FLUID-SOLID SYSTEMS

TCE 3105

LECTURE 1: INTRODUCTION AND PARTICLE

CHARACTERIZATION

Dr HLABANGANA
2018
 INTRODUCTION: PARTICLES IN THE
PROCESS INDUSTRY & ELSEWHERE

Definitions
Particle: a general term for any small fragment of solid substance
Particulate matter: a solid material in the form of particles
Particulates: abbreviation of “particulate matter” often implying a very
diverse range of kinds or sizes of particles e.g. in urban air samples
Particulate technology: involves study of processes using or producing
particles
Micron: or µm i.e 10-6 m

These terms can cover a wide range of sizes, typically about 1 to 10,000
micrometres (1 cm), but the limits are not rigid.
 INTRODUCTION: PARTICLES IN THE
PROCESS INDUSTRY & ELSEWHERE

More specific terms suggest narrower size ranges:

Powder: smaller particles (when manufactured)

Dust: smaller particles (when produced by chance or by natural processes)

Granules: larger particles (often produced by binding the particles of a

powder into clusters) – typically of the order of 1 mm in size.

Pellets: large particles (e.g. catalysts) of defined shape and size, perhaps
as large as several centimeters.
TYPICAL PARTICULATE MATERIALS & SIZES

Many important industrial

processes use particle
technology and a huge number
of products & materials, both
natural and man-made are
particulate in nature.

Thus, particle technology finds

application in a wide range of
industries such as food
manufacturing, chemical
manufacture, pollution control
etc
 CHARACTERISTICS OF PARTICULATE MATTER

We can distinguish between characteristics of the material itself

(individual particles) and those of a large volume of particles (bulk
characteristics)

Material Individual Particles

• Chemical composition
• Homogeneity- does the
chemical composition vary
between particles? Differences
may be minor as in natural
products or major as in a
mixture of cement and sand
• Structure- e.g. crystalline or
amorphous
• Size- often the most important single
characteristic
• Size distribution- important if the
particles are not uniform, which is
common
• Shape- compact or elongated,
regular or irregular. If regular what
shape are they?
• Structure- solid or hollow/diffuse e.g.
snowflakes or diatomaceous earth
• Strength- are the particles liable to
deform or break up
• Surface:volume ratio- small particles
have a higher ratio i.e. more reactive
than an equal mass of larger
particles.
 CHARACTERISTICS OF PARTICULATE MATTER

We can distinguish between characteristics of the material itself

(individual particles) and those of a large volume of particles (bulk
characteristics)

Bulk Characteristics
• Bulk density- may be very low (e.g. snow is only 10% as
dense as ice)
• Voidage- the fraction of space in a bed of particles. (Ranges
from 0.0-1.0, typically about 0.6 for a random bed of
compact particles but about 0.1 for snow and almost 1.0 for
some neatly stacked solids, such as bricks.)
• Caking- do the particles tend to stick together. This is
common with hygroscopic materials if not kept dry.
• Mixing- If particles vary in composition, is the bed well
mixed or segregated?
 CHARACTERISTICS OF PARTICULATE
MATTER: A fourth state of matter?

Particles can almost be considered a fourth state of matter, in addition to

solid, liquid and gas. Although the material is in solid form, dividing it into
tiny particles can give it some of the properties of a fluid, such as high
reactivity and the ability to flow, like sand in an hour-glass.

Sometimes particulate matter displays unique behaviour unlike anything

seen in a solid, a liquid or gas. Consider the following situation, what
would happen and why?

A steel ball is resting on the bottom of a bed of sand (a less dense

material) in a bucket at the back of the lorry. A long journey over rough
roads vibrates the bucket vertically. Where does the ball end up?
 PARTICLE CHARACTERIZATION: Particle
Size and Particle Size Distribution (PSD)

Particle size and PSD the most important variable and also hard to
measure.

Size easily defined for particles of regular shape e.g.

• Sphere: diameter
• Cube: length
• Cuboid: L×W×D
• Cylinder: D×L

Particle size much harder

to measure and define for
an irregular particle
 PARTICLE CHARACTERIZATION: How to
measure size?

