Data for the standard material NBS SRM 674, TiO2, were collected on two diffractometers: a) a Philips PW 1050/37 standard diffractometer of the Bragg-Brentano type equipped with a post diffraction curved Ge monochromator, b) a Stoe Stadi P diffractometer of transmission type equipped with a curved incident beam Ge monochromator. Both monochromators were set to select pure CuKα1 radiation. The reflection type instrument gives a much larger peak to background ratio than the transmission instrument, for which the background is much higher than with the reflection instrument. Rietveld refinements were carried out on both data sets with the programs DBWS-9807 and general structure analysis system (GSAS). The structural parameter of the oxygen atom of rutile depends neither on data set nor program, whereas, e.g., thermal displacement parameters seem to depend on both data set and program.

A modified method for polynomial smoothing and the calculation of derivatives of equally spaced step scan powder diffraction data is presented. The algorithm takes the angular dependence of the full width at half maximum (FWHM) of diffraction peaks into account, is very effective, and easy to code.

Mixed lead chloride oxalate, Pb2Cl2(C2O4), has been obtained in a polycrystalline form in the course of a study on precursors of nanocrystalline PZT-type oxides. Its crystal structure has been solved ab initio from powder diffraction data collected using a monochromatic radiation from a conventional X-ray source. The symmetry is monoclinic, space group C2/m, the cell dimensions are a=5.9411(3) Å, b=5.8714(4) Å, c=9.4212(4) Å, β=95.232(4)° and Z=2. The structure consists of a stacking of complex double sheets, built from lead polyhedra, parallel to (001) and connected together through oxalate groups. The lead atom is nine-fold coordinated by four O atoms from one bidentate and two monodentate oxalate groups and five Cl atoms. The polyhedron can be described as a highly distorted square antiprism mono-capped by a Cl atom. The thermal behavior of lead chloride oxalate, in vacuum and in air, is carefully described from temperature-dependent powder diffraction and thermogravimetric measurements. It is shown that reaction pathways are complicated by the identification of various oxide chloride phases.

A powder neutron diffraction study has been undertaken for the titled compounds at room temperature. Data were analyzed using the Rietveld method. With increasing Nd content the unit cell has been found to contract very slightly, which is in accordance with the ionic radii of La3+ and Nd3+.

The powder pattern of Rb3Ta5O14 is reported here for the first time. Single crystals of Rb3Ta5O14 of 0.1–0.2 mm in size were grown using a RbCl flux at 1100 °C. The Rb3Ta5O14 powders were synthesized at 1200 °C by firing the Rb2CO3 and Ta2O5 raw materials with starting Rb/Ta ratios ranging from 0.450 to 0.800. The products with Rb/Ta ratios between 0.550 and 0.633 contained almost pure Rb3Ta5O14 with Rb/Ta ratio of 0.600, while those with Rb/Ta ratio larger than 0.677 also contained the α form of Rb4Ta6O17 with the Rb/Ta ratio of 0.677. Past studies of the synthesis and characterization of Rb4Ta6O17 should be carefully examined in the light of possible coexistence with Rb3Ta5O14, because the former structure has not been completely solved, and thus the powder pattern is inaccurate, while the presence of the latter had not been known until the present study.

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.

The crystal structure of anhydrous δ-D-mannitol (C6H14O6) was solved from high-resolution synchrotron X-ray powder diffraction data collected on a mixture containing 20% and 80% w/w of β- and δ-D-mannitol, respectively. The direct space simulated annealing program PSSP, and Rietveld analysis employing GSAS were used to determine and refine the structure. The polymorph has monoclinic symmetry, space group P21 with a=5.089 41(5) Å, b=18.2504(2) Å, c=4.917 02(5) Å, and β=118.303(2)°. There is one molecule in the irreducible volume of the unit cell. The pattern of hydrogen bonding is significantly different than the previously known α and β forms.

Two-dimensional X-ray diffraction refers to X-ray diffraction applications with two-dimensional detector and corresponding data reduction and analysis. The two-dimensional diffraction pattern contains far more information than a one-dimensional profile collected with the conventional diffractometer. In order to take advantage of two-dimensional diffraction, new theories and approaches are necessary to configure the two-dimensional X-ray diffraction system and to analyze the two-dimensional diffraction data. This paper is an introduction to some fundamentals about two-dimensional X-ray diffraction, such as geometry convention, diffraction data interpretation, and advantages of two-dimensional X-ray diffraction in various applications, including phase identification, stress, and texture measurement.

So-called alite is a solid solution of tricalcium silicate Ca3SiO5 with a few percent of impurities. It constitutes the major phase of anhydrous Portland cement. In industrial compounds, alite crystallizes into two monoclinic forms designated M1 and M3. The possibility of correlation between the crystallographic structure of the clinker and its reactivity is still an open question. The answer of such a question involves a proper quantitative analysis of the various phases—including the exact alite polymorph—of the industrial product. The rather similar structure of the two alites makes it difficult to distinguish them from their XRD patterns. This paper shows that five angular windows in the X-ray diffraction patterns can be used with synthetic alites as well as industrial compounds, to identify the nature of the actual polymorph (M1 or M3) present and the structural model to be used (with or without superstructure) in subsequent Rietveld analysis of the data.

