LAB MANUAL

PARTICULATE TECHNOLOGY CHE-121

PREPARED BY:
ENGR. TAHIR SAIF
ENGR. SHSHZAD ALI

DEPARTMENT OF CHEMICAL ENGINEERING

COMSATS INSTITUTE OF INFORMATION
TECHNOLOGY, LAHORE
 LIST OF EXPERIMENTS

Sr.No. Experiment / Objective

Jaw Crusher
 To report the energy required for crushing one ton of red bricks (-3” +2”)
using the laboratory jaw crusher.
 To report the total energy required for crushing one ton of red bricks (-3”
+2”) for the same equipment.
 To report the results of screen analysis, for the product obtained, in the
1
form of cumulative and fractional distributional plots, and give
inferences.
 To report different types of diameters, for the product obtained, such as
Bond‟s diameter, weight(volume) mean diameter, mean volume
diameter, surface mean diameter(Sauter mean diameter), and mean
length diameter.
Disc Mill
 To report the energy required for crushing one ton of rock salt (-2 +4) using
laboratory disc mill.
 To report the total energy required for crushing one ton of rock salt (-3” +2”)
for the same equipment.
 To report the results of screen analysis, for the product obtained, in the
form of cumulative and fractional distributional plots, and give
inferences.
2
 To report different types of diameters, for the product obtained, such as
Bond‟s diameter, weight(volume) mean diameter, mean volume
diameter, surface mean diameter(Sauter mean diameter), and mean
length diameter.
 To report the properties such as bulk density and voidage of the product
obtained.
High Shear Mill
 To report the energy required fir crushing one ton of rock salt (-2 +4) using
laboratory high shear Mill.
 To repot the total energy required for crushing one ton of the rock salt (-2
+4)for the same equipment.
 To report the results of screen analysis for the product obtained in the
form of cumulative & fractional distributional plots and give inference.
3  To report different types of diameters for the product obtained such as
bonds diameters weight (Volume) mean diameter , mean volume
diameter , surface mean diameter (sauter mean diameter) and mean
length.
 To report the properties such bulk density and voidage of the product
obtained.
 Sieves and Dyes
 To enlarge the size of given material (powder) using sieves and dies.
4
 To find the total time to dry the product.
 To find the bulk properties of the product.
Kneader Mixer for Dry Solids
 To find out the energy required to mix (blend) one ton of sand and
sodium carbonate (Na2CO3) in the ratio 10:1 using laboratory kneader
5
mixer used for flowing solids (dry Solids).
 To find out the total energy required for the case mentioned above.
 To find out the total time of mixing and show it graphically.
Kneader Mixer for Pastes
 To find out the energy required to mix (blend) one ton of clay and
sodium carbonate (Na2CO3) in the ratio 5:1 using laboratory kneader
6
mixer used for cohesive solids (or paste-mixing).
 To find out the total energy required for the case mentioned above.
 To find out the total time of mixing and show it graphically.
Oil Extractor
 To report the required to extract one ton of oil from the given feed using a
laboratory oil extractor.
 To report the total energy to extract one ton of oil from the given seed using
a laboratory oil extractor.
7
 To report the results of screen analysis, for the product obtained, in the form
of cumulative and fractional distributional, and give inferences.
 To report the different types of diameters , for the product obtained, such as
Bond‟s diameter , weight (Volume) mean diameter, surface mean diameter
(sauter mean diameter), and mean length diameter.
 Course Objectives (CO’s)

To provide the knowledge & skills, for efficient and safe utilization of crushing
equipments,calculation of energy requirements of equipments, chahracterization of crushed
product and their application in industrial processes.

Course Learning Outcomes vs Course Objectives (CO’s)

COs

Course Learning Outcomes CLOs 1 2 3 4

To perform analysis and calculations for 1

characterization of the crushed products and energy
requirements for crushing.

Describe the major components, working principle, 2

construction of different Lab & industrial equipment
related to subject Lab.
Adapt to SOPs of equipment, troubleshooting 3
protocols & report writing techniques while operating
any eqipment.
Adopt safety measures during work to avoid any 4
accident & be prepared for any unwanted event.
 %age CLO Distribution

Sr. # Assessments
CLO CLO CLO CLO

1 2 3 4

4.3 3.9 0.6 1.2

1 Sessional-1
(Week- 5) Quiz/
6 2 0 2
Assignment

Sessional-2 5.25 5.25 1.5 3

2

(Week- 10)
Quiz/
2 6 0 2
Assignment

12.5
Terminal 17.5 12.5 7.5
3

(Week- 16) 0 9
Project 0 0

4 Total 26 - 14-16
34 % 24 %
28 % %
 Safety Rules & Regulations

Do’s
 Learn about the hazards or potential hazard before performing the experiments
 Always use goggles, mask, face shield, lab coat, gloves etc. keeping in mind the
potential hazards.

Don’ts
 Don‟t fondle with apparatus
 Don‟t operate an apparatus until you are permitted by instructor
 Don‟t put your bags and other stuff on apparatus table
 Don‟t let the power cords drapes across the floor
 Don‟t get too close to the moving parts
 Don‟t get close to running equipment with loose clothes
 No smoking or drinking allowed in lab
 Jaw Crusher

Objectives:
o To report the energy required for crushing one ton of red bricks (-3” +2”) using the
laboratory jaw crusher.
o To report the total energy required for crushing one ton of red bricks (-3” +2”) for the same
equipment.
o To report the results of screen analysis, for the product obtained, in the form of cumulative
and fractional distributional plots, and give inferences.
o To report different types of diameters, for the product obtained, such as Bond‟s diameter,
weight(volume) mean diameter, mean volume diameter, surface mean diameter(Sauter
mean diameter), and mean length diameter.

Concepts:
The main objective of this experiment is to introduce the concept of crushing in main chemical
industries. A crusher is a machine designed to reduce a large solid material objects into a smaller
volume, or smaller pieces. Crushers may be used to reduce the size, or change the form, of waste
materials so they can be more easily disposed or recycled, or to reduce the size of a solid mix
materials(as in rock ore) so that pieces of different compositions 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 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.
Querns and mortars are types of these crushing devices.
Theory:
The crushing form of this series Jaw Crusher is driven squeezing style. Its working principle is:
Motor drives the belt and belt pulley, makes moving jaw up and down through eccentric shaft.
When the moving jaw is up, the angle between lining plate and moving jaw becomes large, and
this will push moving jaw plate close to the fixed jaw plate. During this process material is
crushed and ground, thus the crushing will be done. When the moving jaw is down, the angle
between lining plate and moving jaw becomes small, the moving jaw plate will leave the fixed
jaw plate on account of the of the effect of pulling bar and spring, and then the crushed material
will be discharged from the lower opening of the crushing room. With the motor continuously
rotating and the material periodically crushed and discharged by the crusher, the mass production
can be realized.

