Ray Diffraction Analysis

A fiber-diffraction pattern is recorded on a flat-film camera in which the fiber-to-photographic film distance is typically in the range of 3 to 4 cm. During exposure to X-rays, the specimen chamber is continuously flushed with a slow and steady stream of helium gas that has been bubbled through a saturated salt solution so that (a) the fiber is maintained at a constant desired r.h. and (b) fogging of the photographic film from air scattering is reduced. 

X-rays. The diffraction from this polycrystalline and disoriented fiber is the sum of the diffraction from all the randomly oriented microcrystallites, and it corresponds to a series of concentric rings, each with its characteristic (/-spacing. The intensity is uniform on a ring, but it varies among rings. This type of diffraction, commonly referred to as a powder pattern, is prevalent among minerals and polymers that have a low degree of polymerization. 

(continued)—(b) an assembly of randomly oriented microcrystallites (left) diffracts to produce a series of concentric rings (right) (c) an assembly of partially oriented blocks of microcrystallites (left) diffracts to produce large arcs (right). 

When the fiber is stretched, longer blocks of unit cells might be facilitated, as shown in Fig. 2c. This falls under the second category, as the orientation of the large microcrystallites is no longer random, but somewhat tempered, Consequently, circles are trimmed down to arcs in the diffraction pattern in response to enhancement in orientation. 

The third category, shown in Fig. 2d, results when all of the long molecules or microcrystallites are aligned along the fiber axis, but they aggregate with little lateral ordering. This assembly, called an oriented fiber, diffracts to produce a series of layer lines that are perpendicular to the fiber axis. The intensity is nonuni- 

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X-Ray Methods. In x-ray fluorescence the sample containing mercury is exposed to a high iatensity x-ray beam which causes the mercury and other elements ia the sample to emit characteristic x-rays. The iatensity of the emitted beam is directly proportional to the elemental concentration ia the sample (22). Mercury content below 1 ppm can be detected by this method. X-ray diffraction analysis is ordinarily used for the quaUtative but not the quantitative determination of mercury. 

Crystallinity. Generally, spider dragline and silkworm cocoon silks are considered semicrystalline materials having amorphous flexible chains reinforced by strong stiff crystals (3). The orb web fibers are composite materials (qv) in the sense that they are composed of crystalline regions immersed in less crystalline regions, which have estimates of 30—50% crystallinity (3,16). Eadier studies by x-ray diffraction analysis indicated 62—65% crystallinity in cocoon silk fibroin from the silkworm, 50—63% in wild-type silkworm cocoons, and lesser amounts in spider silk (17). 

Chain Structure. The chemical composition of poly (vinyhdene chloride) has been confirmed by various techniques, including elemental analysis, x-ray diffraction analysis, degradation studies, and in, Raman, and nmr spectroscopy. The polymer chain is made up of vinyhdene chloride units added head-to-tail ... 

A progressive etching technique (39,40), combined with x-ray diffraction analysis, revealed the presence of a number of a polytypes within a single crystal of sihcon carbide. Work using lattice imaging techniques via transmission electron microscopy has shown that a-siUcon carbide formed by transformation from the P-phase (cubic) can consist of a number of the a polytypes in a syntactic array (41). 

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. 

Another major difference between the use of X rays and neutrons used as solid state probes is the difference in their penetration depths. This is illustrated by the thickness of materials required to reduce the intensity of a beam by 50%. For an aluminum absorber and wavelengths of about 1.5 A (a common laboratory X-ray wavelength), the figures are 0.02 mm for X rays and 55 mm for neutrons. An obvious consequence of the difference in absorbance is the depth of analysis of bulk materials. X-ray diffraction analysis of materials thicker than 20—50 pm will yield results that are severely surface weighted unless special conditions are employed, whereas internal characteristics of physically large pieces are routinely probed with neutrons. The greater penetration of neutrons also allows one to use thick ancillary devices, such as furnaces or pressure cells, without seriously affecting the quality of diffraction data. Thick-walled devices will absorb most of the X-ray flux, while neutron fluxes hardly will be affected. For this reason, neutron diffraction is better suited than X-ray diffraction for in-situ studies. 

Garavito, R. M., et al., 1983. X-ray diffraction analysis of matrix porin, an integral membrane protein from Escherichia coli outer membrane. Journal of Nlolecular Biology 164 313—327. 

Except for Ceo, lack of sufficient quantities of pure material has prevented more detailed structural characterization of the fullerenes by X-ray diffraction analysis, and even for Ceo problems of orientational disorder of the quasi-spherical molecules in the lattice have exacerbated the situation. At room temperature Cgo crystallizes in a face-centred cubic lattice (Fm3) but below 249 K the molecules become orientationally ordered and a simple cubic lattice (Po3) results. A neutron diffraction analysis of the ordered phase at 5K led to the structure shown in Fig. 8.7a this reveals that the ordering results from the fact that... 

Figure 8.11 (a) Stmeture of C6oOs04(NCsH4Bu )2 as determined by X-ray diffraction analysis, (b) A sehematie representation of the stmeture. 

The product is a black-brown solid that is very sensitive to oxygen. The same cation can be obtained by oxidation of S4N4 with AsFs and is unusual in being the only sulfur-nitrogen (paramagnetic) radical that has been obtained as a stable crystalline salt. X-ray diffraction analysis shows the structure to be a planar 5-membered ring with approximate... 

X-Ray diffraction analysis of phthaleine and sulfophthaleine pigments 97YZ764. 

The solid state structure of 3-methyl- and 3-phenyl-4-hydroxy-2-oxo-2/7-pyrido[2,l-Z)]-[l,3]oxazinium inner salts were established by X-ray diffraction analysis (00JCS(P2)2096). The amide type N(5)-C(4)0 bonds are... 

The relative stereostructure of 9-acetyl-7-hydroxy-l,2-dimethyl-7-meth-oxycarbonyl-4-phenyl-6-oxo-l, 4,7,8-tetrahydro-6/7-pyrido[l, 2-u]pyri-midine-3-carboxylate 122 was justified by an X-ray diffraction analysis (97JOC3109). The stereochemistry and solid state structure of racemic trans-6,9-//-l, 6-dimethyl-9 z-ethoxy-9-hydroxy-4-oxo-l,6,7,8,9,9 z-hexahydro-4//-pyrido[l,2- z]pyrimidine-3-carboxylate (123), adopting a cw-fused conformation, were determined by X-ray investigations (97H(45)2175). 

The solid state structure of (3>S,8 Sj-10-(8-amino-6-azaspiro[3,4]octan-6-yl)-9-fluoro-3-methyl-7-oxo-2,3-dihydro-7//-pyrido[l,2,3-dfe]-l,4-benzoxa-zine-6-carboxylic acid (218) was determined by X-ray diffraction study (98CPB1710). The structure of 6,10-dihydropyrido[2,l-c][l,4]benzoxazine-6,10-dione 219 was established by X-ray diffraction analysis. It contains a crystal solvate with /j-xylene (99MI40). 

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