Methods of the structure analysis were used to determine the incommensurate structure modulation in a sample of hauyne from Laacher Lake, Germany. The modulation parameter n=0.145, determined using single-crystal patterns, was refined using powder data. An indexing technique for additional reflections (satellites) using a parameter subcell and Miller index main reflections was suggested. Crystallographic characteristics of the hauyne of Laacher Lake are compared with that of hauyne from Sacrafano (Italy) and with lazurtes from Baikal, Pamir, and Afghanistan. We found that the crystal structure modulation can serve as a source of paragenesis information on sulphate bearing sodalte group minerals.

X-ray powder diffraction is one of the most sensitive methods for the analysis of crystalline forms of silica. In addition to detection and quantification, it can determine the specific crystalline species in the sample. The principal limitations of the method depend on the effective volume of the sample in the X-ray beam and the number of crystallites in the proper orientation to diffract. Detection limits are usually reported as 2 μg in thin-film filter mounts and 0.1% in bulk samples that are free of interference from associated minerals. Filter methods are most often used for air quality monitoring and several standardized procedures have been certified. Standard procedures for bulk samples are difficult to certify because of the variability of the matrices and their potential interferences. All of the methods of quantification require calibration with known samples of quartz or cristobalite. Certification of standard samples involves characterization of the particle and crystallite size and size distribution and amorphous content as well as determining the X-ray diffraction response. Although quartz is readily available and cristobalite is easy to synthesize, preparation of quantities of sufficient uniformity and stability is a limiting factor in certifying such samples for reasonable costs. Conventional diffraction equipment can be used for crystalline silica analysis at the present detection limits required by safety standards. Relatively simple modifications of the diffractometer will increase its sensitivity to small amounts of silica and improve the lower limits of quantification.

Using the Rietveld profile method, the atomic coordinates and anisotropic temperature factors of KCaF3 were refined. At room temperature, KCaF3 crystallizes in monoclinic B21/m symmetry, with the lattice parameters: a=8.754(2) Å, b=8.765(4) Å, c=8.760(5) Å, β=90.48(3)°, V=672.1(3) Å3, Z=8. The refinement procedure was stopped when RB=0.05 and the Durbin–Watson statistic factor=0.85 had been reached. The structure determined is related to the tilting of CaF6 octahedra of the a−b+c− type, which are responsible for the monoclinic distortion in perovskite crystals.

The compound DyNiSn has been studied by X-ray powder diffraction. The X-ray diffraction patterns for this compound at room temperature are reported. DyNiSn is orthorhombic with lattice parameters a=7.1018(1) Å, b=7.6599(2) Å, c=4.4461(2) Å, space group Pna21 and 4 formula units of DyNiSn in unit cell. The Smith and Snyder Figure-of-Merit F30 for this powder pattern is 26.7(0.0178,63).

X-ray powder diffraction data are reported for α-brass with the composition Cu: 63.44±0.04 wt %, Zn: 36.45±0.06 wt %. No valid reference card for this material is present in the JCPDS-ICDD database. The investigated brass composition is cubic (Fm3m) with a0: 3.69612±0.00014 Å, unit cell volume: 50.4938±0.0058 Å3, density calculated: 8.44±0.05 g/cm3, density measured: 8.43±0.03 g/cm3. The X-ray diffraction pattern presented resembles that of deleted reference card 6-657 in great detail.

A new mixed lead thorium phosphate, Pb0.5Th2(PO4)3, has been isolated in the system PbO–ThO2–P2O5. Its crystal structure (monoclinic symmetry, a=17.459(1) Å, b=6.8451(4) Å, c=8.1438(5) Å, β=101.247(5)°, space group C2/c) has been determined from conventional monochromatic X-ray powder diffraction data. The structure is related to the MITh2(PO4)3 structure type. Lead atoms are located in the channels parallel to the c axis, out of the twofold axis for 0.97 Å, and are statistically distributed on a quarter of crystallographic positions. The thermal stability of this material is greater than that of the monazite-type compound PbTh(PO4)2.

An organic nonlinear optical material, 3-methyl-4-methoxy-4′-nitrostilbene (C16H15NO3), has been characterized by X-ray powder diffraction. Experimental values of 2θ corrected for systematic errors, relative peak intensities, values of d, and the Miller indices of 77 observed reflections with 2θ up to 82° are reported. The powder diffraction data have been evaluated, and the figures-of-merit are reported. The unit cell parameters least-squares refined from 30 non-overlapping peaks of the orthorhombic compound with a Aba2 space group are a=15.7882(3) Å, b=13.4892(4) Å, c=13.3940(2) Å, V=2852.5(4) Å3, Z=8, Dx=1.254 g/cm3. The powder diffraction results are in a agreement with those obtained from single-crystal structure data.

2,4,6-Trimercapto-s-triazine, trisodium salt (ideally, Na3S3C3N3·9H2O), also known as TMT-55, is a white powder that is used to precipitate heavy metals from contaminated waters. Chemical analyses confirmed the nominal composition. TMT-55 crystals are uniaxial negative with indices of refraction (25 °C) of nε=1.520 and nω=1.675. The structure was determined by single-crystal methods at 25 and −110 °C. A powder pattern was determined and compared to a simulated pattern based on the 25 °C structure data. Crystal data at 25 °C are: R3;Z=6; a=17.600(1) Å and c=9.720(2) Å; V=2607.5(5) Å3; Dx=1.55 g/cm3.

