Compression and consolidation

Angles of repose: It is the maximum angle that can be obtained between the freestanding
surface of a powder heap and the horizontal plane.
Tan θ = 2h/D

As a general guide, powders with angles of repose greater than 50° have unsatisfactory flow
properties, whereas minimum angles close to 25° correspond to very good flow properties.
 Mass volume relationship:
(i) Open intraparticulate voids
(ii) closed intraparticulate voids
(iii) interparticulate void
True volume (Vt): the total volume of the solid particles, which excludes all spaces greater than
molecular dimensions and which has a characteristic value for each material.
Granular volume (particle volume Vg): the cumulative volume occupied by the particles, including all
intraparticulate (but not interparticulate) voids, depends on the method of measurement.
Bulk volume (Vb): the total volume occupied by the entire powder mass under the particular packing
achieved during the measurement. Depends on the method.
Relative volume (Vr): where v = volume of the sample under specific conditions
Vr = V/Vt
Porosity: void volume (Vv) = Vb –Vt
Density

Where M is the mass of sample.

Relative density

Bulk density is proportional to true density.

Bulk density = k true density.
k = bulk density/ true density
The constant of proportionality, k, is known as the packing fraction or fractional solids content.
E = 1-k
where e is the fractional voidage of the powder bed, which is usually expressed as a percentage and
termed the bed porosity.
Compression:
Closer packing, particle deformation, elastic, Yield point. Several
pharmaceutical materials are compressed within the range of elastic
deformation.
In other cases, the applied force is beyond yield point and the
deformation not immediately reversible on removal of applied field,
plastic deformation.
Bulk reduction from plastic deformation and /or viscous flow of the
particles which are squeezed into the remaining void spaces. shear
strength<tensile strength.
If shear strength>tensile strength, fracture of particles. Common with
brittle particles known as brittle fractures.
Small particles disform plastically, process known as microsquashing.
(proportion of fine powder is important)
Chemicophysically, bond breaking and new bond formation.
Some deformation are time dependent and occur at various rates.
Consolidation: The free energies of particles less than 50nm, results in attractive force,
known as cold welding. The nature of the bonds so formed are similar to those of molecular
structure of the interior of particles, but because of the roughness of the surface, the actual
surface area will be small.
Generation of heat, fusion bonding, increase in mechanical strength of mass.
Pharmaceutical products have low specific heat and poor thermal conductivity.
Both cold or fusion welding is influenced by several factors, including
1. The chemical nature of material
2. The extent of the available surface
3. The presence of surface contaminants
4. The intersurface distances
Material with cubic lattice arrangement can get tabletted easily than having rhombohedral
lattice., not always true. Routine testing of compaction characteristics in some type of
instrumented tableting machine constitute a desirable and informative part of such products.
The consolidation mechanisms :
• Mechanical theory : As the particles undergo deformation, the particle boundaries that the
edges of the particle intermesh, forming a mechanical bond.
• Intermolecular forces theory : Under pressure the molecules at the point of true contact
between new, clean surface of the granules are close enough so that van der Waals forces
interact to consolidate the particle. E.g microcrystalline cellulose is believed to undergo
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 to solutions at the particle
interface followed by subsequent solidification or crystallization thus resulting in the
formation of bonded surfaces.
Commercially available direct compression excipients as microgranules imparts the desired overall
qualities (i) strong tablet by providing a plastically deforming component to relieve internal stresses
(ii) strongly bonding surfaces to enhance consolidation.
Granulation: Granulation is the process in which primary powder particles are made to adhere to
form larger, multiparticle entities called granules. Pharmaceutical granules typically have a size range
between 0.2 and 4.0 mm, depending on their subsequent use.
• To prevent segregation of the constituents of the powder mix
• To improve the flow properties of the mix
• To improve the compaction characteristics of the mix
Granules should possess sufficient strength to withstand normal handling and mixing processes
without breaking down and producing large amounts of fine powder.
Strength may be expressed in terms of compressive, tensile, shear, bending impact and abrasion test.
Compression or crushing test: soft granules and hard granules, Abrasion test: amount of fines, Soft
porous vs hard and dense granules
Compression and consolidation under high loads: The force transmitted from the upper
punch to the lower is considered to depend on a number of factors, including the friction
between the powder and the die wall. These factors can be summarized in the following
expression:
Fa = Fl eKH/D
where Fa and Fl are applied and transmitted forces, H and D are the height and diameter of
the powder column within the cylindrical die and K is a constant. The constant K is
experimentally determined material dependent constant and a function of the friction
coefficient between particles and the die wall.
• Interparticulate friction: expressed in terms of a coefficient of interperticulate friction μ i;
more significant at low applied loads. glidants
• Die-wall friction: expressed in terms of a coefficient of die wall friction μw; more
significant at high applied loads when particles rearrangement has ceased. lubricants
Force distribution : Most investigations are carried out on Single
station presses (eccentric presses) or even on isolated punches and
die sets in conjugation with hydraulic press. These must be an axial
balance of forces.
FA = FL +FD
FA = Applied force to the upper punch
FL = Force transmitted to lower punch
FD = axial frictional force.
Development of Radial Force: As the compressional force is
increased and the repacking of tabletting mass is completed, the
material may be regarded as a single solid body. Then, as with all
other solids, compressive force applied in one direction (e.g.:
vertical) results in a decrease in ∆H i.e., height.
In case of unconfined solid body, this would be accompanied by an expansion in the
horizontal direction of ∆D. The ratio of these two dimensional changes is known as poisson
ratio (λ) of the material
λ = ∆D/ ∆H.
λ is characteristic constant for each solid.
Consequently a radial die-wall force FR develops perpendicular to the die-wall surface.
Materials with larger values of λ give rise to larger values of FR. The relationship between
FD (axial frictional force) and FR is given by the expression: FD= μw.FR (μw = coefficient of
die wall friction, related with shear strength of the particles and the total effective area of
contact Ae between the two surfaces). FD can be reduced by ensuring adequate lubrication at
the die wall and maintaining a minimum tablet height.
Coefficient of lubricant efficiency or R value = FL/FA perfect lubrication approached unity.
Practically it can be .98. further low value as .8 means low lubrication.
Die-wall lubricants: function by inter posing a film of
low shear strength at the interface between tabletting
mass and die-wall. There is some chemical bonding
between boundary lubricant and the surface of die-wall
as well as at edge of the tablet. The best lubricants are
those of low shear strength but have strong cohesive
tendency in directions at right angle to the plane of
shear.
Ejection forces: Force necessary to eject a finished tablet. Ejection force for a finished tablet
consists 3 stages.
Stage1: Peak force required to initiate ejection by breaking of tablet/die-wall adhesions.
Stage 2 : Small force, that required to push the tablet up the die-wall .
Stage 3: Declining force of ejection as the tablet emerges from the die.
Slip-stick conditions occur between the tablet/die wall adhesions if lubrication is insufficient.
Force volume relationships:
• Force volume relationships i- initial repacking of particles ii- elastic deformation until
elastic limit is reached iii- plastic deformation and/or brittle fracture dominates iv –
compression of solid crystal lattice formation
• In many tabletting processes, when appreciable force has been applied, the relationship
between applied pressure (p) and volume parameter such as porosity E does 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
Heckel equation: 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.
The applied compressional force F and the movements of the punches during a compression
cycle and applied pressure P, porosity E. For a cylindrical tablet,

