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Particle Technology Course Outline

This course outline covers topics related to particle technology over 10 weeks. Week 1 discusses particle characterization and properties. Weeks 2-3 cover particle sizing methods and the motion of particles in fluids based on Stokes and Newton's laws. Later weeks discuss topics like fluidization, sedimentation, filtration, particle size reduction, and classification. The course introduces particulate materials used widely in various industries and processing steps involving particles. Key particle characteristics of composition, size, and shape are described. Methods of describing single particle size and distributions are also presented.

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0% found this document useful (0 votes)
148 views61 pages

Particle Technology Course Outline

This course outline covers topics related to particle technology over 10 weeks. Week 1 discusses particle characterization and properties. Weeks 2-3 cover particle sizing methods and the motion of particles in fluids based on Stokes and Newton's laws. Later weeks discuss topics like fluidization, sedimentation, filtration, particle size reduction, and classification. The course introduces particulate materials used widely in various industries and processing steps involving particles. Key particle characteristics of composition, size, and shape are described. Methods of describing single particle size and distributions are also presented.

Uploaded by

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

CHE372: PARTICLE TECHNOLOGY 3 CREDITS

COURSE OUTLINE
Week Date Topic
1 12/06-16/06 Properties of particles- Particle characterization
2 19/06-23/06 Properties of particles- Particle sizing methods
3 26/06-30/01 Motion of particles in a fluid: Stokes and Newton’s laws
4 03/07-07/07 Particles falling under gravity through a fluid; Drag coefficient of spherical
and non-spherical particles
5 10/07-14/07 Flow through packed beds- Pressure drop relationships; packed bed
pressure gradient prediction
6 17/07-21/07 Fluidization-bubbling and non-bubbling fluidization; applications of
fluidized bed
7 24/07-28/07 Sedimentation and flocculation filtration
8 31/07-04/08 Screening- size separation of particles; types of screens and distribution
Classification of particles
9 07/08-11/08 Particle Size reduction- Particle fracture mechanisms; size distribution and
prediction of product size distribution; types of Comminution equipment

10 14/03-18/03 Revision and Continuous assessment test

Recommended Textbooks

1. Unit operations of chemical Engineering By W.L. McCabe, J.C. Smith and P


Harriot
2. Introduction to Particle Technology, Edited by Martin Rhodes

INTRODUCTION

Particulate materials, powders or bulk solids are used widely in all areas of the
process industries, for example in the food processing, pharmaceutical,
biotechnology, oil, chemical, mineral processing, metallurgical, detergent, power
generation, paint, plastics and cosmetics industries. These industries involve many
different types of professional scientists and engineers, such as chemical engineers,
chemists, biologists, physicists, pharmacists, mineral engineers, food technologists
and metallurgists.
Some examples of the processing steps involving particles and powder include
particle formation processes (such as crystallization, precipitation, granulation,
spray drying, tabletting, extrusion and grinding), transportation processes (such as
pneumatic and hydraulic transport, mechanical conveying and screw feeding) and
mixing, drying and coating processes. In addition, processes involving particulates
require reliable storage facilities and give rise to health and safety issues, which
must be satisfactorily handled. Design and operation of these many processes across
this wide range of industries require knowledge of the behaviour of powders and
particles. This behaviour is often counterintuitive, when intuition is based on our
knowledge of liquids and gases. For example, actions such as stirring, shaking or
vibrating, which would result in mixing of two liquids, are more likely to produce size
segregation in a mixture of free-flowing powders of different sizes. A storage
hopper holding 500 t of powder may not deliver even 1 kg when the outlet valve is
opened unless the hopper has been correctly designed.

Particle technology is essentially concerned with techniques for processing and


handling particulate solids and the importance of its knowledge to the process
industries cannot be overemphasized. Very often, difficulties in the handling or
processing of powders are ignored or overlooked at the design stage, with the result
that powder-related problems are the cause of an inordinate number of production
stoppages. However, it has been demonstrated that the application of even a basic
understanding of the ways in which powders behave can minimize these processing
problems, resulting in less downtime, improvements in quality control and
environmental emissions.

PROPERTIES OF PARTICLES

The three most important characteristics of an individual particle are its


composition, its size and its shape.

i. Composition: composition determines such properties as density and


conductivity, provided that the particle is completely uniform. In many cases,
however, the particle is porous or it may consist of a continuous matrix in which small
particles of a second material are distributed.
ii. Particle size: particle size is important in that this affects properties such
as the surface per unit volume and the rate at which a particle will settle in a fluid.

Large quantities of particles are handled on the industrial scale, and it is frequently
necessary to define the system as a whole. Thus, in place of particle size, it is
necessary to know the distribution of particle sizes in the mixture and to be able to
define a mean size which in some way represents the behaviour of the particulate
mass as a whole. Important operations relating to systems of particles include
storage in hoppers, flow through orifices and pipes, and metering of flows. It is
frequently necessary to reduce the size of particles, or alternatively to form them
into aggregates or sinters. Sometimes it may be necessary to mix two or more solids,
and there may be a requirement to separate a mixture into its components or
according to the sizes of the particles.

iii. Particle shape: particle shape may be regular, such as spherical or cubic, or it
may be irregular as, for example, with a piece of broken glass. Regular shapes are
capable of precise definition by mathematical equations, but irregular shapes are
not and the properties of irregular-shaped particles are usually expressed in terms
of some particular characteristics of a regular shaped particle.

PARTICLE CHARACTERISATION

DESCRIBING THE SIZE OF A SINGLE PARTICLE

The simplest shape of a particle is the sphere in that, because of its symmetry, any
question of orientation does not have to be considered, since the particle looks
exactly the same from whatever direction it is viewed and behaves in the same
manner in a fluid, irrespective of its orientation. No other particle has this
characteristic. Frequently, the size of a particle of irregular shape is defined in
terms of the size of an equivalent sphere although the particle is represented by a
sphere of different size according to the property selected. Some of the important
sizes of equivalent spheres are:

(a) The sphere of the same volume as the particle.


(b) The sphere of the same surface area as the particle.
(c) The sphere of the same surface area per unit volume as the particle.
(d) The sphere of the same area as the particle when projected on to a plane
perpendicular to its direction of motion.
(e) The sphere of the same projected area as the particle, as viewed from
above, when lying in its position of maximum stability such as on a
microscope slide for example.
(f) The sphere which will just pass through the same size of square aperture
as the particle, such as on a screen for example.
(g) The sphere with the same settling velocity as the particle in a specified
fluid.

Several definitions depend on the measurement of a particle in a particular


orientation.

A measure of particle shape which is frequently used is the sphericity, ψ, defined


as:

(1)

Regular-shaped particles can be accurately described by giving the shape and a


number of dimensions. Examples are given in Table 1. For an irregular-shaped
particle, no single physical dimension can adequately be used to describe the size.

If we are using a microscope, perhaps coupled with an image analyser, to view the
particles and measure their size, we are looking at a projection of the shape of the
particles.

The common diameters used in microscopy analyses are :

i. Martin’s diameter: this is the length of the line which bisects the particle image,

ii.Feret’s diameter: this is distance between two tangents on opposite sides of the
particle.

iii. Shear diameter: this is particle width obtained using an image shearing device

iv. Equivalent circle diameters: This is diameter of circle with an area equal to
projected area of particle.
Figure 1 gives pictorial representation of these diameters

Fig 1: Some diameters used in microscopy

Table 1: Regular-shaped particles


Shape Sphere Cube Cylinder Cuboids Cone
Dimensions Radius Side length Radius and Three side Radius and
height length height
Note: In microscopy, 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.

Comparison of equivalent diameters

• The volume equivalent sphere diameter is a commonly used equivalent sphere


diameter. This is the diameter of sphere with equivalent volume.
• Surface-volume diameter is the diameter of a sphere having the same
surface to volume ratio as the particle.

