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Size_Reduction

The document provides comprehensive notes on size reduction in pharmaceutical engineering, covering its importance, mechanisms, energy laws, and various milling equipment such as hammer mills, ball mills, fluid energy mills, edge runner mills, and end runner mills. It details the principles, construction, working, advantages, and disadvantages of each milling type, along with factors affecting size reduction and exam preparation tips. The content aligns with the PCI BP304T syllabus for B. Pharm 2nd Year students.

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Govinda jadhav
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0% found this document useful (0 votes)
0 views24 pages

Size_Reduction

The document provides comprehensive notes on size reduction in pharmaceutical engineering, covering its importance, mechanisms, energy laws, and various milling equipment such as hammer mills, ball mills, fluid energy mills, edge runner mills, and end runner mills. It details the principles, construction, working, advantages, and disadvantages of each milling type, along with factors affecting size reduction and exam preparation tips. The content aligns with the PCI BP304T syllabus for B. Pharm 2nd Year students.

Uploaded by

Govinda jadhav
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd

SIZE REDUCTION

Pharmaceutical Engineering – B. Pharm 2nd Year / Semester III


Detailed PCI-aligned notes with original educational mill diagrams
KEY CONCEPT: The PCI BP304T syllabus includes objectives, mechanisms and laws of size
reduction; factors affecting size reduction; and the principle, construction, working, uses, merits
and demerits of hammer mill, ball mill, fluid energy mill, edge runner mill and end runner mill.
citeturn0search32

Syllabus component Coverage in this document


Fundamentals Definition, objectives, applications and importance
Mechanisms Cutting, compression, impact, attrition and combined
mechanisms
Energy laws Kick’s, Rittinger’s, Bond’s and general Walker relationship
Factors Material properties, equipment variables and process
conditions
Mills Hammer, ball, fluid energy, edge runner and end runner
mills
Exam preparation Comparisons, formulas, viva questions and common
mistakes

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
1. Introduction to Size Reduction
Size reduction is the mechanical process of reducing large solid masses into smaller particles, coarse
powders, fine powders or very fine particles. It is also called comminution or grinding. When mechanical
equipment is used for this purpose, the operation is commonly described as milling.
KEY CONCEPT: Size reduction does not mean simply making a material ‘smaller’. In pharmaceutical
manufacturing, the target is a controlled particle-size range and suitable particle-size distribution
while preserving product quality.

1.1 Pharmaceutical importance


 Increase surface area of a solid and thereby improve the rate of dissolution, extraction, drying or
chemical reaction.
 Produce particles of a desired size for tablets, capsules, powders, suspensions and other dosage forms.
 Improve uniformity during mixing and reduce segregation caused by large differences in particle size.
 Facilitate extraction of active constituents from crude drugs.
 Improve handling, flow and downstream processing when the appropriate particle size is selected.
 Provide controlled particle size for inhalation and other specialized dosage forms where particle size is a
critical quality attribute.
 Prepare material for size separation, granulation, blending and other unit operations.

1.2 Objectives of size reduction


1. Increase specific surface area.
2. Obtain a desired particle size and size distribution.
3. Improve dissolution and extraction rates.
4. Improve mixing and content uniformity.
5. Facilitate drying and other mass-transfer operations.
6. Improve handling and transport of solids.
7. Prepare feed material for subsequent unit operations.
8. Control the physical properties of powders where particle size is important.

2. Mechanisms of Size Reduction


The actual fracture of a particle depends on the nature of the material and the type of stress applied. Five
mechanisms are especially important in pharmaceutical engineering.
Mechanism What happens Typical equipment / example
Cutting Material is cut by a sharp edge or knife. Cutter mill; fibrous materials.
Compression Particle is squeezed between two Edge runner, end runner; brittle
surfaces until it fractures. materials.
Impact A moving body or particle strikes the Hammer mill; ball mill; fluid energy mill.
material at high velocity.
Attrition Particles or surfaces rub against one Ball mill; fluid energy mill.
another, producing fine particles.
Shear A particle is subjected to tangential Fine grinding systems; shear-type
forces causing deformation and mills.
fracture.
KEY CONCEPT: Most practical mills use more than one mechanism. For example, a ball mill
combines impact and attrition, while a fluid energy mill combines particle–particle impact and
attrition.
Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
2.1 Selection of mechanism
Feed characteristic Preferred approach
Fibrous / tough Cutting is often preferred; preliminary cutting may be
required.
Hard and brittle Compression and/or impact can be effective.
Friable crystalline material Impact is commonly effective.
Need for very fine powder Impact + attrition or fluid-energy grinding may be
appropriate.
Heat-sensitive material Fluid energy milling may be advantageous because the
process can reduce direct mechanical contact and can use
controlled/inert gas.
Sticky / soft material Conventional impact mills may be difficult; process cooling
or another milling strategy may be needed.

3. Laws Governing Size Reduction


Energy consumption during comminution is a major engineering consideration. Several empirical laws relate
the energy required to the change in particle size.

3.1 Kick’s law


Kick’s law is more applicable when relatively coarse particles are being reduced and the geometrical
similarity of the particles is important.
E = Kₖ log(D₁/D₂)
E = energy required per unit mass; Kₖ = Kick’s constant; D₁ = initial characteristic size; D₂ = final
characteristic size.
KEY CONCEPT: Kick’s law predicts that equal ratios of size reduction require approximately equal
energy, making it more useful for coarse crushing than fine grinding.

