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Department of Pharmacy (Pharmaceutics) | Sagar savale
04/21/16 Sagar KiShor Savale
CONTENTS.
Definition.
Inherent properties of powder solids.
Solid air interface.
Angle of repose and flow rates.
Mass volume relationship.
Process of compression.
2204/21/16 Sagar KiShor Savale
Die wall lubricant.
Force and volume relationship.
Heckel plot and kawatika equation.
Compaction profile.
Energy expenditure.
Measurement of energy.
 transmission of force.
 force displacement curve.
Strength of tablet and its estimation.
References.
3304/21/16 Sagar KiShor Savale
WHAT IS COMPRESSION ?
Compression means reduction of bulk volume of
material as a result of the removal of gaseous
phase (air) by applied pressure
WHAT IS CONSOLIDATION?
Consolidation is an increase in mechanical
strength of material resulting from particle -
particle interactions.
4404/21/16 Sagar KiShor Savale
WHAT IS COMPACTION ?
The compression and consolidation of a two
phase (solid + gas) system due to an applied
force, resulting in the formation of a compact
but porous mass of definite geometry.
Compaction =compression + consolidation
of two phases (solid-gas) on
application of force.
5504/21/16 Sagar KiShor Savale
Inherent properties of
powder solids
Solid –air interfaces.
Angle of repose.
Fixed funnel and free standing cone method.
Tilting box method.
Revolving cylinder method.
Mass –volume relationships.
Methods to mesure volume of powder.
 Helium pycnometer
 Liquid displacement method (specific gravity
bottle method
604/21/16 Sagar KiShor Savale
7
Angle of repose.
The maximum angle possible
between the surface of pile of
the powder and the horizontal
plane. (also called as Dynamic angle)
704/21/16 Sagar KiShor Savale
8
METHODS TO MEASURE
ANGLE OF REPOSE.
a.Fixed funnel and free standing cone method.
b.Tilting box method.
c.Revolving cylinder method
04/21/16 Sagar KiShor Savale
9
FORMULA FOR MEASURING
ANGLE OF REPOSE
1. θ = Tan-1
(h/r)
here, h =height of pile
r = radius of the base of
the pile
θ = angle of repose.
2. θ = cos-1
D/ (l1+l2)
here, D = diameter of base
l1+l2 = the opposite sides
Angle of
repose
Flow
property of
powder
<25
25-30
Excellent
Good
30-40 Passable
>40 poor
904/21/16 Sagar KiShor Savale
10
CONSOLIDATION
INDEX (Carr, % )
FLOW
5-15 EXCELLENT
12-16 GOOD
18-21 FAIR TO PASSABLE
23-35 POOR
33-38 VERY POOR
>40 VERY VERY POOR
1004/21/16 Sagar KiShor Savale
11
MASS-VOLUME RELATIONSHIPS.
TYPE OF VOIDS OR AIR SPACES:
 Open intraparticulate voids-
 Closed intraparticulate voids-
 Interparticulate voids-
11
Fig:- types of voids and air
spaces.
04/21/16 Sagar KiShor Savale
METHODS TO MEASURE
VOLUME OF POWDER.
 Helium pycnometer
 Liquid displacement method (specific gravity bottle
method)
HELIUM PYCNOMETER
Vt = Vc/U1-U2x[U1-Us]
Vt = true volume of sample.
Vc =true volume of stainless steel spheres.
U1=Volume of empty cell.
U1-U2=Volume occupied by the std. sample.
U1-Us = volume occupied by sample.
121204/21/16 Sagar KiShor Savale
13
Helium pycnometer.
04/21/16 Sagar KiShor Savale
Liquid displacement method.
Solvent used are ---e.g., ethyl alcohol ,water,
mercury , etc.
Pycnometer or specific gravity bottle used.
True density= w3/(w4-w2) = (w2-w1)/(w4-w2)
w1 = wt. of Pycnometer
w2 = Wt. of Pycnometer +sample or glass
beads
w4 = Wt. ofPycnometerwith powder & filled with
solvent
w3=w2-w1=Wt. of sample
w4-w2=Volume of liquid displaced by the solid
141404/21/16 Sagar KiShor Savale
15
specific gravity bottle
1504/21/16 Sagar KiShor Savale
Tablet Press Machine
1604/21/16 Sagar KiShor Savale
.
