RAJALAKSHMI ENGINEERING COLLEGE

(AN AUTONOMOUS)
Affiliated To Anna University, Chennai-602105

DEPARTMENT OF
CHEMICAL
ENGINEERING
DEPARTMENT OF CHEMICAL
ENGINEERING CH23621 - MASS TRANSFER
CH23621
LABORATORY LABORATORY MANUAL
B.TECH CHEMICAL ENGINEERING
MASS TRANSFER
R2023

LABORATORY MANUAL

0
 RAJALAKSHMI ENGINEERING COLLEGE

DEPARTMENT OF CHEMICAL ENGINEERING

VISION OF INSTITUTION

To be an institution of excellence in Engineering, Technology and Management Education &

Research. To provide competent and ethical professionals with a concern for society.

MISSION OF INSTITUTION

i. To impart quality technical education imbibed with proficiency and humane values.
ii. To provide right ambience and opportunities for the students to develop into
creative, talented and globally competent professionals.
iii. To promote research and development in technology and management for the benefit
of the society.

VISION OF DEPARTMENT

To be a center of excellence in chemical engineering to provide well prepared professionals to

the industries and society.

MISSION OF DEPARTMENT

i. To provide state of art environment to the students for better learning to cater for
the chemical industries and pursue higher studies.
ii. To provide space to the students in research to think, create and innovate things.

PEOs
I. To produce employable graduates with the knowledge and competency in Chemical
Engineering complemented by the appropriate skills and attributes.
II. To produce creative and innovative graduates with design and soft skills to carry out
various problem solving tasks.
III. To enable the students to work as teams on multidisciplinary projects with effective
communication skills, individual, supportive and leadership qualities with the right
attitudes and ethics.
IV. To produce graduates who possess interest in research and lifelong learning, as well as
continuously striving for the forefront of technology.

Chemical Engineering CH23621 1

 PROGRAM OUTCOMES (POS)

Engineering Graduates will be able to

1. Engineering Knowledge:
Apply the knowledge of mathematics, science, and engineering fundamentals, to solve the complex
chemical engineering problems

2. Problem analysis:
Identify, formulate, review research literature, and analyze complex chemical engineering problems
reaching substantiated conclusions using first principles of mathematics, natural sciences and
engineering sciences.

3. Design/development of solutions:
Design solutions for complex chemical engineering problems and design system components or
process that meet the specified needs with appropriate consideration for the public health and
safety, and the cultural, societal and environmental considerations.

4. Conduct investigations of complex problems:

Use research based knowledge and research methods including design of experiments, analysis and
interpretation of data, and synthesis of the information to proceed valid conclusions.

5. Modern tool usage:

Create, select and apply appropriate techniques, resources and modern engineering and IT tools
including prediction and modeling to complex chemical engineering activities with an
understanding of the limitations.

6. The engineer and society:

Apply reasoning informed by the contextual knowledge to assess societal, health, safety, legal and
cultural issues and the consequent responsibilities relevant to the professional chemical
engineering practice.
7. Environment and sustainability:
Understand the impact of the professional chemical engineering solutions in societal and
environmental contexts, and demonstrate the knowledge of and need for sustainable
development.

Chemical Engineering CH23621 2

8. Ethics:
Apply ethical principles and commit to professional ethics and responsibilities and norms of the
chemical engineering practice.

9. Individual and team work:

Function effectively as an individual and as a member or leader in diverse teams, and in
multidisciplinary settings.

10. Communication:
Communicate effectively on complex chemical engineering activities with the engineering
community and with society at large, such as, being able to comprehend and write effective
reports and design documentation, make effective presentations, and give and receive clear
instructions.

11. Project management and finance:

Demonstrate knowledge and understanding of the engineering and management principles and
apply these to one’s own work, as a member and leader in a team, to manage projects and in
multidisciplinary environments.

12. Life-long learning:

Recognize the need for, and have the preparation and ability to engage in independent and life-
long learning in the broadest context of technological changes in chemical engineering.

PSO:

1. Graduates will be able to apply chemical engineering principles to design equipment and
a process plant.

2. They will be able to control and analyse chemical, physical and biological
processes including the hazards associated with these processes.

3. Will be able to develop mathematical models of real world industrial problems and
compute solutions to dynamic processes

Chemical Engineering CH23621 3

 RAJALAKSHMI ENGINEERING COLLEGE

DEPARTMENT OF CHEMICAL ENGINEERING

MASS TRANSFER LABORATORY LTPC

0 0 4 2
COURSE OBJECTIVES:

 To train the students to develop knowledge on different types of mass transfer equipment.

 To perform the rate studies of different types of dryers

 To train on understanding the parameters in different types of column like

absorption, distillation and packed bed distillation.

 To emphasis on the concept on stage wise performance on extraction and leaching

 To carry out the adsorption studies

LIST OF EXPERIMENTS

1. Separation of binary mixture using Simple Distillation

2. Separation of binary mixture using Steam Distillation

3. Separation of binary mixture using Packed Column Distillation

4. Liquid-Liquid Extraction

5. Drying characteristics of Vacuum Dryer

6. Drying characteristics of Tray Dryer

7. Drying characteristics of Rotary Dryer

8. Water purification using Ion Exchange Columns

9. Estimation of mass/heat transfer coefficient for cooling tower

10. Demonstration of Gas – Liquid Absorption

11. Vapor liquid Equilibrium

TOTAL: 60 PERIODS

Chemical Engineering CH23621 4

COURSE OUTCOMES

 Identify and apply the data for separation process using different distillation method

 Understand and apply the data for the given binary mixture in the liquid extraction process

 Apply and interpret the data for different dryer types

 Apply and infer the parameters for separation process using different process

equipment’s like ion exchange and cooling tower.

 Illustrate the data for the absorption phenomena

CO PO PSO MAPPING

PO
CO
1 2 3 4 5 6 7 8 9 10 11 12
1 3 3 3 2 1 2 2 3 3 3 2 2
2 3 2 2 2 1 2 2 2 2 2 1 2
3 3 2 1 2 2 1 3 1 2 1 2 2
4 3 2 2 2 3 2 2 1 2 1 1 2
5 3 1 1 2 2 1 2 1 1 1 1 2

CO PSO MAPPING

PSO
CO
1 2 3
1 3 2 3
2 3 2 3
3 3 1 2
4 3 1 2
5 3 2 3

REFERENCES:

1. Lab Manual
2. Treybal, R.H., “Mass-Transfer Operations”, 3rd ed., McGraw-Hill, NY, 1981, Page 70-72.
3. Coulson & Richardson’s, “Chemical Engineering”, Vol-2, 4thed, Asian Books Pvt.
Ltd, ND,
1998, Page539-542.

Chemical Engineering CH23621 5

 RAJALAKSHMI ENGINEERING COLLEGE

DEPARTMENT OF CHEMICAL ENGINEERING

MASS TRANSFER LABORATORY

DOs and DONTs in the Laboratory

• Before coming to the laboratory, understand the theory behind the experiment that you are
going to carry out.
• Keep the work - bench and sink neat and clean. Don’t allow filter paper, broken bits of
glass, sticks of matches etc., to lie on the table or in sink. Put these things in the dustbin
placed at the worktable.
• Apparatus should be in non-greasy condition.
• Keep the apparatus clean and properly arranged on the work - bench.
• If any piece of apparatus is broken, report at once to the staff members / Lab Assistant.
• Once you have transferred a reagent from a reagent bottle, never pour it back even if there is
some excess.
• Arrange reagent bottles in their proper places after use and see that they are properly
stoppered.
• Handle reagent bottles / chemicals carefully.
• Use only minimum possible quantity of chemicals / Reagents for any experimental procedure.
• Close the water tap immediately after use; do not waste water.
• Precautions should be taken to avoid fire accidents.
• After the class, before you leave the laboratory, wash the apparatus clean, wipe the table
and keep the apparatus in proper place.
• Wearing Lab coats and shoes is mandatory inside the laboratory
• Wear gloves while handling the chemicals
• No edible items are allowed inside the laboratory.
• Switch off the fans and lights while leaving the laboratory.
• Incase of any medical emergency, report to staff members / lab assistant.

Chemical Engineering CH23621 6

 RAJALAKSHMI ENGINEERING COLLEGE

DEPARTMENT OF CHEMICAL ENGINEERING

MASS TRANSFER LABORATORY

INDEX

S.NO DATE NAME OF THE EXPERIMENT PAGE / T.SIGN

MARK

1.

2.

3.

4.

5.

6.

7.

8.

9.

10.

Chemical Engineering CH23621 7

EX.NO:
DATE:

SIMPLE DISTILLATION
AIM:
To verify Rayleigh’s equation graphically as well as analytically for the given system
(acetone-water)
APPARATUS:
Simple distillation Setup, measuring jar specific gravity bottle, beaker
THEORY:
In simple distillation, a batch of liquid is charged to a kettle or flask fitted with some sort of
heating device. The charge is boiled slowly and the vapors are withdrawn as rapidly as they
form in a condenser where they are liquefied and the distillate collected in the receiver the
vapor leaving the flask at any time is in equilibrium with the liquid in the flask, but since the
vapor is richer in the more volatile component, the composition of liquid and vapor are not
constant. The first portion of the distillate will be the richest in the more volatile component
and as distillation proceeds, the vaporized product become leaner, the distillate can therefore be
collected in several separate batches to give a series of distilled product of various purity.
Rayleigh’s equation is:
xf
Z2
∫ dZ/Z = In(F/W) = ∫ dx/(y *
− x)
Z1 xw

PROCEDURE:
1. Find out the specific gravity of a given binary system at various compositions.
2. Take 200 ml of component A (Acetone) and 100ml of component B (Water) in
the distillationflask and heat it over a heating mantle.
3. Note down the temperature at which the first drop of the distillate is collected.
4. Carry out the distillation until 2/3rd of the mixture get distilled.
5. Collect the distillate in conical flask.
6. Find out the volume of distillate and the residue.
7. Cool the residue to room temperature.
8. Find out the specific gravity of residue and distillate using specific gravity bottles.

Chemical Engineering CH23621 8

 9
OBSERVATION
Tabular column: 1

S.n Volume Volume Weight of Specific Weight of Weight of Total Moles Moles Total Mole Mole
o of of water mixture gravity of acetone water weight of of water moles fraction fraction
acetone (ml) (g) mixture (g) (g) (g) acetone (g. mol) (g. mol) of of water
(ml) (g. mol) acetone
( Xw )
1.

2.

3.

4.

CH23621
5.

6.

7.

8.

9.

10

Chemical Engineering
11

9
OBSERVATION
Temperature at which the first drop of condensate collected =
°C Room temperature =
°C
Density of water at room temperature= g/cc
Volume of Acetone taken = ml
Volume of Water taken = ml
Total volume of Residue Collected = ml
Total volume of Distillate Collected = ml
Weight of specific gravity bottle + water = g
Empty weight of specific gravity bottle = g
Weight of water = g
Similarly;
Weight of acetone = g
Weight of condensate = g
Weight of residue = g

CALCULATION:
Specific gravity of acetone = Weight of acetone/ Weight of water
=
Specific gravity of condensate = Weight of condensate/ Weight of water
=
Specific gravity of residue = Weight of residue / Weight of water
=
Density of Acetone = Specific gravity of Acetone* Density of water
=
= g/cc
Density of Water = Specific gravity of water * Density of water
=
= g/cc
Weight of Acetone = (Volume of Acetone)*(Density of Acetone)
=

Chemical Engineering CH23621 10

 = g
Weight of Water = (Volume of Water)*(Density of Water)
=
= g
Moles of Acetone taken = (Weight of Acetone) / (Molecular Weight of Acetone)
= g.mol
Moles of Water taken = (Weight of Water) / (Molecular Weight of Water)
= g.mol
Total Moles = Moles of Acetone + Moles of Water
= g.mol
Mole Fraction of Acetone = Moles of Acetone/Total Moles
=
Mole Fraction of Water = Moles of Water / Total Moles

Antoine’s equation: log P sat= A - B/ (T+C)Where A, B, C are the constants

For acetone, A= For water, A=
B= B=
C= C=
In the temperature range of °C,
In the temperature range of °C
Where,
T is the temperature in °C,
P is vapour pressure in mm
Hg. For Acetone:

log PA sat= A - B/ (T+C)

For water:

log PB sat= A - B/ (T+C) X= (Pt-PB ) / (PA-PB)

= Y*= (XAPA) / Pt =

Y*-X =
1/ (Y*-X) =

Chemical Engineering CH23621 11

 Tabular column: 2
S.NO Temp PA PB X Y* Y*-X 1/ (Y*-X)
(º C) mm Hg mm Hg
1.

2.

3.

4.

5.

6.

7.

8.

9.

10.

