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Ana Marie L. Rubenicia, RPh
             March 14, 2012
Micromeritics is the science of small particles. It is
 the study of a number of characteristics, including
 paticle size and size distribution, shape, angle of
 repose, porosity, true volume, apparent demsity nd
 bulkiness.
Particles are any unit of
   matter having defined
   physical dimensions.




  Physical state of particles
  can be altered by physical
        manipulation




Particle characteristics
 can alter therapeutic
     effectiveness.
MICROMERITICS
FACTORS AFFECTING FLOW PROPERTIES
1.    PARTICLE SIZE AND SHAPE
       250-2000m = 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
      Elongated or flat particles tend to pack resulting to high
       porosity powders
2. POROSITY AND DENSITY
      High density, low porosity = FREE FLOWING
3. SURFACE ROUGHNESS
      Leads to poor flow characteristics
MICROMERITICS
Techniques of determining particle size
MICROSCOPIC METHOD(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.
The microscopic method can include counting not
  fewer than 200 particles in a single plane using
  calibrated ocular on a microscope.
Particle Size
SIZE OF  MIDDLE    # OF     “ND”     1. Given the following
PARTICLE VALUE     PARTICLE
IN uM    “D”(um)   PER                 data, what is the
                   GR ”N”              average diameter of
40-60     50       15       750        the particles?
60-80     70       25       1750     dav= ∑ nd / ∑n
80-100    90       95       8550      dav = 36,850 / 355
100-120   110      140      15400    dav = 103.8uM
120-140   130      80       10400

                   ∑n=355   ∑nd=
                            36,800
PARTICLE SIZE
SIEVING - uses standard sieves; generally used for grading
  coarser particles. May be employed for screening materials
  as fine as 44 m (No. 325 sieve)
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.
PARTICLE SIZE
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.
PARTICLE SIZE
 0.5 um – 10um – suspensions and fine
    emulsions
   10 um – 50um - upper limit of subsieve
    range; coarse emulsion particles;
    flocculated suspension particles
   50 um – 100um – lower limit of sieve range;
    fine powder range
   150 um – 1000um – coarse powder range
   1000 um – 3360um –average granule size
A stack of sieve is arranged in order, the powder placed in the
top sieve, the stack shaken, the quantity of powder resting on
each sieve weighed, and this calculation performed:




            dav= ∑(% retained)x(ave size) / 100
               dav = 29.232 / 100 = 0.2923mm
PARTICLE SIZE
 Other ways of particle size determonation elutriation,
  centrifugation, permeation, adsorption, the Coulter Counter, and
  light obstruction and the use of Andreasen pipet.
               dst = 18 h /(i - e)gt

Angle of repose
 A relative simple technique for estimating the flow properties of a
 powder. It can easily be determined by allowing a powder to flow
 though a funnel and fall feerly onto a surface. The height and
 diameter of the resulting cone are measured and the angle of repose
 calculated as:
               tan Ѳ = h/r
h is the height of the powder cone and r is the radius of the powder cone
Low angle of repose – flow freely; high angle of repose – flow poorly
PARTICLE SIZE
Charateristics used to describe powder –
 porosity, true volume, bulk volume,
 apparent density, true density, and
 bulkiness.
Void= Vbulk - V  ; Porosity = Vbulk - V x 100
          Vbulk                           Vbulk
Apparent Density pa =    Weight of the sample ;
                            Vbulk
true density p = Weight of the sample
                       V
       Bulkiness, B = 1/pa
PARTICLE SIZE
EXAMPLE


