Topics /Course structure

1. Introduction - √

2. Properties and Handling of Particulate Solids:

Characterization of Solid Particles
Some properties of masses of particles
Size Reduction
Equipment of Size reduction

3. Mechanical Separations
Screening
Filtration
Cake Filters
Clarifying Filters
Crossflow filtration
Gravity sedimentation process
Centrifugal sedimentation

4. Agitation and mixing

Reading:

1.McCabe W. L., Jullian Smith C. and Peter Harriott - Unit Operations of Chemical Engineering, 7thEdition, McGraw-Hill international Edition,
2005.

2. Coulson J.M., Richardson J.F, Chemical Engineering, Vol. II, 4th Edition, Elsevier India, 2006.
3. Alan S. Foust, Leonard A. Wenzel, Curtis W. Clump, Louis Maus, L. Bryce Andersen, Principles of Unit Operations, Wiley, 2nd Edition, 2008.
4. Walter L. Badger, Julius T. Banchero, Introduction to Chemical Engineering, Tata McGraw Hill Edition, 2001.
5. Christie John Geankoplis, Transport Processes and Separation Process Principles (Includes Unit Operations), Prentice Hall India Learning
Private Limited, 4th Edition, 2004.

NITW Mechanical Operations Topic 2 2.1. Characterization of solid particles 11

Topic 2. Properties and Handling of Particulate Solids:

2.1. Characterization of Solid Particles

Importance of solid particles
Handling and processing of solid particles are more difficult than fluids (Liquids & Gases) – Why?
Why measure properties (characterization) of solid particles?
Which particle properties are important to measure?

2.1.1. Particle size (single)

Why is particle size important?
How do we define particle size?
The equivalent spherical diameter

2.2.2. Particle shape

Why is particle shape is important?
How do we define particle size?
Sphercity

2.2. Mixed particle sizes and analysis

Specific surface of mixture
Average mixture
Number of particles in mixture
Screen analysis
Size measurements with fine particles

2.3. Properties of masses of particles

Storage and conveying of solids
Bulk storage
Bin storage
Flow out of bins
Conveyors
1
 Topic 2.

Properties and Handling of Particulate Solids

NITW Mechanical Operations Topic 2 2.1. Characterization of solid particles 2

 2.1. Characterization of Solid Particles

2.1. Characterization of Solid Particles

• Importance of solid particles

• Handling and processing of solid particles are more difficult than fluids (Liquids &
Gases) – Why?
• Why measure properties (characterization) of solid particles?
• Which particle properties are important to measure?

2.1.1. Particle size (single)

Why is particle size important?
How do we define particle size?
The equivalent spherical diameter

2.2.2. Particle shape

Why is particle shape is important?
How do we define particle size?
Sphercity

NITW Mechanical Operations Topic 2.1 2.1. Characterization of solid particles 3

 2.1. Characterization of Solid Particles

 In introduction,
Mechanical operation/Mechanical unit operation /Mechanical separations based on
mechanical-physical forces and the classification involves operation with particulate solids.

 The objective of the subject is to separate the solids.

What is a particle?

At the most basic level, we can define a particle as being a discrete sub portion of a substance.
 2.1. Characterization of Solid Particles
Importance of solid particles

 Enni (a researcher) reported that in 1985&1982 Dupont (which covers the business of
chemicals, dyes, ceramics, pharma) is found to that 60% of its products are solid in
particulate form (powder, crystalline, granular, flakes)

 Dow chemical – 50% products are solids

 These two companies have thousands of major unit operations involving solid particles

The most common types of materials consisting of particles are:

• powders and granules e.g. pigments, cement, pharmaceutical ingredients

• suspensions, emulsions and slurries e.g. vaccines, milk, mining muds

• aerosols and sprays e.g. asthma inhalers, crop protection sprays

 2.1. Characterization of Solid Particles
Importance of solid particles

• powders and granules e.g. pigments, cement, pharmaceutical ingredients

Granulation is the process in which primary powder A powder is a mixture of finely divided drug
particles are made to adhere to form larger and /or chemicals in dry form
Multiparticle emtitites called granules.
which do not flow
• Granules are agglomerates of powdered which do flow
materials prepared into larger Free flowing particles

• But what about dry sand? It flows in an hourglass.

It takes the shape of its container, as liquids do.

• One grain of sand is of course a solid, but a whole

lot of grains together are a granular material,
with quite different properties.

