Particulate systems

Characterisation of particles
 Solids
• Solids have different forms making them difficult to handle
 Examples of forms, soft or fragile

• In general, solids are more difficult to handle than liquids,

vapors and gases because they appear in many forms. They
can be
 large angular pieces,
 wide continuous sheets,
 finely divided powders,
 and they may be hard and abrasive, tough and rubbery,
soft or fragile, dusty, plastic sticky.
• Whatever their form, means must be found to manipulate
these solids as they occur and if possible to improve their
handling characteristics.
Why measure particle properties?
Better control of quality of product (cement,
minerals etc)
 Better understanding of products,
ingredients.
 Designing of equipment for different
operations such as crushing, grinding,
conveying, separation, storage etc.
 Continued…..
• 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.
Describing the size of a single particle
• Regular-shaped particles can be described by
 their shape
number of dimensions.
 Shape of a particle
Simplest shape of a particle is a sphere because
of
Symmetry- orientation is not considered
Particle looks the same from whatever
direction it is viewed
Behaves the same in a fluid irrespective of
orientation
Methods for measuring particle shape
• The shape of an individual particle is expressed in
terms of the sphericity, Φ𝑠 which is independent of
particle size.
• Sphericity is the ratio of surface area of sphere of same
volume as particle to the surface area of particle.

– For a spherical particle of a diameter Dp ; Φ𝑠 =1

6𝑣𝑝
– For a non spherical particle; Φ𝑠 =
𝐷𝑝 𝑆𝑝

where: Dp = equivalent diameter or nominal diameter of particle

Sp= surface area of one particle
vp=volume of one particle

Equivalent diameter – is sometimes defined as the diameter of a sphere of equal volume

 For fine granular materials:
Nominal Size – based on screen analyses or microscopic examination
Surface Area – found from adsorption measurements or from pressure
drop in a bed of particles
• For many crushed materials, Sphericity is between 0.6 and 0.8.
• For particles rounded by abrasion, their sphericity may be as high as 0.95.
• For cubes and cylinders, for which length L equals the diameter, the equivalent
diameter is greater than L and, Φ𝑠 found from the equivalent diameter would
be 0.81 for cubes and 0.87 for cylinders
– it is more convenient to use nominal diameter L for these shapes
– Surface area to volume ratio is 6/Dp

For column packings (rings and saddles), nominal size is also used for Φ𝑠
• Task: Determine the sphericity of a particle
which has a surface area of 20 mm2 and
volume 4 mm3
Methods for measuring particle shape
• Another method of indicating shape is to use
the factor by which the cube of the size of
the particle must be multiplied to give the
volume.
 Particle size
• By far the most important physical property of particulate samples is particle size.
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.