By convention, particle sizes are expressed in different units depending on the size
range involved: Coarse particles are measured in inches or millimetres; fine particles
in terms of screen size; very fine particles in micrometres or nanometres; ultra fine
particles are usually described in terms of their surface area per unit mass (m2/g)

Worked Example 1

For a regular cuboid particle of dimension 1.00 mm x 2.00 mm x 6.00 mm, calculate
the following diameters:

a) The equivalent volume sphere diameter


b) The equivalent surface sphere diameter
c) The surface-volume diameter (the diameter of a sphere having the same
external surface to volume ratio as the particle)
d) The sieve diameter ( the width of the minimum aperture through which the
particle will pass)
e) The projected area diameters (diameter of the circle having the same area as
the projected area of the particle resting in a stable position)

Solution
a) Volume of cuboid = 12 mm3
Let xV = Diameter of equivalent volume sphere

Hence, xV = 2.840 mm
b) Surface area of cuboid = (6*2)2 +(6*1)2 + (1*2)2 = 40 mm2 Let xS = Diameter
of equivalent surface sphere

Hence, xS = 3.568 mm

c)

Let xSV = Surface-volume sphere diameter

Hence, xsv = 1.8 mm

d) The sieve diameter is the second smallest dimension, that is, 2 mm


e) The cuboid has three stable resting positions, and therefore has three
projected areas:
Projected area 1 = 6 mm2
Projected area 2 = 2 mm2
Projected area 3 = 12 mm2

Let diameters of the circles be xp1, xp2 and xp3

Hence, xp1 = 2.76 mm

Hence, xp2 = 1.60 mm

Hence, xp3 = 3.91 mm

CLASS WORK
Calculate the equivalent volume sphere diameter xV and the surface-volume
equivalent sphere diameter xSV of a cuboid particle of side length 2, 4 , 6 mm. [ xV
= 4.51 mm; xSV = 5.29 mm ]

HOME WORK
Calculate the equivalent volume sphere diameter xV of a cylinder of diameter 0.100
mm and length 2 mm [Answer: (a) 0.31 mm ]

Repeat class work now using a cylinder of diameter 0.100 mm and length 1.00 mm.
[Answer: (a) 0.247 mm; (b) 0.324 mm; (c) 0.142 mm; (d) 0.10 mm; (e) 0.10 mm (unlikely
to be stable in this position) and 0.357 mm.]

MEASUREMENT OF PARTICLE SIZE

By convention, particles are expressed in different units depending on the size


range involved. Coarse particles are measured in inches or millimetres; fine
particles in terms of screen size; very fine particles in micrometres or
nanometres. Ultrafine particles are sometimes described in terms of their
surface area per unit mass, usually in square metres per gram.

Measurement of particle size and of particle size distribution is a highly


specialised topic, and considerable skill is needed in the making of accurate
measurements and in their interpretation.

Before a size analysis can be carried out, it is necessary to collect a


representative sample of the solids, and then to reduce this to the quantity which
is required for the chosen method of analysis. Samples will generally need to be
taken from the bulk of the powder

A wide range of measuring techniques is available both for single particles and for
systems of particles. In practice, each method is applicable to a finite range of
sizes and gives a particular equivalent size, dependent on the nature of the
method. The common methods used for determining the size of a particle are:
sieving, microscopy, sedimentation, permeametry, electrozone sensing and laser
diffraction
SIEVING

Dry sieving using woven wire sieves is a simple, cheap method of size analysis
suitable for particle sizes greater than 45 µm. Sieving gives a mass distribution
and a size known as the sieve diameter. Since the length of the particle does not
hinder its passage through the sieve apertures (unless the particle is extremely
elongated), the sieve diameter is dependent on the maximum width and maximum
thickness of the particle. The most common modern sieves are in sizes such that
the ratio of adjacent sieve sizes is the fourth root of two (eg. 45, 53, 63, 75, 90,
107 µm). If standard procedures are followed and care is taken, sieving gives
reliable and reproducible size analysis. Air jet sieving, in which the powder on the
sieve is fluidized by a jet or air, can achieve analysis down to 20 µm. Analysis down
to 5 µm can be achieved by wet sieving, in which the powder sample is suspended
in a liquid.

MICROSCOPY

The optical microscope may be used to measure particle sizes down to 5 µm. For
particles smaller than this diffraction causes the edges of the particle to be
blurred and this gives rise to an apparent size. The electron microscope may be
used for size analysis below 5 µm. Coupled with an image analysis system the
optical microscope or electron microscope can readily give number distributions
of size and shape. Such systems calculate various diameters from the projected
image of the particles (e.g. Martin’s, Feret’s, shear, projected area diameters,
etc.). Note that for irregular-shaped particles, the projected area offered to the
viewer can vary significantly depending on the orientation of the particle.
Techniques such as applying adhesive to the microscope slide may be used to
ensure that the particles are randomly orientated.

SEDIMENTATION
In this method, the rate of sedimentation of a sample of particles in a liquid is
followed. The suspension is dilute and so the particles are assumed to fall at their
single particle terminal velocity in the liquid (usually water). Stokes’ law is assumed
to apply (Rep < 0:3) and so the method using water is suitable only for particles
typically less than 50 μm in diameter. The rate of sedimentation of the particles
is followed by plotting the suspension density at a certain vertical position against
time. The suspension density is directly related to the cumulative undersize, and
the time is related to the particle diameter via the terminal velocity.

PERMEAMETRY

This is a method of size analysis based on fluid flow through a packed bed. The
Carman–Kozeny equation for laminar flow through a randomly packed bed of
uniformly sized spheres of diameter x is:

(1)

where -ΔÞ is the pressure drop across the bed, ε is the packed bed void fraction,
H is the depth of the bed, µ is the fluid viscosity and U is the superficial fluid
velocity.

In this method, the pressure gradient across a packed bed of known voidage is
measured as a function of flow rate. The diameter we calculate from the Carman–
Kozeny equation is the arithmetic mean of the surface distribution

ELECTROZONE SENSING

Particles are held in suspension in a dilute electrolyte which is drawn through a


tiny orifice with a voltage applied across it. As particles flow through the orifice
a voltage pulse is recorded.

The amplitude of the pulse can be related to the volume of the particle passing
the orifice. Thus, by electronically counting and classifying the pulses according
to amplitude this technique can give a number distribution of the equivalent volume
sphere diameter. The lower size limit is dictated by the smallest practical orifice
and the upper limit is governed by the need to maintain particles in suspension.
Although liquids more viscous than water may be used to reduce sedimentation,
the practical range of size for this method is 0.3–1000 µm. Errors are introduced
if more than one particle passes through the orifice at a time and so dilute
suspensions are used to reduce the likelihood of this error.

LASER DIFFRACTION
This method relies on the fact that for light passing through a suspension, the
diffraction angle is inversely proportional to the particle size. An instrument
would consist of a laser as a source of coherent light of known fixed wavelength
(typically 0:63 mm), a suitable detector (usually a slice of photosensitive silicon)
with a number of discrete detectors, and some means of passing the sample of
particles through the laser light beam (techniques are available for suspending
particles in both liquids and gases are drawing them through the beam).

To relate diffraction angle with particle size, early instruments used the

Fraunhofer theory, which can give rise to large errors under some circumstances
(e.g. when the refractive indices of the particle material and suspending medium
approach each other). Modern instruments use the Mie theory for interaction of
light with matter. This allows particle sizing in the range 0.1–2000 µm, provided
that the refractive indices of the particle material and suspending medium are
known.

This method gives a volume distribution and measures a diameter known as the
laser diameter. Particle size analysis by laser diffraction is very common in
industry today. The associated software permits display of a variety of size
distributions and means derived from the original measured distribution.

MIXED PARTICLE SIZES AND SIZE ANALYSIS


In a sample of uniform particles of diameter Dp, the total volume of the particles
is m/ρp, where m and ρp are the total mass of the sample and the density of the
particles, respectively. Since the volume of one particle is vp, the number of
particles in the sample N is:
The total surface area, A will be the product of the surface area of one particle
and the number of particles:

(3)

To apply Eqs (2) and (3) to mixtures of particles having various sizes and densities,
the mixture is sorted into fractions, each of constant density and approximately
constant size. Each fraction can then be weighed, or the individual particles in it
can be counted or measured by any one of a number of methods. Equations (2) and
(3) can then be applied to each fraction and the results added.