• As with solids, they can withstand deformation

and form heaps; as with liquids, they can flow; as
with gases, they exhibit compressibility
 2.1. Characterization of Solid Particles
Importance of solid particles
• suspensions, emulsions and slurries e.g. vaccines, milk, mining muds
Stability in Suspensions/emulsions
=> A suspension is a mixture between two substances, one of which is finely divided and dispersed in the other.
Common suspensions include sand in water, dust in air, and droplets of oil in air.
Ex. Paracetamol suspension, calamine lotion etc.,
=> Emulsions (Pickering emulsion) are consisting
of ateast two immiscible liquid phases and one
stabilized by third emulsifying agent an example
of colloids composed of tiny particles suspended
in another immiscible (unmixable) material.
Ex. Gelatin, cheese

If oil and water are mixed and small oil droplets are
formed and dispersed throughout the water, eventually
the droplets leads to Flocculation or Coalescence or
sedimentation

However, if solid particles are added to the mixture,

they will bind to the surface of the interface and prevent
the droplets from coalescing, making the suspension or
emulsion more stable.

Slurry is a semi-liquid mixture, typically of fine particles of manure, cement, or coal suspended in water.
 2.1. Characterization of Solid Particles
Importance of solid particles

• aerosols and sprays e.g. asthma inhalers, crop protection sprays

An aerosol (abbreviation of "aero-solution") is a suspension of fine solid particles or liquid particles in

air or another gas
 2.1. Characterization of Solid Particles

Handling and processing of solid particles are more difficult than fluids (Liquids & Gases) – Why?

 Unlike solids, Fluids do not have shape and size

Solids appear in different forms – angular pieces,

powder, continuous sheets etc.,

Also the properties of individual solid particles have a considerable effect on solids in bulk.

 Engineer & scientists are used to dealing with gases & liquids whose properties can be
easily readily measured
• Boiling point of benzene at atm pressure safely assumed 80.1 degree centigrade
• Thermal conductivity of copper 377 w/m k at 100 degree centigrade
• Viscosity of water at 20 degree centigrade to be 0.0001 pa sec

With particulate solids, however the situation is quite different

• Flow pattern of sodium bicarbonate powder depends not only particle size, but also
particle shape and surface area (properties) etc.,
 2.1. Characterization of Solid Particles

Why measure properties (characterization) of solid particles?

1. Better control of product quality:

In an increasingly competitive global economy, better control of product quality delivers real economic benefits such
as:
• ability to charge a higher premium for your product
• reduce customer rejection rates and lost orders
• demonstrate compliance in regulated markets

2. Better understanding of products, ingredients and processes:

In addition to controlling product quality, a better understanding of how particle properties affect your products,
ingredients and processes will allow you to:

• improve product performance

• troubleshoot manufacturing and supply issues
• optimize the efficiency of manufacturing processes
• increase output or improve yield
• stay ahead of the competition.

NITW Mechanical Operations Topic 2 2.1. Characterization of solid particles 3

 2.1.1 Characterization of Solid Particles

Why measure properties (characterization) of solid particles?

Therefore,
 Design and operation of these any processes require Knowledge of the behavior of solid
particles

 So the particle characterizations is important in all aspects of productions, manufacturing,

handling processing and application.

 Characterization of particles is first necessary task required in process involving solid

particles.
 2.1.1. Characterization of Solid Particles
Which particle properties are important to measure?

In addition to chemical composition, the behavior of particulate materials is often dominated by the physical
properties of the constituent particles.

These can influence a wide range of material properties including, for example, reaction and dissolution rates, how
easily ingredients flow and mix, or compressibility and abrasivity.

From a manufacturing and development perspective, some of the most important physical properties to measure
are:
 particle size
 particle shape
 surface properties
 mechanical properties
 charge properties
 microstructure.
Depending upon the material of interest, some or all of these could be important and they may even be
interrelated: e.g. surface area and particle size.

In this subject area, we will concentrate on two of the most significant and easy to measure properties –
particle size and
particle shape.
 2.1.1. Characterization of Solid Particles – Particle properties
Particle Size
Why is particle size important?

By far the most important physical property of particulate samples is particle size.

Particle size measurement is routinely carried out across a wide range of industries and is often a critical parameter
in the manufacture of many products.

