Other Methods of Flow Characterization

Other Methods of Flow Characterization A variety of other test methods to characterize flowability of powders have been proposed, which include density ratios, flow from funnels and orifices, angles of repose and sliding, simplified indicizer flow testing, and... 

This brought a bout a keen interest in other methods of intensification in processing. Lately, the directed effect of physical (mechanical) fields on molten polymers has become one such area. These effects, as demonstrated in many works published in the 1970s and in the 1980s, (see for examples [6-9]) result in altered parameters of micro- and macrostress of the system. Molding under conditions of directed physical fields, in particular, in the case of mechanical and acoustic vibration effects upon melts, is performed so that an additional stress superimposed on the polymer s main shear flow and the state of material is characterized by combined stress. 

Other methods involve the use of continuous-flow reactors, and in certain cases, the rate is measured directly rather than indirectly. One advantage of a flow method is that a steady-state can usually be established, and this is an advantage for relatively fast reactions, and for continuous monitoring of properties. A disadvantage is that it may require relatively large quantities of materials. Furthermore, the flow rate must be accurately measured, and the flow pattern properly characterized. 

In this chapter, we consider nonideal flow, as distinct from ideal flow (Chapter 13), of which BMF, PF, and LF are examples. By its nature, nonideal flow cannot be described exactly, but the statistical methods introduced in Chapter 13, particularly for residence time distribution (RTD), provide useful approximations both to characterize the flow and ultimately to help assess the performance of a reactor. We focus on the former here, and defer the latter to Chapter 20. However, even at this stage, it is important to realize that ignorance of the details of nonideal flow and inability to predict accurately its effect on reactor performance are major reasons for having to do physical scale-up (bench —> pilot plant - semi-works -> commercial scale) in the design of a new reactor. This is in contrast to most other types of process equipment. 

The particle beam LC/FT-IR spectrometry interface can also be used for peptide and protein HPLC experiments to provide another degree of structural characterization that is not possible with other detection techniques. Infrared absorption is sensitive to both specific amino acid functionalities and secondary structure. (5, 6) Secondary structure information is contained in the amide I, II, and III absorption bands which arise from delocalized vibrations of the peptide backbone. (7) The amide I band is recognized as the most structurally sensitive of the amide bands. The amide I band in proteins is intrinsically broad as it is composed of multiple underlying absorption bands due to the presence of multiple secondary structure elements. Infrared analysis provides secondary structure details for proteins, while for peptides, residual secondary structure details and amino acid functionalities can be observed. The particle beam (PB) LC/FT-IR spectrometry interface is a low temperature and pressure solvent elimination apparatus which serves to restrict the conformational motions of a protein while in flight. (8,12) The desolvated protein is deposited on an infrared transparent substrate and analyzed with the use of an FT-IR microscope. The PB LC/FT-IR spectrometric technique is an off-line method in that the spectral analysis is conducted after chromatographic analysis. It has been demonstrated that desolvated proteins retain the conformation that they possessed prior to introduction into the PB interface. (8) The ability of the particle beam to determine the conformational state of chromatographically analyzed proteins has recently been demonstrated. (9, 10) As with the ESI interface, the low flow rates required with the use of narrow- or microbore HPLC columns are compatible with the PB interface. 

Other classification systems are used less frequently. Carr " also devised a system to classify materials as to their floodability. He defines the floodability of a material as its tendency to flow like a liquid because of the natural fluidization of a mass of particles by air. In order to so classify a material, the flowability is determined utilizing the method just described. This value is equivalent to a measurement Carr calls the angle of fall, angle of difference, and dispersibility. Though referred to in any of the papers mentioned here, this system is much less utilized then the flowability measurements. Geldart reported on a characterization system of powders according to their ability to aerate and later Molerus modified this system. In a more recent symposium this method of powder classification was examined. ... 

Alternatively, nano-ESl is used in continuous-flow mode by injecting samples in a mobile-phase flow or in on-line combination with nano-LC (Ch. 17.5.2) and other low-flow separation methods (Ch. 6.6.2 and Ch. 17.5.5-6). As such, nano-ESl plays an important role in the progress in the field of protein characterization. 

Field-flow fractionation (FFF) describes a group of analytical techniques that are becoming quite useful in the separation and characterization of dissolved or suspended materials such as polymers, large particles, and colloids. Although the FFF concept was first described by Giddings in 1966, only recently have practical applications and advantages over other methods been shown. 

The validity of Frenkel s model is limited to Newtonian flow and can only be used to predict the early stage of the coalescence process, when the diameter of the two spherical particles remains nearly unchanged. The inadequacy of a Newtonian model in describing the coalescence of polymers was also demonstrated in other studies, as reviewed by Mazur, and has led to the development of models as well as alternative methods for the characterization of the coalescence behavior of polymers for rotational molding applications.Based on theoretical and experimental analyses of the coalescence phenomenon, the material properties of primary interest in the evaluation of resin coalescence behavior in rotational molding have been identifled as the resin viscosity, surface tension, and elasticity. 

V. Experimental Characterization of Reaction Intermediates Flow and Other Methods... 

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