Outline * Introduction * The solid-air Interface * Determination of Flow Ability of Powders = Mass volume relationship = Compression * Consolidation = ConclusionIntroduction Compaction The compression and consolidation of two phases (particulate solid- gas) system due to applied force. Compression It is the reduction in the bulk volume of the material as a result of displacement of gaseous phase. ccc) Consolidation It is an increase in the mechanical strength of material, resulting from particle-particle interaction.The Solid Air Interface * Distribution of intra and intermolecular bonding between atoms or ions located at the surface of solid particles. * Unsatisfied attractive molecular forces extends out at small distance beyond the solid particle surface. * This conditions gives rise to “free surface energy of solid” which plays role in interactions between particles and particles and its environment. * Adsorption, cohesion, adhesion rate of solution and crystallization are manifestations of this fundamental property of solids.The Solid Air Interface Cohesion Unsatisfied bonding forces at the surface of particles which are attracted and tend to stick to one another . Adhesion When particles approached to other types of particles or solid surfaces, they are attracted to them known as adhesion.The Solid Air Interface This attraction gives rise to an intrinsic property to all bulk powdered solids, they resist to different movement of particles when they are subjected external forces. This will affect several operation like flow of granules from hoppers or feeders, relative motion in mixing and compression to produces granules and tablets. * The second factor is the presence of an adsorbed layer of moisture on particles. Decreased chance of any complicating path for charge dissipation. These films of moisture can form liquid bridges which holds the particles together by surface tension effect and by a negative capillary pressure.Determination of Flow Ability of Powders Angle of Repose The maximum angle that can obtained between free standing surface of powder heap and horizontal plane. 2h h tan@ = > or tan@ =— D r It gives qualitative assessment of internal cohesive and frictional effects. It can be determined by three methods * Hollow Cylinder Method a * Rectangular box method = Fixed Funnel MethodDetermination of Flow Ability of Powders Revolving Cylinder Method * Hollow cylinder half filled with test powder with one end sealed by transparent plate. * Cylinder in rotated about its horizontal axis, until and unless the powder surface cascades. “The curved wall is lined with sandpaper to prevent preferential slip at this surface Tilting Box Method Sandpaper lined rectangular box is filled with the powder10 Determination of Flow Ability of Powders Fixed Funnel Method © The material is poured through a funnel to form a cone on an inverted petri dish. ‘Stop pouring the material when test powder starts to fall from the sides of petri dish. ° Measure the height of the pile and take the diameter of petri dish as diameter of the pile and angle of repose is determined through formula.Determination of Flow Ability of Powders If <40° - reasonable flow If >40° - poor flow If 90° or more - no flowDetermination of Flow Ability of Powders Flow Rates Flow rates can be determined by determining the Compressibility Index. Compressibility Index It is the indication of ease with which a material is induced to flow. It is given as percentage and determined by following formula. 1=[1-{]x 100 If <15% - good flow ability and compressibility If >25% - poor flow and compressibility“\ Mass-volume Relationships Volume The volume of a substance will depend upon following types of Voids * Open Intra-particulate Voids; Spaces inside the particles, OPEN to external environment = Closed Intra-particulate Voids; Spaces inside the particles, NOT OPEN to external jironment * Inter-particulate Voids; Spaces in between different particles.Mass-volume Relationships So depending upon particles properties three interpretations of powder volume can made: The true-volume (V,) * The total volume which excludes all spaces greater than molecular dimensions. The granular-volume (V,) © The cumulative volume occupied by particles, including all intra-particulate voids but not inter-particulate voids. The bulk-volume (Vs) » The total volume occupi the erMass-volume Relationships Relative Volume (Vr) The ratio of volume under specific experimental conditions to true volume. v Wea Volume of Voids (Vv) It is the volume occupied by the voids. Y= W—-Ve Eq. (1)Mass-volume Relationships Porosity (E) The ratio of total volume of voids (Vv) to bulk volume (Vb) of material. = [= Eq. (2) Putting the value of Vv from Eq. (1) to Eq. (2) gate yh Yo Vp Porosity is frequently expressed as percentage. = _*] B= 100.