VERIFICATION:
Rayleigh’s equation is verified by analytically:

NAO= mass of acetone in feed / molecular weight of =

acetone
= g.mol
NBO= mass of water in feed / molecular weight of =
water
= g.mol
F = No= NAO + NBO = = g.mol

Average Molecular Weight of Residue= (Xw) Molecular weight of Acetone +(1- Xw) Molecular weight
of
water

W= Mass of residue / Average Molecular Weight of Residue =W = g.mol

Chemical Engineering CH23621 12

 Rayleigh’s equation is verified by graphically:
Mole Fraction of Acetone in feed: Xf = NAO / No = =

FROM GRAPH 1
Mole Fraction of Acetone in Residue Xw =

FROM GRAPH 2, USING Xf & XW

Area under the curve of the graph =

Thus the Rayleigh’s equation is verified by analytically and graphically:

L.H.S= R.H.S

Graph:
Specific gravity of mixture Vs mole fraction of acetone (Xw) 1/ (Y*-X) Vs mole fraction of acetone (Xw)

RESULT:

VIVA QUESTIONS:
Define simple distillation
Give the significance of rayleigh equation
What s relative volatility
Differentiate partial pressure and vapor pressure
Define specific gravity

Chemical Engineering CH23621 13

 EXP.NO:
DATE:
SINGLE STAGE AND MULTI STAGE EXTRACTION

AIM:
To determine the percentage recovery of solute in single and multi-stage extraction and to
determine which is more efficient.
APPARATUS REQUIRED:
Beaker, weighing machine, watch glass, stirrer, Conical flask, separation flask, Burette
CHEMICALS REQUIRED:
Water,1 N NaOH solution, Benzene, acetic acid
THEORY:
Solvent extraction is a simple technique for the separation of the components of a liquid
mixture by contacting with an immiscible or partially miscible liquid solvent. separation is
due to the differential distribution of components between the two soluble phases. The
products that are separated are the solvent rich phase called the extract and the carrier rich
phase called raffinate.
EXPERIMENTAL PROCEDURE:
SINGLE STAGE EXTRACTION:
1. 10 ml of acetic acid, 30 ml of benzene and 40 ml of water were taken in a beaker.
2. The contents in the beaker were stirred vigorously for 15 minutes.
3. The contents were poured in the separation flask and waited for 10 minutes till the
separation happens.
4. Then, the raffinate phase was taken out and the amount of it was measured and 10 ml
of raffinate was taken and phenolphthalein was added.
5. The raffinate was titrated against IN NaOH and the appearance of pink colour happens.
6. The volume of NaOH in beaker and amount of extract in Separation flask were noted
dawn.
MULTI STAGE EXTRACTION:
1. 30 ml of benzene was added to the remaining raffinate.
2. Again, the contents were stirred continuously for 15 minutes.
3. Then the contents were poured to the separation flask and it took about 10 minutes of
complete separation to take place.
4. Then from the extracted raffinate 10 ml was takes and some drops of phenolphthalein
was added to it.
5. It was titrated against IN NaOH, so that the raffinate was turned into pink colour.

14
Chemical Engineering CH23621
OBSERVATION:
SINGLE STAGE EXTRACTION:

S.NO Volume of Solution Burette Reading NaOH(ml) Volume of NaOH

(ml) (ml)
Initial (ml) Final (ml)

Volume of raffinate = ml
MULTI STAGE EXTRACTION:
Stage 1:

S.NO Volume of Solution Burette Reading NaOH(ml) Volume of NaOH

(ml) (ml)
Initial Final
(ml) (ml)

Volume of raffinate = ml
Stage 2:

S.NO Volume of Solution Burette Reading NaOH(ml) Volume of NaOH

(ml) (ml)
Initial (ml) Final (ml)

Volume of raffinate = ml

15
Chemical Engineering CH23621
 FORMULAE:
weight of solute in raffinate =
𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦 𝑜𝑓 𝑟𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒 × 𝐸𝑞𝑢𝑖𝑣𝑎𝑙𝑒𝑛𝑡 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 ×
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑟𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒 1000

𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑓𝑒𝑒𝑑 − 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒

𝑖𝑛 𝑟𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒 ) × 100%
%𝑅𝑒𝑐𝑜𝑣𝑒𝑟𝑦 = (
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑓𝑒𝑒𝑑

RESULT:
The extraction experiment was conducted and the percentage recovery for single and
multistage were found to be
Single stage -
Multi stage –
VIVA QUESTIONS:
Define liquid liquid extraction
What is tie line
Brief on Binodal Curve
List some solvents used in extraction

16
Chemical Engineering CH23621
 EXP.NO:
DATE:

LIQUID - LIQUID EQUILIBRIUM

AIM :
To study the ternary liquid equilibrium.
APPARATUS REQUIRED:
Burette, Measuring jar, stirrer, Conical flask, Beaker.
CHEMICALS REQURED:
Benzene, acetic acid, Water
THEORY:
Liquid- liquid extraction involves distribution of the components between two immiscible or
partially miscible liquids.The feed solution which is a mixture of solute c and carrier liquid
water A is extracted with solvent B. The extract will be rich in solvent and raffinate will be
rich in carrier If the carrier A and solvent B are partially miscible, the extract and raffinate
phases are ternary liquid mixtures are A,B and C.
The equilibrium behaviour of such mixtures are conventionally represented on the equilateral
triangular Coordinates.
EXPERIMENTAL PROCEDURE:
 Two burettes were takes. one was filled with benzene and other with water.
 The second beaker with water was titrated against benzene 6 beaker were taken and
filled as follows,

1 - 10ml of water + 0 ml & CH3COOH

2 - 8 ml of water + 2ml of CH3COOH
3 - 6 ml of water + 4 ml of CH3COOH
4 - 4 ml of water + 6 ml of CH3COOH
5 - 2 ml of water + 8ml of CH3COOH
6 - 0 ml of water + 10 ml of CH3COOH

 All the beaker were shaken vigorously for 15 minutes.

 It was titrated against benzene and the turbidity occurred.
 To titrate against water 6 beakers were taken and filled as follows,

1-10 ml of benzene + 0ml CH3COOH

2- 8 ml of benzene + 2 ml CH3COOH
3- 6 ml of benzene + 4 ml CH3COOH
4- 4 ml of benzene + 6ml CH3COOH

17
Chemical Engineering CH23621
 5- 2 ml of benzene + 8ml CH3COOH
6- 0 ml of benzene + 10 ml CH3COOH
 It was vigorously shaken for 15 minutes and titrated against water and the turbidity
occurred.
 The burette readings were noted for each beaker and the LLE graph was plotted.

OBSERVATION:
Benzene Vs Acetic acid and water
Volume of H2Volume
0 of Volume of Total Wt- Wt- fraction Wt- fraction
CH3COOH C6H6 weight fraction for for C6H6
for H20 CH3COOH

Acetic acid and water Vs Benzene

Volume of Volume of Volume of H2Total
0 Wt- Wt- fraction Wt- fraction
CH3COOH C6H6 weight fraction for for C6H6
for H20 CH3COOH

18
Chemical Engineering CH23621
 RESULT:
The ternary liquid equilibrium experiment was conducted and LLE graph was plotted and
verified
CONCLUSION:
The ternary liquid was studied for liquid-liquid equilibrium.
VIVA QUESTIONS
Define Liquid Liquid Equilibrium
List the ternary mixture used for LLE
Give the significance of Ternary Diagram
Define solubility
What is selectivity in LLE

19
Chemical Engineering CH23621
 EXP.NO:
DATE:

DISTRIBUTION COEFFICIENT
AIM:
To determine the distribution coefficient of the acetic acid – water mixture.
APPARATUS REQUIRED:
Beaker, Iodine Flasks, Stirrer, Separating Funnel, Conical Flasks, Burette
CHEMICALS REQUIRED:
1 N NaOH, Water, Oxalic Acid, Acetic Acid, Benzene, Phenolphthalein Indicator
THEORY:
The liquid – liquid equilibrium can be represented by means of distribution curve as
well. The ratio of the weight fraction of the solute in the extract to that in the raffinate is
called Distribution Coefficient (m). The distribution coefficient curve shows graphically the
relationship between the weight fraction of solute in extract phase (y) taken on y-axis and the
weight fraction of solute in raffinate (x) taken on x-axis.
EXPERIMENTAL PROCEDURE:
STANDARDISATION OF 1 – N NaOH:
1. 40g of NaOH was taken and mixed it with 1 liter of water. It was stirred vigorously
for 5 minutes.
2. 62.6 g of oxalic acid as taken in 1 liter of water and stirred for 5 minutes.
3. 10 ml of NaOH in the conical flask was taken and filled the burette with oxalic acid.
4. To the 10 ml of NaOH, phenolphthalein was added as an indicator.
5. The solution was titrated and it turned pink in color.
6. The procedure was repeated until the burette reading was 10 ml.
7. Hence it was ensured that the NaOH taken was 1-N solution.

PROCEDURE:
1. Three iodine flask was taken and 25 ml of distilled water and 25 ml of benzene wore
added.
2. 1ml of acetic acid was added to the 1st iodine flask.
3. 5ml of acetic acid was added to the 2nd iodine flask.
4. 10ml of acetic acid was added to the 3rd iodine flask.
5. The solution contained in the iodine flask was stirred vigorously for 15 minutes.
6. The solution gets separated after some time.
7. All the three solutions were poured in the separating funnel one by one and the
raffinate and the extract were separated.
8. The volume of raffinate and extract were noted down.
9. 10 ml of raffinate solution was taken and phenolphthalein indicator was added into it.

20
Chemical Engineering CH23621
 10. It was titrated against 1-N NaOH solution and it turned into pink color at some point.
11. The Burette reading was noted down.
12. The experiment was repeated for other two solutions.

FORMULAE USED:

Weight of solute in raffinate

𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦 𝑜𝑓 𝑟𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒 × 𝐸𝑞𝑢𝑖𝑣𝑎𝑙𝑒𝑛𝑡 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 × 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓
𝑟𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒
=
1000

Weight of solute in solute = Weight in feed − Weight in raffinate

Concentration of solvent in Weight of solvent in

raffinate (X) = raffinate Volume of
raffinate

Concentration of solvent in Weight of solvent in

Extract (Y) = Extract Volume of
Extract

Y
Distribution coefficient (K) =
X

21
Chemical Engineering CH23621
 22
TABULATION:

Volume Volume Volume Volume Weight Volume Normalit Weight of Weight Conc of Conc of K=Y/X
of of of of of of y of CH3COO of CH3COO CH3COO Distribution
CH3COO Extract Raffina Rundo CH3COO CH3COO CH3COO H CH3COO H H Coefficient
H (ml) te wn H H H in H in in
(ml) (ml) NaOH In feed in in raffinate in extract raffinate extract
(ml) (ml) raffinate raffinate (ml) (X) (Y)
(N) (g)
(ml)

CH23621
Chemical Engineering
 RESULT:
By conducting the experiment, the Distribution Coefficient was found to be
Analytically, K=
Graphically, K=

CONCLUSION:
The larger the Distribution Coefficient values, smaller the quantity of solvent required for
Extraction
VIVA QUESTION :
Define Distribution Coefficient
What is miscibility
List some application of extraction
Recite some of the solvent used for extraction
What is extract and raffinate

Chemical Engineering CH23621 23

 EXP.NO:
DATE:

SINGLE STAGE AND MULTI STAGE ADSORPTION

AIM:
To determine the percentage recovery of single and multistage adsorption and to also determine
which is more efficient.
APPARATUS REQUIRED:
Burette, Beaker, stirrer, filter paper, Conical flask, funnel
CHEMICALS REQUIRED:
NaOH pellets, Acetic acid, charcoal, Distilled water.
THEORY:
Adsorption is a process in which the components of a gas or liquid phase are selectively
transferred on to a solid surface lending to separation of components of the fluid phase.In
adsorption molecules distribute themselves between two phases, one a solid and the other a gas
or liquid. The solid is known as adsorbent and the fluid transferred to and adsorbed on the sold is
called the adsorbate.
EXPERIMENTAL PROCEDURE:

SINGLE STAGE ADSORPTION:

1. 40 ml of water, 10 ml of acetic acid and 4.5 gram of charcoal were taken in a beaker.
2. The contents were mixed in the beaker vigorously for about 15 minutes.
3. The solution was filtered using funnel and filter paper.
4. The amount of raffinate was measured and 10 ml was taken from it.
5. Phenolphthalein was added to it and was titrated against 1 N NaOH solution.
6. The volume of NaOH in burette was noted.
MUTI STAGE ADSORPTION:
1. 1.5 g of charcoal powder, 40 ml of water and 10 ml of acetic acid were taken in the
beaker containing remaining raffinate solution.
2. The contents were stirred vigorously for 15 minutes.
3. The solution was filtered using filter paper and funnel. The volume of raffinate was noted
down.
4. Phenolphthalein indicator was added to 10 ml of raffinate in a beaker.
5. It was titrated against IN NaOH and the burette reading was noted down.
6. The experiment was repeated for next stage of adsorption by adding 1.5 g of charcoal to
the raffinate of 2nd stage.