3.2 Rittinger’s law


Rittinger proposed that the energy required is proportional to the new surface area produced. It is therefore
particularly relevant to fine grinding.
E = Kᵣ (1/D₂ − 1/D₁)
The exact constant and units depend on the selected basis and size definition.
KEY CONCEPT: Rittinger → new surface area. Think ‘fine grinding’ and ‘surface creation’.

3.3 Bond’s law


Bond’s law is intermediate between Kick’s and Rittinger’s approaches and is widely used for practical
estimation of grinding energy.
E ∝ (1/√D₂ − 1/√D₁)
The industrial Bond equation is commonly expressed using a work index and suitable size units.
KEY CONCEPT: Bond’s law is often treated as the intermediate law: Kick → coarse; Bond →
intermediate; Rittinger → fine.

3.4 General Walker relationship


A generalized relationship may be represented as:

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
dE/dD = −K / Dⁿ
Different values of n give different empirical forms. The exact interpretation depends on the definition of E
and D used in the derivation.
Law Typical exponent concept Main emphasis
Kick n≈1 Coarse size reduction
Bond n ≈ 1.5 Intermediate practical range
Rittinger n≈2 Fine size reduction / new surface

4. Factors Affecting Size Reduction


4.1 Factors related to the material
Factor Effect on milling
Hardness Hard materials require greater energy and may cause
greater equipment wear.
Toughness Tough materials resist fracture and may require cutting or
special pretreatment.
Friability Friable materials fracture readily and are often suitable for
impact milling.
Elasticity Elastic materials may absorb energy and deform instead of
fracturing efficiently.
Fibrous nature Fibrous materials may wrap around moving parts; cutting-
type equipment is often preferred.
Moisture content Excess moisture can cause sticking, agglomeration and
reduced screening/milling efficiency; the optimum moisture
depends on material.
Softening / melting point Heat generated during milling may soften or melt low-
melting materials, causing sticking.
Hygroscopicity Moisture uptake can alter flow, cohesion and milling
behavior.
Structure / crystallinity Crystal defects and internal structure influence fracture
behavior.
Initial particle size Large feed particles may require pre-crushing before fine
grinding.

4.2 Equipment and operating factors


 Mill type and dominant mechanism.
 Rotor or drum speed.
 Feed rate and residence time.
 Screen opening or classifier setting where applicable.
 Size and material of grinding media in ball mills.
 Clearance between moving and stationary parts where applicable.
 Gas pressure and nozzle conditions in fluid energy mills.
 Temperature control and cooling.
 Open- or closed-circuit operation.
 Cleaning, wear and contamination control.
KEY CONCEPT: The optimum operating condition is not simply the highest speed. Excessive speed
can increase heat, wear, dust generation and undesirable particle-size fractions.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
5. Hammer Mill
A hammer mill is a high-speed impact mill in which hammers attached to a rotating rotor strike the feed
material. A screen is usually provided so that sufficiently reduced particles can leave the milling chamber.

Figure 1. Original schematic diagram of a hammer mill (educational, not a reproduction of a textbook figure).

5.1 Principle
Impact between rapidly moving hammers and the feed material is the principal mechanism. Additional
particle–screen and particle–particle interactions may contribute.

5.2 Construction
 Strong metal housing / grinding chamber.
 High-speed rotor or shaft.
 Several hammers mounted on the rotor; depending on design they may be fixed or pivoted.
 Screen fitted around part of the grinding chamber.
 Feed hopper and discharge arrangement.
 Motor and drive assembly.

5.3 Working
9. Material enters through the feed hopper.
10. Rotor rotates at high speed and the hammers move rapidly.
11. The hammers strike the particles and fracture them mainly by impact.
12. Additional impact occurs when particles strike the casing or screen.
13. Particles continue to break until they are small enough to pass through the screen openings.
14. Reduced material is collected at the discharge.

5.4 Uses
 Grinding brittle crystalline materials and dry plant materials.
 Reducing particle size of many pharmaceutical chemicals.
Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
 Preliminary/intermediate grinding where a controlled screen size is suitable.

5.5 Advantages
 Simple construction and operation.
 High throughput for suitable materials.
 Screen can help control the maximum discharge size.
 Useful for many brittle materials.

5.6 Disadvantages
 Heat generation may be significant at high speed.
 Not ideal for sticky, very soft or highly fibrous materials.
 Screen and hammer wear can introduce contamination.
 Dust generation may require suitable containment.
KEY CONCEPT: Hammer mill = impact + high-speed rotor + screen. In exams, these three points
should immediately appear in your answer.

6. Ball Mill
A ball mill consists of a rotating cylindrical vessel partially filled with grinding balls. As the cylinder rotates,
the balls are lifted and then fall or cascade, causing impact and attrition of the material.

Figure 2. Original schematic diagram of a ball mill.

6.1 Principle
Size reduction occurs mainly by impact of falling/rolling balls and attrition between balls, particles and the
mill lining.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
6.2 Construction
 Horizontal cylindrical shell.
 Grinding balls made from suitable material.
 Drive mechanism for rotation.
 Lining of suitable wear-resistant material.
 Feed and discharge arrangement.

6.3 Working
15. Feed material and grinding balls are loaded into the mill.
16. The cylinder rotates.
17. The balls are carried upward by the rotating shell and then fall/cascade.
18. Impact and rubbing actions fracture the particles.
19. With continued operation, the particle size decreases.
20. The product is discharged by the selected batch or continuous arrangement.

