Compression

Compression and
and consolidation
consolidation of
of
powder
powder solids
solids
Presented by
PAYAL H. PATIL (M.pharm 1st yr.)

Dept. of pharmaceutics and Q.A

R.C.Patel Institute of Pharmaceutical Education and 1
Research, Shirpur.
 CONTENTS
 DEFINATIONS

 DERIVED PROPERTIES OF POWDERED SOLID

 EFFECT OF APPLIED FORCES ON COMPRESSION

 GRANULATION

 COMPRESSION & CONSOLIDATION UNDER HIGH LOAD

 FORCE VOLUME RELATIONSHIP

 HECKEL PLOT

 KAWAKITA EQUATION

 COOPER & EATON EQUATION

 DECOMPRESSION

 COMPACTION PROFILE

 ENERGY OF COMPRESSION

 REFERENCES
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 Definitions

• Compression- Compression means

reduction of bulk volume of material as a
result of displacement of gaseous phase.

• Consolidation – Consolidation is an increase

in mechanical strength of material from
particle - particle interactions.

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 Derived properties of powdered
solids
1. The solid-air interface
2. Angle of repose
3. Flow rates
4. Mass-volume relationships
5. Density

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 THE SOLID-AIR INTERFACE
 COHESION:
Attraction between like
particle.Experienced by
particles in bulk.
 ADHESION:
Attraction between unlike
particle.Experienced
by particles at surface.
 Resistance to movement of particles is affected by two
factors:-
a) Electrostatic forces.
b)Adsorbed layer of moisture on particles.

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 ANGLE OF REPOSE

• DEFINITION:
The maximum angle
possible between the
surface of pile of the
powder and the
horizontal plane.

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METHODS TO MEASURE
ANGLE OF REPOSE

Wall is lined by sandpaper

a. Fixed funnel and free standing cone method.

b. Tilting box method.
c. Revolving cylinder method.
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 FORMULA FOR MEASURING
ANGLE OF REPOSE.
1. θ = Tan-1(h/r)
ANGLE OF FLOW
here, h = height of pile REPOSE (Ø)
r = radius of the base of (Degrees)
EXCELLENT
< 25
the pile GOOD
θ = angle of repose 25-30
PASSABLE
*30-40
2. θ = cos-1 D/ (l1+l2) VERY POOR
>40
Adding glidant,0.2% aerosil may
here, D = diameter of base improve flow.

l1+l2 = the opposite sides

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of pile
 ANGLE OF REPOSE
STATIC ANGLE OF KINETIC/DYNAMIC
REPOSE ANGLE OF REPOSE
•It is angle of repose •It is angle of repose
determined by 1st two determined by the 3rd
methods (a. & b.) method ( c.)
•It is preferred since
they most closely
mimic the
manufacturing
situation in which
powder is in motion.
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 FLOW RATES
CONSOLIDATION FLOW
• Compressibility index (Carr's INDEX (Carr, % )
consolidation index)
EXCELLENT
5-15
I = [1-v/vo]x100 GOOD
12-16
FAIR TO
here, V = Tapped Volume *18-21 PASSABLE
V0 = Volume before POOR
*23-35
tapping
VERY POOR
33-38
VERY VERY
>40 POOR
Adding glidant,0.2% aerosil may improve
flow.
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 MASS-VOLUME RELATIONSHIPS
 TYPE OF VOIDS OR AIR
SPACES:

 Open intraparticulate voids

 Closed intraparticulate voids

 Interparticulate voids

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 TYPES OF VOLUME

 True volume (Vt)

 Granule volume (Vg)
 Bulk volume (Vb)
 Relative volume (Vr)
Vr = V/ Vt

Vr tends to become unity as all air is eliminated from the mass

during the compression process

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 POROSITY (E)
 porosity, E = VV/ Vb
here, VV = Void volume
Vb = Bulk volume
now,
Void volume (VV) = Vb –Vt
Therefore,
Porosity (E) =(Vb–Vt)/ Vb
Porosity when expressed as percentage
E =100.[(Vb–Vt)/ Vb]
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 METHODS TO MEASURE VOLUME
OF POWDER.

 Helium pycnometer

 Liquid displacement method (specific gravity bottle

method)

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 HELIUM PYCNOMETER
Vt = Vc/U1-U2x[U1-Us]
Here, 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
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HELIUM PYCNOMETER
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 LIQUID DISPLACEMENT METHOD

• Solvent used are

e.g., ethyl alcohol ,water, mercury , etc.
• Pycnometer or specific gravity bottle
used.
Specific gravity bottle
True density= w3/(w4-w2) = (w2-w1)/(w4-w2)
Here , w1 = wt. of Pycnometer
w2 = Wt. of Pycnometer + sample or glass beads
w4 = Wt. of Pycnometer with powder & filled with
solvent
w3 = w2-w1 = Wt. of sample
w4-w2 = Volume of liquid displaced by the solid 17
 DENSITY
 DIFFERENT TYPE OF DENSITY :

True density
ρt=M/vt
Granule density
ρg=M/vg
Bulk density
ρb=M/vb
 relative density
ρr= ρ/ ρt
Tapped density-tester

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 Effect of applied forces
I. DEFORMATION:
• Strain: The relative amount of deformation
produced on a solid body due to applied force.
• It is dimensionless quantity.
• Compressive strain,
Z = ∆H/Ho
• Stress(σ):
σ = F/A
here, F is force required to produce
strain in area A
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 D0

H D H0

a)Tensile strain b)Compressive strain c)Shear strain

FIG. Diagram shows changes in geometry (strain) of solid body
resulting from various types of applied forces.

