Slags sourced from a derelict zinc–lead–copper–silver–tungsten mine were examined for their bulk elemental composition and mineralogy. pH, oxidation–reduction potential, and the leachability of selected elements (sulphur, calcium, iron, copper, zinc, and lead) were assessed during a 130-day deionised water extraction conducted under oxic conditions. Slags were rich in silicon, iron, copper, zinc, and lead, hosted within minerals including quartz (SiO2), goethite [FeO(OH)], augite [Ca(Mg,AI,Fe)Si2O6], and lead (Pb0). Leachates from the slags increased in analyte concentration throughout the 130-day experiment, with iron, copper, zinc, and lead attaining >5 mg l−1 in some samples. These findings indicate that this pyrometallurgical waste should not be considered environmentally inert, as leachates emanating from them in the field might pose a significant risk to the environment.

This study focuses on characterization of an (Al,Cr)3Ti alloy processed together with titanium powder by reactive mechanical milling (RMM) to produce an ultrafine grained intermetallic alloy matrix with in situ carbide and hydride phases formed during processing. Observations of X-ray scattering as RMM processing time increases show severe broadening of matrix diffraction peaks, accompanied by the appearance of diffraction peaks resulting from the formation of very small crystallites of TiC and TiH1.92 phases with increasing volume fractions, and finally, increasing background intensity as the crystallite size of the matrix phase decreases to ∼2 nm. Estimates of phase volume fractions were made by the direct comparison method, along with crystallite sizes by Warren–Averbach peak profile analysis. The general increase in background intensities has been attributed to random static displacements of the large fraction of atoms located within the grain boundary regions. Further, it has been concluded that the matrix material with a crystallite size of a few nanometers has about half the atoms in statically displaced positions defining the boundary regions. The results argue that background intensity changes should not be ignored and are useful in interpreting scattering from these nano-scale materials.

As a producer of certified reference materials (CRMs), NIST faces high demand for Standard Reference Materials (SRMs). The demand is exacerbated by widespread misuse of CRMs. When should one use CRMs? When should one not use CRMs? Must labs always use NIST SRMs? How can labs demonstrate analytical capabilities for their accreditation scopes? Why so many questions? Standards developers, laboratory accreditors, and laboratory staff must be able to understand these topics with respect to quality systems in compliance with ISO/IEC 17025. They must calibrate and validate test methods and document traceability to the International System of Units (SI). Many people working in laboratory accreditation and under the umbrella of a quality system do not fully understand what these things are, let alone the language of chemical metrology. On average, they have little training in analytical chemistry, elemental analysis, and reference material development. It is hoped this paper will impress upon the reader the need for understanding how CRMs can be best used in the laboratory. This paper provides a brief background on the above problems and then looks at some of the support and reference information provided by NIST to metals and mining industries labs, commercial CRM producers, and accrediting bodies. The concepts and guidance apply broadly to chemical metrology and fundamental analytical chemistry. The paper includes examples (some from X-ray fluorescence spectrometry) to illustrate concepts.

The crystal structure of danofloxacin mesylate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Danofloxacin mesylate crystallizes in space group P1 (#1) with a = 6.77474(8), b = 12.4973(4), c = 12.82826(28) Å, α = 84.8709(29), β = 87.7501(10), γ = 74.9916(4)°, V = 1044.723(11) Å3, and Z = 2. The protonation of the danofloxacin cations was established by the analysis of potential intermolecular interactions and differs from that expected from isolated-cation calculations. The crystal structure consists of alternating layers of cations and anions parallel to the ac-plane. There is parallel stacking of the oxoquinoline rings along the a-axis. The expected N–H⋯O hydrogen bonds between the cations and anions are not present. Each cation makes an N–H⋯O hydrogen bond with the other cation, resulting in zig-zag chains along the a-axis. Both cations have strong intramolecular O–H⋯O hydrogen bonds. There are several C–H⋯O hydrogen bonds between the danofloxacin cations and mesylate anions. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

This paper describes a method to determine the equilibrium transformation temperatures in low C steels using the in situ high-temperature X-ray diffraction technique. The samples were heated and then cooled from 1000 to 720 °C in a stepwise manner decreasing to −10 °C. Austenite and ferrite fractions were determined by a quantitative method using the integrated intensities of austenite (111)γ and ferrite (110)α peaks from X-ray diffraction patterns. The effect of the temperature on interplanar d spacings of (111) and (110) crystallographic planes was determined using 2θ maximum positions of the austenite (111)γ and ferrite (110)α peaks. The equilibrium transformation temperatures were determined to be Ae1=720 °C and Ae3=950 °C. The results are in excellent agreement with those obtained by dilatometric analysis and Thermo-Calc phase diagram simulation software. In addition, the results were supported by microstructural observations: the formation of thin ferrite films (5–10 μm) was observed at temperatures near to experimental Ae3.

