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COMPACTION,
COMPRESSION
&
CONSOLIDATION

 CONTENTS:
 Compression
 Consolidation
 Decompression
 Compaction of powders with a particular reference to
distribution and measurement of forces within the powder
mass undergoing compression
 COMPRESSION:
 Compression is the process of applying pressure to a material.
 In pharmaceutical tableting an appropriate volume of granules in a die cavity is compressed between
an upper and a lower punch to consolidate the material into a single solid matrix, which is
subsequently ejected from the die cavity as an intact tablet.
 COMPACTIBILITY:
 The ability of powder bed to cohere into or to form a compact or it is the ability of powder material
to be compressed in to a tablet of specified tensile strength.
 CONSOLIDATION:
 Consolidation is an increase in mechanical strength of material from particle- particle interaction.
Mechanism:
i. Cold welding
ii. Fusion welding
iii. Recrystallization
I. Cold welding:
 When the surface of 2 particles approach each other closely enough <50 nm, their energies result in
a strong attractive forces.
 This mechanisms is cold welding.
II. Fusion welding:
 When load is applied, frictional heat can be generated.
 If this heat is not dissipated, the local rise in temperature could be sufficient to cause melting of the
contact area of the particles, which would relieve the stress in that particular region.
 In that case, the melt solidifies giving rise to fusion bonding.
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III. Recrystallization:
 The actual solubility of solid also depends somewhat on the applied pressure, so that if a film of
moisture is present on the solid surface then the high pressure at the point solid contact could force
more material into solution.
 This dissolved solid would crystallize on relief of the applied stress to form a solid bridge whose
strength would partly depend on the rate of recrystallization.
 In general, slow rate should produce a more prefect crystal structure with consequent higher strength.
Factors Affecting Consolidation process:
 Chemical nature of material
 Extent of available surface
 Presence of surface contaminants
 Inter-surface distance
i. Chemical nature of material:
 The type and degree of crystallinity in a particular material influences its consolidative behaviour
under appreciable applied force.
 Substances possessing the cubic lattice arrangement were tableted more satisfactorily than those with
a rhombohedral lattice.
ii. Extent of available surface:
 The compressional process is affected by the extent of available surface.

Fig: Effect of increasing compressional force on specific area of powder mass


 When a powder mass is subjected to increasing compressional force, there is initial particle fracture,
which gives rise to increased surface area(O to A).
 At the point A, particles re-bonding becomes dominant factor, and from then on surface area
decreases unless tablet lamination begins.
iii. Presence of surface contaminants:
 The compressional process is affected by the extent of presence of surface contaminant.

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 For example, lubricants such as magnesium stearate form weak bond, so that over lubrication or even
over-mixing of lubricant into the tableting mass, results in a continuous coating of the latter, and
hence in some cases weak tablets are formed.
iv. Inter-surface distance:
 At the low level of external forces, molecular and electrostatic forces are source of attractive
tendencies between individual particles.
 Van Der Waal’s forces however may exert a significant effect at distance upto 100nm, so that once
an agglomerate of particles has been formed, they may serve to prevents its breakdown.
 COMPRESSION PROCESSES
 The various events that occur in the process of compression are,
A. Transitional repacking
B. Deformation at the points of contact
C. Fragmentation and/or deformation
D. Bonding
E. Deformation of the solid body
F. Decompression and
G. Ejection
A. Transitional repacking or Particle rearrangement:
 The particle size distribution of the granules and the shape of the granules determine the initial
packing (bulk density) as the granulation is delivered in to the die cavity.
 The granules flow with respect to each other, with the finer particles entering the void between the
larger particles, and the bulk density of the granulation is increased.
 Spherical particles undergo less particle rearrangement than irregular particles as the spherical
particles tend to assume a close packing arrangement initially.
 To achieve a fast flow rate required for high speed presses the granulation is generally processed to
produce spherical or oval particles.
 Particle rearrangement and the energy expended in rearrangement are minor considerations in the
total process of compression.
B. Deformation at the points of contact:
 When a stress is applied to a material, deformation (change of form) occurs.
 If the deformation disappears completely (returns to the original shape) upon release of the stress, it
is elastic deformation.
 A deformation that does not completely recover after release of the stress is known as a plastic
deformation.
 The force required to initiate a plastic deformation is known as the yield stress.

