A new Tutton’s salt Tl2[Mn(OH2)6](SO4)2 was grown from aqueous solutions and characterized by chemical analysis and X-ray powder diffraction. It was found to be monoclinic, space group P21/a, a=0.93276(6), b=1.25735(8), c=0.62407(4) nm, and β=106.310(3)°. It is unstable in warm air and dissolves incongruently. A comparison of unit cell volumes for all 37 Tutton sulfate phases found in ICDD’s PDF-2 database (86 entries) reveals a reasonable correlation with Shannon and Prewitt’s ionic radii [Acta Crystallogr. 25, 925–926 (1969)] and several deviations, most of them seeming to be erroneous entries.

Yttrium oxalate dihydrate, Y2(C2O4)3.2H2O, has been investigated by means of X-ray powder diffraction. Unit cell dimensions were determined by an indexing program based on the variation of parameters by successive dichotomies. The diffractometer data were collected with strictly monochromatic radiation. A monoclinic cell was found: a=9.3811(8)Å, b=11.6385(15)Å, c=5.9726(7)Å, β=96.079(8)°, which is characterized by the figures of merit M20=87 and F30=112 (0.0065,41). A preliminary analysis of the anisotropic line broadening has revealed some microstructural properties. It is shown that line broadening is mainly due to a micro-strain effect.

A two-stage procedure is described for quantitative phase analysis of multicomponent mixtures. Profile analysis of the diffraction pattern of a mixture of phases is done in stage one to obtain integrated intensities with higher accuracy. In stage two a structural refinement is done which yields a scale factor. The weight of a phase in a mixture is proportional to its specific scale factor. The two-stage method was found to be effective for the quantitative phase analysis of a mixture of minerals which always contain structural defects. The procedure was tested first by using two artificial mixtures and then it was applied to natural kaolin. The results obtained were more accurate than some of the other methods used for quantitative analysis; moreover, it can also be used with mixtures containing amorphous or undetermined phases.

Crystal structure analyses by the Rietveld method have shown that the framework structures of zeolites ZSM-5 and ZSM-8 are essentially identical. Therefore, it is difficult to distinguish the two phases especially when the template-free H forms are studied. In addition, some inconsistencies in publications on the two zeolites aggravate the correct interpretation of the powder diagrams. A powder pattern published for ZSM-8 which indicates significant differences between the lattice constants of ZSM-8 and ZSM-5 is shown to be incorrectly indexed. Correct reindexing gives lattice constants for ZSM-8 matching average ZSM-5 values. Peak splitting of a ZSM-8 reflection at 2θ≈23° (CuKα) has been used frequently to distinguish ZSM-8 from ZSM-5. However, it is also a common feature of ZSM-5 diagrams when the difference between a and b lattice constants is big enough to separate hkl and khl reflections within the instrumental resolution. Our data on two ZSM-8 samples indicate that cell dimensions of ZSM-8 do not deviate from average ZSM-5 values. It is suspected that effects in the decomposition of crystals upon calcination, and/or morphology and shape of twin individuals, and/or stacking faults account for different sorption properties of the two zeolites rather than differences in their average crystal structures.

The ferroelectric liquid crystal material [4-[(4-methyloxyfenyl) carbonyloxyl] bifenyl-4′-yl]-(S)-2-methylbutoxypropionate containing a lateral methyl group on the aromatic ring of the alkoxybenzoate unit and two chiral carbons has been investigated by X-ray powder diffraction analysis at the 28 °C–105 °C temperature range. On cooling through the SmC temperature range, the layer spacing decreases from 28.3 to 27.7 Å with a small variation of average intermolecular distances. Lattice parameters of tetragonal and monoclinic crystalline phases occurring at lower temperatures have been determined.

The X-ray powder diffraction pattern for the title compound is reported in the range 5 ≤ 2θ ≤ 125°. The sample was prepared through solid-state reaction of BaCO3, CuO, and Pr6O11, and characterized with respect to oxygen content through iodometric titration. Refined parameters for the orthorhombic (space group Pmmm) unit cell are a = 3.8587(2) Å; b = 3.9302(1) Å; c= 11.7126(3) Å; a/b = 0.98181(6); a/c = 0.32945(2); b/c = 0.33555(1); Z = 1; Dx = 6.705(2) Mg m−3; V = 177.62(1) Å3; formula wt. = 717.48(16) g mol−1; SS/FOM: F30 = 48(0.005,127).