• Particle size measurement is routinely carried out across a wide range of industries and is often a critical
parameter in the manufacturing of many products.
• Units used for particle size depend on the size of particles.
– Coarse particles: inches or millimetres
– Fine particles: screen size
– Very fine particles: micrometers or nanometers
– Ultra fine particles: surface area per unit mass, m2/g
 Particle size determination
Sieving (<50 um) -a nest of sieves, each lower sieve being
of smaller aperture size
Sieves may either be:
• mounted on a vibrator, which gives a degree of vertical
movement in addition to the horizontal vibration,
• may be hand shaken
Whether or not a particle passes through an aperture
depends on
• size,
• Orientation at the surface of the screen.
• Sieves are available in a number of standard
series
 Microscopic analysis
• Microscopic examination- measurement of
the projected area of the particle
• Also enables assessment of its two-
dimensional shape.
• The apparent size of particle is compared with
that of circles engraved on a graticule in the
Eyepiece
 Sedimentation and elutriation
methods (> 1 um)
• Method depends on terminal falling velocity
of a particle- terminal falling velocity increases
with size
• Two types of sedimentation methods
• Pipette: samples are abstracted from the
settling suspension at a fixed horizontal level
at intervals of time. Each sample contains a
representative sample of the suspension.
• Second method
Involves the use of the sedimentation balance,
particles settle on an immersed balance pan
which is continuously weighed.
The largest particles are deposited preferentially
and consequently the rate of increase of weight
falls off progressively as particles settle out.
 Elutriation method
• The elutriation method is really a reverse
sedimentation process
• Particles are dispersed in an upward flowing
stream of fluid.
• All particles with terminal falling velocities less
than the upward velocity of the fluid will be
carried away
 Particle size determination
• Give the experimental method and
procedures for sampling particles
 Determining particle size
• expressing a single particle size is not simple when its shape is
irregular
• Irregular particles can be described by a number of sizes.
• There are three groups of definitions:
 Equivalent sphere diameters: the diameters of a sphere which
would have the same property of the particle itself are found (e.g.,
the same volume, the same settling velocity)
 Equivalent circle diameters,:the diameters of a circle which would
have the same property of the projected outline of the particle are
considered (e.g., projected area or perimeter).
 Statistical diameters,:sizes are obtained when a linear dimension is
measured (usually by microscopy) parallel to a fixed direction.
Equivalent spherical diameters
• By definition,
• the equivalent volume sphere diameter is the diameter
of a sphere having the same volume as the particle.
• The surface-volume (equivalent sphere) diameter is the
diameter of a sphere having the same surface to
volume ratio as the particle.
• In practice it is important to use the method of
• size measurement which directly gives the particle
size which is relevant to the situation
• or process of interest
 Methods for measuring particle
diameter
• Feret’s statistical diameter is the mean distance
apart of two parallel lines which are tangential to the
particle in an arbitrarily fixed direction, irrespective
of the orientation of each particle coming up for
inspection.

• shear diameter - particle width obtained using an

image shearing device)
• Equivalent circle diameters – area of circle with
same area as the projected area of the particle
resting in a stable position.

• Martin’s diameter -length of the line which

bisects the particle image
• remember that the orientation of the particle on
the microscope slide will affect the projected
image and consequently the measured equivalent
sphere diameter.
• If we use a sieve to measure the particle size we
come up with an equivalent sphere diameter,
which is the diameter of a sphere passing through
the same
• sieve aperture.
• If we use a sedimentation technique to measure
particle size then it is expressed as the diameter
of a sphere having the same sedimentation
velocity under the same conditions.
Worked example
 Total particle surface area
• In a sample of uniform particles of
diameter Dp, the total volume of the particles
is m/ρp, where m = mass of the sample, ρp =
density. Since the volume of one particle is vp,
the total number of particle, N in the sample
is:
𝑚
• 𝑁=
𝜌𝑝 𝑣𝑝
 Class example
• What is the total number of particles and the
total surface area of uniform particulate
sample consisting of short cylindrical particles
of diameter and height 1mm each and density
2650 kg/m3 if the sample mass is 20 kg.
Description of populations of particles
• A population of particles is described by a particle size distribution.
Particle size distributions may be expressed as frequency distribution
curves or cumulative curves.
• The two are related mathematically in that the cumulative distribution is
the integral of the frequency distribution;
• i.e. if the cumulative distribution is denoted as F, then the frequency
distribution dF/dx.
• For simplicity, dF/dx is often written as f(x): The distributions can be by
• number, surface, mass or volume (where particle density does not vary
with size, the mass distribution is the same as the volume distribution).
Incorporating this information into the notation, fN(x) is the frequency
distribution by number, fS(x) is the frequency distribution by surface, FS is
the cumulative distribution by surface and FM is the cumulative
distribution by mass.
• In reality these distributions are smooth continuous curves. However, size
measurement methods often divide the size spectrum into size ranges or
classes and the size distribution becomes a histogram.
Determining total surface and total
volume of particles in a mixture
 Specific surface of mixture
• If the particle density ρp and sphericity Φs are known,
the surface area of particles in each fraction can be
calculated and added to give the specific surface, Aw
(The total surface area of the unit mass of particles):

