Evidence is provided that the tridymite component observed in the X-ray diffraction patterns of some sewage sludge ashes (SSAs) should not be interpreted as the tridymite modification of SiO2 but as the tridymite form of AlPO4. This proof is based on a combined X-ray Powder Diffraction (XRD), X-ray fluorescence (XRF) and Mossbauer spectroscopy investigation of two SSAs produced at two fluidized bed incineration facilities, located in different municipalities and operated differently. The structural and chemical characterization was carried out on the ‘as received’ SSA samples as well as on the residues of these two SSAs pretreated by leaching in citric acid. In addition, direct proof is presented that the tridymite form of AlPO4 does crystallize from X-ray amorphous precursors under conditions that mimic the huge heating rate and short retention time (just seconds at T ≈ 850 °C) typical for fluidized bed incinerators.

X-ray powder diffraction is a convenient tool for monitoring changes in structural parameters due to modifications in sample composition and processing conditions. Due to the complexity of incommensurate modulated structures powder diffraction techniques have not been commonly applied. Programs ALSQ and QRIET have been produced to perform lattice parameter and structure refinements on incommensurate modulated materials with a displacive modulation model. In applying these programs to the Bi2Sr2CaCu2O8 superconductor which has this type of structure, it is shown that a decrease in the lattice parameters and an increase in the modulation vector occurs as the Ca content of the Bi-2212 phase, controlled by the use of the glass ceramic process, increases.

A new mixed lead thorium phosphate, Pb0.5Th2(PO4)3, has been isolated in the system PbO–ThO2–P2O5. Its crystal structure (monoclinic symmetry, a=17.459(1) Å, b=6.8451(4) Å, c=8.1438(5) Å, β=101.247(5)°, space group C2/c) has been determined from conventional monochromatic X-ray powder diffraction data. The structure is related to the MITh2(PO4)3 structure type. Lead atoms are located in the channels parallel to the c axis, out of the twofold axis for 0.97 Å, and are statistically distributed on a quarter of crystallographic positions. The thermal stability of this material is greater than that of the monazite-type compound PbTh(PO4)2.

X-ray powder diffraction data of BaFCl are reported for 2θ from 5° to 150° at 25 °C. Strain-free and dendrite-free single crystals of BaFCl, grown by flux method with KCl as flux, were powdered for recording this data. BaFCl is tetragonal, space group P4/nmm, with a=4.3964(1) Å and c=7.2315(3) Å.

Na4CrNi(PO4)3 orthophosphate powder was prepared from acid solutions of NiO, Na2CO3 and aqueous solutions of Cr(NO3)3.9H2O, and (NH4)2HPO4 at a final temperature of 750 °C. The hexagonal unit cell parameters were determined to be ah≈8.789 Å and ch≈21.481 Å in space group R3¯c. These parameters were compared to those of Na4AA′(PO4)3 (AA′=CrMg, CrCo, TiNa, ZrNa). The linear variations of these parameters versus the mean A cation radius (rAA′) are consistent with the atomic distribution found for the structure of Na4NiCr(PO4)3. The ah and ch parameters are functions of the An+ ion size.

A new trimetallic compound with formula (NH4)H2Co2O(OH)(MoO4)1.6(WO4)0.4•H2O and lamellar structure was prepared by hydrothermal synthesis. The solid was characterized using X-ray diffraction (XRD), thermogravimetric (TGA) and differential thermal (DTA) analyses, Fourier-transform infrared spectroscopy (FT–IR), laser Raman spectroscopy (LRS), and atomic absorption spectroscopy (AA). Crystallographic studies showed that the solid crystallizes with hexagonal symmetry in space group R-3 m with a = 6.0807 and c = 21.7591 Å.

Crystal structures of types II and III chlorothalonil, 2,4,5,6-tetrachloro-1,3-dicyanobenzene, (C8Cl4N2) were solved by applying Monte Carlo simulated annealing techniques to X-ray powder diffraction data and refined using the Rietveld method. Both types of chlorothalonil crystallize in monoclinic symmetry (space group P21 and two molecules per unit cell). Lattice parameters are: a=8.1615(18) Å, b=9.4191(19) Å, c=6.4728(14) Å, β=93.7307(64)° and V=497.8 Å3 for type II, and a=8.6003(10) Å, b=9.2382(11) Å, c=6.3024(7) Å, β=96.2152(60)° and V=498.5 Å3 for type III. The structures of both types of chlorothalonil are stacked by two coplanar molecular sheets paralleled to the b-axis. The adjacent two paralleled molecules in type II are on the same plane, while those in type III are on two different parallel planes.

