Diffractometry, x-ray

X-ray diffractometry (XRD), the most widely used X-ray diffraction technique in materials characterization, was originally used for examining the crystal structure of powder samples thus, traditionally it is called X-ray powder diffractometry. In fact, polycrystalline aggregate 

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The structure of PP-g-polystyrene was studied by wide and narrow angle x-ray diffractometry. The polystyrene component formed discrete amorphous structures, which were identified after chloromethylation [143]. Structure of Rayon-Styrene graft copolymer was characterized by IR, wide angle x-ray, and SEM, grafting occurred mainly in the amorphous regions of rayon [1441. 

Person, A., Bocherens, H., Saliege, J.-F, Paris, F., Zeitoun, V. and Gerard, M. 1995 Early diagenetic evolution of bone phosphate an x-ray diffractometry analysis. Journal of Archaeological Science 22. 211-221. 

Suhtnicion nickel powders luive been synthesized successfully from aqueous NiCh at various tempmatuTKi and times with ethanol-water solvent by using the conventional and ultrasonic chemical reduction method. The reductive condition was prepared by flie dissolution of hydrazine hydrate into basic solution. The samples synthesized in various conditions weae claractsiz by the m ins of an X-ray diffractometry (XRD), a scanning electron microscopy (SEM), a thermo-gravimetry (TG) and an X-ray photoelectron spectroscopy (XPS). It was found that the samples obtained by the ultrasonic method were more smoothly spherical in shape, smaller in size and narrower in particle size distribution, compared to the conventional one. 

Bulk characterization of calcined precursors and reduced catalysts was carried out by X-ray diffractometry using Cu K radiation. Reduced catalysts were first passivated by exposure to N2O as described above. Line-broadening analysis was carried out on the Fe(llO) reflection to obtain the iron particle size. Overlap with the MgO(200) reflection limited its usefulness to the more highly-loaded catalysts. 

In the cements of this type a number of phases are known to be present. For example, in the zinc oxychloride cement two discrete phases, corresponding to the composition ZnO. ZnCl. H O in the ratios 4 1 5 and 1 1 2 respectively, are known to occur (Sorrell, 1977). Similarly, in the magnesium oxychloride cement, phases corresponding to Mg(OH)a. MgClj. HjO in the ratios 5 1 8 and 3 1 8 have been shown to exist and have been studied by X-ray diffractometry (Sorrell Armstrong, 1976). 

Detailed TEM investigations as well as small-angle X-ray diffractometry show the clusters organized via their edges, as is indicated in Figure 17b. 

The boron nitride obtained in this study was characterized by infrared spectroscopy, powder x-ray diffractometry and transmission electron microscopy. Trace elemental analyses were also performed by energy dispersive x-ray analysis and carbon arc emission spectroscopy. Representative spectra are displayed in Figures 2-4. 

In this paper we present results from independent studies on the stage 2 to stage 1 transition area that show some unexpected features (anomalies). The results are obtained by electrochemical impedance spectroscopy (EIS), entropy measurements (AS(x)) and in situ x-ray diffractometry (XRD). The aim is to understand the mechanism of stage transition dealing with the observed anomalies. 

X-ray powder patterns can be obtained using either a camera or a powder diffractometer. Currently, diffractometers find widespread use in the analysis of pharmaceutical solids. The technique is usually nondestructive in nature. The theory and operation of powder diffractometers is outside the purview of this chapter, but these topics have received excellent coverage elsewhere [1,2]. Instead, the discussion will be restricted to the applications of x-ray powder diffractometry (XPD) in the analysis of pharmaceutical solids. The U.S. Pharmacopeia (USP) provides a brief but comprehensive introduction to x-ray diffractometry [3],... 

II, and III), two were monohydrates (termed a-monohydrate and /3-monohydrate) and one was a ferf-butylamine disolvate. The differences in the powder patterns of the phases were readily evident (Table 1). This study demonstrates the unique ability of x-ray diffractometry for the identification of (1) anhydrous compound existing in both crystalline and amorphous states, (2) different polymorphic forms of the anhydrate, (3) the existence of solvates where the solvent of crystallization is water (hydrate) or an organic solvent (in this case, /m-butylamine), and (4) polymorphism in the hydrate. 