Chemical Engineering CH23621 24

 OBSERVATION:
SINGLE STAGE ADSORPTION:

S.NO Volume of Solution Burette Reading NaOH(ml) Volume of NaOH

(ml) (ml)
Initial (ml) Final (ml)

Volume of raffinate = ml
MULTI STAGE ADSORPTION:
Stage 1:

S.NO Volume of Solution Burette Reading NaOH(ml) Volume of NaOH

(ml) (ml)
Initial Final
(ml) (ml)

Volume of raffinate = ml
Stage 2:

S.NO Volume of Solution Burette Reading NaOH(ml) Volume of NaOH

(ml) (ml)
Initial (ml) Final (ml)

Volume of raffinate = ml

Chemical Engineering CH23621 25

 FORMULAE:

I. Weight of solute in raffinate =

𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦 𝑜𝑓 𝑟𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒 × 𝐸𝑞𝑢𝑖𝑣𝑎𝑙𝑒𝑛𝑡 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 ×
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑟𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒 1000

%𝑅𝑒𝑐𝑜𝑣𝑒𝑟𝑦 (=
w𝑒𝑖gℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑓𝑒𝑒𝑑 −w𝑒𝑖gℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛
) × 100%
𝑟𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒
II.

w𝑒𝑖gℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑓𝑒𝑒𝑑

RESULT:
The adsorption experiment was conducted and the percentage recovery of
Single stage -
Multi stage -
CONCLUSION:
The percentage recovery of multistage adsorption is higher than the single stage adsorption.

VIVA QUESTIONS:
Define Adsorption
List some applications in adsorption
What is the significance of adsorption equilibrium
Define percentage recovery
Why adsorption is a mass transfer operation.

Chemical Engineering CH23621 26

 EXP.NO:
DATE:

SINGLE - STAGE AND MULTI - STAGE LEACHING

AIM:
To determine the percentage recovery of solute in single stage and multi stage leaching and
to determine which is more efficient.
APPARATUS REQUIRED:
Beaker, Watch-glass, Stirrer, Weighing machine, Funnel, Conical Flask, Filter Paper,
Burette.
CHEMICALS REQUIRED:
Sand, NaOH Pellets, Water, 1-N HCl solution.
THEORY:
Leaching is the process by which the solute constituents of a solid feed are separated by
dissolving in liquid solvents. The solute gets dissolved in the solvent and the insoluble solids are
separated from the resulting solution. The thickened sludge is called “Underflow” and a clear
solution that contains solute is called “Overflow”.
EXPERIMENTAL PROCEDURE:
SINGLE STAGE LEACHING:
1. 48 g of sand and 2 g of NaOH pellets were taken in a beaker.
2. 50 ml of water was added into the beaker.
3. The contents were stirred vigorously for about 15 minutes.
4. Filter paper was taken and placed in the funnel.
5. The contents were taken and poured in the funnel which contains filter paper and the
liquid extract and the residual sand were separated.
6. 10 ml from the liquid extract was taken and phenolphthalein indicator was added into it.
7. It was titrated against 1N HCl and the volume was noted down.
8. The solution was turned from pink to transparent colour.
MULTI STAGE LEACHING:
1. The solid that had leached before was taken and 50 ml of water was added into it.
2. Again, it was stirred vigorously for 15 minutes and the solution mixture was filtered
using filter paper and funnel.
3. 10 ml of leached solution was taken and phenolphthalein indicator was added into it and
the solution became pink in colour.
4. It was titrated against 1N HCl until the disappearance of pink colour and the volume was
noted down.

Chemical Engineering CH23621 27

 OBSERVATON:
SINGLE STAGE LEACHING:

S.NO Volume of Solution Burette Reading HCl(ml) Volume of HCl

(ml) (ml)
Initial (ml) Final (ml)

Volume of filtrate = ml
MULTI STAGE LEACHING:
Stage 1:

S.NO Volume of Solution Burette Reading HCl(ml) Volume of HCl

(ml) (ml)
Initial Final
(ml) (ml)

Volume of filtrate = ml
Stage 2:

S.NO Volume of Solution Burette Reading HCl(ml) Volume of HCl

(ml) (ml)
Initial (ml) Final (ml)

Volume of filtrate = ml

Chemical Engineering CH23621 28

 FORMULAE USED:

Weight of solute in 𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦 × 𝐸𝑞𝑢𝑖𝑣𝑎𝑙𝑒𝑛𝑡 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 ×

Filtrate =
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐹𝑖𝑙𝑡𝑟𝑎𝑡𝑒 1000

% Recovery 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑓𝑒𝑒𝑑 − 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓

= 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝐹𝑖𝑙𝑡𝑟𝑎𝑡𝑒 × 100
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑓𝑒𝑒𝑑

RESULT:
Thus, by conducting the leaching experiment we observed as follows
Single stage -
Multi stage -
CONCLUSION:
The percentage recovery of solute was more in multi-stage leaching.
VIVA QUESTIONS:
Define leaching
Why percentage recovery is commonly more in multistage leaching
What are the factors affecting leaching efficiency
What is leaching equilibrium
Define underflow and overflow in leaching process

Chemical Engineering CH23621 29

 EXP.NO:
DATE:

FORCED DRAFT TRAY DRYER

AIM:
To determine the drying rate of a solid under forced draft condition and determine the
critical moisture content.

THEORY:
In many cases, drying of materials is the final operation in the manufacturing process,
carried out immediately prior to packaging or dispatch. Drying refers to the final removal of
water, and the operation often follows evaporation, filtration or crystallization. Drying is carried
out for one or more of the following reasons:
a) To reduce the cost of transport.
b) To make a material more suitable for handling.
c) To provide definite properties.
d) To remove moisture this may otherwise lead to corrosion.

Drying of solids is considered to occur in two stages, a constant rate period followed by a falling
rate period. In the constant rate period, the rate of drying corresponds to the removal of water
from the surface of the solid. The falling rate period corresponds to the removal of water from
the interior of the solid. The rate in either case is dependent on:
 Flow rate of air.
 The solid characteristics.
 Tray material.
The rate of drying can be determined for a sample of substance by suspending it over an
electronic balance in the duct, in a stream of air, from a balance. The weight of the drying
sample can then be measured as a function of time. Certain precautions must be observed if the
data are to be of maximum utility. The sample should not be too small. Further, the following
conditions should resemble as closely as possible those expected to prevail in the contemplated
large-scale operation:
• The sample should be similarly supported in a tray or frame.
• It should have the same ratio of drying to non-drying surface.
• It should be subjected to similar conditions of radiant heat transfer; and
• The air should have the same temperature, humidity and velocity (both speed and
direction with respect to the sample).
If possible, several tests should be made on samples of different thicknesses. The dry weight of
the sample should also be obtained. The drying rate is calculated from:

Chemical Engineering CH23621 30

 A schematic diagram of the experimental set-up is given below:

AIR IN

It is a wind-tunnel type tray dryer. The main components are;

 Drying chamber
 Air blower
 Heater
 Orifice in the air duct
 A tray
 Balance
The air flow is controlled by a valve in the blower outlet and its flow rate is measured by a pre-
calibrated orifice meter. Thermometers are placed at the inlet and outlet of the drying chamber.

EXPERIMENTAL PROCEDURE:

1. Load the pre-weighed tray with solid and record the weight of sand & tray.
2. Start the blower and heater. Fix the air flow rate and let the system to achieve steady
state as the air flow rate would make the temperature steady.
3. When the desired conditions of temperature and air velocity are reached (in about
10- 15min), remove the sample tray and put known amount of water in it to give
desired initial moisture content.
4. Place the tray gently in the drying chamber and start the stopwatch.
5. Record the balance reading with time at about 3-5min time interval.
6. Drying is assumed to be complete when atleast 3 consecutive readings are unchanged.
7. The temperatures at the inlet and outlet of the drying chamber and the air flow rate
(manometer reading fixed across the orifice) are recorded at least three times during
the course of run to give average operating conditions.

Chemical Engineering CH23621 31

 8. The same steps are repeated for other runs at different operating conditions.

The range of variables may be fixed as given below:

Air Flow rate = 8 to 10 cm manometric difference (with water as manometric fluid)
Initial Moisture Content = 20-50% (Prepare the sample in this range of
moisture content)

CALCULATION FORMULAE:
Moisture content present in solid, X = (W-S)/S (kg water/kg dry solid) The
drying rate is thus calculated from:

𝑁 = 𝑆 ∆𝑥
−
𝐴 ∆𝜃

OBSERVATIONS AND CALCULATIONS:

Tray diameter = 150 mm

Surface area of solid = 0.0706 m2
Solid dry weight = kg
Initial moisture content = (kg water/kg dry solid)

ρm
Manometric difference, R = m

ℎ = 𝑅 × ( − 1)
ρ
a
Superficial air flow rate, G = 0.61 × ao × √2gh × ρa kg/m2s
TABULATION:

𝑆
𝚫𝑥
𝑁=−
S.NO Time, θ Weight of solid X= [W-S]/S

𝐴
(s) (Solid + water) (kg water/kg dry solid)
𝚫𝜃
(Kg)

Chemical Engineering CH23621 32

 Plot X Vs θ and draw a straight line through all points. Fit a second degree polynomial to the X
Vs θ data and obtain the slope dX/dθ corresponding to various values of θ
The drying rate is thus calculated from:

𝑁 = 𝑆 ∆𝑥
−
𝐴 ∆𝜃
Plot drying rate N (kg/m2-s) Vs moisture content X (kg of water/kg of dry solid). From this plot
critical moisture content (Xc) can be obtained.
The experiment can be repeated at constant air flow rate and constant air temperature.

NOMENCLATURE:
A = Drying surface area, m2
G = Mass velocity of gas, kg/m2. s
N = Drying rate, kg/m2. s
Nc = Constant drying date, kg/m2. s
S = Mass of dry solid, kg
Tg = Absolute temperature of gas(dry bulb), k
X = Moisture content of solid, (kg water/kg dry solid)
θ = Time, sec
𝜌 = Density, kg/m3
ρm = Density of manometric fluid, kg/m3
ρa = Density of air, kg/m3
ao = Area of orifice, m2
W= Mass of wet solid, kg

RESULT:

VIVA QUESTIONS:
Define drying
List the application of tray drier
What is rate of drying
Define critical moisture content
What is bound and unbound moisture

Chemical Engineering CH23621 33

 EX.NO:
DATE:

ROTARY DRYER

AIM:
To determine the drying rate of a solid under forced draft condition and determinethe critical
ChemmoicisatluErencgoinneteenritn. g CH23621
THEORY:
In many cases, drying of materials is the final operation in the manufacturing process, carried
out immediately prior to packaging or dispatch. Drying refers to the final removal of water, and
the operation often follows evaporation, filtration or crystallization. Drying is carried out for
one or more of the following reasons:
 To reduce the cost of transport.
 To make a material more suitable for handling.
 To provide definite properties.
 To remove moisture this may otherwise lead to corrosion.
The rotary dryer is a type of industrial dryer employed to reduce or minimize the liquid moisture
content of the material it is handling by bringing it into direct contact with a heated gas.
The dryer is made up of a large, rotating cylindrical tube, usually supportedby concrete
columns or steel beams. The dryer is inclined to slopes slightly so that the discharge end is lower
than the material feed end in order to convey the material through the dryer under gravity.
Material to be dried enters the dryer, and as the dryer rotates, the material is lifted up by a series
of internal fins lining the inner wall of the dryer. When the material gets high enough to roll back
off the fins, it falls back down to the bottom of the dryer, passing through the hot gas stream as it
falls. This gas stream can either be moving toward the discharge end from the feed end (known
as co-current flow), or toward the feed end from the discharge end (known as counter- current
flow). The gas stream can be made up of a mixture of air and combustion gases from a burner,
in which case the dryer is called a direct heated dryer. Alternatively, the gas stream may consist
of air or another (sometimes inert) gas that ispreheated. When the gas stream is preheated by
some means where burner combustion gases do not enter the dryer, the dryer known as an
indirect-heated type. Often, indirect heated dryers are used when product contamination is a
concern. In some cases, a combination of direct-indirect heated rotary dryers are also available to
improve the overall efficiency.A rotary dryer is suitable to dry metallic and nonmetallic mineral,
clay in cement industrial and coal slime in coal mine, etc. Rotary dryers can be widely used to
dry various materials, and are simple to operate.
The dry weight of the sample should also be obtained. The drying rate is calculated from:

Chemical Engineering CH23621 34

 The main components are;
 Drying chamber
 Air blower
 Heater
 Orifice in the air duct
The air flow is controlled by a valve in the blower outlet and its flow rateis measured
by a pre-calibrated orifice meter. Thermometers are placed at the inlet and outlet of the drying
pipe.

EXPERIMENTAL PROCEDURE:
1. Measure the weight of dry wheat and then get it wet by adding it into a containerwith
water. Measure the weight of this wet wheat also.
2. Start the blower and heater. Fix the air flow rate and let it run for 15-20 minutes tillsteady
state is achieved. (for pre heating)
3. Place this measured wet wheat into the entry section. Start the stop watch.
4. Let it run for time till we get all the wheat from the other end. Also measure the
temperature readings at inlet and outlet of the section.
5. Measure the weight of extracted wheat.
6. The same steps are repeated for other runs at different operating conditions.