where D is the tablet diameter. Similarly E can be calculated by:

where, w is the weight of the tabletting mass, ρt is its true density, H is the thickness of the
tablet.
• HECKEL plots :Materials that are comparatively
soft and that readily undergo plastic deformation
retain different degrees of porosity, depending upon
the initial packing in the die. 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 materials with higher yield
pressure values usually undergo compression by
fragmentation first, to provide a denser packing. Ex:
Lactose (type b, in graph)
• HECKEL plots Type-a plots exhibits higher slope
(Ky) then type b. Because type-a materials have
lower yield stress. Type-b plots exhibits lower slope
because brittle, hard materials are more difficult to
compress.
Decompression: The removal of applied force leads to new set of stresses within the tablet,
as a result of elastic recovery, which is augmented by the forces necessary to eject the tablet
from the die.
If the stress relaxation process involves plastic flow, it may continue after all compressional
force has been removed and the residual radial pressure will decay with time. The plastic
flow can be interpreted in terms of a viscous and elastic parameter in series.

Where Ft is the force left in the viscoelastic region at time t and Fm is the total magnitude of
this force at time t = 0, K is the viscoelastic slope and measure of degree of the plastic flow.
Material with higher K values undergo more plastic flow and forms strong tablets at
relatively low compaction forces.
Compaction profile
Strength of tablet:
Crushing strength Sc can be defined as the compressional force Fc which when
applied diametrically to a tablet, just fracture it.

Where ST is tensile strength, D and H are diameter and height of tablet.

Work Wf required to cause tablet failure correlates with other mechanical strength
tests and is a more sensitive parameter for comparison with other tabletting
parameters.

