Sedimentation techniques, particle size analysis using

During particle size analysis, in addition to screening, sifting, and counting, sedimentation techniques are often used which produce unequivocal results only if the individual particles can move without influencing each other. For that reason, very dilute suspensions are used. Nevertheless, it is possible that agglomerates form or already... 

The sedimentation methods of particle size analysis, both gravitational and centrifugal, have, over the years, generated many contributions and are still extensively used in many traditional industries. PSA 91 saw however only three such contributions [Allen (2) Bernhardt], one which was a Keynote lecture reviewing the historical developments of this fundamental method. The Andreasen sedimentation technique and sieving continue as essential methods used for the characterisation of many certified reference materials. 

Sedimentation (qv) techniques, whether based on gravitational forces or centrifugation, derive the particle size from the measured travel rates of particles in a Hquid. Before the particle analysis is carried out, the sample is usually dispersed in a medium to break down granules, agglomerates, and aggregates. The dispersion process might involve a simple stirring of the powder into a Hquid, but the use of an ultrasonic dispersion is preferred. 

Various techniques and equipment are available for the measurement of particle size, shape, and volume. These include for microscopy, sieve analysis, sedimentation methods, photon correlation spectroscopy, and the Coulter counter or other electrical sensing devices. The specific surface area of original drug powders can also be assessed using gas adsorption or gas permeability techniques. It should be noted that most particle size measurements are not truly direct. Because the type of equipment used yields different equivalent spherical diameter, which are based on totally different principles, the particle size obtained from one method may or may not be compared with those obtained from other methods. 

Information on particle size may be obtained from the sedimentation of particles in dilute suspensions. The use of pipette techniques can be rather tedious and care is required to ensure that measurements are sufficiently precise. Instruments such as X-ray or photo-sedimentometers serve to automate this method in a non-intrusive manner. The attenuation of a narrow collimated beam of radiation passing horizontally through a sample of suspension is related to the mass of solid material in the path of the beam. This attenuation can be monitored at a fixed height in the suspension, or can be monitored as the beam is raised at a known rate. This latter procedure serves to reduce the time required to obtain sufficient data from which the particle size distribution may be calculated. This technique is limited to the analysis of particles whose settling behaviour follows Stokes law, as discussed in Section 3.3.4, and to conditions where any diffusive motion of particles is negligible. 

Other techniques, such as fight scattering and sedimentation, are also sensitive to particle shape. The direct observation of particles by a scanning electron microscope and distribution measurements by image analysis would appear to overcome many of the problems associated with the various other techniques, but problems of describing irregularly shaped particles remain. A universal particle size descriptor has not yet been developed. The technique adopted and the results obtained are most useful when empirical correlations with the end use can be made. 

Walden, J. M. C. Slattery, 1993. Verification of a simple gravity technique for separation of particle size fractions suitable for mineral magnetic analysis. Earth Surf. Proc. Landforms. 18 829-833. Yu, L. F. Oldfield, 1993. Quantitative sediment source ascription using magnetic measurements in a reservoir catchment system near Nijar, S.E. Spain. Earth surf. Proc. Landforms 18 441 54. 

Other techniques of deducing shape (or size) include using sieve analysis or sedimentation. The equivalent diameter for a sieve analysis is the mesh size of the upper sieve through which particles pass. (A more precise definition of the sieve diameter is the mean between the mesh size through which the particles pass and on which the particles are retained.) The characteristic diameter of a sedimentation technique would be the diameter of a sphere that has the same settling velocity. 

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