Synchrotron X-ray powder diffraction (XRPD) data were collected for the silver(I)-aspartame complex [Ag(C14H17N2O5)]∙1∕2H2O. The complex was obtained from a stoichiometric mixture of aspartame (3-amino-N-(α-carboxyphenethyl)-succinamic acid N-methyl ester, C14H18N2O5), Na2CO3, and AgNO3. Indexing using Crysfire and Chekcell proposed an orthorhombic unit cell with space group P2221. The lattice parameters are a=12.4750(1) Å, b=21.60614(14) Å, and c=4.88888(9) Å.

Two different approaches for studying sample’s contributions to diffraction-line broadening are analyzed by applying them to several nickel hydroxide samples. Both are based in the refinement of powder diffraction data but differ in the microstructural model used. The first one consists in the refinement of the powder diffraction pattern using the FAULTS program, a modification of DIFFaX, which assigns peak broadening mainly to the presence of stacking faults and treats finite size effects by convolution with a Voigt function. The second method makes use of the program FULLPROF, which allows the use of linear combinations of spherical harmonics to model peak broadening coming from anisotropic size effects. The complementary use of transmission electron microscopy has allowed us to evaluate the best approach for the Ni(OH)2 case. In addition, peak shifts, corresponding to reflections 10l (l≠0) were observed in defective nickel hydroxide samples that can be directly correlated with the degree of faulting.

The ternary nitridotungstate Li6WN4 has been synthesized via the solid state reaction of lithium subnitride, Li3N, with W under nitrogen. High quality X-ray powder diffraction data were collected for the crystal-structure determination. Li6WN4 crystallizes in the tetragonal system, space group P42∕nmc, with cell parameters a=6.6759(3) Å and c=4.9280(3) Å, Z=2. Preliminary thermal stability measurements of Li6WN4 show that it is sensitive to moisture, even at room temperature, and decomposes at high temperatures below 1000 °C under flowing nitrogen.

X-ray diffraction investigations of two phenol derivatives - 2,2′-Thiobis(4-methyl-6-tert-butylphenol) and 2,2′-Methylenebis(4-methyl-6-tert-butylphenol) were carried out. Both compounds at room temperature have similar cell volume and the same number of molecules in an unit cell. However, 2,2′-Thiobis(4-methyl-6-tert-butylphenol) crystallizes in the monoclinic system with unit cell parameters refined to a=0.8278(2) nm, b=1.2968(4) nm, c=1.9493(7) nm, β=90.93(2)°, space group P21∕n(14), whereas 2,2′-Methylenebis(4-methyl-6-tert-butylphenol) crystallizes in the orthorhombic system with unit cell parameters refined to a=1.6203(5) nm, b=1.2827(5) nm, c=1.0197(3) nm, space group Pna21(33). The investigated C22H30O2S turned out to be a new polymorph of 2,2′-Thiobis(4-methyl-6-tert-butylphenol).

Ab initio crystal structure solution by powder diffraction data is based on the experimental full pattern decomposition process: the resulting structure factor moduli are used for direct phasing. The extracted intensity estimates are scarcely accurate (overlapping, background, and preferred orientation are the main causes of the lack of accuracy), no matter if Le Bail or Pawley method is adopted: consequently the structure solution process is not straightforward. We have focused our attention on the relation between the efficiency of the EXPO2004 phasing process and the various parameters which are normally used in the full pattern decomposition process, e.g., the peak shape function, the number of refinement cycles, the degree of overlapping. Different steps of the phasing process are considered: the definition of the unit cell, the determination of the space group, and the application of direct methods.

