Presentation on,
“MICROMERITICS”
Presented by-
Mr. Firodiya S.R. ([Link],Pharmaceutics)
Assistant Professor,
Department Of Pharmaceutics
MES College of Pharmacy, Sonai.
Mula Education society’s college of pharmacy,
sonai.
Defination-
“The science and technology of small
particles is known as micromeritics.”
Particle size importance in pharmacy
Physical property of powder
Flow property of powder
Rate of dissolution
Chemical property of powder
Rate of absorption
Elegance of pharmaceutical preparation
Stability of system.
Extraction and drying process
Adsorption capacity
Properties of powder
Fundamental properties Derived properties
Derived
From
Individual particle.
Fundamental properties
Fundamental properties:-
1. Particle size and size distribution
2. Particle shape
3. Particle surface area
4. Particle weight
5. Particle number
Derived properties:-
1. Density of powders
2. Flow properties of powders
3. Porosity
4. Bulkiness
[Link] size
Denoted in micrometers
One micrometer is equal to 10-3 mm or 10-6 m
One millimicrometer is called one nanometer
(nm)
One nanometer = 10-9 m or 10-6 mm or 10-3 μm
1 m = 1000 mm
1 mm = 1000 μm
1 μm = 1000 nm
Particle size determination (PSD) Methods-
1. Optical Microscopy
2. Sieving Method
3. Sedimentation Method
4. Conductivity Method
1. OPTICAL MICROSCOPY
Particle size in the range of 0.2 – 100 μm can be measured.
This method gives number distribution which can be converted to
weight distribution
Optical microscope lens has limited resolving power
Advanced microscopes have better resolving power and can
measure size in nano range: Ultramicroscope, Electron microscope-
Scanning Electron microscope (SEM), Transmission Electron
microscope (TEM).
Application:
Particle size analysis in suspensions, aerosols, globule size analysis
in emulsion.
Procedure:
Eye piece of the microscope is fitted with a micrometer.
This eye-piece micrometer is calibrated using a
standard stage micrometer.
The powder sample is dispersed in a suitable vehicle in
which it does not dissolve and its properties are not
altered.
This sample is mounted on a slide and placed on the
stage under the objective of microscope.
Around 300-500 particles are visualized. Their
diameter is noted and mean is computed.
Calibrated Using A Standard Stage Micrometer.
Advantages-
One can view particles
Any aggregates detected
Contamination of particles detected
Use of cover slip for arresting motion of particles
Easy and simple
Disadvantages-
Length and breadth can be detected but depth or thickness of
particles cannot be measured
Slow- time consuming , tedious, inaccurate Number of particles to
be measured is more
Large sample required
2. Sieving Method-
Particle size in the range of 30–5000 μm can be
measured.
Sieving method is an ordinary and simple method.
It is widely used as a method for the particle size analysis
Sieve analysis is usually carried out using dry powders.
Although, for powders in liquid suspension or which
agglomerate during dry sieving, a process of wet sieving can
be used.
Sieving method directly gives weight distribution.
It find application in dosage form development of
tablets and capsules.
Normally, 15% of fine powder should be present in
granulated material to get proper flow of material and
achieve good compaction.
Thus percent of coarse, moderate, fine powder is
estimated by this method.
Sieve analysis utilizes a wire mesh made of brass,
bronze or stainless steel with known aperture (hole)
diameters which form a physical barrier to particles.
The standard sieve sizes are as per the
pharmacopoeia
Most sieve analyses utilize a series, stack (layer) of
sieves which have the coarser mesh at the top of
the series and smallest mesh at the bottom above
a collector tray.
(The mesh size goes on decreasing from top to bottom)
METHOD OF SIEVING
1. Mechanical dry sieving method
A-Agitation method (Oscillation,Vibration,Gyration)
B-Brushing method
C-Centrifugal method
2. Wet sieving method
Method:
A sieve stack usually comprises 6-8 sieves.
Powder is loaded on to the coarsest sieve of the stack and
then it is subjected to mechanical vibration for specified
time.
After this time, the powder retained on each sieve is
weighed.
The particles are considered to be retained on the sieve
mesh with an aperture corresponding to the sieve diameter.
The size is estimated as per the standards given in
pharmacopoeia.
Care should be taken to get reproducible results.
The type of motion, time of operation, speed,
weight of powder should be fixed and standardized.
Advantages-
Inexpensive, Simple, Rapid, Reproducible results.
(if parameters are standardized)
Disadvantages-
lower limit is 30 microns
Powder if moist, can cause clogging of apertures
Attrition between particles during the process may
cause size reduction giving inaccurate results.
3. Sedimentation Method
In this method particle size can be determined
by examining the powder as it sediments out.
Sample preparation: Powder is dispersed in
a suitable solvent
If the powder is hydrophobic, it may be necessary to
add dispersing agent to aid wetting of the powder.
In case where the powder is soluble in water it
will be necessary to use non- aqueous liquids or carry
out the analysis in a gas.
Principle of Measurement
Particle size analysis by sedimentation method can be
divided into two main categories according to the method of
measurement used.
One of the type is based on measurement of particle in a
retention zone.
Another type uses a non-retention measurement zone.
An example of a non-retention zone measurement is
known as the pipette method.
Andreasen pipette method:
One of the most popular of the pipette methods was that
developed by Andreasen and Lundberg and commonly
called the Andreasen pipette.
In this method , known volumes of suspension are
drawn off and the concentration differences are measured
with respect to time.
It involves measuring the % of solids that settle with time
in a graduated vessel.
Construction:
The Andreasen fixed-position pipette consists of a 200
mm graduated cylinder which can hold about 500 ml of
suspension fluid.
A pipette is located centrally in the cylinder and is held in
position by a ground glass stopper so that its tip coincides
with the zero level.
A three way tap allows fluid to be drawn into a 10 ml
reservoir which can then be emptied into a beaker or
centrifuge tube.
Method:
A 1% suspension of the powder in a suitable liquid
medium is placed in the pipette.
At a given intervals of time, samples are withdrawn from
a specified depth without disturbing the suspension.
The amount of powder can be determined by weight
following drying or centrifuging; alternatively, chemical
analysis of the particles can be carried out.
The particle size is determined in terms of stokes’ diameter
(the diameter of a particle measured during sedimentation
at constant rate) using modified Stokes' equation.
dst=18nh/(ps-pf)gt
4. Conductivity methods
There are various subtypes. Two popular methods are-
Electrical stream sensing zone method
(Coulter counter)
Laser light scattering methods
It is based on the principle of change in light intensity.
The measurement of this change in light intensity gives
estimate of particle size.
Advantage:
Particle size ranging from 0.5 – 500 microns
Gives number distribution, Particle volume measured
and can be converted to diameter.
Accurate, sensitive, fast technique.
4000 particles per second can be counted.
Disadvantage
Expensive