There are many different types of equipment and typically provide

equivalent spherical diameters.
NAME EQUIVALENT REFERENCE
SPHERICAL DIAMETER
Microscope Projected area www.atmcorporation.com
LasentecTM (particle length www.lasentec.com
chord length FBRM)
MalvernTM (laser Area-light scattering www.malvern.co.uk
diffraction) properties

Coulter CounterTM volume www.beckman.com

(electric zoning sensing) see Multisizer
Sedigraph and Andeasen sedimentation www.micromeritics.com
pipette see Sedigraph
 PARTICLE CHARACTERIZATION: How to
measure size?

Brief summary for these methods given below. For detailed descriptions
consult reference given and Coulson and Richardson’s, vol. 2, 5th edn., pp
4-11.
Sieving
One of the simplest and most traditional method, ideal for larger particles of hard
dry material e.g. mineral ores. The process itself can be mechanized but loading
the sample, weighing the fractions produced and data recordings all manual
operations. The data it yields is in the form of ‘x grams retained by sieve 1’, ‘y
grams passed through sieve 1 but was retained by sieve 2’. Knowing the size of
the holes, you can work out what % of the sample by mass falls into each size
range. The sieves are made from strong wire woven into a square mesh, so that
the largest dimensions of the smallest projected area of the particle determines
the smallest size opening it will pass through-in theory! In practice sieving is not
suitable for elongated particles, as these are likely to lie flat on the sieve and be
retained.
 PARTICLE CHARACTERIZATION: How to
measure size?

Laser diffraction
One of the most modern methods and is widely used for particles of 0.1-2000
micron diameter, a wide operating range. The sample is usually suspended in a
liquid or gas, so this method is particularly ideal for suspensions. A beam of laser
light is scattered by any particle in its path into detectors alongside the beam and
the angle of diffraction is inversely proportional to the volume of the particle.
Complex mathematical analysis of the signals from these detectors can give direct
output of PSD. It gives a distribution by volume but this data can be readily
converted into another base, such as number or mass. The whole process can be
largely automated, so this method is often preferred where labour costs are high
enough to justify buying the costly equipment.
 PARTICLE CHARACTERIZATION: How to
measure size?

Microscopy
This is another standard method, useful over a wide size range. Manual recovery
of data from such work is very laborious, so automation is common. Essentially
this requires linking a microscope to a video camera, serving a PC with image
analysis software. This can distinguish individual particles from the background
and measure apparent size. An adhesive layer may be used on the microscope
slide to ensure elongated particles are randomly positioned, rather than lying
down. In automated microscope analysis three diameters are often used: Feret,
Martin and Image Sheared.
PARTICLE CHARACTERIZATION: How to
measure size?
 PARTICLE CHARACTERIZATION: How to
measure size?

Electrozone sensing
This method is ideal for counting the number of particles in a suspension of small
particles which are all of similar size e.g. red cells in blood or yeast in beer, but
can be adapted to measure PSD over a wide size range. The well known Coulter
Counter uses this principle. The sample is passed through a small orifice between
two elecrodes. The voltage across the orifice is measured and shows a ‘blip’ as
the particle passes. The sample may require diluting so that, so that two particles
are unlikely to pass together. Then each blip represents a particle and the
magnitude of the blip is related to its volume. Data logging and analysis can be
largely automated quite easily. However, a single orifice can only handle a narrow
range of particle sizes: large particles may block it, while small ones maybe
undetectable or they may not pass through one at a time. So a decreasing series
of orifices must be used to obtain PSD data.
 COMPARING SIZE OF IRREGULAR
PARTICLES

A common yardstick is required when shapes differ. In engineering we

perform calculations using diameter so we need some simple basis for
describing irregular shaped particles.

Consequently comparison with an equivalent sphere is used as a

convenient yardstick.

A physical property of the particle is related to a sphere that would have

the same property e.g. same volume, surface area etc. Thus for the same
particle the equivalent spherical diameter depends on the property
selected for equivalence.

