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Er. PERUMAL MANIMEKALAI

POLYTECHNIC COLLEGE
NBA Accredited: Chemical | CSE | ECE | EEE | MECH | T&D | E (Robotics)

ISO 9001: 2015 Certified Institution

(Approved by AICTE, New Delhi and Government of Tamil Nadu)Koneripalli,

Hosur - 635 117.

DEPARTMENT OF CHEMICAL ENGINEERING

A TEXT BOOK ON
MASS TRANSFER -I
(TN DOTE N SCHEME)

(For V-Semester Diploma in Chemical Engineering)

COURSE CO ORDINATOR : M.DHILIP

DESIGNATION : LECTURER
NAME OF THE COURSE : MASS TRANSFER - I
SAR/COURSE CODE : C501/C4076510
YEAR / SEM : III / V

PREPARED BY APPROVED BY
Mr.M.DHILIP M.E Mrs.K.RENUGADEVI M.E
LECTURER/ CHEMICAL HOD/ CHEMICAL
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Vision of the Institution

PMC Tech Polytechnic College shall emerge as a premier Institute for valued added technical
education coupled with Innovation, Incubation, Ethics and Professional values

Mission of the Institution

1. To foster the professional competence through excellence in teaching and learning.

2. To nurture overall development of students by providing Quality Education & Training.
3. To provide innovative environment to learn, innovate and create new ideas for the betterment
of oneself and society.

DEPARTMENT OF CHEMICAL ENGINEERING

Vision of the Department

To prepare the chemical engineers who can pursue their goals which will benefit the society and
environment.

Mission of the Department

1. Impart Quality education and training in Chemical Engineering and associated fields to
enable the students to imbibe technical and analytical skills through logical thinking.
2. Groom the students with leadership skills, professional Ethics, transparency and
accountability with technical knowledge
3. Inculcate sense of social and environmental responsibility among students which inspires
them to apply Chemical Engineering principles in solving industrial problems through
sustainable and eco-friendly technologies for betterment of industry and nation.

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Programme Educational Objectives (PEO’s)

After the completion of this course, the students will be able to:

Have good training in fundamental and advanced concepts of Chemical and allied
PEO 1 Engineering for good career in industry or for Higher Studies.
Demonstrate professional excellence, ethics, soft skills and leadership qualities through
PEO 2 skill development
Contribute to the economic and environment of their communities by providing
PEO 3 opportunities for innovation and lifelong learning

Programme Specific Outcomes (PSO’s)

After the completion of this course, the students will be able to:

Apply knowledge of the basic science, mathematics and chemical engineering in the design
PSO 1
and operations of chemical processes.
Have an ability to identify, formulate, and solve complex problems in the various domains
PSO 2 of chemical engineering such as momentum transfer, heat transfer, mass transfer and
mechanical operation in chemical process industries
Possess the attitude of innovation and lifelong learning as per the need of wider context of
PSO 3
technological changes in the field of chemical engineering

PROGRAMME OUTCOMES

PO1: Basic and Discipline specific knowledge: Apply knowledge of basic mathematics, science and
engineering fundamentals and engineering specialization to solve the engineering problems.

PO2: Problem analysis: Identify and analyse well-defined engineering problems using codified standard
methods.

PO3: Design/ development of solutions: Design solutions for well-defined technical problems and assist with
the design of systems components or processes to meet specified needs.

PO4: Engineering Tools, Experimentation and Testing: Apply modern engineering tools and appropriate
technique to conduct standard tests and measurements.

PO5: Engineering practices for society, sustainability and environment: Apply appropriate technology in
context of society, sustainability, environment and ethical practices.

PO6: Project Management: Use engineering management principles individually, as a team member or a
leader to manage projects and effectively communicate about well-defined engineering activities.

PO7: Life-long learning: Ability to analyse individual needs and engage in updating in the context of
technological changes.

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COURSE OBJECTIVE:
To understand the fundamentals of mass transfer mechanisms in fluids and solids and their applications
in various mass transfer equipment in process industries

CURRICULAM TABLE:

UNIT TOPIC HOURS PER UNIT

PRINCIPLES OF MASS TRANSFER
I 15Hrs
ABSORPTION
II 20Hrs
HUMIDIFICATION
III 20Hrs
FUNDAMENTALS OF DISTILLATION
IV 16Hrs
DESIGN AND TECHNIQUES OF DISTILLATION COLUMN
V 18Hrs

TOPICS BEYOND THE SYLLABUS: DESIGN TECHNIQUES AND 05Hrs

CALCULATIONS OF REACTIVE DISTILLATION PROCESS.

TEST AND MODEL EXAM

7Hrs
TOTAL
101Hrs

C4076510 - MASS TRANSFER - 1

DETAILED SYLLABUS

UNIT NAME OF THE TOPICS & DESCRIPTION Hrs

PRINCIPLES OF MASS TRANSFER

Diffusion and mass transfer operation- molecular diffusion and eddy diffusion - Fick's
law of diffusion-.Equimolar counter diffusion-special case Diffusion of A through
stagnant non-diffusing B-.Mass transfer coefficients – units of mass transfer coefficient-
I relation between mass transfer coefficients -inter phase mass transfer- Overall mass 17
transfer coefficient.
Classification of mass transfer operations - methods of conducting mass transfer
operations - unsteady state and steady state operations-stage wise and differential contact
operation
ABSORPTION

Principles of Gas absorption - equilibrium solubility of gases - ideal and non-ideal liquid
solutions - Henry's Law - choice of solvent for absorption-absorption factor - Tray towers
II and packed towers for absorption –equilibrium curve and operating line for absorption- 20
concepts of minimum Gas-Liquid ratio.
Construction and principle of operation of packed bed absorption column- packing
materials- random packing and regular packing-Operating problems like loading,
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flooding, entrainment, priming, weeping

and coning – HTU, NTU and HETP concepts.
HUMIDIFICATION

Humidification operation-Terminology used in humidification operation such as

Absolute humidity , Molal humidity , Dry bulb temperature , Wet bulb temperature ,
Relative humidity ,Percentage saturation ,Dew point, Adiabatic saturation temperature
III ,Humid heat and Humid volume -Lewis relation- simple problems in Humidification
20
Equipment for Humidification operations-construction and working principle of cooling
towers - arrangements of cooling towers- natural draft, forced draft and induced draft –
Cooling tower efficiency – common problems in cooling tower and solutions.
FUNDAMETALS OF DISTILLATION

Distillation- relative volatility- boiling point diagram and equilibrium diagram–

construction of boiling point and equilibrium diagram for a binary system using vapour
pressure data - Raoult's law –azeotropic mixture- maximum and minimum boiling
IV azeotropes – simple or differential distillation- Rayleigh's equation- flash distillation –
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vacuum distillation- continuous multistage rectification.
Dimensionless numbers in mass transfer and its significance- Schmidt number, Lewis
number, and Sherwood number (Brief description only).
DESIGN AND TECHNIQUES OF DISTILLATION COLUMN

Tray towers - calculation of number of trays - McCabe Thiele method - Assumptions in

McCabe-Thiele method -Graphical procedure to determine the number of theoretical
trays -total reflux - minimum reflux - optimum reflux- q line –values of q based on five
V different feed conditions-operating lines – feed tray location.- Types of distillation
15
column trays- Types of plate efficiencies- Overall efficiency and Murphree plate
efficiency.
Azeotropic distillation - Extractive distillation - Steam distillation.

COURSE OUTCOMES:
After the completion of this course, the students will be able to:

DOTE
BLOOMS
COURSE COURSE OUTCOMES
LEVEL
CODE

C4076510.1 Explain the fundamentals of mass transfer operation. Un

C4076510.2 Analyze gas absorption and tower characteristics. AN

Design cooling tower and calculate rate of mass transfer in

C4076510.3 Cr
humidification.

C4076510.4 Explain enhanced distillation. Un

C4076510.5 Design calculation of distillation columns. Cr

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COURSE OUTCOMES VS PO’S MAPPING

DOTE

PSO3
PSO1

PSO2
COURSE OUTCOMES-BRIEF

PO6
PO1

PO2

PO3

PO4

PO5

PO7
COURSE
CODE
Explain the fundamentals of
C4076510.1 3 3 1 1 3 3 2 3 3 2
mass transfer operation.
Analyze gas absorption and
C4076510.2 3 1 3 1 2 3 2 3 2 2
tower characteristics.
Design cooling tower and
C4076510.3 calculate rate of mass 3 3 3 1 3 3 2 3 3 3
transfer in humidification.
Explain enhanced
C4076510.4 3 1 3 1 2 3 2 3 2 2
distillation.
Design calculation of
C4076510.5 3 3 3 1 2 3 2 3 3 3
distillation columns.

C4076510 CO average 3 2.2 2.6 1 2.4 3 2 3 2.6 2.4

DETAILED:

HIGH : 3 MEDIUM: 2 LOW: 1* For Entire Course, PO /PSO Mapping; 1 (Low); 2(Medium); 3(High)
Contribution to PO/PSO

CONTENTS

Unit.No Unit Title Page. No

1 PRINCIPLES OF MASS TRANSFER

8

2 ABSORPTION
27

3 HUMIDIFICATION
37

4 FUNDAMETALS OF DISTILLATION 61

5 DESIGN AND TECHNIQUES OF DISTILLATION

COLUMN 71

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UNIT-I
PRINCIPLES OF MASS TRANSFER
Introduction
When a system contains two or more components whose concentrations vary from point to point,
there is a natural tendency for mass to be transferred, minimizing the concentration differences within a
system. The transport one constituent from a region of higher concentration to that of a lower
concentration is called mass transfer.
The transfer of mass within a fluid mixture or across a phase boundary is a process that plays a
major role in many industrial processes. Examples of such processes are:
 Dispersion of gases from stacks
 Removal of pollutants from plant discharge streams by absorption
 Stripping of gases from waste water
 Neutron diffusion within nuclear reactors
 Air conditioning
Many of our day-by-day experiences also involve mass transfer.
For example:
1. A lump of sugar added to a cup of coffee eventually dissolves and then eventually diffuses to
make the concentration uniform
2. Water evaporates from ponds to increase the humidity of passing-air stream
3. Perfumes present a pleasant fragrance, which is imparted throughout the surrounding atmosphere.
The mechanism of mass transfer involves both molecular diffusion and convection.
Molecular Diffusion and Eddy Diffusion
The mass transfer of the species from a region of higher concentration to a region of lower
concentration is accomplished by the migration of molecules; this phenomenon is called molecular
diffusion.
Molecular diffusion is concerned with the movement of individual molecules through a substance
by virtue of their thermal energy.
The kinetic theory of gases provides a means of visualizing what occurs and quantitatively
describes the diffusional phenomenon.
In the kinetic theory, a molecule is imagined to travel in a straight line at a uniform velocity until
it collides with another molecule, whereupon is velocity changes both in magnitude and direction.
The phenomenon of molecular diffusion ultimately leads to a completely uniform concentration of
substances throughout a solution which may initially have been non uniform.
Thus for example, if a drop of blue CuSO4 solution is placed in a beaker of water, the CuSO4
eventually permeates the entire liquid. The blue colour in time becomes everywhere uniform, and no
subsequent change occurs.