Particle size has a direct influence on material properties such as:

• reactivity or dissolution rate e.g. catalysts, tablets

• stability in suspension e.g. sediments, paints
• efficacy of delivery e.g. asthma inhalers
• texture and feel e.g. food ingredients
• appearance e.g. powder coatings and inks
• flowability and handling e.g. granules
• viscosity e.g. nasal sprays
• packing density and porosity e.g. ceramics.
 2.1.1. Characterization of Solid Particles – Particle properties
Particle Size
Why is particle size important?

Small Vs large size: The size and shape of powders influences flow and compaction properties.

• Larger, more spherical particles will typically flow more easily than smaller particles.

• Smaller particles dissolve more quickly and lead to higher suspension viscosities than larger
ones.

• Smaller droplet sizes and higher surface charge will typically improve suspension and
emulsion stability.

• Powder or droplets in the range of 2-5μm aerosolize better and will penetrate into lungs
deeper than larger sizes.
 2.1.1. Characterization of Solid Particles – Particle properties
Particle Size
Why is particle size important?

Some applications:

• In the paint and pigment industries particle size influences appearance properties including gloss
and tinctorial strength.

• Particle size of the cocoa powder used in chocolate affects color and flavor.

• Cement particle size influences hydration rate & strength.

• In the pharmaceutical industry the size of active ingredients influences critical characteristics
including content uniformity, dissolution and absorption rates.

• Other industries where particle size plays an important role include nanotechnology, proteins,
cosmetics, polymers, soils, abrasives, fertilizers, and many more

For these and many other reasons it is important to measure and control the particle size
distribution of many products.
 2.1.1. Characterization of Solid Particles – Particle properties
Particle Size
Why is particle size important?

Measuring particle size and understanding how it affects your products and processes can be critical to the
success of many manufacturing businesses.

Particle size influences many properties of

particulate materials and is a valuable indicator of
quality and performance.
 2.1.1. Characterization of Solid Particles – Particle properties
Particle Size
How do we define particle size?

Particle sizes express in terms of : coarse particles - inches or millimeters (coarse particles)
fine particles – screen size
very fine particles – micrometers or nanometers
ultrafine particles – surface area per unit mass

Regular shaped particles:

Simplest Single dimensional case - a spherical, solid, single component particle. Critical dimension or particle
size?

radius or diameter
 2.1.1. Characterization of Solid Particles – Particle properties
Particle Size
How do we define particle size?

Multi dimensional case:

1. cubes  side length

cone  base diameter and height (Two dimension)
cuboid three dimension

2. Imagine that I give you a matchbox and a ruler and ask you to tell me the size of it.

You may reply saying that the matchbox is 20 x 10 x 5mm.

You cannot correctly say "the matchbox is 20mm" as this is only one aspect of its size.

So it is not possible for you to describe the 3-dimensional matchbox with one unique number.

This is the basic problem of particle size analysis –

• how do we describe a multi dimensional object with one number only?
• What size are they?
Particles are 3-dimensional objects, and unless they are perfect spheres (e.g. emulsions or bubbles), they cannot be fully
described by a single dimension such as a radius or diameter.
 2.1.1. Characterization of Solid Particles – Particle properties
Particle Size
How do we define particle size?

More complicated: irregular particles

Obviously the situation is more difficult for a complex shape like a grain of sand or
a pigment particle in a can of paint.

If I am a Q.A. Manager, I will want one number only to describe my particles – I

will need to know if the average size has increased or decreased since the last
production run (for example)

This is the basic problem of particle size analysis –

• how do we describe a irregular object with one number only?
• What size are they?

How to quote the size of a particles in terms of a single quantity?

The concept of
“Equivalent diameter”
 2.1.1. Characterization of Solid Particles – Particle properties
Particle Size
How to find particle size for irregular particles ?
The equivalent diameter

An irregular particle can be described by a number of sizes depending on what dimension or property is
measured

Equivalent spherical diameter:

The diameter of sphere that would behave the same property as particle itself. (same volume, same projected
area, same settling velocity etc.,)

This refers to the diameter of sphere that would behave in the same manner as the particle can submitted to
specified operation.

In which some physical property of the particle is related to a sphere that would have the same property.
Name Equivalent property of sphere
Volume diameter Volume
Surface diameter Surface to volume ratio
Drag diameter Resistance to motion in the same fluid at same
Sieve diameter Passing through same square mesh

There is only one shape that can be described by one unique number and that is the sphere. If we
say that we have a 50μ sphere, this describes it exactly. We cannot do the same even for a cube
where 50μ edge or to a diagonal.
 2.1.1. Characterization of Solid Particles – Particle properties
Particle Size
The equivalent spherical diameter

 The sphere of the same weight

 The sphere of the same volume of the particle.