Information from such a particle size analysis is tabulated to show the mass or
number fraction in each size increment as a function of the average particle size
(or size range) in the increment. An analysis tabulation in this way is called a
differential analysis. The results are often presented as a histogram , as shown
in Figure 1a, with a continuous curve like the dashed line used to approximate the
distribution. A second way to present the information is through a cumulative
analysis obtained by adding, consecutively, the individual increments, starting with
that containing the smallest particles, and tabulating or plotting the cumulative
sums against the maximum particle diameter in the increment. Figure 1b is a
cumulative analysis plot of the distribution shown in Figure 1a. In a cumulative
analysis, the data may appropriately be represented by a continuous curve.

Calculations of average particle size, particle surface area, or particle population


of a mixture may be based on either a differential or a cumulative analysis.
Figure 1: Particle-size distribution for powder:
(a)differential analysis (b)cumulative analysis

Specific Surface of Mixture : if the particle density ρp and sphericity φ are


known, the surface area of the particles in each fraction may be calculated from
Equation (3) and the results for all fraction added to give Aw, the specific surface
(the total surface area of a unit mass of particles). If and ρp and φ are constant,
Aw is given by:

OR

(4)

where subscripts = individual


increments xi = mass fraction in a
given increment n = number of
increments

=average particle diameter, taken as arithmentic average of smallest and


largest diameters in increment.

Average Particle Size: Average particle size for a mixture of particles is defined
in several different ways. Probably the most used is the volume surface mean
diameter, Ds. It is defined by the equation:

(5)
Substituting Eq.(4) in Eq.(5) gives:

(6)

If the number of particles in each fraction Ni is known instead of the mass


fraction is given by :

(7)

Other averages are sometimes useful. The arithmetic mean diameter is

(8)

where NT is the number of particles in the entire sample.

The mass mean diameter is found from the equation :

(9)

Dividing the total volume of the sample by the number of particles in the mixture
, gives the average volume of a particle. The diameter of such a particle is the
volume mean diameter , which is found from the relation:

(10)

Number of Particles in Mixture : To calculate from the differential analysis,


the number of particles in a mixture Eq. (2) is used to compute the number of
particles in each fraction, and Nw, the total population in one mass unit of
samples, is obtained by summation over all the fractions. For a given particle
shape, the volume of any particle is proportional to its “diameter” cubed or

(11)

where a is the volume shape factor. From Eq. (2), then assuming that a is
independent of size:

(12)
The specific surface area, the various average diameters, and the number of
particles are readily calculated from the particle analyses through the use of
simple computer programs.

Screen Analysis: Standard Screen Series

Standard screens are used to measure the size (and size distribution) of particles
in the size range between about 3 and 0.0015 in. (76 mm and 38 μm). Testing sieves
are made of woven wire screens, the mesh and dimensions of which are carefully
standardized. The openings are square. Each screen is identified in meshes per
inch. The actual openings are smaller than those corresponding to the mesh
numbers, however, because of the thickness of the wires. Considering the Tyler
standard screen series., the area of the openings in any one screen in the series
is exactly twice that of the opening in the next smaller screen. The ratio of the
actual mesh dimension of any screen to that of the next smaller screen is 1.41 (
).

In making an analysis a set of standard screens is arranged serially in stack, with


the smallest mesh at the bottom and the the largest at the top. The sample sample
is placed on the top screen and the stack shaken mechanically for a definite time.
The particles retained on each screen are removed and weighed, and the masses
of the individual screen increments are converted to mass fractions or mass
percentages of the total sample. Any particles that pass the finest screen are
caught in a pan at the bottom of the stack.
Example

The screen analysis shown in the table below applies to a sample of crushed quartz.

Mesh Screen Mass of


opening particles
Dpi, mm retained, g
4 4.699 0

6 3.327 10.04

8 2.362 50.00

10 1.651 128.28

14 1.168 102.80

20 0.833 63.60

28 0.589 21.52

35 0.417 8.40

48 0.295 4.08

65 0.208 3.08

100 0.147 2.32

150 0.104 1.64

200 0.074 1.24

Pan ---- 3.00

The density of the particles is 2650 kg/m3 (0.00265 g/mm3), and the shape
factors are a = 2 and φ= 0.571. For the material between 4-mesh and 200-mesh in
particle size, calculate:
a) Aw in square millimetres per gram and Nw in particles per gram
b) Dv ;

c) ;
d) Ni for the 150/200-mesh increment
f) what fraction of the total number of particles is in the 150/200-mesh
increment?

Solution

Note : we need to first determine the mass fraction of particle, xi retained on


each screen. The total mass of particles is the sum of mass of particles on all
screens and on the pan.

Therefore, the total mass of particles = 400 g

COL. A COL.. B COL.. C COL.. D COL. E COL. F COL. G COL. H COL. I

Average
Screen Mass Cumulative particle
Mass
openin fraction fraction diameter
Mesh Retained smaller than xi/Dpi xi/D3pi xi*Dpi
g, Dpi, retained, in
,g
mm xi Dpi increment
, Dpi, mm
4 4.699 0 0.0000 1

6 3.327 10.04 0.0251 0.9749 4.013 0.0062547 0.00039 0.1007263


8 2.362 50.00 0.1250 0.8499 2.8445 0.0439445 0.0054 0.3555625
10 1.651 128.28 0.3207 0.5292 2.0065 0.1598306 0.0397 0.64348455
14 1.168 102.80 0.2570 0.2722 1.4095 0.1823342 0.0918 0.3622415
20 0.833 63.60 0.1590 0.1132 1.0005 0.1589205 0.1588 0.1590795
28 0.589 21.52 0.0538 0.0594 0.711 0.0756681 0.1497 0.0382518
35 0.417 8.40 0.0210 0.0384 0.503 0.0417495 0.1650 0.010563
48 0.295 4.08 0.0102 0.0282 0.356 0.0286517 0.2261 0.0036312
65 0.208 3.08 0.0077 0.0205 0.2515 0.0306163 0.4840 0.00193655
100 0.147 2.32 0.0058 0.0147 0.1775 0.0326761 1.0371 0.0010295
150 0.104 1.64 0.0041 0.0106 0.1255 0.0326693 2.0742 0.00051455
200 0.074 1.24 0.0031 0.0075 0.089 0.0348315 4.3974 0.0002759
Pan ---- 3.00 0.0075 0

0.828 8.830 1.677


Sum

To find Aw and Nw , recall that:

a) For the 4/6-mesh increment, is the arithmetic means of the mesh openings
of the definite screens, or, from the above table , (4.699+3.327)/2 = 4.013 mm
For this increment, xi = 0.0251; hence xi/Dpi = 0.0251/4.013 = 0.0063 and xi/D3pi
=

0.0004. Corresponding quantities are calculated for the other increments and

summed to give = 0.828 and (as shown in table). Since the

pan fraction is excluded, the specific surface area and number of particles per
unit mass of particles 200-mesh or larger can be found by dividing the results
from Eqs. (4) and (12) by 1-xi. or 1-0.0075= 0.9925 (since xi for pan is 0.0075).
Then:

b) From Eq. (10)


c) The volume-surface mean diameter is found from Eq. (6)

d) Mass mean diameter is obtained from Eq. (9). For this from the data in the
Table,

e) The number of particles in the 150/200-mesh increment is found from Eq. (12).

This is 836/1679 = 0.498 or 49.8 % of the particles in the top 12 increments.