Where F is the force applied to tablet, z is the deformation resulting from it,
represented by the relative displacement of the anvil and plunger.
Friability: It is designed to evaluate the ability of the tablet to with stand aberration in
packing, Handling and shipping. Friability is usually measured by the use of Roche
fibrilator or tumbler test. A number of tablets (20 Nos.) are weighed and placed in the
apparatus where they are exposed to rolling and repeated shocks as they fall 6 inches in
each turn within the apparatus. After 4 minutes of this treatment or 100 revolutions, the
tablets are weighed and the weight (W) compared with initial weight (W0). The loss due to
abrasion is a measure of tablet friability. The value is expressed in percentage.

The value of 0.8-10% are considered as the upper limit of acceptability.

Lamination or capping of tablets:
entrapment of air
Decompression
• Gradual loading and unloading by utilizing large compression rolls, precompression, and slow press
speeds.
• Less compression force
• Lubrication and moisture levels and tooling geometry and condition and compression mechanism.
Instrumentation of tablet machines
• Tabletting process involves the utilization of unsatisfied bonds at the solid surface. The process can be
enhanced by the generation of large areas of clean surface, if pressed together as might occur if
appreciable brittle fracture and plastic deformation were introduced into the system.
• Behavior on decompression can affect the characteristics of finished tablets because the structure must be
strong enough. Ability to monitor ejection forces leads to valuable information on lubricant efficiency.
https://www.youtube.com/watch?v=UOfBT-dTig8
• Measurement of punch and die forces, relative displacement of the punches can provide raw
data which when suitably processed and interpreted, facilitate evaluation of many of these
parameters.
• The sensitivity of the formulation being tested to loading rate should be determined by
compression at different speeds and by monitoring of any changes in tablet properties.
Because of this rate factor, instrument have several isolated punch and die sets and to carry
out compression experiments using these sets in conjunction with a compression/tension
testing machine.
Compaction simulators Recently a sophisticated system has been described, capable of
mimicking the precise compression cycle means it has single station tooling and follows rotary
press action. The system contains micro processer representing the precise compression cycle of
the press, which in turn controls the movements of isolated punches, reproduces the exact
loading profile of the press. This assembly facilitate compressional studies at various
compressional rates, results in maximum amount of information while using the minimum
amount of material and time. They are now often referred to as “compaction simulators”.
Single station presses: Strain gauge networks as
transducers were used for measuring the magnitude of the
forces operating during the compression cycle. Resistive
gauges are usually preferred. They should be bonded as
near to the active site like punch surfaces so as to
eliminate the lack of correlation between signals obtained
from the remote regions of the machine and actual forces
present in tooling.

• The bonding must be over the entire area of the

correctly aligned gauge, at a site where the elastic
change in linear dimension of the stress bearing
member can be measured.

https://www.youtube.com/watch?v=ofo6Zr2NyMo
• Die wall instrumentation requires machining of die wall to accommodate
the gauges and reduce the thickness to a point at which the adequate
sensitivity is achieved, original geometry is restored with silicone rubber or
similar material.
• The foregoing procedure necessitate annealing and subsequent re-hardening
and tempering of the die, and this treatment should not change the precise
geometry of bore.
• A stabilized supply is essential since the system is a input voltage
dependent, and this arrangement is mounted as Poisson configuration as
compensation is provided for both temperature and bending of piece.
• Transducers based on piezo electric effect in crystals like quartz may be
used for measuring the mechanical force. Transducer is connected to a
charge amplifier converts the electrical charge into a directly proportional
DC voltage. Disadvantage is that the charge is inevitably dissipates with
time, and since the difference is being measured, they are unsuitable for
measuring static forces.
strain gauge only monitor radial forces over a localized region of the die wall. They have to
be sited at same level on the die wall as the region at which the tablet is being compressed.
The advantage of piezo electric devices include high sensitivity, robust construction, no
bonding to machine fabric which allows easy changing of tooling.
Calibration of instrumentation: Calibration of instrumentation with punch assemblies was
achieved by use of a calibrated load cell which was placed on die table, its signal can be
compared with signal from instrumented punches as they are simultaneously loaded.
Alternative method was, entire punch assemblies can be removed from the press and
mounted in an accurate compression/ tension test press.
The measurements are made by sealing the open ends of the die cavity then pumping in oil
at known pressures and noting the response. A close fitting rubber plug or rubber powder in
the die cavity can also act as a perfectly elastic material (radial die wall reaction = any
applied force) and can be substituted for oil.
The preferred form of transducer for measuring punch displacements is based on the
differential inductor principal and is commonly a linear variable differential transformer
LVDT.
Multi station presses: Major differences in the instrumentation of multi station as opposed
to single station presses is the inherent difficulty in retrieving electrical signals from a
revolving turret. This was overcame by employing radiotelemetry to transmit the force
signal from upper and lower punches to external recorders. This was unsuitable for
normal production conditions, since only few stations are operative, and only low machine
speeds are possible. Ho and co workers however overcome this and a significant proportion
of the stations remain active as in telemetry system.
More popular arrangements on modern high speed
presses is to attach strain gauges or to incorporate
piezo electric load cell into one of the tie rods.
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https://www.youtube.com/watch?v=4xggZRckfTE
Instrumenting the normal ejection cam on a rotary tablet machine by attaching strain gauges
to its bolts is of limited value, because the resulting signal is a summation of the effects of
the several lower punches on it at any instant.
The solution adapted by Wray employed a two part cam so that the region responsible for
tablet ejection is separate and in the form of a beam fixed at one end. But this method
necessitated minor modifications to other parts of the machine and there is no affect on the
normal operation. Flexure of beam caused by lower punches during ejection was monitored
by strain gauges and was found to mimic the ejection response of an instrumented lower
punch.
Alternatively, the normal cam can be cut into three sections each clamped to the frame by a
bolt, two of which are fitted with a piezo electric load washer for instance. The division
should be such that there is only one punch on each section at a time.
The first transducer then monitors the force to initiate
ejection and the second monitors the force necessary to
push the tablet clear of the die.