A novel sealed gaseous parallel plate avalanche chamber detector is described which is significantly less prone to discharges and can consequently achieve high gas gains at high counting rates. The detector has demonstrated stable gains greater than 104 at counting rates in excess of 107 counts/mm2 s.

The crystal structure of varenicline hydrogen tartrate Form B (Chantix®) has been refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Varenicline hydrogen tartrate Form B crystallizes in space group P212121 (#19) with a = 7.07616(2), b = 7.78357(2), c = 29.86149(7) Å, V = 1644.706(6) Å3, and Z = 4. The hydrogen bonds were identified and quantified. Hydrogen bonds link the cations and anions in zig-zag chains along the b-axis. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

Pyrolytic graphite is frequently used as a post diffraction monochromator with powder diffractometers of the Bragg-Brentano type. Curved graphite monochromators yield high intensities and suppress efficiently fluorescent radiation except from the element which is the same as the target element of the X-ray tube. They are not, however, able to separate the Kα1 line from the Kα2 component with the X-ray targets normally used in powder diffraction. Crystals with smaller mosaic spread than graphite are needed for selecting a pure Kα1 line. Commercially available crystals which are suitable for this purpose are asymmetrically cut curved quartz and germanium monochromators of the Johansson type. Experiments have been carried out in this laboratory with two quartz monochromators and one germanium monochromator.

Polycrystalline BaTi1−x(Zn1/3Nb2/3)xO3 (x=0.025 and 0.9) compounds were synthesized successfully and studied by XRD and dielectric measurements. The effects of the Ti/(Zn,Nb) ratio on the structure and dielectric properties of the compounds were investigated. XRD results indicated that the crystal structure of the x=0.09 compound is cubic perovskite with space group Pm3m and a=4.0095(4) Å. For the x=0.09 compound, a splitting of the (200) peak was observed near 40.2°, indicating that the crystal structure changed from cubic to tetragonal, with space group P4mm, a=4.026(4) Å, and c=4.0091(4) Å. Rietveld refinement of the crystal structures led to final confidence factors Rp=0.0353 and Rp=0.0349 for x=0.025 and 0.9, respectively. Dielectric measurements showed a relaxor behavior present in BaTi0.1(Zn1/3Nb2/3)0.9.

In the preparation of ceramic SrCe0.95Yb0.05O3−α great care was taken to obtain a homogeneous, carbonate free and dense material of exactly the given composition. The material is an important high-temperature protonic conductor (HTPC). X-ray powder diffraction data are reported. The cell parameters obtained are a=6.007(2) Å, b=12.296(3) Å, c=8.588(2) Å, cell volume 634.4(1) Å3, Z=8. The space group is most probably Pnma (62) and Dx=5.806(2) g/cm3. The bending strength of the sintered dense material is 175±6 MPa.

A new software application has been developed to provide a convenient method for the submission of diffraction data directly to the International Centre for Diffraction Data, for inclusion in the Powder Diffraction File (PDF)™. The application, titled Genie, acts as a portal for the merging of data from separate sources allowing the user to quickly and easily submit their data for the PDF. Using Java Web Start technology Genie can be run using all common computer platforms. Genie is flexible and can be used to read a variety of common file formats. Furthermore, Genie can also be used for submission of New Diffraction Data for publication in the Powder Diffraction Journal.

Laboratory X-ray powder diffraction was used to solve and refine the crystal structures of appended guest molecules within the pores of metal–organic frameworks (MOFs). Herein, we report the crystal structure of 1-propanethiol adsorbed in the pores of Co2(dobdc) (dobdc4– = 2,5-dioxido-1,4-benzenedicarboxylate, MOF-74). Soaking the activated MOF in neat 1-propanethiol resulted in the formation of 1-propanethiol–Co2(dobdc). The thiol appendant MOF maintained the crystal symmetry, with a rhombohedral space group R-3 and unit-cell parameters a = 25.9597(9) Å, c = 6.8623(5) Å, and V = 4005.0(4) Å3. As expected, the thiol sulfur formed a bond with the open cobalt metal site. The alkane chain was directed toward the center of the pore, participating in numerous van der Waals weak interactions with neighboring molecules. For the final Rietveld refinement, soft restrains were applied using bond distances obtained by periodic density functional theory (DFT) geometry optimization.

Polycrystalline Ba0.8Sr0.2Ti0.6Zr0.3Mn0.1O3 was synthesized by solid-state reaction at 1600°C. The single phase formation of the compound without any impurities was confirmed by the X-ray diffraction technique. The prepared compound crystallized to a cubic structure with a space group of Pm-3m and the refined lattice parameters were a = b = c = 4.0253 Ǻ, α = β = γ = 90°. Rietveld refinement was carried for the powder XRD data using GSAS software and the experimental data peaks were indexed by Powder X software.