• Where xi = mass fraction in a given increment,

Dpi = average diameter (taken as arithmetic
average of the smallest and largest particle diameters
in increment).
 Average particle size
• The average particle size for a mixture of particles
is defined in several different ways.
• Volume surface mean diameter Ds:

•
If number of particle Ni in each fraction is known,
instead of mass fraction xi, then:
Arithmetic mean diameter:
NT = number of particles
in the entire sample

• Mass mean diameter:

• Volume mean diameter:

• For sample consisting of uniform particles these average diameters are, of

course, all the same. For mixture containing particle of various sizes,
however, the several average diameters may differ widely from one
another.
Shape factors
The volume of any particle is proportional to its
"diameter" cubed.

a = volume shape factor

Assuming that a is independent of size, then:
 Methods for measuring volume of a
particle
• Displacement
• Electrical resistance of suspension
Specific surface
 Other important properties of
particles
• Crystallinity
• Porosity
• Surface characteristics
• Roughness
 Filtration
• Filtration is the process whereby a solid separates
from a fluid by making the suspension pass
through a porous bed, known as a filter medium.
• The bed retains the particles while the fluid
passes through the filter medium and becomes a
filtrate.
• To establish a flow of filtrate, it is necessary to
apply a pressure difference, called a pressure
drop, across the filter medium.
How to formulate a pressure drop?
Gravity,
Vacuum,
Applied pressure,
Vacuum and pressure combined,
Centrifugal force, and
 Saturation gradient.
Filtration processes can be classified in accordance with different
criteria:
1. Location of particle retention
The particles can be separated on the outer surface of the filter medium (surface filtration,
cake filtration) or inside of the filter medium (depth filtration, deep bed filtration)
2. Generation of the pressure difference
Pressure filtration, vacuum filtration, gravity filtration, centrifugal filtration
3. Operation mode
discontinuous, continuous, quasi-continuous.
Dynamic filtration and static (normal) filtration. In case of dynamic filtration are during
the filtration process mechanisms active which helps to reduce the build up of a filter
cake. The most common dynamic filtration process is cross-flow-filtration
4. Application
For example water filtration,
 Three classes of filtration

Filtration with cake-formation,

Filtration without cake-formation

Deep filtration
 Types of filtration
Filtration with Cake Formation (Give examples of metallurgical
processes where this is done)
• During filtration with cake-formation, the filter medium retains the
solid of the suspension on the surface of the filter medium as a
layer called a filter cake.
• This layer forms naturally when the pores of the filter medium are
smaller than the particles.
• When this is not the case, it is necessary to cover the filter medium
with a thin sheet of a fibrous material, called a filter aid that blocks
the particles from passing to the filter medium.
• This type of filtration, in which the flow is perpendicular to the filter
medium surface, is the most commonly used in the mineral
• industry (see Fig. 9.1).
 TYPES OF FILTRATION
Filtration without cake formation
• When the suspension flow is parallel to the filter medium surface,
the medium retains the particles and allows the fluid pass through.
• However, the flow produces a high shear at the solid surfaces that
prevents the formation of a solid layer over the filter medium,
returning the particles to the suspension.
• In this way, the filtrate crosses the filter medium while the particles
increase the suspension concentration with time.
• This type of filtration, which is called cross flow filtration, is useful
when suspensions are to be concentrated and there is no need for a
dry solid product.
• Although filtration without cake formation is also used in solid–
liquid filtration, it is mainly used in solid–gas separation
 Types of filtration
• Deep bed filtration

