Properties and

Parameters of the Powders

• Powders consist of solid particles surrounded by spaces filled with fluid
(typically air) and uniquely possess some properties of solids, liquids, and
gases.
• Powdered solids are heterogeneous. They are composed of individual
particles of widely differing sizes and shapes, randomly interspersed with
air spaces.
• Physical properties of the powders predict the flow properties, flowability
and their compressibility.
• The uniform flow of the powder mixture is a vital parameter for
maintaining the consistency of the tablet weight and the uniformity of the
content of the tablets.
Classification of Powders
Classification of powders based on dispensing:
• Bulk powders
• Divided powders
Classification of powders based on particle size:
• Very coarse (No. 8) powder
• Coarse (No. 20) powder
• Moderately coarse (No. 40) powder
• Fine (No. 60) powder
• Very fine (No. 80) powder: All particles pass through a No. 80 sieve
Powder Compaction
• Compaction can be defined as the compression and consolidation of
a two-phase (particulate solid-gas) system due to the applied force.
• Compression is the reduction in the bulk volume (Vb) of the material
as a result of displacement of the gaseous phase.
• Consolidation is an increase in the mechanical strength of the
material resulting from particle/ particle interactions.
Powder Technology
• Cohesion – attraction between like particles
• Adhesion – attraction between unlike particles
• Interparticle contacts
• Solid/ fluid interactions
• Adhesion of the unlike particles generates the resistance to
differential movement of their constituent particles when subjected
to external forces.
• The overall resistance to the relative movement of particles may be
markedly affected by electrostatic forces and the presence of an
adsorbed layer of moisture on the particles.
Inter-particular forces
• The interarticular forces are roughly classified according to their origin
as Electrostatic interactions and Molecular interactions.
• Many powders of pharmaceutical interest readily develop
electrostatic forces, especially when subjected to internal friction.
• The electrostatics forces are relatively small, but significant because
they act over the distance than the molecular forces do.
• The molecular interactions are secondary bonds or van der Waals
attractions that can be classified as ion-dipole, dipole-dipole, or van
der Waals-London interactions.
Electrostatic interactions
• The electrostatic interactions between powder particles can be
described using Coulomb’s Law.
Electrostatic interactions
• Particles with highly polar surfaces have, under normal conditions, a
water sorption layer that can distribute the transferred charge over
the surface.
• The thicker this layer, the higher its conductivity and the more easily
this charge distribution is affected on the surface.
• The distribution becomes relatively homogeneous on the surface of
an amorphous spherical particle.
Electrostatic interactions
• But in the case of crystalline non-
spherical particles, especially of
milled crystals with pointed
edges, extremely high values of
charge will be concentrated in
the tops of the edges.
Electrostatic interactions
Tribo-electrostatic
Charge:
• An intensive
movement of the
material causing a
charge transfer is
called a tribo-
electrostatic charge
transfer.
Electrostatic interactions
Permanent Electrostatic Charge:
• The permanent electrostatic charge occurs as a consequence of the
surface structure of the powder.
• Unlike amorphous materials, the surface of a crystalline material is
not uniform.
• Each face has its own energy level, its own surface or interface
tension and with the presence of polar functional groups, its own
polarity.
Electrostatic interactions
Permanent Electrostatic Charge:
• Due to the special chemical and crystallographic state of the surface
of solid particles, surfaces can be charged, even if each particle in
total is neutral.
• Amorphous materials also may have uniform charged ions on their
surface which are responsible for electrostatic attractions or
repulsions.
• A crystalline material with highly ordered functional polar groups can
also be the reason for a permanent charge on the surface.
Solid/ fluid interactions
• Atoms or ions located at the surface of any solid particle are exposed
to a different distribution of intramolecular and intermolecular
bonding forces than those within the particle.
• The free surface energy of the solid, which plays a major role in the
interaction between particles, and between a particle and its
environment.
• Particles with highly polar surfaces have, under normal conditions, a
water sorption layer that can distribute the transferred charge over
the surface.
Solid/ fluid interactions
• An adsorbed layer of moisture
reduces the chance of any
complicating electrostatic effect by
providing a conducting path for
charge dissipation.
• These films of moisture can form
liquid bridges which hold the
particles together by surface tension
effects and by negative capillary
pressure.
Solid/ fluid interactions
• When the surface free energy of the solid is high, it is usually easily
wetted by any liquid.
• A wetted powder contains, in addition to the sorption water, water as
a separate phase, with the typical properties of a liquid.
• If the angle of contact between the water and the surface is small, a
limited amount of water takes a preferred place in the inter-particular
contact regions with the formation of a meniscus.
Solid/ fluid interactions
Flow properties & Flowability
• While flow properties are independent of the equipment in which
they were determined, the term flowability always is connected with
the equipment and how it was tested.
• Inter-particulate attractions in any case make the flow properties
worse.
• On the other hand, electrostatic repulsions may facilitate the flow of a
powder bed.
• Despite this, tribo-electrostatic charges should be avoided, especially
for powders provided for direct compression to tablets or capsule
