European Community Directive 2002∕95∕EC restricts the use of certain hazardous substances in electrical and electronic equipment. In particular, restrictions are placed on lead, mercury, cadmium, hexavalent chromium, and bromine (in polybrominated biphenyls or polybrominated diphenyl ethers). XRF is a convenient method for detecting the presence and measuring the amounts of these elements. Reliably quantifying all of these elements in plastics typically requires a large number of standards that are not yet readily available. Because of the light element matrix, using a “standardless” fundamental parameters method requires some reliance on the primary beam scatter, complicating the analysis algorithm and increasing the uncertainty. We have tested a simplified fundamental parameters method that determines the matrix via difference, requiring only one standard. The method was tested on a series of reference materials containing all of the regulated elements in a variety of plastic resins. One multi-element reference standard was used. It was necessary to include all of the additives in the specimens to achieve good quantitative accuracy. In addition, the scattered primary intensity was used in one set of tests to compensate for variations in specimen thickness. This thickness compensation was necessary to get acceptable results for Cd. Results were very promising, with average relative errors and relative standard deviations of about 10%.

Gallium iron oxide GaFeO3 and the substituted GaFeO3 with Cr and Mn, i.e., Ga(Fe0.95Me0.05)O3, and (Ga0.95Me0.05)FeO3; Me=Cr and Mn, have been synthesized and investigated by X-ray powder diffraction. The refined structural parameters of the considered samples using the Rietveld technique showed a considerable distortion in the polyhedron around different cations, which may have an effect on the piezoelectricity of the studied samples. There are also changes in the interatomic distances between different cations, which may have a direct influence on the ferromagnetic properties of the samples. Crystallite size and microstrain are anisotropic and the largest along the b axis, which may be responsible for the piezoelectricity. The correlations between all these changeable parameters will be discussed.

X-ray powder diffraction data collected for the complex silver(I) cyclamate [Ag(C6H12NO3S)] are reported. This material was obtained from a stoichiometric mixture of sodium cyclamate and AgNO3. The analysis of the data using the Le Bail method showed that the complex has monoclinic symmetry (space group C2/c). The unit cell parameters are a=31.85852(16) Å, b=6.25257(6) Å, c=8.46165(7) Å, and β=95.7651(5)°.

Internal stresses and textures of electroplated copper films (t=2, 8, 15, 30, 45, and 60) electrodeposited on Al substrates were studied using X-ray diffraction techniques. Results show that the stresses in the films are tensile. The 8 to 60 μm thick films have (220) fiber texture, in good agreement with strain energy minimization calculation. Results also show that a further rotational alignment of the fiber-textured grains was developed, and small amounts of the fiber-textured grains have their (2, −2, 0) planes aligned parallel to the flow direction of the electrodeposited currents. The degree of the rotation alignment increases with film thickness. Values of stress and the degree of texture of copper films were found to be adjustable using an ultrasound technique. Internal stress and the degree of the (220) texture decrease significantly by applying an ultrasound treatment during the electrodeposition process.

The value assignment of candidate Standard Reference Material (SRM®) 57b Silicon Metal provided an opportunity to develop an alkali reaction procedure as a precursor to borate fusion for the preparation of test specimens from the metal powder for X-ray fluorescence spectrometry (XRF). Suggested for this purpose by Blanchette in a 2002 Advances in X-ray Analysis article [45, 415–420 (2002)], the alkali reaction uses LiOH∙H2O to convert Si to Li2SiO3. Lithium silicate is fused with lithium borate flux without damage to platinum ware. Once specimens are fused and cast as beads, calibration standards are prepared to closely match the compositions of the specimens, allowing a linear calibration for each analyte. The XRF method yields results that are directly traceable to the mole through NIST SRM spectrometric solutions. The method was validated in two ways. First, the reaction was used on older SRMs for Si metal: SRM 57 and SRM 57a. Second, XRF results for candidate SRM 57b were compared to results obtained using prompt gamma-ray activation analysis (PGAA) and inductively coupled plasma optical emission spectrometry (ICPOES). Bias tests show the XRF results are accurate for the elements Al, S, Ca, Ti, Cr, Mn, Ni, Cu, and Zr. Levels of S, Ca, Cr, and Cu in candidate SRM 57b are near the limits of quantification of the borate fusion method. Iron results may be subject to a low bias. Phosphorus is not quantitatively retained during the alkali reaction and borate fusion. These elements, plus B, which cannot be determined after borate fusion, are listed in manufacturing specifications for Si metal.