Depending on the water vapor pressure, cephalexin can exist as an anhydrate (C16Hi7N304S), a monohydrate (C16H17N304S H20) or a dihydrate (C16H17N304S 2H20) at 25°C [10]. The monohydrate and the dihydrate were characterized by the pronounced differences in their powder x-ray diffraction patterns. Thus, x-ray diffractometry can be used to characterize several hydrated states of a compound. 

The /3-polymorphic form of anhydrous carbamazepine is official in the USP [3], The USP stipulates that, The X-ray diffraction pattern conforms to that of USP Carbamazepine Reference Standard, similarly determined. No limits have been set in the USP for the other polymorphs of anhydrous carbamazepine. Although several polymorphic forms of anhydrous carbamazepine have been reported, only the a- and /3-forms have been extensively studied and characterized [49]. A comparison of the powder x-ray diffraction patterns of these two forms revealed that the 10.1 A line (peak at 8.80° 26) was unique to a-carbamazepine, and so this line was used for the analysis (Fig. 5). It was possible to detect a-carbamazepine in a mixture where the weight fraction of a-carbamazepine was 0.02 at a signal-to-noise ratio of 2. Much greater sensitivity of this technique has been achieved in other systems. While studying the polymorphism of l,2-dihydro-6-neopentyl-2-oxonicotinic acid, Chao and Vail [50] used x-ray diffractometry to quantify form I in mixtures of forms I and II. They estimated that form I levels as low as 0.5% w/w can be determined by this technique. Similarly the a-inosine content in a mixture consisting of a- and /3-inosine was achieved with a detection limit of 0.4% w/w for a-inosine [51]. 

In x-ray diffractometry, quantitative analyses of mixtures of phases usually requires that at least one high-intensity peak unique to each of the phases be available for intensity measurement. Organic pharmaceutical compounds, how-... 

The mechanism of adsorption of drugs by montmorillonite has been studied using infrared (IR) spectroscopy and XPD [68,69]. X-ray diffractometry and a host of other techniques were used to study the interaction of bovine serum albumin with the surface of a microcrystalline aluminum oxide hydroxide compound [70]. 

Another characteristic point is the special attention that in intermetallic science, as in several fields of chemistry, needs to be dedicated to the structural aspects and to the description of the phases. The structure of intermetallic alloys in their different states, liquid, amorphous (glassy), quasi-crystalline and fully, three-dimensionally (3D) periodic crystalline are closely related to the different properties shown by these substances. Two chapters are therefore dedicated to selected aspects of intermetallic structural chemistry. Particular attention is dedicated to the solid state, in which a very large variety of properties and structures can be found. Solid intermetallic phases, generally non-molecular by nature, are characterized by their 3D crystal (or quasicrystal) structure. A great many crystal structures (often complex or very complex) have been elucidated, and intermetallic crystallochemistry is a fundamental topic of reference. A great number of papers have been published containing results obtained by powder and single crystal X-ray diffractometry and by neutron and electron diffraction methods. A characteristic nomenclature and several symbols and representations have been developed for the description, classification and identification of these phases. 

The diffusion layers obtained in specimens were investigated by means of metallography, electron microscopy, microhardness test. X-ray diffractometry and Mossbauer spectroscopy. 

The amorphous state of the lyophilized solids was verified by powder X-ray diffractometry (Rigaku Denki Co., Ltd., Danvers, MA), and their Ca/P04 ratios after dissolution in HCl were determined by atomic absorption (AAS, Perkin Elmer, Norwalk, CT) and UV spectrophotometric [6] (Varian Analytical Instruments, Palo Alto, CA) measurements of Ca + and PO4, respectively. Dissolution of the ACP fillers was studied by kinetically following the changes in Ca + and PO4 concentrations in continuously stirred HEPES-buffered (pH = 7.4) solutions adjusted to 240 mOsm/kg with NaCl at 37°C. All solutions initially contained 0.8 mg/mL of the ACP filler. 

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