This document discusses several common methods for testing powder flow properties: angle of repose, compressibility index, flow through an orifice, and shear cell testing. It provides details on how each test is performed, considerations that affect the results, and recommended procedures. Angle of repose involves forming a cone of powder and measuring its slope. Flow through an orifice measures the mass or volume flow rate of powder passing through an opening. Shear cell testing involves consolidating powder in a cell and measuring the force required to move portions relative to each other. Standardized procedures are advised where possible given variations across methods.
This document discusses several common methods for testing powder flow properties: angle of repose, compressibility index, flow through an orifice, and shear cell testing. It provides details on how each test is performed, considerations that affect the results, and recommended procedures. Angle of repose involves forming a cone of powder and measuring its slope. Flow through an orifice measures the mass or volume flow rate of powder passing through an opening. Shear cell testing involves consolidating powder in a cell and measuring the force required to move portions relative to each other. Standardized procedures are advised where possible given variations across methods.
This document discusses several common methods for testing powder flow properties: angle of repose, compressibility index, flow through an orifice, and shear cell testing. It provides details on how each test is performed, considerations that affect the results, and recommended procedures. Angle of repose involves forming a cone of powder and measuring its slope. Flow through an orifice measures the mass or volume flow rate of powder passing through an opening. Shear cell testing involves consolidating powder in a cell and measuring the force required to move portions relative to each other. Standardized procedures are advised where possible given variations across methods.
This document discusses several common methods for testing powder flow properties: angle of repose, compressibility index, flow through an orifice, and shear cell testing. It provides details on how each test is performed, considerations that affect the results, and recommended procedures. Angle of repose involves forming a cone of powder and measuring its slope. Flow through an orifice measures the mass or volume flow rate of powder passing through an opening. Shear cell testing involves consolidating powder in a cell and measuring the force required to move portions relative to each other. Standardized procedures are advised where possible given variations across methods.
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POWDER FLOW
• Four commonly reported methods for testing
powder flow are (1) angle of repose, (2) compressibility index or Hausner ratio, (3) flow rate through an orifice, and (4) shear cell. In addition, numerous variations of each of these basic methods are available. Given the number of test methods and variations, standardizing the test methodology, where possible, would be advantageous. ANGLE OF REPOSE • Angle of repose is a characteristic related to interparticulate friction or resistance to movement between particles. • The most common methods for determining the static angle of repose can be classified on the basis of the following two important experimental variables: • 1. The height of the “funnel” through which the powder passes may be fixed relative to the base, or the height may be varied as the pile forms. • 2. The base upon which the pile forms may be of fixed diameter or the diameter of the powder cone may be allowed to vary as the pile forms. Variations in Angle of Repose Methods • Drained angle of repose is determined by allowing an excess quantity of material positioned above a fixed diameter base to “drain” from the container. Formation of a cone of powder on the fixed diameter base allows determination of the drained angle of repose. • Dynamic angle of repose is determined by filling a cylinder (with a clear, flat cover on one end) and rotating it at a specified speed. The dynamic angle of repose is the angle (relative to the horizontal) formed by the flowing powder. The internal angle of kinetic friction is defined by the plane separating those particles sliding down the top layer of the powder and those particles that are rotating with the drum (with roughened surface). Angle of Repose General Scale of Flowability • There are examples in the literature of formulations with an angle of repose in the range of 40 to 50 that were manufactured satisfactorily. When the angle of repose exceeds 50, the flow is rarely acceptable for manufacturing purposes. Experimental Considerations for Angle of Repose • Angle of repose is not an intrinsic property of the powder; i.e., it is very much dependent upon the method used to form the cone of powder. The following important considerations are raised in the existing literature: • The peak of the cone of powder can be distorted by the impact of powder from above. By carefully building the powder cone, the distortion caused by impact can be minimized. • The nature of the base upon which the powder cone is formed influences the angle of repose. It is recommended that the powder cone be formed on a “common base,” which can be achieved by forming the cone of powder on a layer of powder. This can be done by using a base of fixed diameter with a protruding outer edge to retain a layer of powder upon which the cone is formed. Recommended Procedure for Angle of Repose • Form the angle of repose on a fixed base with a retaining lip to retain a layer of powder on the base. The base should be free of vibration. Vary the height of the funnel to carefully build up a symmetrical cone of powder. Care should be taken to prevent vibration as the funnel is moved. The funnel height should be maintained approximately 2–4 cm from the top of the powder pile as it is being formed in order to minimize the impact of falling powder on the tip of the cone. If a symmetrical cone of powder cannot be