filling.
Flow properties & Flowability
• The tribo-electrostatic charge is not reproducible, does not distribute
homogeneously within a batch of a powder, and changes rapidly
during storage and the operation of tablet compression.
• Because of this the tribo-electrostatic charge influences negatively
the uniformity of the bulk density and with this the uniformity of
dosage.
• Depending on the composition of the powder mixture and the
intensity of the movement, one can observe an increase in the bulk
density and a decrease in the flowability.
Flow properties & Flowability
• There are various ways to diminish the tribo-electrostatic charge
transfer or to discharge the material.
• The powder should have a sufficiently polar surface and a water
sorption layer.
• The polarity of the surface can be enhanced by small concentrations
of excipients.
• Tribo-electrostatic charged materials can be discharged by treatment
with ionized air.
Flow properties & Flowability
• All charges discussed, which are located in the particle surface
independent of their nature—can be compensated by the addition of
amphiphilic excipients.
• These considerations show that the normally used excipients in
powder technology (e.g., lubricants) diminish the negative influence
of the charges.
• But they demonstrate also that after the treatment of a powder with
these excipients, intensive powder movements must be avoided.
Powder Properties & Flowability
• Flowability increases with decreasing width of the particle size
distribution (PSD).
• Flowability generally improves with coarser particles.
• Flowability decreases with increasing moisture content until
saturation with liquid.
Powder Parameters
Flow property and compressibility of the powdered materials used in
the pharmaceutical industry can be measured in terms of various
parameters:
• Hausner’s ratio (HI)
• Carr’s index (CI)/ Compressibility index (CI)
• Angle of repose (α)
• Particle size distribution
Hausner’s ratio & Compressibility index
• Values of I below 15% usually give rise to good flow characteristics,
but readings above 25% indicate poor flowability.
Angle of repose (α)
• Angle of repose is a characteristic related to inter-particulate friction
or resistance to movement between particles.
• It is the constant, three-dimensional angle (relative to the horizontal
base) assumed by a cone-like pile of material formed by any of several
different methods (USP or BP methods).
• There are two variation methods are described in the USP to
determine the Angel of repose: Drained angle of repose and Dynamic
angle of repose.
Angle of repose (α)
Angle of repose (α)
The dynamic angle of repose:
• The dynamic angle method was most preferred since it closely mimics
the manufacturing situation in which the powder is in motion.
• A typical dynamic test involves a hollow cylinder half-filled with the
test powder, with one end sealed with a transparent plate.
• The cylinder is rotated until the powder surface cascades.
Angle of repose (α)
• Alternatively, resistance to the movement of particles, especially for
granular powders with little cohesiveness, may be assessed by
determining their flow rate (Q) through a circular orifice (a tablet die,
for instance) fitted in the base of a cylindric container.
• Flow experiments with mixtures of different size fractions of the same
material can be particularly valuable because, in many instances,
there exist optimum proportions that lead to a maximum flow rate.
Particle Size Distribution (PSD)
• Small particles (<20 μm) have a relatively high surface area to volume
ratio, causing inter-particulate attractive forces to dominate and
resist bulk flow when a shear stress is applied.
• Very fine particles possess attractive forces such as Van Der Waals,
electrostatics, surface tension etc. resulting cohesion of powder and
poor flow properties.
• As particle size increases, the flow of the powders also increases and
after a certain level works as free-flowing.
• Appropriate blend of coarse and fine particles or in other words the
selection of particle size distribution improves the flow properties.
Particle Size Distribution (PSD)
• Particle size distribution is a
measurement that defines
the number of particles
present according to their
size.
• In the pharmaceutical sector,
it is the width of the
distribution curve that is of
most importance.
Particle Size Distribution (PSD)
• The key measurements that we use in
setting up the Quadro Mills is to cite three
values—the D10, D50 and D90 as shown in
Figure.
• The D50, the median, is defined as the
particle size where half the population lies
below this value.
• Similarly, 90 percent of the population lies
below the D90 point, and 10 percent of the
population lies below the D10.
Powder Compaction Process
• Tablets usually have smooth surfaces, low friability, and sufficient
strength (e.g., tensile strength or hardness).
• For the production of such tablets, the compressional stress σc needs
to be significant enough to induce plastic flow and/ or brittle fracture
of the primary granules to produce simultaneously new surfaces and
bonds in this dense powder compact.
• Compactibility is the ability of a material to yield a compact with
adequate strength.
Mechanical Properties of Particles
• Elastic and plastic deformations are mechanical properties of
particles, in addition to brittle fracture.
• Plastic deformation is an irreversible process causing permanent
alterations of the particle shape.
• Elastic deformation is a reversible process causing non-persistent
alterations of the particle shape.
• Inherent plastic material deformation is characterized by particle
yield stress (σy ) which is the stress required to induce plastic flow.
• A high deformation propensity is often correlated with a high intra-
granular porosity due to the large available space for plastic flow.
Mechanical Properties of Particles
• The elastic material properties are usually defined by Young’s
modulus E (Hooke’s law of elasticity), and Poisson’s ratio (ν).