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 When the particles of granulation are so closely packed that no further filling of the void can occur,
a further increase of compressional force causes deformation at the points of contact.
 Both plastic and elastic deformation may occur although one type predominates for a given material.
 Deformation increases the area of true contact and the formation of potential bonding areas.
C. Fragmentation and/or deformation:
 At higher pressure, fracture occurs when the stresses within the particles become great enough to
propagate cracks.
 Fragmentation furthers densification, with the infiltration of the smaller fragments into the void
space.
 Fragmentation increases the number of particles and forms new, clean surfaces that are potential
bonding areas.
 In some materials fragmentation does not occur because the stresses are relieved by plastic
deformation.
 The influence of applied pressure on the specific surface area of sulfathiazole tablets is shown below,
the specific surface of the starch and sulfathiazole granulation was 0.18 𝑚 𝑔⁄; the tablet compressed
at a pressure of 1600 𝑘𝑔𝑐𝑚 ⁄ had a specific surface of 0.9 𝑚 𝑔⁄.

D. Bonding:
 Several mechanisms of bonding in the compression process have been conceived, but they have not
been substantiated by experimentation and have not been useful in the prediction of the
compressional property of material.
 The three theories which describe the bonding process are,
i. The mechanical theory,
ii. The intermolecular theory and
iii. The liquid surface theory.
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i. The Mechanical theory:
 It proposes that under pressure the individual particles undergo elastic, plastic or brittle
deformation and that the edges of the particles intermesh, forming a mechanical bond.
 If only the mechanical bond exists, the total energy of compression is equal to the sum of the
energy of deformation, heat and energy adsorbed for each constituent.
 Mechanical interlocking is not a major mechanism of bonding in pharmaceutical tablets.
ii. The Intermolecular theory:
 The molecules (or ions) at the surface of a solid have unsatisfied intermolecular forces (surface
free energy) which interact with other particles in true contact.
 According to the intermolecular theory, under pressure the molecule at the points of true contact
between new, clean surfaces of the granules are close enough so that Van der Waals forces
interact to consolidate the particles.
iii. The liquid surface theory:
 The liquid-surface film theory attributes bonding to the presence of a thin liquid film, which may
be the consequence of fusion or solution, at the surface of the particle induced by the energy of
compression.
 During compression an applied force is exerted on the granules; however, locally the force is
applied to a small area of true contact so that a very high pressure exist at the true contact surface.
 The local effect of a high pressure on the melting point and the solubility of the material is
essential for bonding.
 The relation of pressure and melting point is expressed by the Clapeyron equation,

Where, dT/dP = Change in melting point with change in pressure,


T = Absolute temperature,
ΔH = Molar latent heat of fusion,
V1 & Vs = Molar volume of the liquid melt and the solid respectively.
 If the pressure at the point of true contact is exerted only on the solid and the liquid phase is
subjected to a constant atmospheric pressure, the relationship simplifies to,

 Where, dT/dP is positive, regardless of the expansion or contraction of the solid, the pressure
acting locally at the point of true contact lowers the melting point.

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E. Deformation of the solid body:
 As the applied pressure is increased, the bonded solid is consolidated towards a limiting density by
plastic and/or elastic deformation of the tablet within the die.
 The effect of applied pressure on the apparent density of tablets of sulfathiazole is given below,

F. Decompression:
 The success or the failure to produce an intact tablet depends on the stresses induced by elastic
rebound and the association deformation process during decompression and ejection.
 Often, if capping or lamination of the eject tablet has occurred, the individual pieces are dense, hard
and strongly bonds indicating that sufficient areas of true contact existed during compression.
 As the upper punch withdraw from the die cavity, tablet is confined in the die cavity by a radial
pressure.
 Ideally, if only elastic deformation occurred, with the sudden removal of the axial pressure the
granule would return to their original form breaking any bonds that may have formed under pressure.
 Also the die wall pressure will be zero as the elastic material recovered axially and contracted
radially.
 As the movement of tablet is restricted by the residual die wall pressure and friction, the stress from
axial elastic recovery and radial contraction cause capping.
 Capping is due to uniaxial relaxation in the die cavity at the point where the upper punch pressure is
release.
 If decompression occurs simultaneously in all directions capping is reduced.
 Stress relaxation of plastic deformation is time dependent.
 Material having slow rates of stress relaxation crack in the die upon decompression.
 In fig, the ratio of pressure at time to the maximum pressure is plotted against the logarithm of the
time.
 The change of the initial slope suggest some prominent mechanism of bonding soon becomes
negligible.

