The aim of this work was to compare different excitation modes for the analysis of light elements from carbon (Z = 6) upwards using a total reflection X-ray fluorescence analysis (TXRF) vacuum chamber which allows the attachment of different X-ray tubes and detectors. In the first set of experiments, two water-cooled high-power X-ray tubes with Cr (Z = 25) and Cu (Z = 29) anodes, respectively, were compared with an air-cooled low-power tube with Mo anode (Z = 42) and a thin Be window for the transmission of Mo-L lines. In the first two cases, monochromatic Kα radiation was used for excitation, while in the case of the Mo tube the multilayer acted as a cut-off reflector and part of the Mo bremsstrahlung continuum together with the Mo-L series were used for excitation. Multi-element standards containing elements ranging from Na (Z = 11) to Ti (Z = 22) were analyzed by a silicon drift detector (SDD) with a 300 nm ultrathin polymer window (UTW). Detection limits were calculated and compared for the three excitation modes. The second set of experiments was performed using an air-cooled low-power X-ray tube with Rh anode (Z = 45) in order to show that a conventional SDD with a 25 μm beryllium window can be used for the detection of elements from Na upwards. The use of compact air-cooled low-power X-ray tubes together with Peltier-cooled SDDs with UTW should lead to the development of highly sensitive tabletop vacuum TXRF spectrometers with a design optimized for the analysis of light elements. Detection limits as achieved by vacuum chambers using conventional water-cooled high-power tubes (e.g. Streli et al., 2004) are realistically achievable with the new approach.

The quantification of stress in polycrystalline materials by diffraction-based methods relies on the proper choice of grain interaction model that links the observed strain to the elastic stress state in the aggregate. X-ray elastic constants (XEC) relate the strain as measured using X-rays to the state of stress in a quasi-isotropic ensemble of grains. However, the corresponding interaction models (e.g., Voigt and Reuss limits) often possess unlikely assumptions as to mechanical response of the individual grains. The Kröner limit, which employs a self-consistent scheme based on the Eshelby inclusion method, is based on a more physical representation of isotropic grain interaction. For polycrystalline aggregates composed of crystals with cubic symmetry, Kröner limit XEC are equal to those calculated from a linear combination of Reuss and Voigt XEC, where the weighting fraction, x Kr, is solely a function of the single-crystal elastic constants and scales with the material's elastic anisotropy. This weighting fraction can also be experimentally determined using a linear, least-squares regression of diffraction data from multiple reflections. Data on metallic thin films reveals that this optimal experimental weighting fraction, x*, can vary significantly from x Kr, as well as that of the Neerfeld limit (x = 0.5).

Electron backscatter diffraction (EBSD) is a micro-analytical technique typically attached to a scanning electron microscope (SEM). The vast majority of EBSD measurements is applied to planar and polished surfaces of polycrystalline bulk specimen. In this paper, we present examples of using EBSD and energy-dispersive X-ray spectroscopy (EDX) to analyze specimens that are not flat, not planar, or not bulk – but pillars, needles, and rods. The benefits of low vacuum SEM operation to reduced drift problems are displayed. It is further demonstrated that small and thin specimens enhance the attainable spatial resolution for orientation mapping (by EBSD or transmission Kikuchi diffraction) as well as for element mapping (by EDX).

X-ray fluorescence (XRF) is a well-established method for quantitative elemental analysis. For accurate quantification, secondary excitation has to be taken into account. In this paper, the secondary excitation process was discussed for analysis by confocal micro-XRF. Experimental depth profiles were shown for a layered sample of Co and Cu. An additional peak was observed in the depth profile of Co, and it was explained by secondary excitation process. Additionally, a Mosaic model was proposed for quantification of confocal micro- XRF analysis.

The authors present and discuss a method for simultaneous quantitative analysis of total loss on ignition (LOI) (CO2 + H2O) and CO2 content separate from the LOI, in an industrial environment of quicklime production. Total LOI is determined by the Compton scattered RhKα tube radiation which is used directly in the calibration equation. The resulting calibration curve for LOI, including matrix correction shows an accuracy of 0.15 mass%. The carbon content (CO2) is distinguished from total LOI by measuring CKα radiation, which is possible with the required accuracy by employing a new multilayer analyzer with greatly improved background characteristics. The method aims at high reliability and sample throughput and at becoming a less time-consuming alternative to the conventional method of LOI determination by weighing sequences before and after “ignition” at 1050 °C.