• These quantities are measures of the elastic stiffness and the lateral
expansion, respectively of the material during load.
• Stiffness is the extent to which an object resists deformation in
response to an applied force.
Mechanical Properties of Particles
Pressure-Density Relationship
• Traditionally pharmaceutical powder compaction is analyzed based
on pressure–density relationships obtained from the compaction of a
tablet.
• This analysis addresses the applied pressure and the resulting density
as an average magnitude without any regard to variations within the
tablet.
Powder Compaction Process
• Particle rearrangement
• Elastic deformation of
particles
• Plastic deformation of
particles
• Fragmentation of
particles
• Formation of inter
particulate bonds
Powder Compaction Process
Powder Compaction Process
Deformation
• When any solid body is subjected to opposing forces, there is a finite
change in its geometry, depending upon the nature of the applied
load.
• The relative amount of deformation produced by such forces is a
dimensionless quantity called strain.
• The ratio of the force F necessary to produce this strain to the area A
over which it acts is called the stress (σ).
Stress (σ) = F/A
• Three types of forces bring out the deformation of a powder bed:
Tensile strain, Compressive strain, Shear strain.
Deformation
• If a solid rod is
compressed by forces
acting at each end to
cause a reduction in
length of Н from an
unloaded length of Ho,
then the compressive
strain (Z) is given by:
Tensile strain Compressive strain Shear strain
Strain (Z) = ΔH/ H0
Deformation
• Temporary deformation is called elastic deformation, while
permanent deformation is called plastic deformation.
• Time-dependent recoverable deformation under load is called
anelastic deformation, while the characteristic recovery of temporary
deformation after removal of load as a function of time is called
elastic aftereffect.
• Change over from elastic state to plastic state is characterized by the
yield strength (σ0) of the material.
Deformation
• The phenomenon of gradually increasing strain under constant stress
is called creep, while the phenomenon of gradually diminishing stress
under constant strain is called stress relaxation.
• Materials deviating from ideality may not be able to recover their
deformation instantaneously and/or completely upon the removal of
stress and are called viscoelastic materials.
• Viscoelasticity is the property of materials that exhibit both viscous
and elastic characteristics when undergoing deformation.
• The strain in viscous materials is non-recoverable upon the removal of
stress.
Deformation
• Applied external forces on the powder reduce the bulk volume of the
powder.
• Bulk volume reduction in these cases results from repacking, plastic
deformation and consolidation of the particles.
• This mechanism predominates in materials in which the shear
strength is less than the tensile or breaking strength.
• when the shear strength is greater, particles may be preferentially
fractured, and the smaller fragments then help to fill up any adjacent
air space.
Deformation
• This is most likely to occur with hard, brittle particles and is known as
brittle fracture (Sucrose behaves in this manner).
• Irrespective of the behavior of large particles of the material, small
particles may deform plastically, a process known as micro-squashing,
and the proportion of fine powder in a sample may therefore be
significant.
• If the dwell time under the compressive load is prolonged, the
deformation may continue, leading to more consolidation.
• Dwell time is the time that the punch head remains in contact with
the compression roller.
Formation of inter particulate bonds
• Solid bridges
• Moveable liquids
• Non–freely moveable binders
• Attraction between solid particles
• Mechanical interlocking

