In pursuit of design and characterisation of Cu adsorbing in thin films, we present data from a large variety of Cu-K edge X-ray Absorption Near Edge Spectroscopy (XANES) spectra obtained from organic and inorganic standards. Additionally, we have explored the impact of beam damage inducing redox alterations. Polymer nanoparticles were tested against films to produce higher concentration samples while maintaining high surface area to bulk effects. Spectra from nanoparticles were highly comparable to thin films of ~8 nm thickness, implying comparable contributions by surface effects on copper association. Finally, we observed no impact on Cu XANES spectra from vitrification with dimethyl sulfoxide to produce amorphous frozen, hydrated samples. The spectra should act as a valuable resource in assisting the design of experiments and identification of copper associations.

Crystal data and results of structure refinements for ScPO4 are reported. The material is tetragonal, I41/amd, with a = 6.5787(2) Å, c = 5.7963(2) Å, Vd = 250.86(2) Å3, Z = 4, Dx = 3.704 Mg/m3. Intensity data were obtained from a Stoe transmission type diffractometer equipped with a position sensitive detector. CuKα1 radiation, λ = 1.5405981 Å was employed. Silicon, SRM 640b (a = 5.43094 Å) was used as an internal standard. The structure was refined by the Rietveld method by aid of three different programs.

Powder X-ray diffraction was used to monitor the solvent-free synthesis of two-dimensional (2D) metal–organic frameworks (MOFs) via mechanochemical methods. For four isophthalic acid-based, alkoxide-functionalized organic ligands, optimal milling times were found to vary from 12 to 48 min. This work confirms that mechanochemical synthesis routes can be utilized to afford highly-crystalline, 2D MOFs.

Aluminum borate (9Al2O3·2B2O3) whiskers were chemically synthesized in potassium sulphate flux by using the starting chemicals of aluminum sulphate and boric acid. The synthesis temperature of 1075 °C was found to be the optimum with respect to whisker morphology. A tentative X-ray diffraction (XRD) pattern was suggested for the whiskers produced after heating at 1150 °C. The product purity, phase composition, and whisker morphology were investigated by XRD, energy dispersive X-ray spectroscopy, and scanning electron microscopy, respectively.

To achieve increased case and precision of alignment, and to allow for convenient alteration between normal usage with filtered radiation and crystalmonochromated radiation, the G. E. goniometer has been mounted on milling machine beds allowing for x-y translation and 360° rotation; in addition the tube mount was repositioned. The usefulness of this apparatus has been demonstrated by accurately aligning the goniometer for usage with filtered radiation, with a new alignment procedure. As a demonstration of the accuracy and precision of alignment, the lattice parameter of silicon was determined from a powder sample. A least-squares analysis of the data gave a0 = 5.43046 Å with a standard deviation of ±0.00005 Å, in excellent agreement with the value of 5.43054 ± 0.00017 Å determined in a recent International Union of Crystallography test in many laboratories.

A monochromator housing has been built for use with all types of direct-beam monochromators and all radiations. This apparatus attaches to the new tube mount and was used to determine the optimum procedure for preparing the doubly bent LiF monochromator crystals designed by Warren to minimize the volume sampled in the reciprocal space of a single crystal. According to a suggestion made by Chipman, a doubly bent monochromator for use with poly crystalline specimens has been formed and its geometry and applications are presented. This monochromator gives about one-half as much intensity as that obtainable using filtered radiation and similar operating conditions ; this type of monochromator is therefore a powerful tool for use with powder specimens. A transmission diffracted-beam monochromator has also been constructed which attaches in a simple manner under the counter tube housing. Under similar operating conditions with a LiF monochromator, this yields intensities only one-tenth of those obtained using filtered radiation.

The analysis of the distribution of pharmaceutical materials in tablet formulations, such as drugs and matrix elements, is critical to product performance and is used in such areas as quality control, impurity testing, and process monitoring. Recently imaging techniques, such as Raman, near-IR, and fluorescence imaging, have become popular for “visualization” of pharmaceutical formulations, allowing for spatial and chemical composition information to be obtained simultaneously. These methods have been primarily focused on molecular imaging, or spatial analysis of the molecular characteristics of the tablet formulation. However, elemental species are also an important part of pharmaceuticals. Micro X-ray fluorescence (MXRF) elemental imaging offers complementary information to molecular imaging techniques. In this study, MXRF was used for the elemental imaging of various commercial pharmaceutical drug and vitamin supplements. Specifically, elemental composition and heterogeneity were monitored for each different tablet.

