2. 1
Experiment 1
To Determine the Angle of Repose of Solid Particles
Objective:
The purpose of angle of repose is to find the maximum steepest angle up to which the materials
can be piled without slumping.
Apparatus and Required Material:
1. Rotary cylinder
2. Rice grains
3. Sand
4. Coal
Theory
The angle of repose, or critical angle of repose, of a granular material is the steepest angle of
descent or dip relative to the horizontal plane to which a material can be piled without slumping.
At this angle, the material on the slope face is on the verge of sliding. The angle of repose can
range from 0Β° to 90Β°. The morphology of the material affects the angle of repose; smooth, rounded
3. 2
sand grains cannot be piled as steeply as can rough, interlocking sands. The angle of repose can
also be affected by additions of solvents; if a small amount of water is able to bridge the gaps
between particles, electrostatic attraction of the water to mineral surfaces will increase the angle
of repose, and related quantities such as the soil strength.
When bulk granular materials are poured onto a horizontal surface, a conical pile will form. The
internal angle between the surface of the pile and the horizontal surface is known as the angle of
repose and is related to the density, surface area and shapes of the particles, and the coefficient of
friction of the material. Material with a low angle of repose forms flatter piles than material with
a high angle of repose.
The term has a related usage in mechanics, where it refers to the maximum angle at which an
object can rest on an inclined plane without sliding down.
Application of Theory
The angle of repose is sometimes used in the design of equipment for the processing of particulate
solids. For example, it may be used to design an appropriate hopper or silo to store the material, or
to size a conveyor belt for transporting the material. It can also be used in determining whether or
not a slope (of a stockpile, or uncompacted gravel bank, for example) will likely collapse;
the talus slope is derived from angle of repose and represents the steepest slope a pile of granular
material will take. This angle of repose is also crucial in correctly calculating stability in vessels.
It is also commonly used by mountaineers as a factor in analyzing avalanche danger in
mountainous areas
Q : What is morphology of material?
Morphology, from the Greek and meaning "study of shape". The morphology of something is
its form and structure. The study of the forms of things which are in particular form, shape or
structure. In particle technology we deal morphology with particles shape, size and other
physical properties.
Q : What is effect of shape on angle of repose?
4. 3
Shape and roughness of particles affect the angle of repose and friction coefficients of the
particles. The irregularity present in the shape of the clump particles acts as inter-locking
mechanism between the clumps. The circular or spherical particles minimizes the angle of
repose. Rough sized particles increases angle of repose. the angle of repose decreases when the
particle size of increases.
Q : What is effect of surface area on angle of repose?
Surface area also affects the angle of repose. Greater the surface area then there is greater free
spaces between molecules and then molecules have less force will be present between molecules
and hence angle of repose decreases.
Q : What is the effect of density on angle of repose?
The correlation between density and angle of repose can also be observed, the higher
density, the lower angle of repose.
Q : What will be the effect on angle of repose on adding solvent?
The angle of repose can also be affected by additions of solvents. If a small amount of water is
able to bridge the gaps between particles, electrostatic attraction of the water to mineral surfaces
will increase the angle of repose, and related quantities such as the soil strength. Hence angle of
repose increases by addition of solvents.
Procedure:
1. Take the sample of rice grains in the rotary cylinder until it is half filled and make the
sample parallel to the horizontal. Same do this for coal and sand.
2. Then rotate the cylinder in the clockwise direction and note the angle the sample makes
with that scale on the cylinder.
3. Repeat the experiment in the anticlockwise direction.
4. Calculate the angle of repose of rice grains by taking the mean of both the angles.
5. 4
OBSERVATIONS & CALCULATIONS
TYPE OF
MATERIAL
ANGLE IN
CLOCKWISE
DIRECTION (A)
ANGLE IN
ANTICLOCKWISE
DIRECTION (B)
ANGLE OF REPOSE
C = (A+B / 2)
RICE 300
400
350
SAND 200
250
22.50
COAL 420
480
450
Remarks:
1. We concluded that those particles who have regular shape like spherical have less angle
of repose than those of irregular shaped particles.
2. Regular shaped particles have packing closer to each other and also molecules can slide
over them easily and hence there angle of repose is less as compared to those irregular
shaped particles.