Procedure:

o Prepare 5 kg of feed (red bricks) of the size that can pass through a 3 in hole and retain on
a 2 in hole.
o Note down the time (t1) required for 2 revolution (n1) of the energy meter disc under un-
loaded conditions. Also note down the energy meter factor (N).
o Note down the initial meter reading (R1) and turn on the crusher. Start introducing the
feed pieces one by one and start the stopwatch simultaneously in order to measure the
total time (T) required for the crushing.
o While crushing, note down the time (t2) required for 2 revolutions (n2) under loaded
conditions.
o When crushing is completed, stop the stopwatch and turn off the crusher. Note down the
total time required for crushing and the final meter reading (R2).
o Again turn on the crusher and note down the time required for 2 revolutions under un-
loaded conditions. Take the average value of two t1 s.
o Analyze the material by sieving (using preferably 2, 4, 6, 10, 20, 30, 40, 50, 70, and 100
US ASTM mesh sieves) and weigh out the mass retained on each sieve and in the pan.
Activities:

o Repeat the objectives using clay, limestone, rock salt etc. Plot for all on the same
plane.
o Repeat the objectives for (-2” +1”) using all the above materials, and plot results
on the same plane.
o What would be the values of the Kick‟s Law Constant and Rittinger‟s Law
Constant for the jaw crusher-red bricks system and the jaw crusher-clay system
etc?
o Find out the work indices o the materials mentioned above.
o Report the capacity of the crusher.

Observations and Calculations:

Energy:

Total weight of the feed taken = W = ------ kg

No. of revolutions of energy meter for un-loaded conditions = n1 = --------

Time elapsed for “n1” revolutions = t1 = ------- s

No. of revolutions of energy meter for loaded conditions = n2 = --------

Time elapsed for “n2” revolutions = t2= ------- s

Energy meter factor =N= ---------- rev/kWh

Total time of crushing = T = ---------- s

Energy (including energy required to run the equipment) used for crushing one ton material
(E) ,

𝑛1 𝑛1 1000
E= − 𝑇1 ∗ , Kwh/ton
𝑡2 𝑡1 𝑁∗𝑊

Putting values we have

E = ............ Kw/ton
Total energy (including energy required to run the equipment) used for crushing one ton material
=ET

𝑛2 1000
ET = 𝑇2 ∗ 𝑁∗𝑊 , Kwh/ton
𝑡2

Putting value we have

ET = ............ Kw/ton

Alternate method for the measurement of energy required for crushing:

Initial meter reading = R1 =............ Kwh

Final meter reading = R2= .............Kwh
Total energy required = R2 - R1 = ............ Kwh
Total energy required for one ton of material

1000
ET = 𝑅2 − 𝑅3 ∗ =............ Kwh/ton
𝑊
 Distribution of particle size
Table for fractional and cumulative plot

Us Fractional distribution plot Cumulative distribution plot

ASTM
Mesh
Weight Weight Average particle Stated particle Cumulative fraction
retained fraction size size less than stated size
(g) “X” “d” (µm) (µm)
-2 +4
-4 +10
-10 +20
-20 +30
-30
+40
-40 +50
-50 +70
-70 +100
-100
+pan
Note: try also to present the fraction distribution plot on a semi-log graph paper and cumulative
fractional plot on log-log paper

Inferences:
1. Inferences from fractional distribution plot

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2. Inferences from cumulative distribution plot

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Diameters:
1. Bond‟s diameter=𝑑80
From the plot of cumulative fractional less than stated size

𝑑80 =_____ µm=_____ in

Table for the Measurement of Average Diameters
US ASTM Weight Average
Mesh Fraction Practice xd 𝑥 𝑥 𝑥
“X” Size 𝑑 𝑑2 𝑑3
“d” (µm)

-1 +2

-2 +4

-4 +10

-10 +20

-20 +30

-30 +40

-40 +50

-50 +70

-70 +100

-100
+pan
 𝑛 𝑛 𝑛 𝑛
𝑥𝑖 𝑥𝑖 𝑥𝑖
𝑥𝑖 𝑑𝑖 𝑑𝑖 2
𝑑𝑖 𝑑𝑖 3
𝑖=1 𝑖=1 𝑖=1 𝑖=1

= _____ = _____ = _____ = _____

2. Weight (volume) mean diameter =𝑑𝑣 , and

𝑛
𝑑𝑣 = 𝑖=1 𝑥𝑖 𝑑𝑖 = _____µm= _____in
3. Mean Volume Diameter=𝑑𝑣′
1
3
1
𝑑𝑣′ = 𝑛 (𝑥 𝑖 = _____ µm = _____ in
)
𝑖=1 𝑑𝑖 3

4. Surface mean diameter or Sauter mean diameter = 𝑑𝑠 , and

1
𝑑𝑠 = 𝑛 (𝑥 𝑖 = _____ µm = _____ in
𝑖=1 𝑑𝑖 )
5. Length mean diameter = 𝑑𝑙 , and 𝑑𝑠 =
Results:
1. Total energy required for crushing red bricks and running the machine is _____
kWh/ton.
2. Energy required for crushing the red bricks only is _____ kWh/ton.
3. Average particle diameters of product.

Sr. No. Average Diameter (µm) (in)

1. Bond‟s Diameter
2. Weight (volume)
mean diameter
3. Mean Volume
Diameter
4. Surface mean
diameter or
Sauter mean
diameter
5. Length mean
diameter
Discussion:

Precautions:
1. Average size lumps should be used for crushing.
2. The machine should be run at proper voltage.

Industrial Applications:
Jaw crushers can be used in metallurgical industry, mining industry, chemical industry, building
material, highway, railway, water industry and etc. They can be used to crush all kinds of mine
and other massive materials into the granule, for the secondary crushing and the fine crushing.
 Disc Mill

Objectives:
o To report the energy required for crushing one ton of rock salt (-2 +4) using laboratory disc
mill.
o To report the total energy required for crushing one ton of rock salt (-3” +2”) for the same
equipment.
o To report the results of screen analysis, for the product obtained, in the form of cumulative
and fractional distributional plots, and give inferences.
o To report different types of diameters, for the product obtained, such as Bond‟s diameter,
weight(volume) mean diameter, mean volume diameter, surface mean diameter(Sauter
mean diameter), and mean length diameter.
o To report the properties such as bulk density and voidage of the product obtained.

Concept:
The main objective of this experiment is to introduce the concept of grind, cut, shear, shred,
fiberize, and granulate. A disc mill, is a type of crusher that can be used grind, cut, shear, shred,
fiberize, pulverize, granulate, crack, rub, curl, fluff, twist, hull, blend or refine. It works in a
similar manner to the ancient Buhrstone mill in that the feedstock is fed between opposing discs
or plates. The discs may be grooved, separated or spiked.

