A polycrystalline sample of YbCoO3 was prepared using a water-soluble complex method at relatively low temperatures. Common chelating ligands such as citric acid were employed for the synthesis of complex-based precursors, followed by thermal decomposition of the precursors at high temperatures. X-ray diffraction data were collected and the crystal structure was refined by the Rietveld method. The structure of YbCoO3 can be described as a sesquioxide C-M2O3-like structure with space group Ia-3 and unit-cell parameter a=10.4470 (2). The Yb3+ and the Co3+ cations are found to preferentially occupy the two nonequivalent 8d and 24d sites, respectively. The two independent atoms Yb/Co have octahedral coordination; however, the degrees of distortion of their coordination polyhedron are different. The relationship between the title compound and the orthorhombic Perovskite structure of YbCoO3 reported in the literature is established.

XRD analysis of plasma-vapor-deposited ErT2 films during aging (T decay to 3He) reveals an hkl-dependent unit-cell expansion in which (200) grains expand out-of-plane as much as 0.01 Å more than (111) out-of-plane grains. Texture analysis of an aged ErT2 film reveals a bimodal (111)/(200) out-of-plane preferred orientation. sin2 ψ analysis reveals significant in-plane macro-strain due to 3He bubble formation/growth. The mechanistic origins regarding these observations are also discussed.

A new polymorph of Al2(WO4)3 is observed from in situ high pressure powder X-ray diffraction (ADXRD) measurements at 3.4 GPa. The ADXRD pattern at 3.4 GPa could be explained based on a monoclinic lattice (space group P21) with unit cell parameters: a=9.5884(24), b=12.5204(38), c=7.8463(33) Å, and β=91.98(2)°.

A state-of-art semiconductor technology-based position sensitive area detector, namely D/teX-25, has recently been developed for high-speed and high-sensitivity X-ray diffraction (XRD) analysis of materials. X-ray powder diffraction intensities obtained by a D/teX-25 detector were found to over 50 times higher than those by a conventional scintillation counter. A D/teX-25 detector mounted on a conventional 2 kW XRD system has been used to collect ultrafast XRD data with scanning speeds up to 160°2θ per minute. Ultrahigh-speed XRD is particularly useful for time-resolved dynamical and in-situ studies. A D/teX-25 detector was successfully used on a Rigaku XRD differential scanning calorimetry (DSC) system for simultaneous measurements of XRD and DSC data under controlled temperature and humidity conditions. This has made possible the study of complex and rapid phase transformations of pharmaceutical terfenadine. The D/teX-25 area detector has also been used for recording two-dimensional XRD patterns showing the particle-size effects on α-quartz powder intensities and to obtain digital X-ray topographic images of a complex dislocation network in a Si wafer.

Four aliphatic-aromatic diols with ether linkages [4, 4′-Bis(2-hydroxyethoxy)benzophenone, 4, 4′-Bis(3-hydroxypropoxy)benzophenone, 4, 4′-Bis(6-hydroxyhexyloxy)benzophenone, 4, 4′-Bis(11-hydroxyundecyloxy)benzophenone] and two aliphatic-aromatic diols with sulfur linkages [4, 4′-Bis[(2-hydroxyethyl)thio]benzophenone, 4, 4′-Bis[(3-hydroxypropyl)thio]benzophenone] have been characterized by X-ray powder diffraction. These diols can be used for synthesis of thermoplastic nonsegmented polyurethanes. Experimental 2θ peaks positions, relative peak intensities, values of d, and Miller indices as well as unit-cell parameters are presented.

Botallackite, Cu2(OH)3Cl, from the Botallack mining area in Cornwall, United Kingdom, has been reinvestigated regarding physical, optical, chemical, and X-ray powder diffraction data. It forms emerald-green tabular crystals slightly elongated along [010] with {001} (dominant), {100}, {010}, and {011}. Botallackite is biaxial positive, 2V=70(2)°, the optical orientation is Y∧c 22(2)° (in obtuse β), Z=b. Electron-microprobe analyses gave CuO 73.26, ZnO 0.22, Cl 16.80, H2O (calc) 12.37, total 102.65, less O=Cl 3.79, total 98.86 wt %, corresponding to the empirical formula Cu1.99Zn0.01(OH)2.97Cl1.03 (based on four anions). Unit cell parameters refined from X-ray powder diffraction data are a 5.7155(5), b 6.1255(6), c 5.6336(4) Å, β 93.090(8), V 196.95(2)Å3,Z=2.

X-ray diffraction pattern from cotton fiber (dch32) grown in the Karnataka state of India has been recorded. Fiber was found to contain 17 Bragg reflections, of which 11 are broadened because of crystal size and intrinsic strain influences. Contributions to integrated intensities from intrinsic strain in the fiber have been estimated using line profile analysis. A molecular model was first constructed with standard bond lengths and angles using helical symmetry and layer-line spacings observed in the X-ray pattern. The model was then refined against observed X-ray data using the linked atom least squares (LALS) method. The refinement has been done with and without the intrinsic strain correction to find the extent of structural changes. These changes have been quantified in terms of bond angles, bond lengths, and torsion angles. Young’s modulus has been estimated for these fibers using the results of line profile analysis, and a broad agreement with the reported physical measurements has been obtained.