OBSERVATION TABLE:

S.NO T1(⸰C) T2(⸰C) T3(⸰C) T4(⸰C) R1(cm) R2(cm)

OBSERVATIONS & CALCULATIONS:

Diameter of rotary dryer pipe, d = m
Length of pipe, L = m
Area of orifice, ao = 1.5386 × 10-4 m2
Dry weight of sample, S = gm
Wet weight of sample, W = gm
Initial moisture content, X (W – S) = gm
Weight after drying, WD = gm
Density of water, ρm = 1000 Kg/m3
Density of air, ρa = 1.21 Kg/m3

Chemical Engineering CH23621 35

 NOMENCLATURE:

R1, R2 = Higher and lower manometer readings resp., cm.

R = manometric difference, m
h = Pressure head in terms of m of H2O
G = Mass velocity of gas, kg/s
S = Mass of dry solid, kg
W = Mass of wet sample, Kg
WD = Mass of sample after drying
X = Moisture content of solid (kg of water/kg of dry solid)
ρm = Density of manometric fluid, kg/m3
ρa = Density of air, kg/m3
a0 = Area of orifice, m2
T1 = Dry bulb temperature of air at inlet, ⸰C
T2 = Wet bulb temperature of air at inlet, ⸰C
T3 = Dry bulb temperature of air at outlet, ⸰C
T4 = Wet bulb temperature of air at outlet, ⸰C

Chemical Engineering CH23621 36

 PRECAUTIONS & MAINTENANCEINSTRUCTIONS:
1. Measure the exact volume of water and weigh the Mixture.
2. Always use clean water and good quality raw material for mixing.
3. Use electronic balance for weighing of mixture.

RESULT:

VIVA QUESTIONS:
How rotary drier works
What is the range of particle size of the feed can be feed to the drier
Define equilibrium moisture content
Define rate of drying
Give the significance of counter current flow in rotary drier

Chemical Engineering CH23621 37

 EXP.NO:
DATE:

VACUUM DRYER
AIM:
The rate of drying curve for a vacuum dryer. To study the drying characteristics of a
solid material under batch vacuum condition.
INTRODUCTION:
Dryers are used to remove liquids or moisture from bulk solids, powders, parts,
continuous sheets or other liquids by evaporation or sublimation. Dryers can be broken up into
two main types: direct and indirect. Direct dryers convectively heat a product through direct
contact with heated air, gas or a combusted gas product. Indirect dryers conductively heat a
product through contact with a heated wall. Tray vacuum Dryer is used for the best drying
results in conventional process. It is a double walled cabinet with Single or Two doors. The gap
between two walls is filled with high density fiber glass wool insulation material to avoid heat
transfer. Doors are provided with gaskets. Stainless steel trays are placed on the movable
trolleys. Tray Dryer is provided with control panel board, process, Digital temperature
controller cum indicator etc.
THEORY:
Vacuum drying is the mass transfer operation in which the moisture present in a
substance usually wet solid is removed by means of creating vacuum. In chemical process
industries like food, pharmaceutical, agricultural, textile, paper & pulp etc. drying is an
essential unit operation to remove the moisture from various substances to get a solid finished
product. Vacuum drying is generally used for the drying of those substances which are
hygroscopic and heat sensitive and is based on the principle of creating vacuum. With the help
of vacuum the pressure is reduced around the substance to be dried and boiling point of water
inside that product decreases and rate of evaporation of water increases significantly thus
increasing drying rate.
SPECIFICATIONS:
 Pump capacity = 0.5 hp
 Area of the tray = m2
 Height of the tray = m
 Length of the tray = m
 Least count of the weighing balance = 0.01 g
 Heater capacity = 250 w

EXPERIMENTAL PROCEDURE:

9. Load the pre-weighed tray with solid (e.g. saw dust or sand).
10. Place it over the weighing balance.
11. Record the weight of sand & tray.
12. Set the desired temperature of chamber with the help of temp. controller.
13. Switch ON the load and adjust the heater knob to desired position.
14. Keep the tray gentle in the drying chamber and close the chamber.
15. Switch ON the vacuum pump.
16. Switch ON the stopwatch.
Chemical Engineering CH23621 38
 17. Keep the pressure knob in open condition until it reaches the desired vacuum
pressure in mmHg and close it.
18. Switch OFF the Vacuum pump to maintain the vacuum pressure inside the drying
chamber.
19. Wait until the vacuum pressure reaches to zero and note down the time taken.
20. Open the chamber and remove the tray from the chamber and weigh the sample
tray.
21. Note the loss of weigh in the mixture.
22. Dry the mixture until 85% of dry rate is achieved by repeating the following
procedure (5-13).
23. Once the process completes, Switch OFF the load and adjust the heater knob to
zero position.
24. Switch OFF the main power supply.
25. Calculate the moisture content and drying rate of the solid.

OBSERVATION & CALCULATIONS:

Weight of empty tray = kg Solid
dry wt.(S) = kg
Volume of the water = ml
Solid wet weight(Wi) = kg
Initial moisture content(x) = [Wi-S]/S
= kg water/kg dry solid

S.NO Vacuum Time, θ Weight of solid Moisture content Rate of

Pressure after vacuum present in solid drying, N
(s)
drying, Wf at θ, X (kg
(mmHg)
water/kg dry
(Kg)
solid
X= Wf – Wi / S

To find out rate of drying

𝑋
𝐴*𝜃
Rate of drying, N =

Chemical Engineering CH23621 39

 = (Moisture content at θ/ Area of tray * Time)

Graph: Time, θ vs Rate of drying, N

NOMENCLATURE:

A= drying surface area, m2

N= drying rate, kg/m2-s
Nc = constant drying rate, kg/m2-s
S= mass of dry solid (kg)
X= moisture content of a solid (kg of water/kg of dry solid)
θ= time, s
μ= viscosity kg/m-s
𝜌 = density kg/m3

PRECAUTIONS & MAINTENANCE INSTRUCTIONS:

1. Measure the exact volume of water and weigh the Mixture.
2. Always use clean water and good quality saw dust for mixing.
3. Use electronic balance for weighing of mixture.
4. Keep close the front door if chamber while working.
5. Don’t ON heater switch before putting the mixture in chamber.

RESULT:
Rate of drying =

VIVA QUESTIONS:
Define vacuum drying
What the optimal range of vaccum pressure to operate for drying
What is rate of drying
What is the effect of temperature in vacuum drying
Define critical moisture content

Chemical Engineering CH23621 40

 EX.NO:
DATE:

EXPERIMENTAL WATER COOLING TOWER

AIM:
Study of the heat & mass transfer in Water Cooling Tower for different flow &
thermodynamic conditions.
To find out tower characteristics:
 Range
 Approach
 Water to air mass flow ratio (L/G)
 Effectiveness of the tower
 Evaporation losses
 Percentage evaporation losses
 Blow down losses
 Drift losses
 Make up water requirements

THEORY:
Water from condensers and heat exchangers is usually cooled by an air stream in spray
ponds or in Cooling Towers using natural draft or forced flow of the air. Mechanical draft
towers are of the forced draft type, where the air is blown into the tower by a fan atthe bottom.
The forced draft materially reduces the effectiveness of the cooling.
Water may be cooled by the air as long as its temperature is above the wet bulb temperature of
the entering air. In a counter flow design, the air flow is directly opposite to the water flow. Air
flow first enters an open area beneath the fill media, and is then drawn up vertically. The water
is sprayed through pressurized nozzles near the top of thetower, and then flows downward
through the fill, opposite to the airflow. Advantages of the counter flow design:
a. Spray water distribution makes the tower more freeze-resistant.
b. Breakup of water in spray makes heat transfer more efficient

Chemical Engineering CH23621 41

 The carrying of liquid with the gas stream is termed as Liquid Entrainment. This may be due to
a high rate of air flow. This should be avoided to get better performance. This can be avoided
by following the Operational limits of the equipment.
The apparatus is provided for the process of Forced draft countercurrent cooling of hot water
using air. The water to be cooled is heated in a heating tank using a heater. It is then circulated;
through a rotameter; to the top of the cooling tower mounted over the heating tank. Cooled
water is then re-circulated to the heating tank. A blower is providedfor the cooling air. Speed of
blower can be regulated with the help of variable speed drive (VSD). A valve is provided in
airline to regulate the flow rate of air. There is an orifice meter mounted with its taps connected
to a manometer to find the flow rate of air.A set of two temperature sensors is provided at both
inlet and outlet of air stream. These sensors gives Dry bulb & Wet bulb air temperatures. The
cooling tower is packed with Aluminum expanded wire mesh.
Description of temperature sensors are as follows:

T1 = inlet dry bulb temp air.

T2 = inlet wet bulb temp air.

T3 = outlet dry bulb temp air.
T4 = outlet wet bulb temp air.
T5 = inlet water temp.
T6 = outlet water temp.

EXPERIMENTAL PROCEDURE:
1. Fill the heating tank with water, set the temperature with the help of D.T.C.and
switch on heater.
2. Switch on pump & blower after desired temperature achieved.
3. Set the flow rate of water and air.
4. Record the flow rate of water and manometer reading after steady state achieved.
5. Record the temperatures.
6. Steps 3 to 5 may be repeated for different water & air flow rates withinoperational
range.

OBSERVATION & CALCULATION:

DATA:
Orifice dia.,( d1) = 0.026 m
area of Orifice,( a1) = 5.30 × 10-4 m2
Dia. of Pipe) (d2) = 0.052 m
area of Orifice, (a2) = 2.12 × 10-3 m2
Coefficient of Discharge,( Cd) = 0.64
Density of water (𝜌water) = 1000 kg/m3

Chemical Engineering CH23621 42

 Density of water (𝜌air) = 1.21

kg/m3 Acceleration due to gravity(g) =9.81

m/s2

OBSERVATION TABLE:

h Water temp. Air Temperature (⸰C)

(in cm) Flow rate (⸰C) Inlet Outlet
ofwater
T1 T2 T3 T4
Fw (LPH)
S. T5 T6 Dry bulb Wetbulb Dry bulb Wetbulb
No. h1 h2 Inlet Outlet

CALCULATION :

Range (r) = 𝑇5 − 𝑇6 , ℃

Approach (A) = 𝑇6 − 𝑇2 , ℃

𝑅𝑎𝑛g𝑒
𝑅𝑎𝑛g𝑒+𝐴𝑝𝑝𝑟𝑜 × 100%
Effectiveness(𝜀)=
𝑎𝑐ℎ

=𝑇5−𝑇2 × 100%
𝑇5−𝑇6

Flow rate of air, (Qa) = Qa = Cd ,

m3/se Flow rate of air, G = Qa ×3600, m3/hr

Chemical Engineering CH23621 43

 Flow rate of water, L= 𝐹𝑊 , m3/hr
1000
𝐿
=
𝐺
Evaporation Losses(EL) = 0.00085×1.8×mass flow rate of water × (T5-T6), m3/hr

𝖶𝑎𝑡𝑒𝑟 𝑙𝑜𝑠𝑠 𝑑𝑢𝑒 𝑡𝑜

𝑒𝑣𝑎𝑝𝑜𝑟𝑎𝑡𝑖𝑜𝑛 × 100% =
Percentage Evaporation loss(EL)=

𝑀𝑎𝑠𝑠 𝑓𝑙𝑜w 𝑟𝑎𝑡𝑒 𝑜𝑓

w𝑎𝑡𝑒𝑟

Blow down losses (BD) = 0.2 × EL , m3/hr

Drift Losses(DL) = 0.002 × L ,

,m3/h
m3/hr
𝐸𝑣𝑎𝑝𝑜𝑟𝑎𝑡𝑖𝑜𝑛 𝐿𝑜𝑠𝑠 +𝐵𝑙𝑜w
𝐷𝑜w𝑛 𝑙𝑜𝑠𝑠+𝐷𝑟𝑖𝑓𝑡 𝑙𝑜𝑠𝑠
Makeup water Requirement (M) =

NOMENCLATURE:

Nom Column Heading Units Type

d1 Diameter of Orifice m Given

d2 Diameter of the pipe in which Orifice-meter is installed m Given

a1 Cross Section area of orifice m2 Given

a2 Cross Section area of pipe m2 Given

Co Coefficient of discharge of orifice --- Given

g Acceleration due to gravity m/s2 Given
G flow rate of air m3/hr Calculated
L Flow rate of water m3/hr Calculated
h1 Manometric higher scale reading cm Observed
h2 Manometric lower scale reading cm Observed
ΔR Manometric difference m calculated
ΔH Head in term of air m of air calculated

water Density of manometer fluid (water) Kg/m3 Given

Density of the fluid whose flow rate is to be measured
air Kg/m3 Given
(air)
Qa Flow rate of air m3/sec Calculated

Chemical Engineering CH23621 44

 L/G Water to air flow ratio ----- Calculated

T1 Air inlet dry-bulb temperature oC Observed

T2 Air inlet wet-bulb temperature oC Observed

T3 Air outlet dry-bulb temperature oC Observed

T4 Air outlet wet-bulb temperature oC Observed

T5 Water inlet temperature oC Observed

T6 Water outlet temperature oC Observed

EL Evaporation losses m3/hr Calculated

DL Drift losses m3/hr Calculated
BD Blow down losses m3/hr Calculated
M Makeup Water Required m3/hr Calculated

r range oC Calculated

A Approach oC Calculated

ε Effectiveness of tower % Calculated

PRECAUTIONS & MAINTENANCE INSTRUCTIONS:

1. Heater should not be switched on before filling the water in heating tank.
2. Pump should not be switched on at low voltage.
3. Water in heating tank should be properly drained after experiment is over.
4. Cotton jacket over the wet bulb arrangement should be in its place properly.
5. Wet bulb bottle should be filled with water before starting the experiment.