A new hydrate of magnesium chromate is synthesized by quenching aqueous solutions of MgCrO4 in liquid nitrogen. MgCrO4·11H2O is isostructural with the rare mineral meridianiite (MgSO4·11H2O) being triclinic, , Z = 2, with unit-cell parameters a = 6.811 33(8) Å, b = 6.958 39(9) Å, c = 17.3850(2) Å, α = 87.920(1)°, β = 89.480(1)°, γ = 62.772(1)°, and V = 732.17(1) Å3 at −15 °C. The difference in unit-cell parameters between SO4- and CrO4-bearing species is only partially accounted for by the difference in S–O and Cr–O bond lengths; the remainder of the difference (over 90% in the cell volume) is attributed to weakening of the interpolyhedral hydrogen-bond network.

Fourteen reference patterns of oxide ceramics are reported. Included in the fourteen reference patterns are data for nine high critical temperature super-conducting oxide related phases: (BaCuEr2O5, Ba2Cu3EuO7, BaCuGd2O5, Ba2Cu3GdO7, Ba2.4Cu5La4O13, Ba1.9cu3La1.1O7, Ba2Cu3SmO7 and (Ba0.4Sr0.6)2Cu3 YO7). The general methods of producing these X-ray powder diffraction reference patterns were described previously in this journal (Vol. 1, No. 1, pg. 40 (1986)). The symbols used in this article are defined in the PDF cards.

Observed powder diffraction data for two tetracyclines were interpreted with the aid of calculated patterns based upon the crystal structures determined from a single crystal of the same batch for each compound. The results consist of high quality standard powder patterns with the usual supporting data.

A total pattern analysis suite of programs has been developed and incorporated into the ICDD® PDF-4 database. While the suite of programs is intended for the analysis of any diffraction pattern, particular attention was focused on the analysis of common amorphous, non-crystalline, or partially crystalline materials found in minerals, polymers, and pharmaceuticals. The suite of programs directly interfaces to the ICDD database and libraries of non-crystalline references.

The speciation of vanadium in the electrolyte of vanadium redox flow batteries (VRFBs) is important to determine the state of charge of the battery. To obtain a better understanding of the transport of the different vanadium species through the separator polymer electrolyte membranes, it is necessary to be able to determine concentration and species of the vanadium ions inside the nanoscopic water body of the membranes. The speciation of V in the electrolyte of VRFBs has been performed by others at the synchrotron by X-ray absorption near-edge structure analysis (XANES). However, the concentrations are quite high and not necessarily justify the use of a large-scale facility. Here, we show that vanadium species in the electrolyte and inside the ionomeric membranes can be determined by laboratory XANES. We were able to determine V species in the 1.6 M electrolyte with a measurement time of 2.3 h and V species having a concentration of 9.8 g kg−1 inside the membranes (178 µm thick) with a measurement time of 5 h. Our results show that laboratory XANES is an appropriate tool to study these kind of samples.

In the conventional X-ray reflectivity (XRR) analysis, the reflectivity is calculated based on the Parratt formalism, incorporating the effect of the interface roughness according to Nevot and Croce. However, the results of calculations of the XRR have shown strange outcomes, where interference effects increase at a rough surface because of a lack of consideration of diffuse scattering within the Parratt formalism. Therefore, we have developed a new improved formalism in which the effects of the surface and interface roughness are included correctly. In this study, for deriving a more accurate formalism of XRR, we tried to compare the measurements of surface roughness of the same sample by atomic force microscopy (AFM) and XRR. It is found that the AFM result could not be completely reproduced even with the improved XRR formalism. By careful study of the AFM results, we determined the need for an additional effective roughness term within the XRR simulation that depends on the angle of incidence of the beam.

