The 1-[N-(methyl)-(3,5-dimethylphenylamino)]methylnaphthalene (chemical formula C20H21N) was prepared by means of a condensation between alpha-naphthylaldehyde and 3,5-dimethylaniline in anhydrous ethanol to obtain the aldimine (1) which was reduced with NaBH4 to afford the 1-[N-(3,5-dimethylphenylamino)]methylnaphtalene (2), and finally, the compound (3) was obtained by N-alkylation reaction of (2) with methyl iodine (CH3I) and potassium carbonate (K2CO3) in acetone. Final compound (3) was purified by chromatographic column. The XRPD pattern for the new compound, 1-[N-(methyl)-(3,5-dimethylphenylamino)]methylnaphthalene, was obtained. This compound crystallizes in monoclinic system with space group P21/a (No. 14) and refined unit-cell parameters a=13.260(4) Å, b=15.495(5) Å, c=7.719(5) Å, β=90.19(6), and V=1586(1) Å3.

Using a recent proposed analysis procedure for quantitative phase determination by X-ray powder diffraction, YBa2Cu3O7−x solid state formation reaction kinetics at 900 °C was studied. Although there was the presence of partial amorphous components, it was possible to determine a reaction route for the synthesis of the title compound from X-ray powder diffraction data collected at various stages of the thermal treatment and using the Rietveld method for the quantitative determination of the phase composition

The characteristics of the (101) peak of α-quartz and the (104) peak of the NIST SRM 1976 alumina flat plate standard have been measured in dependence of time for 60 h with Cu-Kα1 radiation in Bragg-Brentano geometry with a Philips X’Pert diffractometer equipped with a primary Ge(111) monochromator. It was found that the reproducibility of the peak position and the peak shape falls well in the ±3σ range, whereas the peak intensity strongly depends on the power history of the X-ray generator and the temperature of the diffraction system. The effects on Rietveld refinements are discussed and recommendations are given for optimized data collection.

The crystal structures of four samples of anhydrite, CaSO4, were obtained by Rietveld refinements using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and space group Amma. As an example, for one sample of anhydrite from Hants County, Nova Scotia, the unit-cell parameters are a = 7.00032(2), b = 6.99234(1), c = 6.24097(1) Å, and V = 305.487(1) Å3 with a > b. The eight-coordinated Ca atom has an average <Ca-O> distance of 2.4667(4) Å. The tetrahedral SO4 group has two independent S-O distances of 1.484(1) to O1 and 1.478(1) Å to O2 and an average <S-O> distance of 1.4810(5) Å. The three independent O-S-O angles [108.99(8) × 1, 110.38(3) × 4, 106.34(9)° × 1; average <O-S-O> [6] = 109.47(2)°] and S-O distances indicate that the geometry of the SO4 group is quite distorted in anhydrite. The four anhydrite samples have structural trends where the a, b, and c unit-cell parameters increase linearly with increasing unit-cell volume, V, and their average <Ca-O> and <S-O> distances are nearly constant. The grand mean <Ca-O> = 2.4660(2) Å, and grand mean <S-O> = 1.4848(3) Å, the latter is longer than 1.480(1) Å in celestite, SrSO4, as expected.

Ternary Al-Cu-W alloys were investigated. The previously reported Al3Ti-type phase (space group I4/mmm) with the average composition Al67Cu11.5W21.5 was found to have a=3.7296(4) Å and c=8.3797(10) Å. The ternary phase forming around Al67Cu21W12 has a hexagonal structure with a=8.6594(13) Å and c=15.2677(21) Å.

GSAS instrument parameters are tabulated for a variety of laboratory and synchrotron diffractometers to give users an idea of the typical ranges of profile parameters when they generate their own instrument parameter files. For modern high-resolution laboratory diffractometers, the parameters fall in the ranges 0<U<3, V=0, 0<W<4, 1<X<3, 0<Y<3, 1<asym<3, and 0<S/L<0.03. For synchrotron diffractometers, the parameters fall in the ranges 0<U<1.2, −1<V<0, 0<W<1, 0<X<1, 0<Y<1, 0<asym<0.5, 0<S/L<0.001, and 0<H/L<0.007. FULLPROF equivalents are also reported. The factors which are convoluted together to generate the instrument profile are described.

The aim of this work was to design, construct, install, and commission an on-line, X-ray diffraction (XRD) analyzer capable of continuously monitoring phase abundances for use in process plant control. This has been achieved through a joint project between CSIRO Minerals and Fuel & Combustion Technology Pty. Ltd. with an instrument designed for use in a Portland cement manufacturing plant. Key factors in tailoring such an instrument to the cement industry were (i) the handling and presentation of a dry sample and (ii) the development of an analytical method suitable for the complex suite of phases contained within Portland cement. The instrument incorporates continuous flow of sample through the diffractometer using a purpose-built sample presentation stage. The XRD data are collected simultaneously using a wide range (120° 2θ) position sensitive detector, thus enabling rapid collection of the full diffraction pattern. The data are then analyzed using a Rietveld analysis method to obtain a quantitative estimate of each of the phases present. The instrument is controlled by a PC linked to the diffractometer through a purpose built interface. The phase abundance information is then transmitted to the central computer in the cement plant where it can be used for the control of mill parameters such as temperature and retention times as well as gypsum feed rate.