 The sphere of the same surface area as the

particle.

 The sphere which will just pass through the

same size of square aperture as the particle (as
on a screen).

 The sphere of the same sedimentation area

 The sphere with the same settling velocity as

Many and above particle sizing techniques are the particle in a specified fluid
based on a simple 1-dimensional sphere equivalent
measuring concept
 2.1.1. Characterization of Solid Particles – Particle properties
Particle Size
The equivalent spherical diameter

Q1. Equivalent spherical diameter of cylinder 100 X 20 μm

Imagine a cylinder of diameter D1=20 μm & height 100 μm .

There is a sphere of diameter D which have an equivalent volume to

cylinder.

 Volume of cylinder Volume of cylinder 3

D
 Volume of sphere

Volume
  of sphere

  4 𝜋 𝑥 3 =10000 𝜋
3
   This is the equivalent sphere theory.

Diameter (D) = 39.1  We measure some property of our particle and assume
that this refers to a sphere, hence deriving our one
unique number (the diameter of this sphere) to describe
  Therefore, Diameter of cylinder is 39.1 our particle.
 2.1.1. Characterization of Solid Particles – Particle properties
Particle Size
The equivalent diameter

Different techniques:

• Appropriate particle size characteristic may depend on measurement technique .

• However, there are many different types of equipment's and they typically provide equivalent spherical
diameters based on method of measurement.

Technique method of measurement

Microscopy Projected area
Sieves mesh
Coulter counter volume
Sedigraph Sedimentation
Laser diffraction Length

• therefore will give a different answer from another

technique which measures an alternative
dimension

• Each technique is not wrong – they are all right –

it is just that a different property of the particle is
being measured.
 2.1.2 Characterization of Solid Particles – Particle properties
Particle Shape
Why is particle shape is important?
• Cancer treatment:
Particle shape is another vital parameter when designing NPs (Nano Particles) because it regulates the mobility of Nano Particles in
blood circulation systems, immune responses, and behavior in internalized cells.

• Cement industry:
Compared with spherical NPs, no spherical NPs are more effective and remain longer in the blood due to their increased blood
circulation time.
Rod-shaped NPs demonstrate superior uptake performance, followed by cubical, cylindrical, and spherical NPs.

• Catalysis:
Particle shape dictates the morphology of exposed facets that come into play during a catalytic reactions.

***Shirish H Sonawane and Uday Bhaskar Babu* (*very small contribution) are working on synthesis Flower shaped Janus nano
particles for some selected reactions  To Improve yield, conversion and other properties

• The shape of the particles can impact on many properties of a powder sample, including specific surface area,
flow ability, magnetic property, packing property, abrasive property and chemical activity.

• In order to improve the characteristics and performance of some products, particle shapes have been designed
and produced based on their applications by industrial and scientific research

The shape of particles can also have significant impact upon the performance or processing of particles.
 2.1.2. Characterization of Solid Particles – Particle properties
Particle Shape
How do we define particle shape?
For regular Particles:

Sphere Cube

such as sphere & cubes – shape can easily specified

But for irregular particles (sand grain or mica flakes) – Shape ?

– The term shape is not clear and must be arbitrarily defined for irregular particles.
 2.1.2. Characterization of Solid Particles – Particle properties
Particle Shape
How do we define particle shape?

– How to quantify the shape for particle?

– One simple way to quantify shape is using Wadell’s Sphercity (ϕ), Sphericity is a measure of how
spherical an object is. Proposed by Waddell in 1935,
 – The shape of individual particles is conveniently expressed in terms of Sphercity ()

 – For a spherical particle, Sphercity () can be defined as

Surface − volume ratio of spherical of diameter   D P
  𝑠=
ϕ
Surface − volume ratio for particle whose nominal ¿   D P

 - nominal diameter of spherical particle

6 / DP (or) Equivalent diameter – diameter of a
 
Hence ,the sphercity of particle is defined as : ϕ 𝑠= sphere of equal volume
S p/ V p - Surface area of one particle
- Volume of one particle
 2.1.2. Characterization of Solid Particles – Particle properties
Particle Shape
Sphercity
Q1.
  For a spherical particle for diameter , Sphercity () = ?