This arrangement minimizes the fulcrum effect as the

punches move over the cam surface toward and then away
from the actual transducer location. Certain aspects like
sticking of the lower punches due to frictional effects can
also be detected by sensitive instrumentation of this type.

Regardless of selection of remote site for instrumentation

the response should always be checked periodically against
signals obtained from directly instrumented tooling over the
whole working range of the machine to ensure consistency
in response relationships.
Signal processing: Instrumentation described here are usually DC voltages and can therefore be
retrieved, stored, processed. Displaying the signals on a cathode ray oscillograph (CRO) enables the
instant visualization of instrumentation out put. Displays were often photographed to provide permanent
record.
Role of instrumentation in production: Innovation towards direct compression methods, availability
of machines with increased out put and to reduce tablet to tablet variations. Design of instrumentation
that exercises some degree of control over the tabletting process to reduce labor involvement.
Attempt to limit weight and hardness deviations based upon the premise that compressional force is
directly proportional to tablet weight providing the following:
• The formulation is homogeneous(i.e., has uniform density).
• The compressional force/ tablet weight function is constant.
• The volume of die cavities at the point of maximum compression is constant (valid only when over
all length of punches and tip geometry are constant, the die bores are uniform and the pressure rolls
are perfectly cylindrical and mounted centrally).
The out put from the electronic unit of most force measuring systems is a DC voltage which
produces series pulses of short duration, each proportional to the weight of an individual
tablet. Signals can be conditioned to provide a wide range of monitoring and control facilities
of increased complexity.
The individual compression pulses can also be used to drive counting mechanisms and to
provide a reliable figure for the number of tablets made. These devices are uncomplicated,
inexpensive, and there is a desire to extend the signal conditioning system to control the
process to some extent. ex: one can set upper and lower limits for acceptable tablet weight
and then distinguish pulses from tablets lying outside these thresholds.
When the frequency of these out of specification tablet exceeds some present value a relay
can be tripped to activate an alarm and the machine can automatically stopped. Machines can
be fitted with mechanical accept/reject gates at machine outlet so that individual out of
specification tablets can be diverted to separate container. This function requires a high level
of sophistication because the defective tablets must be memorized until they reach the outlet.
A second approach is to take the amplified out put signals and feed them into an averaging
network. This average DC voltage is compared with reference voltage and any difference is
converted into an AC signal for amplification and drive a two phase servomotor, which can be
connected to the weight or pressure adjustment control of the press so that any change in the
average compressional force is reflected in an adjustment of either the weight or force control.
Regardless of which transducer system, sites, forces selected, it is essential to ascertain that the
response of instrumentation is a direct function of the property needing to be monitored. The work
of Wray and his colleagues is important in that it establishes that stresses generated in certain parts
of machine frame are directly proportional to the punch forces which in turn are related to
compressional weights. Machine out puts are now exceeding 12,000 tablets per minute which
means the frequency of force pulses is approximately 0.1kHz. Since the detection of small
differences in individual pulses may be necessary all units should have flat responses well beyond
this level up to approximately 1.0kHz.
Instrumented tablet machine technology is advancing rapidly. Useful for better under standing of
the tabletting process, in turn will assist in formulation development and batch quality control .