X-ray reflectometry is a powerful tool for investigating rough surface and interface structures. Presently, X-ray reflectivity is based on Parratt formalism, accounting for the effect of roughness by the theory of Nevot–Croce. However, the calculated results showed a strange phenomenon in that the amplitude of the oscillation because of interference effects increases in the case of a specific roughness of the surface. We propose that the strange results originated from the currently used equation because of a serious error in which the Fresnel transmission coefficient in the reflectivity equation is increased at a rough interface, and the increase in the transmission coefficient completely overpowers any decrease in the value of the reflection coefficient because of lack of consideration in diffuse scattering. In the present study, we present a new improved formalism that corrects this error, and thereby derives an accurate analysis of X-ray reflectivity from a multilayer surface, taking into account the effect of roughness-induced diffuse scattering.

A new Matlab-based software suite called Tilt-A-Whirl has been applied to XRD data from textured gold films electro-deposited onto nickel substrates. The software routines facilitate phase identification, texture analysis via pole figure visualization, and macrostrain determination. The use of principal component analysis with multivariate curve resolution (PCA/MCR) revealed the extraction of texture components. The unusual hardness properties of one Au film (deposited from a 30% gold depleted BDT-200 bath) were found to be dependent on the (210) out-of-plane preferred orientation of the polycrystalline gold film. The progressive nucleation of Au crystallites during electro-plating has been tied to improved hardness properties of this film.

Clenbuterol hydrochloride is an active pharmaceutical ingredient usually prescribed for treatment of respiratory diseases due to its activity as a decongestant and bronchodilator. It has also been used as a performance-enhancing drug. In the PDF-4/Organics 2012 database there are six entries related to this compound: three for its hydrochloride phase calculated using single-crystal data, two for a MeOH and a DMSO solvate of two Cu-clenbuterol complexes, and one experimental unindexed pattern. In this contribution the powder diffraction pattern and the crystal structure, determined using single crystal X-ray diffraction techniques of clenbuterol hemihydrate, C12H18Cl2N2O·0.5H2O, an unreported phase, are presented.

A new methodology based on maximum likelihood estimation for structure refinement using powder diffraction data is proposed. The method can not only optimize the parameters adjusted in Rietveld refinement but also parameters to specify errors in a model for statistical properties of the observed intensity. The results of structure refinements with relation to fluorapatite Ca5(PO4)3F, anglesite PbSO4, and barite BaSO4 are demonstrated. The structure parameters of fluorapatite and barite optimized by the new method are closer to single-crystal data than those optimized by the Rietveld method, while the structure parameters of anglesite, whose values optimized by the Rietveld method are already in good agreement with the single-crystal data, are almost unchanged by the application of the new method.

Recently, a new experimental setup for quick X-ray reflectivity (q-XRR) measurements was proposed, which is based on simultaneous recording of an X-ray reflectivity curve over all angles of interest. This new setup for q-XRR allows measurements to be done within seconds, thus permitting studies of the time evolution of chemical, thermal, and mechanical changes at the surfaces and interfaces of different materials. Since the q-XRR measurement setup utilizes an extended X-ray source and detector, it is important to develop models and to account for the following two effects: (i) diffuse scattering associated with different points of the source and (ii) sample curvature. Models accounting for both effects are presented, and their influences on interpretation of the q-XRR measurement results are discussed.

X-ray powder diffraction data, unit-cell parameters, and space group for deoxyschisandrin, C24H32O6, are reported [a = 13.083(3) Å, b = 19.563(9) Å, c = 8.805(6) Å, β = 90.472(0)°, unit-cell volume V = 2253.82 Å3, Z = 4, and space group P21]. All measured lines were indexed and are consistent with the P21 space group. No detectable impurity was observed.

A novel concept of immobilization of light water nuclear reactor fuel reprocessing waste effluent through interaction with sodium zirconium phosphate (NZP) has been established. It was found that a large number of hazardous cations could be loaded in the NZP-based matrix without significant change of three-dimensional framework structure. Starting from the raw powder diffraction data of polycrystalline solid phases, crystal structure of substituted NZP phases has been investigated using the General Structure Analysis System (GSAS) package. Cation(s) substituted NZP phases crystallize in rhombohedral symmetry (space group R-3c and Z = 6). Powder diffraction data have been subjected to Rietveld refinement to reach satisfactory structural convergence of R-factors. Unit cell parameters, inter atomic distances, bond angles, reflecting planes (h, k, l), structure factors, polyhedral (ZrO6 and PO4) distortion, and particle size have been reported. PO4 stretching and bending vibrations in the Infra red (IR) region have been assigned. SEM and EDAX analysis provide analytical evidence of fixation of cations in the matrix.

A number of spatially resolved elemental imaging techniques are commonly employed to examine plutonium and other nuclear materials (e.g., scanning electron microscopy). Up until the past 10–15 years, micro-X-ray fluorescence (MXRF) instrumentation had been relatively uncommon, and even currently, it is underutilized for spatially resolved nuclear materials analysis and imaging. In the current study, a number of plutonium materials problem solving applications are presented to demonstrate the power and utility of MXRF for providing unique, spatially resolved elemental composition information. Applications discussed include identification of multiple insoluble fractions in plutonium and neptunium mixed oxide, spatially resolved imaging of plutonium residue and other elements on surface swipes, and spatial mapping of impurities in plutonium metal. The mixed oxide particle analysis demonstrated the ability to non-destructively identify particles of interest for potential extraction and analysis by other methods. The surface swipes study demonstrated the unique ability of MXRF to non-destructively image large multiple cm2 sized, non-conducting, radiologically contaminated samples. The plutonium metal investigation showed the capability of MXRF to non-destructively map elemental heterogeneity directly in an actinide matrix. Such information is extremely valuable prior to using destructive analysis (DA) trace elemental analytical chemistry techniques. If a metal is found to contain significant elemental impurity heterogeneity by MXRF, time consuming destructive sample preparation and analysis do not need to be repeated to confirm that the sample is indeed heterogeneous.

In an effort to study an alternative approach to make graphene from graphene oxide (GO), exposure of GO to high-energy X-ray radiation has been performed. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM) have been used to characterize GO before and after irradiation. Results indicate that GO exposed to high-energy radiation is converted to an amorphous carbon phase that is conductive.

X-ray powder diffraction data, unit-cell parameters, and space group for inclusion complex of β-cyclodextrin with fraxinellone, C42H70O35·C14H16O3·3H2O, are reported [a = 19.294(2) Å, b = 26.639(1) Å, c = 16.467(3) Å, β = 110.451(9)°, cell volume V = 7930.34 Å3, Z = 4 and space group C2]. All measured lines were indexed and are consistent with the C2 space group. No detectable impurities were observed.