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S.S.P. SHIKSHANSANTHA’S
SIDDHI COLLEGE OF PHARMACY
SIZE REDUCTION
Ms. Saroja P. Adepawar
Department of
Quality Assurance Techniques
Introduction
 Definition- Size reduction is the process of reducing substances
to smaller particles OR
 Process of reducing large solid unit masses into small unit
masses i.e. Coarse or fine particle
 When the particle size of solids is reduced by mechanical
means it is known as milling.
 The size reduction operation can be divided into two major
categories depending on whether the material is a solid or a
liquid. If the material is solid, the process is called grinding and
cutting, if it is liquid, emulsification or atomization.
Objectives
 Improvement in dissolution and absorption of drug
 Effective extraction of drug
 Increased therapeutic effectiveness of drug
 Effective mixing of material
 Improved physical appearance
 Improved physical stability
objectives
 Content Uniformity- Mixing becomes effective if particle size
is uniform and small. With smaller particle size , number of
particles per unit dose increases. Larger the number of particle,
better is the mixing. Therefore better content uniformity can be
achieved
 Uniform flow- Smaller and controlled particle size promotes
the flow of powder, this helps in tablet compression and
capsule filling.
 Effective drying- Rate of drying increases as size
reduction increases the surface area.
Disadvantages
Drug degradation
Poor mixing
Contamination
Mechanism of size reduction
 Cutting
 Compression
 Impact
 Attrition
Mechanism
Impact —particle concussion by a single rigid
force/pressure (hammer). Moving objects strikes particle
surface- particle strikes stationary surface- Hammer mill
Attrition —arising from particles collision/scraping against
one another or against a rigid surface. Caught between
two moving surface – Fluid energy mill
Cutting —produced when the particle is compressed
between the edges of two hard surfaces moving
tangentially. Strong force by sharp object on a narrow
area. Lab scale- blade, knife. Large scale- Cutter mill.
Waxy substances- during semisolid preparations.
Compression—particle disintegration by two rigid forces
(nutcracker). Crushed by application of pressure- Mortar
pestle
Theory and laws governing size
reduction
Griffith theory
Rittinger’s theory
Kicks theory
Bonds theory
Relationship between Stress and
Strain
Griffith theory
 According to Griffith theory, all solids have some structural
weakness or flaws in them.
 A flaw developes into crack under strain
 Amount of force to be applied depends on crack length &
focus of stress at the atomic bond of crack apex.
laws governing size
 Energy required to reduce the size of particles
is inversely proportional to the size raised to
the some power.
dE
d
D
=
C
-D n
Where E= Amount of energy required to produce a
change
D = Size of unit mass
C, n = Constants
 Integrating equation (1),
E= C ln(di/dn)
 (di/dn) = reduction ratio.
 If n=1.0 equation (2) becomes Kick’s theory.
 If n=1.5 equation (2) becomes Bond’s theory.
 If n=2.0 equation (2) becomes Rittinger’s theory
Rittinger theory
 According to this theory energy E required for size
reduction of unit mass is directly proportional to the new
surface area produced.
E=KR (Sn – Si) …. (3)
Where
 Si = initial surface area
 Sn = new specific surface area
 KR = Rittinger’s constant.
 E= amount of energy.
Bonds theory
 States that energy used in crack propagation is
proportional to new crack length produced.
 crack propagation- deforming or fracturing set of
particles
 new crack length produced- change in particle
dimension
KB – work required to reduce unit weight from infinite size to 100
Kicks theory
.
For compression of large particles kick’s theory is
useful.