  6/ D P
S phercity of particle is defined as : ϕ𝑠 = −− −(1)
S p/ V p

 
Surface
  area ( S p )=π D P 2 ,
  1
Volume ( p ) 6 π D P3 ,
V =
 S p
=6 /DP
Vp
Substitute in (1) =>
  6/ D P
ϕ 𝑠= =1
6/ D P

  Therefore, for a spherical particle of diameter ; =1

 2.1.2. Characterization of Solid Particles – Particle properties
Particle Shape
Sphercity
Q2.
  For a cylinder of diameter and Length L, Sphercity () = ?
 Sphercity of cylinder particle is defined as : ϕ = 6/ D P −− (1)
𝑠
S p/V p
 
Need
  to find of sphere i.e., Equivalent diameter concept

Volume of cylinder particle of diameter has same Volume of

sphere of diameter

6 6
  2 1 /3
D P 𝑜𝑓 𝑠𝑝h𝑒𝑟𝑒 (6 𝐷 𝑃 , 𝑐 𝐿/ 4)
ϕ 𝑠= = 2 2
Sp DP DP 𝐿
𝑜𝑓 𝑐𝑦𝑙𝑖𝑛𝑑𝑒𝑟 (π   D P L+π )/ π
Vp 2 4
 2.1.2. Characterization of Solid Particles – Particle properties
Particle Shape
Sphercity

 Q3. Calculate a Sphercity () of cylinder of diameter 1 cm and length (L) 3 cm

  phercity of cylinder particle is : ϕ = 6 / DP

S 𝑠 − −−(1)
Sp/ V p

Need
  to find of sphere i.e., Equivalent diameter
  concept
2
 Surface area of cyliner ( S )=π   D L+π DP
p P Volume
  of cylinder particle of diameter has same
2
Volume of sphere of diameter
 
Volume
  of sphere ( V p ) =Volume of cyliner ( V p )
¿  10.99
2
1
  π D P3 =2.356
  DP 𝐿 6
Volume of cyliner ( V p )=π
4
  2.356 cm3  6 = 6 =3.634
DP 1.651

 S p = 10.99 =4.666   1.651 cm

Vp 2.356

  6/ D P 3.634
ϕ 𝑠= = =0.779
S p / V p 4.666
 2.1.2. Characterization of Solid Particles – Particle properties
Particle Shape
Sphercity

 Q4. Calculate a Sphercity () of cube dimensions 1*1*1 cm

  phercity of cube particle is : ϕ = 6/ D P

S 𝑠 − − − (1)
S p/V p

  Need
  to find of sphere i.e., Equivalent diameter
concept
 
¿  6 ∗1 Volume
  of cube particle of diameter has same
Volume of sphere of diameter
¿  6 𝑐𝑚 2
Volume
  of sphere ( V p , s ) =Volume of cube ( V p , c )
Volume of cube ( V p ) =𝑎 3 1
  π D P3 =1
 
3
6
  1 𝑐𝑚
¿
 

 S p = 6 =6 𝑐𝑚 D
  P of sphere=1.24 cm
Vp 1

  6/ DP 4.84
ϕ 𝑠= = =0.806
S p /V p 6
 2.1.2. Characterization of Solid Particles – Particle properties
Particle Shape
Description Sphercity Example
Spherical 1.000 Glass beads
Cubic 0.806 Sugar, calcite
Angular 0.66 Crushed minerals
Flaky 0.54 Gypsum
Platelet 0.22 Mica, graphite
-- -- --

Sphercity quantify the shape of particle and it will be fractional Sphercity (shape factor) describe the departure of particle from a
spherical form
 2.1.2. Characterization of Solid Particles – Particle properties
Numerical Problems

 Q1. Calculate a Sphercity () of cylinder of diameter 2 cm and length (L) 5 cm

0.87 / 0.8064/ 0.878/ 0.804/0.805 /0.8045/
Q2.
  Calculate a Sphercity () of cylinder of diameter 1.5 cm and length (L) 3.5 cm
0.832/0.814/0.816/0.812/0.8136

Q3.
  Calculate a Sphercity () of cube dimensions 3*3*3 cm
0.806/0.806/

Q4. Equivalent spherical diameter of cylinder 50 X 10 μm

33.47 - volume/ 19.57 – volume / area – 23.45/23.01/23.45

Q5. Equivalent spherical diameter of cylinder 100 X 20 μm

39.149 – volume/ 46.9 - area
Thank You
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