The present paper establishes that the ratio between the XRD pulse counts of cement clinkers at d=0.278 and 0.274 nm bears a distinct relationship with the degree of sintering of the clinker, which is one of the factors that determine the cement quality. The paper also presents a rapid and accurate method for predicting both 3- and 28-day compressive strength (CCS) of cement mortar cubes based on XRD of the cement clinkers. The method is based on an index Xn derived from the XRD pulse counts at d=0.2959 and 0.287 nm corresponding to alite (hkl=202) and belite (hkl=102) phases of the clinker, respectively. The regression equation derived for a particular plant is (1) 3 day CCS=Xn×240 kg/cm2, when Xn<1 and 240+26 (Xn−1) kg/cm2, when Xn>1, where Xnmaximum=5.5. (2) 28 day CCS=C+C×In/100, where C=3 days CCS estimated by XRD (1), In=90−10Xn, where Xnmax=5.5. Calculated CCS values, in average, vary from the conventional test values by +5.9% to −5.4% and +3.8% to −3.5% in cases of 3- and 28-day CCS, respectively.

Near-surface triaxial strain/stress states in polycrystalline solids are required for a full tensorial treatment including all elements of the strain/stress tensor. A possible depth dependency of the strain/stress is at best observed by grazing incidence diffraction in Seemann–Bohlin geometry (SBG). The computer program SBGBBG calculates the full strain/stress tensor from X-ray diffraction data measured either in SBG or in Bragg–Brentano geometry (BBG). At present SBGBBG is applicable only on texture-free materials.

The crystal structure of a novel high-energy density material 3-[(3,4-dinitro-1H-pyrazol-1-yl)-NNO-azoxy]-4-nitro-1,2,5-oxadiazole C5HN9O8 was determined and refined using laboratory powder diffraction data. The diffraction data and database analysis were insufficient to distinguish two candidate structures from the solution step. Density functional theory with periodic boundary conditions optimizations were used to choose the correct one. 3-[(3,4-Dinitro1H-pyrazol-1-yl)-NNO-azoxy]-4-nitro-1,2,5-oxadiazole crystallizes in space group Pbca with a = 8.3104(2) Å, b = 14.2198(5) Å, c = 19.4264(7) Å, V = 2295.66(14) Å3. The molecular conformation contains a weak intramolecular hydrogen bond C–H⋯O–N, and the structure is dominated by weak O⋯π and O⋯O contacts.

At the Institute of Microstructure Technology (IMT) of the Karlsruhe Institute of Technology (KIT), a new type of refractive X-ray optics has been developed. Owing to its comparably easy fabrication method and the large aperture, the so-called Rolled X-ray Prism Lenses (RXPL) have the potential to be used with X-ray tubes in an industrial environment as a low-cost alternative to existing optics. The lens itself is built out of a micro-structured foil which is cut into shape and rolled around a winding core to form a refracting element for X-rays. The resulting refractive structure can be used as illumination optics. Diffractometry experiments with an NIST 1976a sample were performed and showed up to an 18-fold enhanced integrated intensity compared to that acquired with a steel tube collimator.

Diblock copolymers (BCPs) show phase separation on mesoscopic length scales and form ordered morphologies in both bulk and thin films, the latter resulting in nanostructured surfaces. Morphologies in thin films are strongly influenced by film parameters, the ratio of film thickness and bulk domain spacing. Laterally structured polymer surfaces may serve as templates for controlled assembly of nanoparticles (NPs). We investigated the BCP of poly(n-pentyl methacrylate) and poly(methyl methacrylate) which show bulk morphologies of stacked lamellae or hexagonally packed cylinders. Thin films were investigated by atomic force microscopy and grazing-incidence small-angle X-ray scattering. For film thicknesses f well below d bulk, standing cylinder morphologies were observed in appropriate molar ratios, while film thicknesses around and larger than d bulk resulted in cylinders arranged parallel to surface. To alter and/or improve the morphology also in presence of different NPs (e.g., silica, gold), solvent vapour annealing (SVA) was applied. The BCP morphology usually remains unchanged but periodicities change depending on type and amount of incorporated NPs. It was found that silica clusters enlarge lateral distances of cylinders, whereas Au NPs reduce it. The effect of SVA is weak. The quality of morphology is slightly improved by SVA and lateral distances remain constant or are slightly reduced.

We report on the X-ray diffraction data and unit-cell parameters of Mn4C, which has a cubic perovskite-type structure with a = 3.8726 Å and unit-cell volume V = 58.1 Å3. The measured lines were indexed and are consistent with the space group $ Pm { \bar {\it 3}} m$ (No. 221).