17
The process of compression.
17
REMOVAL OF PRESSURE
04/21/16 Sagar KiShor Savale
Deformation
• The force required to initiate a plastic
deformation is called as yield stress or elastic
limit.
181804/21/16 Sagar KiShor Savale
Effects of compression force.
19
INITIALLY
REPACKING
DEFORMATION
1904/21/16 Sagar KiShor Savale
Transitional repacking/particle
rearrangement.
202004/21/16 Sagar KiShor Savale
Fragmentation and deformation.
Fragmentation do not occur when applied stress-
 is balanced by a plastic deformation.
change in shape.
sliding of groups of particle (viscoelastic flow).
212104/21/16 Sagar KiShor Savale
22
If, only elastic deformation occurs –
Under nonisostatic conditions-
Uniaxial
relaxation
2204/21/16 Sagar KiShor Savale
Ejection.
2323
Portion under strain caps strain > shear strength.
04/21/16 Sagar KiShor Savale
3 stages of force necessary to eject a finished
table,
1. Peak force required to initiate ejection.
2. Small force required to push tablet up to die-
wall .
3. Decline force as tablet emerge from die.
242404/21/16 Sagar KiShor Savale
Compression and consolidation
under high loads.
2525
Thin layer is abrasion resistant but it –
Retards air escape during compression.
Retards the ingress of liquid media during dissolution.
punch
Die wall
tablet
04/21/16 Sagar KiShor Savale
Die-wall lubrication
• Best lubricant has low shear strength & strong
cohesive tendencies.
• Lubricant forms a film of low shear strength at
the interface between tabletting mass & die-wall.
2626
LUBRICANT SHEAR
STRENGTH
(M pa)
Stearic acid 1.32
Calcium stearate 1.47
Magnesium
stearate
1.96
Boric acid 7.16
graphite 7.35
04/21/16 Sagar KiShor Savale
Force volume relationship.
2727
FIG. Decreasing porosity with increasing
compressional force
for single ended pressing
i) initial repacking
ii) Elastic deformation
iii) Plastic deformation
iv) compression
End of compressional process is when
bulk volume = tapped volume.
porosity (E)= 0
 Decrease in porosity is due to two process:
1. Filling of large spaces by Interparticulate
Slippage.
2. Filling of small voids by deformation or
fragmentation at high loads.
 A more complex sequence of events
during compression process involves four
stage as shown in fig.,
04/21/16 Sagar KiShor Savale
Heckel plot.
• It follows 1st
order
The pore in the mass are the reactant.
log 1/E = KyP + Kr
E = porosity
P = Applied pressure
Ky= material dependent constant
Ky inversely proportional to it’s yield strength (S)
(Ky = 1/3S)
Kr = related to repacking stage &
hence E0
For cylindrical tablet,
P = 4F / ∏×D2
here, P = applied pressure
D = tablet diameter
F = applied compressional force
282804/21/16 Sagar KiShor Savale
2929
E = 100×[1 – 4w/ρt ×∏×D2×H]
here, w = weight of tabletting mass.
ρt = true density.
H = thickness of tablet.
•Type a : Soft material(e.g., NaCl)
• Type b: Hard material(e.g., lactose)
• Crushing strength of tablet
is directly proportional to Ky.
APPLICATION OF HECKEL PLOT:
•Used to check lubricant efficacy.
• For interpretation of consolidation
mechanisms.
•Duberg & nystom distinguish between
plastic and elastic deformation
characteristics of a material.
04/21/16 Sagar KiShor Savale
Kawakita Equation.
C = Vi – Vp/ Vt = abPa / 1+ bPa
C = degree of volume reduction,
Vi = initial apparent volume,
Vp =powder volume under applied pressure Pa,
Vt = true volume,
a & b = constants.
 LIMITATION: Compaction process can be
described upto certain pressure, above which the
equation is no longer linear.
303004/21/16 Sagar KiShor Savale
Cooper and Eaton Equation.
Vi – Vp/ Vi– Vt = C2 exp (-K2/Pa ) + C3 exp (-K3/Pa)
C2,C3, K2,K3 = constants.
 LIMITATION : Applies only to single
component analysis.
313104/21/16 Sagar KiShor Savale
Energy expenditure.
