X-ray powder diffraction, use

Chipera SJ, Bish DL. 2002. FULLPAT a full-pattern quantitative analysis program for X-ray powder diffraction using measured and calculated patterns. J. Appl. Cryst. 35 744-749. 

Shankland, K., David, W. I. E. and Sivia, D. S. (1997). Routine ab initio structure determination of chlorothiazole by X-ray powder diffraction using optimized data collection and analysis strategies. J. Mater. Chem., 1, 569-72. [111]... 

Catalysts were characterized by X-ray powder diffraction, using a Philips PW 1050/81 diffractometer, with Cu Ka as the radiation source. 

Fig. [, Continues X-Ray powder diffraction using Cu Ka radiation source at a scan rate of4 7min.

Smith, D.K., Johnson, G.G., Scheible, A., Wims, A.N., Johnson, J.L., and Uhnan, G. Quantitative X-ray powder diffraction using the full diffraction pattern. Powder Diffr. 2 (1987) 73-77. 

Solid products were examined by X-ray powder diffraction using the Cu K radiation. BET areas were determined by N2 volumetric adsorption at 77 K. Chemical analyses were performed by atomic absorption spectroscopy. 

X-ray powder diffraction studies are perfonned both with films and with counter diffractometers. The powder photograph was developed by P Debye and P Scherrer and, independently, by A W Hull. The Debye-Scherrer camera has a cylindrical specimen surrounded by a cylindrical film. In another commonly used powder... 

The formation of such materials may be monitored by several techniques. One of the most useful methods is and C-nmr spectroscopy where stable complexes in solution may give rise to characteristic shifts of signals relative to the uncomplexed species (43). Solution nmr spectroscopy has also been used to detect the presence of soHd inclusion compound (after dissolution) and to determine composition (host guest ratio) of the material. Infrared spectroscopy (126) and combustion analysis are further methods to study inclusion formation. For general screening purposes of soHd inclusion stmctures, the x-ray powder diffraction method is suitable (123). However, if detailed stmctures are requited, the single crystal x-ray diffraction method (127) has to be used. 

Analysis. Excellent reviews of phosphate analysis are available (28). SoHds characterization methods such as x-ray powder diffraction (xrd) and thermal gravimetric analysis (tga) are used for the identification of individual crystalline phosphates, either alone or in mixtures. These techniques, along with elemental analysis and phosphate species deterrnination, are used to identify unknown phosphates and their mixtures. Particle size analysis, surface area, microscopy, and other standard soHds characterizations are useful in relating soHds properties to performance. SoHd-state nmr is used with increasing frequency. 

Many of the procedures used for technical analysis of aluminum hydroxides are readily available from the major producers of aluminum hydroxides. Phase Composition. Weight loss on ignition (110°—1200°C) can differentiate between pure (34.5% Al(OH)2) ttihydroxides and oxide—hydroxides (15% Al(OH)2). However, distinction between individual ttihydroxides and oxide —hydroxides is not possible and the method is not useful when several phases are present together. X-ray powder diffraction is the most useful method for identifying and roughly quantifying the phase composition of hydroxide products. 

The crystal structures of four chlorinated derivatives of di-benzo-p-dioxin have been determined by x-ray diffraction from diffractometer data (MoKa radiation). The compounds, their formulae, cell dimensions, space groups, the number of molecules per unit cell, the crystallographic B.-factors, and the number of observed reflections are given. The dioxin crystal structures were performed to provide absolute standards for assignment of isomeric structures and have been of considerable practical use in combination with x-ray powder diffraction analysis. 

The films were characterized using x-ray powder diffraction (XRD), x-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The photoelectron spectroscopy utilized a Vacuum Generators ESCA Lab II system with Mg(Ka) radiation. Binding energies (BE) were measured with respect to the surface C(ls) peak (284.5 eV) which was always present In these films. Scanning electron microscopy was done with a JEOL JSM-35C system. 

Materials Characterization. Regarding education in the characterization or analysis of materials—a central topic of materials chemistry—there is a similar hierarchy of importance of subjects that chemistry students (and faculty) will need to have learned. Reference 7 treats this topic systematically, and Roy and Newnham (11) presented a comprehensive (albeit somewhat outdated) presentation of the architecture of materials characterization. Thus Rutherford backscattering and extended X-ray absorption fine structure (EXAFS) are excellent characterization research tools, but in the sequence of tools used every day on every sample, they are insignificant. Thus for structural characterization, X-ray powder diffraction reigns supreme, yet the full power of the modern automated search routines that can be universally applied are taught only to a minuscule fraction of even the materials science student body. 

The presence of triethylenetetramine in the hydrothermal synthesis of open-framework zinc phosphates results in a number of frameworks with one- to three-dimensional structures. The structures include one-dimensional ladders, two-dimensional layer structures, and one structure where the tetramine is bound to the zinc center. The structural type was highly sensitive to the relative concentration of the amine and phosphoric acid.411 Piperazine and 2-methylpiperazine can be used as templating molecules in solvothermal syntheses of zinc phosphates. The crystallization processes of the zinc compounds were investigated by real time in situ measurements of synchrotron X-ray powder diffraction patterns.412... 

The X-ray powder diffraction pattern of miconazole was performed using a Simmons XRD-5000 diffractometer. Figure 1 shows the X-ray powder diffraction pattern of miconazole nitrate, which was obtained on a pure sample of the drug substance. Table 1 shows the values for the scattering angles (26 (°)), the interplanar <7-spacing (A), and the relative intensities (%) observed for the major diffraction peaks of miconazole. 

Arndt and Ahlers [38] used X-ray powder diffraction method for studying the influence of cations on the mode of action of miconazole on yeast cells. The influence of miconazole nitrate on yeast plasma membranes was studied in a concentration range of 0-100 pM. The reaction of 100 pM miconazole with the... 

The X-ray powder diffraction pattern of niclosamide has been measured using a Philips PW-1050 diffractometer, equipped with a single-channel analyzer and using a copper Ka radiation. The pattern obtained is shown in Fig. 1, and the data of scattering angle (degrees 20) and the relative intensities (///max) are found in Table 1. 

The X-ray powder diffraction pattern of (o)-penicillamine was obtained using a Siemens XRD-5000 diffractometer, and the powder pattern is shown in Fig. 1. A summary of the crystallographic data deduced from the pattern of (r>)-penicilla-mine is located in Table 1. 

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