Factors Affecting Size
Reduction
Factors related
to the nature of
raw material
Hardness
Toughness
Abrasiveness
Stickiness
Softening
temperature
Material
structure
Ratio of feed size
to product size
Factors related to
the nature of
Finished product
Particle Size
Ease of Sterilization
Contamination of
milled material
Factors related to
safety and economy
Hardness
Hardness:
An arbitrary scale of hardness has been devised known as
Moh’s Scale;
 Moh’s Scale =1 is for graphite
 Moh’s Scale <3is for soft
material
 Moh’s Scale >7 is for hard
material
 Moh’s Scale =10is fordiamond
 The harder the material the
more difficult it is to reduce in
size
Toughness and Abrasiveness
Toughness:
 Toughness of material is more important
 Fibrous drugs: moisture content
Abrasiveness:
 Property of Hard material (particularly those of mineral
origin)
 Grinding of abrasive material leads to contamination of
finished product.
Stickiness
 Material may adhere to grinding surfaces
 The meshes of the Screen may be choked
 If the material used for size reduction produces heat then
substance that are gummy or resinous may be
troublesome to the size reduction process
 Sometimes the addition of inert substance may
sometimes assistance such as kaolin to sulphur.
Softening temperature &
Slipperiness
Softening temperature:
 Heat generated during grinding cause some substance to be
soften.
 Waxy substances, such as stearic acid, or drugs containing
oils or fat
Slipperiness:
 The reverse of stickiness
 The material acts as a lubricant and lowers the efficiency to
the grinding surfaces.
 This also give rise to size reduction difficulties
Material structure & Moisture
content
Material Structure:
 Some substances are homogeneous in character, but the
majority shows special structure.
 eg. Mineral substances, vegetable drugs.
Moisture content:
 Moisture content influence the hardness, toughness,
stickiness.
 Usually, < 5% of moisture is suitable if substance is to be
ground dry or
 > 50% if it is being subjected to wet grinding.
Physiological effect and purity
Physiological effect:
 Some substances are very potent
 Small amount of dust may have effect on operator
 Enclosed mills used to avoid dust
Purity required:
 If high degree of purity needed then cleaning between
the batches is to be done
Ratio of feed size to product
size
 Machines that produces a fine product require a small
feed size
Factors related to nature of finished
product
 Particle Size: Griseofulvin
 Ease of Sterilization: Parentrals and ophthalmics
 Contamination of milled materials: For potent and low
dose drugs
 Factors related to safety and economy: Safety,
irritability and toxicity
* Cost
* Power consumption
* Space occupied
* Labour Cost
Equipments for size reduction
General parts of size reduction
equipment
 Hopper
 Milling chamber
 Receiver
 Other accessories
 Sieves/ Screens
 Cyclone separators
 Dust Collectors
 Cooling devices
Hammer Mill
 Principle: Impact
 Range :40 to 8000 µm
 Construction:
 Hopper
 Jacket wall
 Central shaft
 Hammers ( 4 or more)
 Screen
 Receiver
 Working
Hammer mills
 In a hammer mill, swinging hammer heads are attached to a
rotor that rotates at high speed inside a hardened casing.
 The hammer mill consists of a steel casing in which a
central shaft is enclosed to which a number of swinging
hammers are attached.
 When the shaft is rotated the hammers swing out to a radial
position.
 On the lower part of the casing a screen of desired size is
fitted which can be easily replaced according to the particle
size required.
 The material is crushed and between the hammers and the
casing and remains in the mill pulverizeduntil it is fine
enough to pass through a screen which forms the bottom of
Construction & working:
 A hammer mill is essentially a steel drum containing a vertical or
horizontal rotating shaft or drum on which hammers are mounted.
 The hammers swings on the ends of the cross freely or fixed to the
central rotor. The rotor is rotates at a high speed (8000-15000rpm)
inside the drum while material is fed into a feed hopper.
 The material is impacted by the hammer bars and expelled
through screens in the drum of a selected size.
 Both brittle and fibrous materials can be handled in hammer mills,
though with fibrous material, projecting sections on the casing may
be used to give a cutting action.
 The hammer mills are available in various designs and shapes.
 In pharmaceutical industry they are used for grinding dry materials,
wet filter cakes, ointments and slurries
Advantages
 It is rapid in action, and is capable of grinding many
different types of materials.
 They are easy to install and operate, the operation is
continuous.
 There is little contamination of the product with metal
abraded from the mill as no surface move against each
other.