Single crystals and powder samples of Ca2Bi5O5and Ca4Bi6O13have been synthesized and studied using single crystal X-ray diffraction as well as X-ray and neutron powder diffraction. Unit cell dimensions were calculated using a least squares analysis that refined to a δ2θof no more than 0.03°. A triclinic cell was found with space group , a = 10.1222(7), b = 10.1466(6), c = 10.4833(7) Å. α= 116.912(5), β= 107.135(6) and γ= 92.939(6)°, Z = 6 for the Ca2Bi2O5compound. An orthorhombic cell was found with space group C2mm, a = 17.3795(5), b = 5.9419(2) and c = 7.2306(2) Å, Z = 2 for the Ca4Bi6O13compound.

Weight fractions of four dominant phases (C3S, C2S, C4AF, and C3A) present in five industrial clinkers were estimated by a series of neutron and X-ray Rietveld refinements. Calculated powder patterns were derived from the structural data for monoclinic and triclinic C3S, monoclinic C2S, orthorhombic C4AF, cubic C3A and MgO. Neutron diffraction data were collected with the high resolution E9 diffractometer (BENSC) using two different wavelengths, X-ray diffraction data with a high resolution transmission diffractometer. Elemental composition of the samples obtained by ESEM/EDX technique were in a good agreement with the data delivered by the producers. Convergence of the refinements was remarkably different for X-ray and for neutron data. Several refinements were not completed due to numerical instabilities. Neutron refinements were found to be more stable than X-ray, but there was not any notable difference in the final estimated phases’ compositions. Calculated absolute deviates of phases’ weight fractions were mostly within ±10%, which for the less abundant phases corresponded to relative deviations within ±50%. © 2004 International Centre for Diffraction Data.

X-ray powder diffractograms from fcc crystals containing high concentration (more than 1%) of planar defects [deformation stacking faults (SF), double deformation SF, twin boundaries (TB)] have been simulated by Monte Carlo method in kinematic approach. It was shown that the characteristics of powder diffraction peak profiles (except peaks with indexes H00) dependent nonmonotonically on PD concentration, during which peak maximums stay in Bragg positions. An addition point to emphasize is that an appearance of TB only in the crystal not affects on position of all peaks. Several types of PD to be occurred simultaneously in the crystal influence on powder diffractograms additively. Peculiarities of the powder diffraction pattern inherent in different types of PD have been revealed to permit predominant PD type to be found with a high degree of accuracy based on experimental data.

Two-dimensional proportional detectors with their faster data collection, large dynamic range, and more available information than point or linear proportional detectors make them ideal for microdiffraction analysis. The unique capabilities of these detectors coupled with a rotating anode source, capillary optics, and a variety of accessories allow for a wide range of applications.

Indexed X-ray powder diffraction data are reported for the semiconducting compound Ba2Cl2Cu3O4. The structure was refined by the Rietveid technique on the basis of the space group I4/mmm. Refined unit cell dimensions are a = 5.5156(1) Å, c = 13.8221(3) Å, V = 420.49 Å3Dx = 4.74 g/cm3, F30 = 129(0.0075,30), M20 = 121, Rp = 6.58, Rwp = 8.66, and RB = 4.49.

An energy dispersive X-ray fluorescence spectrometer using pulsed X-ray excitation has been developed for use in large-scale environmental analysis programs. A grid controlled X-ray tube is coupled with variable secondary fluorescence targets to analyze for a wide variety of elements with almost optimum sensitivity. The operation of the pulsed tube in a feedback loop with the semiconductor detector spectrometer results in a substantial increase in output counting rates without pile-up. The loop functions by turning off the excitation immediately upon detection of an event by the spectrometer. Pileup events are virtually eliminated and the X-ray tube's available anode power is better utilized.

The electronic control of this feedback mode results in some unique features in the response of the system to varying sample mass. These features are discussed in detail. Experimental results for sensitivity and accuracy over the range of elements measured are presented. Early operating experience with the unit indicates increases of counting rates of a factor of five compared with similar conventional systems.

The spherical wave theory of X-ray Pendellosung fringes in perfect crystals (N. Kato, Acta Cryst, 14: 526, 627, 1961) is extended to the case of crystals including a single stacking fault in an arbitrary way, Kelvin's stationary phase method is used extensively. The stationary phase condition gives us the trajectories of X-ray beams in the crystal. The phase and the amplitude along each trajectory are obtained by straightforward calculation. Based on this crystal wave field, the section patterns in X-ray diffraction topographs are obtained both for the direct and the Braggreflected waves. Characteristic fringe-patterns are expected. Through the image of a fault plane in a single section pattern, the geometrical configuration inside the crystal and the magnitude of the fault vector can be determined. Traverse patterns are also discussed. The fault image based on the plane wave theory (Whelan and Hirsch, Phil. Mag. 2: 1121, 1303, 1957) is also reformulated in the most general Laue case without the use of ad hoc assumptions on the shape of the dispersion surface.