X-ray powder diffraction data for Mo2.85Al1.91Si4.81 are reported. The new Mo2.85Al1.91Si4.81 compound was successfully prepared using the self-propagating high-temperature synthesis (SHS) technique. The starting atomic mixture of reactant powders was Mo+2(1−x)Si+2xAl with x=0.3. The final powder compound obtained by the SHS technique was determined to be Mo2.85Al1.91Si4.81 by ICP-AES. X-ray powder diffraction pattern of Mo2.85Al1.91Si4.81 was recorded using an X-ray powder diffractometer, Cu Kα radiation, and analyzed by automatic indexing programs. Mo2.85Al1.91Si4.81 was found to be hexagonal with a=4.6929(2) Å and c=6.5515(4) Å. The XRD results are in good agreement with those of Mo2.85Ga2Si4.15.

The solid-state phase transitions of the KNO3–NH4NO3 solid solutions have been determined by high temperature X-ray diffractometry, and lattice parameter calculation has also been performed. Ammonium nitrate (AN) is of great use for gas generators of automobile air bag systems. The X-ray diffraction results showed the single (AN) phase III from 5% to 20% KNO3 in NH4NO3 and up to 373 K, which is the important temperature range for the air bag gas generator applications. The X-ray diffraction patterns of the low temperature KNO3 phase (KN II) are from 92% to 100% KNO3 composition range and up to 393 K temperature. The high temperature KNO3 phase (KN I) showed very broad composition range from 20% up to 100% KNO3 at various temperature ranges. The lattice parameters of the NH4NO3-rich (AN III) and KNO3-rich (KN II and KN I) solid solutions have been calculated at different temperature range. The volumes of AN III phase decrease from 0.3201(4) to 0.3166(1) nm3 at room temperature and from 0.3250(6) to 0.3215(3) nm3 at 373 K as the compositions increase from 5% to 20% KNO3. The lattice constants of the hexagonal KN I phase show that there is no significant change in a direction when the temperature increases. Details of X-ray results, lattice expansions, and equations during heating are presented.

Crystal structure and phase transformation behaviors in two Ni-Mn-Ga ferromagnetic shape memory alloys (FSMAs) with compositions of Ni48Mn30Ga22 and Ni53Mn25Ga22 (at. %) as a function of temperature were investigated by in situ neutron diffraction experiments. Neutron diffraction technique proves to be highly efficient in characterizing structural transformation in Ni-Mn-Ga FSMAs, which consist of nearby elements in the periodic table. Our neutron results show that Ni48Mn30Ga22 has a cubic, L21 Heusler structure from 373 to 293 K. Its crystal structure changes into a seven-layered orthorhombic martensitic structure when cooled to 243 K, and no further transformation is observed upon cooling to 19 K. Neutron diffraction results also show that Ni53Mn25Ga22 has a tetragonal I4/mmm martensitic structure from 20 to 403 K. A pre-transformation around room temperature is observed from an abrupt jump in unit-cell volume of Ni53Mn25Ga22, which corresponds with an endothermic peak detected in a heated DSC curve.

Total reflection X-ray fluorescence analysis (TXRF) is an established technique for trace element analysis in various sample types. Restricted in the past to expensive large-scale systems, in this study the capability of a benchtop system for trace element analysis is reported. By analysing various heavy metals in raw and digested sewage as well as mercury in recycling glass, the suitability of the TXRF system for these kinds of applications could be proven. Based on this data, the benefits, disadvantages, and restrictions of the benchtop system in comparison to other trace element techniques like inductively coupled plasma optical emission spectroscopy (ICP-OES) and atomic adsorption spectroscopy (AAS) are evaluated.

X-ray powder diffraction was used to analyze and evaluate 11 samples of traditional Chinese medicine, Costustoot, found at various locations in China. A reference fingerprint pattern with 48 characteristic peaks for Costustoot was obtained from X-ray diffraction patterns of six Costustoots from the rhizomes of Aucklandia lappa Decne. The reference fingerprint pattern with 48 characteristic peaks for Costustoot was then used to evaluate the remaining five Costustoot materials. X-ray diffraction results show that the X-ray diffraction Fourier fingerprint pattern method can be used for rapid classification, identification, and quality control of Costustoots.