While all these bindings are significant, solid bridge formation,

intermolecular forces, and mechanical interlocking are dominant.
Formation of inter particulate bonds
• Solid bridges are formed between two particles by processes such as
crystallization, sintering, or chemical reactions (such as salt formation
between adjacent particles).
• Bonding between moveable liquids is related to surface tension
forces. As compaction is assisted by the presence of some moisture,
this may well play a role in the process for tablets.
• Non–freely moveable binders would include the binders used in wet
granulation processing, such as polyvinylpyrrolidone, which make
powders into better compact formers.
Consolidation
• Consolidation is an increase in the mechanical strength of the
material resulting from particle-particle interactions.
• When the surfaces of two particles approach each other closely
enough, their free surface energies result in a strong attractive force,
a process known as cold welding.
• Any applied load to the powder bed must be transmitted through
these particle contacts.
• Under appreciable forces, this transmission may result in the
generation of considerable frictional heat.
• Frictional heat can cause melting of the contact area of the particles.
Consolidation
• The melt solidifies giving rise to fusion bonding, which in turn results
in an increase in mechanical strength of the mass.
• Many pharmaceutical solids possess a low specific heat and poor
thermal conductivity so heat transfer away from the contact points is
slow.
• The differences between this form of bond formation and cold
welding are somewhat pedantic and the end results are essentially
the same.
• In both cold and fusion welding, the process is influenced by several
factors: the chemical nature of the materials, available surface area,
presence of surface contaminants and the inter-surface distances.
Consolidation
• During normal tableting operations, consolidation is accentuated in
those regions adjacent to the die wall, owing to the intense shear to
which material is subjected, as it is compressed axially and is pushed
along the wall surface.
• This consolidation results in a “skin” of material that is denser over
the lateral tablet surface than in the rest of the tablet mass.
Consolidation
The predominant consolidation mechanisms:
• Mechanical theory: As the particles undergo deformation, the particle
boundaries intertwine to form mechanical bonds.
• Intermolecular forces theory: van der Waals forces bond the molecules
together at the newly sheared surfaces of the particle boundaries e.g.,
MCC undergoes significant hydrogen bonding during tablet compression.
• Liquid-surface film theory: Thin liquid films form which bond the particles
together at the particle surface. The energy of compression produces
melting or solution at the particle interface followed by subsequent
solidification or crystallization thus resulting in the bonded surfaces.
Mechanical theory
The effect of increasing compressional
force on the specific surface area of a
powder mass:
• When a powder mass is subjected to
O; increasing compressional force,
there is an initial particle fracture,
which gives rise to increased surface
area (O to A).
Mechanical theory
The effect of increasing compressional
force on the specific surface area of a
powder mass:
• At some point around A, particle re-
bonding becomes the dominant factor,
and from then on, the surface area
decreases (region A to B) unless tablet
lamination begins.
• After point B, lamination of the tablet
structure happens if considerable elastic
recovery on decompression takes place.
Liquid-surface film theory
• The actual solubility of solids also depends somewhat on the applied
pressure, so that if a film of moisture is present on the solid surface,
then the high pressures at points of solid contact could force more
material into the 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 this recrystallization.
• In general, slow rates should produce a more perfect crystal structure
with consequent higher strength.
Liquid-surface film theory
• At least some moisture is present
in virtually all capsule and tablet
formulas.
• concentrations well below the 1%
level can dramatically affect the
behavior of these feed materials
and that of the finished product.
Frictional Forces
• Depending on the motion, there are two types of frictional forces:
sliding motion – tangential force, rotational motion – torque force
• The resistance to differential movement of particles caused by their
inherent cohesiveness results in the applied force not being
transmitted uniformly throughout the entire mass.
• The discrepancy between the two punch forces should be minimized
in pharmaceutical tableting operations so that there is no significant
difference in the amount of compression and consolidation between
one region of the tablet and another.
Force Distribution
• The force exerted by the upper punch
diminishes exponentially at increasing
depths below it.
• Thus, the relationship between upper
punch force FA and lower punch force
FL can be expressed as:
• The values H and D are the height and
diameter of the tablet, respectively.
Frictional Forces
• Two major components of the frictional
forces can be distinguished.
• Inter-particulate friction arises at
particle-particle contacts and can be
expressed in terms of a coefficient of
inter-particulate friction μ1
• Die-wall friction results from the material
being pressed against the die wall and
moved down it and it is expressed as μ2,
the coefficient of die-wall friction.
Frictional Forces
• Inter-particulate friction is more significant at low applied loads.
• Die-wall friction effect becomes dominant at high applied forces
when particle rearrangement has ceased.
• Materials that reduce the Inter-particulate friction effect are referred
to as glidants. Colloidal silica is a common example.
• Most tablets contain a small amount of lubricant to reduce die-wall
friction. Magnesium stearate is a common choice.
• Having a smaller tablet height-to-diameter ratio also helps reduce die-
wall friction.
Force Distribution