This study examined basal peak irrationalities according to boundary conditions of the hectorite basal diffraction unit (BDU), which were recognized as the total assembly of 2:1 phyllosilicate layer plus interlayer material. The hectorite basal profiles were computer-simulated using the three kinds of BDU settings identified from the middle of octahedral sheets in the nearest neighbor (centrosymmetric model), the middle of interlayers in the nearest neighbor (centrosymmetric model), and a basal oxygen plane to the margin of interlayer in contact with the next phyllosilicate layer (non-centrosymmetric model). In the results of simulations, irrationality and asymmetry of the hectorite basal peaks relied straightforwardly on the BDU scattering modulations for the non-Bragg angles containing information on the synergic scattering events of phyllosilicate layer and interlayer material. Among the concerned BDU boundaries, the non-centrosymmetric model more effectively represented the real hectorite profile than the two previously reported centrosymmetric models.

X-ray powder diffraction data for the high temperature phase of NaBi3V2O10 obtained from in situ high temperature XRD studies are presented. NaBi3V2O10 undergoes a phase transition from triclinic to monoclinic at about 600 °C. The unit cell parameters of the high temperature monoclinic phase at 600 °C are: a=12.3899(21), b=5.5642(10), c=7.1543(18) Å and β=98.393(16)°, V=487.94(13) Å3 and Z=2, ρcal=6.20 g∕cc. On further increasing the temperature, it partially decomposes to a γ-Bi4V2O11 type phase. The details of this phase as well as the stability of NaBi3V2O10 are discussed.

The value assignment of candidate Standard Reference Material (SRM®) 57b Silicon Metal provided an opportunity to develop an alkali reaction procedure as a precursor to borate fusion for the preparation of test specimens from the metal powder for X-ray fluorescence spectrometry (XRF). Suggested for this purpose by Blanchette in a 2002 Advances in X-ray Analysis article [45, 415–420 (2002)], the alkali reaction uses LiOH∙H2O to convert Si to Li2SiO3. Lithium silicate is fused with lithium borate flux without damage to platinum ware. Once specimens are fused and cast as beads, calibration standards are prepared to closely match the compositions of the specimens, allowing a linear calibration for each analyte. The XRF method yields results that are directly traceable to the mole through NIST SRM spectrometric solutions. The method was validated in two ways. First, the reaction was used on older SRMs for Si metal: SRM 57 and SRM 57a. Second, XRF results for candidate SRM 57b were compared to results obtained using prompt gamma-ray activation analysis (PGAA) and inductively coupled plasma optical emission spectrometry (ICPOES). Bias tests show the XRF results are accurate for the elements Al, S, Ca, Ti, Cr, Mn, Ni, Cu, and Zr. Levels of S, Ca, Cr, and Cu in candidate SRM 57b are near the limits of quantification of the borate fusion method. Iron results may be subject to a low bias. Phosphorus is not quantitatively retained during the alkali reaction and borate fusion. These elements, plus B, which cannot be determined after borate fusion, are listed in manufacturing specifications for Si metal.

An incident beam X-ray collimator for Mao-Bell type diamond anvil cell (DAC) has been developed. Alignment of the collimator is carried out in situ while viewing the image of the collimated X-ray spot formed on a thin layer of fluorescent material spread on the diamond anvil culets with the help of a microscope. Special precaution has been taken to meet the radiation safety requirements during alignment and routine use. This collimator is of immense help for laboratory based high pressure X-ray diffraction experiments.

Single-phase samples of La1−xCaxMnO3 compounds have been synthesized by solid-state reaction. Detailed Rietveld analysis of powder X-ray diffraction data showed that La1−xCaxMnO3 undergoes a structural phase transformation from R-3c to Pnma at X=0.05–0.075. There is a linear variation of lattice parameters as a function of calcium concentration. The slope of this linear variation changes at X=0.6. A correlation between observed Mn-O bond lengths, corresponding to different compositions, and possible magnetic phases is discussed.

In the course of our research on normal alkanols, the crystal structure of 1-pentanol has been solved by applying Patterson-search methods to laboratory powder X-ray diffraction data recorded on a curved position-sensitive detector (CPS120) at 183 K. The crystal structure was refined with the rigid-body Rietveld least-squares method. The cell is monoclinic, space group P21∕c, Z=4, and the cell parameters are a=15.592(9) Å, b=4.349(1) Å, c=9.157(1) Å, β=104.7(7)°, V=600.6(3) Å3. There is one molecule in the asymmetric unit with the O–H bond in gauche conformation with respect to the alkyl skeleton. Packing is defined by the hydrogen bonds linking the 1-pentanol molecules along zigzag chains parallel to b.