 The particle size of the material to be reduced can be
easily controlled by changing the speed of the rotor,
Disadvantages
 The high speed of operation causes generation of heat
that may affect thermolabile materials or drugs containing
gum, fat or resin. The mill may be watercooled to reduce
this heat damage.
 The rate of feed must be controlled carefully as the mill
may be choked, resulting in decreased efficiency or even
damage.
 Because of the high speed of operation, the hammer mill is
susceptible to damage by foreign objects such as stones
or metal in the feed. Magnets may be used to remove iron,
but the feed must be checked visually for any other
Ball mill
 Principle: Impact & Attrition
 Range :1 to 100 µm
 Construction –
 Hollow cylinder
 Metallic frame
 Inner wall-
 Balls
 Working
Working
a) slow- low
centrifugal force–
balls roll over each
other– only attrition
b) very high-high
centrifugal force–
balls thrown to wall-
only compression
c) correct- moderate
centrifugal force- balls
lifted to top & cascade
at bottom- both impact
& attrition
Ball mill depend on Speed
Uses and advantages
Use:
 for fine grinding, 100 to 5 mm or less
 for abrasive material
 for dyes & pigments
Advantages:
 Installation, operation and labour costs are low
 Efficient for dry & wet grinding
 Inert gas, unstable & explosive material
 Suitable for grinding toxic substances
 for ophthalmic and parental products sterility can be achieved
 can be adopted to continuous process
 Installation & operation - economical
Disadvantages:
 Noisy
 Not Suitable For Sticky
 Wear- Contamination
 Slow Process
 Soft, fibrous material cannot be milled
Fluid energy mill
 Principle: Impact & Attrition
 Range : 1 to 20 µm
 Construction
• Hollow elliptical tube-
Height 2 m,
Diameter – 20-200 mm,
Inner surface- stainless steel or ceramic.
• Feeder – Near bottom
• Fluid inlet jets – compressed air- 600 kilopascal to 1 mega
pascal
• Classifier (Bag filters / cyclone separator) – Air escape /
fine particles
WORKING
 Powder is introduced through the solid inlet
 fluid enters, the suspended particles colloid
with each other and break.
 Attrition (particle collide with each other) &
 Impact (particle collide with casing of mill)
 Small particles carried to outlet and
removed by cyclone separator or filters
 The coarse particles undergo re-circulation
in the chamber until size reduced sufficiently
Uses:
 For hard particles
 for ultrafine grinding
 Strict control of particle size
 Examples are antibiotics, sulphonamides and vitamins.
Advantages Disadvantages
Smaller particle size produced
than other methods
Expensive
Upto 6000 kg of feed is
milled/hour
Not suitable for milling soft,
tacky and fibrous material
No wear of the mill so no
contamination
-
Thermolabile substance can be
ground
-
Less maintenance -
Edge runner mill
 Principle: compression
 Range: 50 to 10000 µ
 Construction:
 2 heavy rollers
 Bed containing feed of material
 Shaft
 Scraper
Working
 Material placed on bed (mortar)
 Wheels (rollers) are rotated and move along the bed
 Material crush by compression
 Scrappers redirect in zone
 Effective size reduction takes place
 USE:
• For tough material & those obtained from natural sources.
 Advantages:
• Material produced- high density - not segregate easily
• Easy to operate
• Material produced- spherical
 Disadvantages:
• Not useful for sticky material
• Mill requires more space
• Slow milling/ Time Consuming
• Energy consumption is quite high
• Contamination possible
End Runner Mill
 Principle: Compression & attrition
 Range : 5 to 10000 µ
 Construction
 Mortar & pestle – steel or porcelain
 Pestle- Heavy – weight - crushing
 Scrapper
WORKING
 Material placed at bottom of mortar
 The pestle is placed in the mortar
 Mortar revolves with high speed
 Cause pestle to revolve- attrition
 Weight of pestle - compression
 Scrapper- keep material in zone
 Powder is collected and passed
through sieves to get desired size.