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Molecular diffusion is a slow process, and the more rapid mixing which can be brought about by
mechanical stirring and convective movement of the fluid Consider a tank as shown in the following
figure. Here a 0.75 m - deep layer of pure water has been carefully placed over the brine solution without
disturbing the brine solution in any way.

If the contents of the tank are left completely, undisturbed by molecular diffusion, the salt will completely
permeate the liquid, ultimately coming everywhere to one-half its concentration in the original brine. But
this process is very slow, and it is estimated that the salt concentration at the top of the surface will be
only 87.5% of its final value after 10 years and will reach 99% of its finalvalue only after 28 years. Now
consider the following figure.

If we place a simple paddle type agitator rotating in the same tank as shown in the above figure at
22 rpm will bring complete uniformity in about 1 min. The mechanical agitation has produced rapid
movement of relatively large chunks or eddies, of fluid characteristic of turbulent motion, which has
carried the salt with them. This method of solute transfer is called as eddy or turbulent diffusion.
FICK'S LAW OF DIFFUSION
Molecular diffusion or molecular transport can be defined as the transfer or movement of
individual molecules through a fluid by means of the random, individual movements of the molecules.
We can imagine the molecules traveling only in straight lines and changing direction by bouncing off
other molecules after collision. Since the molecules travel in a random path, molecular diffusion is often
called a random-walk-process.

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In the following figure the molecular diffusion process is shown schematically. A random path that
molecule A might take in diffusing through b molecules from point (1) to (2) is shown. If there are a
greater number of A molecules near point (1) than at (2), then, since molecules diffuse randomly in both
directions, more A molecules will diffuse from (1) to (2) than from (2) to (1). The net diffusion of A is
from high to low concentration regions.
If a drop of blue liquid dye is added to a cup of water. The dye molecules will diffuses slowly by
molecular diffusion to all parts of the water .To increase this rate of mixing of the dye, the liquid can be
mechanically agitated by a spoon and convective mass transfer will occur.
First, we will consider the diffusion of molecules when the whole bulk fluid is not moving but is
stationary. Diffusion of the molecules are due to a concentration gradient. The general Fick's Law
equation can be written as follows for a binary mixture of A and B.
JAZ = -cDAB dx/dz ------ (1)
Where, c is total concentration of A and B in kg mol of A + B/m³, and
xA is the mole fraction of A in the mixture of A and B.
If c is constant, then since cA = cxA
cdxA = d(cxA) = dcA ------- (2)
Substitute equation (2) in (1) we get the following equation for total constant concentration:
JAZ= -DAB dc dz ------- (3)
This is the more commonly used equation in molecular diffusion.
For steady state, the flux JAZ in the above equation is constant. Also DAB constant. Rearranging the
equation (3) and integrating.

Where, CA1 & CA2 is concentration of component A at point I and at point 2, (Z2-Z2) is distance between
the points 1 and 2.
For ideal gases,

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Where, PA1 & PA2 is partial pressure of component A at point I and at point 2 respectively.
MOLECULAR DIFFUSION IN GASES: (A) Equimolar Counter Diffusion in Gases:

In the above figure a diagram is given of two gases A and B at constant total pressure in two large
chambers connected by a tube where molecular diffusion at steady state is occurring. Stirring in each
chamber keeps the concentration in each chamber uniform. The partial pressure PP. Molecules of A
diffuse to the right and B to the left. Since the total pressure P is constant throughout, the net moles of A
diffusing to the right must equal the net moles of B to the left. If this is not so, the total pressure would
not remain constant. This means that,

This shows that for a binary gas mixture of A and B, the diffusivity coefficient D, for A diffusing into B is
the same as D, for B diffusing into A.

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(B). Diffusion of gases A and B plus Convection

Up to now we have considered Fick's law for diffusion in a stationary fluid; that is, there has been
no net movement or convective flow of the emire phase of the binary mixture A and B. The diffusion flux
J, occurred because of the concentration gradient. The net rate at which moles of A passed a fixed point to
the right, which will be taken as a positive flux, is JA kg mol A/s.m2. This flux can be converted to a
velocity of diffusion of A to the right by
JA (kg.mol A/s.m2) = VADCA (m/s * kg.mol.A / m3) --------- (6)
Where, VAD - is the diffusion velocity of the A in m/s
Now let us consider what happens when the whole fluid is moving in bulk or convective flow to
the right. The molar average velocity of the whole fluid relative to a stationary point is vm m/s.
Component A is still diffusing to the right, but now its diffusion velocity v AD is measured relative to the
moving fluid. To stationary observer A is moving faster than the bulk of the phase, since its diffusion
velocity is added to that of the bulk phase vm. Expressed mathematically, the velocity of A relative to the
stationary point is the sum of the diffusion velocity and the average or convective velocity:
VA =VAD +VM --- (7)
Where, VA is the velocity of A relative to the stationary point.
Multiplying the equation (7) by CA
CAVA = CAVAd + CAVM --- (8)
Each of the three terms represents a flux.
Where, CAVA=NA = Total flux of A relative to the stationary point in (kg.mol of A/sm2)
CAVAd = JA = Diffusion flux relative to the moving fluid,
CAVM = Convective flux relative to the stationary point.
Hence the Eqn. (8) becomes
NA = JA + CAVM ------ (9)
Let N be the total convective flux of the whole stream relative to the stationary point. Then,
N = CVM = NA+NB
NA+ NB
VM = ------- (10)
C

Substituting Eqn. (10) in Eqn. (9),

CA
NA = J A + (NA+NB) ------- (11)
C

But Fick's law is,

dXA
JA = - CDAB dZ

Then the Eqn. (11) becomes,

dXA CA
NA = - CDAB + (NA +NB) ------ (12)
dZ C

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This is the general equation for diffusion plus convection to use when the flux N, is used, which is related
to stationary point. A similar equation for B can be written as,
dXB CB
NB = - CDBA + (NA +NB) ------ (12)
dZ C

(C). Special case of A Diffusing through Stagnant, non-diffusing B

The case of diffusion of A through stagnant or non diffusing B at steady state often occurs. In this case
one boundary at the end of the diffusion path is impermeable to component B, so it cannot pass through.
One example, shown in the above figure, is an evaporation of a pure liquid such as benzene (A) at the
bottom of a narrow tube, where a large amount of inert or non diffusing air (B) is passed over the top. The
benzene vapour (A) diffuses through the air (B) in the tube. The boundary at the liquid surface at point I
is impermeable to air, since air is insoluble in benzene liquid. Hence air (B) cannot diffuse into or away
from the surface. At point 2 the partial pressure, P=0, since a large volume of air passing by. To derive the
case for A diffusing in stagnant, non-diffusing B, N = 0 is T substituted into the general equation (12).

This is the general flux equation for diffusion of A through stagnant and non diffusing B.
Mass Transfer Coefficients
Definition

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To increase the rate of mass transfer per unit area, turbulent flow is desired in all mass transfer
operations. In such cases, the mass transfer rate is expressed in terms of mass transfer coefficients. The
flux equations for such situations are as follows:
Flux = (Mass transfer Co efficient) x (Concentration gradient)
As the concentration can be expressed in number of ways, we have a various types of mass transfer
coefficients.
Mass transfer coefficient is defined as the rate of mass transfer per unit area per unit concentration
gradient. The flux equation obtained for the steady state equimolar counter for turbulent motion becomes
NA = DAB.P / RTZG (pA1-pA2)
For a given situation, the term DAB.P / RTZG transfer film coefficient for the gas, K’G
NA = K’G (pA1-pA2)
The flux equation obtained for the steady state diffusion of A through non- diffusing B for turbulent
motion may be written as:
NA = DAB.P / RT(z2-z1)pBM * (pA1-pA2)

Where
ZL= the effective laminar film thickness and
kL = the mass transfer film coefficient for the liquid
Mass transfer film coefficient may be defined as the rate of mass transfer from the bulk of one phase to an
interface of unit area for unit driving force.
The flux equation for transfer of A through non-transferring B in terms of the driving force
expressed in terms of concentration and mole fraction are:

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Relation between mass transfer coefficients:

Interphase Mass Transfer:

So far we considered mass transfer from a fluid phase to another phase which was the most often a
solid phase. The A was usually transferred from the fluid phase by convective mass transfer and through
solid by diffusion. In this section we shall be concerned with the mass transfer of solute A iro one fluid
phase by convection and then through a second fluid phase by convection. For example, the solute may
diffuse through a gas phase and then diffuse through and be absorbed in an adjacent and immiscible liquid
phase. This occurs in case of absorption of ammonia from air by water.
The two phases are in direct contact with each other, such as in a packed tower, tray tower or
spray type tower, and the interfacial area between the phases is usually not well defined. In two phase
mass transfer, a concentration gradient will exist in each phase, causing mass transfer to occur. At the
interface between the two fluid phases, equilibrium exists in most cases.
Local two phase mass transfer coefficients:
In the majority of mass transfer systems, two phases, which are essentially immiscible I each other, are
present together with an interface between these two phases. Assuming solute A is diffusing from the bulk
gas phase G to the liquid phase L. it must pass through phase G, through the interface, and into the phase
E in series. A concentration gradient must exist to cause this mass transfer through the resistances in each
phase, as shown in the following figure.