The crystal structure of Tl4V2O7 is solved ab-initio from powder diffraction data collected in Debye-Scherrer geometry using an Inel X-ray Position Sensitive Detector. The structure has been determined from Rietveld analysis in space group ml, Z = 1, with a = 5.9388(2)Å and c = 7.7322(3)Å. The structure of Tl4V2O7 is built up from isolated V2O7 groups aligned along the trigonal c axis. Thallium atoms alternate along a 3-fold axis. The presence of stereochemically active lone pairs is demonstrated and their positions are calculated using a self-consistent electrostatic model. The influence of sample absorption is briefly discussed and the results are compared with those obtained in Bragg-Brentano geometry using flat-plate specimen.

New X-ray powder data for CaWO4 (synthetic scheelite) are presented and compared with the current PDF patterns and with a calculated pattern.

A specimen containing nanograms of sulfur, calcium, and 3d transition metal elements was measured by incident X-ray beams of various sizes restricted by a waveguide placed in a portable TXRF spectrometer. The signal to background ratios of spectra decreased with an increase in incident X-ray beam size. The portable spectrometer was also applied to rainwater and a specimen containing antimony and rare earth elements. Nanograms of elements in these specimens were detected by K-line or L-line excitation.

Solid lipid nanoparticles (SLNs) were characterized by differential scanning calorimetry (DSC) and powder diffraction. The DSC thermograms showed a slight reduction in the melting point of lipid matrix and a broadening of its melting peak, indicating an increased number of lattice defects in SLNs. X-ray powder diffraction data also revealed a slightly broader reflection for SLNs and the presence of X-ray peaks of the all-trans retinoic acid (RA) crystals outside of the lipid matrix of SLNs without stearylamine (STE). These data suggest the presence of an extensive association of ion pairing components (RA and STE), and indicate that the utilization of some specific types of compounds containing amine groups is an interesting approach to improve the encapsulation efficiency of RA in SLNs. The formation of the ion pairing is an interesting alternative for RA encapsulation in SLNs, improving the benefits obtained by the drug incorporation in lipid matrix (increased stability, controlled release, and targeting effect), which are important for the topical treatment of acne.

Laboratory X-ray powder diffraction was used to investigate mineralogical compositions of green pigments labeled by suppliers as “green earths.” It was found that glauconite and celadonite—minerals historically considered as the main ingredient of this pigment—were present only in Bohemian green earth, green earth from Thuringen (glauconite), and Bavarian green earth (celadonite). Other investigated pigments consist of mineralogical-component minerals with added synthetic organic colorants. The obtained results may be useful for scientists, restorers, and artists in proper choices of the pigments they use in their works.

The crystal structure of trandolapril has been solved by parallel tempering using the FOX software package with laboratory powder diffraction data submitted to and published in the Powder Diffraction File. Rietveld refinement was performed with the software package GSAS yielding orthorhombic lattice parameters of a = 19.7685(4), b = 15.0697(4), and c = 7.6704(2) Å (C24H34N2O5, Z = 4, space group P212121). The Rietveld refinement results were compared with density functional theory (DFT) calculations performed with CRYSTAL14. While the structures are similar, discrepancies are observed in the configuration of the octahydroindole ring between the Rietveld and DFT structures, suggesting the refined and calculated molecules are diastereomers.

Quantitative analysis by x-ray fluorescence and photoelectron and Auger electron analysis can be effectively extended through a precise knowledge of the total aad subshell photoionization cross sections. Light element and intermediate element analysis, as based upon K and L series fluorescence respectively, involve x-ray interactions in the low energy region, Optimized analysis for essentially all the elements by x-ray induced photoelectron and Auger electron spectroscopy involves both x-ray and electron interactions in the low energy region. Unfortunately, theory and measurement for interaction cross sections in this 100-1500 eV region are difficult, particularly for the heavier elements. Nevertheless, recent advances in experimental and computerized-theoretical techniques for the determination of low energy interaction coefficients do permit establishing appreciatly more complete tabulations of cross sections than are currently available in this energy region.

In this paper, the types of interaction cross section data that are needed for quantitative x-ray and electron analysis are defined. Such data that are available from experiment and from theory are reviewed and compared. Some newer techniques for the measurement of cross sections are discussed. And finally, new “state of the art” tables are presented for the mass absorption coefficients of all of the elements and of some special laboratory materials. These are tabulated specifically for twenty-six of the most commonly applied characteristic wavelengths in the 8-110 A region and are based upon the best currently available theoretical and experimental data.