• FD is a reaction at the die wall due to friction at

this surface.
• Because of this difference between the force
applied at the upper punch and the lower
punch, a mean compaction force FM has been
proposed.
Force Distribution
• In single-station presses, where the applied
force transmission decays exponentially as in
the equation, a more appropriate geometric
mean force FG has been proposed.
Radial Die-wall Force
• In the tableting process, compressive force
applied in the vertical direction results in a
decrease ΔН in the height.
• In the case of an unconfined solid body, this
would be accompanied by an expansion in the
horizontal direction of ΔD.
• The ratio of these two-dimensional changes is
known as the Poisson ratio λ of the material.
Radial Die-wall Force
• When the material is not free to expand in
the horizontal plane because it is confined in
the die, a radial die-wall force FR develops
perpendicular to the die-wall surface.
• Materials with larger Poisson ratios give rise
to higher values of FR.
Force Distribution
• Axial frictional force FD is related to FR by the
expression:

• μw is the coefficient of die-wall friction

• The frictional effect represented by μw arises
from the shearing of adhesions that occurs as
the particles slide along the die wall.
Ejection Forces (Fe)
• The force necessary to eject a finished tablet follows a distinctive
pattern of three stages.
• The first stage involves the distinctive peak force required to initiate
ejection, by breaking of tablet/ die-wall adhesions.
• A smaller force usually follows to push the tablet up the die wall.
• The final stage is marked by a declining force of ejection as the tablet
emerges from the die.
Ejection Profile

• Point A = the static ejection force (Fse)

Ejection Forces (Fe)
• For a constant applied compaction pressure, the ejection pressure
can be given by:

• H = compact height
• D = diameter
• Te = mean interface shear stress acting on the surface in contact with
the die wall
Ejection
• It is at this point that the compact can suffer mechanical failure
because of the release of stored energy.
• Radial die-wall forces and die-wall friction also affect the ease with
which the compressed tablet can be removed from the die.
• Including a lubricant in a formulation to reduce friction at the die wall
minimizes the potential for failure of the compact structure during
the ejection process.
Lubricants
• Die-wall lubricants function by interposing a film of low shear
strength at the interface between the tableting mass and the die wall.
• Preferably, there is some chemical bonding between this “boundary”
lubricant and the surface of the die wall as well as at the edge of the
tablet.
• The best lubricants are those with low shear strength but strong
cohesive tendencies in directions right to the plane of shear.
• By utilizing materials with low shear strength as lubricants, shear
failure occurs in the lubricant layers and not at the compressed
powder or resultant wall interfaces.
Lubricant Efficiency
• Lubricant efficiency/ degree of lubrication is given by the coefficient
of lubricant efficiency or R-value.