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The concentration of A in the main body of the gas is "yAG" mole fraction, where yAG (pA/P), and the
concentration of A in the main body of the bulk liquid phase is 'XAL.
The concentration in the bulk gas phase 'yAG decreases to "yAi at the interface. The liquid
concentration starts at 'x' at the interface and falls to XAi the interface, since there would be no resistance
to transfer across this interface, y and XA, are in equilibrium and are related by the equilibrium
distribution relation,
yAi = f (xAi) Where yAi is a function of xAi
From the above figure it is clear that the concentration rise at the interface, from to X, is not a
barrier to diffusion in the direction gas to liquid. They are T equilibrium concentrations and hence
correspond to equal chemical potentials of A in both phases at the interface.
The various concentrations can also be shown in the following graph, whose coordinates are those
of the equilibrium-distribution curve. Point P represents the two bulk phase concentrations and M those at
the interface.
For steady state mass transfer, the rate at which A reaches the interface from the must equal that at
which it diffuses to the bulk liquid, so that no accumulation or c gas depletion of A at the interface occurs.
We can write the flux of A in terms of mass transfer coefficients from each phase and the concentration
changes appropriate to each. Thus, when ky and k, are the locally applicable coefficients,
NA = ky ( yA,G – yA,i) = kx (xA,i– xA,L) ----------- (1)
Where, ky is the gas phase mass transfer coefficient in kg.mol/s.m2 mol fraction,

Kx is the liquid phase mass transfer coefficient in kg.mol/s.m2 mol fraction.

Rearranging the above eqn. (1),

The driving force in the gas phase = (yA,G – yA,i)

The driving force in the liquid phase = (xA,i – xA,L)
The slope of the line PM = - kx / ky

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This means that if the two film coefficients kx and ky are known the interface k compositions can be
determined by drawing line PM with a slope of - kx / ky intersecting the equilibrium line.
The bulk phase concentrations yA,G and xA,L can be determined by simply sampling A. G the mixed bulk
phase and sampling the mixed bulk liquid phase. The interface concentrations are determined by the
above eqn. (2).
Overall mass transfer coefficients:
Film or single phase mass transfer coefficients ky and k, are often difficult to measure
experimentally, except in certain experiments designed so that the concentration difference across one
phase is small and can be neglected. As result, overall mass-transfer coefficients K, and K, are measured
bsed on the gas phase or Su liquid phase.
This method is used in heat transfer, where overall heat transfer coefficients are measured based
on inside or outside areas instead of film coefficients.
The overall mass transfer coefficient Ky is defined as,

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1/ kx =1/ky
The Liquid Phase Is Controlling And XA,i = X*A

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CLASSIFICATION OF MASS TRANSFER OPERATIONS

Mass transfer operations are classified as follows,
 Direct contact of Two immiscible phases,
 Phases separated by membrane,
 Direct contact of Miscible phases,
 Use of Surface Phenomena, and
 Direct and indirect operations.
Direct contact of two immiscible phases:
The three states of aggregation, gas, liquid, and solid, permit six possibilities of phase contact.
Gas-liquid
If all components of the system distribute between the phases at equilibrium, the operation is
known as fractional distillation (Distillation).
In this instance the gas phase is produced by application of heat; or th conversely liquid is created
from the gas by removal of heat.
For example, if a liquid solution of acetic acid and water is partially vaporized by heating, it is
found that the newly created vapor phase and the residual liquid contain acetic acid and water but in
different proportions.
If a mixture of ammonia and air is contacted with water, a large portion w of ammonia, but not air
will dissolve in water, ammonia and water are separated. This operation is called gas absorption.
If air is brought into contact with ammonia-water solution, some of the ammonia will leave the
liquid and enters the air. This operation called as t desorption or stripping.
If dry air is contacted with liquid water, some of the water will evaporates and enters into the air,
this is called humidification of air.
Conversely, contact of very moist air with pure liquid water may results condensation of part of
moisture in the air, this is called dehumidification of air.

Gas-solid
If a solid solution is partially vaporized without the appearance of a liquid phase, the newly
formed vapor phase and the residual liquid solid cach contains all the original components, but in
different proportions, and the operation is fractional sublimation.
Not all components may be present in both the phases, however. If a solid which is moistened with
a volatile liquid is exposed to a relatively dry gas. the liquid leaves the solid and diffuses into the gas, an
operation generally known as drying.
If the diffusion of gas is takes place in the opposite direction, the operation is known as
adsorption.
If a mixture of water vapor and air is brought into contact with activated silica gel, the water vapor
diffuses to the solid, which retains it strongly and the air is dried.

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Liquid-liquid
Separations involving the contact of two insoluble liquid phases are known as liquid- extraction
operations.
For example, if an acetone water solution is shaken in a separatory funnel with carbon tetra
chloride and the liquid allowed to settle, a large portion of the acetone will be found in the carbon tetra
chloride -rich phase, and thus separated from the water.
Liquid-solid
When all the constituents are present in both the phases at equilibrium, we have the operation of
fractional crystallization.
For example, zone refining, which is used to obtain ultra pure metals and semiconductors.
Another example is adductive crystallization, where a substance such as urea, has a crystal lattice
which will selectively entrap long straight- chain molecules like the paraffin hydrocarbons.
Cases where the phases are solutions containing but one common component occur more
frequently. Selective solution of a component from a solid mixture by a liquid solvent is known as
leaching.
Solid-solid
Because of the extraordinary slow rates of diffusion within solid phases, there is no industrial separation
in this category.
Phases separated by membrane:
In this method separation of components is carried out in the presence of col membrane.
Membranes are operating in different ways; they serve to prevent intermingling of two miscible
phases. Membranes also prevent the ordinary hydrodynamic flow, And movement of substance through
them is by diffusion.
Membranes permit a component separation by selectively controlling passage of the components
from one side to the other.
Gas-gas
In gaseous diffusion or effusion, the membrane is micro porous.
If a gas mixture whose components are of different molecular weights is brought into contact
with such diaphragm, the various components of the gas pass through the pores at rates dependent upon
the molecular weights.
This leads to different compositions on opposite sides of the membrane and consequent separation
of the mixture.
For example, separation of isotopes of uranium, in the form of gaseous uranium hexafluoride.
In permeation, the membrane is not porous, and the gas transmitted through the membrane first
dissolves in it and then diffuses through.
Separation in this case is brought about by difference in the solubility of the components.

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Gas-liquid
These are permeation separations where, for example, a liquid solution of alcohol and water is
brought into contact with a suitable nonporous membrane.
In which the alcohol preferentially dissolves. After passage through the membrane the alcohol is
vaporized on the other side.
Liquid-liquid
The separation of a crystalline substance from a colloid, by contact of their solution with a liquid
solvent with an intervening membrane permeable only to the solvent and the dissolved crystalline
substance, is known as dialysis.
For example, aqueous beet- sugar solutions containing undesired colloidal material are freed of
the latter by contact with water with an intervening semi permeable membrane.
Sugar and water diffuse through the membrane, but the larger colloidal particles cannot.
If an electromotive force is applied across the membrane to assist in the diffusion of the charged
particles, the operation is electro dialysis.
Direct contact of miscible phases
Because of the difficulty in maintaining concentration gradients without mixing the fluid, the
operation in this category are not generally considered.
Thermal diffusion involves the formation of a concentration difference within a single liquid or
gaseous phase by imposition of a temperature gradient upon the fluid.
Thus making a separation of the components of the solution possible. In this way, 3He is separated
from its mixture with 4He.
If a condensable vapor, such as steam, is allowed to diffuse through a gas mixture, it will
preferentially carry one component along with it, thus making a separation by the operation known as
sweep diffusion.
If the two zones within the gas phase where the concentrations are different are separated by a
screen containing relatively large openings, the operation is called atmolysis.
If a gas mixture is subjected to a very rapid centrifugation, the components will be separated be
cause of the slightly different forces acting on the various molecules owing to their different masses. *.
The heavier molecules thus tend to accumulate at the periphery of the centrifuge. This method is used for
separation of uranium isotopes.
Use of Surface Phenomena:
Substance which when dissolved in a liquid produce a solution of lowered surface tension are
known to concentrate in solution at the liquid surface.
By forming a foam of large surface, as by bubbling air through the solution, and collecting the
foam, the solute can be concentrated.
In this manner, detergents have been separated from water, this operation is known as foam
separation.

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Direct and indirect operations:

The operations depending upon contact of two immiscible phases s particularly can be further sub
classified into two types.
The direct operations produce the two phases from a single-phase c solution by addition or
removal of heat.
Examples are fractional distillation, fractional crystallization, and one form of fractional
extraction.
The indirect operations involve addition of foreign substance and include gas absorption and
stripping, adsorption, drying, leaching, liquid extraction.
Methods of Conducting Mass Transfer Operations:
The following are the important methods to conduct mass transfer operations.
Solute Recovery and Fractionation
If the components of a solution fall into two distinct groups of quite different properties, so that
one group of components constitutes the solvent and the other group the solute.
Separation according to these groups is usually relatively easy and amount to a solute recovery
or solute removal operation.
For example, a gas consisting of methane, pentane, and hexane can be imagined to consist of
methane as solvent with pentane plus hexane as solute.
The solvent and solute in this case differing considerably in at least one property, vapor pressure.
A simple gas- absorption operation, washing the mixture with nonvolatile hydrocarbon oil, will
easily provide a new solution of pentane plus hexane in the oil, essentially methane free.
And the residual methane will be essentially free of pentane and hexane. On the other hand, a
solution consisting of pentane and hexane alone can not be classified so readily.
While the components properties differ, the differences are small, and separate them into relatively
pure components requires a different technique, suc as fractionations.
Unsteady-State operation
An operation in which the values of any one of process variables like, temperature, pressure,
volume and concentration are changing with time, such operation is called unsteady state operation or
process. The change in concentration with time may result from changes in concentrations of feed
materials, flow rates, or conditions of temperature or pressure.
In any case, batch operations are always of the unsteady-state type.
In purely batch operations all the phases are stationery from a point of view outside the apparatus,
i.e., no flow in or out, even though there may be relative motion within.
For example, the familiar laboratory extraction procedure of shaking a solution with an
immiscible solvent.