• To filter fine particles in diluted suspensions, filter media

are used.
• The filters have pores that are larger than the particles they
retain.
• Since they have greater depths, particles penetrate the
interior of the filter medium and are captured by the fibers
or particles forming the medium.
• This type of filter loses its properties with time, and it is
necessary to clean it to eliminate particles from its interior
or replace the filter with a new one. Two examples of deep
filtration are sand filters and car air filters (see Fig. 9.3).
 Selection of a filtration process
depends on :
• Fluid properties, such as density and viscosity,
• Nature of the solid, such as its size, shape and size
distribution,
• Properties of the suspension, such as concentration
and compressibility,
• Filter capacity,
• Commercial value of the material and whether the
solid or the fluid is the valuable material,
• Whether it is necessary to wash the cake,
• Whether it is important to keep the product from
contamination
Filtration cycles
All filtration equipment, whether batch or continuous, operate in cycles of cake
formation, washing, drying and discharge
.
• Cake formation: The first step in a filtration process is the formation of the cake.
A pump feeds the pulp into the filter chamber for pressure filtration, or the suspension
of solid particles is suctioned through the filter medium during vacuum filtration. The
magnitude of the deposited material depends on the pressure gradient, on the
suspension concentration and on the filtration time. In this stage of the cycle there is a
continuous flow of filtrate across the cake and filter medium.

• Cake washing: When it is necessary to eliminate impurities from the filter cake,
washing is part of the process. Washing implies calculating the minimum
amount of water necessary to displace the liquor from the cakes pores and the
time necessary to do this.
• Cake drying: Drying is a key part of the filtration process. Usually the overall requirement is
a cake with a small amount of moisture, for example 8 % by weight for copper concentrates.
Drying is accomplished by blowing dry air over the filter cake until enough water is displaced
from the pores to obtain a given humidity. To control this part of the process it is necessary to
know the amount of water retained in a saturated filter cake and the tolerated residual
humidity in the product. Generally, this is a technical and an economic choice.
• Cake discharge: The separation of the cake from the filter medium and its discharge are
important steps for efficient filtration. In vacuum filtration, blades scrape the filter cloth and
discharge the cake by gravity. In hyperbaric, or pressure filtration, removing the dried cake is
complicated because of the need to maintain pressure in the filtration chamber. Valves
pressurize and de-pressurize the discharge area, depending on the filtration cycle.
Filter media
The choice of a proper filter medium can often be the most important
consideration in assuring satisfactory operation of a filter. It should be
capable of properly retaining the solids that are to be separated from the
liquid, with suitable length of life. The following criteria are usually used in
the selection of a filter medium:
a- Ability to bridge solids across its pores quickly after feed is started.
b- The solids should not blind the filter openings.
c- Minimum filter medium resistance.
d- Resistance to chemical attack.
e- Acceptable resistance to mechanical wear.
f- Sufficient strength to support the filtration pressure.
g- Ability to discharge the cake easily and cleanly.
h- Relatively low cost.

