X-ray diffraction units

Model 12045 x-ray diffraction unit, Philips Electronic Instruments Co., Mount Vernon, NY. 

This is defined as the ratio of the mass of a collection of discrete pieces of solid to the sum of the volumes of each piece, if the solid has an ideal regular arrangement at the atomic level. Theoretical volumes are determined from x ray diffraction unit cell measurements, so this density is also known as the x-ray or unit cell density. Ideal volumes are of little use in catalysis, and this term has hardly any applicability. 

Bulk characterization tools. The formation of nanostructured AIN powders have been confirmed by FT-IR spectroscopy (Nicolet 60SX), Raman spectrometry (Dilor microprobe). X-ray diffraction (XRD) (Norelco X-ray diffraction unit with wide range goniometer), and transmission electron microscopy (TEM), along with the corresponding electron diffraction in a JEOL 200CX microscope. 

The chemical analysis of the sample was accomplished by using an atomic absorption spectrophotometer or digital photometer and wet chemical methods (Table 5). X-Ray diffraction studies on the sample were undertaken using a Philips X-Ray diffraction unit. The particle size distribution of the sample was measured by using a Sedigraph (5000D Micrometries). The photographs of the samples were taken with an optical microscope (Olympus BH2-IMA). 

Rosalind Franklin (1920-1958) was born in London. She graduated from Cambridge University and studied X-ray diffraction techniques in Paris. In 1951 she returned to England and accepted a position to develop an X-ray diffraction unit in the biophysics... 

A convenient procedure for obtaining the x-ray powder pattern of the active adrenal steroids involves the use of a Debye-Scherrer camera in a standard x-ray diffraction unit, employing a nickel filter and copper radiation. 

The X-ray diffraction patterns were obtained by means of a General Electric X-ray diffraction unit, model XRD-6, using Ni filtered CuK radiation. 

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%. 

Poly(vinyl fluoride) [24981-14-4] (PVF) is a semicrystaltiae polymer with a planar, zig-zag configuration (50). The degree of crystallinity can vary significantly from 20—60% (51) and is thought to be primarily a function of defect stmctures. Wide-line nmr and x-ray diffraction studies show the unit cell to contain two monomer units and have the dimensions of a = 0.857 nm, b = 0.495 nm, and c = 0.252 nm (52). Similarity to the phase I crystal form of poly (vinytidene fluoride) suggests an orthorhombic crystal (53). 

Glass-forming systems other than siUca have been examined. The fraction of three- and four-coordinated boron in borate glasses can be determined by nmr (29). Both nmr and x-ray diffraction (30) results led to the suggestion that the boroxyl ring is the stmctural unit of vitreous The... 

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). 

Specific optical rotation values, [a], for starch pastes range from 180 to 220° (5), but for pure amylose and amylopectin fractions [a] is 200°. The stmcture of amylose has been estabUshed by use of x-ray diffraction and infrared spectroscopy (23). The latter analysis shows that the proposed stmcture (23) is consistent with the proposed ground-state conformation of the monomer D-glucopyranosyl units. Intramolecular bonding in amylose has also been investigated with nuclear magnetic resonance (nmr) spectroscopy (24). 

The monolayer resulting when amphiphilic molecules are introduced to the water—air interface was traditionally called a two-dimensional gas owing to what were the expected large distances between the molecules. However, it has become quite clear that amphiphiles self-organize at the air—water interface even at relatively low surface pressures (7—10). For example, x-ray diffraction data from a monolayer of heneicosanoic acid spread on a 0.5-mM CaCl2 solution at zero pressure (11) showed that once the barrier starts moving and compresses the molecules, the surface pressure, 7T, increases and the area per molecule, M, decreases. The surface pressure, ie, the force per unit length of the barrier (in N/m) is the difference between CJq, the surface tension of pure water, and O, that of the water covered with a monolayer. Where the total number of molecules and the total area that the monolayer occupies is known, the area per molecules can be calculated and a 7T-M isotherm constmcted. This isotherm (Fig. 2), which describes surface pressure as a function of the area per molecule (3,4), is rich in information on stabiUty of the monolayer at the water—air interface, the reorientation of molecules in the two-dimensional system, phase transitions, and conformational transformations. 

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 ... 

For a two-dimensional array of equally spaced holes the difftaction pattern is a two-dimensional array of spots. The intensity between the spots is very small. The crystal is a three-dimensional lattice of unit cells. The third dimension of the x-ray diffraction pattern is obtained by rotating the crystal about some direction different from the incident beam. For each small angle of rotation, a two-dimensional difftaction pattern is obtained. 

In principle, it is possible to calculate the detailed three-dimensional electron density distribution in a unit cell from the three-dimensional x-ray diffraction pattern. 

Crystal Structure. Diamonds prepared by the direct conversion of well-crystallized graphite, at pressures of about 13 GPa (130 kbar), show certain unusual reflections in the x-ray diffraction patterns (25). They could be explained by assuming a hexagonal diamond stmcture (related to wurtzite) with a = 0.252 and c = 0.412 nm, space group P63 /mmc — Dgj with four atoms per unit cell. The calculated density would be 3.51 g/cm, the same as for ordinary cubic diamond, and the distances between nearest neighbor carbon atoms would be the same in both hexagonal and cubic diamond, 0.154 nm. 

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