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MICROMERETICS

The science and technology of small


particles
Fundamental properties of
particles
1. Size of particle
2. Surface area of the particle
(particle shape)
POLYDISPERSE SYSTEM
Collection of particles of more than one size
Properties can be described in terms of:
1. Shape and surface area of individual
particles
2. The size range and number or weight of
particles
MONODISPERSE SYSTEM
Particles of approximately uniform size
USES
1. Diagnostic tests
2. Particle size standards for particle analyzers
3. For accurate determination of pore size in filters
4. As uniformly sized surfaces upon which antigens may
be coated for effective immunization
5. For instrument calibration and quality control in the
manufacture of submicron-sized products such as
liposomes, nanoparticles, and microemulsions
METHODS OF DETERMINING
PARTICLE SIZE

1. OPTICAL MICROSCOPY
2. SIEVING
3. SEDIMENTATION
4. PARTICLE VOLUME MEASUREMENT
1. OPTICAL MICROSCOPY
Uses an ordinary microscope for particle
measurement in the range of 0.2 m to 100
m.
Presence of agglomeration and particles of
more than one component may be detected
The diameter is obtained only from two
dimensions: length and breadth, the
thickness/depth in not measured.
2. SIEVING
Uses standard sieves
Generally used for grading coarser particles
May be employed for screening materials as
fine as 44 m (No. 325 sieve)
CAUSES OF ERRORS
1. Sieve loading
2. Duration and intensity of agitation
Disadvantage: Attrition of particles (rubbing
together/pulverization)
POWDERS OF VEGETABLE AND ANIMAL DRUGS ARE
OFFICIALLY DEFINED AS:

VERY COARSE (#8) all particles pass through no.8 sieve


and not more than 20 % through sieve no. 60.
COARSE (#20) all particles pass through no.20 sieve and
not more than 40 % through sieve no. 60.
MODERATELY COARSE (#40) - all particles pass through
no.40 sieve and not more than 40 % through sieve no. 80.
FINE (#60) - all particles pass through no.60 sieve and not
more than 40 % through sieve no. 100.
VERY FINE (#80) all particles pass through a no. 80 sieve.
There is no limit as to greater fineness.
POWDERS OF CHEMICAL DRUGS ARE OFFICIALLY
DEFINED AS:
COARSE (#20) all particles pass through no.20 sieve and
not more than 40 % through sieve no. 60.
MODERATELY COARSE (#40) - all particles pass through
no.40 sieve and not more than 60 % through sieve no.
60.
FINE (#80) - all particles pass through no.80 sieve and
there is no limit as to greater fineness.
VERY FINE (#120) all particles pass through a no. 120
sieve. There is no limit as to greater fineness.
SEDIMENTATION
The particles size may be obtained by gravity
sedimentation as expressed by STOKES LAW.
Uses Andreasen pipet

dst = 18 h
(i - e)gt
PARTICLE VOLUME
MEASUREMENT
Uses Coulter Counter
An instrument used to measure the volume
of particles
Capable of counting particles at the rate of
approximately 4000 per second, thus both
gross counts and particle size distributions are
obtained in relatively short period of time
Average Particle size
determination
BY WEIGHT BY VOLUME
Sieving method Light scattering
Light scattering Electronic senzing
Sedimentation zone
Light obstruction
Air permeation
Optical microscopy
PARTICLE SHAPE
Sphere
Affects the flow and packing of a powder

SURFACE AREA
Determined by the shape of particles
Affects adsorption and dissolution rate
SPECIFIC SURFACE surface area per unit
volume or per unit weight
METHODS OF DETERMINING
SURFACE AREA
1. ADSORPTION METHOD
Uses Quantasorb
2. AIR PERMEABILITY METHOD
Uses Fisher subsieve sizer