In this work, we present a systematic study on the solid solution, lattice parameters and superconductivity on the Fey Te1−x X x (X = Se, S) system. It has been found that the limit of the Te-site doping with Se and S is around 0.5 and 0.15, respectively. The solid solution with the Fe content changing is also measured in this work, and the single-phase region for preparing pure sample is presented. Based on the magnetic susceptibility measurements, we presented a three-dimensional graph for showing the variation of superconducting critical temperature as a function of both the chalcogen and Fe content in Fey Te1−x X x .

A first attempt to differentiate goethite- and hematite-based natural materials, used for several purposes during the Late Palaeolithic in the Lessini Mountains (Italy), is here proposed. All raw materials were collected from known geological sites within a distance of about 20 km from archaeological excavations (Tagliente and Fumane caves) where ochre fragments were found. X-ray powder diffraction allowed the mineralogical composition of samples collected from carbonate and volcanic geological host and parent rocks to be inferred; in addition, a preliminary distinction based on the different mineral assemblages, on the presence of distinctive mineral phases and on the degree of crystallinity of some compounds such as hematite, became possible. The acquired data thus represent a sort of preliminary inventory for provenance studies on archaeological samples originating in the same region, for which ancillary micro-analytical and geochemical techniques are planned.

The structure of Cs2AlF5 obtained by thermal dehydration of Cs2AlF5•H2O is determined ab initio from powder diffraction data, space group Pmn21, a = 6.36216 (17) Å, b = 12.7523 (4) Å, c = 11.4102 (3) Å, and Z = 6. Contrarily to most A2MF5 compounds presenting MF5cis or trans-chains of corner-sharing MF6 octahedra, Cs2AlF5 is characterized by the rare occurrence of the face-sharing anion Al2F93− combined with an isolated AlF63− octahedron, the sum leading to Al3F156−. The structure of Cs3Al2F9 [space group P63/mmc, a = 6.2535 (2) Å, c = 14.7193 (6) Å, Z = 2] is confirmed to be isostructural with Cs3Fe2F9, built up from the same M2F93− dimers (M = Fe, Al). Both crystal structures are optimized by energy minimization density funtional theory (DFT) in the solid state using a hybrid PBE0 functional, and their relations with the hexagonal perovskites and elpasolites are discussed.

X-ray structural characterization and X-ray reference powder patterns have been determined for two series of iron- and cobalt-containing layered compounds (Bax Sr1− x )2Co2Fe12O22 (x = 0.2, 0.4, 0.6, 0.8) and (Bax Sr1− x )Co2Fe16O27 (x = 0.2, 0.4, 0.6, 0.8). The (Bax Sr1− x )2Co2Fe12O22 series of compounds crystallized in the space group R $\bar 3$ m (No. 166), with Z = 3. The structure is essentially that of the Y-type hexagonal ferrite, BaM 2+Fe6 3+O11. The lattice parameters range from a = 5.859 15(8) to 5.843 72(8) Å, and c = 43.4975(9) to 43.3516(9) Å for x = 0.2 to 0.8, respectively. The (Bax Sr1− x )Co2Fe16O27 series (W-type hexagonal ferrite) crystallized in the space group P63/mmc (No. 194) and Z = 2. The lattice parameters range from a = 5.902 05(12) to 5.8979(2) Å and c = 32.9002(10) to 32.8110(13) Å for x = 0.2 to 0.8. Results of measurements of the Seebeck coefficient and resistivity of these two sets of samples indicated that they are insulators. Powder X-ray diffraction patterns of these two series of compounds have been submitted to be included in the Powder Diffraction File.

Several hitherto unknown hydrates of magnesium selenate have been formed by quenching aqueous solutions of MgSeO4 in liquid nitrogen. MgSeO4·11H2O is apparently isostructural with the mineral meridianiite (MgSO4·11H2O), being triclinic, $P{\rm \bar 1}$, Z = 2, with unit-cell parameters a = 6.779 00(8) Å, b = 6.965 16(9) Å, c = 17.4934(2) Å, α = 87.713(1)°, β = 89.222(1)°, γ = 63.121(1)°, and V = 736.15(1) Å3 at −25 °C. MgSeO4·9H2O represents a new hydration state in the MgSeO4–H2O system; it is monoclinic, space-group P21/c, Z = 4, with unit-cell parameters a = 7.270 24(6) Å, b = 10.510 94(9) Å, c = 17.4030(2) Å, β = 109.447(1)°, and V = 1254.02(1) Å3 at −22 °C. The heavy-atom structure of MgSeO4·9H2O has been determined by direct-space methods from X-ray powder diffraction data and consists of isolated Mg(H2O)62+ octahedra and SeO42− tetrahedra linked by hydrogen bonds. The remaining three water molecules occupy the space between the polyhedral ions, contributing to the H-bonded network, which comprises 4-, 5-, and 6-membered rings. A third phase has been observed to crystallise prior to the 11-hydrate upon warming of liquid-nitrogen-quenched glass, but this transforms rapidly to the meridianiite-structured 11-hydrate and the identity of this phase is unclear.