6.4 Critical speed


There is a critical rotational speed at which the balls tend to remain pressed against the mill wall instead of
falling effectively. Practical operation is generally below the critical speed so that useful
cascading/cataracting action occurs.
Conceptual critical-speed relation for a simple ball mill: N_c ∝ 1/√D
The exact numerical equation depends on the diameter definition and unit system used.

6.5 Uses
 Fine grinding of many crystalline and brittle materials.
 Wet or dry milling depending on formulation/process requirements.
 Preparation of powders where impact and attrition are desired.

6.6 Advantages
 Can produce fine powders.
 Can be operated batchwise or continuously depending on design.
 Suitable for many materials and can be enclosed.

6.7 Disadvantages
 Relatively slow compared with some high-speed impact mills.
 Noisy and energy intensive.
 Grinding-media or liner wear can contaminate product.
 Generally unsuitable for highly fibrous or very sticky feed.
KEY CONCEPT: Ball mill = impact + attrition. Ball movement and mill speed determine whether
useful grinding occurs.

7. Fluid Energy Mill (Jet Mill / Micronizer)


A fluid energy mill uses a high-velocity compressed gas stream to accelerate particles. Particle–particle
collisions and attrition cause very fine grinding.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
Figure 3. Original schematic diagram of a fluid energy mill.

7.1 Principle
Impact and attrition produced by high-velocity particle collisions in a turbulent gas stream.

7.2 Construction
 Grinding chamber, often loop/annular in configuration.
 High-pressure air or inert-gas nozzles.
 Feed inlet or venturi-type feed arrangement.
 Classifier/outlet arrangement.
 Cyclone, filter or other powder-collection system where required.

7.3 Working
21. Feed powder enters the high-velocity gas stream.
22. Gas accelerates the particles and produces turbulent circulation.
23. Particles collide with one another at high relative velocity.
24. Impact and attrition reduce particle size.
25. Fine particles are carried toward the outlet/classifier while larger particles remain in circulation until
sufficiently reduced.
26. The product is collected downstream.

7.4 Uses
 Production of very fine pharmaceutical powders.
 Heat-sensitive materials where conventional mechanical grinding may generate excessive local heating.
 Micronization of selected drugs and excipients.
 Processes requiring low metal-to-product contact when suitable materials and design are selected.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
7.5 Advantages
 Very fine particles can be produced.
 No conventional grinding media are required.
 Can be operated with inert gas for oxygen-sensitive materials.
 Potentially useful for thermolabile materials because there are few/no moving grinding parts in the
product zone.

7.6 Disadvantages
 High compressed-gas requirement.
 Higher operating and equipment cost.
 Not ideal for all soft, sticky or fibrous materials.
 Requires effective dust collection and process containment.
KEY CONCEPT: Fluid energy mill → high-velocity gas + particle–particle impact/attrition + very fine
particles.

8. Edge Runner Mill


An edge runner mill consists of heavy wheels that roll on a pan or bed containing the material. The rolling
action produces compression and rubbing/attrition.

Figure 4. Original schematic diagram of an edge runner mill.

8.1 Principle
Compression combined with attrition as heavy wheels roll over the material.

8.2 Construction
 Two heavy wheels or runners.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
 Horizontal pan or grinding bed.
 Central/overhead driving arrangement.
 Scraper or suitable mechanism to keep material in the grinding path.
 Drive system.

8.3 Working
27. Material is placed on the pan.
28. The heavy wheels rotate/roll over the material.
29. Compression between wheel and pan fractures particles.
30. Rubbing and rolling produce additional attrition.
31. Material is repeatedly exposed until the required consistency is obtained.

8.4 Uses
 Grinding and trituration of certain crude drugs and brittle materials.
 Mixing and grinding operations where heavy rolling action is useful.
 Preparation of pastes or coarse-to-intermediate powders depending on process design.

8.5 Advantages
 Simple and robust.
 Combines grinding with mixing/trituration.
 Useful for certain tough or semi-coarse materials.

8.6 Disadvantages
 Large and heavy equipment.
 Relatively slow.
 Not suitable when very fine, narrow particle-size distributions are required.
 Cleaning can be more difficult than with compact enclosed mills.

9. End Runner Mill


An end runner mill has a heavy runner that rotates and/or rolls on the material contained in a pan. The
process combines compression and rubbing/attrition.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
Figure 5. Original schematic diagram of an end runner mill.

9.1 Principle
Compression and attrition produced by a heavy runner acting on material in a pan.

9.2 Construction and working


 Heavy runner connected to a vertical drive shaft.
 Pan containing the feed material.
 The runner rotates/rolls over the material.
 Compression fractures particles and rubbing further reduces size.
 The product is removed when the required degree of reduction is reached.

9.3 Uses
 Trituration and grinding of selected pharmaceutical materials.
 Preparation of powders or pastes where a heavy rolling/rubbing action is desirable.

9.4 Advantages and disadvantages


Advantages Disadvantages
Simple and robust. Slow compared with high-speed impact mills.
Combines grinding and mixing/trituration. Bulky and relatively labour intensive.
Useful for selected tough/coarse materials. Not the preferred choice for very fine micronization.

