The crystal structure of K2Zn(PO3)4 was determined and refined using the Rietveld method based on the isostructure model of K2Cu(PO3)4. This compound belongs to the monoclinic system with space group Cc and lattice parameters of a=11.0941(2) Å, b=12.5215(3) Å, c=7.6597(2) Å, and β=102.47(2)°. The chemical formula unit per unit cell is Z=4 and the calculated density is 2.938(3) g∕cm3. Zigzag [PO3]∞ chains formed along the a axis, and their period contains eight PO4 tetrahedrons.

Powder diffraction experiments performed as a function of external variables like, e.g., temperature, pressure, or time open possibilities to gain additional information about the physical and chemical properties of the system under study. Sensible extraction of such information directly from in situ experiments requires the treatment of the dataset with methods like sequential and/or parametric refinements. We are progressing towards the development of the parametric refinement method, which performs simultaneous phase refinements of in situ powder patterns by imposing several rational physical models of the evolving parameters on the calculated powder diffraction profiles. One of the fundamental prerequisites for this method is that the powder patterns in the in situ dataset be grouped to their relevant phases. In this paper, we present an analytical method which uses the Pearson’s correlations coefficients of the powder patterns to automatically determine the phase transition points of the in situ powder dataset. The phase transition points determined are used to group the powder patterns belonging to identical phases and to prepare the patterns for automated sequential phase refinements. The proposed algorithm is implemented as an automated module in the multi powder diffraction pattern, data reduction software Powder 3D.

Quantification of potentially toxic single mineral phases in natural dusts of heterogeneous composition is critical for health hazard assessment. For example, crystalline silica, a human carcinogen, can be present as respirable particles in volcanic ash such as quartz, cristobalite, or tridymite. A method to rapidly identify the proportions of crystalline silica within mixed dust samples, such as volcanic ash, is therefore required for hazard managers to assess the potential risk of crystalline silica exposure to local populations. Here we present a rapid method for quantifying the proportions of single phases in the mineral assemblage of mixed dusts using X-ray diffraction (XRD) with a fixed curved position-sensitive detector. The method is a modified version of the whole-pattern peak-stripping (PS) method (devised by Cressey and Schofield [Powder Diffr.11, 35–39 (1996)]) using an internal attenuation standard (IAS) but, unlike the PS method, it requires no knowledge of other phases present in the sample. Ten synthetic sample mixtures were prepared from known combinations of four pure phases (cristobalite, hematite, labradorite, and obsidian), chosen to represent problematic constituents of volcanic ash, and analyzed by XRD. Results of the IAS method were directly compared with those of the PS method. The proportions of cristobalite estimated using the methods were comparable and accurate to within 3 wt %. The new IAS method involved less sample preparation and processing and, therefore, was faster than the original PS method. It therefore offers a highly accurate rapid technique for determination of the proportions of individual phases in mixed dusts.

The successful synthesis of ZnS hollow microspheres by a solvothermal route is reported. The synthesis was achieved by a proper selection of a sulfur source, i.e., Na2S2O3⋅5H2O or (NH2)2CS, to react with Zn(CH3COO)2⋅2H2O in mixed solvents of ethylene glycol and deionized water. The ZnS products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and photoluminescence spectroscopy. XRD identified the ZnS products to have either zinc blende or wurtzite structure. SEM images revealed hollow ZnS microspheres with 1 to 2 μm diameters and 100 to 200 nm shell thicknesses. TEM images confirmed that the hollow ZnS microspheres were assembled by ZnS crystalline nanocrystallites. The room-temperature photoluminescence spectrum of the zinc blende hollow microspheres showed a strong green emission at 514 nm and weak emission at 379 nm.

A monoclinic phase isostructural to Al4W was revealed in Al–Ni–Re close to the Al–Re terminal. It is assumed to be a ternary extension of the high-temperature Al4Re phase usually transforming in binary alloys even by sharp quenching from the existence temperatures. The powder X-ray diffraction pattern of this phase of the Al77Ni2.5Re20.5 composition was indexed for the Cm space group with a=5.1538(12) Å, b=17.410(5) Å, c=5.1546(15) Å, and β=100.548(16)°.

X-ray powder diffraction data, unit cell parameters, and space group for alaptide are presented (a=21.136(4) Å, b=7.212(4) Å, c=6.126(3) Å, space group P212121, cell volume=933.8(8) Å3, and Z=4). All measured lines were indexed and are consistent with the P212121 space group. No detectable impurities were observed.