Note 1679 represents the total number of particles in one mass unit ( refer to

a) PRACTICE PROBLEM

Table A. Screen Analysis result for a sample of Crushed rock

Mesh size Mass retained Mass fraction % cumulative


on each retained on Mass fraction
screen, g each screen, x (less than)

8 2.52 0

9 2.10 5

10 1.75 9

12 1.46 12

14 1.22 12

16 1.02 13

20 0.85 13
24 0.71 12

28 0.59 8

32 0.49 6

35 0.41 3

42 0.34 3

Pan 4

a). For Table A above fill in values for the mass fraction and cumulative mass

fractions retained on each screen in the fourth and fifth columns.

b) For the screen analysis result shown in Table A above for a sample of

crushed rock, the density of the particles is 1,260 kg/m3 and the shape

factors are a=2 and s =0.54. Calculate Aw and Nw

c) Represent the particle size distributions for the crushed rock using the:

i.Differential method of analysis

ii. Cumulative method of analysis

SAMPLING

In practice, the size distribution of many tonnes of powder are often assumed
from an analysis performed on just a few grams or milligrams of sample. The
importance of that sample being representative of the bulk powder cannot be
overstated. However, on mixing and segregation, most powder handling and
processing operations (pouring, belt conveying, handling in bags or drums, motion
of the sample bottle, etc.) cause particles to segregate according to size and to a
lesser extent density and shape. This natural tendency to segregation means that
extreme care must be taken in sampling.

There are two golden rules of sampling:

1. The powder should be in motion when sampled.


2. The whole of the moving stream should be taken for many short time
increments.

Since the eventual sample size used in the analysis may be very small, it is often
necessary to split the original sample in order to achieve the desired amount for
analysis. These sampling rules must be applied at every step of sampling and sample
splitting.

Example

The screen analysis shown in the table below applies to a sample of crushed quartz.

Mesh Screen opening Mass of particles


Dpi, mm retained, g
4 4.699 0
6 3.327 10.04
8 2.362 50.00
10 1.651 128.28
14 1.168 102.80
20 0.833 63.60
28 0.589 21.52
35 0.417 8.40
48 0.295 4.08
65 0.208 3.08
100 0.147 2.32
150 0.104 1.64
200 0.074 1.24
Pan ---- 3.00

The density of the particles is 2650 kg/m3 (0.00265 g/mm3), and the shape
factors are a = 2 and φ= 0.571. For the material between 4-mesh and 200-mesh in
particle size, calculate:

a) Aw in square millimetres per gram and Nw in particles per gram


b) ;
c) The volume-surface mean diameter, ;
d) Ni for the 150/200-mesh increment
f) what fraction of the total number of particles is in the 150/200-mesh
increment?

Solution

Note : we need to first determine the mass fraction of particle, xi retained on


each screen. The total mass of particles is the sum of mass of particles on all
screens and on the pan.
Therefore, the total mass of particles = 400 g

COL. A COL.. B COL.. C COL.. D COL. E COL. F COL. G COL. H COL. I

Average
Screen Mass Cumulative particle
Mass
openin fraction fraction diameter
Mesh Retained smaller than xi/Dpi xi/D3pi xi*Dpi
g, Dpi, retained, in
,g
mm xi Dpi increment
, Dpi, mm
4 4.699 0 0.0000 1

6 3.327 10.04 0.0251 0.9749 4.013 0.0062547 0.00039 0.1007263


8 2.362 50.00 0.1250 0.8499 2.8445 0.0439445 0.0054 0.3555625
10 1.651 128.28 0.3207 0.5292 2.0065 0.1598306 0.0397 0.64348455
14 1.168 102.80 0.2570 0.2722 1.4095 0.1823342 0.0918 0.3622415
20 0.833 63.60 0.1590 0.1132 1.0005 0.1589205 0.1588 0.1590795
28 0.589 21.52 0.0538 0.0594 0.711 0.0756681 0.1497 0.0382518
35 0.417 8.40 0.0210 0.0384 0.503 0.0417495 0.1650 0.010563
48 0.295 4.08 0.0102 0.0282 0.356 0.0286517 0.2261 0.0036312
65 0.208 3.08 0.0077 0.0205 0.2515 0.0306163 0.4840 0.00193655
100 0.147 2.32 0.0058 0.0147 0.1775 0.0326761 1.0371 0.0010295
150 0.104 1.64 0.0041 0.0106 0.1255 0.0326693 2.0742 0.00051455
200 0.074 1.24 0.0031 0.0075 0.089 0.0348315 4.3974 0.0002759
Pan ---- 3.00 0.0075 0

Sum 0.828 8.830 1.677

To find Aw and Nw , recall that:

a) For the 4/6-mesh increment, is the arithmetic means of the mesh openings
of the definite screens, or, from the above table , (4.699+3.327)/2 = 4.013 mm
For this increment, xi = 0.0251; hence xi/Dpi = 0.0251/4.013 = 0.0063 and xi/D3pi
=

0.0004. Corresponding quantities are calculated for the other increments and

summed to give = 0.828 and (as shown in table). Since the

pan fraction is excluded, the specific surface area and number of particles per
unit mass of particles 200-mesh or larger can be found by dividing the results
from Eqs. (4) and (12) by 1-xi. or 1-0.0075= 0.9925 (since xi for pan is 0.0075).
Then:
b) From Eq. (10)

c) The volume-surface mean diameter is found from Eq. (6)

d) Mass mean diameter is obtained from Eq. (9). For this from the data in the
Table,

e) The number of particles in the 150/200-mesh increment is found from Eq. (12).

This is 836/1679 = 0.498 or 49.8 % of the particles in the top 12 increments.

Note 1679 represents the total number of particles in one mass unit ( refer to a)
PRACTICE PROBLEM

Table below shows a screen analysis result for a sample of Crushed rock.

Mesh Size Mass retained


on each
screen, g
8 2.52 0
9 2.1 5
10 1.75 9
12 1.46 12
14 1.22 12
16 1.02 13
20 0.85 13
24 0.71 12
28 0.59 8
32 0.49 6
35 0.41 3
42 0.34 3
Pan 4
The density of the particles is 1260 kg/m3 , and the shape factors are a = 2 and
φ= 0.54. For the material between 4-mesh and 42-mesh in particle size. calculate:

a) Calculate the: i. Specific surface, Aw in mm2/g ii. total population in onemass


unit of sample, Nw in particles per gram
b) Represent the particle size distributions for the crushed rock using the:

i.Differential method of analysis ii. Cumulative method of analysis

Solution

Mesh size Mass Mass %


Average
retained fraction cumulative particle
on each retained Mass diameter
screen, g on each fraction xi/Dpi xi/D3pi xi*Dpi
in
screen, x (less than)
increment,
Dpi, mm

8 2.52 0 0 100
9 2.1 5 0.05 95 2.31 0.0216 0.00406 0.1155
10 1.75 9 0.09 86 1.925 0.0468 0.01262 0.17325
12 1.46 12 0.12 74 1.605 0.0748 0.02902 0.1926
14 1.22 12 0.12 62 1.34 0.0896 0.04987 0.1608
16 1.02 13 0.13 49 1.12 0.1161 0.09253 0.1456
20 0.85 13 0.13 36 0.935 0.1390 0.15904 0.12155
24 0.71 12 0.12 24 0.78 0.1538 0.25287 0.0936
28 0.59 8 0.08 16 0.65 0.1231 0.29131 0.052
32 0.49 6 0.06 10 0.54 0.1111 0.38104 0.0324
35 0.41 3 0.03 7 0.45 0.0667 0.32922 0.0135
42 0.34 3 0.03 4 0.375 0.0800 0.56889 0.01125
Pan 4 0.04 0
Sum
sum 100 1 1.0225 2.1705 1.11205

a) Since the pan fraction is excluded, the specific surface area and number of
particles per unit mass of particles 42-mesh or larger can be found by dividing
the results from Eqs. (4) and (12) by 1-xi. or 1-0.04= 0.96 (since xi for pan is 0.04).

Then:

b)
120

100

80

60

40

20

0
0 0.5 1 1.5 2 2.5 3
Particle size, mm

SAMPLING

In practice, the size distribution of many tonnes of powder are often assumed
from an analysis performed on just a few grams or milligrams of sample. The
importance of that sample being representative of the bulk powder cannot be
overstated. However, on mixing and segregation, most powder handling and
processing operations (pouring, belt conveying, handling in bags or drums, motion
of the sample bottle, etc.) cause particles to segregate according to size and to a
lesser extent density and shape. This natural tendency to segregation means that
extreme care must be taken in sampling.