• The ratio approaches unity for perfect lubrication (no wall friction),
and in practice, values as high as 0.98 may be realized.
• Values below 0.8 probably indicate a poorly lubricated system.
• Values of R should be considered as relating only to the specific
system from which they were obtained, because they are affected by
other variables, such as compressional force and tablet H/D ratio.
Summary of compaction properties
- Alternatively, the changing at relatively low compaction forces thickness of the
tabletting mass due to the compactional force, and subsequently due to elastic
recovery during unloading, can be used to obtain a measure of plastoelasticity ϒ：

ϒ=
where Ho, Hm, and Hr are the thickness of the tablet mass at the onset of loading, at
the point of maximum applied force, and on ejection from the die, respectively.
➢A linear relationship between у and log reciprocal of the tensile strength of the
tablets has been demonstrated.
➢In general, values of ϒ above 9 tend to produce tablets that are laminated or
capped.
 STRENGTH OF TABLETS
- The mechanical strength of tablets has been described in a
variety of ways, including hardness, bending strength, fracture
resistance, friability, and crushing strength.
- The most popular estimate of tablet strength has been crushing
strength, Sc, which may be defined as “that compressional force
(Fc) which, when applied diametrically to a tablet, just fractures
it.

where ST is the tensile strength, and D and H are the diameter and
thickness of the tablet, respectively.
 STRENGTH OF TABLETS

The work Wf required to cause tablet failure correlates better

with other mechanical strength tests and is a more sensitive
parameter for comparison with other tabletting parameters.
Wf is obtained from the equation:

where F is the force applied to the tablet and z, the

deformation resulting from it, is represented by the relative
displacement of the anvil and plunger.
 Determination of brittle fracture index (BFI)
Crack theory can be used to develop a quantitative expression for the
measurement of the brittle fracture tendency;

Where, To and T are the tensile strengths of tablets with and without
a central hole, respectively.
• The BFI value thus has a range of 0 (no fracture tendency) to 1
(maximal fracture tendency).
 Compression Cycle
Powder compression can be divided to
few phases accordingly to the time of
the compression.
These are:
(i)Consolidation time: time to reach
maximum force.
(ii) Dwell time: time at maximum force.
(iii)Contact time: time for compression
and decompression excluding ejection
time.
(iv)Ejection time: time during which
ejection occurs.
(v)Residence time: time during which
the formed compact is within the die.

The materials with higher К values undergo more plastic flow; such materials often form strong tablets.
 Compression Cycle
The force-time profile gives
information about these phases as
well as various characteristic
parameters of the compression cycle.
➢Consolidation time is the time to
reach maximum force.
➢dwell time is the time at puncher
no longer experience vertical
displacement .
➢contact time is the time for
compression and decompression. Some researchers have defined dwell time as an interval
during which maximum compaction pressure is
maintained by the punches during the compaction cycle
 Compression Cycle
➢The decompression stage is as important as (but not
independent of) the compression stage in determining
whether or not a tablet formulation will form
satisfactory tablets.
➢Some deformation processes are time-dependent and
occur at various rates during the compaction
sequence, so that the tablet mass is never in a state of
stress/strain equilibrium during the actual tabletting
process.
 Compression Cycle
➢The rate at which load is applied and removed may be a critical
factor in materials for which dependence time is significant.
➢More specifically, if a plastically deforming solid is loaded (or
unloaded) too rapidly for the process to take place, the solid may
exhibit brittle fracture.
➢ In view of this, research investigations in recent years have shifted
to relating the capping and lamination tendenciesof tablet
formulations to their plastic and elastic behavior during the
compression/ decompression/ ejection cycle.
FORCE-VOLUME RELATIONSHIPS IN THE COMPRESSION
- The end of the compressional process may be recognized as being the point
at which all air spaces have been eliminated.
The decreasing porosity resulted from a two-step process:
1. The filling of large spaces
2.The filling of small voids by deformation or fragmentation at higher loads.