The Nd1.7Ba0.3Ni0.9Cr0.1O4+δ polycrystalline sample was synthesized by the sol–gel process and a subsequent annealing at 1523 K in 1 atm of flowing argon. X-ray diffraction (XRD) analysis and electrical transport properties have been investigated as well. The oxygen non-stoichiometry was determined by iodometric titration. The sample shows adoption of the K2NiF4-type structure based on a tolerance factor calculation. Rietveld refinement of the crystal structure from X-ray powder diffraction data confirmed that Nd1.7Ba0.3Ni0.9Cr0.1O4+δ adopts the tetragonal structure (space group I4/mmm, Z = 2). The room temperature unit-cell parameters are determined to be a = 3.82515(2) and c = 12.47528(6) Å. The reliability factors are: RB = 0.043, Rwp = 0.012 and χ2 = 3.00. The Nd1.7Ba0.3Ni0.9Cr0.1O4+δ compound exhibits a semi-conductive behaviour. The electrical transport mechanism has been investigated and it agrees with the adiabatic small polaron hopping model in the temperature range 313 K ≤ T ≤ 708 K.

Stability of Na-titanate-based nanotubes at high temperature and pressure is investigated using X-ray diffraction and energy-dispersive X-ray diffraction (EDXRD). Our results show that the nanotubes can be stable at ~400 °C. Higher temperature annealing of nanotubes result in opening and flattening of the nanotubes, and subsequent structural transformation to Na2Ti6O13-based structure via an intermediate phase with Na0.23TiO2-like structure. In situ EDXRD using diamond anvil cell indicates that the nanotubes collapse at about 15 GPa, and are finally transformed into an amorphous phase at about 30 GPa. The nanotubes kept in an amorphous state were further compressed to 50 GPa according to our in situ EDXRD observation. Titanate nanotubes are mechanically stronger than carbon nanotubes under static compression.

Residual strain in electrodeposited Li films may affect safety and performance in Li metal battery anodes, so it is important to understand how to detect residual strain in electrodeposited Li and the conditions under which it arises. To explore this Li films, electrodeposited onto Cu metal substrates, were prepared under an applied pressure of either 10 or 1000 kPa and subsequently tested for the presence or absence of residual strain via sin2(ψ) analysis. X-ray diffraction (XRD) analysis of Li films required preparation and examination within an inert environment; hence, a Be-dome sample holder was employed during XRD characterization. Results show that the Li film grown under 1000 kPa displayed a detectable presence of in-plane compressive strain (−0.066%), whereas the Li film grown under 10 kPa displayed no detectable in-plane strain. The underlying Cu substrate revealed an in-plane residual strain near zero. Texture analysis via pole figure determination was also performed for both Li and Cu and revealed a mild fiber texture for Li metal and a strong bi-axial texture of the Cu substrate. Experimental details concerning sample preparation, alignment, and analysis of the particularly air-sensitive Li films have also been detailed. This work shows that Li metal exhibits residual strain when electrodeposited under compressive stress and that XRD can be used to quantify that strain.

The structure of [Pd(NH3)4]Cr2O7 has been determined ab initio from conventional X-Ray powder diffraction data by the Patterson method. The cell is monoclinic (space group P21/c, Z = 4), with a = 7.771(3) Å, b=11.578(1) Å, c=11.852(4) Å, and β= 105.50(4)°. Refinements of 57 parameters by the Rietveld method, using 852 reflections lead to RB = 0.032, RP = 0.075, and Rwp = 0.092. The structure is built up from PdN4 square planes linked to Cr2O7 groups by hydrogen bonds. Hydrogen atoms could not be located.

The synthesis, thermal behavior, crystallographic and X-ray powder diffraction data, and infrared spectral data for Ca8ZnSi4O16Cl2 have been determined. This compound is cubic with isolated silicate tetrahedra.

Mirabegron, (C21H24N4O2S), is a β3-adrenoceptor agonist approved in Japan, the USA, Canada and Europe, for the treatment of overactive bladder symptoms. There are no entries for this important active pharmaceutical ingredient in the Cambridge Structural Database or the Powder Diffraction File-4/Organics database. In this contribution, the powder diffraction pattern of Mirabegron, an unreported phase, are presented with a study by spectroscopy methods (Fourier-transform infrared spectroscopy [FT-IR] and RAMAN) and thermal analysis (thermogravimetric analysis [TGA]-differential scanning calorimetry [DSC]).