There are two golden rules of sampling:

1. The powder should be in motion when sampled.


2. The whole of the moving stream should be taken for many short time
increments.

Since the eventual sample size used in the analysis may be very small, it is often
necessary to split the original sample in order to achieve the desired amount for
analysis. These sampling rules must be applied at every step of sampling and sample
splitting.

MOTION OF PARTICLES IN A FLUID

All bodies immersed in a fluid are subject to a buoyancy force. In a very slow
steady relative motion (creeping motion) of a flowing fluid, there is an additional
force which is made up of two components: the skin friction (or viscous drag) and
the form drag (due to the pressure distribution).

The drag force resisting very slow steady relative motion (creeping motion)
between a rigid sphere of diameter d and a fluid of infinite extent, of viscosity
µ is composed of two components:

(17)

(18)
(19)

where U is the relative velocity. This [Eq. 19 ] is known as Stokes’ law.


DRAG COEFFICIENTS ON A SPHERICAL PARTICLE

The most satisfactory way of representing the relation between drag force and
velocity involves the use of two dimensionless groups:

(20)
I
R is the force per unit projected area of the particle in a plane perpendicular to
the direction of motion. For a sphere, the projected area is that of a circle of the
same diameter as the sphere.

(21a)

(21b)

RI/ fU2 is a form of drag coefficient, often denoted by the symbol C’D. Frequently,
a drag coefficient CD is defined as the ratio of RI to ½ U2

(22)
It is seen that CID is analogous to the friction factor φ(= R/ U2) for pipe flow, and
CD is analogous to the Fanning friction factor f .

(23)
At higher relative velocities, the inertia of the fluid begins to dominate (the fluid
must accelerate out of the way of the particle). Analytical solution of the Navier–
Stokes equations is not possible under these conditions. However, experiments
give the relationship between the drag coefficient and the particle Reynolds
number in the form of the so-called standard drag curve (Figure 5). Four regions
are identified: the Stokes’ law region; the Newton’s law region in which drag
coefficient is independent of Reynolds number; an intermediate region between
the Stokes and Newton regions; and the boundary layer separation region. The
Reynolds number ranges and drag coefficient correlations for these regions are
given in Table 3.

Table 3: Reynolds number ranges for single particle drag coefficient correlations

Figure 5: Standard drag curve for motion of asphere in a fluid

PARTICLES FALLING UNDER GRAVITY THROUGH A FLUID

The relative motion under gravity of particles in a fluid is of particular interest.


In general, the forces of buoyancy, drag and gravity act on the particle: gravity -
buoyancy - drag = acceleration force (24)

A particle falling from rest in a fluid will initially experience a high acceleration
as the shear stress drag, which increases with relative velocity, will be small. As
the particle accelerates the drag force increases, causing the acceleration to
reduce. Eventually a force balance is achieved when the acceleration is zero and a
maximum or terminal relative velocity is reached. This is known as the single
particle terminal velocity.
For a spherical particle, Equation (24) becomes:

(25)

Combining Equation (25) with Equation (22):

(26)

where UT is the single particle terminal velocity. Equation (26) gives the following
expression for the drag coefficient under terminal velocity conditions:

(27)
Thus in the Stokes’ law region, with CD = 24/Rep; the single particle terminal
velocity is given by:

(28)
Note that in the Stokes’ law region the terminal velocity is proportional to the
square of the particle diameter.
In the Newton’s law region, with CD = 0.44, the terminal velocity is given by:

(29)

Note that in this region the terminal velocity is independent of the fluid viscosity
and proportional to the square root of the particle diameter. In the intermediate
region no explicit expression for UT can be found.

Generally, when calculating the terminal velocity for a given particle or the particle
diameter for a given velocity, it is not known which region of operation is relevant.
One way around this is to formulate the dimensionless groups, CDRep2 and CD/Rep
:

• To calculate UT, for a given size d. Calculate the group:

(30)
which is independent of UT

(Note that CDRep2= 4Ar/3, where Ar is the Archimedes number.) For given particle
and fluid properties, CDRep2 is a constant and will therefore produce a straight
line of slope -2 if plotted on the logarithmic coordinates (log CD versus log Rep) of
the standard drag curve. The intersection of this straight line with the drag curve
gives the value of Rep and hence UT

• To calculate size d, for a given UT. Calculate the group

(31)

which is independent of particle size d.

For a given terminal velocity, particle density and fluid properties, CD/Rep is
constant and will produce a straight line of slope +1 if plotted on the logarithmic
coordinates (log CD versus log Rep) of the standard drag curve. The intersection
of this straight line with the drag curve gives the value of Rep and hence, x (Figure
6). An alternative to this graphical method, but based on the same approach, is to
use tables of corresponding values of Rep; CD; CDRep2, and CD/Rep.

Figure 6: Method for estimating terminal velocity for a given size of particle and
vice versa
NON-SPHERICAL PARTICLES

The effect of shape of non-spherical particles on their drag coefficient has


proved difficult to define. This is probably due to the difficulty in describing
particle shape for irregular particles. Engineers and scientist often require a
single number to describe the shape of a particle. One simple approach is to
describe the shape of a particle in terms of its sphericity, the ratio of the
surface area of a sphere of volume equal to that of the particle to the
surface area of the particle. For example, a cube of side one unit has a volume
of 1 (cubic units) and a surface area of 6 (square units). A sphere of the same
volume has a diameter, xv of 1.24 units. The surface area of a sphere of diameter
1.24 units is

4.836 units. The sphericity of a cube is therefore 0.806 (= 4.836/6).

For non-spherical particles the particle Reynolds number is based on the


equalvolume sphere diameter, i.e. the diameter of the sphere having the same
volume as that of the particle. Figure 7 shows drag curves for particles of
different sphericities. This covers regular and irregular particles. The plot should
be used with caution, since sphericity on its own may not be sufficient in some
cases to describe the shape for all types of particles.
Figure 7: Drag coefficient CD versus Reynolds number Rep for particles of
sphericity φ ranging from 0.125 to 1.0. (Note Rep and CD are based on the
equivalent volume diameter)

EFFECT OF BOUNDARIES ON TERMINAL VELOCITY

When a particle is falling through a fluid in the presence of a solid boundary the
terminal velocity reached by the particle is less than that for an infinite fluid. In
practice, this is really only relevant to the falling sphere method of measuring
liquid viscosity, which is restricted to the Stokes’ region. In the case of a particle
falling along the axis of a vertical pipe this is described by a wall factor, f w, the
ratio of the velocity in the pipe, UD to the velocity in an infinite fluid, U∞. The
correlation of Francis for fw is given in Equation (32).

(32)

where d and D are the diameters of the particle and the tube respectively.
WORKED EXAMPLE 1
A sphere of diameter 12 mm and density 8000 kg/m3 falls under gravity at
terminal conditions through a liquid of density 980 kg/m3 in a tube of diameter 14

mm. The measured terminal velocity of the particle is 1.4 mm/s. Calculate the
viscosity of the fluid. Verify that Stokes’ law applies.

Solution

To solve this problem, we first convert the measured terminal velocity to the
equivalent velocity which would be achieved by the sphere in a fluid of infinite
extent. Assuming Stokes’ law we can determine the fluid viscosity. Finally we
check the validity of Stokes’ law.

Using the Francis wall factor expression [Eq 32]

Thus, terminal velocity for the particle in a fluid of infinite extent,

Equating this value to the expression for ∞ in the Stokes’ regime

Hence, fluid viscosity, µ = 4.92 Pa s.

Checking the validity of Stokes’ law:

Rep is less than 0.3 and so the assumption that Stokes’ law holds is valid.
WORKED EXAMPLE 2
A particle of equivalent volume diameter 0.6 mm, density 2200 kg/m3 and
sphericity 0.22 falls freely under gravity in a fluid of density 740 kg/m3 and
viscosity 2*10-4 Pa s. Estimate the terminal velocity reached by the particle.