Theory:
The material to be ground is crushed between two counteracting grinding disks with course
radial toothing on the inside as a result of compressive and sheering stresses. The staged toothing
means that the material is preground in the inner chamber of the grinding disks before being
finely ground in the outer chamber.

The material is gravity fed through a hopper into the center ofstationary grinding disk straight
into the sealed grinding chamber. Here it is taken up by the rotating grinding disk and crushed.
The slow, powerful motor combined with the special form of grinding disks make it possible to
grind even very hard sample materials. The broken and ground material is fed into a collecting
vessel. The gap between the two grinding disks is set from the outside – also during operation –
and determines the fineness of the end product.

Procedure:

o Prepare 0.5 kg of feed (rock salt) of the size that can pass through the 2 mesh sieve and
retains on the 4 mesh sieve.
o Note down the time (t1) required for 2 revolution (n1) of the energy meter disc under un-
loaded conditions. Also note down the energy meter factor (N).
o Note down the initial meter reading (R1) and turn on the crusher. Start feeding crusher
and start the stopwatch simultaneously in order to measure the total time (T) required for
the crushing. Feed the mill gradually and slowly otherwise there is chance of choking of
the mill.
o During the course of crushing, note down the time (t2) required for 2 revolutions (n2)
under loaded conditions.
o When crushing is completed, stop the stopwatch and turn off the crusher. Note down the
total time required for crushing and the final meter reading (R2).
o Again turn on the crusher and note down the time required for 2 revolutions under un-
loaded conditions. Take the average value of two t1 s.
o Analyze the material by screening (using preferably 2, 4, 6, 10, 20, 30, 40, 50, 70, and
100 US ASTM mesh sieves) and weigh out the mass retained on each sieve and in the
pan.
o Mix all the fractions that has retained on each sieve and in the pan.
o Take 100 c𝑚3 of the mixed material in a 500 ml measuring cylinder.
o Weigh out the mass of the 100 c𝑚3 material taken in cylinder and find out the bulk
density of the product.
o Take another 500 ml cylinder and fill it with carbon tetra chloride (CC𝑙4 ) upto 150 c𝑚3 .
Pour the 100 c𝑚3 material into the carbon tetra chloride (contained in the cylinder).
CC𝑙4 ‟s level rises, note down the rise in the volume of the CC𝑙4 and find out the voidage
of the product.
Activities:
1. Repeat the objectives using oil seeds, clay, limestone, red brick, etc. Plot the all on a
same plane.
2. Repeat the objects for (-4 +6) and (-6 +8) using all of the above mentioned materials,
and plot results on the same plane.
3. What would be the values of Kick‟s Law Constant and Rittinger‟s Law Constant for the
disc crusher-red bricks system and of the disc crusher-clay system etc?
4. Find out the work indices of the materials mentioned above.
5. Report the capacity of the crusher.

Observations and Calculations:

Energy:

Total weight of the feed taken = W = _____ kg

No. of revolutions of energy meter for un-loaded conditions= 𝑛1 = _____
Time elapsed for “𝑛1 ” revolutions = 𝑡1 = _____ s
No. of revolutions of energy meter for loaded conditions = 𝑛2 = _____
Time elapsed for “𝑛2 ” revolutions = 𝑡2 = _____ s
Energy meter factor = N = _____ rev/kWh
Total time of crushing = T = _____ s

Energy (excluding energy required to run the equipment) used for crushing one ton (1000
kg) of feed= E, and

𝑛2 𝑛 1 𝑇∗100
E= − , kWh/ton
𝑡2 𝑡1 𝑁∗𝑊

Putting values, we have

 E= _____ kWh/ton

Total energy (including energy required to run the equipment) used for crushing one ton
material = 𝐸𝑇 , and

𝑛 2 𝑇∗100
𝐸𝑇 = , kWh/ton
𝑡2 𝑁∗𝑊
Putting values, we have

𝐸𝑇 = _____ kWh/ton

Alternate method for measurement of the total energy required for crushing:

Initial meter reading = 𝑅1 = _____ kWh

Final meter reading= 𝑅2 = _____ kWh

Total energy required= 𝑅2 - 𝑅1 = _____ kWh

Total energy required for one ton of material

𝑅2 − 𝑅! ∗100
𝐸𝑇 = = _____ kWh/ton
𝑊

Us ASTM Fractional distribution plot Cumulative distribution plot

Mesh
Weight Weight Average Stated particle Cumulative fraction
retained fraction particle size size less than stated size
(g) “X” “d” (µm) (µm)
-2 +4
-4 +10
-10 +20
-20 +30
-30 +40
-40 +50
-50 +70
-70 +100
-100 +pan
 DISTRIBUTION OF PARTICLE SIZE
Table for fractional and cumulative plot

Note: try also to present the fraction distribution plot on a semi-log graph paper and cumulative
fractional plot on log-log paper
Inferences:

1. Inferences from fractional distribution plot

............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
.....................................................................................................................................

2. Inferences from cumulative distribution plot

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Diameters:
1. Bond‟s diameter = d80

From the plot of cumulative fractional less than stated size

d80 = _____ µm = _____ in

Table for the measurement of Average diameters

US Weight Average
ASTM Fraction Particle xd x/d x/d^2 x/d^2
MESH “ x” Size “ d ”
(µm)

∑ (xi ai ∑ ∑ ∑
)=_____ xi/di=_____ xi/di^2=_____ xi/di^3=_____
_____ _____ - --
 2. Weight (Volume ) mean diameter =dv , and

dv= ∑ (xiai)= _____ µm = _____ inch

3. Mean Volume Diameter = d‟v , and

1
1 3 1
d‟v= = ( −−−−)1/3 = _____ - -- µm = _____ inch
(𝑥𝑖 /𝑑𝑖 ^3)

4. Surface mean diameter or Sauter mean diameter =ds. and

1
ds= = ----in=-----µm
(𝑥𝑖 /𝑑𝑖 )

5. Length mean diameter =dl and

−−−−−
dl = ( 𝑥𝑖/𝑑𝑖)/ ( 𝑥𝑖/𝑑𝑖^2) =−−−−− = ______ µm = _______ in

Bulk Properties of the Product:

Bulk Density:
Bulk volume of the bed of material = VB = 100 cm3
Mass of the bed of the material = m _____ - g
B

𝑀𝑎𝑠𝑠 𝑜𝑓 𝑡ℎ𝑒 𝑏𝑒𝑑 𝑚𝐵

Bulk Density= = = _____ -g/cm3
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝐵𝑒𝑑 𝑉𝑅

Voidage (fractional Voidage):

Volume of the bed (of material) taken =VB =100 cm3
Volume of the liquid displaced = _____ - - cm3
As the volume of the liquid displaced = volume of the particles, so
Volume of the particles = Vp= _____ - - cm3
 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑏𝑒𝑑 −𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒𝑠
Fractional Voidage =
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑏𝑒𝑑

𝑉𝐵−𝑉𝑝 100−𝑉𝑝
ɛ= =
𝑉𝐵 100
Results
1-Total energy required for crushing red bricks and running the machine is ------- kWh/ton.
2-Energy required for the crushing the red bricks only is ------ kWh/ton.
3-Average particle diameters of the product.