Powders of large surface area are good adsorbents


DERIVED PROPERTIES OF POWDERS
1. POROSITY (VOIDS)
Defined as the ratio of the void volume to
the bulk volume of the packing
Void volume = volume of spaces
Bulk volume = volume occupied
total = (Vb Vp)/Vb
intraparticle = (Vg Vp)/Vg
interspace = (Vb Vg)/Vb
POROSITY CALCULATIONS
1. Calculate the porosity of a sample of
aluminum oxide having a true density of 4.0
g/cm3. When 75 g of the powder was placed
in a graduated cylinder, The Al2O3 was found
to have a bulk volume of 62 cm3.
= Vb Vp
Vb
2. The true density of Aspirin is 1.37 and the granule density
is 1.33. What is the porosity or percent void spaces within
the granules?
intraparticle = Vg Vp
Vg
intraparticle = 1 granule density
true density
3. A 1-g sample of a granular powder has a true volume of
0.3 cm3; volume of intraparticle pores = 0.1 cm3; volume
of spaces between particles = 1.6 cm3. Calculate the
interspace porosity.
Vg = 0.3 + 0.1 = 0.4 cm3
Vb = 0.3 + 0.1 + 1.6 = 2.0 cm3

interspace = Vb Vg =1- bulk density___


Vb granule density
2. PACKING ARRANGEMENT
TWO IDEAL PACKING ARRANGEMENTS
1. CLOSEST PACKING (OR
RHOMBOHEDRAL)
angles of 60 and 120 are common
porosity is 26%
2. MOST OPEN, LOOSEST,
OR CUBIC PACKING
Packed at 90 to each other resulting to
a porosity of 47-48%
III. DENSITIES OF PARTICLES

TRUE DENSITY is the density of the


actual solid, exclusive of voids and
intraparticle pores
GRANULE DENSITY density of the
powder particles together with their
intraparticle pores.
BULK DENSITY density of material as
determined from the bulk volume and
weight of a dry powder
IV. BULKINESS
Or BULK, is the specific bulk volume
Reciprocal of bulk density
An important consideration in packaging
powders
Bulkiness increases with a decrease in
particle size
V. FLOW PROPERTIES
FLOW PROPERTIES EXHIBITED BY POWDERS
1. PLASTIC FLOW
2. DILATANT FLOW
FACTORS AFFECTING FLOW PROPERTIES
1. PARTICLE SIZE AND SHAPE
250-2000m = free flowing
75 250 m = flow freely or cause problem
depending on shape
Very fine particles (less than 10 m) = do not
flow freely as large particles
Particle shape and flow properties
Spherical shape flow better than needle
particles
Free flowing
Elongated or flat particles tend to pack
resulting to high porosity powders
FACTORS AFFECTING FLOW
PROPERTIES
2. POROSITY AND DENSITY
High density, low porosity = FREE
FLOWING
3. SURFACE ROUGHNESS
Leads to poor flow characteristics
ANGLE OF REPOSE
A technique for estimating the flowability
of a powder
Measures the frictional forces in a loose
powder
The maximum angle possible between the
surface of a pile of powder and the
horizontal plane
ANGLE OF REPOSE
tan = h/r
Where
h = height of the
powder cone
r = radius of the
powder cone
tan = 3.3cm/ 4.5 cm 3.3 cm
tan = 0.7333333
= arc tan 0.73333 9.0 cm
= 36.25
9.0 cm
Powders of low repose angles
are FREE FLOWING; high
angle of repose poorly flow
and has low bulk density
FREE FLOWING POWDERS
Characterized by dustibility
Examples:
Talcum= 57%
Potato starch = 27%
Fine charcoal = 23%
COHESIVE POWDERS
Cohesiveness may be a result of:
1. Presence of fines
2. Presence of moisture
Materials used to improve flow properties
are called GLIDANTS

Example: Magnesium stearate, starch, talc


VI. Compaction/
DILATANCY
Dilatancy is the expansion of powder
under the influence of stress
Porosity of powders increases upon
compression
Important in pharmaceutical tableting