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Consolidation seminar......

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Consolidation seminar......

  1. 1. CONSOLIDATION Presented By Vrushali V. Sonawadekar M-pharm 1st year Dept. of pharmaceutics KLE’U collage of pharmacy , Belagavi.
  2. 2. Content..  Definition  Consolidation process  Mechanisms of consolidation  Factors affecting consolidation  Compression & Consolidation under high loads  Force volume relationship  Heckel Equation  Heckel plot  Kawakita equation  Conclusion  Reference
  3. 3. Consolidation An increase in the mechanical strength of the material resulting from particle or particle interaction. ( Increasing in mechanical strength of the mass)
  4. 4. Consolidation Process  Cold welding : when the surface of two particles approach each other closely enough , their free surface energies result in strong attractive force , a process known as cold welding. E.g. At separation of less than 50nm  Fusion bonding : Multiple point contacts of particles upon application of load produces heat which causes fusion or melting. Upon removal of load it gets solidified & increase the mechanical strength of mass.
  5. 5. Consolidation Mechanism Mechanical theory :  It occurs btw irregular shaped particles.  Also increases the number of contact points btw the particles  As the particle undergo deformation , the particle boundaries that the edges of the particles intermesh , forming a mechanical bond. Intermolecular force theory : Under pressure the molecules at the points of true contact between new , clean surface of the granules are close enough so that van der waals force interact to consolidate the particles. E.g , microcrystalline cellulose is believed to undergo significant hydrogen bonding during tablet compression e pa
  6. 6. Liquid – Surface film theory : Thin liquid films form which bond the particles together at the particles surface . The energy of compression produces melting of solutions at the particles interface followed by subsequent solidification or crystallization thus in the formation of bonded surface.
  7. 7. Factors affecting consolidation The chemical nature of the material. The extent of the available surface. The pressure of the surface contaminants. The inter surface distance.
  8. 8. Role of moisture  Moisture is necessary for formation of tablets. it can fill the small voids present between the particles. Moisture is also important in wet / moist granulation.  A small proportion of moisture content is required in the formulation of tablet. This moisture content is important for the mechanical strength of tablet.
  9. 9. If moisture content is less there will be increase in the die wall friction. If moisture content is increased there will be decrease in compact strength . Moisture content is determined by loss on drying given by formula Percentage moisture content= (loss in wt/ initial wt) x 100
  10. 10. Eg : As a results of increasing compressional force , result in this water being squeezed out to the surface of the tablet . This expelled moisture may act as a lubricant at the die wall, but it could be cause material to stick to the punch faces .
  11. 11. Different types of states during moist granulation 1. Pendular state (powder + binding agent) 2. Funicular state (powder + more binding agent) 3. Capillary state(powder + even more binding agent) 4. Droplet state(powder + even more & more binding agent)
  12. 12.  Pendular state :  This state is occurs at low moisture level.  In this state particles are held together by lens shaped rings of liquid .  These cause adhesion because of the surface tension force of the liquid – air interface & the hydrostatic suction pressure in the liquid bridge.
  13. 13. Funicular state :  This state represents an intermediate stage btw the pendular & capillary state.  When the air start to displace from btw the particles , the particles arrange in funicular state.  After the funicular state ,the particles arrange themselves in capillary state & there is no air btw them.
  14. 14. Capillary state :  When all the air has been displaced from btw the particles the capillary state is reached .  Moist granules tensile strength increases about three times btw the pendular & the capillary state .  This state is most desirable state in the process of granulation.
  15. 15.  Droplet state  This is another state in the process but this step is undesirable .  This will be important in the process of granulation by spray drying of a suspension.
  16. 16. Compression & Consolidation under high loads Effect of Friction Force Distribution Development of radial force Die-wall lubrication Ejection force
  17. 17. 1. Effect of Friction :  Frictional forces are inter particulate friction and die wall friction  Inter particulate friction occurs due to particle- particle contact and it is more significant at low applied load .These forces are reduced using glidants. Eg : colloidal silica , talc , corn starch,  Die wall friction forces occur from material pressed against die wall and moved, it is dominant at high applied load. These forces are reduced using lubricants like magnesium stearate , talc , stearic acid , waxes etc,
  18. 18. 2 . Force distribution : Most investigations are carried out on single station presses or even on isolated punches & die sets in conjugation with hydraulic press, These must be an axial balance of forces.  A force is applied on cylinder on top of cylinder of powder mass
  19. 19. FA=FL +FD Where… FA…Applied force to the upper punch FL…Force transmitted to lower punch FD…Reaction at die –wall due to friction at surface
  20. 20. 3. Development of radial force :  As the compressional force is increased & the repacking of tableting mass is completed ,the material may be regard as a single solid body.  Then as with all the solids , compressive force applied in one direction (eg: vertical) results in a decrease in ΔH i.e. height  In case of unconfined solid body , this would be accompanied by an expansion in the horizontal direction of ΔD.  The ratio of these two directional changes is known as poisson ratio (λ) of the material. λ=ΔD/ΔH  λ is characteristic constant for each solid
  21. 21.  Consequently a radial die-wall force  F R develops.  Materials with larger values of λ gives rise to larger value of F R  The relation ship btw F D & F R is given by the expression : FD=µw. FR  µW =coefficient of radial die wall friction.