The mixed ligand complexes of manganese(II), nickel(II), copper(II), zinc(II), and cadmium(II) involving aspartic acid and benzoic acid have been synthesized. The complexes were studied by various spectroscopic techniques such as infrared, electronic, X-ray diffraction, and magnetic measurements. The complexes were found to have octahedral geometry. The X-ray powder diffraction results show that the crystal systems of Mn(II)-Asp-Ben complex are hexagonal, and Ni(II)-Asp-Ben, Cu(II)-Asp-Ben, Zn(II)-Asp-Ben, and Cd(II)-Asp-Ben complexes are found to be triclinic. The value of unit-cell parameters and XRD data for the five mixed ligand complexes are reported.

A powder neutron diffraction study has been undertaken for the titled compounds at room temperature. Data were analyzed using the Rietveld method. With increasing Nd content the unit cell has been found to contract very slightly, which is in accordance with the ionic radii of La3+ and Nd3+.

X-ray powder diffraction data, unit cell parameters, and space group for a new platinum-based anticancer complex cis-[bis(acetonitrile)]-[(1R,2R)-1,2-diaminocyclohexane-κN, κN′]platinum (II)nitrate (1:2) monohydrate, cis-[Pt(C2H3N)2(C6H14N2)](NO3)2·H2O, are presented [a=12.638(3) Å, b=12.153(2) Å, c=11.881(3) Å, β=95.145(4)°, space group P21, cell volume=1817.5 Å3, and Z=4]. All measured lines were indexed and are consistent with the P21 space group. No detectable impurities were observed.

Palmierite (K2Pb(SO4)2) has been prepared via a chemical synthesis method. Intensity differences were observed when X-ray powder data from the newly synthesized compound were compared to the published powder diffraction card (PDF) 29-1015 for Palmierite. Investigation of these differences indicated the possibility of preferred orientation and/or chemical inhomogeneity affecting intensities, particularly those of the basal (00l) reflections. Annealing of the Palmierite was found to reduce the effects of preferred orientation. Electron microprobe analysis confirmed K:Pb:S as 2:1:2 for the for the annealed Palmierite powder. Subsequent least-squares refinement and Rietveld analysis of the annealed powder showed peak intensities very close to that of a calculated Palmierite pattern (based on single crystal data), yet substantially higher than many of the PDF 29-1015 published intensities. Further investigation of peak intensity variation via calculated patterns suggested that the intensity discrepancies between the annealed sample and those found in PDF 29-1015 were potentially due to chemical variation in the K2Pb(SO4)2 composition. X-ray powder diffraction and crystal data for Palmierite are reported for the annealed sample. Palmierite is trigonal/hexagonal with unit cell parameters a=5.497(1) Å, c=20.864(2) Å, space group R-3m(166), and Z=3.

Fe–N thin films were deposited on glass substrates by dc magnetron sputtering under various Ar∕N2 discharge conditions. Crystal structures and elemental compositions of the films were characterized by X-ray diffraction and X-ray photoelectron spectroscopy. Magnetic properties of the films were measured using a superconducting quantum interference device magnetometer. Films deposited at different N2∕(Ar+N2) flow ratios were found to have different crystal structures and different nitrogen contents. When the flow ratios were 60%, 50%, and 30%, a nonmagnetic single-phase FeN was formed in the films. At the flow ratio of 10%, two crystal phases of γ′-Fe4N and ε-Fe3N were detected. When the flow ratio reduced to 5%, a mixture of α-Fe, ε-Fe3N, FeN0.056, and α″-Fe16N2 phases was obtained. The value of saturation magnetization for the mixture was found to be larger than that of pure Fe.

A recently developed Rigaku parallel-beam X-ray diffraction system equipped with a parabolic graded-multilayer mirror in the incident beam and a parallel-slits analyzer in the diffracted beam was used for precision high-temperature diffraction studies. The lattice parameters a and c of α-Al2O3 at room temperature and up to 1473 K were determined with precision in the range of 0.6–7.3×10−5. The thermal expansion coefficients for a and c agreed with literature values to better than 3%. The system was used successfully also to determine the Debye characteristic temperature of Si and to study structural phase transition of LaCoO3 from rhombohedral at room temperature to cubic at 1700 K.

New salts of barium with dicarboxylic acids (glutaric, adipic, pimelic, suberic, sebacic, and dodecanedioic) were synthesized and characterized by powder diffraction techniques. In addition to the basic crystallographic data and chemical analyses of barium glutarate hexahydrate {1}, barium adipate {2}, barium pimelate {3}, barium disuberate {4}, barium sebacate {5}, and barium dodecanedioate {6}, the processes of their thermal decomposition were investigated by XRPD. All the compounds decompose to barium carbonate at temperatures between 400 and 500 °C.