Lead poisoning is a preventable condition caused by exposure to environmental sources such as lead-containing dust or lead-painted consumer products. The history of lead poisoning prevention has been defined to some extent by the quality of the analytical methods available for lead measurements whether in environmental samples or biological tissues and fluids. The quality of blood lead methods has improved so greatly over the last three decades that we now know far more about the adverse health effects from low-level exposures. Recent evidence suggests that effects such as deficit in IQ occur below the current (periodically revised) U.S. CDC threshold of 10 μg/dL, such that no safe threshold appears to exist for children. Improvements in analytical techniques have also had an impact on the environmental measurement quality, yet many environmental thresholds have remained unchanged for decades. In light of our current understanding of the adverse health effects at low levels of exposure, new thresholds for lead in children’s products have been introduced by the U.S. CPSC. The adequacy of current analytical techniques to detect lead accurately at the new, lower thresholds is questionable. XRF offers the advantage of being rapid and nondestructive compared to techniques such as AAS that require extensive sample preparation. However, the accuracy of handheld XRF determinations of lead in painted toys is generally limited. A brief comparative study on the performance of several analytical techniques for the determination of lead in toys is presented at the end of this paper.

An electron probe X-ray microanalysis (EPMA) technique using an energy-dispersive X-ray detector with an ultrathin window, designated low-Z particle EPM, has been developed. The low-Z particle EPMA allows the quantitative determination of concentrations of low-Z elements, such as C, N, and O, as well as higher-Z elements that can be analyzed by conventional energy-dispersive EPMA. The quantitative determination of low-Z elements (using full Monte Carlo simulations, from the electron impact to the X-ray detection) in individual environmental particles has improved the applicability of single-particle analysis, especially in atmospheric environmental aerosol research; many environmentally important atmospheric particles, e.g. sulfates, nitrates, ammonium, and carbonaceous particles, contain low-Z elements. The low-Z particle EPMA was applied to characterize loess soil particle samples of which the chemical compositions are well defined by the use of various bulk analytical methods. Chemical compositions of the loess samples obtained from the low-Z particle EPMA turn out to be close to those from bulk analyses. In addition, it is demonstrated that the technique can also be used to assess the heterogeneity of individual particles.

The cubic Al18Ti2Mg3 phase (184 atoms/unit cell, Z = 8, space group Fdm) has been fabricated by reaction hot isostatic pressing. Quantitative energy dispersive X-ray analysis showed the phase to have nearly ideal stoichiometry. Interplanar spacings and diffraction peak intensities have been determined by X-ray diffraction. The experimental data show good agreement with the pattern calculated using atomic site positional parameters for A118Cr2Mg3, confirming that A118Cr2Mg3 is the prototype for A118Ti2Mg3.

We present a detailed description of the SESAME Materials Science (MS) beamline for X-ray diffraction (XRD) applications, presently under construction in Allan, Jordan. The beamline is based on components previously installed at the Swiss Light Source, but modifications in the beamline design have been introduced to match the characteristics of the SESAME storage ring. The SESAME MS beamline will accommodate XRD experiments in the energy range between 5 and 25 keV. The beamline ray tracing analysis at 10 keV estimates the flux at the sample to be of the order of 1013 (photons s−1), the energy resolution is about 2 eV and the effective beam size at the sample of 300 × 2800 µm2. Investigations of microstruture will be possible as the instrumental broadening, resulted from simulating the diffraction pattern for a standard material, is of the order of 0.01° at 15 keV. A wide range of applications will be possible at the beamline, such as powder diffraction studies, single crystals and in situ XRD. The commisioning of the beamline is expected to be in the second half of 2017.

Two-dimensional X-ray diffraction (XRD2) pattern can be described by the diffraction intensity distribution in both 2θ and γ-directions. The XRD2 images can be reduced to two kinds of profiles: 2θ-profile and γ-profile. The 2θ-profile can be evaluated for phase identification, crystal structure refinement, and many applications with many existing algorithms and software. In order to evaluate the materials structure associated with the intensity distribution along γ-angle, either the XRD2 pattern should be directly analyzed or the γ-profile can be generated by 2θ-integration. A γ-profile contains information on texture, stress, crystal size, and crystal orientation relations. This paper introduces the concept and fundamental algorithms for stress, texture, and crystal size analysis by the γ-profile analysis.

The thermal decomposition of mill scale, and the effect of mill scale addition on the formation and decomposition of Silico-Ferrite of Calcium and Aluminium (SFCA) and SFCA-I iron ore sinter bonding phases, has been investigated using in situ X-ray diffraction. Application of the external standard method of quantitative phase analysis of the in situ data collected during decomposition of the mill scale highlighted the applicability of this method for the determination of the nature and abundance of amorphous material in a mineral sample. Increasing mill scale addition from 2.6 to 10.6 and to 21.2 wt% in an otherwise synthetic sinter mixture composition designed to form SFCA did not significantly affect the thermal stability ranges of SFCA-I or SFCA, nor did it significantly affect the amount of each of SFCA or SFCA-I, which formed. This was attributed to the low impurity (i.e. Mn, Mg) concentration in the mill scale, and also the transformation to hematite during heating of the wüstite and magnetite present in the mill scale, with the hematite available for reaction to form SFCA and SFCA-I.