USE:
 For fine grinding
 For natural products
Advantages:
 The mill is suitable for dry as well as wet grinding.
Disadvantages:
 Not useful for sticky material
 Mill requires more space
 Slow milling
Size reduction ppt

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Size reduction ppt

  • 1. S.S.P. SHIKSHANSANTHA’S SIDDHI COLLEGE OF PHARMACY SIZE REDUCTION Ms. Saroja P. Adepawar Department of Quality Assurance Techniques
  • 2. Introduction  Definition- Size reduction is the process of reducing substances to smaller particles OR  Process of reducing large solid unit masses into small unit masses i.e. Coarse or fine particle  When the particle size of solids is reduced by mechanical means it is known as milling.  The size reduction operation can be divided into two major categories depending on whether the material is a solid or a liquid. If the material is solid, the process is called grinding and cutting, if it is liquid, emulsification or atomization.
  • 3.
  • 4. Objectives  Improvement in dissolution and absorption of drug  Effective extraction of drug  Increased therapeutic effectiveness of drug  Effective mixing of material  Improved physical appearance  Improved physical stability
  • 5. objectives  Content Uniformity- Mixing becomes effective if particle size is uniform and small. With smaller particle size , number of particles per unit dose increases. Larger the number of particle, better is the mixing. Therefore better content uniformity can be achieved  Uniform flow- Smaller and controlled particle size promotes the flow of powder, this helps in tablet compression and capsule filling.  Effective drying- Rate of drying increases as size reduction increases the surface area.
  • 7. Mechanism of size reduction  Cutting  Compression  Impact  Attrition
  • 8. Mechanism Impact —particle concussion by a single rigid force/pressure (hammer). Moving objects strikes particle surface- particle strikes stationary surface- Hammer mill Attrition —arising from particles collision/scraping against one another or against a rigid surface. Caught between two moving surface – Fluid energy mill Cutting —produced when the particle is compressed between the edges of two hard surfaces moving tangentially. Strong force by sharp object on a narrow area. Lab scale- blade, knife. Large scale- Cutter mill. Waxy substances- during semisolid preparations. Compression—particle disintegration by two rigid forces (nutcracker). Crushed by application of pressure- Mortar pestle
  • 9.
  • 10. Theory and laws governing size reduction Griffith theory Rittinger’s theory Kicks theory Bonds theory Relationship between Stress and Strain
  • 11. Griffith theory  According to Griffith theory, all solids have some structural weakness or flaws in them.  A flaw developes into crack under strain  Amount of force to be applied depends on crack length & focus of stress at the atomic bond of crack apex.
  • 12. laws governing size  Energy required to reduce the size of particles is inversely proportional to the size raised to the some power. dE d D = C -D n Where E= Amount of energy required to produce a change D = Size of unit mass C, n = Constants
  • 13.  Integrating equation (1), E= C ln(di/dn)  (di/dn) = reduction ratio.  If n=1.0 equation (2) becomes Kick’s theory.  If n=1.5 equation (2) becomes Bond’s theory.  If n=2.0 equation (2) becomes Rittinger’s theory
  • 14. Rittinger theory  According to this theory energy E required for size reduction of unit mass is directly proportional to the new surface area produced. E=KR (Sn – Si) …. (3) Where  Si = initial surface area  Sn = new specific surface area  KR = Rittinger’s constant.  E= amount of energy.
  • 15. Bonds theory  States that energy used in crack propagation is proportional to new crack length produced.  crack propagation- deforming or fracturing set of particles  new crack length produced- change in particle dimension KB – work required to reduce unit weight from infinite size to 100
  • 16. Kicks theory . For compression of large particles kick’s theory is useful.