A novel borate compound Ba3ScB9O18 has been synthesized by solid-state reaction and its structure has been determined and refined from powder X-ray diffraction data. This compound crystallizes in a hexagonal cell (space group P63/m) with lattice parameters a=7.1360(4) Å and c=16.5420(9) Å, and each unit cell contains two formulas. Its crystal structure is made up of planar B3O6 groups parallel to each other along the [001] direction, regular ScO6 octahedra, irregular BaO6 hexagons, and BaO9 polyhedra to form an analogue structure of Ba3YB9O18. DTA and TGA curves for Ba3ScB9O18 show that it is a chemically stable and congruent melting compound. Luminescence properties for Ba3ScB9O18 were investigated using fluorescence spectroscopy and X-ray excited luminescence measurements. Its emission spectrum upon UV excitation (330 nm) has exhibited a prominent blue-green emission band at about 490 nm, and its XEL spectra show an intense emission band in the range of 360 to 500 nm with peak center at 400 nm. The light yield of Ba3ScB9O18 powders is about 23% as large as that of BGO powders under the same measurement conditions. There seems to be a certain relationship between the scintillation properties and the structural features of Ba3ScB9O18.

X-ray powder diffraction data and unit cells parameters for a monoclinic variety of the popular herbicide 2-chloro-N-(pyrazol-1-ylmethyl) acetyl-2′, 6′-xylidide, commonly known as metazachlor, butisan, and butichlor, is presented [a=7.306(3) Å, b=17.824(9) Å, c=10.728(3) Å, β=98.46(4)°, space group P21/c, cell volume=1381.82 Å3, Z=4]. The four strongest peaks (Irel>25) at 8.87, 7.19, 4.57, and 4.45 Å are quite distinctive, thus X-ray powder diffraction provides a quick, simple, and definitive method of identifying this form of material from other commercially available herbicide products.

Four aliphatic-aromatic diols with ether linkages [4, 4′-Bis(2-hydroxyethoxy)benzophenone, 4, 4′-Bis(3-hydroxypropoxy)benzophenone, 4, 4′-Bis(6-hydroxyhexyloxy)benzophenone, 4, 4′-Bis(11-hydroxyundecyloxy)benzophenone] and two aliphatic-aromatic diols with sulfur linkages [4, 4′-Bis[(2-hydroxyethyl)thio]benzophenone, 4, 4′-Bis[(3-hydroxypropyl)thio]benzophenone] have been characterized by X-ray powder diffraction. These diols can be used for synthesis of thermoplastic nonsegmented polyurethanes. Experimental 2θ peaks positions, relative peak intensities, values of d, and Miller indices as well as unit-cell parameters are presented.

Crystal structure of high-temperature modification of Pd73Sn14Te13 has been refined by the Rietveld method from laboratory X-ray powder diffraction data. Refined crystallographic data of Pd73Sn14Te13 are a=7.6456(3) Å, c=13.9575(9) Å, V=706.75(6) Å3, space group P63cm (No. 185), Z=6, and Dx=10.71 g/cm3. The title compound is isostructural with Pd5Sb2 and Ni5As2; it can be considered as a stacking and filling variant of the Ni2In structure. An important structural feature in the high-temperature modification of Pd73Sn14Te13 is the presence of various Pd-Pd bonds.

We know a lot about normal values of bond distances, bond angles, torsion angles, and other molecular parameters. This knowledge can be incorporated into the structure solution process and into Rietveld refinement through the use of restraints and rigid bodies. An important measure of the quality of the refined model is the chemical reasonableness of molecular geometry. Refinement of the structures of calcium tartrate tetrahydrate and guaifenesin is used to illustrate the importance of chemical reasonableness in determining the quality of a Rietveld refinement.