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In semi batch operations, one phase is stationary while the other flows continuously in and out of
the apparatus.
For example, drier where a quantity of wet solid is contacted continuously with fresh air, which
carries away the vaporized moisture until the solid, is dry.
Steady-State Operation
An operation in which the values of any one of the process variables like Temperature, Pressure,
Volume and Concentration etc are do not change with time such operation is called steady state
operations.
Steady state operation requires continuous, invariable flow of all phases into and out of the
apparatus, and a persistence of the flow regime within the apparatus.
For example, all continuous operations are steady-state operations.
Stage wise operation
If two insoluble phases are first allowed to come into contact, the various substances will start to
distribute themselves between the phases. To separate these two phases, mechanical separation methods
like filtration and decanting are followed.
The combined operation (equipments) which involves the above said phase distribution and
separation is called one stage.
Example: Separation of oil and water mixture by using separating funnel in laboratory.
In order to get greater concentration changes, any number of stages can be arranged in series, such
arrangement is called a cascade. Equibrium stage or theoretical stage is defined as one in which the
effluent (both the phases) are in equilibrium (same composition).
Once the equilibrium reached, there will not be any further diffusion of component between the
phases even though for longer time of contact. The approach to equilibrium realized in any stage is then
defined as the stage of efficiency.
Stage wise operation can be carried out in continuous fashion or batch wise fashion.
Differential contact (continuous contact) operation
If the phases flow through the equipment in continuous, intimate contactthroughout, without
repeated physical separation and recontacting is called differential contact or continuous contact
operation. This can be either semi batch or continuous fashion.
In this operation equilibrium between the phases is never established at any position in the
equipment. So that the diffusional flow of components between thephases is continuing without
interruption.
For low stage efficiency operation, the differential contact operation is more desirable for reasons
of cost and certainity.

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UNIT-I
PRINCIPLES OF MASS TRANSFER
Diffusion and mass transfer operation- molecular diffusion and eddy diffusion - Fick's law of diffusion-
.Equimolar counter diffusion-special case Diffusion of A through stagnant non-diffusing B-.Mass transfer
coefficients – units of mass transfer coefficient-relation between mass transfer coefficients -inter phase mass
transfer- Overall mass transfer coefficient. Classification of mass transfer operations - methods of
conducting mass transfer operations - unsteady state and steady state operations-stage wise and differential
contact operation
PART – A

Q.NO QUESTIONS CO Map BT MARKS

1 Define Mass transfer with example? CO 1 Re 3

2 What are the types of diffusion? CO 1 Re 3
3 What is meant by Molecular diffusion & Eddy (or) turbulent diffusion ? CO 1 Re 3
4 State Fick’s Law of diffusion? CO 1 Re 3
5 What is meant by Inter-phase mass transfer? CO 1 Re 3
6 Define mass transfer flux? CO 1 Re 3
7 Write the classification of mass transfer? CO 1 Re 3
8 What is meant by Equimolar counter diffusion? CO 1 Re 3
9 Define thermal diffusion and sweep diffusion? CO 1 Re 3
10 Write methods of mass transfer operations? CO 1 Re 3
11 Define steady state and unsteady state operation? CO 1 Re 3
12 Define mass transfer coefficient? CO 1 Re 3
13 Write the equations of total flux , diffusion and convective flux ? CO 1 Re 3
14 Write the example of direct, indirect mass transfer operations? CO 1 Re 3
PART-B
1 Discuss various mass transfer equipments involved in separation process. CO 1 Cr 14
2 Explain fick’s law of diffusion and Equimolar counter diffusion? CO1 UN 14
Derive the expression for special case of diffusion of A through non-diffusing CO 1
3 Ap 14
B.
Derive the expression for overall mass transfer co-efficient from local two CO 1
4 Ap 14
phase mass transfer coefficient.
5 Explain with detail on mass transfer coefficient and explain fick’s law? CO 1 Un 14
6 Explain with details on classification of mass transfer operation? CO 1 Un 14
7 Explain with details on methods of conducting mass operation? CO 1 Un 14

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UNIT-II
ABSORPTION
Introduction
Principle of Gas absorption
Gas absorption is an operation in which a gas mixture is contacted with a liquid for the purpose of
preferentially dissolving one or more components of the gas and to provide a solution of them in the
liquid. This is also called scrubbing.
Examples:
The gas from by-product coke ovens is washed with water to remove ammonia and again with an
oil to remove benzene and toluene vapours
Removal of H2S from naturally occurring hydrocarbon gases by washing with various alkaline
solutions in which it is absorbed.
A mass transfer operation which occurs in reverse of absorption. i.e. transfer of gas is from liquid
to gas is called desorption or stripping.
Example:
Benzene and toluene are removed from the absorption oil mentioned above by contacting the
liquid with steam.
Equilibrium solubility of gases
The rate at which a gaseous constituent of a mixture will dissolve in an absorbent liquid depends
upon the departure from equilibrium with exist.
Two component system:
If a quantity of a single gas and a relatively non-volatile liquid are brought to equilibrium, the
resulting concentration of dissolved gas in the liquid is said to be the gas solubility at the prevailing
temperature and pressure.
At fixed temperature the solubility concentration will increase with pressure.
 Solubility of various gases in water is as shown in the above fig.
 Different gases and liquids yields separate solubility curve, which must ordinarily be determined
by experimentally for each system.
 If the equilibrium pressure of a gas is low as in the curve 'c', the gas is highly soluble in the liquid.
 The equilibrium solubility of gas is influenced by the temperature, in most cases the solubility of a
gas decreases with increasing temperature.
 On the other hand, the solubility of many of the low molecular-weight gases such as H2, O2, N2
and CH4 in water increases with increased temperature about 100°C and above atmospheric
pressure.

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Multicomponent System:
 If a mixture of gases is brought into contact with a liquid, under certain conditions the equilibrium
solubility's of each gas will be independent of the others.
 If all but one of the components of the gas are substantially insoluble, their concentrations in the
liquid will be so small that they cannot influence the solubility of the relatively soluble
component.
IDEAL AND NON-IDEAL SOLUTIONS
Ideal Solutions:
A solution which follows raoult's law, that solution called ideal solution. Raoult's states that,
When the gas mixture in equilibrium with an ideal liquid solution also follows the ideal gas law,
the partial pressure P of a solute gas equals the products of its vapour pressure 'P' at the same temperature
and its mole fraction in the solution 'x'.
i.e.
p* = Pvx
Where, p*-partial pressure
Pv - vapour pressure
An ideal solution can also be defined as a solution in which there is complete uniformity of cohesive
forces. i.e. the molecules in an ideal solution will exert the same force on each other irrespective of their
nature.
For ideal solutions there is neither absorption nor evolution of heat in mixing the constituents.
The volume of the solution varies linearly with composition, the total volume equal to the sum of volume
of individual components.
The total vapour pressure of the solution varies linearly with composition expressed as mole fractions.

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 Example: solution of benzene in toluene solution of ethyl and propyl alcohol and solution of
paraffin hydrocarbon gases in. paraffin oils.
NON-IDEAL SOLUTIONS:
A solution which does not obey or which deviates from Raoult's law is called non-ideal solution.
Non-ideal solution can also be defined as a solution in which there is n complete uniformity of cohesive
force. The molecules in the non ideal solution having different molecular structure. Hence the cohesive
force between the molecules is not same.
For non-ideal solution, enthalpy or heat evolution or absorption are takes place dosing mixing the
constituents. The volume of the solution does not vary linearly with composition. The suitable law used to
express non-ideal solution is Henry's law.

Example: acetone-carbon disulphide, choloroform-ethyl alcohol & benze cyclohexane etc.

HENRY'S LAW
To illustrate the obtaining of experimental gas-liquid equilibrium W data, the system SO2-air-
water is considered. An amount of gaseous SO2, air, and a water are put in a closed container and shaken
repeatedly at a given temperature C until equilibrium is reached. Samples of the gas and liquid are
analyzed to determine the partial pressure p, in atm of SO2 (A) in the gas and mole fraction x XA in the
liquid. The following figure shows a plot of partial pressure pa of SO2 in the vapor in equilibrium with
the mole fraction x, of SO; in the liquid at 293K.

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Henry's Law states that the equilibrium relation between pa in the gas phase and x can be expressed by
straight line. Henry's law equation at low concentrations:
PA=HxA
Where, H is the Hendry's Law constant in atm/mole fraction for the given system. If both sides of the
above equation are divided by total pressure P in atm.
yA = H'xA
Where, H' is Henry's law constant in mole fraction gas/ mole fraction of liquid and is equal to H/P. note
that H' depends on total pressure, whereas H does not.

Choice of Solvent for Absorption

Selection suitable solvent for absorption is important one the following properties of solvent are to
be considered,
Gas Solubility:
The solubility of a solute in the solvent should be high i.e, the solvent should have high capacity
to dissolve large amount of solute with less amount of solvent.
For good solubility the solvent of chemical nature similar to that of the solute, must be searched
out.
Volatility: As gas
leaving the absorber is generally saturated with the solvent there will be a loss of solvent with gas during
absorption. To minimize the solvent loss, the solvent should be less volatile, i.e, solvent should have low
vapor pressure at the operating conditions.
Corrosive nature:
Solvent should not be corrosive to the common materials of construction so that the construction
material for absorber will not be too expensive.
Viscosity:
The solvent should have low viscosity for rapid absorption rates, low pumping cost and better heat
transfer.
Cost and Availability:
The solvent should be cheap, so that losses are not costly, should be readily available.
Miscellaneous:
The solvent should be non-toxic, non- flammable and chemically -stable for handling and storage.
Absorption factor:
Absorption factor is a ratio of slope of the operating line to the slope of the equilibrium curve.
This is given by A =L/mg. For quick calculation the economical 'A' value in the range of 1.25 to 2.0. This
provides a quick method of estimating theoretical number of stages or transfer units in absorbers and
strippers.

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A=L / mG
For tray tower:
Number of theoretical stages, For absorber,

EQUILIBRIUM CURVES AND OPERATING LINES

Equilibrium curve:
Equilibrium curve is a curve, obtained by plotting the values of x and 'y
Where,
x-Mole fraction of solute in liquid phase,
y- Mole fraction of solute in gas phase.
Equilibrium curve for acetone -water system is explained below,
For acetone-water system McCabe gives us equilibrium data in terms of partial pressure of
acetone in the gas phase, p, as a function of mole fraction of acetone in liquid, ‘xA’,
i.e. P̅A=Pvap(xA)ℽA ----------(1)
Where,
Pvap-Vapor pressure of acetone = 0.33 atm.
ℽA -Activity coefficient for liquid mixture.
Activity coefficient is a measure of non ideality of the liquid phase For ideal solutions the activity
coefficient is unity.