10. Comparison of PCI-Specified Mills


Feature Hammer Ball Fluid energy Edge runner End runner
Main mechanism Impact Impact + attrition Impact + attrition Compression + Compression +

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
attrition attrition
Typical product Coarse/ Fine Very fine Coarse/ Coarse/
intermediate to intermediate intermediate
fine
Main moving part High-speed rotor Rotating cylinder Gas stream; no Heavy wheels Heavy runner
conventional
grinding rotor
Screen/classifier Screen commonly Depends on Classifier Usually no screen Usually no screen
used design commonly used as core as core
mechanism mechanism
Heat concern Moderate/high at Can be significant Often Lower speed but Lower speed but
high speed advantageous for process process
heat-sensitive dependent dependent
materials
Key advantage High throughput Fine grinding Very fine particle Robust trituration Simple trituration
size
Key limitation Heat/dust/wear Slow/noisy/media Gas Bulky/slow Bulky/slow
contamination cost/containment

11. Factors in Selection of a Mill


32. Define the required final particle-size range and particle-size distribution.
33. Characterize hardness, toughness, friability, elasticity and fibrous nature of the feed.
34. Assess moisture, hygroscopicity, stickiness and melting/softening behavior.
35. Consider heat sensitivity and the allowable product temperature.
36. Consider risk of contamination from contact surfaces and grinding media.
37. Determine whether the process is dry or wet and whether the liquid phase is compatible with the
product.
38. Consider capacity, feed rate, batch size and continuous/batch operation.
39. Assess cleaning, containment, dust control and cross-contamination requirements.
40. Consider explosion, flammability, toxicity and occupational-safety risks.
41. Balance capital cost, operating cost, energy consumption and maintenance.
KEY CONCEPT: Mill selection is a material–process–product decision. There is no single ‘best’ mill
for all pharmaceutical powders.

12. Open-Circuit and Closed-Circuit Milling


In open-circuit milling, material passes through the mill without deliberate recirculation of oversize particles.
In closed-circuit milling, a classifier separates the discharge and oversize material is returned to the mill.
Open circuit Closed circuit
Simple arrangement. More controlled particle-size distribution.
Single pass is possible. Oversize is recycled for further reduction.
May give broader product distribution. Can improve uniformity and reduce excessive overgrinding.
Lower equipment complexity. Requires classifier and recirculation system.

13. Dry vs Wet Size Reduction


Dry milling Wet milling
No liquid carrier is intentionally added. Material is processed in a liquid medium.
Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
Useful when product must remain dry or is moisture Useful for suspensions, dispersions and some colloidal
sensitive. systems.
Dust generation may be significant. Dust can be reduced substantially.
Heat and electrostatic effects may require control. Viscosity and liquid-solid interactions influence milling.
Downstream drying may not be required. May require subsequent separation/drying depending on
product.

14. Pharmaceutical Applications


 Reduction of crude drug particle size before extraction.
 Preparation of powders for tablets and capsules.
 Improvement of dissolution rate by increasing surface area.
 Micronization of selected active pharmaceutical ingredients.
 Preparation of inhalation-grade or other specialized particle-size fractions where applicable.
 Improvement of blend uniformity and processing consistency.
 Preparation of materials for granulation, compression or encapsulation.
 Preparation of suspensions/dispersions using suitable wet-milling equipment.

15. Important High-Yield Concepts


KEY CONCEPT: Size reduction increases surface area; this is a major reason it can accelerate
dissolution, extraction and drying.

KEY CONCEPT: Impact = striking; compression = squeezing; cutting = slicing; attrition = rubbing.

KEY CONCEPT: Kick = coarse; Bond = intermediate; Rittinger = fine / new surface.

KEY CONCEPT: Hammer mill = impact. Ball mill = impact + attrition. Fluid energy mill = particle–
particle impact + attrition. Edge runner = compression + attrition. End runner = compression +
attrition.

KEY CONCEPT: Excessive milling can cause heat generation, overgrinding, dust, equipment wear
and product contamination.

KEY CONCEPT: The desired particle-size distribution—not merely the smallest possible particle—is
the usual process target.

16. Common Examination Questions


42. Define size reduction and discuss its objectives in pharmaceutical engineering.
43. Explain the mechanisms of size reduction with suitable examples.
44. Discuss Kick’s, Rittinger’s and Bond’s laws.
45. Explain factors affecting size reduction.
46. Describe the principle, construction, working, uses, advantages and disadvantages of a hammer mill
with a neat labelled diagram.
47. Describe the construction and working of a ball mill with a neat diagram. Explain critical speed.
48. Explain the principle, construction and working of a fluid energy mill with a neat diagram.
49. Explain edge runner mill and end runner mill with diagrams.
50. Compare hammer mill, ball mill and fluid energy mill.
Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
51. Discuss factors affecting selection of a size reduction mill.

17. Viva / Short Questions


52. What is another name for size reduction?
53. Why is surface area important in pharmacy?
54. Which mechanism is dominant in a hammer mill?
55. Which mechanisms operate in a ball mill?
56. Which mill is commonly used for very fine grinding?
57. What is critical speed?
58. Why is fluid energy milling useful for selected heat-sensitive materials?
59. What is the main difference between edge runner and end runner mills?
60. What is the role of a screen in a hammer mill?
61. Which law is associated with new surface area?
62. Which law is generally used for coarse size reduction?
63. What factors determine mill selection?