successfully or reproducibly prepared, this method is not appropriate. Determine the angle of repose by measuring the height of the cone of powder and calculating the angle of repose, , from the following equation: FLOW THROUGH AN ORIFICE • The flow rate through an orifice is generally measured as the mass per time flowing from any of a number of types of containers (cylinders, funnels, hoppers). Measurement of the flow rate can be in discrete increments or continuous. Basic Methods for Flow Through an Orifice • There are a variety of methods described in the literature. The most common method for determining the flow rate through an orifice can be classified on the basis of three important experimental variables: • 1. The type of container used to contain the powder. Common containers are cylinders, funnels, and hoppers from production equipment. • 2. The size and shape of the orifice used. The orifice diameter and shape are critical factors in determining powder flow rate. • 3. The method of measuring powder flow rate. Flow rate can be measured continuously using an electronic balance with some sort of recording device (strip chart recorder, computer). It can also be measured in discrete samples (for example, the time it takes for 100 g of powder to pass through the orifice to the nearest tenth of a second or the amount of powder passing through the orifice in 10 seconds to the nearest tenth of a gram). Variations in Methods for Flow Through an Orifice • Either mass flow rate or volume flow rate can be determined. Mass flow rate is the easier of the methods, but it biases the results in favor of high- density materials. Because die fill is volumetric, determining volume flow rate may be preferable. A vibrator is occasionally attached to facilitate flow from the container; however, this appears to complicate interpretation of the results. A moving orifice device has been proposed to more closely simulate rotary press conditions. The minimum diameter orifice through which powder flows can also be identified. Experimental Considerations for Flow Through an Orifice Flow rate through an orifice is not an intrinsic property of the powder. It very much depends on the methodology used. Several important considerations affecting these methods are discussed in the existing literature: • The diameter and shape of the orifice • The type of container material (metal, glass, plastic) • The diameter and height of the powder bed. Recommended Procedure for Flow Through an Orifice • Flow rate through an orifice can be used only for materials that have some capacity to flow. It is not useful for cohesive materials. Provided that the height of the powder bed (the “head” of the powder) is much greater than the diameter of the orifice, the flow rate is virtually independent of the powder head. Use a cylinder as the container because the cylinder material should have little effect on flow. This configuration results in flow rate being determined by the movement of powder over powder rather than powder along the wall of the container. Powder flow rate often increases when the height of the powder column is less than two times the diameter of the column. The orifice should be circular and the cylinder should be free of vibration. General guidelines for dimensions of the cylinder are as follows: • Diameter of opening > 6 times the diameter of the particles • Diameter of the cylinder > 2 times the diameter of the opening • Use of a hopper as the container may be appropriate and representative of flow in a production situation. It is not advisable to use a funnel, particularly one with a stem, because flow rate will be determined by the size and length of the stem as well as the friction between the stem and the powder. A truncated cone may be appropriate, but flow will be influenced by the powder-wall friction coefficient, making selection of an appropriate construction material an important consideration. • For the opening in the cylinder, use a flat-faced bottom plate with the option to vary orifice diameter to provide maximum flexibility and to better ensure a powder-over-powder flow pattern. Rate measurement can be either discrete or continuous. Continuous measurement using an electronic balance can more effectively detect momentary flow rate variations. SHEAR CELL METHODS • One type of shear cell is the cylindrical shear cell that is split horizontally, forming a shear plane between the lower stationary base and the upper moveable portion of the shear cell ring. After powder bed consolidation in the shear cell (using a well-defined procedure), the force necessary to shear the powder bed by moving the upper ring is determined. Annular shear cell designs offer some advantages over the cylindrical shear cell design, including the need for less material. A disadvantage, however, is that because of its design, the powder bed is not sheared as uniformly; i.e., material on the outside of the annulus is sheared more than material in the inner region. A third type of shear cell (plate-type) consists of a thin sandwich of powder between a lower stationary rough surface and an upper rough surface that is moveable. • All of the shear cell methods have their advantages and disadvantages, but a detailed review is beyond the scope of this chapter. As with the other methods for characterizing powder flow, many variations are described in the literature. A significant advantage of shear cell methodology in general is a greater degree of experimental control. The methodology is rather time-consuming and requires significant amounts of material and a well-trained operator. • The many existing shear cell configurations and test methods provide a wealth of data and can be used very effectively to characterize powder flow. They are also helpful in the design of equipment such as hoppers and bins. Because of the diversity of available equipment and experimental procedures, no specific recommendations regarding methodology are presented in this chapter. It is recommended that the results of powder flow characterization using shear cell methodology include a complete description of equipment and methodology used.