The crystal structure of levalbuterol hydrochloride polymorph A has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Levalbuterol hydrochloride polymorph A crystallizes in space group P21 (#4) with a = 8.499 352(15), b = 6.511 726(13), c = 13.182 256(25) Å, β = 102.1157(2)°, V = 713.327(2) Å3, and Z = 2. The most prominent feature of the structure is the two different sorts of hydrogen bonds. Both of the ammonium hydrogens and O17–H40 act as donors to Cl18. The graph sets are C1,2(4) and C1,2(7). The result is a zig-zag chain parallel to the b-axis. The two hydroxy groups at the phenyl end of the molecule form another set of chains, both with graph set C1,1(6), also resulting in a chain parallel to the b-axis. The bulk of the molecule connects these chains in the (101) plane to form a three-dimensional network. The powder pattern is included in the Powder Diffraction File™ as entry 00-064-1494.

The salt [NH3(CH2)2SS(CH2)2NH3][CuCl4] was obtained by crystallization after adding CuCl2 to cystamine (Cysta), solved in hydrochloric acid. The assumption of conserved disulfide connection (S–S) in the compound, made on the basis of infrared spectroscopy, is further supported by the crystal structure determined from X-ray powder diffraction data. The compound has an ionic structure. [CuCl4]2− and CystaH22+ ions package in the form of inorganic and organic layers in the cell, interconnected through the formation of hydrogen bonds via NH3-groups and chlorine atoms of the complex [CuCl4]2−. Inorganic layers are additionally stabilized in the parquet package of [CuCl4]2− ions which provides a Cu-distorted octahedral coordination. CystaH2[CuCl4] is stable in air up to 200 °C. Thermal decomposition occurs in several stages, accompanied by breaking of S–S bonds, releasing of the organic component and yielding CuO.

The crystal structure of rilpivirine has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Rilpivirine crystallizes in space group P21/c (#14) with a = 8.39049(3), b = 13.89687(4), c = 16.03960(6) Å, β = 90.9344(3)°, V = 1869.995(11) Å3, and Z = 4. The most prominent features of the structure are N–H···N hydrogen bonds. These form a R2,2(8) pattern which, along with C1,1(12) and longer chains, yield a three-dimensional hydrogen bond network. The powder pattern has been submitted to International Centre for Diffraction Data, ICDD, for inclusion in future releases of the Powder Diffraction File™.

X-ray powder diffraction data, unit-cell parameters, and space group for beta-methyl vinyl phosphate (MAP), C29H27N2O10P, are reported [a = 17.293(4) Å, b = 6.142(6) Å, c = 14.464(8) Å, α = γ = 90°, β = 112.048(0)°, unit-cell volume V = 1424.19 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.

X-ray powder diffraction data, unit cell parameters, and space group for 1-methylhydantoin, C4H6N2O2, are reported [a = 5.6070(9) Å, b = 12.170(1) Å, c = 8.097(1) Å, β = 105.41(1), Z = 4, unit cell volume V = 532.66(9) Å3, with M20 = 50.2 and F30 = 62.2 (0.0082, 59)]. All measured lines were indexed and are consistent with the monoclinic P21/c space group.

X-ray powder diffraction data, unit cell parameters, and space group for a new organometallic compound, lanthanum trilactate trihydrate, LaC9H21O12, are reported [a = 9.986(1) Å, b = 9.158(1) Å, c = 11.200(1) Å, α = 115.08(1), β = 117.41(1), γ = 88.61(1), unit cell volume V = 804.70 Å3, Z = 2 and space group P1]. All measured lines were indexed. No detectable impurity was observed.

X-ray powder diffraction data, unit-cell parameters, and space group for calcium(II)–naproxen complex, C28H26CaO6·2H2O, are reported [a = 36.918(2) Å, b = 5.655(6) Å, c = 12.505(6) Å, β = 91.263(2)°, cell volume V = 2610.47 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.