  • 17. Factors Affecting Size Reduction Factors related to the nature of raw material Hardness Toughness Abrasiveness Stickiness Softening temperature Material structure Ratio of feed size to product size Factors related to the nature of Finished product Particle Size Ease of Sterilization Contamination of milled material Factors related to safety and economy
  • 18. Hardness Hardness: An arbitrary scale of hardness has been devised known as Moh’s Scale;  Moh’s Scale =1 is for graphite  Moh’s Scale <3is for soft material  Moh’s Scale >7 is for hard material  Moh’s Scale =10is fordiamond  The harder the material the more difficult it is to reduce in size
  • 19. Toughness and Abrasiveness Toughness:  Toughness of material is more important  Fibrous drugs: moisture content Abrasiveness:  Property of Hard material (particularly those of mineral origin)  Grinding of abrasive material leads to contamination of finished product.
  • 20. Stickiness  Material may adhere to grinding surfaces  The meshes of the Screen may be choked  If the material used for size reduction produces heat then substance that are gummy or resinous may be troublesome to the size reduction process  Sometimes the addition of inert substance may sometimes assistance such as kaolin to sulphur.
  • 21. Softening temperature & Slipperiness Softening temperature:  Heat generated during grinding cause some substance to be soften.  Waxy substances, such as stearic acid, or drugs containing oils or fat Slipperiness:  The reverse of stickiness  The material acts as a lubricant and lowers the efficiency to the grinding surfaces.  This also give rise to size reduction difficulties
  • 22. Material structure & Moisture content Material Structure:  Some substances are homogeneous in character, but the majority shows special structure.  eg. Mineral substances, vegetable drugs. Moisture content:  Moisture content influence the hardness, toughness, stickiness.  Usually, < 5% of moisture is suitable if substance is to be ground dry or  > 50% if it is being subjected to wet grinding.
  • 23. Physiological effect and purity Physiological effect:  Some substances are very potent  Small amount of dust may have effect on operator  Enclosed mills used to avoid dust Purity required:  If high degree of purity needed then cleaning between the batches is to be done
  • 24. Ratio of feed size to product size  Machines that produces a fine product require a small feed size
  • 25. Factors related to nature of finished product  Particle Size: Griseofulvin  Ease of Sterilization: Parentrals and ophthalmics  Contamination of milled materials: For potent and low dose drugs  Factors related to safety and economy: Safety, irritability and toxicity * Cost * Power consumption * Space occupied * Labour Cost
  • 26. Equipments for size reduction
  • 27. General parts of size reduction equipment  Hopper  Milling chamber  Receiver  Other accessories  Sieves/ Screens  Cyclone separators  Dust Collectors  Cooling devices
  • 28. Hammer Mill  Principle: Impact  Range :40 to 8000 µm  Construction:  Hopper  Jacket wall  Central shaft  Hammers ( 4 or more)  Screen  Receiver  Working
  • 29. Hammer mills  In a hammer mill, swinging hammer heads are attached to a rotor that rotates at high speed inside a hardened casing.  The hammer mill consists of a steel casing in which a central shaft is enclosed to which a number of swinging hammers are attached.  When the shaft is rotated the hammers swing out to a radial position.  On the lower part of the casing a screen of desired size is fitted which can be easily replaced according to the particle size required.  The material is crushed and between the hammers and the casing and remains in the mill pulverizeduntil it is fine enough to pass through a screen which forms the bottom of
  • 30. Construction & working:  A hammer mill is essentially a steel drum containing a vertical or horizontal rotating shaft or drum on which hammers are mounted.  The hammers swings on the ends of the cross freely or fixed to the central rotor. The rotor is rotates at a high speed (8000-15000rpm) inside the drum while material is fed into a feed hopper.  The material is impacted by the hammer bars and expelled through screens in the drum of a selected size.  Both brittle and fibrous materials can be handled in hammer mills, though with fibrous material, projecting sections on the casing may be used to give a cutting action.  The hammer mills are available in various designs and shapes.  In pharmaceutical industry they are used for grinding dry materials, wet filter cakes, ointments and slurries