RESULT:

VIVA QUESTIONS:
Define range and approach
What is the application of cooling tower
Difference between dry bulb and wet bulb temperature
How flow rate of water and air affects the cooling tower efficiency
Define blow down losses.

Chemical Engineering CH23621 45

 EX.NO:
DATE:

SIMPLE BATCH DISTILLATION

AIM:
To verify Rayleigh equation for batch distillation.
THEORY:
Batch distillation is a process by which a mixture of volatile components is partially
separated by evaporation and condensation. The feed mixture is initially charged into the
still (boiler), heated and the vapour emerging from the still is condensed and collected as
distillate. As the distillation proceeds, the liquid in the still becomes more
concentrated in the less volatile component while the distillate tends to have a higher
concentration of the more volatile component. The distillate can be collected as a whole
or several fractions can be taken.The simplest and most frequently used batch distillation
configuration is the batch rectifier, including the alembic and pot still. The batch
rectifier consists of a pot(or reboiler), rectifying column, a condenser, some means
of splitting off a portion of the condensed vapour (distillate) as reflux, and one or more
receivers.
The pot is filled with liquid mixture and heated. Vapour flows upwards in the rectifying
column and condenses at the top. Usually, the entire condensate is initially returned to
the column as reflux. This contacting of vapour and liquid considerably improves the
separation.Generally, this step is named start-up. The first condensate is the head, and it
contains undesirable components. The last condensate is the feints and it is also
undesirable, although it adds flavor. In between is the heart and this forms the desired
product.The head and feints may be thrown out, refluxed, or added to the next batch of
mash/juice, according to the practice of the distiller. After some time, a part of the
overhead condensate is withdrawn continuously as distillate and it is accumulated in the
receivers, and the other part is recycled into the column as reflux.
Owing to the differing vapour pressures of the distillate, there will be a change in the
overhead distillation with time, as early on in the batch distillation, the distillate will
contain a high concentration of the component with the higher relative volatility. As the
supply of the material is limited and lighter components are removed, the relative
fraction of heavier components will increase as the distillation progresses.The equipment
consists of a distillation still made of stainless steel. The feed in the still is heated
externally by heater. The vapors form the top of the vessel is condensed in the type
condenser by circulating cooling water. Temperature of the feed mixture is controlled by
means of a digital temperature Controller. The condensate is collected in a receiver
made of stainless steel.
EXPERIMENTAL PROCEDURE:
1. Prepare methanol water solution by mixing known amount of water and
methanol.
2. The total amount of solution should not be less than 3 liters.
3. The composition of methanol in solution should be in the range of15 to 25 %
by volume.

Chemical Engineering CH23621 46

 4. Note down the volume of water and methanol.
5. Close all the valves.
6. Ensure that switches given on the panel is at OFF position.
7. Fill water in cooling water tank.
8. Fill the vessel with methanol-water solution by open the valve and air vent
valve.
9. Connect electric supply to the set-up.
10. Set a process temperature for the process using the digital temperature
controller (DTC). The temperature should be in the range of85 to 95 ºC.
11. Start the heater & cooling water pump.
12. Adjust the cooling water flow rate by valve to a moderate value.
13. Wait 25-30 minute for the system to achieve steady state.
14. Now take out the samples from the bottom & distillate stream by open the
valve
15. Cool down the samples to room temperature & measure the refractiveindices.
16. Repeat the experiment for different set point temperatures.
17. When experiment is over stop the water supply.
18. Switch OFF the main power supply.
19. Drain the vessel by open the valve.

OBSERVATION & CALCULATION:

DATA:
Refractive Index of the feed R.IF =

Initial concentration of the feed, XF = gm/mol

OBSERVATION TABLE:

S. No. T1 T2 T3 T4

Draw a calibration graph of refractive index v/s concentration and find out the concentration of
the feed, distillate and bottom product.

Chemical Engineering CH23621 47

 Mole fraction of
% of methanol % of water R.I at 250C
methanol (x)
100 0 1 1.3268
90 10 0.802 1.3300
80 20 0.643 1.3330
70 30 0.512 1.3356
60 40 0.403 1.3381
Ch emical Engineering CH23621
50 50 0.310 1.3398
40 60 0.231 1.341
30 70 0.162 1.3411
20 80 0.101 1.3394
10 90 0.047 1.3363
0 100 0 1.3321

NOMENCLATURE

Nom Column Heading Units Type

R.I.F Refractive Index of FEED - -

R.I.D Refractive Index of Distillate - -

R.I.B Refractive Index of Distillate - -
PRECAUTIONS & MAINTENANCE INSTRUCTIONS:
1. Use the stabilize A.C. Single Phase supply only.
2. Never switch on mains power supply before ensuring that all the ON/OFF
switchesgiven on the panel are at OFF position.
3. Keep all the assembly undisturbed.
4. Never run the apparatus if power supply is less than 180 volts and above than
240 volts.
5. Operate selector switch for temperature indicator gently.
6. Do not start heater supply unless water is filled in the test unit.
7. Always keep the apparatus free from dust.

RESULT:
VIVA QUESTIONS
Define simple batch distillation
What is relative volatility
List some application of batch distillation
Define vapour pressure
Give the significance of condenser in batch distillation

Chemical Engineering CH23621 48

 EXP.NO:
DATE:

STEAM DISTILLATION
AIM:
To study the characteristics of Steam Distillation using Turpentine oil as a feed
stock.
THEORY:
In a steam distillation process, the liquid is distilled by feeding open steam to the
distillation still. The steam carries with it vapor of volatile liquid and is then condensed
to separate the liquid from water. The essential requirement for carrying out steam
distillation is:
1. Substance does not react with steam.
2. Substance is in-soluble in
water. If P is the total system pressure
PA is the vapor pressure of turpentine (A) PB is the vapor pressure of water (B)
then
P=PA + PB (1)

For atmospheric distillation- P = 101.3 KN/m2

Plot of PAVs T and (101.3 - PB) Vs T

On the same graph gives HAUSBRAND Vapor Pressure diagram. The intersection of the
two curves gives the distillation temperature.

Vapor Pressure

T Distillation Temp.

Chemical Engineering CH23621 49

 Let NA be the number of moles of Turpentine oil in vapor phase.

Let NB be the number of moles of Water in the vapor phase.

∴ Partial pressure of Turpentine oil in the vapor phase

Po A = P[N A/N A+N B] (2)

and Partial pressure of water in the vapor phase
Po B = P[N B/N A+N B] (3)

= =
PoA NA
𝖶𝐴/𝑀𝐴 (4)
PoB NB 𝖶𝐵/𝑀𝐵

Where, WA& WB represent the grams or kgs of turpentine & water respectively in the
Vapor phase
MA& MB are the corresponding molecular weights. Equation (4) can be written in terms
of vapor pressure as:

= =
𝖶𝐵 PoB
𝑀𝐵 (5)
𝖶 Po 𝑀𝐴
𝐴 A

(Assuming 100% vaporization efficiency)

Knowing the vapor pressure (PA) of turpentine oil (from Hausbrand Vapor Pressure
diagram) at the distillation temp. (T D), amount of open steam required (i.e; amount of
steam condensed per unit weight of turpentine condensed in the distillate) can be
computed. The actual steam requirement is higher due to:
2. Steam is used externally to provide the sensible heat for heating the feed
charge from ambient temp. to the distillation temp.
3. Due to heat losses from the still.
4. Due to in-adequate steam- liquid contact, actual state of equilibrium is difficult
to achieve.
Since vaporization efficiency is usually < I, defining vaporization efficiency  as:

PoA
  𝑃𝐴
Equation (5) is written as:

Chemical Engineering CH23621 50

 = ×
𝖶𝐵 (101.3−𝑛𝑣.𝑃𝐴)
𝑀𝐵
(6)
𝖶 𝑛𝑣.𝑃 𝑀𝐵
𝐴 𝐴

Overall energy balance around the distillation unit shall give the thermal efficiency.

Q𝑜𝑢𝑡
 = Q𝑖𝑛

Qout = WAF (Tb-TR) CpA + A WAD = WS + A WAD

Neglecting heat losses from the still

Qin = WSS + (WBD+WBB) (SCp (TS - TD))

The equipment consists of jacketed pressure vessel for distillation. Steam from a steam generator can
either be allowed to enter in the outer jacket or in the vessel. The vapors form the top of the vessel are
condensed in the shell and tube type condenser by circulating cooling water, supplied by laboratory
overhead tank. The condensate is collected in a separating chamber. The set-up is fitted with steam
trap, control valves, pressure gauge, temperature sensors and other instrumentations required.

EXPERIMENTAL PROCEDURE:

1. Form the Hausbrand vapor pressure diagram for turpentine water system at 101.3 kN/m2
pressure, obtain the distillation temperature, TD, oC( 95°C).
2. Charge the distillation still with 2kg of turpentine oil.
3. Adjust the jacket steam pressure to 170 kN/m2 (Pg,) and start the cooling Water
supply to the condenser. Record the still temp. Collect the steam condensed in the
jacket.
4. When the temp. in the still reaches 2°C below the distillation temp. (Td), the jacket
steam is stopped and the flow of livestream is started through the steam sparger.
The live steam pressure is adjusted around. 150 kN/m2 (Ps).
5. Weigh the steam condensed in the jacket (WS), kg.
6. Continue the distillation process for sufficient time so that about 50-70% turpentine
changed is distilled (around 1 hr).
7. Stop the steam supply and collect the distillation in the 2L separating funnel. Allow
the formation of organic layer and an aqueous layer. Separate the two phases and
weigh them, (WAD, WBD), kg.
8. Collect the residue, separate the two layer and weigh WAB, WBB (kg).
9. Stop the supply to the condenser.

Chemical Engineering CH23621 51

OBSERVATION AND CALCULATIONS:
DATA:
Mol. Wt. of turpentine oil =MA =136.22
Normal boiling point of turpentine oil = 160oC
Sp. heat of turpentine oil at 20°C = CpA = 1.8 kJ/kg °C Sp.
heat of turpentine oil at 50°C = CpA =1.926kJ/kgoC Sp.
heat of turpentine oil at 100°C = CpA = 2.093 kJ/kgoC
Latent heat of vap. of turpentine oil= A = 74 kcal/kg = 309.84 kJ/kg
Mol. wt. of Water= MB = 18

OBSERVATION:

VNaOH = ml

CALCULATIONS:

No. of moles of turpentine oil in feed

WAF
NAF = ----------
MA

No. of moles of turpentine oil in distillate

WAD
NAD = ----------
MA

No. of moles of turpentine oil in Residue

WAB
NAF = -----------
MA

Chemical Engineering CH23621 52

 No. of moles of water in distillate
WBD
NBD = ------------
MB

No. of moles of water in residue

WBB
NBB = ----------
MB

Applying Material balance:

Turpentine Oil:

NAF = NAD + NAB

Vaporization efficiency =

PAC
= ---------
PA

WBD (P -  PA) MB
and = x
WAD  MA

Observed WBD/WAD in distillate

NOMENCLATURE:
WAF = Wt. of turpentine in feed (kg)
TD = Distillation temp. °C
TR = Reference temp. (ambient temp.) °C
Cp = Specific heat of turpentine oil (kJ/kgoC)
A = Latent heat of evaporation of turpentine (kJ/kg)
WAD =Wt. of turpentine in distillate, (kg)
WS = Wt. of Steam Condensed in the jacket during pre-heating or charge (kg)
 = Latent heat of steam corresponding to jacket steam pressure P (kN/m2)
WBD =Wt. of water in distillate (kg)
WBB =Wt. of water in residue, kg
S = Latent heat of steam at live steam pressure PS
(kN/m2) TS = saturation temp. of steam at PS

Cp = Specific heat of steam (kJ/kgoC)

Chemical Engineering CH23621 53

PRECAUTIONS & MAINTENANCE INSTRUCTIONS:
1. Measure the exact volume of water.
2. Always use clean water and good quality chemicals.
3. Use electronic balance for weighing of chemicals.
4. Keep close all the drain valves and vent valve should open while filling the boiler.
5. Flow should not be disturbed during the experiments.
6. Don’t ON heater switch before filling the water in the boiler.

RESULT:

VIVA QUESTIONS:
Define steam distillation
List the application of steam distillation
Define vapour pressure
What are the commom solvents used in steam distillation
What is Hausbrand vapor pressure diagram

Chemical Engineering CH23621 54

EXP.NO:
DATE:

PACKED BED DISTILLATION COLUMN

AIM:
 To investigate the basic principles of Packed bed Distillation Column.
 To distillate the mixture of water and methanol using packed bed distillation column.