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i.e, y, 1(For ideal solution)

For ideal solution the above equation (1) is reduces to Raoult's law Our solution of acetone in
water is not ideal solution, but McCabe kindly gives us a model.

From the above equation (5) we can get the equilibrium data ‘YA’ for different ‘XA’ and equilibrium curve
is plotted as shown below.

Operating line for absorber and stripper:

Consider an absorber shown below, in which gas and liquid flows counter currently.

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Material balance:
Let, GS = Inert gas flow gas
G1 = Leaving gas rate (total)
G2 =Entering gas rate (total)
L1 = Total entering liquid flow rate
L2 =Total leaving liquid flow rate
LS =Pure solvent flow rate
y2 = Composition of solute in entering gas in mole fraction
y1 = Composition of solute in leaving gas in mole fraction
x2 = Composition of solute in leaving liquid in mole fraction
x1 = Composition of solute in entering liquid in mole fraction
X₁ = Composition of solute in entering liquid in mole ratio
X2 = Composition of solute in leaving liquid in mole ratio
Y₁ =Composition of solute in leaving gas in mole ratio
Y2= Composition of solute in entering gas in mole ratio

Overall material balance:

L1+G₂= L₂+ G₁
Component balance (mole fraction):
L₁ X1+ G₂ y₂ = L2X₂+ G₁ Y₁
Component balance (mole ratio):
LS X1+GS Y2 = GS y1+ LSX₂

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GS(Y2-Y₁)=LS(X2-X₁)
(Y2 - Y1)= Ls\GS (X₂-X₁)
This is the equation of operating line which is a straight line passing through the points (Y2,X2) and
(Y1,X1) with a slope of (LS/GS).
Other equations used for calculations are,
X=x\ 1-x , Y= y \1-y

Minimum Gas-Liquid Ratio:

In the design of absorber, the feed gas flow rate, gas stream inlet and exit concentrations and
liquid stream exit concentration are fixed by process requirements. But only the quantity of liquid to be
used subject to choice.

In the figure (a) the operating line must pass through point D and must end at the ordinate Y₁. If
such quantity of liquid is used to give operating line DE, the exit liquid will have the composition X1. If
less liquid is used, the exit-liquid composition will clearly be greater, as at point F, but since the driving

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forces for diffusion are less, the absorption is more difficult. Then the time of contact between gas and
liquid must then be greater, and the absorber must be correspondingly taller. The minimum liquid which
can be used corresponds to the operating line DM, which has the greatest slope for any line touching the
equilibrium curve and is tangent to the curve at P. At P the diffusional driving force is zero, the required
time of contact for the concentration change desired is infinite. This then represents the limiting liquid-gas
ratio.
The equilibrium curve is frequently concave upward, As in figure (b), and the minimum liquid-gas
ratio then corresponds to an exit- liquid concentration in equilibrium with the entering gas.

TRAY TOWER

Construction:
Tray towers are vertical cylinders in which the liquid and gas are contacted in step wise fashion.
Construction of tray tower is as shown in the following figure The tower is usually made up of any of the
following materials, Glass, Glass lined metal, impervious carbon, plastics even wood also used. But most
frequently metal is used.

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Inside the tower large number of trays/plates is mounted to increase the area of contact between
gas and liquid. Equal space maintained between the trays/plates. Trays are usually made up of sheet metal
of special alloys, if necessary. Trays spacing is choosing on the basis of construction, maintenance. cost
and height of tower, and number of trays. Three types of trays are commonly used.
o Bubble cap tray/Plate
o Sieve tray/Plate
o Valve tray/Plate
In tray towers, trays/plates are provided with down comers and weirs. The function of the down
comer is to provide a passage for the downward flow of the liquid from a top tray to a lower tray. The
down comer area for each tray is limited to 10% of total area of the plate. Various types of down comers
are used as follows.
o Pipe type,
o Segmental type, and
o Chord type.
Weir is used to maintain a depth of liquid on each tray required for contacting with gas.
Operation:
In tray absorption tower gas enters at the bottom of the tower and leaves at the top. The liquid
enters at top and leaves at bottom. From the top, the liquid flows down by gravity, on the way, it flows
across each tray and through downspout to the tray below. The gas passe upward through the openings at
one sort or another in the tray, then bubbles through the liquid to form a froth, then the gas disengages
from the froth, and passé on to the next tray above the overall effect is multiple counter current contact of
gas and liquid, although each tray is characterized by a cross flow of the two. Each tray of the tower is
stage, since on the tray the fluids are brought into intimate contact, interface diffusion occurs, and the
fluids are separated.
The following are important problems/difficulties arise during the operation of tray towers.

Packed Tower
Construction
The device consists of a cylindrical column equipped with a gas inlet and distributing space at the
bottom, a liquid inlet and distributing space at the top. gas and liquid outlets at the top and bottom
respectively and a supported mass of invert solid shapes called packings. In general, shell of the column
may be constructed from metal, ceramics, glass or plastic material or metal from corrosion resistant
lining. The column must be mounted vertically for uniform liquid distribution. The following are the
important parts of packed tower.
(i). Distributors:
At the top of the packed column bed, a liquid distributor of suitable design provides for the
uniform irrigation of the packing. The following are the different types of distributors.
 Orifice type,
 Notched chimney type.

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 Notched trough distributor type, and

 Perforated ring type distributor.
(ii). Redistributor: If the tower is high, redistributing plates are necessary for uniform liquid flow. These
plates are needed at intervals of about 2.5 to 3 column diameters for raschig ring and 5 to 10 column
diameter for pall rings, but usually not more than 6 m apart.
(iii). Packing supports: An open space at the bottom of the tower is required for ensuring good
distribution of the gas into the packing. Consequently, the packing id must be supported above the open
space. The support must be reasonably strong to a carry the weight of a reasonable height of packing and
must have ample free area e for the flow of liquid and gas with the minimum of restriction.
iv) Entrainment eliminators. When the gas velocities are very high, the gas leaving the top of the packing
may carry off droplets of liquid as a mist. To avoid this entrainment eliminator are installed at the top of
the tower.
(v). Hold down plate: It is placed at the top of a packed tower to minimize movement and breakage of the
packing cost by the surges in flow rates. (vi) Packings Tower is packed with packing materials to increase
the interfacial area for contacting gas and liquid. There are two types of packings are used,
(a) Random packing, and
(b). Regular packing.
(a) Random packing:
In this, packing materials are simply dumped into the tower during installation and allowed to fall
at random.
Common types of random packings are raschig rings, lessing rings, berl saddle, intallox saddle, pall
rings, cascade rings and tellerates.
(b) Regular packing:
In this, packing materials are arranged in a proper manner. Common types of regular packings are
stacked rashig ring, wood grids or hurdle and knitted or gauge like arrangements.
(vii). Packing restrainers:
It is necessary when gas velocity is high and is used to guard against lifting of packing during
sudden gas surge. Heavy screens or bars are used as packing restrainers.
Operation:
The liquid is introduced from top through liquid distributor, which irrigates the packings
uniformly and liquid trickles down the bed, and finally liquid phase (solute + solvent) leaves the bottom
of the column. The liquid flow rate should be sufficient for good wetting of packing. The gas is
introduced from the bottom of the tower and rise upward. The lean gas leaves the tower from the top.

PACKINGS
Many types of packings are in use ranging from simple to complex geometric shapes packings are
made of ceramics, metals and plastics and vary in re from 6 to 75 mm.

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Characteristics of Tower Packings

 It should provide large interfacial area for phase contacting. i.e. it should have large wetted
surface area per unit volume of packed space for high efficiency.
 It should provide large void volume or empty space in a packed bed so that reasonable
throughput of phases is handled without excessive pressure drop.
 It should posses good wetting characteristics. It should have high corrosion resistance
 It should have low bulk density so that the weight of entire packed bed is low which
thereby reduces serious support problems.
 It should posses enough structured strength.
 It should be chemically inert to the fluids in the tower.

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Types of packings:
There are two types of packings are used as follows.
i. Random packing
ii. Regular packing
Random Packings
Random packings are simply dumped into the tower during installation and allowed to fall at
random. The materials used earlier are stone, gravel, lumps of coke etc. common types of random packing
materials are.
 Rashig ring
 Lessing ring
 Berl ring
 Intallox saddle
 Pall rings
 Partition rings, and
 Tellerate

Some random lower packings: (a) Raschig rings, (6) Lessing ring. (c) partition ring, (d) Berl saddle fcoursery of
Maurice A. Knight). (e) Intalox saddle (Chemical Processing Products Dica Norton Co.). Tellerette (Ceilcote
Company, Inc), and (g) pall ring (Chemical Processing Products

Generally random packings offer layer specific surface in the smaller sizes. but cost less per unit
volume in large sizes.
During installation packings are poured into the tower to fall at random and in order to prevent breakage
of ceramic or carbon packings. The tower may first be filled with water to reduce the velocity of fall.
Regular Packings
These are of great variety. The regular packings offer the advantages of low pressure drop for the
gas and greater possible fluid flow rates, usually at the expense of costlier installation than random
packing various types of regular packing is as shown in the following figure.
In regular packing, packing materials arranged in particular manner unlike in random packing.

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Stacked raschig rings are economically practical only in very large sizes. These are several modifications
of the expanded metal packings. Wood grids (or) hurdles, are inexpensive and frequently used where large
void volume required.
Knitted or woven wire screen, rolled as a fabric into cylinders or other metal gauzelike
arrangements provide a large inter facial surface of contacted liquid and gas and very low gas pressure
drop, especially useful for vacuum distillation.
Leading and Flooding
At a fixed gas velocity, the gas pressure drop increases with increased liquid rate, principally
because of the reduced free cross section available for flow of gas resulting from the presence of the
liquid.

In the region of figure below A, the liquid holdup, i.e. the quantity of liquid contained in the
packed bed is reasonably constant with changing gas velocity, although it increases with liquid rate.
In the region between A and B, the liquid hold up increases rapidly with gas rate, the free area for
gas flow becomes smaller, and the pressure drop rises more rapidly. This is known as loading.
As the gas rate is increased to B at fixed liquid rate, one of the numbers of changes occurs as
follows.
 A layer of liquid, through which the gas bubbles, may appear at the top of the packing.
 Liquid may fill the tower, starting at the bottom or at any intermediaterestriction such as a
packing support, so that there is a change from gas-continuous, liquid-dispersed to liquid-
continuous, liquid-dispersed.
 Slugs of foam may rise rapidly upward through the packing.

