Analytical techniques diffraction

Nickel also is deterrnined by a volumetric method employing ethylenediaminetetraacetic acid as a titrant. Inductively coupled plasma (ICP) is preferred to determine very low nickel values (see Trace AND RESIDUE ANALYSIS). The classical gravimetric method employing dimethylglyoxime to precipitate nickel as a red complex is used as a precise analytical technique (122). A colorimetric method employing dimethylglyoxime also is available. The classical method of electro deposition is a commonly employed technique to separate nickel in the presence of other metals, notably copper (qv). It is also used to estabhsh caUbration criteria for the spectrophotometric methods. X-ray diffraction often is used to identify nickel in crystalline form. 

A. Segmuller and M. Murakami. X-Ray Diffraction Analysis of Strains and Stresses in Thin Films. In Analytical Techniques for Thin Films. (K.N. Tu and R. Rosenberg, eds.) Academic, San Diego, 1988, p.l43. 

Applications The general applications of XRD comprise routine phase identification, quantitative analysis, compositional studies of crystalline solid compounds, texture and residual stress analysis, high-and low-temperature studies, low-angle analysis, films, etc. Single-crystal X-ray diffraction has been used for detailed structural analysis of many pure polymer additives (antioxidants, flame retardants, plasticisers, fillers, pigments and dyes, etc.) and for conformational analysis. A variety of analytical techniques are used to identify and classify different crystal polymorphs, notably XRD, microscopy, DSC, FTIR and NIRS. A comprehensive review of the analytical techniques employed for the analysis of polymorphs has been compiled [324]. The Rietveld method has been used to model a mineral-filled PPS compound [325]. 

ABSTRACT The aim of this study was to test portable infrared spectroscopy for non-destructive analysis of ancient construction mortar. Mortar samples from the House of the Vestals, in Pompeii, Italy, were initially examined with traditional analytical techniques, including X-ray fluorescence, X-ray diffraction and thin section analysis. These techniques were used to establish mineralogical and chemical profiles of the samples and to verify the results of experimental field methods. Results showed the lime-based binder was composed of calcite, and the volcanic sand aggregate contained clinopyroxene, plagioclase, sanidine and olivine crystals. 

Z-4A), and zeolite H-ZSM-5. The interlayer distance varied by the intercalation was determined from X-ray diffraction patterns. The interlayer space of the crystalline zeolite is separated by the three-dimensional cage structures. The mean diameters of particles were approximately 1 ym. Such small particles formed very stable suspensions with no sign of sedimentation over the time course of the kinetic measurements. The analytical techniques used to obtain the equilibrium concentration are described elsewhere (10-22). All samples were equilibrated for 24-72 h after preparation. The temperature was controlled at 25 °C. 

Thus, in order to describe adequately any pure substance, its structure must be elucidated. Before the advent of modern analytical techniques, such as X-ray diffraction analysis, structure elucidation was a much more complicated and time-consuming task than the separation and identification of a compound and occupied the life-work of many eminent chemists. 

In this chapter we introduce high resolution diffraction studies of materials, beginning from the response of a perfect crystal to a plane wave, namely the Bragg law and rocking curves. We compare X-rays with electrons and neutrons for materials characterisation, and we compare X-rays with other surface analytic techniques. We discuss the definition and purpose of high resolution X-ray diffraction and topographic methods. We also give the basic theory required for initial use of the techniques. 

The identification of the superconducting phase YBagCug-O7 g provides an example in which knowledge of thermodynamics, i.e. the Gibbs phase rule and the theory of equilibrium phase diagrams coupled with X-ray diffraction techniques led to success. Further, the use of databases that can now be easily accessed and searched on-line provided leads to a preliminary structure determination. The procedures outlined here are among the basic approaches used in solid state chemistry research, but by no means are they the only ones. Clearly the results from other analytical techniques such as electron microscopy and diffraction, thermal... 

An overview of the analytical techniques most frequently used that provide molecular and crystalline structure is illustrated in Scheme 1.8. Basically, they can be grouped into histochemical and immunological methods, diffraction, spectroscopic, spectrometric, chromatographic, and thermoanalytical techniques. 

Quality attributes of food emulsions, such as appearance, stability, and rheology, are strongly influenced by the size of the droplets that they contain (Friberg and Larsson, 1997 McClements, 1999). For example, the creaming stability of an emulsion decreases as droplet size increases. Analytical techniques that provide quantitative information about droplet size are therefore required to aid in the development and production of high-quality emulsion-based food products. A variety of analytical techniques have been developed to measure droplet size, e.g., laser diffraction, electrical pulse counting, sedimentation techniques, and ultrasonic spectrometry (McClements, 1999). These techniques are used for fundamental research, product development, and quality assurance. This unit focuses on the two most commonly used techniques in the food industry, laser diffraction and electrical pulse counting. 

The kinetics of transition from the liquid crystal to the fully ordered crystal of flexible, linear macromolecules was studied by Warner and Jaffe 38) on copolyesters of hydroxybenzoic acid, naphthalene dicarboxylic acid, isophthalic acid, and hydro-quinone. The analytical techniques were optical microscopy, calorimetry and wide angle X-ray diffraction. Despite the fact that massive structural rearrangements did not occur on crystallization, nucleation and growth followed the Avrami expression with an exponent of 2. The authors suggested a rod-like crystal growth. 

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