INTRODUCTION:
The unit operation distillation is used to separate the components of a liquid solution,
which depends upon the distribution of these various components between a vapor and a liquid phase.
All components are present in both phases. The vapor phase is created from the liquid phase by
vaporization at the boiling point. If a homogeneous liquid solution is boiled, the vapor is richer in the
more volatile components than is the liquid, whereas the remaining liquid is richer in the less volatile
components. The separation of crude petroleum into gasoline, kerosene, fuel oil and lubricating stock
and the separation of a mixture of alcohol and water into its components are examples of distillation.

THEORY:
Distillation may be carried out by either of two principal methods.
1. Based on the production of a vapour by boiling the liquid mixture to be separated and
condensing the vapor without allowing any liquid to return to the still in contact with the
vapor.
2. Based on the return of part of the condensate to the still under such conditions that this
returning liquid is brought into intimate contact with the vapor on their way to the
condenser. Either of these methods may be conducted as a continuous process or as a batch
process.
3. Batch distillation, which is the process of separating a specific quantity of a liquid mixture into
products, is used extensively in the laboratory and in small production units that may have to
serve for many mixtures. In batch distillation, a batch of liquid is charged to the reboiler and
the system is first brought to uniform operation under total reflux. Then a portion of the
overhead product is continuously withdrawn in accordance with the established reflux policy.
The column operates as an enriching section. The progress of batch distillation can be
controlled in several ways.
4. Constant reflux, varying overhead composition. The reflux is set at a predetermined value
where it is maintained for the run. Since the composition of the pot is changing the
composition of the distillate also changes.
5. Constant overhead composition, varying reflux. If it is desired to maintain a constant overhead
composition, the amount of reflux returned to the column must be increased. As time proceeds,
the reboiler is gradually depleted of the lighter component. Finally, a point is reached where
the reflux ratio attains a very high value. The receivers are then changed, the reflux is reduced,
and an intermediate cut is taken.

Chemical Engineering CH23621 55

Bubble Cap Plates:
The vapor and liquid are brought into contact efficiently in distillation via tray towers such
as sieve, valve and bubble-cup trays. The most common gas disperser for cross-flow plates has been
the bubble-cap. This device has a built-in seal which prevents liquid drainage at low gas flow rates.
Gas flows through a centre riser, reverses the flow under the cap, passes downward through the
annulus between riser and cap and finally passes into the liquid through a series of openings or “slots”
in the lower side of the cap.

McCabe Thiele Graphical Method:

Since the composition within the column is continuously changing, rigorous calculation
methods are extremely complex. The McCabe-Thiele graphical method gives a fast and easy but an
approximate solution of binary distillation problems. It is based upon representation of the material
balance equations as operating lines on the x-y equilibrium diagram. The operating lines relate the
composition of liquid leaving the plate to the composition of vapor beneath the plate, and are
determined by material balances. The equilibrium data relate the composition of liquid leaving the
plate to the composition of vapor over the plate. McCabe-Thiele suggested that the operating line be
plotted on the same graph as the equilibrium curve of y versus x, so that the number of equilibrium
stages can be determined by a graphical construction. For methanol water system vapor liquid
equilibrium data is given at Appendix.

Chemical Engineering CH23621 56

  The equation for the operating line

 Where,R is reflux and xD is the composition of distillate.

Density of distillate can be determined by gravimetric analysis, and corresponding mole fraction is
given at Appendix.

Tray Efficiencies:
In the distillation column, tray efficiency compares the vapor temperature leaving a tray to the liquid
temperature leaving the tray. Three kinds of tray efficiency are utilized:
1. Overall efficiency, which concerns the entire column.
2. Murphree efficiency, which has to do with a single plate.
3. Local efficiency, which pertains to a specific location on a single plate.
The overall efficiency is defined as the ratio of the number of ideal trays or plates needed
in an entire column to the number of actual plates
𝑁𝑜 𝑜𝑓 𝑖𝑑𝑒𝑎𝑙 𝑡𝑟𝑎𝑦𝑠(𝑝𝑙𝑎𝑡𝑒𝑠)
𝑂𝑣𝑒𝑟𝑎𝑙𝑙 × 100
𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 = 𝑁𝑜 𝑜𝑓 𝑎𝑐𝑡𝑢𝑎𝑙
𝑡𝑟𝑎𝑦𝑠

This experiment aims to study basic principles of batch distillation in bubble-cap column. McCabe-
Thiele diagram is drawn and number of ideal trays is obtained, then overall efficiency of column is
evaluated.

Chemical Engineering CH23621 57

Chemical Engineering CH23621 58
 The column is made of stainless steel material packed with Borosilicate Glass raschig rings. An
electrically heated re-boiler is installed at the bottom of the column. The bottom product is collected in
the tank. The vapors form the top of column are condensed in the shell and tube type condenser by
circulating cooling water, supplied by laboratory overhead tank. The complete column is insulated for
minimizing the heat loss. Instrumentation is provided for pressure & temperature measurement
wherever necessary.

EXPERIMENTAL PROCEDURE:
1. Make a feed solution at least 20 litre, by adding 15 wt % methanol and 85% water,
then mix the liquid well before fed in to the reboiler.
2. The column takes a long time (about 1 hour) to heat up. Familiarize yourself with the
operation of the column and the Refractometer.
3. Charge the feed to the Reboiler.
4. Start heaters and adjust the temperature of the boiler using DTC. Using the highest
allowable setting will speed the experiment considerably.
5. Open the vent valve time to time to release air from column.
6. As the column heats up, adjust the cooling water flow rate to the condenser so that the
entire vapor is condensed.
7. Allow the mixture to boil in the reboiler and close the vent valve of the condenser shell as
the vapor coming out from the shell.
8. Place the distillate tank at the product outlet point. Keep collecting the distillate from the
condenser.
9. Take the sample of distillate and analyse it under refractometer.
10. The refractometer will show value in percentage of brix sugar (0-85%)
11. A data is given in the manual below, find the refractive index of the product
corresponding to the value obtained from the refractometer.

12. Also, a reference data is given for refractive index and concentration or mole fraction
(methanol) below and hence can be used to figure out the concentration or mole fraction of
the product.
13. Take a final set of readings and switch off the heaters. Shut off all column inputs.

Chemical Engineering CH23621 59

CALIBRATION CURVE/TABLE:
Prepare a calibration curve for CH3OH-Water by plotting R-I as a function of mole fraction CH3OH at
the ambient temperature or at 250C. Prepare different mixtures of CH3OH + Water by volume and
measure the R-I of each mixture. Measure the density of CH3OH (ρA=803 kg/m3) and water
(ρB=1000kg/m3) at the ambient temperature or 250C and knowing the molecular weight of CH 3OH
(MA=32) and Molecular weight of Water (H2O=18). Convert your volume fractions to mole
fractions and plot mole fraction CH3OH vs R-I on a simple graph.

If VA m1 of CH3OH mixed with VB mL of water. Then

Mole Fraction of CH3OH

% of methanol % of water Mole fraction of R.I at 250C

methanol (x)
100 0 1 1.3268
90 10 0.802 1.3300
80 20 0.643 1.3330
70 30 0.512 1.3356
60 40 0.403 1.3381
50 50 0.310 1.3398
40 60 0.231 1.341
30 70 0.162 1.3411
20 80 0.101 1.3394
10 90 0.047 1.3363
0 100 0 1.3321

Chemical Engineering CH23621 60

 % of methanol in water Density(kg/m3)

0 998.2

10 981.5

20 966.6

30 951.5

40 934.5

50 915.6

60 894.6

70 871.5

80 846.9

90 820.2

100 791.7

Plot R.I vs x using excel or plot x vs R.I and fit two polynomials one for CH3OH rich section (to be
used for finding the distillate composition) and the other for water rich section (to be used for finding
the feed and bottoms composition).
At 250C
e.g.
for CH3OH rich section : x = 57.3625- 42.5319 R.I----------------------------------(1)
and for water rich section :x =1865.11-2827.05 R.I + 1071.23 RI2-------------(2)

OBSERVATION& CALCULATION:
DATA:

R-I of Feed :
R-I of Distillate :
R-I of Bottoms :
From the calibration curve, corresponding mole fractions of CH3OH are:
Xf =
XD =

Chemical Engineering CH23621 61

XB =

OBSERVATION TABLE:

S. No. T1 (oC) T2 (oC) T3 (oC) T4 (oC) F (LPH)

1.
2.
3.

x-y data for CH3OH-H2O System

Temperature (0C) x Y
100 0 0
96.4 0.020 0.134
93.5 0.040 0.230
91.2 0.060 0.304
89.3 0.080 0.365
87.7 0.100 0.418
84.4 0.150 0.517
81.7 0.200 0.579
78 0.300 0.665
75.3 0.400 0.729
73.1 0.500 0.779
71.2 0.600 0.825
69.3 0.700 0.870
67.5 0.800 0.915
66 0.900 0.958
65 0.950 0.979
64.5 1 1

Chemical Engineering CH23621 62

PRECAUTIONS & MAINTENANCE INSTRUCTIONS:
1. Use the stabilize A.C. Single Phase supply only.
2. Never switch on mains power supply before ensuring that all the ON/OFF switches
given on the panel are at OFF position.
3. Voltage to heater starts and increases slowly.
4. Keep all the assembly undisturbed.
5. Never run the apparatus if power supply is less than 180 volts and above than 240 volts.
6. Operate selector switch for temperature indicator gently.
7. Do not start heater supply unless water is filled in the test unit.
8. Always keep the apparatus free from dust

RESULT:

VIVA QUESTIONS
What is packed bed distillation
List the application of packed bed distillation
What are the common packing materials used for packed bed distillation
Define calibration curve
Define mole fraction

Chemical Engineering CH23621 63

EX.NO:
DATE:

LIQUID-LIQUID EXTRACTION

AIM:
i.
To determine the overall mass transfer coefficient (KWa) based oncontinuous phase.
ii.
To determine the overall mass transfer coefficient (KTa) based on dispersedphase.
iii.
To determine the overall height of transfer unit (HOW) based on continuous phase.
iv.
To determine the overall height of transfer unit (HOT) based on dispersed phase.
v.
To determine the individual height of transfer unit (HW) based on continuousphase.
vi.
To determine the individual height of transfer unit (HT) based on dispersed phase.

THEORY
Liquid- liquid extraction, sometimes called solvent extraction, is the separation of the
constituents of a liquid solution by contact with another insoluble liquid. If the substances constituting
the original solution distribute themselves differently between thetwo liquid phases, a certain degree of
separation will results, and this can be enhanced byuse of multiple contacts or their equivalent in the
manner of gas absorption and distillation.
Packed towers filled with some random packing (say rasching rings) are widely used for extraction of
valuable chemicals from dilute solutions by liquid-liquid extraction. The packing provides a larger
extract area for mass transfer and also reduces theaxial mixing to some extent. The extraction
rate in such columns depends on:
a) Choice of either continuous or dispersed phase.
b) Packing and column variables.
c) Velocity of the liquid phases in the tower.
For dilute solutions and where the equilibrium relation is straight line, a simpleexpression can
be obtained for determining the required height of a column (Z).

𝐿𝑇𝑑𝐶𝑇 = 𝐾𝑇𝑎(𝐶𝑇 − 𝐶*�

)𝑑𝑍 − − − − − − − − − (1)
�

Where LT, CT, C*T and KTa are volumetric flow rate, concentration of extract material,
concentration of extract material at equilibrium and overall mass transfer coefficient indispersed
phase.

∆𝐶𝑇1 = (𝐶𝑇 −
�𝐶 )
*

∆𝐶𝑇2 = (𝐶𝑇 − �
𝐶*)
�

Chemical Engineering CH23621 64

 (∆𝐶𝑇 ∆𝐶𝑇1 − ∆𝐶𝑇2
)𝐿 = ∆𝐶𝑇1
ln
( )
𝑀
∆𝐶𝑇2

On solving equation (1) became:

𝐿𝑇(𝐶𝑇1 − 𝐶𝑇2) = 𝐾𝑇𝑎(∆𝐶𝑇)𝐿𝑀𝑍 − − − − − − − − − (2)

Where 𝐶𝑇1, ∆𝐶𝑇2, ∆𝐶𝑇1, (∆CT )LM are inlet, outlet concentration, concentration difference at
inlet, concentration at outlet and log mean concentration difference indispersed phase.The overall
mass transfer coefficient based on dispersed phase (toluene), KTa is definedas:

(3)

Where L’T is molar flow rate of toluene and benzoic acid mixture, V is volume of packing.Similarly
overall mass transfer coefficient based on continuous phase (water), KWais defined as:

Where L’w is Malor flow rate of water.