Solution

In this case we know the particle size and are required to determine its terminal
velocity without knowing which regime is appropriate. The first step is, therefore,
to calculate the dimensionless group CDRep2

This is the relationship between drag coefficient CD and single particle Reynolds
number Rep for particles of size 0.6 mm and density 2200 kg/m3 falling in a fluid
of density 740 kg/m3 and viscosity 2 * 10-4 Pa s. Since CDRep2 is a constant, this
relationship will give a straight line of slope -2 when plotted on the log–log
coordinates of the standard drag curve. For plotting the relationship:

Rep CD
10 763.1
100 7.63

These values are plotted on the standard drag curves for particles of different
sphericity. The values of Rep and CD plotted in Drag coefficient CD versus
Reynolds number Rep graph
Where the plotted line intersects the standard drag curve for a sphericity of
0.22 , Rep =60

The terminal velocity UT may be calculated from


Hence, terminal velocity, UT = 0.027m/s.

Example 3

A sphere 1.5 mm diameter falls in water. The density of the sphere is 2500
kg/m3. The density and dynamic viscosity of water are 997 kg/m3 and 0.89* 10-3

N.s/m2 respectively. The drag coefficient is given by the formula


.Determine the terminal velocity.
Solution

Next, complete a table using the formula:

Re 0.1 1 10 100 1000


CD 247 27.6 4.15 1.09 0.438288
CDRe2 2.47 27.6 415 10900 438288

We are looking for a value of CDRe2 = 83513 and it is apparent that this occurs
when Re is between 100 and 1000. We narrow down our search to, between 100
and 1000, by trial and error we find that the correct value of Re is 362.5
Re 100 200 300 400
CD 1.09 0.8056 0.6839 0.6119

CDRe2 10900 32224 61551 97904

Re 300 320 340 360


CD 0.6839 0.6668 0.6513 0.6371

CDRe2 61551 68280 75290.3 82568.2


Re 362 362.2 362.4 362.6
CD 0.6357 0.6356 0.6354 0.6353

CDRe2 83304.7 83384 83449.5 83528.5

U = 0.215 ms-1 and this is the terminal velocity.

Alternative Method

By trial and error, we have that Re = 362.56

Worked Example 4

What is the terminal velocity of a spherical steel particle, 0.40 mm in diameter,


settling in an oil of density 820 kg/m3 and viscosity 10 mN s/m2? The density of
steel is 7870 kg/m3. [ Take g = 9.81 m/s2]

Solution

d = 0.4 mm = 0.0004 m

Rep CD
1 48.39
10 0.48
These values are plotted on the standard drag curves for particles of different
sphericity. The values of Rep and CD plotted in Drag coefficient CD versus
Reynolds number Rep graph
Where the plotted line intersects the standard drag curve for a sphere

(sphericity =1) , Rep = 1.5


The terminal velocity UT may be calculated from

Hence, terminal velocity, UT = 0.045 m/s.

Worked Example 5

Solve example 4 for a particle with equivalent sphere diameter of 0.40 mm and
sphericity of 0.25 [ Ans: UT = 0.012 m/s]

PRESSURE DROP–FLOW RELATIONSHIP

1. Laminar Flow

In the nineteenth century Darcy (1856) observed that the flow of water through a
packed bed of sand was governed by the relationship:

(33)

where U is the superficial fluid velocity through the bed and (-△p) is the frictional
pressure drop across a bed depth H. (Superficial velocity = fluid volumetric flow
rate/cross-sectional area of bed, Q/A).

The flow of a fluid through a packed bed of solid particles may be analysed in terms
of the fluid flow through tubes. The starting point is the Hagen–Poiseuille equation
for laminar flow through a tube:

(34)
where D is the tube diameter and μ is the fluid viscosity.

Consider the packed bed to be equivalent to many tubes of equivalent diameter De


following tortuous paths of equivalent length He and carrying fluid with a velocity Ui.
Then, from the Hagen–Poiseuille Equation (Eq. 34).

(35)

Ui is the actual velocity of fluid through the interstices of the packed bed and is
related to superficial fluid velocity by:

(36)

where is the voidage or void fraction of the packed bed.

Although the paths of the tubes are tortuous, we can assume that their actual length
is proportional to the bed depth, that is,

(37)

The tube equivalent diameter is defined as:

(38)

where flow area=εA, where A is the cross-sectional area of the vessel holding the
bed; wetted perimeter is SBA, where SB is the particle surface area per unit volume
of the bed.

That this is so may be demonstrated by comparison with pipe flow: Total

particle surface area in the bed =SBAH. For a pipe,

Now if Sv is the surface area per unit volume of particles, then

(39)
(40)

Substituting Equations (36), (37) and (40) in (35):

(41)

where K3 = K1K2. Equation (41) is known as the Carman–Kozeny equation describing


laminar flow through randomly packed particles. The constant K3 depends on particle
shape and surface properties and has been found by experiment to have a value of
about 5. Taking K3 = 5, for laminar flow through a randomly packed bed of monosized
spheres of diameter x (for which S = 6/x) the Carman–Kozeny equation becomes:

(42)

Turbulent Flow

For turbulent flow through a randomly packed bed of monosized spheres of diameter
x the equivalent equation is:

(43)

General Equation for Turbulent and Laminar Flow

Based on extensive experimental data covering a wide range of size and shape of
particles, Ergun (1952) suggested the following general equation for any flow
conditions:

(44)

In terms of the Reynolds number defined in Equation (45),

Fully laminar flow exists when Reynolds number, Re* < 10

Fully turbulent flow exists when Reynolds number, Re* > 2000

(45)
In practice, the Ergun equation is often used to predict packed bed pressure
gradient over the entire range of flow conditions.

Ergun also expressed flow through a packed bed in terms of a friction factor defined
in Equation (46):

(46)

Relating Equation (44) to Equation (46) gives:

(47)

Non-spherical Particles

The Ergun and Carman–Kozeny equations also accommodate non-spherical particles if


x is replaced by xsv the diameter of a sphere having the same surface to volume ratio
as the non-spherical particles in question. Use of xsv gives the correct value of
specific surface S (surface area of particles per unit volume of particles).
Recalling Equation (41)

Thus, in general, the Ergun equation for flow through a randomly packed bed of
particles of surface-volume diameter xsv becomes:

(48)

and the Carman–Kozeny equation for laminar flow through a randomly packed bed of
particles of surface-volume diameter xsv becomes:

(49)

NOTE

If the particles in the bed are non-spherical not mono-sized, then the correct mean
size to use in these equations is the surface-volume mean, .

Example
A packed bed of solid particles of density 2,500 kg/m3 occupies a depth of 1 m in a
vessel of cross-sectional area 0.04 m2. The mass of solids in the bed is 50 kg and
the surface-volume mean diameter of the particle is 1 mm. A liquid of density 800
kg/m3 and viscosity 0.002 Pa.s flows upwards through the bed, which is restrained
at its upper surface. Calculate the:

a) voidage (volume fraction occupied by the voids) of the bed


b) pressure drop across the bed when the volume flow rate of liquid is 1.44 m3/h.

Solution

a) Note that mass of particles in bed, m = A*H(1-ε)ρp

b) With a liquid flow rate of 1.44 m3/h, the superficial liquid velocity
through the bed, U is given by:

We now use the Ergun equation to estimate the pressure drop across the bed at this
flow rate (we assume nonspherical and not monosized particles)

Note that: μ= 0.002 Pa.s, ρf = 800 kg/m3, xsv= 1 mm ( 0.001 m) and H = 1 m

Checking the Reynold’s number

Since the Reynold’s number is less than 10, we might estimate the pressure drop
using the Carman-Kozeny equation

PP
A packed bed of solid particles of density 2,500 kg/m3 occupies a depth of 2 m in a
vessel of cross-sectional area 0.04 m2. The mass of solids in the bed is 50 kg and
the surface-volume mean diameter of the particle is 1 mm. A liquid of density 800
kg/m3 and viscosity 0.002 Pa.s flows upwards through the bed, which is restrained
at its upper surface. Calculate the:

a) voidage (volume fraction occupied by the voids) of the bed


b) pressure drop across the bed when the volume flow rate of liquid is 1.44 m3/h.