18. Quick Formula / Concept Sheet


Topic Key relation / concept
Kick E = Kₖ log(D₁/D₂)
Rittinger E = Kᵣ(1/D₂ − 1/D₁)
Bond E ∝ (1/√D₂ − 1/√D₁)
Walker/general dE/dD = −K/Dⁿ
Critical speed N_c ∝ 1/√D (conceptual relation; units/design dependent)
Surface area Smaller particles generally provide greater specific surface
area.
Hammer mill Impact
Ball mill Impact + attrition
Fluid energy mill Impact + attrition
Edge runner Compression + attrition
End runner Compression + attrition

19. Common Mistakes to Avoid


 Do not write that all mills work by impact; identify the dominant mechanism.
 Do not confuse Rittinger’s law with Kick’s law.
 Do not state that the smallest possible particle size is always the objective.
 Do not ignore heat generation and product degradation.
 Do not omit the screen/classifier when describing equipment that relies on it for product-size control.
 Do not confuse critical speed with the normal operating speed of a ball mill.
 Do not describe fluid energy milling as mechanical rotor grinding; the grinding action is generated by
high-velocity gas and particle collisions.
 Do not use textbook diagrams as if they were your own; use properly labelled original schematics or cite
the source.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
20. Reference Framework
These notes were prepared as an original teaching resource by aligning the PCI Pharmaceutical
Engineering syllabus with standard pharmaceutical engineering principles and the topics associated with
C.V.S. Subrahmanyam’s Pharmaceutical Engineering.
PCI’s BP304T syllabus explicitly lists Size Reduction under Unit I and requires objectives, mechanisms and
laws, factors affecting size reduction, and the principle/construction/working/uses/merits/demerits of the five
specified mills. citeturn0search32turn0search8
C.V.S. Subrahmanyam’s Pharmaceutical Engineering is a standard reference for pharmaceutical unit
operations and includes size-reduction topics and examination-oriented questions on ball mills, hammer
mills, mechanisms, laws and mill selection. citeturn0search9
Additional cross-checking was made against pharmaceutical engineering teaching resources covering the
same PCI unit, including descriptions of hammer, ball and fluid-energy milling.
citeturn0search5turn0search7
KEY CONCEPT: The diagrams in this Word document are original educational schematics created
for these notes. They are intentionally simplified so that students can redraw them in examinations
with clear labels.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
21. Expanded Detailed Study Notes
Purpose of this expanded section: The earlier notes provide an examination-ready overview. This section
expands each PCI-listed point with engineering reasoning, pharmaceutical examples, operating
considerations, process variables, quality attributes, and points useful for long-answer questions.
The PCI BP304T syllabus explicitly requires objectives, mechanisms and laws of size reduction; factors
affecting size reduction; and the principle, construction, working, uses, merits and demerits of hammer, ball,
fluid-energy, edge-runner and end-runner mills. citeturn0search24
C.V.S. Subrahmanyam's Pharmaceutical Engineering, Unit Operations-II, gives Size Reduction as Chapter
1 and organizes it into mechanisms, modes of stress, classification of equipment, equipment, mill selection,
theories and energy of comminution. citeturn0search0turn0search2

22. Size Reduction – Fundamental Concepts in Greater Detail


22.1 What actually happens during comminution?
A solid particle contains internal bonds that hold its structure together. During milling, mechanical energy is
transmitted to the particle through a stress field. If the applied stress exceeds the local strength of the
material, cracks initiate and propagate. The original particle is therefore converted into smaller fragments.
The energy supplied to the mill is not completely converted into new surface; much is dissipated as heat,
sound, vibration, elastic deformation, air movement and equipment friction.
KEY CONCEPT: The useful part of milling energy is the portion that produces fracture and new
surface. A major engineering challenge is to obtain the required particle-size distribution with
minimum unnecessary energy, heat and wear.

22.2 Size reduction ratio


Size reduction ratio expresses the extent to which particle size has been reduced. A simple conceptual
expression is the ratio of characteristic feed size to characteristic product size.
Size reduction ratio ≈ D₁ / D₂
For real powders, particle size is not represented by one perfectly defined dimension. Mean, median, d10,
d50, d90, sieve size or another characteristic diameter may be used depending on the process and
measurement method.

22.3 Why particle-size distribution matters


A mill rarely produces particles of exactly one size. Instead, it generates a distribution. Two powders may
have the same average particle size but different proportions of fines and coarse particles. In
pharmaceutical manufacturing, this can affect flowability, segregation, dissolution, compressibility,
suspension behavior and content uniformity.
Particle-size attribute Meaning / importance
D10 Size below which about 10% of the measured distribution
lies; useful for understanding the fine tail.
D50 Median particle size; about half of the measured population
is smaller and half larger.
D90 Size below which about 90% lies; useful for monitoring the
coarse tail.
Span A common measure of distribution breadth; one form is

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
(D90−D10)/D50.
KEY CONCEPT: A narrow, controlled distribution may be more valuable than simply achieving a very
low average particle size.

23. Detailed Mechanisms and Modes of Stress


23.1 Compression
Compression occurs when a particle is squeezed between two surfaces. Compressive stress causes
deformation and, in brittle materials, crack formation. Compression is especially important in coarse crushing
and in heavy-wheel equipment such as edge runner and end runner mills.
 Best suited to materials that fracture under compressive loading.
 Repeated compression can progressively reduce coarse lumps.
 Excessive compression without adequate fracture may deform soft materials instead of producing
efficient size reduction.
 Compression is often combined with shear or attrition in practical equipment.

23.2 Impact
Impact is a short-duration, high-rate loading event. A moving hammer, ball or particle strikes the material,
producing a rapid stress wave and fracture. Impact is highly effective for brittle materials.
 Hammer mill: hammer-to-particle impact is dominant.
 Ball mill: falling/cascading balls produce impact.
 Fluid energy mill: high-velocity particle-to-particle collisions produce impact.
 Impact intensity increases with relative velocity and mass distribution, but excessive speed can increase
heat, wear and dust.