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At the same time, entrainment of liquid by the effluent gas increases rapidly. and the tower is
flooded.
The gas pressure drop then increases very rapidly.
It is not practical to operate a tower in a flooded condition; most towers operate just below or in
the lower part of, the loading region.
Operating Problems during Operation of packed tower
Flooding:
High pressure drop may lead directly to a condition of flooding When a large pressure difference
in the space between the trays. The liquid level in the downspout will rise further to permit the liquid to
enter the lower tray, if flow rate increases. Ultimately the liquid level may reach that on the tray above.
Further increases in either flow rate then aggravates the conditions rapidly and the liquid will fill the
entire space between the trays. This is called as flooding.
Channeling:
In the case of random packings, the packing density, i.e. the number of packing pieces per unit
volume, is ordinarily less in the immediate vicinity of the tower walls, and this leads to a tendency of the
liquid to segregate toward the walls and the gas to flow in the centre of the tower is called channeling.
Priming:
For liquid gas combinations which tend to foam excessively, high gas velocities may lead to a
condition of priming. Here the foam persists throughout the space between trays and great amount of
liquid is carried by the gas from one tray to the tray above. This is an exaggerated condition of back
mixing.
The liquid so carried recalculates between trays and the added liquid- handling load increases the gas
pressure drop sufficiently lead to flooding.
Coning:
If the liquid rate is too low, the gas rising the through the openings of the tray may push the liquid
is allied as coning. In this situation contact of liquid and gas is poor.
Weeping:
If the gas rate is too low, much of the liquid may rain down through the openings of the tray is
called as weeping. Thus failing to obtain the benefit of complete flow over the trays.
Dumping:
At very low gas rates, none of the liquid reaches the downspout, this is called as dumping.
Height equivalent of a theoretical plate (HETP):
The total height of packed tower is calculated by multiplying number of theoretical plates required
for a given degree of separation by HETP.
HT =(HETP)x(NT)
Height of tower = (HETP) X (No. of theoretical plates required)

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Where, HETP is defined as the height of a section of packing that will gives the same separation
as that achieved with one theoretical plate.
The HETP must be an experimentally determined quantity characteristic for cach packing. Unfortunately
it is found that the HETP, varies, not only with the type and size of the packing but also very strongly with
flow rates of each fluid and for every system with concentration as well, so that an enormous amount of
experimental data would have to be accumulated to permit utilization of the method. Statement of
equation for height of an absorber:
Height of an absorber can be calculated by using the
Z= HTU x NTU------- (1)
Where,
Z = height of absorber, HTU= height of transfer units , NTU= number of transfer units.
HTU and NTU are calculated as follows.
For controlling resistance offered by gas film;

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UNIT-2
ABSORPTION
PART – A
Q.NO QUESTIONS CO Map BT MARKS
1 Define absorption or scrubbing with example? CO 2 Re 3
2 State Henry’s Law. CO 2 Re 3
3 Define Raoult’s law and its applications. CO 2 Re 3
4 What is difference between random packing and regular packing? CO 2 Re 3
5 Define desorption with example. CO 2 Re 3
6 What is HETP? CO 2 Re 3
7 Write the types of equilibrium solubility of gas? CO 2 Re 3
8 Define ideal solution and non-ideal solution with example? CO 2 Re 3
9 Define absorption factor. CO 2 Re 3
10 What is HTU and NTU? CO 2 Re 3
11 What is the choice of solvent for absorption? CO 2 Re 3
12 Define tray tower and its types? CO 2 Re 3
13 Write the types of down comer? CO 2 Re 3
14 Write the problem during the tray tower? CO 2 Re 3
15 Explain flooding and priming? CO 2 Un 3
16 Explain coning and weeping? CO 2 Un 3
17 Explain channeling and dumping? CO 2 Un 3
18 Write any uses of bubble tray, sieve tray and valve tray? CO 2 Re 3
19 Define packed tower and write its uses? CO 2 Re 3
20 Define distributor and write its types? CO 2 Re 3
21 Define packing and its types? CO 2 Re 3
22 Write the characteristics of tower packing? CO 2 Re 3
23 Name three important insulating packings. CO 2 Re 3
24 Define equilibrium curves and operating line? CO 2 Re 3
PART-B
1 Explain the choice of solvent for Absorption. ii) Explain in detail the construction CO 2
RE 14
and operation of Packed absorption tower.
2 Explain in detail the operating problems of Absorption column. ii) Explain the concept CO 2 14
RE
of HTU and NTU
3 (i) Discuss in detail about random packing and regular packings. (ii) Explain the 14
CO 2 CR
concept of minium Gas-liquid ratio.
4 Discuss about various packing materials used in absorption tower and its 14
CO 2 CR
advantages. (or) discuss the characteristics of packing, loading and flooding.
5 Explain with a neat sketch the construction and operation of packed bed 14
CO 2 UN
absorption column. (or) Write in detail the construction of packed tower.
6 Write in detail about construction and working of tray tower. CO 2 RE 14

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UNIT -III
HUMIDIFICATION
Humidification operation
If we contact liquid (water) with dry air result in evaporation of some of water into the air. This
called humidification of air.
If we contact very moist air with pure liquid water may result in condensation of part of the moist
in the air. This called dehumidification of air.
In the both the cases diffusion of water vapor through air is involved.

Terminology used in humidification operation

Absolute humidity (Y):
Absolute humidity is defined as the ratio of mass of water vapor to the mass of dry air (or gas).
Mass of water vapor (A) Mass of (A)
Y’= = Mass --------(1)
Mass of dry air (B) of (B)

Molal absolute humidity (Y):

It is defined as the ratio of moles water vapor to the moles of dry air.
Mass of water vapor (A)
Y= ----------(2)
Mass of dry air (B)

Y=YA/YB
For ideal gases, Pressure % = Volume % = Mole%
Y=PA/PB=PA/PT-PA
Equation can be rearranged as follows,
Mass of water vapor (A) Mole s of (A)
Y= =
Mass of dry air (B) Moles of (B)

Mass of A /Molecular mass of (A)

Y= Mass of (B)/ Molecular mass of (B)

Mass of (A) Molecular mass of (B)

Y= Molecular x
mass of (A) Mass of (B)

Mass of (A) Molecular mass of (A)

Y= x Molecular --------(3)
Mass of (B) mass of (B)

Let, MA-Molecular mass of A (water vapor)

Ma-Molecular mass of B (dry air)
Then equation (3) becomes,

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Mass of (A)
Y= x MB/MA
Mass of (B)

Mass of (A)
But,Y’ = Mass of (B)

Y=Y’x MB/MA ---------(4)

Problem-1
In a mixture of benzene vapour (A) and Nitrogen (B) at the total pressure of 800 mmHg and
a temperature of 60°C, the partial pressure of benzene is 100 mmHg. Express the benzene
concentration in other terms.
Solution:
Given:
Partial pressure of benzene (pA) = 10 mmHg
Partial pressure of Nitrogen (pB)=?
Total pressure (Pr) - 800 mmHg
We know that, according to Dalton's Law,
PT = pA+ pB
P B = PT - PA
PB = 800-100 = 700mmHg
(a) Mole fraction:
Since, Mole fraction = Pressure fraction for ideal gas mixture
moles of benzene
Mole fraction of Benzene (yA) = pA/ pT = Total Moles
100
yA = = 0.125 molefraction of benzene
800

We know that, yA+yB = 1

Mole fraction of Nitrogen (yB) = 1-0.125 = 0.875
(b). Volume fraction:
For ideal gas,
Volume fraction = Mole fraction
The volume fraction benzene = 0.125
(c). Absolute humidity
yA pA 0.125 moles of benzene
Y= = = = 0.143
yB pB 0.875 Moles of nitrogen

78.05
Y = Y’ x ( 28.08 )

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kg benzene
Y’ = 0.398
kg nitrogen

Saturated air or Saturation humidity (Ys):

Saturated air is an air in which the partial pressure of water vapour in air- water vapour mixture is
equal to the vapour pressure of pure water at given temperature.
Saturation humidity is defined as follows,
Ys= PA/ PT-PA
Saturated absolute humidity is defined as follows;
YS=YS x MA/MB
Percentage saturation or percentage absolute humidity (Yp):
It is defined as the ratio of absolute humidity to saturation humidity.
YP=(Y/ YS) x 100
Relative humidity (or) Relative saturation (YR):
It is defined as the ratio of the partial pressure of water vapour in the air- water-vapor system to the vapor
pressure of pure water at dry bulb temperature of gas mixture.
YR=PA/PA(vap)x100
Where, PA(vap)=Vapor pressure of water at DBT
Dew point:
This is the temperature at which a vapour-gas mixture becomes saturated When cooled at constant
pressure (total) out of contact with liquid,
Dry bulb temperature (DBT):
This is the temperature of a vapor gas mixture as ordinarily determined by immersion of a
thermometer in the mixture.
Wet bulb temperature (WBT):
A thermometer whose bulb has been covered with a wet wick is immersed in a rapidly moving
stream of the gas mixture. The thermometer will indicate the temperature lower than the dry bulb
temperature. This temperature is called wet bulb temperature,
Illustration:
Consider a drop of liquid immersed in a moving stream of unsaturated vapour gas mixture. The
vapour pressure of the liquid will higher at the drop- surface; then the partial pressure of vapour in the
gas. The liquid will evaporate and diffuse into the gas. The Latent heat required for he evaporation is
supplied at the expense of sensible heat of the liquid drop, which will then cool down as soon as the liquid
temperature is reduced below the DBT of the gas, heat will flow from the gas of liquid at an increasing
rate as the temperature difference becomes larger Eventually the rate of heat transfer from the gas to the
liquid will equal the rate of heat requirement for evaporation, and the temperature of liquid will remain
constant at some low value, that low temperature is called Wet bulb temperature.