A selected powder has a true density (p)
 of 3.5g/cc. Experimentally, 2.5 g of the
 powder measures 40 mL in a cylindrical
 graduate. Calculate the true volume,
 void, porosity, apparent density, and
 bulkiness.
PARTICLE SIZE
Closest packing:rhombus-triangle – angles
  of 60 deg and 120 deg: void=o.26 ;
  porosity=20%
Open type of packing:cubical – cubes
  packed at 90 deg angle: void=0.47;
  porosity=47%
Importance of packing and flow:
a. Affects the size of the container
b. The flow of granulation
c. Efficiency of filling apparatues for
   making tablets and capsules.
d. Ease of working with powders.
Particle Size Reduction
Comminution, reduction of the particle size of a
  solid substance to a finer state, is used :
1. Facilitate crude drug extraction.
2. Increase the dissolution rates of a drug
3. Aid in the formulation of acceptable
   pharmaceutical forms.
4. Enhance absorption of drugs.
The reduction in the particle size of a solid is accompanied
   by a great increase in the specific surface area of the
   substance.
Particle Size Reduction
EXAMPLE
Increase in number of particles
If a powder consists of 1mm on edge and it is reduced to
   paricles 10 um on edge, what is the number of particles
   reduced?
1. 1mm equals 1000um.
2. 1000um/10um = 100 pieces produced on each edge; that
     is, if the cube is sliced into 100 pieces on the x-axis,each
     10um long, 100 pieces result.
3. If this repeated on the x- and y-axis, the result is
     100x100x100 = 1 million particles produced, each 10um
     on edge, for each original particle 1mm on edge. This can
     also be written an 106 .
Particle Size Reduction
Increase in surface area
What increase in the surface area of the powder is produced by decreasing the
     particle size from 1mm to 10um?
1.   The 1mm cube has 6 surfaces, each 1mm on edge. Each face has a surface area
     of 1 mm2. Because there are 6 surfaces, this 6 mm2 surface area per particle.
2. Each 10um cube has 6 surfaces, each 10um on edge. Each face has a surface
     area of 10x10 = 100 um2 . Because there are 6 faces, this is 6x100 um2 or 600
     um2 surface area per particle. Since 106 particles resulted from comminuting
     the 1m cube, each 10um on edge, the surfaces are now is 600 um2 x 106, or 6 x
     108um2 .
3. To get everything in the same units for ease of comparison, convert the 6 x
     108um2 in to square mm as follows.
4. Since there are 1000um/mm, there must be 1000 2 ,or 1 million um2 / mm2 .
This is more appropriately express as 106 um2 / mm2,
          6 x 108um2      = 6 x 102mm2 The surface area have been increased from
          106 um2 / mm2                        6 mm2 to 600 mm by the reduction in
                                           Particle size of cubes 1mm to cubes 100um
                                          on edge, an hundred fold inc in surface area.
Thank you…
May God Bless All Your
Dreams and Endeavors…