Filter media are manufactured from textiles woven of cotton, synthetic fibers
and sometimes, in case fine crystals are filtered, from metal fabric of about
400 mesh opening.
Filter aids
Filtration of some solids can be accompanied with problems of slow filtration rate or
unsatisfactory filtrate clarity. This may be improved by using a filter aid. This consists of
a granular or fibrous material capable of forming a highly permeable filter cake within
which the troublesome solids will be incorporated. They are usually used when the
solids consist of very fine particles.
The particles of a good filter aid should be light and porous and chemically inert to the
filtrate. The most used types are: Diatomite which is a variety of extremely porous
silica and Expanded Perlite which is a highly porous alkali aluminosilicate. Their bulk
density is in the range of 200 - 400 kg.m-3.
Filter aids are used in two ways:
(1) Either as a pre-coat to protect the filter medium and prevent the escape of
occasional fine particles in the filtrate (the coat is applied at about 0.5 kg.m-2 of
filter area), or
(2) They can be mixed with the slurry to trap the difficult filterable particles in a
permeable cake.
 Task
• Research on the different types of filter
equipment available on the market. Their
advantages and disadvantages and areas of
application in metallurgical processes
 Filtration Parameters and Their
Measurements
• Figure 9.4 shows the several variables and parameters that influence the filtration
• process.
• Inlet variables are feed pulp flow and concentration.
• Outlet variables are filter capacity, mass of solid filtered per time unit and the
thickness and humidity of the filter cake.
• Design variables are filtration area and pressure drop in the equipment.
• Control variables are applied pressure, times for cake formation, washing,
expression and blowing, temperature, pH, additives and pulp agitation.
• Perturbations are the type of material, particle size and size distribution, impurities
• in the feed material.
• Parameters are porosity, permeability and compressibility of the cake, relative
permeabilities for air and water and residual saturation.
• To complete the necessary information to design and simulate a filtration process,
it is necessary to determine the dependence of the parameters on
• the properties of the solid and the liquid.
 Cake porosity
• The cake porosity is a function of the size distribution of the particles forming the porous bed. A
bed formed of particles of only one size will have the same porosity irrespective of the size of the
particles.
• The case of sphere packing illustrates this. Table 9.2 (Wakeman and Tarleton 1999b) shows the
porosity for different types of sphere packing.
• We can see that a three-fold value of the porosity of spheres is possible
• (0.26–0.78) for different types of packing. The nominal value used for porosity in filter cakes is e0 ¼
0:4, a bit lower than the average in Table 9.2.
• In the case of filter cakes, it is more useful to determine the porosity experimentally.
• There are three ways to do that:
1. by drying and weighing the cake,
2. by measuring the depth of the saturated cake,
3. by a water balance at the end of the bed formation time.
When the cake is saturated, the water has disappeared from the suspension and the difference
between the total water in the suspension and the water in the filtrate gives the volume of water
saturating the cake, which is equal to the volume of pores in the cake.
 Filter medium resistance and cake
permeability
• The filter medium is an important component in
the filtration process. It is a medium with pores of
different sizes and geometry, the structure of
which can cause variations in the way in which
the particles are deposited and in the
distributions of the filtrate flow. A filter cloth
must not only retain the solid particles and
produce a clean filtrate, but must also resist the
stresses imposed by the equipment. Therefore in
addition to the specific resistance to filtration, we
must consider the mechanical resistance as
another parameter.
 Filtration theory
• Depending on the material to be filtered, and the magnitude of the
pressure drop, the filter cakes can remain rigid or are compressed.
• Copper concentrates, and in general other metal concentrates, are
incompressible if flocculants are not used during the thickening
process.
• On the contrary, flocculants are always used with flotation tailings,
so their filter cakes are compressible.
• The conclusion is that in the majority of mineral processing plants
filter cakes are nearly incompressible and the theory of flow
through rigid porous beds is valid as the basis to develop a filtration
system.
• If in some instances this is not the case, compression must be
introduced in the theory.
 Assumptions of the filtration theory

Filtration with incompressible cakes

Consider a filtration process under the following restrictions:
1. The properties of the suspension, the cake and the filtrate are constant.
2. The cake formed is incompressible.
3. The filtration surface is plane.
4. The percolation velocity of the filtrate across the filter cake and the filter
medium is slow.
• There are two ways of performing filtration
• Constant pressure filtration
• Constant rate filtration
Constant pressure (batch filtration)
• If the pressure is held constant throughout the whole filtration period,
then due to the continuous deposition of the cake, the rate of filtration
will eventually decrease.
 TYPES OF INDUSTRIAL FILTERS
• Pressure filters
• Pressure filters are operated under pressures. The feed slurry is introduced to the
filter at pressures ranging from 2 to 5 atm gauge reaching in some cases figures as
high as 35 atm. The most commonly used pressure filters are of the batch type.