Synchrotron powder diffraction data have been obtained and indexed for ferrous gluconate, a common supplement used for the treatment and prevention of iron-deficiency anemia. Ferrous gluconate (Fe(C6H11O7)2 · x H2O, Z = 4) crystallizes in a monoclinic cell (space group I2, #5) with lattice parameters a = 19.953 16(9) Å, b = 5.513 92(3) Å, c = 18.470 58(9) Å, and β = 111.3826(3)°. The pattern shows no evidence of impurity reflections.

The engineering of strained semiconductor materials represents an important aspect of the enhancement in CMOS device performance required for current and future generations of microelectronic technology. An understanding of the mechanical response of the Si channel regions and their environment is key to the prediction and design of device operation. Because of the complexity of the composite geometries associated with microelectronic circuitry, in situ characterization at a submicron resolution is necessary to verify the predicted strain distributions. Of the measurement techniques commonly used for strain characterization, synchrotron-based X-ray microbeam diffraction represents the best nondestructive method to provide spatially resolved information. The mapping of strain distributions in silicon-on-insulator (SOI) features induced by overlying silicon nitride structures and embedded heteroepitaxial features adjacent to SOI device channels are presented. The interaction regions of the SOI strain were observed to extend large distances from the SOI/stressor interfaces leading to significant overlap in the strain distributions at technically relevant dimensions. Experimental data were also compared to several mechanical models to assess their validity in predicting these strain distributions.

A relationship is derived between X-ray intensity and particle size for a minor constituent in a powder sample. Theoretical and experimental curves are compared for several elements which are of importance in mining applications. Based upon these curves, some general guides are established relating to a method of predicting the particle size required for a given application. It is also shown that the relative intensity of a minor constituent is independent of the absorption coefficient of the matrix, if the particle size of the matrix is constant. Mineralogical effects, which relate to the occurrence of an element in two or more forms of chemical combination, are discussed and several examples in mining applications are cited.

Powder X-ray diffraction (XRD) data were collected for a new phase of SrGd2O4. Analysis using the Rietveld method was carried out and it was found that the sample crystallizes in the orthorhombic symmetry with CaFe2O4 related structure. The lattice parameters are found to be a=12.0521(2) Å, b=10.1327(2) Å, c=3.4757(4) Å and Z=4. For X-ray data RF=4.9%, RB=7.6%, RP=8.1% and χ2=1.51. The structure can be described as an assembly of bioctahedron [Gd2O10] which are linked together by O2− anions and of dodecahedron of SrO8.

Dental amalgam has been used as a filling material in dentistry for over 100 years. The reactants, Ag3Sn alloy and mercury, form silver-mercury and tin-mercury products. Previous X-ray diffraction studies have resulted in some disagreement concerning unit-cell structure and parameters of the products. In this study, X-ray diffraction measurements were carried out on tin-mercury mixtures, tin-mercury alloys, dental amalgam, and single crystals of tin and mercury. The diffraction data for the tin-mercury alloys were programed for an IBM 650 computer utilizing Cohen's least-squares method. The tin-mercury product was found to be a solid solution possessing hexagonal-symmetry elements. The parameters ranged from: c0 = 2.995 A to 2.984 A, co/ao = 0.931.

The state of the art of stress evaluation on materials having non-linear lattice strain distributions is presented.

New results on heterogeneous materials with measurements conducted on both phases of the material show compensation of the shear stress components σ13 in ground surface layers of (α+β) brass. There is only the compensation of normal components σ11 of (α+γ) steel after plastic straining.

The fundamental aspects and the evaluation of macro- and microresidual stresses on materials having preferred orientation are broadened. The use of Mo-Ka-radiation shows linear lattice strain distributions, as a result of minimizing the influence of micro residual stresses causing oscillations. The interplanar distance- or strain-polefigure shows similarities with the intensity polefigure.

The knowledge of the theoretical influence of stress distribution with depth from the surface of the material is extended. The experimental procedure should use either different radiations having different penetration depths or a low-penetrating radiation in combination with removal of surface layers.

Afghanite is a feldspathoid of the cancrinite-group: It is hexagonal, space group P63mc. The afghanite sample was found in the M. Somma-Vesuvio volcanic complex (Italy) and was previously described as davyne: Calculated cell parameters are a = 12.7997(4) Å, c = 21.4062(11) Å; the volume is 3037.2(2) Å3. The strongest lines are: 3.694(100), 3.647(56), 4.826(30), 2.678(25), 2.134(18), 3.999(12), 2.750(12), and 2.771(10). The new data provide quantitative measurement of intensities, an increased number of indexed peaks, and a different empirical formula with respect to the PDF 20-1086.