Two-dimensional proportional detectors with their faster data collection, large dynamic range, and more available information than point or linear proportional detectors make them ideal for microdiffraction analysis. The unique capabilities of these detectors coupled with a rotating anode source, capillary optics, and a variety of accessories allow for a wide range of applications.

Weight fractions of four dominant phases (C3S, C2S, C4AF and C3A) present in the NIST Reference Portland clinkers 8486, 8487 and 8488 were estimated by a series of Rietveld refinements. Calculated powder patterns were derived from the structural data for monoclinic C3S and C2S, orthorhombic C4AF and cubic C3A. X-ray diffraction data were collected in two laboratories with two diffractometers, a reflection and a transmission one. There were no significant differences between the results of the refinements based on the data sets collected on the machines with different experimental arrangements. Estimated phase compositions were compared to the reference values found by optical microscopy (MPC). Median agreement between refined and reference values within ±5% (absolute) was found only for 8488 clinker; for 8486 and C3A-rich 8487 it was within ±10% (absolute). In the majority of the refinements numerical instabilities were detected, leading to large correlations between FWHM and temperature parameters of some phases. The results obtained for C4AF were probably influenced by the presence of possible solid solutions with the structures close to that of C4AF. Weight fractions of low abundant C3A were estimated with the largest relative errors reaching in several cases ∼100%.

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.

Zn7Sb2O12 is known to adopt an inverse spinel crystal structure, in which Zn2+ occupies the eight tetrahedral positions and Sb5+ and Zn2+ randomly occupy the 16 octahedral positions. Samples of Zn7−xNixSb2O12 (x=0, 1, 2, 3, and 4) were synthesized using a modified polymeric precursor method, known as the Pechini method. The crystal structure of the powders was characterized by Rietveld refinement with X-ray diffraction data. The results show that for x=0, 1, and 2 Ni substitutes for Zn2+ in the octahedral sites, and that for x=3 and 4 it is assumed that Ni2+ replaces Zn2+ ions in both the octahedral and tetrahedral positions. It is also observed for x=3 and 4 the formation of two spinel phases.

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 CaZr(PO4)2 was determined from conventional X-ray powder diffraction data using direct methods, and it was further refined by the Rietveld method. The structure was orthorhombic (space group P212121, Z=4) with a=1.448 76(4), b=0.672 13(1), c=0.623 47(2) nm, and V=0.607 10(3) nm3. Final reliability indices were Rwp=6.49%, RB=2.43%, and S=1.32. The Ca atom is sevenfold coordinated, and the Ca atom and surrounding oxygen atoms form a distorted capped octahedron with a mean Ca–O distance of 0.243 nm. The ZrO7 coordination polyhedron is a distorted pentagonal bipyramid with a mean Zr–O distance of 0.216 nm. CaO7, ZrO7, and PO4 polyhedra share edges to form infinite chains with the composition [CaO3ZrO3P2O8]12− along the [010]. Individual chains are linked together, forming a two-dimensional sheet parallel to (100). These sheets are stacked in the [100] direction to form a three-dimensional structure.

Methods of chemical preparation and crystal data are reported for two new anhydrous cyclotriphosphates MIIK4(P3O9)2 (MII=Co2+ and Mn2+). These anhydrous cyclotriphosphates CoK4(P3O9)2 and MnK4(P3O9)2 were obtained by total dehydration of corresponding hydrated cyclotriphosphates CoK4(P3O9)2.7H2O and MnK4(P3O9)2.2H2O. CoK4(P3O9)2 is triclinic, space group P−1, Z=1 with the following unit-cell dimensions: a=6.29(3) Å, b=8.00(1)Å, c=13.05(8)Å, α=86.03(5)°, β=98.00(1)°, γ=68.11(2)°. MnK4(P3O9)2 crystallizes in the rhombohedral system, space group P−31c, Z=2 with the following unit-cell dimensions: a=b=7.337(3)Å, c=19.920(1)Å.

Two XRD specimen holders we designed for use with highly radioactive specimens are described. An injection mold was fabricated to allow inexpensive production of one of the holders. These holders are suitable for single-time use. The ease of use and disposable nature of this holder resulted in a dramatic reduction in personnel exposure and an uncontaminated diffraction unit. A second holder, based on the design of the first, is used to obtain XRD patterns from powders where preferred orientation is an issue and from clays. Both holders result in negligible background, since the specimen is essentially levitated in the X-ray beam. This is a benefit over other methods, such as collodion, that introduce significant background to the XRD pattern.