Sr. No. Average Diameter (um) (in)

1 Bond‟s Diameter

2 Weight (volume) mean diameter

3 Mean volume diameter

4 Surface mean diameter

5 Length mean diameter

4- Bulk density of the product is ------ g/cm3and Voidage of the product is ---------.
Discussions:

Precautions:
1- Pour chemicals into the cylinder carefully.

Industrial Application
Typical applications for a single-disc mill are three stages of the wet milling of field com, manufacture of
peanut-butter, processing nut shells, ammonium nitrate and urea, producing chemical slurries and
recycled paper slurries, and grinding chromium metal.
Double-disc mills are typically used for alloy powders, aluminum chips, bark, barely, borax, brake lining
scrap, brass chips, sodium hydroxide, chemical salts, coconut shells, copper powder, cork , cotton seed
hulls, pharmaceuticals, feathers, hops, leather , oil seed cakes, phosphates, rice, rosin, sawdust, and seeds.
Disc mills are relatively expensive to run and maintain, and are not used where ball mills or hammer mills
produce the desired results at a lower cost.
 High Shear Mill

Objective:
o To report the energy required fir crushing one ton of rock salt (-2 +4) using laboratory
high shear Mill.
o To repot the total energy required for crushing one ton of the rock salt (-2 +4) for the
same equipment.
o To report the results of screen analysis for the product obtained in the form of cumulative
& fractional distributional plots and give inference.
o To report different types of diameters for the product obtained such as bonds diameters
weight (Volume) mean diameter , mean volume diameter , surface mean diameter (sauter
mean diameter) and mean length.
o To report the properties such bulk density and voidage of the product obtained.

Concept:
As experiment No. 1.2

Theory:
As experiment No. 1.2

Procedure:
o Prepare 0.5 kg of feed (rock salt) of the size that can pass through the 2 mesh sieve and
retains on the 4 mesh sieve.
o Note down the time (t1) required for 2 revolutions (n1) of the energy meter disc under un-
loaded conditions. Also note down the energy meter factor (N).
o Note down the initial meter reading (R1) and turn on the crusher. Start feeding crusher
and start the stop watch simultaneously in order to measure the total time (T) required for
the crushing. Feed the mill gradually slowly otherwise there is chance of choking pf the
mill.
o During the course of crushing, note down twice the time (t2) required for the 2
revolutions (n2) under loaded conditions.
 o When crushing is completed, stop the stopwatch and turn off the crusher. Note down the
total time required for crushing and the final meter reading (R2).
o Again turn on the crusher and note down the time required for 2 revolutions under un-
loaded conditions. Take the average value of the two t1s.
o Analyze the material by screening and weigh out the mass retained on each sieve and in
the pan.
o Mix all the fractions that has retained on each sieve and in the pan.
o Take 100 cm3of the mixed material in the 500 ml measuring cylinder.
o Weigh out the mass of the 100 cm3material taken in the cylinder and find out the bulk
density of the product.
o Take another 500 ml cylinder and fill it with carbon tetra chloride CCl4upto 150 cm3.
o Pour the 100 cm3material into the CCl4cylinder its level rises, note down the rise in the
volume of the CCl4and find out the Voidage of the product.

Activities:
o Repeat the objectives using oil seeds, clay, limestone, red brick, etc. Plot the all on a
sample plane.
o Repeat the objects for (-4 +6) and (-6 +8) using all of the above mentioned materials,
and plot results on the same plane.
o What would be the values of kick‟s Law constant and Ratzinger‟s Law constant for the
disc crusher-red bricks system and of the disc crusher-clay system etc?
o Find out the work indices of the materials mentioned above.
o Report the capacity of the crusher.

Observation and Calculations

Energy Calculations

Total weight of the feed taken=W= -------- kg

No. of the revolutions of energy meter fir un-loaded conditions = n1 = -------
Time elapsed for n1revolutions = t1 = -------- s
 Time elapsed for n2revolutions= t2 = -------- s
Energy meter factor =N= -------- rev/kWh
Total time of crushing = T = ---------- s
Energy (excluding energy required to run the equipment) used for crushing one ton
(1000kg) of feed = E, and

𝑛1 𝑛1 1000
E= − 𝑇1 ∗ , Kwh/ton
𝑡2 𝑡1 𝑁∗𝑊

Putting values we have

E = ............ KWh/ton
Total energy (including energy required to run the equipment ) used for crushing one ton
material =ET and
𝑛2 1000
ET =
𝑡2
𝑇2 ∗ 𝑁∗𝑊 , Kwh/ton

Putting value we have

ET =............ Kw/ton
Alternate method for the measurement of energy required for crushing :
Initial metere reading = R1 = ............ Kwh
Final meter reading = R2= .............Kwh
Total energy required = R2 - R1 = ............ Kwh
Total energy required for one ton of material

1000
ET = 𝑅2 − 𝑅3 ∗ = ............ Kwh/ton
𝑊
 DISTRIBUTION OF PARTICLE SIZE
Table for fractional and cumulative plot

Us ASTM Fractional distribution plot Cumulative distribution plot

Mesh
Weight Weight Average particle Stated particle Cumulative fraction
retained fraction size size less than stated size
(g) “X” “d” (µm) (µm)
-2 +4
-4 +10
-10 +20
-20 +30
-30
+40
-40 +50
-50 +70
-70 +100
-100 +pan
Note: try also to present the fraction distribution plot on a semi-log graph paper and cumulative
fractional plot on log-log paper
Inferences:
1. Inferences from fractional distribution plot

............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
.....................................................................................................................................