323204/21/16 Sagar KiShor Savale
Crushing strength.
Compression force applied diametrically to tablet.
Measured by-
o Monsanto tester.
o Pfizer tester.
o Erweka tester.
o Schleuniger tester.
o Strongcobb tester.
Fracture across granule – size of granule influence
strength
3333
Fig:- pfizer tester.
04/21/16 Sagar KiShor Savale
Friability.
3434
• Measures the resistance for abrasion.
Parameter indicating tablet weight loss.
F = 100 x (1 – wo/w)
0.8% -1.0% upper limit for acceptance .
Fig:- Roche
friabilater
04/21/16 Sagar KiShor Savale
Lamination and Capping.
Laminating-
Separation of tablet into two
or more distinct layer.
Capping –
Partial or complete separation of
top and bottom crowns of tablet
from the main body.
353504/21/16 Sagar KiShor Savale
3636
REASONS FOR CAPPING AND
LAMINATING.
04/21/16 Sagar KiShor Savale
Minimizing capping and lamination.
 use of flat punch.
 use of tungsten carbide insert.
 proper set up of press.
 addition .
 use of binders.
373704/21/16 Sagar KiShor Savale
References:-
 Keith marshall 1987,Compression and consolidation of powderd solids,
Leon lachman, Herbert a.Liberman, & Joseph kanig ,The theory and
practice of industrial pharmacy, third edition varghese publication
house,bombay, pp.66,68,70-88.
 Eugene parrott , 2007,Compression,Herbert A.Liberman, Leon Lachman &
Joseph B.Schwartz ,Pharmaceutical dosage forms, tablets, volume
ii,pp.201-241.
 Stanforth J.N,Aulton’s pharmaceutics the design and manufacturing of
medicine,third edition,Churchill livingstone elsevier,pp.176,177.
 Subrahmanyam C.V. ,Micromeritics, Textbook Of Physical
Pharmaceutics, Second Edition,vallabh prakashan,delhi,Pp-180-234.
 Gilbert S. Banker , Christopher T. Rhodes, Modern
Pharmaceutics , Fourth Edition.Pp.408-409.
 encyclopedia of pharmaceutical Technology, Second Edition,volume-
3.Pp.303-305
383804/21/16 Sagar KiShor Savale
3904/21/16 Sagar KiShor Savale
4004/21/16 Sagar KiShor Savale
Thank YouThank You

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Compression and compaction

  • 1. 11 Department of Pharmacy (Pharmaceutics) | Sagar savale 04/21/16 Sagar KiShor Savale
  • 2. CONTENTS. Definition. Inherent properties of powder solids. Solid air interface. Angle of repose and flow rates. Mass volume relationship. Process of compression. 2204/21/16 Sagar KiShor Savale
  • 3. Die wall lubricant. Force and volume relationship. Heckel plot and kawatika equation. Compaction profile. Energy expenditure. Measurement of energy.  transmission of force.  force displacement curve. Strength of tablet and its estimation. References. 3304/21/16 Sagar KiShor Savale
  • 4. WHAT IS COMPRESSION ? Compression means reduction of bulk volume of material as a result of the removal of gaseous phase (air) by applied pressure WHAT IS CONSOLIDATION? Consolidation is an increase in mechanical strength of material resulting from particle - particle interactions. 4404/21/16 Sagar KiShor Savale
  • 5. WHAT IS COMPACTION ? The compression and consolidation of a two phase (solid + gas) system due to an applied force, resulting in the formation of a compact but porous mass of definite geometry. Compaction =compression + consolidation of two phases (solid-gas) on application of force. 5504/21/16 Sagar KiShor Savale
  • 6. Inherent properties of powder solids Solid –air interfaces. Angle of repose. Fixed funnel and free standing cone method. Tilting box method. Revolving cylinder method. Mass –volume relationships. Methods to mesure volume of powder.  Helium pycnometer  Liquid displacement method (specific gravity bottle method 604/21/16 Sagar KiShor Savale
  • 7. 7 Angle of repose. The maximum angle possible between the surface of pile of the powder and the horizontal plane. (also called as Dynamic angle) 704/21/16 Sagar KiShor Savale