In the area of pharmaceutical

powder technology, the global
models of Heckel and Kawakita have
typically been the most frequently
used model to describe the F-V-P
relationship during the compression.
 THE HECKEL EQUATION

- The equation is based on the assumption that compression of

powders is analogous to a first-order chemical reaction, the pores
being the reactant and densification of the bulk being the product.
- The equation was first developed and applied on compression of
metals, materials known to deform predominately plastically.
 THE HECKEL EQUATION

where E is the porosity of the powder bed and P the applied compression pressure,
A and k are materials dependent parameters.
For a cylindric tablet, P is given by：

where D is the tablet diameter, F - force.

D
Similarly, values of E can be calculated for any stage from：
H
w

where w is the weight of the tabletting mass, is its true density, and H is the thickness of
the tablet at that point (obtained from the relative punch displacement measurements).
 THE HECKEL EQUATION
In 1961, Heckel proposed a relationship between
the constant K and the yield strength for a range
of metal powders.
K = 1/3 σ
where, σ is the yield strength of the material. K is
inversely related to the ability of the material to
deform plastically.

Yield strength is defined in engineering as the amount of stress

(Yield point) that a material can undergo before moving from elastic
deformation into plastic deformation.
Yielding - a material deforms permanently
 THE HECKEL PLOT
A Heckel profile is normally distinguished by
three different regions,
➢ an initial nonlinear part (Region I),
➢followed by a linear part where the data
obey the expression (Region II),
➢ finally, a non-linear region (Region III) .
Heckel parameters have been shown to be
more dependent on the compression–
decompression cycle than on the size of die.
A typical Heckel plot
 THE HECKEL PLOT
➢The crushing strength of tablets can be correlated with the value of Ky
of the Heckel plot; larger values of Ky usually indicate harder tablets.
➢Such information can be used as a means of binder selection when
designing tablet formulations.
➢Note that Heckel plots can be influenced by the overall time of
compression, the degree of lubrication, and even the size of the die, so
that the effect of these variables should be considered.
➢Another important factor in the use of all force-porosity relationships is
that for many formulations, there is a relatively narrow optimum
residual porosity range that provides adequate mechanical strength,
rapid water uptake, and hence, good disintegration characteristics.
➢The initial porosity can affect the course of the entire compressional
sequence, and that in general, slow force application leads to a low
porosity for a given applied load.
 THE KAWAKITA EQUATION
- Another way of representing compression data is to relate the volume
reduction (engineering strain) of a powder bed to the applied pressure, and
the most familiar expression in this class is the Kawakita equation.

𝟎
C=
𝟎
Where C is the degree of volume reduction, (where V0 is the initial volume of
the powder bed and V is the volume under applied pressure), P is the applied
Axial pressure, and a and b are parameters.
The Kawakita equation is often considered to be best suited for analysis of soft,
fluffy powders compressed under low pressures.
 THE KAWAKITA EQUATION

- The physical interpretation of the Kawakita parameters has been discussed

in the literature, and the inverted b-parameter is claimed to reflect the
agglomerate strength, fracture strength of single particles or the plasticity
of a granule.
- The physical interpretation of the b-parameter in terms of bulk powders
have been more complicated to address, represent a resistant towards
compression.
- The Kawakita equation may also be applied to tapping of bulk powders, as a
measure of fluidity and cohesion, replacing the pressure term (P) in Eq by N
– the tapping number.

-
 COMPACTION PROFILES
• The powder particles during compression is governed by factors
such as pressure (or stress), the amount of deformation (or
strain), and the rate of deformation (or strain rate) at the
particulate level.
 Compaction Profile
➢The value of the material modulus of elasticity (Young’s Modulus)
value is low, there is the danger of structural failure.
➢Maximum compressional force level are particularly important in
such case, since most of the stored energy is released on removal
of the applied load.
➢If modulus of elasticity is high, there is a small dimensional
change on decompression and less risk of failure.
 Compaction Profile