Calcium monoaluminate is the main phase in calcium aluminate cements and participates in the hydration, forming calcium aluminate hydrates. The amount of incorporation of foreign ions influences the hydration behaviour. Strontium aluminate is an important phase in producing phosphorescent materials when doped with rare-earth elements (REE) such as Eu, Dy, and La. These monoaluminates occur in different forms. Monocalcium aluminate forms a monoclinic and an orthorhombic modification, whereas monostrontium aluminate forms a monoclinic low-temperature and a hexagonal high-temperature form. Monoclinic calcium monoaluminate and monoclinic strontium aluminate form a partial solid-solution series. The hydration behaviour of different solid solutions was also investigated using calorimetry. The newly formed strontium aluminate hydrates could be identified while similar strontium aluminate hydrates are formed. Solid solutions of strontium- and calcium-aluminate hydrates will be investigated.

Quantitative phase analysis is one of the major applications of X-ray powder diffraction. The essential principle of quantitative phase analysis is that the diffraction intensity of a component phase in a mixture is proportional to its abundance. Nevertheless, the diffraction intensities of the component phases cannot be compared with each other directly since the coherent scattering power per unit cell (or chemical formula) of each component phase is usually different. The coherent scattering power per unit cell of a crystal is well represented by the sum of the squared structure factors, which cannot be calculated directly when the crystal structure data is unavailable. Presented here is a way to approximate the coherent scattering power per unit cell based solely on the unit cell parameters and the chemical contents. This approximation is useful when the atomic coordinates for one or more of the phases in a sample are unavailable. An assessment of the accuracy of the approximation is presented. This assessment indicates that the approximation will likely be within 10% when X-ray powder diffraction data is collected over a sufficient portion of the measurable pattern.

The crystal structure of pomalidomide Form I has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Pomalidomide Form I crystallizes in the space group P-1 (#2) with a = 7.04742(9), b = 7.89103(27), c = 11.3106(6) Å, α = 73.2499(13), β = 80.9198(9), γ = 88.5969(6)°, V = 594.618(8) Å3, and Z = 2. The crystal structure is characterized by the parallel stacking of planes parallel to the bc-plane. Hydrogen bonds link the molecules into double layers also parallel to the bc-plane. Each of the amine hydrogen atoms acts as a donor to a carbonyl group in an N–H⋯O hydrogen bond, but only two of the four carbonyl groups act as acceptors in such hydrogen bonds. Other carbonyl groups participate in C–H⋯O hydrogen bonds. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

This paper describes a straightforward method for the identification of the Miller indices associated with the face of a crystal of low symmetry. The method relies on orienting a crystal face parallel to the sample holder in the goniometer of a powder diffractometer. An intense diffractogram resulting from a single family of lattice planes parallel to the crystal face is obtained. The application of silicon powder to the surface of the crystal provides a means to correct 2Θ values for any misalignment of the crystal face. Calculated 2Θ and intensity values are used to assign the reflections from the corrected single-crystal diffractogram to a particular set of related lattice planes. In this paper are listed the corrected experimental 2Θ and intensity values for a particular face of a large single crystal of monoclinic hydroxylapatite and the theoretical 2Θ and intensity values for the h00 set of planes. Comparison of these parameters leads to the unambiguous assignment of that particular crystal face to the h00 Miller index.

X-ray powder-diffraction data for Pb2(C2O4)(NO3)2·2H2O were obtained. The crystal system was determined to be monoclinic. The unit-cell parameters were refined to a=10.613(2) Å, b=7.947(2) Å, c=6.189(1) Å, and β=104.48(2)°.

Evidence for the recently described 2M2 polytype of brochantite from X-ray powder diffraction investigation of secondary alteration products of ore material from the Pierre Plate Mine, Vizille, Isère, France is presented. This report is the first to describe the 2M2 polytype from locations outside of Italy and through the use of powder XRD methods. In the procedure used herein, developed in a study by Merlino et al. [Eur. J. Mineral 15, 267–275 (2003)], we have used family reflections, common to both main types of brochantite, as the source of approximate cell parameters from which we obtain positions of characteristic reflections to demonstrate the unique choice of polytype, before final refinement stage. This method demonstrates that the determination of polytype is possible from powder data, for samples typical of both geological and urban environments. Least-squares refined cell parameters for the 2M2 polytype from Pierre Plate are a=12.7409(8) Å, b=9.8371(6) Å, c=6.0109(3) Å, and a=90.135(9)°, constrained in space group P21/n11.