2. Inferences from cumulative distribution plot

............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
............................................................................................................................................................
...............................................................................................
Diameters:
1. Bond‟s diameter = d80

From the plot of cumulative fractional less than stated size

d80 = _____ µm = _____ in
Table for the measurement of Average diameters

US ASTM Weight Average

MESH Fraction Particle xd x/d x/d^2 x/d^2
“ x” Size “ d
” (µm)

∑ (xi*ai ) = ∑ xi/di= ∑ xi/di2= ∑ xi/di3=

2. Weight (Volume ) mean diameter =dv , and

dv = ∑ (xi * ai)= __________ µm = _________inch

3. Mean Volume Diameter = d‟v , and

 1
1 3 1
d‟v= = ( −−−−)1/3 = _____ - -- µm = _____ inch
(𝑥𝑖 /𝑑𝑖 ^3)

4. Surface mean diameter or Sauter mean diameter =ds. and

1
ds= = ----in=-----µm
(𝑥𝑖 /𝑑𝑖 )

5. Length mean diameter =dl and

−−−−−
dl = ( 𝑥𝑖/𝑑𝑖)/ ( 𝑥𝑖/𝑑𝑖^2) =−−−−− = ---µm = ---in

Bulk Properties of the Product:

Bulk Denity:
Bulk volume of the bed of material =VB= 100 cm3

Bulk volume of the bed of material = VB = 100 cm3

Mass of the bed of the material = m _____ - g
B
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑡ℎ𝑒 𝑏𝑒𝑑 𝑚𝐵
Bulk Density=𝑉𝑜𝑙𝑢𝑚𝑒 = = _____ -g/cm3
𝑜𝑓 𝑡ℎ𝑒 𝐵𝑒𝑑 𝑉𝑅

Voidage (fractional Voidage):

Volume of the bed (of material) taken =VB =100 cm3

Volume of the liquid displaced = _____ - - cm3
As the volume of the liquid displaced = volume of the particles, so
Volume of the particles = Vp= _____ - - cm3

𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑏𝑒𝑑 −𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒𝑠

Fractional Voidage =
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑏𝑒𝑑
 𝑉𝐵−𝑉𝑝 100−𝑉𝑝
ɛ= =
𝑉𝐵 100

Results
1-Total energy required for crushing red bricks and running the machine is ------- kWh/ton.

2-Energy required for the crushing the red bricks only is ------ kWh/ton.
3-Average particle diameters of the product.

Sr.No. Average Diameter (um) (in)

1 Bond‟s Diameter

2 Weight (volume) mean diameter

3 Mean volume diameter

4 Surface mean diameter

5 Length mean diameter

4- Bulk density of the product is ------ g/cm3and voidage of the product is ---------.
Discussions:

Precautions:
1- Pour chemicals into the cylinder carefully.

Industrial Application

Typical applications for a single-disc mill are three stages of the wet milling of field com,
manufacture of peanut-butter, processing nut shells, ammonium nitrate and urea, producing
chemical slurries and recycled paper slurries, and grinding chromium metal.
 Sieves and Dies
Objectives:

o To enlarge the size of given material (powder) using sieves and dies.
o To find the total time to dry the product.
o To find the bulk properties of the product.

Concept:

There are four different standards of screens. They are B.S (British Standards) screens and are
made in sizes from 300-mesh upwards. I.M.M. (Institute of Mining and Metallurgy) screens are
robust (hard) as the size of the wire that is used to manufacture the screen is equal to the size of
aperture.

Theory:

Particle size can be measured in different ways. There are different techniques to measure the
article size, for example microscopic analysis and sedimentation or elutriation etc. Sieving is one
of the simplest techniques to measure the particle size.

In sieve analysis, we used a nest of sieves one upon the other. The sieve with the largest aperture
size is placed on the top and with the smallest aperture size is placed at the bottom of the set of
screens. Sieves are arranged in such a way that the ratio of the aperture size on consecutive
screens also called screen interval is 2, 21/2 or 21/4according to the closeness of the size required.
Sieves can be shaken mechanically or by hand. All the material is placed on the top screen and
then vibrated or shaken so that the material which is of lower size than the aperture size of the
top most screen falls on the lower screen and so on. The finest size is therefore obtained at the
bottom. The number of holes in one linear inch of screen is called mesh number of the screen. It
means, if there are 20 holes in one linear inch of the screen, its mesh number is 20.

Screen efficiency is defined as the ratio of the weight of the material which passes the screen to
that which is capable of passing. It may be assumed that the rate of passage of a given size
through the screen is proportionalto the weight of the particles of that size on the screen at any
given time. It means, if w is the mass of particles of a particular size on the screen at a time t.
mathematically,
 𝒅𝒘
= −𝒌𝒘
𝒅𝒕

Where negative sign indicates that the mass on the screen decreases as the time passes and
between different time intervals t1 and t2, we have

𝒘𝟐
𝒍𝒏 = −𝒌𝒕
𝒘𝟏

𝒘𝟐 = 𝒘𝟏 𝒆−𝒌𝒕

Procedure:

o Take 100 g of powdered red bricks (of -150+200 size) and mix it with water to form a
paste.
o Place the paste on the die and use a scraper to fill the die holes using the scraper.
o Draw the pellets of red bricks form the die holes and place on a steel plate.
o Place the steel plate in the oven at a suitable temperature.
o Take out the plate from oven and weigh it after every 2 minutes.
o Note down the total time of drying when three constant weighs of the plate are obtained.
o Mix all the pellets and take 100 cm3 of the material in a 500 ml measuring cylinder.
o Weigh out the mass of the 100 cm3 material taken in the cylinder and calculate theBulk
density of the product

Take another 500ml cylinder and fill it with water upto 150 cm3 . pour the 100 cm3 material
into the water (contained in the cylinder ). Water level rises , note down the rise into volume of
water and findout the voidage of product.
 OBSERVATION AND CALCULATION

Total weight of th powder taken =W1=100g = 1kg

Temperature of the oven =To=_______oC
Total time of drying =Tdry= _______min

Table to find the total time of drying

sr. no Time elapsed Weight of steel plate with

pellets
1.
2.
3.
4.
5.
6.
7.

Volume of the bed (of material) taken =VB =100 cm3

Volume of the liquid displaced = _____ - - cm3
As the volume of the liquid displaced = volume of the particles, so
Volume of the particles = Vp= _____ - - cm3

𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑏𝑒𝑑 −𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑝𝑎𝑟𝑡𝑖𝑐𝑙𝑒𝑠

Fractional Voidage =
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑏𝑒𝑑

𝑉𝐵−𝑉𝑝 100−𝑉𝑝
ɛ= =
𝑉𝐵 100
Discussion:

Precaution:
1. Measure the material carefully
2. Set appropriate temperature of drying

Industrial application:
Food industry, cosmetics
 Kneader Mixer for Dry Solids

Objectives:

o To find out the energy required to mix (blend) one ton of sand and sodium carbonate
(Na2CO3) in the ratio 10:1 using laboratory kneader mixer used for flowing solids(dry
Solids).
o To find out the total energy required for the case mentioned above.
o To find out the total time of mixing and show it graphically.

Concept:

Kneading is a method of mixing used with deformable or plastic solids. It involves squashing the
mass flat, folding it over on itself and squashing it once more. Most kneading machines also tear
mass apart and shear it between the moving blades and stationary surface.

Theory:

A two arm kneader hands suspensions, pastes and light plastic masses. Typical applications are
in compounding of lacquer bases from pigments and carriers and in shedding cotton linters into
acetic acid and acetic anhydride. Material to be kneaded is dropped into through and mixed for 5
to 20 minutes or longer. Sometimes mass is heated in machine but mostly it must be cooled to
remove the heat generated by mixing action. The designs of mixing blade vary with purpose of
mixing. The common sigma blade is used for general-purpose kneading.

