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. 2. 3. 4.

OPTICAL MICROSCOPY SIEVING SEDIMENTATION 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 Sieving method Light scattering Sedimentation BY VOLUME Light scattering Electronic senzing 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)

total = (Vb Vp)/Vb intraparticle = (Vg Vp)/Vg interspace = (Vb Vg)/Vb

Defined as the ratio of the void volume to the bulk volume of the packing Void volume = volume of spaces Bulk volume = volume occupied

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 Vb =1bulk density___ 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 tan = 0.7333333 = arc tan 0.73333 = 36.25

3.3 cm

9.0 cm 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