  • 8. 8 METHODS TO MEASURE ANGLE OF REPOSE. a.Fixed funnel and free standing cone method. b.Tilting box method. c.Revolving cylinder method 04/21/16 Sagar KiShor Savale
  • 9. 9 FORMULA FOR MEASURING ANGLE OF REPOSE 1. θ = Tan-1 (h/r) here, h =height of pile r = radius of the base of the pile θ = angle of repose. 2. θ = cos-1 D/ (l1+l2) here, D = diameter of base l1+l2 = the opposite sides Angle of repose Flow property of powder <25 25-30 Excellent Good 30-40 Passable >40 poor 904/21/16 Sagar KiShor Savale
  • 10. 10 CONSOLIDATION INDEX (Carr, % ) FLOW 5-15 EXCELLENT 12-16 GOOD 18-21 FAIR TO PASSABLE 23-35 POOR 33-38 VERY POOR >40 VERY VERY POOR 1004/21/16 Sagar KiShor Savale
  • 11. 11 MASS-VOLUME RELATIONSHIPS. TYPE OF VOIDS OR AIR SPACES:  Open intraparticulate voids-  Closed intraparticulate voids-  Interparticulate voids- 11 Fig:- types of voids and air spaces. 04/21/16 Sagar KiShor Savale
  • 12. METHODS TO MEASURE VOLUME OF POWDER.  Helium pycnometer  Liquid displacement method (specific gravity bottle method) HELIUM PYCNOMETER Vt = Vc/U1-U2x[U1-Us] Vt = true volume of sample. Vc =true volume of stainless steel spheres. U1=Volume of empty cell. U1-U2=Volume occupied by the std. sample. U1-Us = volume occupied by sample. 121204/21/16 Sagar KiShor Savale
  • 14. Liquid displacement method. Solvent used are ---e.g., ethyl alcohol ,water, mercury , etc. Pycnometer or specific gravity bottle used. True density= w3/(w4-w2) = (w2-w1)/(w4-w2) w1 = wt. of Pycnometer w2 = Wt. of Pycnometer +sample or glass beads w4 = Wt. ofPycnometerwith powder & filled with solvent w3=w2-w1=Wt. of sample w4-w2=Volume of liquid displaced by the solid 141404/21/16 Sagar KiShor Savale
  • 16. Tablet Press Machine 1604/21/16 Sagar KiShor Savale
  • 17. . 17 The process of compression. 17 REMOVAL OF PRESSURE 04/21/16 Sagar KiShor Savale
  • 18. Deformation • The force required to initiate a plastic deformation is called as yield stress or elastic limit. 181804/21/16 Sagar KiShor Savale
  • 19. Effects of compression force. 19 INITIALLY REPACKING DEFORMATION 1904/21/16 Sagar KiShor Savale
  • 21. Fragmentation and deformation. Fragmentation do not occur when applied stress-  is balanced by a plastic deformation. change in shape. sliding of groups of particle (viscoelastic flow). 212104/21/16 Sagar KiShor Savale
  • 22. 22 If, only elastic deformation occurs – Under nonisostatic conditions- Uniaxial relaxation 2204/21/16 Sagar KiShor Savale
  • 23. Ejection. 2323 Portion under strain caps strain > shear strength. 04/21/16 Sagar KiShor Savale
  • 24. 3 stages of force necessary to eject a finished table, 1. Peak force required to initiate ejection. 2. Small force required to push tablet up to die- wall . 3. Decline force as tablet emerge from die. 242404/21/16 Sagar KiShor Savale
  • 25. Compression and consolidation under high loads. 2525 Thin layer is abrasion resistant but it – Retards air escape during compression. Retards the ingress of liquid media during dissolution. punch Die wall tablet 04/21/16 Sagar KiShor Savale
  • 26. Die-wall lubrication • Best lubricant has low shear strength & strong cohesive tendencies. • Lubricant forms a film of low shear strength at the interface between tabletting mass & die-wall. 2626 LUBRICANT SHEAR STRENGTH (M pa) Stearic acid 1.32 Calcium stearate 1.47 Magnesium stearate 1.96 Boric acid 7.16 graphite 7.35 04/21/16 Sagar KiShor Savale