The X-ray powder diffraction patterns for two new synthetic calcium uranium (VI) silicate hydrate phases are reported. Ca1.5U6(OH)7O16·7H2O is orthorhombic, space group P*a*, with unit cell a=13.8949(14), b=12.0776(12), c=15.228(3) Å. The structure appears to be related to that of becquerelite. Ca2(UO2)2(Si2O5)3·10H2O was also indexed on an orthorhombic unit cell, a=12.075(3), b=15.406(6), c=26.043(6) Å. The Powder Diffraction File coverage of uranium-containing minerals which could, on the basis of their chemical formula, form in U-containing cements is also reviewed.

The activity of the high Tc task group of the ICDD Ceramic Subcommittee is described. This activity includes the compilation of X-ray powder diffraction patterns of the high Tc superconductors and related phases identified from the International Centre for Diffraction Data/Powder Diffraction File (ICDD/PDF). The coverage of this ICDD/PDF Superconductor SubFile (SC) includes high Tc phases and their structurally related phases, products of elemental substitution in the high Tc phases, phases found in the phase diagrams containing the high Tc phases, as well as potential reaction products with commonly used sample containers, and potential conventional low-temperature (metallic and nonmetallic) superconductors.

We have calculated X-ray powder-diffraction data for schoepite, [(UO2)8O2(OH)12](H2O)12, using unit-cell and atomic parameters from the crystal structure (a 14.337, b 16.813, c 14.781, Z=4, Dx=4.87 gcm−3). Schoepite crystallizes in space group P21ca but is strongly pseudo- centrosymmetric, and observed reflections (Irel>0.1%) conform to space group Pbca. The six strongest reflections for schoepite are [d(Å), hkl (relative intensity)] 7.365, 002 (100), 3.253, 242 (55), 3.626, 240 (36), 3.223, 402 (25), 3.683, 004 (20), 2.584, 244 (18). The calculated intensities of reflections that distinguish space group Pbca from space group Pbna (the space group of metaschoepite), i.e., h0l with h odd and l even, are weak, and may not be evident in experimental powder patterns. The a axis of schoepite (14.34 Å) is significantly longer than that of synthetic metaschoepite (13.98 Å), and the two phases can best be distinguished by their unit-cell parameters. However, potential overlap of the strongest reflections can make identification and unit-cell determination difficult, especially for fine-grained material. Natural samples commonly contain intergrowths of schoepite, metaschoepite, and dehydrated schoepite. The calculated powder pattern for schoepite agrees well with data reported for natural schoepite (PDF 13-241) but shows discrepancies with the data from synthesis products. Data for “synthetic schoepite” indicate that this product was a mixture. Powder data labeled “paraschoepite” in the Powder Diffraction File do not correspond to the mineral of that name.

The two germanates K2MgGeO4 and K2CdGeO4 have been synthesized by solid-state reaction. These compounds are isostructural with K2ZnGeO4, space group Pca21 (No. 29), Z=8. Unit cell parameters were determined: for K2MgGeO4a=11.1810(11), b=5.5708(6), c=15.8694(16) Å, V=988.5(3) Å3 and for K2CdGeO4a=11.4777(24), b=5.7155(7), c=16.1732(17) Å, V=1061.0(5) Å3. Powder diffraction data are reported.

The crystal structure of low temperature NaNiO2 has been refined by Rietveld methods using powder X-ray diffraction and neutron scattering data. The starting model was based on parameters that had been obtained earlier by X-ray film methods. At room temperature NaNiO2 is monoclinic, C2/m, a=0.53192(2), b=0.28451(1), c=0.55826(4) nm, β=110.449(2)°. NaNiO2 has a layered structure. The Ni–O layer is formed by edge sharing of Jahn–Teller elonganted NiO6 octahedra with Ni–O distances of 0.1911(2) nm and 0.2144(4) nm. The Na ions between these layers also exhibit a distorted octahedral coordination with Na–O distances of 0.2328(2) nm and 0.2369(4) nm. The final R values were Rwp=0.069, RI=0.059, Rexp=0.059 for the neutron and Rwp=0.032, RI=0.034, Rexp=0.017 for the X-ray data.

The boron and iron for aluminum substitution in the Rb-leucite structure (RbAlSi2O6, ICDD card 38-201) has been examined by sol-gel preparation of different samples along the three compositional joins Rb(X,Y)Si2O6, where X and Y are any two of the elements Al, Fe, B. The compound RbBSi2O6 (a0=12.831 Å) is here described and characterized by X-ray powder diffraction for the first time, while the compound RbFeSi2O6 is reexamined with a more precise determination of lattice parameters and diffraction intensities with respect to ICDD card 31-1189. The lattice parameters and the space groups of different selected terms of the three solid solutions are reported.

Two compounds with compositions around n=14 and n∼5.4 (n=Bi/Mo molar ratio) have been prepared by solid-state reaction with five heating/grinding cycles at 800 °C. The lattice constants of both compounds can be related to the fluorite-type structure of δ-Bi2O3. Bi14MoO24 has been indexed as an orthorhombic pseudotetragonal (√2×√2×1) superstructure: a=7.812 (±0.005) Å, b=7.762 (±0.005) Å, c=5.7716 (±0.0007) Å (but a+b=15.5750±0.0020). For orthorhombic (3×5×3) Bi38Mo7O78: a=16.8236 (±0.0027) Å, b=28.6182 (±0.0045) Å, c=16.9082 (±0.0027) Å.

X-ray powder diffraction data and refined unit cell parameters for the (Bi, Pb)2Sr2Ca2Cu3Ox (2223) superconducting phase, indexed using incommensurate modulation principles, are reported. Comparison of the results obtained with one- and two-component modulation wave vectors showed that the two-component modulation wave vector is superior for indexing the satellite reflections. A two-component wave vector indexing result seems likely when only the powder diffraction data are considered.