3. Fine grinded materials form a shallower pile with small angle of repose.
6. 5
Experiment 2
Calculate the Apparent & Actual Density of Solid Materials.
Objective
1. Calculate the apparent density of a given samples of solid materials.
2. Calculate the actual density of a given samples of solid materials.
3. Then checking if there is any difference between the two densities due to spaces.
Apparatus and Required Material
1. Sand sample
2. Coal sample
3. Water
4. 1000 ml graduated cylinder
5. Weighing balance
Theory
The density of particles, powders, and compacts is an important property affecting the performance
and function of many pharmaceutical materials. By definition, all density measurements involve
the measurement of mass and volume. Mass is determined with an analytical balance and the key
to obtaining reliable density values is in the accuracy and precision of measuring volume.
True Density
True density is the density of the solid material excluding the volume of any open and closed
pores. Depending on the molecular arrangement of the material, the true density can equal the
theoretical density of the material and therefore be indicative of how close the material is to a
crystalline state or the proportions of a binary mixture. True density measurements can be
performed on APIs, excipients, blends, and monolithic samples such as tablets.
7. 6
Apparent Density
The mass per unit volume (or the weight per unit volume) of a material, including the voids which
are inherent in the material is called apparent density. Apparent density is similar to the true density
except the volume of closed pores is also included. Tablets or excipient materials may have closed
cells or bubbles that are not accessible to the probe gas. In this instance, gas pycnometry produces
the apparent density. If the true density of a powder is known and the density of a tablet composed
of this same material differs, the closed pore volume can be determined. Closed pore volume may
be linked to press performance and die filling,
Bulk Density
Bulk density is a characteristic of a volume of divided material such as powders, grains, and
granules. It includes the volume of the solid material, open and closed pores, and the interparticle
voids. The total volume of interparticle voids can change with packing, thus leading to the concept
of Tap Density, which measures the volume of a mass of sample after inducing a closer packing
of particles by tapping the container. Taking this method to the extreme leads to the determination
of void volume and compressed density after compressing the sample under extreme forces and
measuring the volume change as a function of applied pressure.
Envelope Density
Like bulk density, envelope density is determined from the volume of the solid material, open
pores, and closed pores. Envelope density is determined for a single, consolidate quantity of
material, therefore there are no interparticle voids between packed particles. Envelope density is
the mass of the object divided by the volume within an imaginary, closely conforming skin that
envelops it and, therefore, may include the volume of small surface irregularities. When envelope
and true density both are known, the total pore volume, percent porosity, and solid fraction of the
sample can be calculated.
Porosity
Porosity consists of volume of the pores relative to the envelope volume used to calculate envelope
density. The porosity of pharmaceutical materials and medical devices can impact production,
8. 7
material movement, and pharmacokinetic behavior. Tablet porosity determines the tensile strength
(hardness) of tablets for a given composition. Tablet porosity may be regarded as a measure of the
tableting process. Variations in tablet porosity reflect various aspects of tablet press performance.
Tablet porosity may relate to tablet disintegration and dissolution.
Q : Define Apparent, Actual and Rare density?
Apparent density is defined as the mass of many particles of the material divided by the
total volume they occupy. The total volume includes particle volume, inter-particle void volume,
and internal pore volume. It is measured in kilograms per cubic meter (kg/m3
).
Actual density is the ratio between mass and volume or mass per unit volume. It is a measure of
how much stuff an object has in a unit volume (cubic meter or cubic centimeter).
Rare density or True density is density of solid material excluding the volume of any open and
closed pores depending on the molecular arrangement of the material. The true density can equal
the theoretical density of material.
Method: By using water and measuring cylinder: This method is preferred if the material under
study is not water soluble e.g. sand.
Procedure
1. Weigh the given sample of sand to 500g and then pour it into cylinder. Same did it for
coal with 200g.
2. Note the volume of the sample of sand in the cylinder when it is settled and then calculate
its apparent density (density=mass/volume).
3. After which add some water into the cylinder so that all the sand is covered by the water.
4. Wait for ten minutes so that the sand particles completely settle and no spaces between
particles are left.
5. Then measure the new volume of sand from the cylinder and calculate its actual density
(density=mass/volume).
