X-ray powder diffraction data, unit-cell parameters, and space group for potassium erbium fluoride, K0.5Er0.5F2, are reported [a = 5.6862(5) Å, unit-cell volume V = 183.85 Å3, Z = 4, and space group Fm-3m]. Potassium erbium fluoride is isostructural with a large family of fluorides represented by the mineral fluorite CaF2. All of the measured lines of the title compound were indexed and are consistent with the Fm-3m space group. No detectable impurities were observed.

The X-ray micro-diffraction laboratory technique was applied to study the quantitative changes of austenite content in TRIP steels after deformation and to reveal the phase composition of precipitates in an inner part of a hearth of a blast furnace. The usefulness of this technique was shown by calculating the austenite content after tensile test in three different parts of a small tensile test sample and after a clinching test in two areas of a clinching joint. The calculations showed the decrease in austenite content in deformed parts in comparison to not deformed areas. The presence of various kinds of chlorides, including the iron oxide chloride hydroxide in a sample taken from a graphite refractory lining of blast furnace, was confirmed by micro-diffraction patterns.

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.

Fusion bead method produces homogeneous samples and is suitable for analysis using fundamental-parameter (FP) method in XRF. This report describes an FP method for analysis of non-oxide samples such as metals made into fusion beads. During the fusion process, all non-oxide elements in the sample are oxidized and gain-on-ignition (GOI) occurs. Volatile elements such as carbon do not remain in the sample as a result of fusion. This process is known as loss-on-ignition (LOI). To obtain reliable analysis results of fusion beads with the FP method, weight changes as a result of LOI and GOI must be reflected accurately in software calculation. The newly developed FP method, which takes these weight changes and dilution ratios into consideration, was able to yield accurate analysis results for ferroalloys FeSi, FeMn, and SiMn, some of which have high carbon content. This method is also applicable for sulfides and carbides.

The 2,4-diaryl 1,2,3,4-tetrahydroquinoline derivative (1), described in the title (Chemical formula: C23H22N2O3), was synthesized via the “one-pot” three-component imino Diels–Alder reaction catalyzed by Cu(OTf)2. Molecular characterization was performed by 1H and 13C NMR, Fourier transform-infrared, and gas chromatography-mass spectrometry. The X-ray powder diffraction pattern for the title compound was analyzed and found to be crystallized in an orthorhombic system with space group P212121 (No. 19) and refined unit-cell parameters a = 8.6415(8) Å, b = 12.679(2) Å, c = 17.601(2) Å, and V = 1928.4(2) Å3.

Semifluorinated (SF) side chain polymers show phase separation between polymer backbone and SF side chains. Due to strong interaction between SF segments the side chains determine the structure behaviour strongly, often resulting in layered structures in which backbones and layers of SF side chains alternate. The interest in this work was directed to find out the dependence of these structures on concentration of SF side chains. Thin films of random copolymers consisting of methylmethacrylate (MMA) and semifluorinated side chain methacrylate (SFMA) segments and with different fluorine content in the perfluoroalkyl side chains (abbreviated as H10F10 and H2F8) were prepared by spin-coating. Phase separation and structure changes were initiated by external subsequent annealing. Corresponding bulk material served as basic information. Generation of ordered structures and variation of film parameters were observed using different X-ray scattering methods (XRR, GIWAXS, and GISAXS). The phase behaviour in bulk is governed by the SF side chain amount and their specific fluorine content which control the self-organization tendency of SF side chains. Additionally, the confinement in thin films generates an orientation of side chains normally to film surface.

X-ray powder diffraction data, unit-cell parameters and space group for peiminine, C27H43NO3, are reported (a = 30.2026 Å, b = 5.8468 Å, c = 14.4344 Å, β = 96.9456°, unit-cell volume V = 2530.23 Å3, Z = 2 and space group P21). All measured lines were indexed and are consistent with the P21 space group. No detectable impurity was observed.

Nanocrystalline anatase powders synthesised by various chemical processes as super/subcritical fluid extraction, sol-gel technique and hydrolysis of titanium alkoxides in hydrogen peroxide were studied by X-ray diffraction (XRD) whole profile modelling method (WPPM) in order to reveal correlations between structural and micro-structural parameters as well as sample treatment conditions. Anisotropy of the diffraction line broadening due to truncated bipyramidal shape of anatase crystals was discussed. The hkl-anisotropy can be very strong but also almost negligible in dependence on relative ratio of the crystallite dimensions. The latter was the case for the studied samples. The size of synthesised anatase nanoparticles was within the range 3–25 nm. The theoretical total surface area of crystallites calculated from XRD was in a good correlation with the surface area measured by the nitrogen physisorption up to the temperature 400–450 °C, when the particles started to agglomerate. At atomic scale a unit cell volume contraction with decreasing crystallite size and a significant deficiency in the Ti-site occupancy was observed. Both effects were attributed to the presence of Ti-vacancies and a linear coefficient between the relative cell volume contraction and the fraction of Ti-vacancies was estimated to (–0.017 ± 0.003).

Atomistic copper nanocrystals were investigated via Molecular Dynamics (MD) under hydrostatic pressure to probe the relationship between applied load and structure deformation. The corresponding X-ray powder diffraction patterns were generated from the atomic coordinates. The analysis followed both the traditional Williamson-Hall approach based on pseudo-Voigt fitting and an alternative, more accurate method able to derive the integral breadths without applying a fitting. The Williamson-Hall results show discrepancies not fully associated with an issue of fitting.

The 4-benzyloxy-1-oxaspiro-[4.6]-undec-3-en-2-one (C17H20O3) was prepared through a domino reaction from benzyl α-hydroxycycloheptanecarboxylate and the cumulated ylide Ph3P=C=C=O by: (i) addition and (ii) intramolecular Wittig Olefination reaction. The reaction was carried out using anhydrous toluene as solvent under an argon atmosphere in a Schlenk flask. Molecular characterization was performed by Fourier transform infrared spectroscopy, gas chromatography-mass spectrometry, (1H,13C – mono and bidimensional) nuclear magnetic resonance spectroscopy; crystallographic characterization was completed by X-ray diffraction of polycrystalline samples (XRPD). The title compound crystallized in a monoclinical system and unit-cell parameters are reported [a = 13.207(3) Å, b = 5.972(1) Å, c = 19.719(4) Å, β = 105.67(2)°, unit-cell volume V = 1497.5 (4) Å3, Z = 4]. All of the measured lines were indexed with the P21/n (No. 14) space group.

Calcium hydroxyl and fluoroapatite (CaHAp and CaFAp) were prepared in the presence of the 2-carboxyletylphosphonic acid (2-CEPA), by hydrothermal method. The incorporation of phosphonic acid within the apatite structure was confirmed by powder XRD, IR and MAS-NMR spectroscopies and SSA. The X-ray powder analysis showed that the cristallinity was not affected by the presence of organic moieties. IR spectroscopy showed new vibration modes related to phosphonate groups. 31P MAS-NMR spectra exhibit new signals, assigned to the presence of organic phosphorus. Specific surface area (SSA) increases with increasing of phosphonate amount, especially for CaHAp. According to these results, a mechanism is proposed for the formation of two types of ionic interaction (-C-O-Ca) and (Ca-O-Porg).