[1~ 74]Mass-volume Relationships Density The ratio of mass (weight) to volume is known as the density of the material. More density means less porosity. So, based on powder volume, three densities can be defined; m m m True Density = iy Granular Density = zu Bulk Density = in t f >Mass-volume Relationships Effect of Applied Force When any solid body is subjected to opposing forces, there is finite change in its geometry depending upon nature of applied load. Strain The relative amount of deformation produced by such forces is dimensionless quantity called strain. Stress The ratio of force necessary to produce strain to the area over which it is applied. It is force per unit area.Mass-volume Relationships Three commonest forms of stress are given below showing change in geometry (strain) of solid body resulting from various types of forces. a. Tensile strain b. Compression strain c. Shear strainCompression "The reduction in bulk volume when external mechanical forces are applied. = It can be result of one or more of following effects. Repacking * Main mechanism of initial volume reduction is wtlaity onset of loading is usually done by closer repacking of powder particles. —repacxing pe = 1% stage of compression is repacking of bulk volumeCompression Deformation *As load increases, rearrangement becomes more difficult and further compression process involves some type of particle deformation = Types of deformation: a. Elastic Deformation b. Plastic Deformation c. Brittle fracture “ « Slastic biastecCompression Elastic Deformation: If on removal of load, the deformation is to a large extent reversible, i.e. it behaves like a rubber, the deformation is said to be elastic. All solids undergo some elastic deformation. E.g. Acetylsalicylic acid, Microcrystalline cellulose.Compression = In some cases of powdered solids, an elastic limit or yield point is achieved and load above this level result in deformation not immediately reversable on removal of applied force. * In these cases bulk volume reduction takes place form plastic deformation or viscous flow of particles which are squeezed into remaining void spaces, resembling the behavior of modeling clay. * This mechanism occur in materials in which the shear strength is less than tensile or breaking strength. = Dwell time: > Time required by the punch to remain in force on tablet to complete process of compression. o If it doesn't occur it leads to lami Dwell time moisture act as lubricant .Compression Brittle fracture = When the shear strength is greater, particles may be fractured & the smaller fragments then helps to fill up any adjacent air space. * This occur mostly in solids with hard brittle particles. E.g. Sugar.Consolidation * It is increase in the mechanical strength of material resulting from particle- particle interaction. * It depend upon 2 processes that occur simultaneously; > Cold welding © Fusion bonding:Consolidation Cold welding: = When surface of 2 particles approach each other closely enough(e.g. at a separation of <5Onm), their free surface energies result in a strong attractive force, a process known as cold welding. = The nature of bonds formed are like those of molecular structure of interior of particles. Fusion bonding: * When force is applied to bed particles(which in practice are irregular), under appreciable force, this cause generation of heat. * If this heat is not dissipated, the local rise in temperature could be sufficient to melting of contact area of particles, which relieve stress in particle region. * In that case melt solidifies giving rise to fusion bonding, which in turn increase theNo attractive forces, so poor tablet will form Consolidation Factors Influencing Cold and Fusion bondingConsolidation Role of moisture * At least some moisture is present in capsule & tablet formulas and concentration well below 1% can dramatically affect behavior of feed material & that of finished product. = 0.02% moistures can affect proportion of applied force transmitted to lower punch. * At0.55% moisture, the behavior is in fact reverse of that for totally dry material. * Critical factor concerns the situation where the amount of moisture present on powder surface is just sufficient to fill the remaining voids in the bed.Consolidation Role of moisture * Any reduction in porosity, as @ result of increasing compressional forces, result in water being squeezed out to surface of tablet. = This expelled moisture may act as lubricant at die well, but also cause mat * Recent experiments shown if i iration hit ri th of tablets made from certain hydrates. to stick to punches. This strength depends on temperature at which dehydration is carried out. * Moisture is also important in moist granulation. This dehydration is accompanied by change in the texture of crystals leading to more porous mass.Conclusion Introduction The solid-air Interface Determination of Flow Ability of Powders Mass volume relationship Compression Consolidation