In many kneading machines the trough is open from where material is dropped for kneading. In
some designs mixing chamber is closed during operating cycle with a cover, such kneaders are
called internal kneaders. These are also called continuous kneader. Continuous kneaders have
been developed that can handle light to fairly heavy material. The heat generated in the material
is removed by cooling water sprayed on the walls of mixing chamber and circulated through
hollow agitator shafts.
Procedure:

o Take 300 g of dry sand of the size -30 mesh.

o Take 300 g of sodium carbonate of the size -30 mesh.
o Note down the time (t1) required for 2 revolutions (n1) of the energy meter disc under un-
loaded conditions. Also note down the energy meter factor (N).
o Charge the cleaned and dried mixer with 3000 g sand.
o Place 300 g of sodium carbonate gently over the sand.
o Place a covering (paper or some card board) on the mixer to avoid dust losses.
o Note down the initial meter reading (R1) and turn on the mixer. Start the stop watch
simultaneously in order to measure the total time (T) required for mixing.
o After 2 minutes of total time, turn off the machine and take 2 g sample from the mixer.
o Try to dissolve the sample taken in 50 ml of distilled water present in titration flask. Sand
will settle down and sodium carbonate be dissolved in the water.
o Using methyl orange as indicator and N/10 HCL as titrant, titrate the solution with
constant shaking of the flask.
o Note down the volume used of the HCl when light pink (to red) end point appears.
o Repeat the above experiment i.e. take samples from the mixer after every two minutes
and titrate them against N/10 HCl. Also note down the meter reading (R2) after each two
minutes of machine‟s working.
o During the course of the practical try to note down twice the time (t1) required for 2
revolutions (n2) under loaded conditions. Take the average value of the two t2s.
o Take the average of these two values.
o When three consecutive readings of volume used of HCL are same, stop the mixer for
further analysis.
o Empty the mixer and note down the time (t1) required for two revolutions (n1) of the
energy meter disc under unloaded conditions. Take the average value of two t1s.
Activities:

 Repeat the given objectives using different materials,(say), sand and CaCO3, Clay and
CaCO3, etc.
 Report the results of different systems on the same plane.
 Report the given objectives for different feed ratios, (say), 1:1, 1:3, and 8:1. Plot all the
results on the same plane.
 Repeat the objectives for different mesh sizes of both components, and see the effect of
particle sizes of components on the objective.

Observations & Calculations

Energy and mixing time:

Total weight of the sand taken = W1 = 3000 g = 3 Kg

Total weight of sodium carbonate taken = W2 = 300 g = .30 Kg

Total weight of both the sand & sodium carbonate taken = W = W1 + W2 = 3.3 Kg

No. of revolutions of energy meter for un-loaded conditions = n1 = ------------

Time elapsed for “n1” revolutions = t1 = ------------ s

No. of revolutions of energy meter for loaded conditions = n2 =--------------

Time elapsed for “n2” revolutions = t2 = ------------ s

Energy meter factor = N = -------- rev/kWh

Total time of mixing = T = T mix

 Table for finding Mixing Time

No. of Mixing IBR FBR Volume of Meter

Observations Time (ml) (ml) HCL used reading
(min) (ml) (kWh)
1 0 ----- R1
2 2 V1 .
3 4 V2 .
4 . . .
5 . . .
6 T mix V R2
7 T mix + 2 V .
8 T mix +4 V .

Total time of Mixing = T = T mix = _________ min = ________ s

Graph that shows the required mixing time

Energy (including energy required to run the equipment ) used for crushing one ton material=E ,
and
𝑛1 𝑛1 1000
E= − 𝑇1 ∗ , Kwh/ton
𝑡2 𝑡1 𝑁∗𝑊

Putting values we have;

E= ............ Kw/ton

Total energy (including energy required to run the equipment ) used for crushing one ton
material =ET and
𝑛2 1000
ET = 𝑇2 ∗ , Kwh/ton
𝑡2 𝑁∗𝑊

Putting value we have

ET =............ Kw/ton
Alternate method for the measurement of energy required for crushing :
Initial metere reading = R1 = ............ Kwh
Final meter reading = R2= .............Kwh
Total energy required = R2 - R1 = ............ Kwh
Total energy required for one ton of material

1000
ET = 𝑅2 − 𝑅3 ∗ = ............ Kwh/ton
𝑊
Results:

Energy required to mix one ton of material in the ratio 10:1 ___________kwh

Total energy required to mix one ton of material in the ratio 10:1 is________ kwh.

Total mixing time _________min

Discussion:

Precautions:

1. Material charged to kneader must be bone dry.

2. Material should be mixed in proper ratio.

Industrial applications:

Plastic industry.
 Kneader Mixer for Pastes

Objectives:
o To find out the energy required to mix (blend) one ton of clay and sodium carbonate
(Na2CO3) in the ratio 5:1 using laboratory kneader mixer used for cohesive solids (or paste-
mixing).
o To find out the total energy required for the case mentioned above.
o To find out the total time of mixing and show it graphically.

Concept:
Kneading is a method of mixing used with deformable or plastic solids. It involves squashing the
mass flat, folding it over on itself and squashing it once more. Most kneading machines also tear
the mass apart and shear it between the moving blades and stationary surface.

Theory:
A two arm kneader handles suspensions, pastes and light plastic masses. Typical applications are
in compounding of lacquer bases from pigments and carriers and in shedding cotton linters into
acetic acid and acetic anhydride. Material to be kneaded is dropped into trough and mixed for 5
to 20 minutes or longer. Sometimes mass is heated in the machine but mostly it must be cooled
to remove heat generate by mixing action. The designs of mixing blade vary with purpose of
mixing. The common sigma blade is used for general-purpose kneading.

In many kneading machines the trough is open from where material is dropped for kneading. In
some designs mixing chamber is closed during operating cycle with a cover, such kneaders are
called internal kneaders. These are also called continuous kneader. Continuous kneaders have
been developed that can handle light to fairly heavy material. The heat generated in the material
is removed by cooling water sprayed on the walls of mixing chamber and circulated through
hollow agitator shafts.
Procedure:

o Take 1000 g of dry clay of the size -30 mesh.

o Take 200 g of sodium carbonate of the size -30 mesh.
o Note down the time (t1) required for 2 revolutions (n1) of the energy meter disc under un-
loaded conditions. Also note down the energy meter factor (N).
o Charge the cleaned and dried mixer with 1000 g clay.
o Add suitable quantity of water to clay (preferably using cylinder so that the volume and
hence mass of the water can be measured) in order to form paste of the material.
o Place 200 g of sodium carbonate gently over the clay.
o Note down the initial meter reading (R1), and turn on the mixer. Start the stop watch
simultaneously in order to measure the total time (T) required for the mixing.
o If required, pour further (measured) quantity of water into the mixer to make a proper
paste.
o After 2 minutes of total time, turn off the machine and take 2 g sample (in a watch glass)
from the mixer.
o Try to dissolve the sample taken in 50 ml of distilled water present in a titration flask.
Sand will settle down and sodium carbonate be dissolved in the water.
o Using methyl orange as an indicator and N/10 HCl, titrate the sodium with constant
shaking of the flask.
o Note down the volume used of the HCl when light pink (to red) end point appears.
 Observations and Calculations