The tower performance is generally based on extraction rate data and evaluated interms of over
all height of transfer unit, based on continuous phase, HOW and the extraction factor expressed in
terms of flow rate ratios of the liquid phases, 𝑚Q𝑊
Q𝑇

Where, m is the slope of equilibrium curve, m = dCW/dCT

Under certain conditions (e.g. low concentrations) m is a constant.As per chilton and colburn, the over all
height of transfer unit based on continuous phase(water), HOW is defined as:

And the overall height of transfer unit based on dispersed phase (toluene), HOT isDefined as:

These two variables are plotted against each other on Cartesian co-ordinates. As suggested by colburn,
the slope and intercept of such a plot would represent the Resistance of the individual films as:

Chemical Engineering CH23621 65

Where HW and HT are the individual height of transfer unit in continuous and dispersed phase.The set up
consists of a glass column packed with rasching rings. Rotameters are provided to measure the flow rate
of solvent and solute. Two feed tanks are given with pump for feed supply. Pressure gauge and pressure
regulator are provided to measure the pressure. Two receiving tank are given to collect extract and
raffinate phase product.

EXPERIMENTAL PROCEDURE:
1. Prepare a mixture of toluene and benzoic acid by mixing 488 gm ofbenzoic acid in 20 liter
of toluene.
2. Take 20 liter of distilled water.
3. Fill one burette by N/20 sodium hydroxide solution.
4. Fill other burette by N/5 sodium hydroxide in alcohol solution.
5. Close all the valves V1-V10.
6. Fill the one feed tank with prepared solution (toluene and benzoicacid)and other with water.
7. Connect compressed air supply to the set-up at the valve V10.
8. Open valve V10 and set air pressure 1.0 to 2.0 kg/cm2 by pressure regulator and pressure gauge.
9. Open the valve V3-V4 and fill mixture solution in feed the tank A.
10. Close the valve V3-V4.
11. Open and adjust the flow control valve V1-V2 for dispersed (toluene+benzoic acid) and
continuous (water) phase to same flow rate values.
12. Wait till steady state achieves (approx 20 to 30 minute).
13. Collect the known amount of sample in measuring cylinder from both the outlet and note down
the volume of sample.
14. Titrate the sample solution of dispersed phase, against N/5 sodium hydroxide in alcohol (add
NaOH from burette) by using phenolphthalein as an indicator.
15. Titrate the sample solution of continuous phase, against N/20 sodium hydroxide in water
(add NaOH from burette) by using phenolphthalein as anindicator.
16. Repeat the experiment for different flow rate of feed mixture and water.
17. When experiment is over stop the flow of feed by close the valve V1-V2.
18. Reduce air pressure to 0 kg/cm2 by pressure regulator and pressure gauge.
19. Drain the packed column and feed tanks by open the valve V7-V9.

OBSERVATION & CALCULATION:

DATA:

EQUIPMENT DATA

Diameter of column Dc = 0.048 m

Packed height of column Z = 0.75 m
Weight of benzoic acid in feed solution WB = gm
Molecular weight of benzoic acid MB = 122 g/mole
Volume of toluene in feed solution V = Lit

Chemical Engineering CH23621 66

Normality of NaOH used to titrate the sample of dispersed phase N2 = 0.05 g eq/L
Normality of NaOH used to titrate the sample of continuous phase N1 = 0.2 g eq/L

Inlet concentration of benzoic acid in continuous phase CW 2 = 0 k mole/m3

DATA:

EQUILIBRIUM DATA FOR BENZOIC ACID - TOLUENE - WATER SYSTEM

CW (g mole/L) CT (g mole/L)

0.0000 0.0000
0.0016 0.0080
0.0064 0.0336
0.0080 0.0673
0.00961 0.08811
0.011211 0.12015
0.012816 0.14097
0.01442 0.17301

6.2 OBSERVATION TABLE:

S.No. QT (LPH) QW (LPH) V1 (ml) V2 (ml) VT (ml) VW (ml)

Chemical Engineering CH23621 67

CALCULATIONS:

Plot the graph of CW Vs CT of equilibrium data and find the slope ‘m’.

m=
𝜋
𝐴 = 𝐷2(𝑚2)
4
𝐶 𝐶

𝑉𝐶 = 𝐴𝐶𝑍(𝑚3)

𝑊𝐵
𝐶 = (𝑘𝑚𝑜𝑙/𝑚3)
𝑇1 𝑉 × 𝑀𝐵

𝑁𝑇 𝑁1
= 𝑉1 (𝑔 𝑒𝑞/𝐿)
𝑉𝑇

𝐶𝖶1 = 𝑁𝑇(𝑘𝑚𝑜𝑙/𝑚3)

𝑁𝖶 𝑁2
= 𝑉2 (𝑔 𝑒𝑞/𝐿)
𝑉𝖶

𝐶𝑇2 = 𝑁𝖶(𝑘𝑚𝑜𝑙/𝑚3)

𝐶w1
𝐶. = (𝑘𝑚𝑜𝑙/𝑚3)
𝑇1 𝑚
𝐶w2
𝐶. = (𝑘𝑚𝑜𝑙/𝑚3)
𝑇2 𝑚

∆𝐶𝑇1 = (𝐶𝑇1 − 𝐶𝑇1)(𝑘𝑚𝑜𝑙/𝑚3)

∆𝐶𝑇2 = (𝐶𝑇2 − 𝐶𝑇2)(𝑘𝑚𝑜𝑙/𝑚3)

(∆𝐶𝑇1 − ∆𝐶𝑇2)
∆𝐶𝑇 =
(𝑘𝑚𝑜𝑙/𝑚3)
𝑖𝑚 ∆𝐶𝑇1
ln( )
∆𝐶𝑇2

Chemical Engineering CH23621 68

𝐿𝑇 𝑄𝑇×10−3
= (𝐶𝑇2 − 𝐶𝑇1)(𝑘𝑚𝑜𝑙/𝑠)
3600

Chemical Engineering CH23621 69

 𝐿𝑇
𝐾𝑎 = (𝑘𝑚𝑜𝑙/𝑚3𝑠(𝑘𝑚𝑜𝑙/𝑚3))
𝑇
𝑉𝐶 × ∆𝐶𝑇𝑖𝑚

𝐻0𝑇 = 𝑄𝑇×10−3
𝐾𝑎 × 3600(𝑚)
×𝐴
𝑇 𝐶

𝐶𝖶. = 𝑚 × 𝐶𝑇1(𝑘𝑚𝑜𝑙/𝑚3)
1

𝐶𝖶. = 𝑚 × 𝐶𝑇2(𝑘𝑚𝑜𝑙/𝑚3)
2

∆𝐶𝖶1 = (𝐶𝖶1 − 𝐶𝖶1)(𝑘𝑚𝑜𝑙/𝑚3)

∆𝐶𝖶2 = (𝐶𝖶2 − 𝐶𝖶2)(𝑘𝑚𝑜𝑙/𝑚3)

(∆𝐶𝖶1 − ∆𝐶𝖶2)
∆𝐶𝖶 = ∆𝐶
(𝑘𝑚𝑜𝑙/𝑚3)
𝑖𝑚 ln(∆𝐶 𝖶1)
𝖶2

𝐿𝖶 𝑄𝖶 × 10−3
= (𝐶𝖶2 − 𝐶𝖶1)(𝑘𝑚𝑜𝑙/𝑠)
3600
𝐿𝖶
𝐾𝑎 = (𝑘𝑚𝑜𝑙/𝑚3𝑠(𝑘𝑚𝑜𝑙/𝑚3))
𝖶
𝑉𝐶 × ∆𝐶𝖶𝑖𝑚

𝐻0𝖶 = 𝑄𝑎𝖶 × 10
−3

𝐾 × 3600(𝑚)
×𝐴
𝖶 𝐶

CALCULATION TABLE:

KTa KWa HOT HOW

S. No QT QW m (kmole/ (kmole/ (m) (m)
m3s(kmo m3s(kmo
(LPH) (LPH) (QW/QT)
le/m3)) le/m3))

Chemical Engineering CH23621 70

 NOMENCLATURE:

Nom Column Heading Units Type

Ac Area of the column Calculated

m2
CT Concentration of benzoic acid in dispersed phase gmole/L Given
CT1 Inlet concentration of benzoic acid in dispersed phase Kmole/m3 Calculated
C*T1 Inlet concentration of benzoic acid in dispersed phaseat Kmole/m3 Calculated
equilibrium

CT2 Outlet concentration of benzoic acid in dispersed phase Kmole/m3 Calculated

C*T2 Outlet concentration of benzoic acid in dispersed phaseat Kmole/m3 Calculated
equilibrium
CW Concentration of benzoic acid in continuous phase gmole/L Given

CW1 Outlet concentration of benzoic acid in continuousphase Kmole/m3 Calculated

Outlet concentration of benzoic acid in continuousphase at

equilibrium
C*W1 Kmole/m3 Calculated
CW2 Inlet concentration of benzoic acid in continuous phase Kmole/m3 Given

Inlet concentration of benzoic acid in continuous phaseat Kmole/m3 Calculated

equilibrium
C*W2
Dc Diameter of column m Given
HOT Overall height of transfer unit based on dispersedphase m Calculated

HOW Overall height of transfer unit based on continuousphase m Calculated

HT Individual height of transfer unit based on dispersedphase m Calculated

HW Individual height of transfer unit based on continuousphase m Calculated

KTa Overall mass transfer coefficient based on dispersedphase (kmole/m3s Calculated

(kmole/m3))
KWa Overall mass transfer coefficient based on continuousphase (kmole/m3s Calculated
(kmole/m3))
LT Molar flow rate of dispersed phase Kmole/s Calculated
LW Molar flow rate of continuous phase Kmole/s Calculated

Chemical Engineering CH23621 71

MB Molecular weight of benzoic acid g/mole Given
M Slope of the graph CW vs CT * Calculated
N1 Normality of sodium hydroxide used to titrate thesample of g eq/L Given
continuous phase
N2 Normality of sodium hydroxide used to titrate thesample of g eq/L Given
dispersed phase
NT Normality of benzoic acid in dispersed phase g eq/L Calculated
NW Normality of benzoic acid in continuous phase g eq/L Calculated
QT Volumetric flow rate of toluene (dispersed phase) LPH Measured
QW Volumetric flow rate of water (continuous phase) LPH Measured
V Volume of toluene in feed solution Lit Given
V1 Volume of sample taken from continuous phase ml Measured
V2 Volume of sample taken from dispersed phase ml Measured
Vc Volume of the column Calculated
m3
VT Volume of sodium hydroxide used to titrate the ml Measured
sampleof dispersed phase
VW Volume of sodium hydroxide used to titrate the sample ml Measured
of continuous phase
WB Weight of benzoic acid in feed solution gm Given
Z Packed height m Given
∆CT1 Inlet concentration differenceB of benzoic acid indispersed Kmole/m3 Calculated
phase
∆CT2 Outlet concentration difference of benzoic acid indispersed Kmole/m3 Calculated
phase
( ∆CT)lM Log mean concentration difference of benzoic acid in Kmole/m 3 Calculated
dispersed phase
∆CW1 Outlet concentration difference of benzoic acid Kmole/m3 Calculated
incontinuous phase
∆CW2 Inlet concentration difference of benzoic acid incontinuous Kmole/m3 Calculated
phase
( ∆CT)lM Log mean concentration difference of benzoic acid in kmole/m 3 Calculated
continuous phase

Symbols are unit less.

Chemical Engineering CH23621 72

PRECAUTION & MAINTENANCE INSTRUCTIONS:

Interface should not be disturbed during the experiment.

Don’t exceed the flow rate more than 15 LPH.
Water outlet should be toluene free.
Always use clean water & ensure that there are no foreign particles in it.
Always clean the column feed tanks & receiving tanks properly after experiment.
Never use feed tanks to store the chemicals used in the experiment.
Always drain the column once before running the experiment on desired secondflow rates.

RESULT

VIVA QUESTIONS
Define liquid liquid extraction
What solubility curve
Define extract and raffinate
List some application LLE
Give significance of ternary diagram

Chemical Engineering CH23621 73

EXP.NO:
DATE:

ION EXCHANGE APPARATUS

AIM:
To study the softening of water by ion exchange apparatus.
THEORY:
The usual ion exchange material employed in water softening is a sulphonated styrene- based
resin, supplied in the sodium form. This has a strong affinity for calcium and magnesium ions
and will also remove ferrous ions after the almost complete removal of calcium and
magnesium. Softening may be carried out as a batch process by stirring a suspension of resin
in the water until equilibrium or an accepable level of hardness is reached. It is more
convenient to operate as a continuous flow process, passing the water slowly downwards
through a column of resin beads. The exchange reaction takes place rapidly enough for the
upper layers of the bed to approach exhaustion before the lower layers are able to exchange
ions Thus there is a zone of active exchange which moves down the column until the resin at
all depths becomes exhausted. When the zone of active exchange reaches the bottom of the
column the emerging water begins to show an increasing hardness. This is the breakthrough
point when it becomes necessary to regenerate the resin with a strong sodium chloride
solution.
Of all different natural and synthetic products which show ion exchange properties, the most
important are ion-exchange resins, ion-exchange coals, mineral ion exchangers, and synthetic
inorganic exchangers. Ion exchangers owe their characteristic properties to a peculiar feature
of their structure. They consist of a framework held together by chemical bonds or lattice
energy which carries a positive or negative surplus charge. Counter ions of opposite charge
move throughout the framework and can be replaced by other ions of same sign. For
example, the framework of a cation exchanger can be regarded as a macromolecular or
crystalline polyanion, while the framework of an anion exchanger can be regarded as a
polycation.
The setup consists of two glass columns packed with Cation and anion exchange resins and
one feed tank. Water is fed to the columns through feed tank with the help of a pump. The
flow rate can be adjusted by operating the valve provided. Samples can be taken periodically
from the top outlet of column
EXPERIMENTAL PROCEDURE:
1. Start with any flow rate of water, regulated by feed valve and metered by a rotameter.
2. When the flow rate gets stabilized (steady state is reached).
3. Start the stop watch simultaneously. Collect in 5 beakers about 50-100 ml of exit
stream sample from the top at regular interval of time.
4. Take the sample and check outlet concentration using conductivity meter.
5. Care should be taken to minimize the error in sampling.
6. Above step may be repeated for at least 2-3 flow rates of water.

