The crystalline structure of new TlSr2PrCu207−x was obtained at room temperature (300 K) and low temperature (100 K) from X-ray powder diffraction with CuKα radiation using Rietveld analysis. TlSr2PrCu207−x has an isotypical structure with TlBa2CaCu207 (1212). At 300 K, crystal data: Tl0.864Sr2PrCu2O6.75, Mr=727.811, the tetragonal system, P4/mmm, a =3.85404(5) Å, c = 12.1046(2) Å, V=179.80 Å3, Z=1, Dx =6.7218 g cm−3, μ =1143.922 cm−1 (λ = 1.54051 Å), F(000)=317.0, the structure was refined with 28 parameters to Rwp=5.29%, Rp = 3.65% for 3551 step intensities and Rb=7.40%, Rf=639% for 155 peaks, “goodness of fit” 5=3.05. At 100 K, crystal data: Tl0.858Sr2PrCu2O6.61, Mr=724.345, the tetragonal system, P4/mmm, a =3.84872(6) Å, c = 12.0771(3) Å, V=178.89 Å3, Z=1, Dx=6.7235 g cm−3, μ=1146.939 cm−1 (λ= 1.54051 Å), F(000) = 315.4, the structure was refined with 26 parameters to Rwp=6.70%, Rp=5.11% for 2926 step intensities and Rb=7.83%, Rf=6.70% for 131 peaks, “goodness of fit” S = 1.75.

A new method for the quantification of montmorillonite by full-profile Rietveld analysis of the XRD profile is presented. A measured standard XRD pattern of Algerian bentonite was used to construct a universally applicable montmorillonite (hkl) file for use with a P.C. based Rietveld XRD quantitative analysis system, SIROQUANT. “Universal” means that the standard file can be used for montmorillonites from other localities. The validity of the montmorillonite standard profile was tested with weighed mixtures of quartz and different standard montmorillonites. The results show the montmorillonite observed (hkl) file is generally applicable (i.e., universal), and can be used to quantify montmorillonite in any mineral without modification or chemical treatment of the sample. Two halfwidth functions were used for the montmorillonite, corresponding to the sharp (hk0) and broad (hkl) classes of reflections. A March preferred orientation parameter for montmorillonite was also refined.

A natural olivine sample from a mantle peridotite xenolith has been studied by in situ high-temperature powder diffraction. The structure has been successfully refined from powder data at three temperatures (25, 600, and 800 °C) using the Rietveld method. The study shows that the full-profile technique is well suited for the structure analysis of high-temperature powder diffraction data. The results indicate that, in this temperature range, there is no significant ordering of the Fe,Mg cations in the two crystallographically independent octahedral sites. This has implications for the thermodynamic modeling of olivine at upper mantle conditions. The present experiments allowed measurement of the lattice thermal expansion of olivine in the temperature range 25–800 °C, and assessment of the temperature dependence of the isotropic atomic displacement parameters.

Afghanite is a feldspathoid of the cancrinite-group: It is hexagonal, space group P63mc. The afghanite sample was found in the M. Somma-Vesuvio volcanic complex (Italy) and was previously described as davyne: Calculated cell parameters are a = 12.7997(4) Å, c = 21.4062(11) Å; the volume is 3037.2(2) Å3. The strongest lines are: 3.694(100), 3.647(56), 4.826(30), 2.678(25), 2.134(18), 3.999(12), 2.750(12), and 2.771(10). The new data provide quantitative measurement of intensities, an increased number of indexed peaks, and a different empirical formula with respect to the PDF 20-1086.

Accurate powder diffraction data for the superconducting phase TlBa2Ca2Cu3O9−δ have been obtained. This phase crystallizes in a tetragonal unit cell, with space group P4/mmm. Cell refinement of our material resulted in a tetragonal unit cell with a=3.8453(8)Å and c = 15.909(4)Å. These diffraction data improve on data currently present in the powder diffraction file. Our experimental data also agree with calculated diffraction patterns obtained from published atom positions.

Use of the overlap integral in X-ray diffraction (XRD) powder pattern recognition of crystalline materials is presented. The mathematical expression, derived specifically for diffraction data, provides a measure of similarity between two patterns. Each pattern is represented by a normalized mathematical function. The index of similarity, or overlap integral, indicates how faithfully the two functions overlap and ranges from zero to unity, reaching the latter limit when the two patterns become identical.

Titanium oxycarbonitride was observed to form during the carbothermic reduction of TiO2 in the presence of nitrogen. A powder diffraction pattern for this phase which is isomorphous with TiC, TIN, and TiO is presented. The crystal structure is further discussed in terms of the observed composition and lattice defects.

A computer program for phase identification using powder diffraction data is presented. It works with a small database containing the unit-cell dimensions and Bravais lattice for chosen classes of inorganic substances. The algorithm works for single phase samples and such samples in which a single phase dominates. During the search, the peak positions generated using the reference unit cells are compared with the experimental ones. Unit-cell constants of all obtained solutions are (optionally) immediately refined. Application examples show that the method gives as possible solutions those database entries for which the cell dimensions differ from the investigated sample by not more than about 0.05 Å. These entries may include the true phase or isotypical phases unless the imposed chemical constraint does not exclude them. If the sample is a solid solution, then the algorithm is able to find phases of differing chemical composition belonging to the same solubility range (provided that the difference in lattice constants is not too large). One of the examples illustrates the possibility of application for electron-diffraction data.

Standardized X-ray powder diffraction data for orthorhombic LaCo0.4Fe0.6O3 prepared by calcination of a glycine-nitrate combustion-synthesized precursor are reported. Orthorhombic unit cell parameters: a = 5.4688 (2), b = 5.5100 (2), c = 7.7462 (3) Å. The reference intensity ratio, I/Icor,= 6.12.

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.

Diffraction patterns were recorded, and unit cell dimensions refined by the least-squares method, for lactitol and lactitol monohydrate. Refined unit cell parameters for lactitol are: a =7.622(1) Å, b = 10.764(2) Å, c = 9.375(1) Å, β= 108.25(1)° in space group P21, and those for lactitol monohydrate a =7.844(1) Å, b = 12.673(2) Å, c = 15.942(2) Å in space group P212121.

A new titanate K2ZnTiO4 has been synthesized by solid-state reaction. This compound is isostructural with K2ZnGeO4, space group Pca21, Z=8. Unit-cell parameters were determined: a=11.3352(6) Å, b=5.6352(5) Å, c=16.0125(13) Å, and V=1022.8(3) Å3. Powder diffraction data are reported.