 No. of revolutions of energy meter for un-loaded conditions = n1 = _________

 Time elapsed for “n1” revolutions = t1 = ------------ s
 No. of revolutions of energy meter for loaded conditions = n2 =--------------
 Time elapsed for “n2” revolutions = t2 = ------------ s
 Energy meter factor = N = -------- rev/kWh

Total time of mixing = T = T mix

Table for finding Mixing Time

No. of Mixing IBR FBR Volume of Meter

Observations Time (ml) (ml) HCL used reading
(min) (ml) (kWh)
1 0 ----- R1
2 2 V1 .
3 4 V2 .
4 . . .
5 . . .
6 T mix V R2
7 T mix + 2 V .
8 T mix +4 V .

Total time of Mixing = T = T mix = ------ min = ------- s

Graph that shows the required mixing time

Energy (including energy required to run the equipment ) used for crushing one ton material=E ,
and
𝑛1 𝑛1 1000
E= − 𝑇1 ∗ , Kwh/ton
𝑡2 𝑡1 𝑁∗𝑊

Putting values we have

E= ............ Kw/ton

Total energy (including energy required to run the equipment ) used for crushing one ton
material =ET and
𝑛2 1000
ET = 𝑇2 ∗ , Kwh/ton
𝑡2 𝑁∗𝑊
Putting value we have
ET =............ Kw/ton
Alternate method for the measurement of energy required for crushing :
Initial metere reading = R1 = ............ Kwh
Final meter reading = R2= .............Kwh
Total energy required = R2 - R1 = ............ Kwh
Total energy required for one ton of material

1000
ET = 𝑅2 − 𝑅3 ∗ = ............ Kwh/ton
𝑊

Results:
Energy required to mix one ton of material in the ratio 5:1 -------------- kwh
Total energy required to mix one ton of material in the ratio 5:1 is ---------- kwh.
Total mixing time -------------- min

Discussion:

Precautions:
1. Material charged to kneader must be bone dry.
2. Material should be mixed in proper ratio.

Industrial applications:
Plastic industry, Food industry, Pharmaceuticals etc.
 Oil Extractor

Objectives:

o To report the required to extract one ton of oil from the given feed using a laboratory oil
extractor.
o To report the total energy to extract one ton of oil from the given seed using a laboratory
oil extractor.
o To report the results of screen analysis, for the product obtained, in the form of cumulative
and fractional distributional, and give inferences.
o To report the different types of diameters , for the product obtained, such as Bond‟s
diameter , weight (Volume) mean diameter, surface mean diameter ( sauter mean
diameter), and mean length diameter.

Concept:

Oil is extracted from a number of fruits, nuts and seeds (Table 1) for use in cooking and soap
making1 or as ingredient in other foods such as baked or fried goods. Oil is a valuable product
with universal demand, and possible income from oil extraction is therefore often enough to
justify the relatively high cost of setting up and running a small scale oil milling business.

Theory:

Oil can be extracted by pressing softer oil seeds and nuts, such as groundnuts and shell nuts,
whereas harder, more fibrous materials such as copra and sun flowers seed are processed using
ghanis. Pulped or ground material is loaded into a manual or hydraulic press to squeeze out the
water emulsion. This is more efficient at removing oil than traditional hand squeezing, allowing
higher production rates. Presses have a number of different designs, which can be grouped into
screw or hydraulic operations. Both types can be manual or motor driven. In all types, a batch of
raw materials is placed in a heavy duty perforated metal „cage‟ and pressed by the movement of
a heavy metal plunger. The amount of the material in the cage varies from 5-30 kg with an avg.
of 20 Kg. layer plates can be used in larger cages to reduce the thickness of the layer of raw
materials and speed up removal of oil. The pressure should be increased slowly to allow the time
for the oil to escape. Screw types are more reliable than hydraulic types but are slower and
produce less pressure. Except where a lorry jack is used , hydraulic types are more expensive,
need more maintenance , and risk contaminating oil with poisonous hydraulic fluids.

Procedure:

o Prepare 10 kg of feed with the given feed and moist it with water.
o Note down the time (t1) required for 2 revolutions (n1) of the energy meter disc under
un-loaded conditions. Also note down the energy meter factor (N).
o Note down the initial meter reading (R1) and turn on the crusher. Start introducing the
feed into the extractor and start the stop watch simultaneously in order to measure the
total time (T) required for crushing.
o During the course of crushing, note down the time (t2) required for 2 revolutions (n2)
under loaded conditions. If possible try to note down twice the time (t2) required for 2
revolutions (n2) under loaded conditions.
o When extraction is complete, pass the crushed seed again from the extractor unless no oil
is obtained from the seed.
o Note down the total time required for extraction and final meter reading (R2).
 o Again turn on the extractor and note down the time required for 2 revolutions under un-
loaded conditions. Take the average values of thee two t1s.
o Analyze the material by sieveing (preferably using 6, 8, 10, 20, 30, 40, 50, 70 and 100 US
ASTM mesh sizes) and weight out the mass retained on each sieve and in the pan.
o Mix all the material that has retained on6, 8, 10, 20, 30, 40, 50, 70 and 100 mesh sieves
and in the pan and take 100 cm3 of the material in 500 ml measuring cylinder.
o Weight out the mass of 100 cm3 material taken in the cylinder and calculate bulk density
of product.
o Take another 500 ml cylinder and fill it with water up to 150 cm3. Pour the 100 cm3
material into the water up to 150 cm3. Pour the 100 cm3 material into the water
(contained in cylinder). Water level rises, note down the rise in volume of water and find
out the void age of the product.

Observations and calculations

Extraction:

Weight of seed taken = W1 = ------ Kg

Weight of oil extracted = W2= ------ Kg
Percentage of oil present in the seed = w2/w1 * 100
Results:

Discussion:

Precaution:

 Weigh the raw material carefully.

 Make sure there would be no voltage fluctuation to avoid error.

Industrial Application:

 Many vegetable oils are used to make soaps, skin products. Candles, perfumes and other
personal care and cosmetic products.
 Some oils are particularly suitable as drying agents, and are used in making paints and
other wood treatment products. Dammar oil ( a mixture of linseed oil and dammar resin),
for example, is used almost exclusively in treating the hulls of wooden boats.
 Vegetable oils are increasingly being used in the electrical industry as insulators as
vegetable oils are non- toxic to environment, biodegradable if spilled and have high flash
and fire points.
 Fractional crystallization

Objectives:
1: To report the percentage yield of sodium nitrate obtained from a mixture of sodium chloride
and sodium nitrate using fractional crystallization techniques.