Example 2

A gas absorption tower of diameter 2 m contains ceramic Raschig rings randomly


packed to a height of 5 m. Air containing a small proportion of sulphur dioxide passes
upwards through the absorption tower at a flow rate of 6 m3/s. The viscosity and
density of the gas may be taken as 1.8*10-5 Pa.s and 1.2 kg/m3 respectively. Details
of the packing are given below:

Ceramic Raschig rings


Surface area per unit volume of packed bed, SB = 190 m2/m3
Voidage of randomly packed bed = 0.71
a) Calculate the diameter, xsv, of a sphere with the same surface-volume ratio as
the Raschig rings
b) Calculate the frictional pressure drop across the packing in the tower
c) Discuss how this pressure drop will vary with flow rate of the gas within ±10
% of the quoted flow rate
d) Discuss how the pressure drop across the packing vary with gas pressure and
temperature.

Solution

Recall SB = S(1-ε), where S is surface area per unit volume of rings

If xsv is the diameter of a sphere with the same surface –volume ratio as the rings,
Hence, xsv = 9.16 mm

c)

with μ= 1.8*10-5 Pa.s, ρf = 1.2 kg/m3, xsv = 9.16*10-3 m , H =5 m

(-△p) =72.0+3388.4 = 3460.4 Pa

c) We note that the turbulent component makes up about 98% of the total. Hence,
within ±10% of the quoted flow rate the pressure drop across the bed will increase
with the square of the superficial velocity and hence with the square of the flow
rate:

d) Variation with gas pressure

Pressure increase affects only the gas density. And gas density is directly
proportional to absolute gas pressure (if we assume ideal gas behaviour). Since the
flow is predominantly turbulent, then:

Variation with gas temperature

Since the flow is predominantly turbulent, gas viscosity has almost no effect (see
Ergun equation). Therefore, variation in gas temperature will influence only the gas
density. Assuming ideal gas behaviour,
Hence as temperature increases, the pressure drop decreases
a
CLASSIFICATION OF SOLID PARTICLES

The problem of separating solid particles according to their physical properties is of great
importance with large-scale operations in the mining industry, where it is necessary to separate the
valuable constituents in a mineral from the adhering gangue, as it is called, which is usually of a
lower density. In this case, it is first necessary to crush the material so that each individual particle
contains only one constituent. There is a similar problem in coal washing plants in which dirt is
separated from the clean coal. The processing industries are more usually concerned with
separating a single material, such as the product from a size reduction plant, into a number of size
fractions, or in obtaining a uniform material for incorporation in a system in which a chemical
reaction takes place. As similar problems are involved in separating a mixture into its constituents
and into size fractions, the two processes are considered together. Separation depends on the
selection of a process in which the behaviour of the material is influenced to a very marked degree
by some physical property. Thus, if a material is to be separated into various size fractions, a
sieving method may be used because this process depends primarily on the size of the particles,
though other physical properties such as the shape of the particles and their tendency to
agglomerate may also be involved. In general, large particles are separated into size fractions by
means of screens, and small particles, which would clog the fine apertures of the screen or for
which it would be impracticable to make the openings sufficiently fine, are separated in a fluid.
Fluid separation is commonly used for separating a mixture of two materials though magnetic,
electrostatic and froth flotation methods are also used where appropriate.

PARTICLE SIZE REDUCTION

Materials are rarely found in the size range required, and it is often necessary either to decrease or
to increase the particle size. When, for example, the starting material is too coarse, and possibly in
the form of large rocks, and the final product needs to be a fine powder, the particle size will have
to be progressively reduced in stages. The most appropriate type of machine at each stage depends,
not only on the size of the feed and of the product, but also on such properties as compressive
strength, brittleness and stickiness. For example, the first stage in the process may require the use
of a large jaw crusher and the final stage a sand grinder, two machines of very different characters.
In the materials processing industry, size reduction or comminution is usually carried out in order
to increase the surface area because, in most reactions involving solid particles, the rate of reactions
is directly proportional to the area of contact with a second phase. Thus the rate of combustion of
solid particles is proportional to the area presented to the gas, though a number of secondary factors
may also be involved. For example, the free flow of gas may be impeded because of the higher
resistance to flow of a bed of small particles. In leaching, not only is the rate of extraction increased
by virtue of the increased area of contact between the solvent and the solid, but the distance the
solvent has to penetrate into the particles in order to gain access to the more remote pockets of
solute is also reduced. This factor is also important in the drying of porous solids, where reduction
in size causes both an increase in area and a reduction in the distance. the moisture must travel
within the particles in order to reach the surface. In this case, the capillary forces acting on the
moisture are also affected. There are a number of other reasons for carrying out size reduction. It
may, for example, be necessary to break a material into very small particles in order to separate
two constituents, especially where one is dispersed in small isolated pockets. In addition, the
properties of a material may be considerably influenced by the particle size and, for example, the
chemical reactivity of fine particles is greater than that of coarse particles, and the colour and
covering power of a pigment is considerably affected by the size of the particles. In addition, far
more intimate mixing of solids can be achieved if the particle size is small. The energy required to
effect size reduction is related to the internal structure of the material and the process consists of
two parts, first opening up any small fissures which are already present, and secondly forming new
surface. A material such as coal contains a number of small cracks and tends first to break along
these, and therefore the large pieces are broken up more readily than the small ones. Since a very
much greater increase in surface results from crushing a given quantity of fine as opposed to coarse
material, fine grinding requires very much more power.

Methods of operating crushers

There are two distinct methods of feeding material to a crusher. The first, known as free crushing,
involves feeding the material at a comparatively low rate so that the product can readily escape.
Its residence time in the machine is therefore short and the production of appreciable quantities of
undersize material is avoided. The second method is known as choke feeding. In this case, the
machine is kept full of material and discharge of the product is impeded so that the material
remains in the crusher for a longer period. This results in a higher degree of crushing, although the
capacity of the machine is reduced and energy consumption is high because of the cushioning
action produced by the accumulated product. This method is therefore used only when a
comparatively small amount of materials is to be crushed and when it is desired to complete the
whole of the size reduction in one operation. If the plant is operated, as in choke feeding, so that
the material is passed only once through the equipment, the process is known as open circuit
grinding. If, on the other hand, the product contains material which is insufficiently crushed, it
may be necessary to separate the product and return the oversize material for a second crushing.
This system which is generally to be preferred, is known as closed circuit grinding.

The equipment may also be classified, to some extent, according to the nature of the force which
is applied though, as a number of forces are generally involved, it is a less convenient basis.
Grinding may be carried out either wet or dry, although wet grinding is generally applicable only
with low speed mills. The advantages of wet grinding are:

(a) The power consumption is reduced by about 20–30 per cent.

(b) The capacity of the plant is increased.

(c) The removal of the product is facilitated and the amount of fines is reduced.

(d) Dust formation is eliminated.


(e) The solids are more easily handled.

The choice of a machine for a given crushing operation is influenced by the nature of the product
required and the quantity and size of material to be handled. The more important properties of the
feed apart from its size are as follows:

• Hardness-The hardness of the material affects the power consumption and the wear on the
machine. With hard and abrasive materials, it is necessary to use a low-speed machine and
to protect the bearings from the abrasive dusts that are produced. Pressure lubrication is
recommended. Materials are arranged in order of increasing hardness in the Mohr scale in
which the first four items rank as soft and the remainder as hard.
• Structure- Normal granular materials such as coal, ores and rocks can be effectively
crushed employing the normal forces of compression, impact, and so on. With fibrous
materials a tearing action is required.
• Moisture content-It is found that materials do not flow well if they contain between about
5 and 50 per cent of moisture. Under these conditions the material tends to cake together
in the form of balls. In general, grinding can be carried out satisfactorily outside these
limits.
• Crushing strength- The power required for crushing is almost directly proportional to the
crushing strength of the material.
• Friability. The friability of the material is its tendency to fracture during normal handling.
In general, a crystalline material will break along well-defined planes and the power
required for crushing will increase as the particle size is reduced.
• Stickiness. A sticky material will tend to clog the grinding equipment and it should
therefore be ground in a plant that can be cleaned easily.
• Soapiness. In general, this is a measure of the coefficient of friction of the surface of the
material. If the coefficient of friction is low, the crushing may be more difficult.
• Explosive materials must be ground wet or in the presence of an inert atmosphere.
Materials yielding dusts that are harmful to the health must be ground under conditions
where the dust is not allowed to escape.
SEDIMENTATION

A number of mechanical separations are influenced by the sedimentation of solid particles or liquid
drops through a fluid, impelled by the force of gravity or by centrifugal force. In some cases, the
aim of the sedimentation process is to remove particles from a stream in order to eliminate
contaminants from the fluid or to recover the particles, as in the elimination of dust and fumes
from air or flue gas or the removal of solids from liquid wastes. In other problems, particles are
deliberately suspended in fluids to obtain separations of the particles into fractions differing in size
or density. The fluid is then recovered, sometimes for reuse. from the fractionated particles.

