Particle size distribution instrumental techniques

The instrument design is less complicated as compared with laser diffraction. A stable suspension of particles is placed in a transparent cell, where a laser beam impinges on the particles. As the light is scattered from the randomly moving particles, interference patterns are created. Using suitable mathematical algorithms, these patterns are converted into particle size distributions. This technique is not well suited for material that exhibits a multimodal particle size distribution. One should not use this technique to obtain particle size distributions because of the assumptions that are needed to convert the interference patterns into usable information. The technique should be used to assess average particle size only. Additional information on this technique can be found in the literature.2,6,13... 

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. 

Particle size is one of the principal determinants of powder behavior such as packing and consolidation, flow ability, compaction, etc., and it is therefore one of the most common and important areas of powder characterization. Typically, one refers to particle size or diameter as the largest dimension of its individual particles. Because a given powder consists of particles of many sizes, it is preferable to measure and describe the entire distribution. While many methods of size determination exist, no one method is perfect (5) two very common methods are sieve analysis and laser diffraction. Sieving is a very simple and inexpensive method, but it provides data at relatively few points within a distribution and is often very operator dependent. Laser diffraction is a very rapid technique and provides a detailed description of the distribution. However, its instrumentation is relatively expensive, the analytical results are subject to the unique and proprietary algorithms of the equipment manufacturer, and they often assume particle sphericity. The particle size distribution shown in Figure 1 was obtained by laser diffraction, where the curves represent frequency and cumulative distributions. 

A related technique that is suitable for measurement of aerosols at lower mass loadings is the aerodynamic particle sizer (3, 10). In this instrument the aerosol is rapidly accelerated through a small nozzle. Because of their inertia, particles of different aerodynamic sizes are accelerated to different velocities, and the smallest particles reach the highest speeds. The particle velocity is measured at the outlet of the nozzle. From the measurements of velocities of individual particles, particle size distributions can be determined. The instrument provides excellent size resolution for particles larger than about 0.8 xm in diameter, although sampling difficulties limit its usefulness above 10 xm. 

Laser diffraction is the most commonly used instrumental method for determining the droplet size distribution of emulsions. The possibility of using laser diffraction for this purpose was realized many years ago (van der Hulst, 1957 Kerker, 1969 Bohren and Huffman, 1983). Nevertheless, it is only the rapid advances in electronic components and computers that have occurred during the past decade or so that has led to the development of commercial analytical instruments that are specifically designed for particle size characterization. These instruments are simple to use, generate precise data, and rapidly provide full particle size distributions. It is for this reason that they have largely replaced the more time-consuming and laborious optical and electron microscopy techniques. 

The major disadvantage of the laser diffraction and electrical pulse counting techniques is that they are only directly applicable to dilute emulsions or emulsions that can be diluted without disturbing the particle size distribution. However, many food emulsions are not dilute and cannot be diluted, either because dilution alters the particle size distribution or because the original sample is partially solid. For concentrated systems it is belter to use particle-sizing instruments based on alternative technologies, such as ultrasonic spectrometry or NMR (Dickinson and McClements, 1996). 

Particle Size Analysis. Particle size distribution measurements of the dry resin were made using a Micromeritics Sedigraph 5000D particle size analyzer. This instrument employs a gravity settling technique and uses Stokes law to determine the particle size. The PSD was run over the size range of 0.36 to 100 micrometers. All measurements were made in dibutyl sebacate as the suspending medium. 

Resolution is without question a key element in accurate and detailed particle characterization. Particle populations that cannot be resolved cannot, in any sense, be distinguished from one another. While deconvolution techniques can provide particle size distribution curves from low resolution systems, the deconvolution must be based on assumptions about instrumental band broadening and band shape. In general, any detailed information lost because of poor resolution cannot be recovered by mathematical manipulation alone. In all cases, the quality of a size distribution curve will increase with the intrinsic resolution exhibited by the system. 

The mass versus particle size distribution of several polymer latices with diameters in the range of 30 nm to 1500 nm was determined in less than 20 minutes using an integrated hydrodynamic chromatograph. Distributions obtained were compared with those found by other particle sizing techniques such as electron microscopy to verify validity of the technique. The instrument employed was able to analyze latices re-producibly with different optical properties, even though some of the injected particles may have been trapped within the column. Latex properties were correlated with particle size distribution data to illustrate the benefit of this particle sizing technique. 

Although the effect of the concentration of suspension on the results of the measurement of pigments has never been proven, the development of techniques able to cope with concentrations closer to the applications if of interest These would make it possible, for example, to determine the particle size distribution in a dispersion paint or in a reaction vessel where a pigment is produced by the precipitation process. A measurement technique having no problems, in principle, with high concentration dispersions is the scattering of ultrasonic waves. Nevertheless the instruments on the market have up to now failed to realize the great expectations of this technique. 

An alternative is the use of an optical method to measure particulate concentrations and size distributions. This technique has the obvious advantage of having a negligible effect on the particulates since the equipment would be external to the exhaust system. An optical method also has the potential to be much simpler to use since it would eliminate the need for elaborate and cumbersome systems containing probes, stack samplers, flow development tunnels, filters, and heat exchangers. In addition, final data from an optical system could be immediately obtained electronically as opposed to weighing the various filters in a particle impactor by hand, and as such, the optical analyzer is a real time instrument capable of following exhaust gas fluctuations and other nonsteady effects. 

In-line measurements of particle size distributions are essential in order to maximize production capacity and product quality. Ultrasonic attenuation is emerging as a technique, with capabilities beyond those of light scattering. In addition to the needs of industry for compact, robust instrumentation, this method is capable of operating at high concentrations, thus eliminating the need for an expensive dilution step, which may alter the very properties one wishes to measure [225,226]. 

The use of transmission electron microscopy in heterogeneous catalysis centers around particle size distribution measurement, particle morphology and structural changes in the support. Consideration is given to the limitations of conventional electron microscopy and how modifications to the instrument enable one to conduct in-situ experiments and be in a position to directly observe many of the features of a catalyst as it participates in a reaction. In order to demonstrate the power of the in-situ electron microscopy technique examples are drawn from areas which impact on aspects of catalyst deactivation. In most cases this information could not have been readily obtained by any other means. Included in this paper is a synopsis of the methods available for preparing specimens of model and real catalyst systems which are suitable for examination by transmission electron microscopy. 

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