23.3 Attrition
Attrition is size reduction by rubbing or sliding contact. Material is subjected to tangential forces at contacting
surfaces, which can remove small fragments and progressively create fine particles.
 Important in ball milling through ball–particle and particle–particle rubbing.
 Important in fluid-energy milling through repeated particle collisions and rubbing.
 Useful for producing finer particles than a single large compression event might produce.

23.4 Cutting and shear


Cutting applies a sharp edge to the feed, while shear applies tangential forces that cause layers or portions
of a material to slide relative to one another. Fibrous crude drugs often respond better to cutting than to pure
impact.

23.5 Combined mechanisms


Equipment Dominant mechanisms Why combined mechanisms
matter
Hammer mill Impact + secondary attrition/shear Repeated impact and screen
interaction reduce the particles until
they pass the screen.
Ball mill Impact + attrition Balls fall/cascade and also rub against
particles.
Fluid energy mill Impact + attrition High-velocity collisions repeatedly
fracture particles.
Edge runner Compression + attrition/shear Heavy rolling pressure is combined
Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
with rubbing.
End runner Compression + attrition/shear Runner presses and rubs material
against the pan.

24. Factors Affecting Size Reduction – Detailed Discussion


24.1 Hardness
Hardness is resistance to indentation or localized deformation. Hard materials require greater stress to
initiate fracture and can cause significant wear of hammers, balls, liners and other contacting surfaces.
KEY CONCEPT: Hardness influences energy demand and equipment wear. For a hard abrasive
drug/excipient, material-of-construction and contamination control become especially important.

24.2 Toughness
Toughness is the ability to absorb energy before fracture. A tough material may deform rather than break
when struck. Cutting, shearing or controlled cooling may be more effective than high-impact milling for some
tough materials.

24.3 Friability and brittleness


Friable or brittle materials fracture easily when subjected to impact or compression. Such materials are
generally easier to mill than tough or elastic materials. However, excessive impact can generate too many
fines.

24.4 Elasticity
Elastic materials can store mechanical energy and recover their shape after deformation. This can reduce
fracture efficiency because the energy may be returned as elastic recovery rather than used to propagate
cracks.

24.5 Moisture content


Moisture can change hardness, cohesion, plasticity and surface properties. Some powders become softer
and more cohesive when wet; they may stick to the mill, block screens and form agglomerates. On the other
hand, controlled wet milling can be advantageous when a liquid phase is required for a downstream
suspension or dispersion.

24.6 Melting point and heat sensitivity


Milling generates heat through friction and deformation. A low-melting material may soften, smear or stick to
equipment. Thermolabile drugs may degrade if product temperature becomes excessive. Cooling, lower
energy input, intermittent milling or fluid-energy milling may be considered depending on the material.

24.7 Hygroscopicity
Hygroscopic powders absorb atmospheric moisture. Moisture uptake may increase cohesion and lead to
screen blockage, poor flow and agglomeration. Closed equipment and humidity-controlled processing may
therefore be required.

24.8 Feed particle size


A mill has an effective operating range. Very large feed may overload the equipment, while a feed that is
already extremely fine may be unnecessarily exposed to further milling. Pre-crushing can improve
throughput and protect the fine grinder.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
24.9 Mill speed
Speed controls impact energy, centrifugal effects, residence time and heat generation. For a ball mill, speed
relative to critical speed is particularly important. For a hammer mill, increasing rotor speed generally
increases impact intensity but can also increase heat, dust and wear.

24.10 Feed rate


At excessive feed rates, the mill may be overloaded and particle residence time may become insufficient. At
very low feed rates, energy efficiency may decrease. Optimum feed rate is therefore equipment- and
material-dependent.

24.11 Screen size / classifier setting


In mills equipped with screens or classifiers, the separation setting strongly influences the product. A smaller
screen opening generally requires particles to undergo more breakage before discharge. A classifier can
return coarse particles to the grinding zone.

24.12 Atmosphere
For oxidizable or combustible powders, an inert atmosphere such as nitrogen may be considered where
justified by process safety. Fine pharmaceutical dust can present explosion hazards under suitable
conditions, so dust collection, grounding and explosion protection must be addressed through a formal
safety assessment.
KEY CONCEPT: For pharmaceutical milling, material properties, product CQAs, equipment settings
and safety conditions must be considered together.

25. Hammer Mill – Advanced Details


25.1 Rotor and hammer action
The rotor transfers kinetic energy to the hammers. A particle entering the grinding zone is struck and
accelerated. It may then collide with another particle, the chamber wall or the screen. This sequence can
occur repeatedly. The final product therefore reflects both direct hammer impact and secondary collisions.

25.2 Screen function


The screen is not simply a passive filter. It provides a controlled exit condition. Particles that remain larger
than the effective opening are retained in the chamber and receive additional impacts. Screen area, opening
geometry, wear and blinding therefore affect throughput.

25.3 Why screen opening does not equal final particle diameter
Particles are irregular in shape. They may pass through an opening in an orientation that allows their
shortest dimension to pass. Consequently, the final powder may contain particles with dimensions larger
than the nominal screen opening. The actual distribution depends on particle shape, screen design and
milling conditions.

25.4 Pharmaceutical process controls


 Rotor speed.
 Feed rate.
 Screen opening and screen integrity.
 Product temperature.
 Mill pressure / ventilation where applicable.
 Metal detection and equipment inspection after maintenance.
Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
 Dust containment and cleaning validation.