9. 8
Observations & Calculations:
Apparent Density
Actual Density
Mass of sand π1= 500 g
Mass of sand π2= 500 g
Volume of sand before compacting water
π1= 400 ml
Volume of sand when compacted after
addition of water π2= 365 ml
Density π1 =
π1
π1
β = 1.25 g/ml
Density π2 =
π2
π2
β = 1.369 g/ml
In the end calculate the crushing ratio of material by using formula
Crushing ratio = Ξ¦ =
π΄πππππππ‘ ππππ ππ‘π¦
π πππ ππππ ππ‘π¦
= 0.919
Observations & Calculations:
Apparent Density
Actual Density
Mass of coal π1= 200 g
Mass of coal π2= 200 g
Volume of coal before compacting water
π1= 200 ml
Volume of coal when compacted after
addition of water π2= 192 ml
Density π1 =
π1
π1
β = 1 g/ml
Density π2 =
π2
π2
β = 1.04 g/ml
In the end calculate the crushing ratio of material by using formula
Crushing ratio = Ξ¦ =
π΄πππππππ‘ ππππ ππ‘π¦
π πππ ππππ ππ‘π¦
= 0.9615
Remarks
1. Apparent volume is smaller than the actual volume because there are free spaces
between sand molecule
10. 9
2. By filling any solvent into the sand or coal leads the liquid to settle into the spaces of
the molecules and hence volume gets low.
3. In sand addition of water leads to more settling down of volume than coal because of
shape and size of particles.
4. Crushing ratio of sand is less than crushing ratio of coal.
5. Actual density of powdered coal is greater than apparent density of coal and also in
case of sand.
11. 10
Experiment 3
Sieve Analysis for a Sample of Solid Particles
Objectives
1. To study the particle size distribution and analysis.
2. To separate solid particles of different sizes and then calculating weight of different size
particles in the whole sample.
Apparatus and Required Material
1. Vibratory sieve
2. A set of 7 sieves
3. Weighing balance
4. Coal as solid particles
Theory
A sieve analysis is a practice or procedure used to separate particle on the basis of particle size
distribution (also called gradation) of a granular material. The size distribution is often of critical
importance to the way the material performs in use.
12. 11
This test is performed to determine the percentage of different grain sizes contained within a soil.
The mechanical or sieve analysis is performed to determine the distribution of the coarser, larger-
sized particles.
What is the effect of vibrations on sieve?
Vibrations are very important on sieving. It is because of that when we put particles on sieves, then
those particles which retain on the wire doesnβt go down until we gave them some jerk so that they
come up on sieve hole and then they go down. Hence vibrations are very important so that particles
get down from sieves otherwise they will remain stuck on the top of sieves. Vibrations produce a
higher degree of sieving.
Procedure
1. First, weigh 505g of sand sample and feed it into the vibratory sieve from the top and
close the set of sieves tightly.
2. Start the vibratory sieve and set the timer to 7 minutes.
3. After 7 minutes, switch off the vibratory sieve.
4. The sand particles will be separated on the basis of their size in different sieves.
5. Then, weigh the sample of sand particles in each individual sieve.
Observations and Calculations
Sieve
#
Screen
opening
diameter(mm)
Mass
retained
in
screen(g)
%age mass
retained
Average
particle
size(mm)
Mass
fraction
retained
Cumulative
wt%
undersize
Cumulative
wt%
oversize
π·0 π0 π% π· ππ£π π ππ£π ππ’ππ πππ£π
1 4 70 13.4 0.134 86.6 13.4
2 2.8 26 4.9 3.4 0.049 81.7 18.3
3 2 56 10.7 2.4 0.107 71 29
4 1.4 182 34.8 1.7 0.348 36.2 63.8
5 1 136 26.05 1.2 0.2605 10.15 89.85
6 0.7 20 3.8 0.85 0.038 6.35 93.65
Pan 0.063 32 6.35
Total 525
13. 12
Graphs to be drawn
1) Differential Analysis:
a) π· ππ£π and π ππ£π
2) Cumulative Analysis:
Combined graph between
π) π·0 and ππ’ππ
14. 13
Remarks
1. Through sieve analysis we can separate particles of different sizes according to our need.
2. This process is so easy that it doesnβt need any complex process to separate the particles
and separation is so easy.