  22. 22. 4. Die-wall lubrication Most pharmaceutical tablets formulations requires the addition of a lubricants to reduces friction at the die wall, -Die-wall lubricants function by inter posing a film of low shear strength at the interface btw tableting mass & die-wall there is some chemical bonding btw boundary lubricants & the surface of die-wall as well as at edge of the tablets. -The best lubricants are those of low shear strength but have strong cohesive tendency in direction at right angle to the plane of shear
  23. 23. The shear strength of some lubricants Material Shear strength Stearic acid 1.32 Calcium stearate 1.47 Hard paraffin 1.86 Magnesium stearate 1.96 Potassium stearate 3.07
  24. 24. 5. Ejection force: Force necessary to eject a finished tablets. Ejection force for a finished tablets consists of 3 stages stage-1: Peak force required to initiate ejection by breaking tablets / die wall adhesion. stage-2: Small force , that required to push the tablets up the die wall . stage-3: Declining force of ejection as the tablets emerges from the die.
  25. 25. Radial die wall forces and die wall friction also affects ejection of compressed tablets from die. The force necessary to eject finished tablet is known as ejection force This force can eject tablet by breaking tablet/ die wall adhesion Variation occurs in ejection force when lubrication is inadequate
  26. 26. Measurements of forces 1) Strain Gauge  A coil of high resistant with length width ratio 2:1 & resistant 100 ohm is suitable.  During compression the applied force causes a small elastic deformation of two punches.  Strain gauge are connected to punch as close to the compression site . It is deformed as the punch deformed.  With the deformation , the length of resistant wire decreases & its diameter is increases.  The resulting decrease in resistance I measured by wheat stone bridge as a recording devise.  Care must be taken to use low voltage so that heating effect do not interfere with the strain measurement.
  27. 27. Diagrametic representation of strain gauge
  28. 28. 2) Piezo electric load cells :  Certain crystals like charge quartz may be used. When subjected to external force these develop an electrical charge proportional to the force.  This transducer is connected to amplifier which convert the charge in to dc voltage.  The small piezo – electrical transducer are connected to upper & lower punch holder of single station press.  The disadvantage is the dissipation of charge with time , hence nit suitable for static measurement.
  29. 29. Diagrametic representation of piezo-electric cell
  30. 30. Force volume relationship In many tablets processes , when appreciable force has been applied, the relationship btw applied pressure (p) & volume parameters such as porosity E dose become linear over the range of commonly used pressure. - It can be expressed by shapiro equation Log E =Log E0-K.P. Where….E0=porosity when pressure is zero K=constant P= pressure - Walker expressed similarly 1/1-E=K1-K2.Log P
  31. 31. i. initial repacking of particles ii. Elastic deformation until elastic limit is reached. iii. Plastic deformation or brittle fracture dominates. iv. Compression of solid crystal lattice formation.
  32. 32. Heckel Equation The heckel analysis is a most popular method of deforming reduction under compression pressure . Powder packing with increasing compression load is normally attributed to particles rearrangement , elastic & plastic deformation & particle fragmentation.
  33. 33. It is analogous to first order reaction ,where the pores in the mass are the reactant , that is: Log 1/E= Ky . P + Kr Where….. Ky =material dependent constant inversely proportional to its yield strength ‘s’ Kr=initial repacking stage hence E0
  34. 34. The applied compressional force F & the movement of the punches during compression cycle & applied pressure P , porosity E. For a cylindrical tablets p=4F/л. D2 Where… D is the tablet diameter similarly E can be calculated by E=100.(1-4w/ρt .л.D2.H) Where…w is the weight of the tableting mass , ρt is its true density , H is the thickness of the tablets.
  35. 35. Heckel Plots  Heckel plot is density v/s applied pressure  Follows first order kinetics  As porosity increases compression force also increases  Thus the Heckel’s plot allows for the interpretation of the mechanism of bonding.  Materials that are comparatively soft & that readily undergo plastic deformation retain different degree of porosity , depending upon the initial packing in the die.
  36. 36. This in turn is influenced by the size distribution , shape etc of the original particles. Ex: sodium chloride (shown by type a in graph) Harder material with higher yield pressure values usually undergo compression by fragmentation first , to provide a denser packing. Ex: Lactose, sucrose ( shown in type b in graph).
  37. 37. Type-a plots exhibits higher slop (Ky) then type-b. because type-a materials have lower yield stress. Type-b plots exhibits lower slop because brittle , hard materials are more difficult to compress.
  38. 38. Kawakita Equation Pa /C = 1/ab + Pa /a Where C= degree of volume reduction a,b= constants characteristic to powder being compressed P= pressure it is a plot of p/c v/s p
  39. 39. This equation describes the relationship between the degree of volume reduction of the powder column and the applied pressure The basis for the kawakita equation for powder compression is that the particles are subjected to a compressive load in a confined space are viewed as a system in equilibrium at all stages of compression, so that the product of the pressure term and volume term is a constant.
  40. 40. conclusion The compression & consolidation are important in the tableting of the materials. The important of each will depends upon largely on the type of compact required i.e whether soft or hard & on the brittle properties of the materials. Various mathematical equations have been used to describe the compaction process. The particular value of Heckel plots arises from their ability to identify the predominant form of deformation in a given sample.
  41. 41. Referance  Aulton’s pharmaceutics: The design and manufacture of medicines by Micheal Aulton  The theory and practice of industrial pharmacy by Leon lachman, Herbert A Liberman  Pharmaceutical dosage forms :tablets , vol :1 by Larry Augsburger & Stephen Hoag.  Remington : the science & practice of pharmacy ,21st edition by lippincott willams & wilkins.  Dekker series volume 71  By internet sources.
  42. 42. Thank you

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