25.5 When not to select a hammer mill


 Highly sticky materials that clog the screen.
 Very fibrous materials that wrap around the rotor.
 Extremely heat-sensitive products when the process temperature cannot be controlled.
 Materials for which the required product is substantially finer than the mill can efficiently provide.

26. Ball Mill – Advanced Details


26.1 Cascading and cataracting
At suitable speeds, grinding balls are lifted by the rotating shell and then fall or cascade. Lower-energy
rolling/cascading favors attrition, while higher trajectories produce stronger impact. The operating regime
depends on mill geometry, speed, ball loading and material properties.

26.2 Critical speed


Critical speed is the theoretical speed at which centrifugal force acting on a ball at the mill wall balances the
effective gravitational tendency that would otherwise make it fall. At or above this condition, balls tend to
remain attached to the wall, reducing useful impact.
At critical speed: centrifugal tendency ≈ gravitational tendency
KEY CONCEPT: The practical ball-mill speed is normally below critical speed so that balls repeatedly
fall/cascade rather than remain pinned to the wall.

26.3 Ball size and loading


Large balls are useful for breaking relatively large feed particles because they provide stronger individual
impacts. Smaller balls provide more contact points and can be useful during fine grinding. Ball size
distribution and loading are therefore process variables.

26.4 Wet versus dry ball milling


 Dry milling avoids introducing a liquid but can create dust and electrostatic issues.
 Wet milling can reduce dust and can be useful when the final dosage form is a suspension or dispersion.
 Wet milling changes viscosity, lubrication and collision behavior.
 Downstream separation, solvent removal or drying may be required after wet milling.

26.5 Limitations
Ball milling can be slow and energy intensive. Prolonged grinding may alter crystal form, cause
amorphization or produce heat. The possibility of contamination from balls and liners must be assessed,
particularly for high-potency or sensitive products.

27. Fluid Energy Mill – Advanced Details


27.1 Why very fine particles are possible
The gas stream accelerates particles to high velocities. When particles collide, the relative velocity can be
high enough to produce fracture. A classifier or geometry-based separation allows finer particles to leave
while coarser particles remain in the grinding zone.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
27.2 Heat-sensitive materials
The absence of conventional mechanical grinding elements in the product zone reduces direct mechanical
heat generation. Expansion of compressed gas can also provide a cooling effect. Nevertheless, product
temperature must still be monitored because the feed, gas compression, environment and process
conditions determine the actual thermal behavior.

27.3 Micronization
Micronization is the production of particles in the micrometre range. In pharmaceuticals, micronization can
be used to increase specific surface area and alter dissolution or aerodynamic behavior. It must be
controlled carefully because excessive fines, electrostatic charging and agglomeration can occur.

27.4 Inert gas and containment


Nitrogen or another suitable inert gas may be used where oxidation or combustible-dust risk warrants it.
Selection must be based on formal hazard analysis, oxygen concentration requirements, equipment design
and regulatory/site safety procedures.

28. Edge Runner and End Runner – Advanced Details


28.1 Edge runner
In an edge runner, the heavy wheels travel around a pan and compress the material against the bed. The
rolling motion produces a combination of crushing, rubbing and shearing. The equipment is particularly
useful when substantial mechanical pressure and trituration are required.

28.2 End runner


An end runner uses a heavy runner associated with a vertical shaft. The runner acts on material placed in a
pan. The pressure and rubbing action produces trituration. Compared with high-speed fine grinders, these
machines are slower but useful for robust, relatively coarse operations.

28.3 Difference between edge runner and end runner


Point Edge runner End runner
Runner movement Wheel rolls around the pan/bed. Runner acts from a vertical shaft and
rolls/rotates over the pan.
Main action Compression + rubbing/shearing. Compression + rubbing/shearing.
Typical use Heavy trituration / crushing. Trituration and grinding of selected
materials.
Design impression Horizontal wheel arrangement. Vertical runner arrangement.
Common exam point Heavy wheels on a pan. Heavy runner on/over a pan.

29. Selection of a Mill – Detailed Decision Framework


Mill selection should begin with the product requirement rather than the equipment name. The process
engineer first defines the desired particle size and CQAs, then matches the material and process constraints
to an appropriate mill.
Question Why it matters Possible implication
What final size is required? Determines whether coarse, fine or Hammer/ball/fluid-energy choice may
ultrafine equipment is needed. differ.
Is the material brittle or tough? Determines fracture behavior. Impact for brittle; cutting/shear for
Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
some tough/fibrous materials.
Is it sticky or low-melting? Risk of clogging and heat-related Cooling, wet processing or alternate
smearing. mill may be needed.
Is it thermolabile? Excess heat can degrade Consider cooling, lower-energy
API/excipient. operation or fluid-energy milling.
Is it oxidizable/combustible? Fine dust can present fire/explosion Closed/inert system and appropriate
risk. explosion protection may be required.
Is contamination critical? Wear particles can enter product. Select suitable contact materials and
assess wear.
Is narrow PSD required? Broad distribution may affect Classifier or milling + size separation
formulation performance. may be needed.
Is the process wet or dry? Liquid changes particle interactions Select wet-capable or dry equipment
and downstream operations. accordingly.
What capacity is needed? Lab and production requirements differ. Scale, throughput and
continuous/batch design matter.
KEY CONCEPT: The ‘best mill’ is the one that reliably produces the required CQAs at acceptable
energy, temperature, contamination risk, cost and safety.

