Crystallinity by X-ray diffraction,

Selivanova, Zubova, and Finkel stein [59SEL/ZUB] prepared the salt from silver nitrate and selenic acid. The product was shown to be crystalline by X-ray diffraction. The solubility product of... 

Ag2Se04 was prepared by mixing stoichiometric quantities of silver nitrate and selenic acid. The salt contained 60.04% Ag which is close to the theoretical value of 60.14%. The preparation was shown to be crystalline by X-ray diffraction. The solubility was measured after 15 to 20 days in a thermostat. No increase in solubility was observed between day 15 and day 20. The silver concentration was determined by a tur-bidimetric method. 

The heat of precipitation silver selenate was measured by mixing 0.04241 moles of silver nitrate dissolved in 325 g of water with 0.02122 moles of selenic acid in an isothermal calorimeter equipped with a sensitive thermometer. The acid (7.07 M) was contained initially in a bulb that was broken in order to start the reaction. The Ag2Se04 formed was shown to be crystalline by X-ray diffraction. The water equivalent was determined after each run. The experimental results and the evaluation of the standard enthalpy of formation of Ag2Se04(cr) are shown in Table A-17. 

Ricou P, Pinel E, Juhasz N (2005) Temperature experiments for improved accuracy in the calculation of polyamide-11 crystallinity by X-ray diffraction. In Advances in X-ray analysis, vol 48. International Centre for Diffraction Data, Newtown Square, Pennsylvania, USA, pp 170-175 Roseman S (1972) Carbohydrate transport in bacterial cells. In Holdn LE (ed) Metabolic pathways, vol 6. Academic, London/New York, pp 41-89 Rosenberg E, Ron E (1997) Bioemulsans microbial polymeric emulsifiers. Curr Opin Biotechnol 8 313-316... 

The equimolar copolymer of ethylene and tetrafluoroethylene is isomeric with poly(vinyhdene fluoride) but has a higher melting point (16,17) and a lower dielectric loss (18,19) (see Fluorine compounds, organic-poly(VINYLIDENE fluoride)). A copolymer with the degree of alternation of about 0.88 was used to study the stmcture (20). Its unit cell was determined by x-ray diffraction. Despite irregularities in the chain stmcture and low crystallinity, a unit cell and stmcture was derived that gave a calculated crystalline density of 1.9 g/cm. The unit cell is befleved to be orthorhombic or monoclinic (a = 0.96 nm, b = 0.925 nm, c = 0.50 nm 7 = 96%. 

Crystallinity of polypropylene is usually determined by x-ray diffraction (21). Isotactic polymer consists of heHcal molecules, with three monomer units pet chain unit, resulting in a spacing between units of identical conformation of 0.65 nm (Fig. 2a). These molecules interact with others, or different... 

Properties of PET Molding Resins. The fliU crystal stmcture of poly(ethylene terephthalate) has been estabhshed by x-ray diffraction (134—137). It forms triclinic crystals with one polymer chain per unit cell. The original cell parameters were estabhshed in 1954 (134) and numerous groups have re-examined it over the years. Cell parameters are a = 0.444 nm, b = 0.591 nm, and c = 1.067 nm a = 100°, (3 = 117°, and 7 = 112° and density = 1.52 g/cm. One difficulty is determining when crystallinity is fliUy developed. PET has been aimealed at up to 290°C for 2 years (137). 

The value for the heat of fusion of PPS, extrapolated to a hypothetical 100% crystalline state, is not agreed upon in the literature. Reported values range from approximately 80 J/g (19 cal/g) (36,96,101) to 146 J/g (35 cal/g) (102), with one intermediate value of 105 J/g (25 cal/g) (20). The lower value, 80 J/g, was originally measured by thermal analysis and then correlated with a measure of crystallinity deterrnined by x-ray diffraction (36). The value of 146 J/g was deterrnined independendy on uniaxiaHy oriented PPS film samples by thermal analysis, density measurement via density-gradient column, and the use of a calculated density for 100% crystalline PPS to arrive at a heat of fusion for 100% crystalline PPS (102). The value of 105 J/g was obtained by measuring the heats of fusion of weU-characterized linear oligomers of PPS and extrapolation to infinite molecular weight. 

Amorphous silica, ie, silicon dioxide [7631-86-9] Si02, does not have a crystalline stmcture as defined by x-ray diffraction measurements. Amorphous silica, which can be naturally occurring or synthetic, can be either surface-hydrated or anhydrous. Synthetic amorphous silica can be broadly divided into two categories of stable materials (1) vitreous silica or glass (qv), which is made by fusing quart2 at temperatures greater than approximately 1700°C (see Silica, vitreous silica), and microamorphous silica, which is discussed herein. 

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). 

Crystallization and Melting Point. The abihty of PVA to crystallize is the single most important physical property of PVA as it controls water solubiUty, water sensitivity, tensile strength, oxygen barrier properties, and thermoplastic properties. Thus, this feature has been and continues to be a focal point of academic and industrial research (9—50). The degree of crystallinity as measured by x-ray diffraction can be directly correlated to the density of the material or the swelling characteristic of the insoluble part (Fig. 2). 

Barium can also be deterruined by x-ray fluorescence (XRF) spectroscopy, atomic absorption spectroscopy, and flame emission spectroscopy. Prior separation is not necessary. XRF can be appHed directly to samples of ore or products to yield analysis for barium and contaminants. AH crystalline barium compounds can be analy2ed by x-ray diffraction. 

The geometries of oxiranes have been determined mainly by X-ray diffraction on crystalline natural products, the oxirane ring being widespread in nature (Section 5.05.5.3). However, the detailed structure of the parent compound (Figure 1) has been secured by microwave spectroscopy and electron diffraction studies (64HC(l9-l)l). The strain in this... 

X-ray studies indicate that the vinyl chloride polymer as normally prepared in commercial processes is substantially amorphous although some small amount of crystallinity (about 5% as measured by X-ray diffraction methods) is present. It has been reported by Fuller d in 1940 and Natta and Carradini in 1956 that examination of the crystalline zones indicates a repeat distance of 5.1 A which is consistent with a syndiotactic (i.e. alternating) structure. Later studies using NMR techniques indicate that conventional PVC is about 55% syndiotactic and the rest largely atactic in structure. 

The formation of acyl halide-Lewis acid complexes have been observed by several methods. For example, both 1 1 and 1 2 complexes of acetyl chloride, with AICI3 can be observed by NMR spectroscopy. The existence of acylium ions has been demonstrated by X-ray diffraction studies on crystalline salts. For example, crystal structure determinations have been reported for /i-methylphenylacylium and acetylium ions as SbFg salts. There is also a good deal of evidence from NMR measurements which demonstrates that acylium ions can exist in nonnucleophilic solvents. " The positive charge on acylium ions is delocalized onto the oxygen atom. This delocalization is demonstrated in particular by the short O—C bond lengths in acylium ions, which imply a major contribution from the structure having a triple bond ... 

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... 

Polyester fibers contain crystalline as well as noncrystalline regions. The degree of crystallinity and molecular orientation are important in determining the tensile strength of the fiber (between 18-22 denier) and its shrinkage. The degree of crystallinity and molecular orientation can be determined by X-ray diffraction techniques. ... 

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