– Example of a pressure filter

• A plate and frame filter press is an assembly of alternate solid plates the faces of
which are studded, grooved or perforated to permit drainage and hollow frames in
which the cake collects during filtration. A filter cloth covers both faces of each
plate. Their shape is usually rectangular although circular plates and frames are
sometime used. They are hung in a vertical position on a pair of parallel supporting
bars. During filtration they are compressed between two end half-plates (one of
which is fixed) using a screw or by a hydraulic ram.
• The slurry is fed to the press under a pressure ranging from 3 to 10 atm. and
moves along a duct formed by the alignment of slots present in the top corner of
the plates and the frames. These slots are connected to grooves into the frames so
as to direct the slurry into the frames towards the two plates sandwiching the
• frame. The cake is thus allowed to deposit on the filter clothes and the
discharged filtrate flows through cock valves situated at the bottom of
each plate. During filtration, these valves are open.As the cake builds up to
cover from 70 to 90% of the frame thickness filtration is stopped and
washing begun. The wash liquid is admitted through a duct formed by
slots contained in the top corner of the plates and frames other than
those used for the flow of slurry during the filtration period. These slots
are connected with each other plate (known as wash plates), the valves of
which are closed. The liquid therefore has to pass through the entire cake
thickness until it reaches an open valve down a non-wash plate. Fig.
(8.5(b))
• In designing a filter press, we first determine the required area of
filtration. Then, the number of plates is determined depending on the
chosen dimensions of plates. These are usually of square shape. Their
dimensions range from 150 mm to more than one meter. The thickness of
plates ranges from 6 mm to 50 mm while that of frames ranges from 6 to
200 mm
Example 1
Solution
First calculate the area of the filter
 Pressure filters
• They have the following advantages:
(a) They provide high filtration rates and proper separation of fine
solids.
(b) They usually occupy a small floor space per unit area of filtration.
(c) Their initial cost is low.
(d) They are flexible in their operation, allowing to filter a wide variety
of solids.

• On the other hand, such filters have also some disadvantages:

(a) They are difficult to operate.
(b) Their operating cost is high since they require a lot of labor.
 Vacuum filters
• Vacuum filters: The rotary filter
• The most common type of continuous vacuum filters is the Rotary drum filter. This is shown in Fig.
(8.6) The filter consists of a horizontal drum with a slotted face turning at 0.2 - 2 RPM in an agitated
slurry trough. The face of the drum is covered by a filter medium (usually a cloth known as canvas)
and the drum is partly submerged in the slurry. Under the slotted cylindrical face of the main drum
is a second smaller drum with a solid surface. Between the two drums are radial partitions dividing
the annular space into separate compartments, each connected by an internal pipe to one hole in
the rotating plate of a rotary valve .A strip of filter cloth covers the exposed face of each
compartment to form a succession of panels.
• Consider the panel A in Fig.(8.7). It is about to enter the slurry in the trough. As it dips under the
surface of the liquid, vacuum is applied through the rotary valve. A layer of cake builds up on the
face of the panel as liquid is sucked through the cloth into the compartment, through the internal
pipe, through the valve into a collecting tank. As this panel leaves the drum it enters into the
washing zone. Vacuum is applied to the panel from a separate system sucking wash liquid and air
through the cake of solids. After the cake has dried vacuum is ceased and the cake removed by a
horizontal knife blade. A little air is blown in under the cake to ease its removal from the filter cloth.
Once the cake is taken away, the panel reenters the trough and the cycle is repeated (Figure 2.8).
• Often a precoat is continuously supplied on the filter surface.
 Vacuum filters
• Vacuum filters are operated using a vacuum pump or alternatively a jet
ejector. They are usually more adapted for continuous operation. They
offer the following advantages:
• (a) They use low labor compared to batch filters
• (b) Their surface is opened to the atmosphere allowing easy inspection
and repair.
• (c) The maintenance cost is relatively low.

• Drawbacks of using such filters are:

• (a) A vacuum system has to be maintained throughout the filtration
process
• (b) Due to the low pressure used , this is unsuitable for use in the case of
volatile filtrates
• (c) Such systems cannot handle difficult solids
• (d) They lack flexibility as to the type of solid and the rate of filtration