3. After doing sieve analysis, we can easily measure the weight of particles according to our
need of size.
c) DO & WOVR
15. 14
Experiment 4
Mixing of Different Solid Particles
Objective:
1. To check if different solid particles on mixing form a homogeneous solution or not.
2. To check the rate of blending of solid particles with respect to time.
Apparatus and required material:
1. Blender
2. Solid particles (100g salt and 100g sand)
Theory
In industrial process engineering, mixing is a unit operation that involves manipulation of
a heterogeneous physical system with the intent to make it more homogeneous. Mixing is
performed to allow heat and/or mass transfer to occur between one or more streams, components
or phases. Modern industrial processing almost always involves some form of mixing. Some
classes of chemical reactors are also mixers. With the right equipment, it is possible to mix a solid,
liquid or gas into another solid, liquid or gas. The opposite of mixing is segregation. A classical
example of segregation is the brazil nut effect.
16. 15
Mixing Classification
The type of operation and equipment used during mixing depends on the state of materials being
mixed (liquid, semi-solid, or solid) and the miscibility of the materials being processed. In this
context, the act of mixing may be synonymous with stirring-, or kneading-processes. In this section
we will discuss solid-solid mixing.
Solid-Solid Mixing
Blending powders is one of the oldest unit-operations in the solids handling industries. For many
decades powder blending has been used just to homogenize bulk materials. Many different
machines have been designed to handle materials with various bulk solids properties. On the basis
of the practical experience gained with these different machines, engineering knowledge has been
developed to construct reliable equipment and to predict scale-up and mixing behavior. Nowadays
the same mixing technologies are used for many more applications: to improve product quality, to
coat particles, to fuse materials, to wet, to disperse in liquid, to agglomerate, to alter functional
material properties, etc. This wide range of applications of mixing equipment requires a high level
of knowledge, long time experience and extended test facilities to come to the optimal selection of
equipment and processes.
Machine for incorporating liquids and finely ground solids
One example of a solidβsolid mixing process is mulling foundry molding sand, where
sand, bentonite clay, fine coal dust and water are mixed to a plastic, moldable and reusable mass,
applied for molding and pouring molten metal to obtain sand castings that are metallic parts for
automobile, machine building, construction or other industries.
17. 16
Q : Define Segregation?
In segregation, particulate solids and also quasi solids such as foams tends to segregate by
virtue of differences in the size and also by physical properties such as volume, density, shape
and other physical properties of which they are composed. the opposite of segregation is mixing.
an example of segregation is brazil nut effect.
Q : What are benefits of mixing?
Nowadays the same mixing technologies are used for many more applications: to improve
product quality, to coat particles, to fuse materials, to wet, to disperse in liquid, to agglomerate,
to alter functional material properties, etc. It is also used to study the particles effects in
themselves after mixing.
Procedure:
1. First take sample of salt and sand each 100g and put it into a blender.
2. Switch on the blender and mix it for 3 minutes.
3. Then take out the sample and check it if homogeneous mixture is reached or not.
4. Repeat the procedure for 5 minutes and 7 minutes for mixing.
18. 17
Observations and calculations:
Material Before Mixing After 3 Minutes After 5 Minutes After 7 Minutes
Sand & Salt 200ml 179ml 170ml 160ml
Remarks:
1. In this experiment, we learned that mixing decreases the volume of mixture.
2. It is because that by continuous mixing the particles come close to each other and forces
of attraction between them increases.
3. Mixing reduces the volume by depending on time. After greater time particles gets mixed
more than in lower time.
19. 18
Experiment 5
Flow Pattern of Solid Particles
Objective:
1. To study the flow pattern of a given sample of solid particles through cylinders of
different diameters.
Apparatus and Required Material:
1. Cylinder
2. Cylinder stand
3. Sand
4. Coal
5. Floor
Effect of size/shape of particles on flow rate?
There is so much effect of size and shape of particles on feed flow. Particles with smaller size
will flow greater w.r.t. time than those with greater sized particles as given below. Shape also
have effect on flow. Irregular shaped particles will flow more badly than proper shaped particles.
They will take more time to pass. Spherical shaped particles will flow easily than those of
irregular shaped particles because they can flow easily.
Procedure:
1. Take the given sample of sand and put it in the first cylinder from the top and lid it.
2. When the lid is removed the sand starts falling, and then observe the flow pattern of sand
particles.