30. Energy of Comminution – Detailed Explanation


The energy requirement increases substantially as particle size becomes smaller because creating new
surface becomes progressively more demanding. The empirical laws of Kick, Rittinger and Bond are
therefore different approximations to a complex fracture process.

30.1 Kick – physical interpretation


Kick's approach treats the energy requirement as related to the size-reduction ratio. If two operations reduce
geometrically similar particles by the same ratio, the specific energy requirement is predicted to be similar. It
is therefore more useful for coarse reduction.

30.2 Rittinger – physical interpretation


Rittinger's approach focuses on new surface area. As particle size becomes smaller, surface area per unit
mass increases dramatically. Therefore, the law is more relevant to fine grinding.

30.3 Bond – practical interpretation


Bond introduced an intermediate relationship and a work index to represent the grinding resistance of a
material. It is widely used in industrial grinding calculations and equipment comparisons.

30.4 Important limitation


These laws are empirical or semi-empirical approximations. Actual energy consumption depends on material
properties, particle-size distribution, mill design, speed, feed rate, residence time and operating conditions.
They should not be treated as exact physical laws for every pharmaceutical mill.

31. Critical Quality Attributes (CQAs) and Process Parameters


Milling is a pharmaceutical manufacturing step and should be considered in terms of critical quality attributes
and critical process parameters. The final powder must meet its intended functional requirements.
Potential CQA Examples of milling-related impact
Particle-size distribution Too coarse may reduce dissolution; too fine may increase
cohesion/agglomeration.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
Specific surface area Changes with particle size and can alter dissolution and
adsorption.
Crystal form / solid state High-energy milling can induce structural changes in some
materials.
Moisture Milling can expose fresh surface and alter moisture
interaction.
Bulk/tapped density Particle-size and shape changes can alter packing.
Flow properties Fines may increase cohesion and reduce flow.
Assay / content uniformity Segregation or loss during milling can affect uniformity.
Temperature Excessive temperature can degrade thermolabile materials.
Contamination Wear of mill components may introduce foreign particles.

31.1 Important process parameters


 Mill speed.
 Feed rate.
 Screen size / classifier setting.
 Residence time.
 Grinding-media size and load for ball mills.
 Gas pressure/flow for fluid-energy mills.
 Product temperature.
 Moisture or solvent content.
 Equipment cleanliness and line clearance.
 Sampling and particle-size testing strategy.

32. Additional Worked Examples


Example 1 – Size reduction ratio
A feed has a characteristic size of 4 mm and the desired product has a characteristic size of 0.5 mm.
Size reduction ratio = 4/0.5 = 8
Therefore, the approximate size reduction ratio is 8:1.

Example 2 – Comparing the effect of final size in Rittinger's concept


If the final diameter is reduced substantially, the term 1/D₂ increases strongly.
E ∝ (1/D₂ − 1/D₁)
Thus, fine grinding can require disproportionately more energy because a large amount of new surface is
generated.

Example 3 – Ball mill critical-speed concept


If the mill diameter is increased while all other factors are conceptually held constant, critical speed
decreases approximately with the inverse square root of diameter.
N_c ∝ 1/√D
Therefore, a larger-diameter mill does not operate at the same numerical critical speed as a smaller mill.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm
33. How to Write a 10-Mark Answer on Any Mill
64. Start with a one- or two-sentence definition.
65. State the principle and identify the dominant mechanism.
66. Draw a large, simple, labelled diagram.
67. List the major constructional parts.
68. Explain the working sequentially from feed to product.
69. Give 3–5 pharmaceutical uses.
70. Give at least 3 advantages.
71. Give at least 3 disadvantages.
72. End with a one-line key concept or suitable material statement.
KEY CONCEPT: For university exams, a clear labelled diagram plus principle–construction–
working–uses–merits–demerits is usually more effective than a long unstructured paragraph.

34. One-Page Final Revision Map


Topic Remember this first
Objective Increase surface area + obtain required PSD + improve
downstream processing.
Compression Squeezing / crushing.
Impact Striking at high speed.
Attrition Rubbing.
Cutting Sharp-edge action.
Kick Coarse size reduction.
Bond Intermediate practical grinding.
Rittinger Fine grinding / new surface.
Hammer mill Impact + rotor + screen.
Ball mill Impact + attrition + balls + critical speed.
Fluid energy mill High-velocity gas + particle collisions + micronization.
Edge runner Heavy wheels + compression/attrition.
End runner Heavy runner + compression/attrition.
Selection Material + target PSD + heat + contamination + safety +
cost.
Quality PSD, temperature, solid state, contamination, flow and
dissolution may all be affected.

35. Recommended Textbook Reading


For detailed classroom study, use C.V.S. Subrahmanyam's Pharmaceutical Engineering, Unit Operations-II,
Chapter 1: Size Reduction, along with the current PCI syllabus. The publisher lists the book's Size
Reduction chapter under Unit Operations-II. citeturn0search0
For the B. Pharm examination, students should specifically cross-check the university's adopted syllabus
because PCI has published a new B. Pharm syllabus under NEP 2020 for implementation from academic
sessions 2026–27. citeturn0search4turn0search8
The diagrams included in this document are original simplified teaching schematics, designed to be easy to
understand and redraw in an examination; they are not copied textbook figures.

Size Reduction – Pharmaceutical Engineering | B. PharmSize Reduction – Detailed Pharmaceutical Engineering Notes | B. Pharm

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