Some of the comparative diameters are listed and defined below. Note the
nomenclature varies: some books may use slightly different titles
 COMPARING SIZE OF IRREGULAR
PARTICLES: Equivalent spherical diameters

Equivalent –volume sphere diameter (dv): diameter of a sphere whose volume

equals that of the particle. Sometimes called the volume-equivalent sphere
diameter
Equivalent –surface sphere diameter (ds): diameter of a sphere whose surface
area equals that of the particle.

Surface/volume diameter (dsv): diameter of a sphere whose surface/volume ratio

equals that of the particle. A more logical name would be equivalent-
surface/volume sphere diameter. Often written –less helpfully- as surface-volume
diameter

Sieve diameter (dp): diameter of the largest sphere which will just go through the
smallest square holes which the particle would go through.

Projected area diameter (dpa): diameter of a circle which has the same area as the
projected area of the particle when resting in a stable position. Need to calculate
this for each stable position.
 COMPARING SIZE OF IRREGULAR PARTICLES:
Equivalent spherical diameters Class Tutorial

Calculate the following equivalent diameters for a cuboid measuring

5×3×1 mm.

Equivalent –volume sphere diameter (dv)

Equivalent –surface sphere diameter (ds)

Surface/volume diameter (dsv)

Sieve diameter (dp)

Projected area diameter (dpa):

 PARTICLE SIZE DISTRIBUTION (PSD)

PSD can be shown in several ways:

• As histogram, showing number* of particles in each range of
diameters*
• As a distribution curve (essentially a smoothed histogram)
• As a cumulative distribution curve, showing the number* of particles
above or below a given diameter*
Other variables can replace one or both of the starred ones.

Cumulative distribution curves are often the most useful. They can
show compliance with product specifications e.g. no more than 10%
of the particles below or above x microns.
PARTICLE SIZE DISTRIBUTION (PSD):
PRESENTATION

PSD presented as a histogram and distribution curve

PARTICLE SIZE DISTRIBUTION (PSD):
PRESENTATION

PSD presented as a cumulative % undersize curve

 PARTICLE SIZE DISTRIBUTION (PSD): AVERAGE
DIAMETERS

Mode: most common occurring value in distribution i.e. value at which

frequency is a maximum.
Median: divides distribution into two equal parts. 50% size on
cumulative distribution curve.
Mean: centre of gravity of the distribution.
 PARTICLE SIZE DISTRIBUTION (PSD): SHAPE

In addition to size, shape is also important in particulate systems. Shape

has an important influence on processing requirements.

Particle shape affects powder packing and thus its bulk density, porosity,
permeability, cohesion, flowability, caking behaviour, attrition, interaction
with fluids and the covering power of pigments.

One simple way to quantify shape is using Wadell’s sphericity (ψ).

Example: Calculate the sphericity of a cuboid measuring 5×3×1 mm.

 PARTICLE SIZE DISTRIBUTION (PSD): SAMPLING

Even, if initially well mixed, a mass of particles can easily become unmixed
(segregated) during transportation, making it difficult to get representative
samples.
One obvious point is to ensure you use sample jars much larger than the
largest particle you expect to find.

Ideally:
• Take samples of flowing particles only e.g. from the stream entering
a storage bin rather from the bin itself.
• Take several short samples of the flow (early, middle and late; in
case of variation with time)
• Take samples of the whole flow, rather than just diverting a fraction
of it, in case there is variation through the cross-section i.e. heavier
particles will not follow same trajectory as lighter ones.
 PARTICLE SIZE DISTRIBUTION (PSD): TUTORIAL

• Complete the table rows below and plot the corresponding frequency,
cumulative frequency, and normalised frequency distribution curves.
• Find mean particle size by number.

Size range <5 5-7 7-10 10-15 15-20 20-30 30-40 40-50 >50
(µm)
Number in 0 50 150 200 55 45 20 5 0
range
Relative 0 0.0952
number
Cumulative 0 0.0952 1.000
no. undersize
Relative no. 0 0.0476
per µm