  • 27. Force volume relationship. 2727 FIG. Decreasing porosity with increasing compressional force for single ended pressing i) initial repacking ii) Elastic deformation iii) Plastic deformation iv) compression End of compressional process is when bulk volume = tapped volume. porosity (E)= 0  Decrease in porosity is due to two process: 1. Filling of large spaces by Interparticulate Slippage. 2. Filling of small voids by deformation or fragmentation at high loads.  A more complex sequence of events during compression process involves four stage as shown in fig., 04/21/16 Sagar KiShor Savale
  • 28. Heckel plot. • It follows 1st order The pore in the mass are the reactant. log 1/E = KyP + Kr E = porosity P = Applied pressure Ky= material dependent constant Ky inversely proportional to it’s yield strength (S) (Ky = 1/3S) Kr = related to repacking stage & hence E0 For cylindrical tablet, P = 4F / ∏×D2 here, P = applied pressure D = tablet diameter F = applied compressional force 282804/21/16 Sagar KiShor Savale
  • 29. 2929 E = 100×[1 – 4w/ρt ×∏×D2×H] here, w = weight of tabletting mass. ρt = true density. H = thickness of tablet. •Type a : Soft material(e.g., NaCl) • Type b: Hard material(e.g., lactose) • Crushing strength of tablet is directly proportional to Ky. APPLICATION OF HECKEL PLOT: •Used to check lubricant efficacy. • For interpretation of consolidation mechanisms. •Duberg & nystom distinguish between plastic and elastic deformation characteristics of a material. 04/21/16 Sagar KiShor Savale
  • 30. Kawakita Equation. C = Vi – Vp/ Vt = abPa / 1+ bPa C = degree of volume reduction, Vi = initial apparent volume, Vp =powder volume under applied pressure Pa, Vt = true volume, a & b = constants.  LIMITATION: Compaction process can be described upto certain pressure, above which the equation is no longer linear. 303004/21/16 Sagar KiShor Savale
  • 31. Cooper and Eaton Equation. Vi – Vp/ Vi– Vt = C2 exp (-K2/Pa ) + C3 exp (-K3/Pa) C2,C3, K2,K3 = constants.  LIMITATION : Applies only to single component analysis. 313104/21/16 Sagar KiShor Savale
  • 33. Crushing strength. Compression force applied diametrically to tablet. Measured by- o Monsanto tester. o Pfizer tester. o Erweka tester. o Schleuniger tester. o Strongcobb tester. Fracture across granule – size of granule influence strength 3333 Fig:- pfizer tester. 04/21/16 Sagar KiShor Savale
  • 34. Friability. 3434 • Measures the resistance for abrasion. Parameter indicating tablet weight loss. F = 100 x (1 – wo/w) 0.8% -1.0% upper limit for acceptance . Fig:- Roche friabilater 04/21/16 Sagar KiShor Savale
  • 35. Lamination and Capping. Laminating- Separation of tablet into two or more distinct layer. Capping – Partial or complete separation of top and bottom crowns of tablet from the main body. 353504/21/16 Sagar KiShor Savale
  • 36. 3636 REASONS FOR CAPPING AND LAMINATING. 04/21/16 Sagar KiShor Savale
  • 37. Minimizing capping and lamination.  use of flat punch.  use of tungsten carbide insert.  proper set up of press.  addition .  use of binders. 373704/21/16 Sagar KiShor Savale
  • 38. References:-  Keith marshall 1987,Compression and consolidation of powderd solids, Leon lachman, Herbert a.Liberman, & Joseph kanig ,The theory and practice of industrial pharmacy, third edition varghese publication house,bombay, pp.66,68,70-88.  Eugene parrott , 2007,Compression,Herbert A.Liberman, Leon Lachman & Joseph B.Schwartz ,Pharmaceutical dosage forms, tablets, volume ii,pp.201-241.  Stanforth J.N,Aulton’s pharmaceutics the design and manufacturing of medicine,third edition,Churchill livingstone elsevier,pp.176,177.  Subrahmanyam C.V. ,Micromeritics, Textbook Of Physical Pharmaceutics, Second Edition,vallabh prakashan,delhi,Pp-180-234.  Gilbert S. Banker , Christopher T. Rhodes, Modern Pharmaceutics , Fourth Edition.Pp.408-409.  encyclopedia of pharmaceutical Technology, Second Edition,volume- 3.Pp.303-305 383804/21/16 Sagar KiShor Savale
  • 40. 4004/21/16 Sagar KiShor Savale Thank YouThank You