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Micromeritics

  • 1. Ana Marie L. Rubenicia, RPh March 14, 2012
  • 2. Micromeritics is the science of small particles. It is the study of a number of characteristics, including paticle size and size distribution, shape, angle of repose, porosity, true volume, apparent demsity nd bulkiness.
  • 3. Particles are any unit of matter having defined physical dimensions. Physical state of particles can be altered by physical manipulation Particle characteristics can alter therapeutic effectiveness.
  • 4. MICROMERITICS FACTORS AFFECTING FLOW PROPERTIES 1. PARTICLE SIZE AND SHAPE 250-2000m = 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  Elongated or flat particles tend to pack resulting to high porosity powders 2. POROSITY AND DENSITY  High density, low porosity = FREE FLOWING 3. SURFACE ROUGHNESS  Leads to poor flow characteristics
  • 5. MICROMERITICS Techniques of determining particle size MICROSCOPIC METHOD(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. The microscopic method can include counting not fewer than 200 particles in a single plane using calibrated ocular on a microscope.
  • 6. Particle Size SIZE OF MIDDLE # OF “ND” 1. Given the following PARTICLE VALUE PARTICLE IN uM “D”(um) PER data, what is the GR ”N” average diameter of 40-60 50 15 750 the particles? 60-80 70 25 1750 dav= ∑ nd / ∑n 80-100 90 95 8550 dav = 36,850 / 355 100-120 110 140 15400 dav = 103.8uM 120-140 130 80 10400 ∑n=355 ∑nd= 36,800
  • 7. PARTICLE SIZE SIEVING - uses standard sieves; generally used for grading coarser particles. May be employed for screening materials as fine as 44 m (No. 325 sieve) 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.
  • 8. PARTICLE SIZE 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.
  • 9. PARTICLE SIZE  0.5 um – 10um – suspensions and fine emulsions  10 um – 50um - upper limit of subsieve range; coarse emulsion particles; flocculated suspension particles  50 um – 100um – lower limit of sieve range; fine powder range  150 um – 1000um – coarse powder range  1000 um – 3360um –average granule size
  • 10. A stack of sieve is arranged in order, the powder placed in the top sieve, the stack shaken, the quantity of powder resting on each sieve weighed, and this calculation performed: dav= ∑(% retained)x(ave size) / 100 dav = 29.232 / 100 = 0.2923mm
  • 11. PARTICLE SIZE  Other ways of particle size determonation elutriation, centrifugation, permeation, adsorption, the Coulter Counter, and light obstruction and the use of Andreasen pipet. dst = 18 h /(i - e)gt Angle of repose A relative simple technique for estimating the flow properties of a powder. It can easily be determined by allowing a powder to flow though a funnel and fall feerly onto a surface. The height and diameter of the resulting cone are measured and the angle of repose calculated as: tan Ѳ = h/r h is the height of the powder cone and r is the radius of the powder cone Low angle of repose – flow freely; high angle of repose – flow poorly
  • 12. PARTICLE SIZE Charateristics used to describe powder – porosity, true volume, bulk volume, apparent density, true density, and bulkiness. Void= Vbulk - V ; Porosity = Vbulk - V x 100 Vbulk Vbulk Apparent Density pa = Weight of the sample ; Vbulk true density p = Weight of the sample V Bulkiness, B = 1/pa
  • 13. PARTICLE SIZE EXAMPLE A selected powder has a true density (p) of 3.5g/cc. Experimentally, 2.5 g of the powder measures 40 mL in a cylindrical graduate. Calculate the true volume, void, porosity, apparent density, and bulkiness.
  • 14. PARTICLE SIZE Closest packing:rhombus-triangle – angles of 60 deg and 120 deg: void=o.26 ; porosity=20% Open type of packing:cubical – cubes packed at 90 deg angle: void=0.47; porosity=47% Importance of packing and flow: a. Affects the size of the container b. The flow of granulation c. Efficiency of filling apparatues for making tablets and capsules. d. Ease of working with powders.
  • 15. Particle Size Reduction Comminution, reduction of the particle size of a solid substance to a finer state, is used : 1. Facilitate crude drug extraction. 2. Increase the dissolution rates of a drug 3. Aid in the formulation of acceptable pharmaceutical forms. 4. Enhance absorption of drugs. The reduction in the particle size of a solid is accompanied by a great increase in the specific surface area of the substance.
  • 16. Particle Size Reduction EXAMPLE Increase in number of particles If a powder consists of 1mm on edge and it is reduced to paricles 10 um on edge, what is the number of particles reduced? 1. 1mm equals 1000um. 2. 1000um/10um = 100 pieces produced on each edge; that is, if the cube is sliced into 100 pieces on the x-axis,each 10um long, 100 pieces result. 3. If this repeated on the x- and y-axis, the result is 100x100x100 = 1 million particles produced, each 10um on edge, for each original particle 1mm on edge. This can also be written an 106 .
  • 17. Particle Size Reduction Increase in surface area What increase in the surface area of the powder is produced by decreasing the particle size from 1mm to 10um? 1. The 1mm cube has 6 surfaces, each 1mm on edge. Each face has a surface area of 1 mm2. Because there are 6 surfaces, this 6 mm2 surface area per particle. 2. Each 10um cube has 6 surfaces, each 10um on edge. Each face has a surface area of 10x10 = 100 um2 . Because there are 6 faces, this is 6x100 um2 or 600 um2 surface area per particle. Since 106 particles resulted from comminuting the 1m cube, each 10um on edge, the surfaces are now is 600 um2 x 106, or 6 x 108um2 . 3. To get everything in the same units for ease of comparison, convert the 6 x 108um2 in to square mm as follows. 4. Since there are 1000um/mm, there must be 1000 2 ,or 1 million um2 / mm2 . This is more appropriately express as 106 um2 / mm2, 6 x 108um2 = 6 x 102mm2 The surface area have been increased from 106 um2 / mm2 6 mm2 to 600 mm by the reduction in Particle size of cubes 1mm to cubes 100um on edge, an hundred fold inc in surface area.
  • 18. Thank you… May God Bless All Your Dreams and Endeavors…