3. Repeat the experiment for other cylinders of different diameters.
Observation & Calculations:
1st
cylinder has largest hole in it.
2nd
cylinder has also greater hole but less than 1st
hole
20. 19
3rd
cylinder have hole lesser than 2nd
hole
4th
cylinder has smallest hole.
Time required to flow out of these particles are:
MATERIAL 1st
cylinder 2nd
cylinder 3rd
cylinder 4th
cylinder
SAND 2sec 3.5sec 8sec 19sec
RICE 2.8sec 6.8sec 11.8sec 27sec
FLOOR 4.9sec 6.7sec 15.4sec 38.7sec
Remarks
1. Particles size matter when they flow from some type of opening to pass from one place to
another.
2. Greater the particle size, more the time required to flow from openings. Small sized
particles flow easier than big sized particles.
21. 20
Experiment 6
Size reduction of Coarse Feed Particles with Jaw Crusher
Objective:
1. It is used for increment in the surface area of feed material by crushing coarser feed into
intermediate and fine particles.
Apparatus and Required Material:
1. Jaw Crusher
2. Weighing balance
3. Trays for conveying
4. Stack of sieves
5. Bricks as solid feed
Theory
A crusher is a machine designed to reduce large rocks into smaller rocks, gravel, or rock dust.
Crushers may be used to reduce the size, or change the form, of waste materials so they can be
more easily disposed of or recycled, or to reduce the size of a solid mix of raw materials (as in
rock ore), so that pieces of different composition can be differentiated. Crushing is the process of
transferring a force amplified by mechanical advantage through a material made of molecules that
bond together more strongly, and resist deformation more, than those in the material being crushed
22. 21
do. Crushing devices hold material between two parallel or tangent solid surfaces, and apply
sufficient force to bring the surfaces together to generate enough energy within the material being
crushed so that its molecules separate from (fracturing), or change alignment in relation to
(deformation), each other. The earliest crushers were hand-held stones, where the weight of the
stone provided a boost to muscle power, used against a stone anvil.
Jaw Crusher
Operating principle
Jaw crushers operate according to the principle of pressure crushing. The crushing material is
crushed in the wedge-shaped pit between the fixed crusher jaw and the crusher jaw articulated on
an eccentric shaft. The material is crushed by the elliptic course of movement and transported
downwards. This occurs until the material is smaller than the set crushing size.
A jaw crusher uses compressive force for breaking of particle. This mechanical pressure is
achieved by the two jaws of the crusher of which one is fixed while the other reciprocates. A jaw
or toggle crusher consists of a set of vertical jaws, one jaw is kept stationary and is called a fixed
jaw while the other jaw called a swing jaw, moves back and forth relative to it, by
a cam or pitman mechanism, acting like a class II lever or a nutcracker. The volume or cavity
between the two jaws is called the crushing chamber. The movement of the swing jaw can be quite
small, since complete crushing is not performed in one stroke. The inertia required to crush the
material is provided by a weighted flywheel that moves a shaft creating an eccentric motion that
causes the closing of the gap.
Jaw crushers are heavy duty machines and hence need to be robustly constructed. The outer frame
is generally made of cast iron or steel. The jaws themselves are usually constructed from cast steel.
They are fitted with replaceable liners which are made of manganese steel, or Ni-hard (a Ni-Cr
alloyed cast iron). Jaw crushers are usually constructed in sections to ease the process
transportation if they are to be taken underground for carrying out the operations.
Jaw crushers are classified on the basis of the position of the pivoting of the swing jaw
1. Blake crusher-the swing jaw is fixed at the upper position
23. 22
2. Dodge crusher-the swing jaw is fixed at the lower position
3. Universal crusher-the swing jaw is fixed at an intermediate position
The Blake crusher was patented by Eli Whitney Blake in 1858. The Blake type jaw crusher has a
fixed feed area and a variable discharge area. Blake crushers are of two types- single toggle and
double toggle jaw crushers.
In the single toggle jaw crushers, the swing jaw is suspended on the eccentric shaft which leads to
a much more compact design than that of the double toggle jaw crusher. The swing jaw, suspended
on the eccentric, undergoes two types of motion- swing motion towards the fixed jaw due to the
action of toggle plate and vertical movement due the rotation of the eccentric. These two motions,
when combined, lead to an elliptical jaw motion. This motion is useful as it assists in pushing the
particles through the crushing chamber. This phenomenon leads to higher capacity of the single
toggle jaw crushers but it also results in higher wear of the crushing jaws. These type of jaw
crushers are preferred for the crushing of softer particles.
