data, is fitted to the observed pattern by a program called TRACSCAL which runs in singlepass multiphase mode and, after the above corrections have been applied, the weight percentages of the component phases are calculated from the Rietveld scaling factors.

The program runs on an IBM-compatible AT computer with 640K of RAM, on an extended memory AT, or a mainframe system. Examples of its use are given with standard mixtures and naturally occurring specimens. On an AT computer with 20MHz clock speed a scaling run, including data input, reading of the pattern, processing of (hkl) files, calculation of the profile and one cycle of least squares fitting takes about 30 seconds for binary standard mixtures and about 2.5 minutes for a 7-phase natural bauxite pattern containing 320 independent (hkl) reflections.