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Humid heat (Cs):

Amount of heat required raising the temperature of 1 kg of dry air and water vapour present in it
through 1°C or 1 K is called humid heat. It can be calculated from the following equation.
C₁ = 1005+1.88H Kj/ Kg dry air K
Humid volume (v):
The total volume occupied by 1kg of dry air plus the vapour it contains at absolute pressure and
the given temperature is called humid volume. It can be alculated from the following equation

Adiabatic Saturation Temperature

 Consider the process shown in the figure, where the entering gas of air- water vapour mixture
is contacted with a spray of liquid water.
 The gas leaving having different humidity and temperature and the process is adiabatic.
 The water is recirculated with some make up water added.
 Then the temperature of the water begin recirculated is reaches a steady state temperature
called adiabatic saturation temperature (Ts).
 If entering the gas at temperature T having humidity of H is not saturated, Ts will be lower 'T.
 If the contact between the entering gas and the spray of droplets is enough to bring the gas and
liquid to equilibrium, then the leaving air is saturated at'Ts', having a humidity 'Hs".
 Heat balance of the process is,
 Total enthalpy of entering gas - Enthalpy of leaving gas.
CS (T-TS) + HλS = CS (TS-TS) + HSλS
CS (T-TS) + HλS - HSλS = 0
- CS/λS = (H-HS)/(T-TS)
(1.005+1.88H)
(H-HS)/(T-TS) = -
λs

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Lewis Relation
For the flow of gases past cylinders, such as wet bulb thermometer and past single sphere the
properties of vapour-gas system is correlated by
HG/kY.CS=(SC/Pr)0.567=(Le)0.567
For turbulent flow, independent of NRe the range of Lewis number is 0.335 to 7.2.
For air-water vapour system,
hG / ky=.CS
Approximately. hG / kyCS=1 This is called Lewis relation.
Where,Sc-Schmidt number
Pr-Prantl number
Le-Lewis number
hG/ky S - Psychrometric ratio
Cs-Humid heat.
Equipment for Humidification operations
Cooling Towers
 Air and water low cost substance and where large volume must be handled as in many water
cooling operations, equipment of low initial cost and low operating cost is essential.
 The construction of cooling tower is as shown in the following figure. The framework and internal
packings are frequently of redwood, a material which is very durable in continuous contact with
water.

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 Impregnation of wood under pressure with fuicides such as coal-tar creosote pentachlorophenols,
acid copper chromate and etc.
 Siding of the towers is commonly redwood asbestos cement, gliss reinforced polyester plastic etc.
 Towers have been built entirely plastic.
 The internal packing is usually a modified form of hurdle, horizontal slats arranged staggered with
alternate tires at right angles.
 Plastic packings may be polypropylene, molded in a grid or other form
 The void space is very large greater than 90 percentages.
 So that gas pressure drop will be as low as possible.
Materials used for cooling towers:
The requirements of cooling tower materials classified as,
 Materials for structure.
 Fill material.
 Materials for other components. (water distribution & mechanica components)
Materials for structure:
Structural materials in common use include galvanized steel, stainless steel fibre glass reinforced
polyester (FRP) and wood. Galvanized towers with stainless steel basins are common. FRP exterior
casing is a typical on wood towers.
 FRP towers are costlier than galvanized one.
 While stainless steel is costliest one. Wood is practical material only near to the top of this range
 Fibre glass structures can with stand most corrosive conditions, but fail to meet fire codes of some
cities.
 Stainless steel provides excellent corrosive resistance but cost is high.
Fill material:
 Heat transfer is most modern tower, takes place on film type fill surfaces, because it provides
maximum heat transfer surface area.
 Mostly all film type fill is formed from PVC sheets because it provide excellent manufacture
ability. Outstanding erosion resistant and highly chemical resistance.
 Film type fill is not suitable for water containing suspended solids for this.
 splash type fill bars are used, which is made of treated wood, PVC.
 polypropylene or acrylonitrile-butadiene styrene (ABS).
Materials for other components:
 Water distribution nozzles may be made of propylene, ABS or fibre glass - filled nylon.
 These materials are serve well because of these inherent resistant to chemical attack and
exceptional resistant to erosion.
 Fan blades are made of typically aluminium alloys. As they have to withstand extremely operating
loads in saturated environment.
 FRP or fiber glass reinforced epoxy are also used for fan blades.

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Operation of Cooling Tower:

The principle of cooling the water in cooling tower is similar to the evaporative condenser. The
water goes into the air, in the form of vapor taking its latent heat from the remaining water and causes the
reduction in temperature. The rate of evaporation of water in the cooling tower depends upon the
following actors
1. Amount of water surface exposed.
2. Time of exposure.
3. The relative velocity of air passing over the water droplets formed in the cooling tower.
4. The RH of air and difference below inlet air WBT and the infet water temperature.
5. The direction of air flow relative to water.
Theoretically the water can be cooled upto wet bulb temperature of entering air, if the air leaving
the cooling tower becomes saturated.
Generally, the temperature of water coming out in the cooling tower is 3°C to 5°C above the WBT
of entering air.
The temperature difference between the WBT of incoming air and outgoing temperature of water
circulated lower will be approach of tower. The quantity of water circulated economically is also limited
by the power requirements of the pump.
The following factors are deciding the performance of cooling tower.

✓Cooling approach

✓ Cooling range, and

✓Cooling tower efficiency.

Cooling approach:
It is defined as the difference between cold water inlet temperature and wet bulb temperature of
entering air (T-T).
Cooling range:
It is defined as the difference between inlet (hot) water temperature and outlet (cold) water
temperature of entering air (T-T).
Cooling tower efficiency:
(Hot water temperature −Cold water temperature )
ηc=Cooling x 100
tower inlet temperature −Wet bulb temperature

Range
ηc=Range +Approach x 100

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Cooling tower efficiency is limited by the ambient wet bulb temperature. Ideally, cold water temperature
will be equal to the wet-bulb temperature which is practically impossible to achieve. Hence, cooling
tower efficiency will be in between 70 to 75%.
Water losses in cooling tower:
The following are the important major water losses in the operation of cooling tower.
1. Drift losses
2. Evaporative losses, and
3. Blown down losses.
Drift losses:
In mechanical draft cooling tower some amount of water carried over by the exhaust air, this is
called drift loss. To avoid this, drift eliminators are located at the top of the cooling tower.
Evaporative losses:
In cooling towers, cooling of water produced by evaporative cooling i.e. some amount of water
getting vaporization and mixed with air. The heat required for such vaporization is taken from the water
itself, water temperature will decrease. This is called evaporative cooling.
Blown down losses:
In the cooling tower sump, soda ash and HCI or added to maintain PH of the water. The salts and
chemicals carried out by the hot water from the various parts of the plant are settled down at the bottom
of the sump. By disposing the settled salts some amount water will be loss along with the salts. This is
called blown down loss.
Arrangements of Cooling Towers
Natural draft Towers:

 The atmospheric tower depends on prevailing winds for air movement.

 The natural draft design ensures more positive air movement even in calm weather by depending
upon the displacement of warm air inside the tower by the cooler outside air.
 Fairly tall chimneys are then required.

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 Both these tower types must be relatively tall in order to operate at a small wet bulb temperature
approach.
 Natural draft equipments are used commonly in the South Western United states and in the Middle
East, where the humidity usually low.
Mechanical - Draft Towers (Forced draft and Induced draft)
 It may be the forced draft type, where the air is blown into the tower by a fan at bottom.
 These are particularly subject to recirculation of the hot, humid discharged air into fan intake
owing to the low discharge velocity. Which materially reduce the tower efficiency.
 Induced draft with the fan at the top avoids this and also permits more uniform internal
distribution of air.

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Types of CoolingTower Advantages Disadvantages

Forced draft cooling tower 1. Suitable for high air n Recirculation due to high air-
resistance due to centrifugal entry and low air-exit velocities,
blower fans 2. Fans are relatively which can be solved by locating
quiest towers in plant rooms combined
with discharge ducts

Induced draft cross flow cooling Less recirculation than forced Fans and motor drives
tower draft towers because the speed of mechanism require weather
exit air 3-4 times higher than proofing against moisture and
entering air. corrosion because they are in the
path of humid exit air

Common problems in cooling tower and solutions

Following are the important problems normally associated with the cooling tower operation.
 Biological contamination
 Corrosion
 Fouling and
 Scaling
Biological contamination:
Cooling towers by nature are places that are hot and humid. along with the common and plentiful
nutrients that most water sources contain it Is an ideal place for the growth of unwanted biological
growth, such as bacteria. these contaminants are not good for people, and are worse for the efficiency of
your cooling tower. this comes in the form of biofilm, which is build up on the internal components of
cooling tower. even very thin layers can reduce the thermal efficiency dramatically.
Solution
Biological contamination can be eliminated by treating the system with chlorine over a series of
48 hours in various concentrations followed by complete Bush and refill with new water, to prevent the
future contamination all leaks should be eliminated from the cooling water system. Analyze the sample,
and if the test shows the water is contaminated, then the system should be chlorinated again.
Corrosion
cooling towers and chillers that leak can many times be attributed to cooling systems that are
ignored, this can be especially prevalent in cooling towers that use closed loop systems. when the air,
sodium, and other chemicals that are found in our water supplies are left unchecked to run through a
cooling tower system they eat away at the metal and will lead to leaks.
Solution
There are three ways to control the corrosion such as, epoxy coatings. adding orthophosphate to
the water treatment and raising the pH of water up close to 9.0.
Fouling

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Fouling is the clogging of cooling surfaces or pipes with debris, dirt, and dust. fouling can occur at
different areas of your cooling tower system. the fill is one of the prime locations for fouling to occur.
When water cannot make it into and pass through the fill as designed, the air is not cooled properly. This
means that the system has to work longer to achieve the same results. which means it is using more
electricity.
Solution
To treat fouling chlorine can be used, fill can be changed, and nozzles or other hardware can be
swapped out for new parts to recover the performance of the cooling tower was designed with.
Scaling
The primary role of cooling towers is to exchange heat from the chiller or industrial process. this
means that buildup of minerals in the in the water can create layers that rob efficiency, the different types
of minerals, like calcium, that are part of the high heat system breakdown and are deposited on the
cooling tower heat exchange surfaces.
Solution
Tube coatings which are made from polymers are one of the way to prevent scaling. These
coatings provide a surface which is conductive to heat to maintain performance but do not give calcium a
place to stick to build up.