SrBi2OB4O9 is a novel centrosymmetric borate oxide forming in the SrO–Bi2O3–B2O3 system. Its crystal structure has been determined ab initio from high-resolution X-ray and neutron powder diffraction data with the help of 11B MAS-NMR data. SrBi2OB4O9 crystallizes with a triclinic unit-cell with a=6.8657(1) Å, b=9.7976(1) Å, c=6.8148(1) Å, α=109.1270(8)°, β=101.8971(8)°, γ=96.1445(8)°, V=416.17(1) Å3, Z=2, space group P-1. Its structure consists of Bi2O4+ layers alternating along the b axis with SrB4O94− layers containing isolated B4O96− (〈2Δ〉Δ) tetraborate anions.

A natural sodalite from the geological site Alkaline Complex of Floresta Azul, Bahia, Brazil, has been characterized by electron microprobe, infrared spectroscopy, and powder high-resolution X-ray diffraction techniques. The mineral is an aluminosilicate framework, formed by cages called sodalite unity. Although the sample is natural, the chemical analysis reveals that it is indeed the end member sodalite sensu strictu, Na8[Si6Al6O24]Cl2. Infrared spectroscopy shows Si, Al tetrahedral-oxygen stretching nonsymmetric mode, stretching symmetric mode, and bending modes. Indexing of the experimental X-ray diffraction pattern led to cubic space group P-43n, and unit-cell parameters: a=8.8767(7) Å, Dx=2.301 g cm−3, and V=699.46(1) Å3. X-ray diffraction data are reported. Rietveld refinement was also performed, and the confidence factors are Rp=0.079, Rwp=0.118, and χ2=2.19. The structure of the minerals of sodalite group holds four different tetrahedra: AlO4, ClNa4, Na(ClO3), and SiO4, with Al, Cl, Na, and Si located at the center of each tetrahedron.

Powder X-ray diffraction studies of a lithium salt of thiazolidine-4-carboxylic acid (Li-TC4) of composition LiC4H6NSO2 are presented in this paper. Analysis of the synchrotron powder X-ray diffraction data showed that the complex has an orthorhombic symmetry with space group P212121. Unit cell parameters after the refinement using the Pawley method are: a=19.4931(3) Å, b=4.947 77(6) Å, c=6.201 64(8) Å, and V=598.051 Å3.

Manganese molybdate with the formula Mn2MoO5.0.6H2O was synthesized by hydrothermal reaction at 200 °C. The crystal system of this compound is triclinic, space group P−1, Z=1, unit-cell parameters: a=5.7769(5), b=9.7559(6), c=2.8961(2), α=94.37(1), β=101.37(1), and γ=94.75(1). The measured density (Dm) and calculated density (Dx) are 3.200 and 3.103, respectively.

Co(II) complexes with benzoic acid and ternary complexes with ligands benzoic acid and histidine/aspartic acid have been synthesized and characterized using various spectroscopic methods. On the basis of infrared, UV-visible spectra, and magnetic data the complexes were found to be having octahedral polymeric geometry. X-ray powder diffraction results show that the crystal systems of Co(II)-Ben and Co(II)-Ben-Hist complexes are triclinic with lattice constants a=15.58 Å, b=11.92 Å, c=4.33 Å, α=96.08°, β=104.68°, γ=88.46°, and V=774.15 Å3 and a=18.88 Å, b=17.01 Å, c=15.13 Å, α=93.15°, β=89.41°, γ=100.71°, and V=4768.75 Å3, respectively. The Co(II)-Ben-Asp complex is orthorhombic with lattice constants a=21.57 Å, b=15.06 Å, c=11.40 Å. α=β=γ=90°, and V=3703.38 Å3.

X-ray powder diffraction data for three new bismuth yttrium ytterbium oxide compounds synthesized by solid-state reaction method are reported. The unit-cell dimensions were determined from X-ray diffraction method using Cu Kα radiation and evaluated by indexing programs. The cubic δ-Bi2O3 phase was identified to be the sole crystalline phase in Bi0.82Y0.09Yb0.09O1.5, Bi0.82Y0.12Yb0.06O1.5, and Bi0.82Y0.06Yb0.12O1.5 with lattice constants of a=5.5110(3), 5.5154(2), and 5.5113(2) Å, respectively.

This manuscript describes the construction, testing, and use of a simple side-loading air-tight specimen holder for use with Bruker X-ray powder diffractometers.