In the double toggle jaw crushers, the oscillating motion of the swing jaw is caused by the vertical
motion of the pitman. The pitman moves up and down. The swing jaw closes, i.e., it moves towards
the fixed jaw when the pitman moves upward and opens during the downward motion of the
pitman. This type is commonly used in mines due to its ability to crush tough and abrasive
materials.
In the Dodge type jaw crushers, the jaws are farther apart at the top than at the bottom, forming a
tapered chute so that the material is crushed progressively smaller and smaller as it travels
downward until it is small enough to escape from the bottom opening. The Dodge jaw crusher has
a variable feed area and a fixed discharge area which leads to choking of the crusher and hence is
used only for laboratory purposes and not for heavy duty operations.
Jaw Crusher Opening Size
Jaw crushers are referred to by two sets of numbers, the first being the opening size of the jaw; the
second being the width. So, a "1036" jaw would accept a 10" boulder at the top and be 3' wide. If
the pit where the jaw is being used has river rock which does not exceed 10" in size then this size
crusher would be acceptable. Larger crushers are better choices when the average size is larger,
24. 23
such as where rock is blasted using explosives. The width of the jaw directly impacts its
throughput rate.
Jaw Crusher Nip Angle
The nip angle describes the angle the stationary jaw plate and the pitman make with each
other. The exact value of this angle isn't quoted or even determinable due to curvature in the jaws
themselves but what is important is how wide vs. narrow it is. Wide nip angles can tend to expel
material as the jaw closes as a large ball might squirt out from under a car tire. If the nip angle is
narrow, not much vertical upward force is generated and more consistent crushing takes place.
Feed Product
Procedure:
1. First, we took 6kg of bricks for crushing as a sample.
2. Then we reduced the size of bricks to some extent by hammering.
3. After that we noted the time before putting the bricks into crusher and then added the
feed sample continuously
4. After crushing process, we noted the time again required for crushing.
25. 24
Observations & Calculations:
β A mixture of coarser, intermediate and fine particles is obtained after crushing.
β Total feed input= 6.00kg
β Reduced sized particles=1.5 kg
β Oversized particles=4.2 kg
4.2+1.5=5.7 kg
β Size reduction=300g
Graphs to be drawn:
1) Differential Analysis:
a) π· ππ£π and π ππ£π
Sieve
#
Screen
diameter
(mm)
Mass
retained
(kg)
Percentage
mass
Average
diameter
(mm)
Mass
fraction
retained
Cumulative
wt%
undersize
Cumulative
wt%
oversize
π·0 π π% π· ππ£π π ππ£π ππ’ππ πππ£π
3 0.2 0.114 11.66 0.11 88.34 11.6
4 0.187 0.166 16.22 0.193 0.16 72.12 27.8
7 0.111 0.176 17.99 0.149 0.17 54.13 45.8
8 0.0937 0.24 24.54 0.102 0.24 29.59 70.4
10 0.0781 0.22 20.50 0.086 0.20 9.09 90.9
14 0.0555 0.04 4.09 0.067 0.04 5 95
25 0.028 0.0.003 3.07 0.041 0.03 1.93 98
Pan 0 0.0.189 1.934 0.014 0.019 0 100
Total 0.977 100% 1
26. 25
2) Cumulative Analysis:
Combined graph between
b) π·0 and ππ’ππ
c) π·0 and πππ£π
Remarks:
1) Jaw crusher is used to crush particles into very small size by mechanical ways and then we
can separate these particles into required size.
2) After passing the particles through jaw crusher we can easily handle the particles.
3) These crushing machines is important as it consumes less energy and hence can be used
effectively.
27. 26
UNIVERSITY OF ENGINEERING &
TECHNOLOGY LAHORE
(KSK CAMPUS)
LAB REPORT
PARTICLE TECHNOLOGY
SUBMITTED TO : MAM HAFIZA AROOSA ASLAM KHAN
SUBMITTED BY : USMAN SHAHID
ROLL NO. : 2018-CH-265
SECTION : A
DEPARTMENT OF CHEMICAL ENGINEERING