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 The initial slope reflects the ability of the material to relieve stress during decompression.
 The rate of stress relieve is slow for acetaminophen so cracking occurs while the tablet is within the
die.
 With microcrystalline cellulose the rate of stress relieve is rapid and intact tablets result.

 If stress relaxation is slow and cracking is a problem, a slower operation speed provides more time
for stress relaxation.
 A tablet press that provide pre-compression allows some stress relaxation before the final
compression.
 To optimized the stress relaxation, before final compression the pre-compression pressure should be
approached the maximum pressure.
G. Ejection:
 As lower punch rises and pushes the tablet upward there is continue residual die wall pressure and
energy must be expanded due to die wall friction.
 As the tablet is removed from the die, the lateral pressure is relieved, and tablet under goes elastic
recovery with increase in volume of that portion of the tablet removed from the die.
 During the ejection that portion of the tablet within a die is under strain, and if this strain is exceed
the share strength of the tablet, the tablet caps adjacent to the region in which the strain had just been
removed.
 DESCRIPTION OF PROCESS (IN BRIEF):
 The process of compression has been described in the terms of relative volume and applied pressure.

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 In transitional repacking the granules are packed to an arrangement in which the particles are
immobile and the number of inter-granular points of contact has increased.
 The decrease in the relative volume during transitional repacking is represented by the segment AE.
 With the further increase in the pressure, temporary supports between the particles are formed as
represented by segment EF.
 Fragmentation and or plastic deformation is represented by segment FG.
 As some higher pressure bonding and consolidation of solid occur to some limiting value as indicated
by segment GH.
 FORCE DISTRIBUTION:
 Tablet strength can be found:-
“Particle deformation whether plastic or elastic will be proportional to applied force. The
porosity of tablet &hence its strength. The weakest points in tablet structure will be those that receive
the lowest forces”
FA = FL + FD
Where, FA = Force applied to the upper punch.
FL = Proportion of it transmitted to the lower punch
FD = Reaction at the die wall due to friction at this surface

FM =FA+FL/2
Where, FM = Mean compaction force.
MEASUREMENT OF FORCE:
 Instrumentation:
1. Strain gauge
2. Piezo electric transducer
3. LVDT (linear variable differential transducer)
1. Strain gauge:
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 It is the coil of highly resistant wire mounted on paper backing.
 During compression the force applied cause a very small elastic deformation of two punches.
 If suitable strain gauge is firmly bound to the punch shank as close to the compression site as
practical, it is deformed as the punch is deformed.
 Due to deformation, there is a change in wire resistance as it decrease and the diameter is
increased.
 The resultant decrease in electrical resistance can be measured by wheat stone bridge.
2. Piezo electric transducer:
 When Piezo-electric material is subjected to external force these material develop an electric
charge proportional to force.
 This transducer is connected by a high impedance cable to a charge amplifier which converts the
charge into correctly proportional to dc voltage.
3. Linear variable differential transducer (LVDT):
 Punch displacement is based on differential inductor principle.
 Ferrous core of the transducer is rigidly connected to punch by link, so that movement of punch
unbalances the secondary circuit, the output is attenuated to produce dc voltage which is directly
proportional to displacement.

 REFERENCES
 Leon Lachman; Herbert A. Lieberman: Theory and practice of Industrial pharmacy; Special

Edition 2009.

 E.A. Rawlins: Bentley’s textbook of pharmaceutics; 8TH edition.

 Herbert. A. Lieberman, Leon Lachman: Pharmaceutical dosage forms; Tablets-Vol. 2; 2ND edition

2005.

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