Examples of compaction profiles. Dotted line 0 to A represents a highly variable response due to repacking, while at A,
elastic deformation becomes dominant and continues until the elastic limit В is reached. From В to the point of maximum
compression C, deformation is predominantly plastic, or brittle fracture is taking place. The decompression process C to D
is accompanied by elastic; recovery, and if a second yield point (D) is reached, by plastic deformation or brittle fracture D
to E. The decompression line В to C' represents the behavior of a largely elastic material.
 Compaction Profile
• In many tabletting operations, the applied force exceeds
the elastic limit (point B), and brittle fracture and/or
plastic deformation is then a major mechanism.
• For example, if the material readily undergoes plastic
deformation with a constant yield stress as the material is
sheared, then the region В to C should obey the equation
：
PR = PA - 2S
where S is the yield strength of the material.
• Note that the slope of BC line plot is unity, so that marked
deviation from this value may indicate a more complex
behavior.
• Deviation could also be due to the fact that the material is
still significantly porous
 • Perhaps the residual radial pressure (intercept
EO when all the compressional force has been
removed, is more significant, since this
pressure is an indication of the force being
transmitted by the die wall to the tablet.
• As such, it provides a measure of possible
ejection force level ( ) and likely lubricant
requirements； if pronounced, it suggests a
strong tablet capable of at least withstanding
such a compressive pressure.
• Conversely, a low value of residual radial pressure, or more significantly, a
sharp change in slope (DE) is sometimes indicative of at least incipient failure
of the tablet structure.
• In practical terms, this may mean introducing a plastically deforming component (e.g., PVP
[polyvinyl pyrrolidone] as binder, starch as diluent) to facilitate dissipation of these stresses,
and hence a more gradual change in slope of the decompression plot, a preferred feature.
 ENERGY INVOLVED IN COMPACTION
• Tablet machines, roll compactors, extruders, and similar types of
equipment require a high input of mechanical work.
The work involved in various phases of a tablet or granule compaction
operation includes
(1) that necessary to overcome friction between particles,
(2)that necessary to overcome friction between particles and machine
parts,
(3)that required to induce elastic and/or plastic deformation of the
material,
(4) that required to cause brittle fracture within the material,
(5)that associated with the mechanical operation of various machine
parts.
 WORK OF COMPACTION
• The three main deformation mechanisms that can occur to particles
within the powder bed are elastic deformation, plastic deformation
and fragmentation.
• Elastic deformation is reversible, i.e. the work stored during loading is
recovered during unloading.
• However, a material with time-dependent properties can store elastic
energy and may relax only after a period of time or after ejection from
the die.
• The energy required to cause plastic deformation or fragmentation
cannot be recovered, as these are permanent changes to the structure
of the particle.
 • A typical plot of the force exerted by the
upper punch against the displacement of
the upper punch is shown in Figure.
• The compaction process can be split into
two sections.
• The first section involves increasing the
compaction pressure to a set amount:
this is shown by the curve between A and
B.
• The area under this curve, shown by E2 +
E3, represents the total work of
compaction (WT).
Plot of upper punch force vs. upper punch displacement
during compression and decompression. • Some of the work required to compact
E1- energy for friction. E2- energy accumulated by the the tablet will be recovered in the second
tablet after compression. E3 - energy of decompression section: represented by the curve
between points B and D.
 • The material usually expands to relax at
this stage. The area under this curve (E3)
corresponds to the recovered or elastic
work.
• The deduction of the elastic work from
the total work represents the
unrecoverable work (plastic work): this is
represented by the area E2.
Normally, an appreciable amount of the energy
supplied is converted to heat, which of course does
not contribute toward the main objective of the
process.

• Note that lubrication has no apparent effect on the actual amount of energy
required to compress the material, that is overcome resistance to relative
interparticulate movement.
 ENERGY INVOLVED IN COMPACTION
• The estimation of the total work involved, WT, was obtained by monitoring
punch force and the distance D through which it acted, so that:
𝒎𝒂𝒙
=
𝑭=𝟎

Example of force-displacement (F-D) curve. (▲) upper punch force; (▲) leaver punch force. The area WF represents the
work done in (overcoming friction, while that of area WD is the elastic deformation energy stored in the tablet during
compression. Thus, is the net mechanical energy actually used to form the tablet.