2: To report the result of screen analysis, for the product obtained, in the form of cumulative and
fractional distributional plots, and give interferences.

3: To repot different types of diameters, for the product obtained, such as bond‟s diameter,
volume mean diameter, surface mean diameter, sautermean diameter, length mean diameter (or
arithmetic diameter), and weight mean diameter.

4: To report the properties such as bulk density and voids of the product obtained.

Concept:
Fractional crystallization is one of the most important geochemical and physical process
operating with in earth‟s crust and mental. Fractional crystallization is the removal and
segregation from of melt of mineralprecipitate; except in special cases removal of the crystal
changes the composition of the magma. Fractional crystallization in silicates melts (magma‟s) is
complex compare to crystallization in chemical system at constant pressure and composition
because changes in pressure and composition can have dramatic effect on magmaevaluation.
Addition and loss of water, carbon dioxide, hydrogen and oxygen are among the compositional
changes that must be considered.

Theory:
Fractional crystallization is that technique which enables an industry to separate one solid from
the other in this technique two different solids are dissolved in water and a saturated solution at
the boiling point of water is made. The solution is then cooled to the room temperature. At high
temperatures, the solubility of a single component increases in a solvent. When there are two
solid components, th e solubility of the substance which has more affinity with water increases
considerably while the solubility of the other solid component increased slowly. When the
solution is to room temperature the more soluble compound crystallizes at lower temperature the
solubility of solid is less. The the other component remains in solution. This solution is the
filtered and the crystals obtained are dried and hence the separation is achieved.

The technique requires the availability of solubility data of both single components as well as the
solubility data of both compounds(when dissolved simultaneously) in saturated states. From this
data we can find the theoretical amounts of the solid crystallized and can compare with the
practical values. This way we can find the percentage yield of crystals.

Procedure:
o Take 100 g of water in a beaker
o Weigh out the system including thermometer at this stage
o Place the beaker on the Bunsen burner and start heating the system
o Try to dissolve 160 g of sodium nitrate and 17 g of sodium chloride in the 100 g of water
with constant stirring.
o Heat the mixture upto 100 oC and make saturated solution w.r.t both salts.
o When the temperature reaches 100 oC ,stop heating and allow the solution to cool upto
the room temperature.
o Weight out the system again at this stage and add make up water that has been lost during
the course of experimentation
o Filter off the mass of crystals obtained and dry the contents (residue) in the oven at 70 oC.
o Weigh out the mass of the crystals obtained.
o Analyze the material by sieving (preferably using 8, 10, 20, 30, 40, 50, 70 and 100
USASTM mesh sieves ) and weight out the mass retained on each sieve and in the pan.
o Mix all the fractions that has retained on each sieve and in the pan.
o Take 80 cm3 of the mixed material in a 50 ml measuring cylinder.
o Weight out the mass of 80 cm3material taken in the cylinder and find out the bulk density
of the product.
o Take another 500 ml cylinder and fill it with carbon tetra chloride (ccl4) upto 150 cm3
.pour the 80 cm3 material into the carbon tetra chloride( contained into the cylinder
CCl4‟s level rises, note down the rise in the volume of the in the volume of the ccl4 and
find out the voidage of the product.
 Observation and calculations

Percentage (%) yield:

At 100oC ,
Wt. of the sodium chloride taken =Wse = 17g
Wt. of the sodium nitrate taken = Wsn =160 g
Temperature of cooling = TR = --- g
Weight of the crystal obtained = w1 = ---g
Practical yield = w1 =---g
Theoretical yield = w2 =________(from the fig.15.10,p.675)

𝑝𝑟𝑎𝑐𝑡𝑖𝑐𝑎𝑙 𝑦𝑒𝑖𝑙𝑑
%age yield = x 100
𝑡ℎ𝑒𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑒𝑖𝑙𝑑

𝑊1
%age yield =𝑊2 x 100 = -----
 *Coulson, J.M et al.:Coulson and Richardson chemical engineering ,
vol.2,4thed.,Butterworth-Hienemann, 1991.

DISTRIBUTION OF PARTICLE SIZE

Us ASTM Fractional distribution plot Cumulative distribution plot

Mesh
Weight Weight Average particle Stated particle Cumulative fraction
retained fraction size size less than stated size
(g) “X” “d” (µm) (µm)
-2 +4
-4 +10
-10 +20
-20 +30
-30
+40
-40 +50
-50 +70
-70 +100
-100 +pan

Table for fractional and cumulative plot

Note: try also to present the fraction distribution plot on a semi-log graph paper and cumulative
fractional plot on log-log paper.

Inferences:
3. Inferences from fractional distribution plot

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4. Inferences from cumulative distribution plot

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Diameters:

2. Bond‟s diameter = d80

From the plot of cumulative fractional less than stated size

d80 = _____ µm = _____ in

Table for the measurement of Average diameters

US Weight Average
ASTM Fraction Particle xd x/d x/d^2 x/d^2
MESH “ x” Size “ d ”
(µm)

∑ (xi ai ∑ ∑ ∑
)=_____ xi/di=_____ xi/di^2=_____ xi/di^3=_____
_____ _____ - --

6. Weight (Volume ) mean diameter =dv , and

dv= ∑ (xi ai)= _____ µm = _____ inch

7. Mean Volume Diameter = d‟v , and

1
1 3 1
dv = = ( −−−−)1/3 = _____ µm = _____ inch
(𝑥𝑖 /𝑑𝑖 ^3)
 8. Surface mean diameter or Sauter mean diameter = ds. and

1
ds= = ----in=-----µm
(𝑥𝑖 /𝑑𝑖)

9. Length mean diameter =dl and

−−−−−
dl = ( 𝑥𝑖/𝑑𝑖)/ ( 𝑥𝑖/𝑑𝑖^2) =−−−−− = __________µm = ________in

Bulk Properties of the Product:

Bulk Denity:

Bulk volume of the bed of material = VB = 100 cm3

Mass of the bed of the material = m _____ g

B

𝑀𝑎𝑠𝑠 𝑜𝑓 𝑡ℎ𝑒 𝑏𝑒𝑑 𝑚𝐵

Bulk Density= = = _____ g/cm3
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝐵𝑒𝑑 𝑉𝑅
 Author Notes

Text Book:

 McCabe Warren L., Smith Julian C., Harriott peter “Unit Operations of chemical
Engineering” 6th Ed. 2001. McGraw Hill Inc

Reference Books:

 White, F.M. “Fluid Mechanics”, 4th Edition, McGraw-Hill. 1999.

 “Unit Operation of Chemical Engineering”, VoL.I by P. Chattopadhyay
 Richardson J.F. “Chemical Engineering” Vol-I, 1985. The English Book Society
and Pergamon Press.