Powder X-ray diffraction PXRD

Figure C2.17.8. Powder x-ray diffraction (PXRD) from amoriDhous and nanocry stalline Ti02 nanocrystals. Powder x-ray diffraction is an important test for nanocrystal quality. In the top panel, nanoparticles of titania provide no crystalline reflections. These samples, while showing some evidence of crystallinity in TEM, have a major amoriDhous component. A similar reaction, perfonned with a crystallizing agent at high temperature, provides well defined reflections which allow the anatase phase to be clearly identified.

A fascinating study on the surface science of copper hydride on Si02, as well as on AI2O3, ceria (cerium oxide), and ZnO, has appeared [50]. Pure, yet thermally unstable, CuH can be precipitated as a red-brown solid from aqueous cupric sulfate and hypophosphorous acid in the presence of H2SO4, and has been characterized by powder X-ray diffraction (PXRD) (Eq. 5.25). Transmission electron microscopy (TEM) data suggest that it is most stable when deposited on acidic Si02. 

Information on the morphology of polymers is revealed by techniques such as powder X-ray diffraction (PXRD), which is often called wide-angle X-ray scattering (WAXS) by polymer scientists, and small-angle X-ray scattering (SAXS). The crystallites exist in a polymer sample below the melting temperature T, an order-disorder transition, above which a viscous melt is formed. 

The Mg-Al-C03-LDH used as adsorbent and sorbent was prepared with an Mg Al ratio of 2 1 by the coprecipitation method at variable pH [6], The material obtained was characterised by powder X-ray diffraction (PXRD, using a Siemens D-5005 X-ray diffractometer), and elemental and thermal analyses. The material showed the characteristic lamellar structure with a basal spacing of 7.6 A, specific surface area of 87.1 m2 g 1, determined by the N2-BET adsorption isotherm, and an approximate minimum molecular formula [Mg, MAt, (oh) m ](CO, ) 5 2.3 i(h2o) The size distribution and the average size of the LDH particles were determined by light scattering, using a Zetasizer 4 from Malvern. 

There are a number of crystal aspects of the API that should be briefly examined. Knowledge of crystal habit, particle size distribution, surface area, and optical properties are important because these characteristics will affect the stability of all solid dosage forms in excipient compatibility testing (9,10). Although single crystal data may not be available at early formulation stages, predicted data may be available, based on powder x-ray diffraction (PXRD) studies, and should be considered (11). 

I was characterized by powder X-ray diffraction (PXRD), energy dispersive analysis of X-rays (EDAX), chemical analysis, thermogravimetric analysis (TGA) and IR spectroscopy. EDAX analysis indicated the ratio of Mn S to be 3 2. The presence of fluorine was confirmed by analysis and the percentage of fluorine estimated by EDAX in a field emission scanning electron microscope was also satisfactory. Thermogravimetric analysis also confirms the stoichiometry of the compound. Bond valence sum calculations6 and the absence of electron density near fluorine in the difference Fourier map also provide evidence for the presence of fluorine. The sulfate content was found to be 30.8% compared to the expected 32% on the basis of the formula. 

The term Powder X-ray Diffraction (PXRD), as the name implies, is a diffraction pattern obtained by the interaction of X-rays (usually monochromatic) from a collection of crystallites (powder), which are statistically oriented in all possible crystallographic directions satisfying the Bragg condition ... 

Variable-temperature SSNMR was used by Tozuka et to investigate the observed polymorphism in clarithromycin. Polymorphic interconversions were identified using both powder X-ray diffraction (PXRD) and CPMAS NMR. The authors performed quantitation of two polymorphs (forms I and II) using carbonyl resonances that exhibited 1 ppm resolution. Relaxation and CP rate constants were not taken into account instead, relative peak areas were adjusted using a term derived from the preparation and analysis of a known set of standard mixtures. The correlation coefficient of measured peak intensity and weight content was found to be >0.99. 

Examination of the residual solid from solubility samples is one of the most important but often overlooked steps in solubility determinations. Powder X-ray diffraction (PXRD) is the most reliable method to determine whether any solid state form change has occurred during equilibration. The sample should be studied both wet and dry to determine if any hydrate or solvate exists. Thermal analysis techniques such as differential scanning calorimetry (DSC) can also be used to identify any solid-state transformations, although they may not provide as definitive an answer as the PXRD method. Other methods useful in identifying any solid-state changes include microscopy, Raman and infrared spectroscopy, and solid-state NMR (Brittain, 1999). When changes in solid-state properties are identified in solubility studies, it is important to link the new properties to the properties of known crystal forms so the solubility result can be associated with the appropriate crystal form. 

Analysis and spectroscopic study. The elemental analysis was performed with anICP-6000 spectrometer. The precursors crystallization was studied by thermal analysis methods (TG85). The samples were analysed by IR spectroscopy (Nicollet, FTIR-7500) and powder X-ray diffraction (PXRD, DRON-3). The morphology of surface was studied by scanning electron microscopy (SEM) (JEOL, JSM-6100). The density of KTP particles was determined by a sink-float method. Local x-ray analysis was performed using Link ISIS microanalysis system (Si Li detector) mounted on Jeol 2000 FX microscope. Bruker-400 apparatus was used for P, C and H NMR study of precursor solution. The YAG Nd SHG was measured on LS-10 device. 

Powder X-ray diffraction (PXRD), also known as X-ray powder diffraction (XRPD), is a routine method for both the qualitative and quantitative analysis... 

The enantiomer and the racemic compound possess different crystal structures, which correspond to different intermolecular interactions, as mentioned in Sec. 3. Therefore the enantiomer and the racemic compound exhibit different powder x-ray diffraction (PXRD) patterns, different infrared (IR) and Raman spectra, and different solid-state nuclear magnetic resonance (SSNMR) spectra. However, the opposite enantiomers give identical PXRD patterns, and identical IR, Raman, and SSNMR spectra. Consequently, the PXRD patterns and the above spectra of a conglomerate, which is a physical mixture of opposite enantiomers, are identical to that of the pure enantiomers. In contrast, the diffraction pattern and the various corresponding spectra of the racemic compound usually differ significantly from those of the pure enantiomers. Therefore the type of racemate can be easily determined by comparing the diffraction patterns or the various spectra of the racemic species with that of one of the pure enantiomers (Figs. 3 5). The enantiomeric composition in a racemic mixture may be determined by PXRD, or by IR or SSNMR spectroscopy. Quantitative PXRD has been applied to determine the relative... 

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