Two ternary phases, designated τ4 and τ5, were revealed in Al–Ti–Pt. The τ4-phase with equiatomic composition (i.e., AlTiPt) was found to have a hexagonal structure with a=4.3908(9) Å and c=5.4823(10) Å (space group P63/mmc), and the τ5-phase, forming in a compositional range between ∼Al14Ti58Pt28 and Al21Ti63Pt16, has a tetragonal structure (possible space groups P42nm, P-4n2, and P42/mnm). The refined lattice parameters for Al15Ti60Pt25 are a=9.7019(20) Å and c=5.0231(13)Å.

X-ray powder diffraction data collected in transmission and high-throughput geometries were used to analyze form I of atorvastatin. The X-ray wavelength of the synchrotron radiation used in this study was determined to be λ=1.3771 Å. Form I of atorvastatin was found to be triclinic with space group P1 and unit cell parameters a=5.4568(2) Å, b=9.8887(4) Å, c=30.3091(9) Å, α=76.801(3)°, β=99.177(5)°, γ=105.318(5)°, V=1527.1(1) Å3, Z=1, and M=1209.41 g mol−1 Alternatively, another unit cell dimension can be used to describe the same P1 crystal with a=5.4564(2) Å, b=9.8883(4) Å, c=29.6555(8) Å, α=95.745(3)°, β=94.297(5)°, γ=105.327(5)°, and V=1526.8(1) Å3.

A new method is introduced for the evaluation of experimental stress–strain dependence in thermally cycled thin films. The method is demonstrated on the analysis of an Al thin film on a Si(100) substrate characterized using in situ high-temperature X-ray diffraction 25–450 °C. Diffraction data are used to evaluate in-plane elastic strain in the film as a function of thermal strain originating from the mismatch of thermal expansion coefficients (TECs) between the film and the substrate. The magnitude of the thermal strain is calculated from experimental TECs of the film and the substrate at every measurement temperature. By relating in-plane stresses to thermal strains, an experimental stress–strain dependence for the Al thin film is obtained. The proposed method allows one to identify elastic behavior and to quantify plastic strain in the film. Finally, advantages of the method are discussed in particular its independence from using TECs reported in the literature.

Silver halide based photographic imaging elements have been utilized as detectors for X-rays for over 100 years. These elements comprised of gelatin dispersed silver halide coated on one or both sides of a support, have been utilized in diffraction experiments since the discovery of X-ray diffraction by Laue and co-workers. X-ray film has high spatial resolution and can be adapted to flat or curved two-dimensional detection geometries. This paper describes the use of X-ray film as a two-dimensional detector for X-ray diffraction analysis, and discusses X-ray film composition, exposure, and processing, along with considerations for analyzing X-ray diffraction data collected using X-ray film.

The crystal structure of nilotinib has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Nilotinib crystallizes in space group P1 (#1) with a = 4.518 14(3), b = 10.638 01(5), c = 13.703 77(8) Å, α = 68.8607(4), β = 82.1486(5), γ = 84.1978(5)°, V = 607.62(1) Å3, and Z = 1. The most prominent feature of the structure is two strong hydrogen bonds. These form chains with a graph set C1,1(13); the chains run along [111]. Several weak C–H···O hydrogen bonds also contribute to the packing. The powder pattern has been submitted to ICDD for inclusion in future releases of the Powder Diffraction File™.

The I13 transmission X-ray microscope at Diamond Light Source (DLS) has been designed to cover a broad range of energies and field of views. The beamline operates on an undulator source, and a multilayer monochromator can be used to work at a larger bandwidth to enable faster acquisitions. The experimental design includes large working distances for the optics to allow installing in situ sample environments. This paper presents the current state of the experimental system and shows some of the latest results.

Several methods can be used to obtain, from powder diffraction patterns, crystallite size and lattice strain of polycrystalline samples. Some examples are the Scherrer equation, Williamson–Hall plots, Warren/Averbach Fourier decomposition, Whole Powder Pattern Modeling, and Debye function analysis. To apply some of these methods, it is necessary to remove the contribution of the instrument to the widths of the diffraction peaks. Nowadays, one of the main samples used for this purpose is the LaB6 SRM660b commercialized by the National Institute of Standard Technology; the width of the diffraction peak of this sample is caused only by the instrumental apparatus. However, this sample can be expensive for researchers in developing countries. In this work, the authors present a simple route to obtain micron-sized polycrystalline CeO2 that have a full width at half maximum comparable with the SRM660b and therefore it can be used to remove instrumental broadening.