X-ray diffraction crystallinity

The authors reacted Na2Se03(cr) with a copper sulphate solution in an electrically calibrated calorimeter and measured the enthalpy change of the reaction. The product was CuSe03-2H20(cr) as shown by chemical analysis and X-ray diffraction. Crystalline anhydrous copper selenite was also prepared and the integral enthalpies of dissolution of the two selenites in 8% HMO3 (HNO3, aq 1 40, and denoted sin below) were determined. The data have been used in Table A-45 to calculate standard enthalpies of formation of the copper selenites. 

X-ray diffraction Crystallinity and phase identification, averaged microstructural information Transformation from amorphous to crystalline during firing experiments can be performed in situ... 

X-ray diffraction Crystalline regions very specific in that plane normal directions determined Complete characterisation —any orientation function can be calculated Background scattering can be difficult to estimate... 

This chapter opens with a description of the packing of polymer molecules in crystals. X-ray diffraction gives an extremely precise description of this, since the polymer lattice diffracts X-rays as does any other three-dimensional lattice. The shape and mutual arrangement of the minute crystals are then described. The crystals are separated one from another by amorphous regions whose dimensions are comparable to those of the crystals. The information on these matters stems from electron and light microscopy, techniques which are less precise than X-ray diffraction. Crystalline synthetic polymers are invariably partly crystalline and partly amorphous the term crystalline polymer always implies partially crystalline. 

The advantage of using IR spectroscopy for measuring orientation in polymers is that it can detect the orientation of the geometric isomers in the disordered or amorphous regions, as well as the orientation of the preferred isomer found in the ordered or crystalline phase, because they generally appear as separate IR bands. The other experimental techniques such as X-ray diffraction (crystalline phase only) and refractive index (crystalline and amorphous phases) cannot easily separate the contributions of the separate phases. This attribute of IR dichroism is particularly important in multiphase systems [24] and blends [25]. 

There is a fair amount of work reported with films at the mercury-air interface. Rice and co-workers [107] used grazing incidence x-ray diffraction to determine that a crystalline stearic acid monolayer induces order in the Hg substrate. Quinone derivatives spread at the mercury-n-hexane interface form crystalline structures governed primarily by hydrogen bonding interactions [108]. 

Because x-rays are particularly penetrating, they are very usefiil in probing solids, but are not as well suited for the analysis of surfaces. X-ray diffraction (XRD) methods are nevertheless used routinely in the characterization of powders and of supported catalysts to extract infomration about the degree of crystallinity and the nature and crystallographic phases of oxides, nitrides and carbides [, ]. Particle size and dispersion data are often acquired with XRD as well. 

The first analytical tool to assess tire quality of a zeolite is powder x-ray diffraction. A collection of simulated powder XRD patterns of zeolites and some disordered intergrowths togetlier witli crystallographic data is available from tlie IZA [4o]. Phase purity and x-ray crystallinity, which is arbitrarily defined as tlie ratio of tlie intensity of... 

Figure C2.17.8. Powder x-ray diffraction (PXRD) from amoriDhous and nanocry stalline Ti02 nanocrystals. Powder x-ray diffraction is an important test for nanocrystal quality. In the top panel, nanoparticles of titania provide no crystalline reflections. These samples, while showing some evidence of crystallinity in TEM, have a major amoriDhous component. A similar reaction, perfonned with a crystallizing agent at high temperature, provides well defined reflections which allow the anatase phase to be clearly identified.

Present day techniques for structure determination in carbohydrate chemistry are sub stantially the same as those for any other type of compound The full range of modern instrumental methods including mass spectrometry and infrared and nuclear magnetic resonance spectroscopy is brought to bear on the problem If the unknown substance is crystalline X ray diffraction can provide precise structural information that m the best cases IS equivalent to taking a three dimensional photograph of the molecule... 

Figure 4.7c illustrates how x-ray diffraction techniques can be applied to the problem of evaluating 6. If the intensity of scattered x-rays is monitored as a function of the angle of diffraction, a result like that shown in Fig. 4.7c is obtained. The sharp peak is associated with the crystalline diffraction, and the broad peak, with the amorphous contribution. If the area A under each of the peaks is measured, then... 

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). 

A left-handed double-heUcal stmcture has been proposed for geUan in the crystalline state, based on x-ray diffraction studies (227). The presence of acetyl groups presumably dismpts interchain aggregation, since these groups are postulated to be on the outside of the heUces. The role played by acetyl and glyceryl ester groups and their influence on the double-heUcal stmcture has been studied using computet models (232). 

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. 

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. 

---