  • 31. Advantages  It is rapid in action, and is capable of grinding many different types of materials.  They are easy to install and operate, the operation is continuous.  There is little contamination of the product with metal abraded from the mill as no surface move against each other.  The particle size of the material to be reduced can be easily controlled by changing the speed of the rotor,
  • 32. Disadvantages  The high speed of operation causes generation of heat that may affect thermolabile materials or drugs containing gum, fat or resin. The mill may be watercooled to reduce this heat damage.  The rate of feed must be controlled carefully as the mill may be choked, resulting in decreased efficiency or even damage.  Because of the high speed of operation, the hammer mill is susceptible to damage by foreign objects such as stones or metal in the feed. Magnets may be used to remove iron, but the feed must be checked visually for any other
  • 33. Ball mill  Principle: Impact & Attrition  Range :1 to 100 µm  Construction –  Hollow cylinder  Metallic frame  Inner wall-  Balls  Working
  • 34. Working a) slow- low centrifugal force– balls roll over each other– only attrition b) very high-high centrifugal force– balls thrown to wall- only compression c) correct- moderate centrifugal force- balls lifted to top & cascade at bottom- both impact & attrition Ball mill depend on Speed
  • 35. Uses and advantages Use:  for fine grinding, 100 to 5 mm or less  for abrasive material  for dyes & pigments Advantages:  Installation, operation and labour costs are low  Efficient for dry & wet grinding  Inert gas, unstable & explosive material  Suitable for grinding toxic substances  for ophthalmic and parental products sterility can be achieved  can be adopted to continuous process  Installation & operation - economical
  • 36. Disadvantages:  Noisy  Not Suitable For Sticky  Wear- Contamination  Slow Process  Soft, fibrous material cannot be milled
  • 37. Fluid energy mill  Principle: Impact & Attrition  Range : 1 to 20 µm  Construction • Hollow elliptical tube- Height 2 m, Diameter – 20-200 mm, Inner surface- stainless steel or ceramic. • Feeder – Near bottom • Fluid inlet jets – compressed air- 600 kilopascal to 1 mega pascal • Classifier (Bag filters / cyclone separator) – Air escape / fine particles
  • 38. WORKING  Powder is introduced through the solid inlet  fluid enters, the suspended particles colloid with each other and break.  Attrition (particle collide with each other) &  Impact (particle collide with casing of mill)  Small particles carried to outlet and removed by cyclone separator or filters  The coarse particles undergo re-circulation in the chamber until size reduced sufficiently
  • 39. Uses:  For hard particles  for ultrafine grinding  Strict control of particle size  Examples are antibiotics, sulphonamides and vitamins.
  • 40. Advantages Disadvantages Smaller particle size produced than other methods Expensive Upto 6000 kg of feed is milled/hour Not suitable for milling soft, tacky and fibrous material No wear of the mill so no contamination - Thermolabile substance can be ground - Less maintenance -
  • 41. Edge runner mill  Principle: compression  Range: 50 to 10000 µ  Construction:  2 heavy rollers  Bed containing feed of material  Shaft  Scraper
  • 42. Working  Material placed on bed (mortar)  Wheels (rollers) are rotated and move along the bed  Material crush by compression  Scrappers redirect in zone  Effective size reduction takes place
  • 43.  USE: • For tough material & those obtained from natural sources.  Advantages: • Material produced- high density - not segregate easily • Easy to operate • Material produced- spherical  Disadvantages: • Not useful for sticky material • Mill requires more space • Slow milling/ Time Consuming • Energy consumption is quite high • Contamination possible
  • 44. End Runner Mill  Principle: Compression & attrition  Range : 5 to 10000 µ  Construction  Mortar & pestle – steel or porcelain  Pestle- Heavy – weight - crushing  Scrapper
  • 45. WORKING  Material placed at bottom of mortar  The pestle is placed in the mortar  Mortar revolves with high speed  Cause pestle to revolve- attrition  Weight of pestle - compression  Scrapper- keep material in zone  Powder is collected and passed through sieves to get desired size.
  • 46. USE:  For fine grinding  For natural products Advantages:  The mill is suitable for dry as well as wet grinding. Disadvantages:  Not useful for sticky material  Mill requires more space  Slow milling