Besides statistical and graphical measures, many structural features can be used to assess the quality of a Rietveld refinement. These include the metric symmetry of the lattice (which can assist in determining the true symmetry and in identifying isostructural compounds), bond distances and angles (which should fall within normal ranges), displacement coefficients, refined stoichiometry, the absolute values of the standard uncertainties of the fractional coordinates, the hydrogen bonding pattern, the presence of approximate symmetry, the presence of unindexed peaks in the pattern, and whether the refinement converges at all. Chemical knowledge can be built into a Rietveld refinement though the use of restraints and rigid bodies. A knowledge of chemical reasonableness proved important in refining the correct structures of [Fe(H2O)6](BF4)2, (Ba1.5Sr0.5)TiO4, and (Ba1.25Sr0.75)TiO4.

A novel method for preparing thin films was investigated for quantifying gallium and iron in plutonium solutions using WDXRF. This technique was developed to eliminate the potential for radioactive liquid to leak into the spectrometer, decrease specimen preparation time, and minimize waste. Samples were cast in μL quantities onto Kapton, and a surfactant was added to disperse the solution uniformly across the Kapton. After drying the specimens, they were sealed in a cell for analysis. Results to date indicate the method can provide a relative precision of ∼0.5% for gallium and ∼2% for iron, which is more than sufficient for routine sample analyses.

A series of Internet-distributed audio/visual recordings for learning crystallographic analysis of powder diffraction data is discussed. These recordings provide a compact mechanism for distributing educational information. Such presentations provide hands-on discussion beyond what is usually presented in instructional texts. In some cases similar material can be presented with HTML text, but recordings can be created with significantly less effort and are superior for software demonstration.

Structural properties of Cd1−xCuxCr2O4(CCCO) have been investigated by means of X-ray powder diffraction and Rietveld analysis. A structural phase transformation from Fd3m to I42d at x=0.64 has been detected. The lattice constant a of the cubic unit cell decreases rapidly with increasing Cu content up to x=0.62. At x=0.64, the cubic unit cell is compressed into a tetragonal cell and CrO6 octahedrons are distorted. With continuing Cu content increases above 0.64, the distortion of the unit cell is released slightly according to the changes in c/a. Magnetic properties of Cd1−xCuxCr2O4(x=0.1,0.3,0.5,0.7) have also been measured and are discussed.

Nanocrystallized oxide precursors of colored (oxy)nitrides related to the system Yb-(Zr-W)-O have been successfully prepared using a chimie douce process—the amorphous citrate route. The process involves first a formation of fine and homogeneous powdered solids obtained by calcination at 600 °C, a temperature much lower than that of the conventional solid-state method. At this stage, the X-ray diffraction patterns exhibit large line broadening effects. Finally, two well-crystallized and pure quaternary oxides have been readily obtained by heating and under annealing conditions at 850 and 900 °C for 12 h. For one of the patterns, all the X-ray diffraction lines can be easily indexed to a cubic phase with the fluorite structure conforming to the Fm3m space group [Yb2Zr1.21W0.41O6.65◻1.35 called C-phase: a=5.1864(2) Å]. The second phase adopts the sheelite-type structure [Yb2ZrWO8 called T-phase: space group I41/a, a=5.1584(5), and c=10.8246(6) Å]. By taking into account the present compositions determined by EDS measurements, Rietveld structure refinements produce final RB factors of 0.015 and 0.044, and Rwp factors of 0.069 and 0.089, respectively. In order to characterize the microstructure of the materials (crystallite size and lattice distortion) at the nanometer scale, a study based on diffraction line broadening analysis applying the whole pattern refinement method was also undertaken with confidence. The results show smooth angular variations of the values of FWHMs, indicating that the microstructural properties are isotropic for the cubic and tetragonal oxides. More precisely, the results indicate that whatever the profile fitting approach used (“profile matching” procedure and Rietveld method), the reliability factors Rwp are systematically better with a combined size strain than with zero strain considerations. The strain magnitudes observed for the C-phase-850 °C as well as for the T-phase-900 °C should be viewed as realistic strain.