The rate of sedimentation of a suspension of fine particles is difficult to predict because of the
large number of factors involved. The flocculation of a suspension is usually completed quite
rapidly so that it is not possible to detect an increase in the sedimentation rate in the early stages
after the formation of the suspension. Most fine suspensions flocculate readily in tap water and it
is generally necessary to add a deflocculating agent to maintain the particles individually
dispersed. A further factor influencing the sedimentation rate is the degree of agitation of the
suspension. Gentle stirring may produce accelerated settling if the suspension behaves as a non-
Newtonian fluid in which the apparent viscosity is a function of the rate of shear. A number of
empirical equations have been obtained for the rate of sedimentation of suspensions, as a result of
tests carried out in vertical tubes. For a given solid and liquid, the main factors which affect the
process are the height of the suspension, the diameter of the containing vessel, and the volumetric
concentration

Flocculation

The tendency of the particulate phase of colloidal dispersions to aggregate is an important physical
property which finds practical application in solid–liquid separation processes, such as
sedimentation and filtration. The aggregation of colloids is known as coagulation, or flocculation.
Particles dispersed in liquid media collide due to their relative motion; and the stability (that is
stability against aggregation) of the dispersion is determined by the interaction between particles
during these collisions. Attractive and repulsive forces can be operative between the particles;
these forces may react in different ways depending on environmental conditions, such as salt
concentration and pH. The commonly occurring forces between colloidal particles are van der
Waals forces, electrostatic forces and forces due to adsorbed macromolecules. In the absence of
macromolecules, aggregation is largely due to van der Waals attractive forces, whereas stability is
due to repulsive interaction between similarly charged electrical double-layer. In a flocculated, or
coagulated suspension the aggregates of fine particles or flocs are the basic structural units and in
a low shear rate process, such as gravity sedimentation, their settling rates and sediment volumes
depend largely on volumetric concentration of floc and on interparticle forces.

Filtration

Filtration is the removal of solid particles from a fluid by passing the fluid through a filtering
medium on which the solids are deposited. The fluid may be a liquid or gas; the valuable stream
from the filter may be the fluid, or the solids or both. Sometimes it is neither, as when waste solids
must be separated from waste liquids prior to disposal. Usually, the feed is modified in some way
by pretreatment in order to increase the rate of filtration. This can be done by heating,
recrystallizing or adding ‘filter aid’ such as cellulose. As a result of the fact that there exists a
variety of materials to be filtered, there are many types of filters available.

Areas of application of the filtration process include;

• Water purification
• Ore handling in the mining industry
• Coatings and paint manufacturing
• Chemical process, etc
In most industrial applications, it is the solids that are required during filtration and their physical
size and properties are of paramount importance. Therefore, the main factors to be considered
when selecting equipments and operating conditions for such facilities are:

• The properties of the fluid, particularly its viscosity, density and corrosive properties
• The nature of the solid-its particle size, shape size distribution and packing characteristics
• The concentration of solids in suspension
• The quantity of material to be handled and its value
• Whether the feed liquor requires heating
• Whether it is necessary to wash filtered solids
Filtration occurs by virtue of a pressure differential across the filtering medium. Filters are
classified into those that operate with a pressure above atmospheric pressure on the upstream side
of the filter medium and those that operate with atmospheric pressure on the upstream side and a
vacuum on the downstream side. Most industrial filters are either pressure filters, vacuum filters
or centrifugal separators. They are also either continuous or discontinuous, depending on whether
the discharge of filtered solids is steady or intermittent. During much of the operating cycle of a
discontinuous filter, the flow of fluid through the device is continuous, but must be interrupted
intermittently to allow for discharge of the accumulated solids. In a continuous filter on the other
hand, the discharge of both solids and fluid is uninterrupted as long as the equipment is in
operation.

Filters are divided into three main groups and they are cake filters, clarifying filters and crossflow
filters.

Cake filters

Cake filters separate large amounts of solids as a cake of crystals or sludge. There usually exists a
provision for washing the cake and removal of some of the liquid from the solids before discharge.
At the initial stage of filtration using a cake filter, some solid particles enter the pores of the
medium and are immobilized, but soon others begin to collect on the surface of the septum. At the
end of this brief initial period, the cake of solids does the filtration not the septum; a visible cake
of appreciable thickness builds up on the surface and must be periodically removed. As with other
filters, cake filters may operate either with above atmospheric pressure upstream from the filter
medium or with vacuum applied downstream. As such, cake filters are mainly of two types;
pressure and vacuum filters.

Filter media

The support for the filter cake (septum) must meet the following requirement:
• It must retain the solids to be filtered, giving a reasonably clear filtrate
• It must not plug or blind
• It must be resistant chemically and strong enough physically to withstand the process
conditions
• It must permit the cake formed to discharge cleanly and completely
• It must not be too expensive
Washing filter cakes

In order to wash soluble materials that may be retained on the filter cake following filtration, a
solvent miscible with the filtrate may be used as a wash. Water is the most common wash liquid.
The rate of flow of the wash liquid and the volume of liquid needed to reduce the solute content
of the cake to a desired degree are important in the design. The washing of filter cakes is in three
parts.

During the first part of the wash period, the effluent consists majorly of the filtrate that was left of
the filter which is swept out by the first wash liquid without any dilution. Here the concentration
is nearly constant. This stage of washing, called displacement wash, is the ideal method of washing
a cake.

The second stage of washing is characterized by a rapid drop in concentration of the effluent. In
the third stage, the solute concentration in the effluent is low and the remaining solute is slowly
leached from the cake. If sufficient wash liquid is used, the residual solute in the cake can be
reduced to any desired point; but once it is acceptably low, any further washing should be stopped
when the value of the unrecovered solute is less than the cost of recovering it.

Clarifying filters

Clarifying filters remove small amounts of solids or liquid droplets to produce a clean gas or
sparkling clear liquids such as beverages. The solid particles are either trapped inside the filter
medium or on external surfaces. The particles are caught by surface forces and immobilized on the
surfaces or within the flow channels where they reduce the effective diameter of the channels but
usually do not block them completely.

Principles of Clarification

If the solid particles being removed completely plug the pores of the filter medium and the rate of
plugging is constant with time, the mechanism is known as direct sieving. This phenomenon is
rarely encountered. Much more commonly, the particles partially block the pores giving a gradual
reduction in pore size. This phenomenon is called standard blocking.

Cross-flow filters
In a cross-flow filter, the feed suspension flows under pressure at a fairly high velocity across the
filter medium which prevents the layer of solids formed on the surface of the medium from
building up.

Crossflow filtration is majorly of three types; Microfiltration, ultrafiltration and hyperfiltration.


Microfiltration is used for particles in the size range of 0.5 to 5 micrometer. Ultrafiltration covers
a wider range from 0.5 – 10-3µm. The term hyperfiltration (or reverse osmosis) is used for
separation of small molecules or ions.

The ideal membrane for crossflow filtration should have a high porosity and a narrow pore size
distribution, with the largest pores slightly smaller than the particles or molecules to be retained.

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