Microscopical observation

There are a number of complications in the experimental measurement of the electrophoretic mobility of colloidal particles and its interpretation see Section V-6F. TTie experiment itself may involve a moving boundary type of apparatus, direct microscopic observation of the velocity of a particle in an applied field (the zeta-meter), or measurement of the conductivity of a colloidal suspension. 

Zernike F 1942 Phase contrast, a new method for the microscopic observation of transparent objects I Physica 9 686... 

Jaklevic R C and Elie L 1988 Scanning-tunnelling-microscope observation of surface diffusion on an atomic scale Au on Au(111) Rhys. Rev. Lett. 60 120... 

Most tests of the validity of the BET area have been carried out with finely divided solids, where independent evaluation of the surface area can be made from optical microscopic or, more often, electron microscopic observations of particle size, provided the size distribution is fairly narrow. As already explained (Section 1.10) the specific surface obtained in this way is related to the mean projected diameter through the equation... 

The polyethylene crystals shown in Fig. 4.11 exist as hollow pyramids made up of planar sections. Since the solvent must be evaporated away prior to electron microscopic observation, the pyramids become buckled, torn, and/ or pleated during the course of sample preparation. While the pyramidal morphology is clearly evident in Fig. 4.1 la, there is also evidence of collapse and pleating. Likewise, the ridges on the apparently planar crystals in Fig. 4.1 lb are pleats of excess material that bunches up when the pyramids collapse. 

It is difficult to determine the cross-sectional area of a fiber. Direct observation and measurement of a cross section under a microscope is the most accurate method (15). This is a destmctive test that does not allow subsequent study of fiber mechanical properties, and is slow and tedious. Also, it does not take into account any variations in the cross-sectional area along the fiber length. Measurement of fiber diameters from microscopic observations of longitudinal views is somewhat easier, but the eUipticity of the cross section in certain fibers can lead to serious errors. 

Fig. 3. Schematic illustration of PAN-based carbon fiber microstmcture based on microscopic observations (3).

Membrane Characterization The two important characteristics of a UF membrane are its permeability and its retention characteristics. Ultrafiltration membranes contain pores too small to be tested by bubble point. Direc t microscopic observation of the surface is difficult and unreliable. The pores, especially the smaller ones, usually close when samples are dried for the electron microscope. Critical-point drying of a membrane (replacing the water with a flmd which can be removed at its critical point) is utihzed even though this procedure has complications of its own it has been used to produce a Few good pictures. 

Champion and Rohde [42] investigate the effects of shock-wave amplitude and duration on the Rockwell C hardness [41] and microstructure of Hadfield steel over the pressure range of 0.4-48 GPa (pulse duration of 0.065 s, 0.230 ls, and 2.2 ps). The results are shown in Fig. 7.8. In addition to the very pronounced effeet of pulse duration on hardness shown in Fig. 7.8, postshoek electron microscope observations indicate that it is the final dislocation density and not the specific microstructure that is important in determining the hardness. 

An interesting approach involved microscopic observation of fretting corrosion a glass slide mounted on the stage of a microscope was used for the bearing surface which pressed against a spherical specimen being vibrated by a solenoid... 

Yamazoe, Microscopic Observation of Phase Transitions of Ammonium Nitrate , JCrystal-Growth 2, 255-66 (1968) 30) R.D. Rich,... 

Pyrocollodion and Pyrocellulose powders belong to the single-base type because they contain only NC and about 1% of a stabilizer, diphenylamine. Both are nearly completely sol in eth-alc mixts. According to microscopic observations conducted by Sapojnikoff (Ref 5), Pyrocollodion powder is much more uniform than the Fr Poudre B , both CPL and CP2 types... 

Wischin s study [201] ofnucleation and growth ofthe product barium during decomposition of BaN6. In other rate processes where the crystallites are small, opaque, of roughened surface, etc., reactant and product cannot be distinguished and microscopic observations yield no useful data. 

The characteristic feature of solid—solid reactions which controls, to some extent, the methods which can be applied to the investigation of their kinetics, is that the continuation of product formation requires the transportation of one or both reactants to a zone of interaction, perhaps through a coherent barrier layer of the product phase or as a monomolec-ular layer across surfaces. Since diffusion at phase boundaries may occur at temperatures appreciably below those required for bulk diffusion, the initial step in product formation may be rapidly completed on the attainment of reaction temperature. In such systems, there is no initial delay during nucleation and the initial processes, perhaps involving monomolec-ular films, are not readily identified. The subsequent growth of the product phase, the main reaction, is thereafter controlled by the diffusion of one or more species through the barrier layer. Microscopic observation is of little value where the phases present cannot be unambiguously identified and X-ray diffraction techniques are more fruitful. More recently, the considerable potential of electron microprobe analyses has been developed and exploited. 

X= 2) or (P = 0, X = 3) and the distinction between these possibilities is most satisfactorily based upon independent evidence, such as microscopic observations. The growth of compact nuclei inevitably results in the consumption of surfaces and when these outer faces, the sites of nucleation, have been eliminated, j3 necessarily is zero this may result in a diminution of n. The continued inward advance of the reaction interface at high a results in a situation comparable with the contracting volume reaction (discussed below) reference to this similarity was also made in consideration of the Mampel approach discussed above. Shapes of the deceleratory region of a time curves for nucleation and growth reactions and the contracting volume rate process are closely similar [409]. 

A constant rate (zero-order kinetic behaviour) maintained during all, or the greater part of the process may be accounted for [487] by the following reaction models, illustrated in Fig. 5. These alternatives may be distinguished by microscopic observations. 

K2C03 3 H202 contains hydrogen peroxide of crystallization and the solid phase decomposition involves the production of the free radicals OH and HOi, detected by EPR measurements [661]. a—Time curves were sigmoid and E = 138 kJ mole-1 for reactions in the range 333—348 K. The reaction rate was more rapid in vacuum than in nitrogen, possibly through an effect on rate of escape of product water, and was also determined by particle size. From microscopic observations, it was concluded that centres of decomposition were related to the distribution of dislocations in the reactant particles. 

There have been few satisfactory demonstrations that decompositions of hydrides, carbides and nitrides proceed by interface reactions, i.e. either nucleation and growth or contracting volume mechanisms. Kinetic studies have not usually been supplemented by microscopic observations and this approach is not easily applied to carbides, where the product is not volatile. The existence of a sigmoid a—time relation is not, by itself, a proof of the occurrence of a nucleation and growth process since an initial slow, or very slow, process may represent the generation of an active surface, e.g. poison removal, or the production of an equilibrium concentration of adsorbed intermediate. The reactions included below are, therefore, tentative classifications based on kinetic indications of interface-type processes, though in most instances this mechanistic interpretation would benefit from more direct experimental support. 

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