73
Chemical Engineering CH23621
OBSERVATION & CALCULATION:
Data:
Initial concentration - C0,

ppm Final concentration – Cf,

ppm OBSERVATION
TABLE

S.No. t, min Ion concentration (ppm)

Plot a graph of concentration versus time.

Concentration Time

NOMENCLATURE:

Cf = Final Concentration of ions in water sample, ppm

Ci = Initial Concentration of ions in water sample,
ppm

PRECAUTIONS & MAINTENANCE INSTRUCTIONS:

1. Always use clean water.
2. Keep close all the drain valves while filling the reactant in feed tank.
3. Flow should not be disturbed during the experiments.

RESULT
VIVA QUESTION
Define process of ion exchange

Chemical Engineering CH23621 74

List the application of ion exchange.

Chemical Engineering CH23621 75

EXP.NO:
DATE:

ABSORPTION IN PACKED BED APPARATUS

AIM:
 To estimate, Noy, Numbers of transfer unit, (NTU).
 To estimate, Hoy, Height of transfer unit, (HTU).
 To plot KGa (kgmolels/m3-h-atm) vs. mass velocity of liquid.

THEORY:
Absorption is the one of the many separation process is used in chemical engineering. In absorption a
component of gas stream is removed by passing a stream over the surface of a liquid, the component
to be removed being preferentially soluble in the liquid. Large surface area and intimate contact
between the gas and liquid are obviously desirable. There are many devices used to achieve this end,
the most common of which is packed tower. This consist of a glass column filled with raching rings
which occupy the space but leave voids between the pieces. Thus a liquid stream can be introduced
into the top of the tower and flow down over the surface of the pieces, creating a large surface area for
a given volume of liquid. The gas to be treated is introduced into the tower and flows through the
voids where it comes into intimate contact eith the surface of the liquid In absorption, a gas mixture is
contacted with a liquid for preferential dissolution of one or more components of the gas in the liquid.
Such operations require transfer of mass from gas stream to liquid. In case of absorption wit chemical
reaction, (Here CO2 absorption in NaOH solution). Reaction of absorbed solute provides higher
absorption rates due to:
 Destruction of the absorbed solute as it forms a compound reduces the equilibrium partial
pressure of the solute that in turn increases the concentration difference between the bulk
phase & the interface.
 Increase in liquid phase mass transfer co-efficient.
The equilibrium partial pressure is zero (Y* = 0) (If reaction is reversible).

The experimental set up consists of glass column packed with Rasching rings . One feed tanks
through which chemicals are fed to the column with the help of compressor. The flow rates can be
adjusted by operating the needle valve and measured by rotameter.

Chemical Engineering CH23621 76

One mixing chamber is provided for mixing of CO2 and air, then this mixture is entered into the
column from bottom. For analysis samples are collected fromport is provided at the downside.
UTILITIES REQUIRED:
Electricity Supply: Single Phase, 220 VAC, 50 Hz, 5-15 amp combined socket with earth connection.
Floor Drain.
Floor Area 1.5 m x 1m.
Laboratory glass ware :-
Conical Flask (250 ml) : 03
No. Measuring cylinder (50 ml) : 02
No. Beakers (250 ml) : 02
No. Burette (50 ml) with stand : 01
No. Funnel : 01 o.
Chemicals Required:
N/10 NaOH : 20 Liters.
N/10 HCL : 05Liters
Indicator (Phenolphthalein) : Few drops

EXPERIMENTAL PROCEDURE:
1. Prepare 20L of N/10 NaOH solution by dissolving 80 gm of NaOH in 20L of water.
2. Fill the respective tanks with this solutions.
3. Record column diameter and packed height.
4. Start the compressor and adjust the flow of air with help of pressure regulator.
5. Adjust the flow rate of the feed and select one flow rate .
6. Select the flow rate of CO2& Air (V) & record it.
7. Measure the inlet concentration of CO2 in gas stream ya.
8. Run the experiment at the selected value of L for 15-20 Mining. Measure the concentration
of CO2 in outlet gas stream, yb.
9. Select another liquid flow rate (L) & repeat steps 5 & 6.
10. Repeat step 7 for at least for 5 liquid rates.

OBSERVATION& CALCULATION:
DATA:
Room Temp. (T) =................oC

Atmospheric Pressure (P) = ………

Column Diameter (Dc) = ……….
Crossectional Area of Column(S) = ………...
Total Packed Height (ZT) = ……

Chemical Engineering CH23621 77

OBSERVATION
TABLE: TABLE-1:

S.No. Gas flow Gas density Gas av. Gas mass Mole fraction of CO2
rate, Q (at mol wt., M Velocity, V
PT& T)ρ In outlet gas
In inlet gas y [NaOH]i-
b
ya [NaOH]o

TABLE-2:

S.No. Liquid Liquid Liquid mol. wt.

ML Liquid mass velocity
flow rate, density
L=1 ρL / MLS
1 ρL

TITRATIONS:

Chemical Engineering CH23621 78

 S.No. Vol. of Vol of HCL used
outlet

2𝑉2−𝑉1×𝑁
sample, using using for Na2CO3 for [NaOH]o
V ml. phenolphthalein methyl 2(V1-V2) NaOH

𝑉
V2 orange V1 2V1-V2

Nomenclature:

KGa = Gas phase mass transfer co-

efficient.
Kya = Overall mass transfer co-efficient.
Noy = Number of transfer unit (NTU).
Hoy = Height of transfer unit (HTU).
ya = Mole fraction of CO2 in inlet gas.
ya = Mole fraction of CO2 in outlet gas.
ZT = Total packed height.
V = Gas mass velocity, kgmol/h-m2.
V’ = Molal gas flow rate. kgmol/h.

RESULTS:

Chemical Engineering CH23621 79

EX.NO:
DATE:
VAPOUR LIQUID EQUILIBRIUM

AIM:
To plot the vapour-liquid equilibrium curve for carbon tetrachloride–toluene mixture.
THEORY:
The design of distillation and other contacting equipment requires reliable VLE data. It shows the
relationship between the composition of the vapor and that of liquid in equilibrium with the
vapor for a binary mixture at constant pressure or constant temperature. Although relatively few
ideal solutions are known whose equilibrium relations can be calculated from vapor pressure –
temperature data of the pure components, by far the larger numbers of systems of industrial
importance are non-ideal;and attempts to predict the equilibrium compositions of such mixtures from
theoretical considerations alone have not proved successful. It has been the practice to determine such
data experimentally under various conditions.
Vapour liquid diagram shows relationship between the composition of the vapor and that of liquid in
equilibrium with the vapor for a binary mixture at constant pressure or constant temperature. The
basic data of any distillation problem are the equilibrium between the liquid and vapour phases of
the system subjected to distillation. Hence is of great importance to study the vapour-liquid
equilibrium.
Theoretical VLE curve can thus be calculated by choosing various boiling points of the mixture and
calculate x and y. Carbon tetrachloride and toluene system closely follows ideal behavior. The set-up
consists of distillation still with a heating element. An electrical dimmer stat is connected to heating
element for varying heat input. The vapours form the top of column are condensed in the concentric
tube type condenser by circulating cooling water. The condensate is feedback to column as reflux. A
tank with pump is provided to circulate cold water to condenser. Flow rates can be regulated
through control valve fitted. Instrumentation is done to measure the temperatures at different points.
UTILITIES REQUIRED:
Electrical Supply: Single Phase, 220 V AC, 50 Hz, 5-15 Amp combined socket with earth
connection. Earth voltage should be less than 5 volts.
Water Supply (Initial fill) 6.3 Floor Drain Required. 6.4 Chemicals:
Carbon tetrachloride : 500 ml
Toluene : 700
ml EXPERIMENTAL PROCEDURE:
1. Prepare solution of toluene (Or Water) and carbon tetrachloride (Or Methanol) 500 ml
with 100 ml of CCl4.
2. Close all the valves .
3. Ensure that switches given on the panel are at OFF position.
4. Fill water in the water tank.

Chemical Engineering CH23621 80

 5. Charge the feed solution in the distillation still by open the feed supply valve .
6. Switch ON the power supply.
7. Switch on the heater.
8. For input to heater a variac is provided (70-80 volts).
9. When temperature starts increasing, switch ON the pump.
10. Operate the flow control valve and allows cooling water to pass through the condenser.
11. Maintain temperature above 70oC and below 100oC by rotating the variac provided.
12. After observing constant temperature, collect sample of distillate by open the distillate valve
at the bottom of the condenser.
13. Analyze the sample with Refractrometer.
14. Enter the value of RI of sample collected in software.
15. Repeat the experiment for different feed mixture (Increase the composition of CCL4
or Methanol).
16. When experiment is over switch OFF the pump.
17. switch OFF the heater.
18. Switch OFF the main power supply.
19. Drain the vessel by open the drain valve .
OBSERVATION & CALCULATION:

DATA: 1(FOR CARBON TETRACHLORIDE & TOULENE)

= 15.8742 A' =16.0137

= 2808.19 B' =3096.52
= 227.01 C' =219.33
Boiling Point of CCl4 = 76.5 (oC) Boiling Point of Toluene = 110.6 (oC)

DATA:1 (For CCl4 & Toluene system)

Y 1.000 0.917 0.846 0.733 0.6470.579 0.524 0.468 0.397 0.306 0.180 0.000

RI1.4495 1.453 1.456 1.461 1.4641.467 1.469 1.475 1.477 1.480 1.4831.488

DATA: 2(FOR METHANOL & WATER)

= 18.61042 A' = 18.5882

= 3392.57 B' = 3984.92
= 230 C' = 233.43
Boiling Point of Methanol = 64.5 (oC) Boiling Point of Water = 100 (oC)

Chemical Engineering CH23621 81

 DATA:2 (For Methanol & Water system)

Y
0 0.1 0.2 0.3 0.36 0.40 0.50 0.60 0.70 0.80 0.90 0.92

0.94 0.96 1.0

RI 1 3
1.332 1.336 1.3394 1.3411 1.3411 1.3410 1.3398 1.3381 1.3356 1.3330 1.330 1.3294

1.3286 1.3280 1.326

Chemical Engineering CH23621 82

 OBSERVATION :

Sr.No T1 (oC) T2 (oC) R.I F (LPH)

CALCULATIONS:

𝑌𝐴 = (−24.2 × 𝑅. 𝐼 + 36.1)
[For CCl4-Toluene System]

𝑌𝐴 = (−43.982 × 𝑅. 𝐼. +59.279)
[For Methanol-Water

System]

CALCULATION TABLE:

S. No. T2 (oC) YA XA

Plot the Graph Between T2 Vs YA & XA.

Chemical Engineering CH23621 83

 NOMENCLATURE:

Nom Column Heading Units Type

A Antoine Equation Constant Parameter 1 for * Given
Component A
A' Antoine Equation Constant Parameter 1 for * Given
Component B
B Antoine Equation Constant Parameter 2 for * Given
Component A
B' Antoine Equation Constant Parameter 2 for * Given
Component B
C Antoine Equation Constant Parameter 3 for * Given
Component A
C' Antoine Equation Constant Parameter 3 for * Given
Component B
Pva Vapour Pressure of Component A mmHg Calculated
Pvb Vapour Pressure of Component B mmHg Calculated
R.I Refractive index of sample solution * Measured
T1 Temperature of feed solution oC
Measured
T2 Temperature of vapour oC
Measured
YA Mole fraction of component A in vapour phase * Calculated
XA Mole fraction of component A in liquid phase * Calculated
άab Relative Volatility of Component A with respect to * Calculated
Component B

* Symbols represent unit less quantity.

PRECAUTION & MAINTENANCE INSTRUCTIONS:

1. Fill the vessel at-least half of its capacity.

2. Drain the vessel and water tank after completion of the experiment.
3. Don’t run the pump before filling the tank with water.
4. Don’t start the heater before filling the chemicals into the still.
RESULT:

VIVA QUESTIONS:

Define vapor liquid equilibrium

How antoine equation is applied in VLE Define
relative volatility
What is mole fraction of A in vapor phase and liquid phase Give
the significance of VLE curve.

Chemical 83
Engineering CH23621