Compression
and
Compaction
By:
Rabia Khokhar,
Ph.D. (Pharmaceutics) Scholar, [Link]., [Link].
Contents
• Introduction-
• Derived properties of powdered solids
The solid-Air interface
Angle of repose
Flow rates
Mass volume relationship & Density
• Hackel plots
• Granulation
• Friability
• Compression
• dry method, wet method, slugging
• Physics of tableting
• Tabletting machines and other equipments required
• Problems involved in tableting
• Tablet coating
• Capsulation
• Hard and soft gelatin capsules
Introduction
• Compression
It is the reduction of bulk volume of a material as a result of displacement of the gaseous
phase under pressure
• Consolidation
It is the increase in the mechanical strength of the particle resulting from particle to
particle interaction
• Compaction
It is the compression and consolidation of two phases (solid and gas) system due to
applied force
• Compressibility
It is the ability of the powder to decrease in volume under pressure
Derived properties of powdered solids
Solid-Air interface
• COHESION
Attractive forces between like particles
Bulk particles characteristics
• ADHESION
Attractive forces between unlike particles
Surface particles characteristics
Angle of repose
• Maximum angle that can be obtained between the free standing
surface of powder heap and the horizontal plane
• Qualitative assessment of internal cohesive and frictional effect under
external loading as encountered during manufacturing operation
• Measures the resistance of particles movement
• Denoted by θ
• Material with low angle of repose forms flatter piles than materials
with high angle of repose
• Angle of repose may be determined using following FOUR methods:
Static AoR (fixed funnel and fixed cone methods)
Dynamic/ Kinetic AoR (rotating cylinder and tilting box method)
Methods for determination of AoR
Fixed Fixed Rotating Tilting
funnel cone cylinder box
method method method method
Flow rate
• The flow rate of a material depends upon many factors, some of
which are particle related and some related to the process.
• Monitoring the rate of flow of material through an orifice has
been proposed as a better measure of powder flowability.
• The flow rate through an orifice is generally measured as the
mass per time flowing from any of a number of types of
containers (cylinders, funnels, hoppers).
In labs, commonly use method is….
• 0.5g of particles/ granules are placed in the funnel and allowed to flow
through it on a clean dry paper. The time taken by the particles to flow
completely through the funnel is noted and flow rate is calculated
using the following formula:
Flow rate = Weight of Particles/ granules
Time
Can you recall the methods used for measurement
of Angle of Repose of powders and granules???
1 2 3
Mass volume relationships and Density
• Ratio of mass of an object to its volume is density therefore density of
a solid is a reflection of the arrangement of molecules in a solid
• Mass can be determined with great accuracy BUT volume
measurement is complicated (due to air spaces, or voids present)
Powder Volumes:
1. True volume or
absolute volume
2. Granular volume
3. Bulk volume
bulk
Methods to measure volume of powders by:
Methods like Liquid displacement method (specific gravity bottle method) and
X-ray diffraction methods can be used but most efficiently by the Helium
pycnometer
Helium pycnometer
• A gas displacement method (also called gas pycnometer)
• An inert gas, typically helium, is used as the displacement medium.
• The sample is placed in a sealed cup of a known volume. This cup is then placed
into the sample chamber.
• Gas is introduced to the sample chamber and then expanded into a second empty
chamber with a known volume.
• The pressure observed after filling the sample cell and the pressure discharged into
expansion chamber are measured, and then the volume is calculated.
• The density is determined by dividing the sample weight by the volume measured.
• The density measured by Helium Pycnometry is often referred to as “helium
density”
VIDEO LINK
[Link]
characterization-lab/characterization-
techniques/density-helium-pycnometry
Granulation
Moist granulation
• Preferred method of granulation in industry due to better performance
in both machinery and systemically
• It is important to get the understanding about the granulation stage in
order to ensure the appropriate strength of the final granule
• Stages of granulation include:
A. Pendular state
B. Funicular state
C. Capillary state
D. Droplet state
Stages in the development of moist granules
Moist granulation
In order to ensure the strength of granules,
following parameters should also be considered:
Presence of binder
Optimum moisture content
Drying operation
Technique of Drying
Properties of Granules
• Some finished granule characteristics are important as the directly
effect the tableting process and hence the final tablet produced
• It includes: bulk material properties like Packaging ability and flow
properties and the individual granule properties which include granule
strength and porosity.
• Particle shape and size distribution are important factors in packing
and flow.
• Regular shape, nearly spherical particles led to lower AoR and higher bulk
densities better flow properties. Therefore, smaller tablet weight variation
more efficient compression/ consolidation during tableting
• Size distribution effect on performance is difficult to generalize, optimum
propotion of fines for optimum flow properties
• Porosity of tablet produced
under a certain compressive
load is in many cases a
function of the initial
porosity of the packing in the
die (i.e. packaging ability,
determined by
Compressibility index)
Strength of Granules
Granule strength is determined using
following methods:
1. Compressive strength test
2. Abrasion test