*( In fig. dash line is original shape & solid

line is deformed shape)
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II. COMPRESSION:
 When external mechanical forces are applied to a
powder mass, there is reduction in bulk volume as
follows,
1. Repacking 3.Brittle fracture: e.g., sucrose
2.Particle 4.microquashing
deformation
Elastic e.g., acetyl salicylic acid, MCC
deformation
- when elastic limit or yield point
is reached.
Plastic
deformation

Microsquasing: Irrespective of the behavior

of larger particles smaller particles may
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deform plastically.
FIG.EFFECT OF COMPRESSION FORCE ON BED OF POWDER

INITIALLY

REPACKING

DEFORMATION

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III. CONSOLIDATION:
Mechanism,
1.Cold welding (particle distance <50nm)
2.Fusion welding (caused due to frictional
heat)
3.Recrystallization
 Consolidation process is influenced by,
- Chemical Nature of materials
- Extent of available surface
- presence of surface contaminants
- Intersurface distance

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• Effect of increasing compressional force on specific
surface area of powder mass,

Compressional force

• Increased surface area (from O to A), initial

particle fracture due to increased compression
point A ,Particle rebonding predominates & then

surface area decreases (from A to B). 24

 Granulation
• Addition of granulating liquid to mass of powder mass leads to
following stages,

Or droplet

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• Granulation equipment can be instrument with
the torque measuring devices, which senses the
change in agitator power.

•METHOD TO DETERMINE
STRENGTH OF GRANULE:

1.Compressive strength or
crushing strength.

2.Abrasion tests

FIG. Plot of change in torque of mixer

shaft during addition of granulating
fluid. point F indicates exact end point
to wet massing 26
 Compression and consolidation
under high load
• Relationship between upper punch FA & lower
punch forces FL:
FL = FA × e-KH/D
here, K = constant,
H & D = height & diameter of
tablet
• Effects of friction:
1.Interparticulate friction(μi ): Glidants used e.g.,
colloidal silica
2.Die-wall friction(μw ): lubricants used e.g.,
magnesium stearate
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 Force distribution

-Axial balance of forces in

punches is given by,
FA = FL+FD

-Mean compaction force (FM),

FM = FA+FL/ 2
here, FA = upper punch force,
FL =lower punch force,
FD =axial friction force.
FIG. Cross section of a typical simple punch &
die assembly used for compaction studies
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 Development of radial force:
- Radial force (FR) develops perpendicular to die-wall
surface.
- Poisson ratio , λ = ∆D / ∆H
here, ∆D =change in horizontal direction,
∆H=change in height.
- According to classic friction theory,
FD = μw × FR ‘R’ LUBRICATION
VALUE
here, FD =axial friction force.
1 Perfect
μw = Die-wall friction
- Coefficient of Lubricant efficiency 0.98 Acceptable
(R),
0.8 Poor
R = max. FL
min. FA
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 Ejection forces

- 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.

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  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.

LUBRICANT SHEAR
STRENGTH

Stearic acid 1.32

Calcium stearate 1.47

Magnesium stearate 1.96

Boric acid 7.16

graphite 7.35
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 Force volume relationship
• End of compressional process is when
bulk volume = tapped volume & porosity = 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 FIG. Decreasing porosity with

increasing compressional force
compression process involves four stage as for single ended pressing
shown in fig., i) initial repacking
ii)Elastic deformation
iii)Plastic deformation
iv)compression
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 Heckel plot
• It follows 1st order
•The pore in the mass are the reactant.
log 1/E = KyP + Kr
here, 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 33
F = applied compressional force
 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: FIG. Example 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.
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 Kawakita Equation
C = Vi – Vp/ Vt = abPa / 1+ bPa

here, 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.
Cooper and Eaton Equation
Vi – Vp/ Vi – Vt = C2 exp (-K2/Pa ) + C3 exp (-K3/Pa )

here, C2,C3, K2,K3 = constants

LIMITATION : Applies only to single component
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system.
 Decompression
• Occurs on removal of applied force after compression.
• Tablet must mechanically strong to withstand stresses
produce during decompression.
• Plastoelasticity(γ),
γ = [Ho / Hm - (Hr-Hm) / Ho - Hm]

here, Ho ,Hm, Hr = thickness of tablet mass at onset of

loading, at max. applied pressure & on ejection from die

• γ > 9 produce tablets that are laminated or capped.

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 Compaction profile
• Monitoring of applied pressure transmitted radially to die-
wall gives compaction profile as follow,

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 Energy involved in compaction
• Tablet machine, roll compactor, extruder requires high
input of mechanical work

• Work involve in various phases of compaction are,

1.To overcome interparticulate friction
2.To overcome friction between machine parts and particles
3.To induce deformation
4.For brittle fracture
5.Mechanical operation of various machine parts

• Lubrication reduce energy expenditure by 75%.

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 REFERENCES
• Leon Lachman, Herbert A.Liberman, & Joseph kanig ,THE
THEORY AND PRACTICE OF INDUSTRIAL
PHARMACY, third edition.
• Herbert A.Liberman, Leon Lachman & Joseph B. Schwartz
,PHARMACEUTICAL DOSAGE FORMS, TABLETS,
volume II.
• ENCYCLOPEDIA OF PHARMACEUTICAL
TECHNOLOGY, second edition,volume-3.
• C.V.Subrahmanyam ,TEXTBOOK OF PHYSICAL
PHARMACEUTICS, second edition.
• Gilbert S. Banker , Christopher T. Rhodes, MODERN
PHARMACEUTICS , Fourth Edition.

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THANK YOU

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