UNIT-3
HUMIDIFICATION
Humidification operation-Terminology used in humidification operation such as Absolute humidity , Molal
humidity , Dry bulb temperature , Wet bulb temperature , Relative humidity ,Percentage saturation ,Dew
point, Adiabatic saturation temperature ,Humid heat and Humid volume -Lewis relation- simple problems in
Humidification
Equipment for Humidification operations-construction and working principle of cooling towers -
arrangements of cooling towers- natural draft, forced draft and induced draft –Cooling tower efficiency –
common problems in cooling tower and solutions.
PART – A

Q.N CO MARK
QUESTIONS BT
O Map S
1 What is Humidification and Dehumidification? CO 3 RE 3

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2 What is Relative humidity? CO 3 RE 3

3 What is Dew point of a vapour gas mixture? CO 3 RE 3
4 What is Lewis relation? CO 3 RE 3
5 Explain the significance wet bulb temperature and dry bulb temperature? CO 3 UN 3
6 Define absolute humidity and molal humidity. CO 3 RE 3
7 What is adiabatic saturation temperature? CO 3 RE 3
8 Explain the function of draft in cooling towers. CO 3 RE 3
9 Define humid volume and humid heat CO 3 RE 3
10 Give the advantages of forced draft in cooling towers. CO 3 RE 3

11 Explain the major water losses in cooling tower? CO 3 UN 3

12 Explain the common problems in cooling tower and solutions? CO 3 UN 3

13 Define percentage saturation and saturation humidity. CO 3 UN 3
14 What are the factors are deciding the performances of cooling tower? CO 3 RE 3
15 Explain the performances of cooling tower. CO 3 RE 3
PART-B
Explain in detail the construction, components and working principle of
1 CO 3 UN 14
Cooling Tower.
Explain in detail common problems in cooling tower and cooling tower
2 CO 3 UN 14
Efficiency.
3 Give brief notes on different techniques to measure humidity. CO 3 UN 14
Describe the construction and operation of Forced draft cooling tower with
4 CO 3 UN 14
neat diagram.
Explain in principle, construction and operation of mechanical draft cooling
5 CO 3 RE 14
towers.
What is humidification? Explain in detail any one of the humidification
6 CO 3 RE 14
equipment with a neat sketch.
Explain in detail about common problems encountered in cooling towers and 14
7 CO 3 RE
the solutions.
8 Explain with neat sketch on arrangements of cooling towers CO 3 RE 14
9 Explain with details on types of losses in cooling tower? CO 3 RE 14

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UNIT-IV
FUNDAMENTALS OF DISTILLATION
Distillation
 Distillation is a unit operation in which the constituents of a liquid mixture (solution) are separated
using thermal energy. Basically, the difference in vapor pressures/ boiling point/ volatility of
different constituents at the same emperature is responsible for such separation. This unit
operation is also termed as fractional distillation or fractionation.
 Distillation is commonly encountered in chemical and petroleum industries as a means of
separating the liquid mixture into its component parts.
 The separation of a mixture of ethanol and water, production of absolute alcohol from 95% ethyl
alcohol using benzene.
 The separations of petroleum crude into gasoline, kerosene, fuel oil etc are typical example for
distillation.
Boiling Point:
 For any given pressure, a pure liquid when heated will boil or vaporize at a certain single
temperature known as boiling point of the liquid.
 Boiling points at a given pressure vary greatly for different liquids, for example, boiling point of
water is 100°C, that of toluene is 110°C and that of methanol is 64.7°C at 1 atm. pressure.
 In a binary mixture, the component with lower boiling point or with higher vapor pressure at a
given temperature, is termed as the more volatile or lighter.
 And the component with higher boiling point or with lower vapor pressure at a given temperature
is termed as less volatile or heavier.
 Thus in the case of methanol and water system, methanol is the more volatile component and
water is the less volatile component.
Vapor-Liquid Equilibria
 The successful application of distillation methods depends greatly upon an understanding of the
equilibrium existing between the vapor and liquid phases of the mixture encountered.
 Let us consider a component A of the binary mixture A-B as the more volatile, i.e. the vapor
pressure of the pure A at any temperature is higher than the vapor pressure of pure B.
 Let 'x' is the mole fraction of more volatile substance A in the liquid, and y' is the mole fraction of
more volatile substance A in the vapor.
 A three dimensional diagram as shown in the following figure is necessary to represent the vapor -
liquid equilibrium completely.
 The curve marked pA is the vapor-pressure curve of A. lying entirely in the nearest composition
plane at x = 1.0.
 The curve extends from it critical point CA to its triple point TA, but the complications of solid
phase which do not enter into distillation operations will not be considered. .
 Similarly curve pa is the vapor pressure of pure B, in the far plane at x=0.
 The liquid and vapor regions at compositions between x = 0 and 1.0 are separated by a double
surface which extends smoothly from pɅ to pв. *. The shape of this double surface is more readily
studied by considering sections at constant pressure and constant temperature as follows.

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Constant Pressure Equilibria

 Consider first a typical section at constant pressure.
 The intersection of the double surface of the above figure (a) with the pressure plane produces a
looped curve without maxima or minima constant extending from the boiling point of pure B to
that of pure A at the given pressure.

 The upper curve provides the temperature - vapor composition(t-y') relationship, the lower that of
temperature - liquid composition (t - x)
 Liquid and vapor mixtures ate equilibrium are at the same temperature and pressure throughout, so
that horizontal tie lines such as line DI join equilibrium mixtures at D and F.
 A mixture on the lower curve, as at F, is a saturated liquid, a mixture on the upper curve, as at F, is
a saturated vapor.

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 A mixture at E is a two-phase mixture, consisting of a liquid phase of composition at D and a

vapor phase of composition at F in such proportions that the average composition of the entire
mixture at E.
 The relative amount of the equilibrium phases are related to the segments of the tie line,
Moles of D Line EF
 =
Moles of F Line DE
 Consider the solution at G in a closed container which can be kept at constant pressure by moving
piston.
 The solution is entirely liquid, if it is heated, the first bubble of vapor forms at H and has the
composition at J, richer in the more volatile substance, hence the lower curve is called the bubble-
point-temperature curve.
 The last drop of liquid vaporizes at M and has the composition at N superheating the mixture
follows the path MO.
 The mixture has vaporized over a temperature range from H to M. unlike the single vaporization
temperature of pure substance.
 Thus the term boiling point of a solution has no meaning since vaporization occurs over a
temperature range, i.e. from the bubble point to dew point.
 If the mixture at O is cooled, all the phenomena reappear in reverse order.
 Condensation, for example, starts at M, whence the upper curve is termed the dew point curve,
and continues to H.
 The vapor- liquid equilibrium composition can also be shown on a distribution diagram (x vs y')
as shown in the above figure (b).
 The point P on the diagram represents the tie line DF. Since the vapor richer in the more volatile
substance, the curve lies above 45° diagonal line.
Constant Temperature Equilibria

 A typical constant-temperature section of the three-dimensional phase diagram is shown in the

above figure.

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 The intersection of the constant- temperature plane with the double urface of three dimensional
diagram provides the two curves which extend without maxima or minima from the vapor
pressure of pure B to that of pure A.
 As before, there are an infinite number of horizontal tie-lines, such as TV. which join an
equilibrium vapor as at V to its corresponding liquid at T.
 A solution in a closed container at W is entirely a liquid, and if the pressure is reduced at constant
temperature, the first bubble of vapor forms at U. complete vaporization occurs at S.
 And further reduction in pressure results in a super-heated vapor as at R.
Raoult's Law
It is commonly used to predict vapor liquid equilibrium for an ideal solution in equilibrium with
an ideal gas mixture from vapor pressure data. It states that, in a binary system of A and B, the
equilibrium partial pressure of a constituent at a given temperature is equal to the product of its
vapor pressure in a pure state and its mole fraction in the liquid phase.
Mathematically.
PA = PA(vap) * xA and PB=PB(vap) * xB
= PB (vap) * (1- xA) , as xA + xB = 1
Where.
PA & PB-Equilibrium partial pressure of A and B respectively,

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The vapor- liquid equilibrium data for (A) and (B) between the given temperature range are tabulated as
follows;
Problem-1:
Compute the vapor and liquid equilibrium composition at constant pressure of 101.32 kPa for a mixture
of benzene and toluene using vapor pressure data. Construct x-y diagram.

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Relative Volatility
Volatility of A:
It is defined as the ratio of the partial pressure of A to the mole fraction of A in the liquid phase.
Volatility of A= PA / XA ---------- (1)
Similarly,
Volatility of B= PB / XB ---------- (2)
Relative volatility is the ratio of the volatility of A (more volatile component) to that of B. It is also
known as volatility of A with respect to B and denoted by a symbol ∝AB

∝AB = (PA / XA) / (PB / XB)

= (PA * XB) / (PB * XA)

According to Dalton’law, for ideal gas or vapor, the partial pressure is related to the mole fraction of the
component in the gas or vapor phase by the relation.

Partial pressure = Mole fraction x Total pressure

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Form the above equation (12), knowing α for a given system ,x-y data (equilibrium data) can be generated
by taking x = 0, 0.1, 0.2. to 1.0 and evaluating corresponding values of y (equilibrium vapor phase
composition). When a = 1, separation by distillation is not possible. Separation by distillation is possible
for relative volatility values greater than one. Larger values of a' easier the separation by distillation.
Problem-2
Compute the vapor-liquor equilibrium data for methanol- water system at 1 atm pressure and plot x-y and
t-x-y diagrams. The vapor pressure data for methanol- water system as follows: Temp.(C)

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Minimum and Maximum Boiling Azeotropes

An azcotrope is a liquid mixture with an equilibrium vapor of the same composition as the liquid
(the composition of the vapor generated from the liquid s same as that of liquid mixture
As the dew point are identical at the azeotropic composition ,the azeotropes are called the as
constant boiling mixture .
Close boiling components showing small deviations from ideality form an azeotrope.
An azeotrope exhibits a maximum or minimum boiling point relative to boiling points of pure
liquids and thus are classified as follows;
- Maximum boiling azeotropes and
- Minimum boiling azeotropes.
A minimum boiling azeotrope will boil at a temperature lower than the boiling points of the pure
components.
And a maximum boiling azeotrope will boil at a temperature higher than the boiling points of the
pure components.
The temperature composition diagrams of and equilibrium diagrams for the mixture forming an
azeotrope at constant pressure are shown in the following figure.

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For all mixtures of compositions less than P, an equilibrium vapor is richer in the more volatile
component than the liquid.
While for all mixtures of composition greater than P. the equilibrium vapor is less rich in the more
volatile component than the liquid.
The mixture of composition gives the vapor of composition identical with the liquid.
At the point P, the vapor and liquid are identical in composition and separation past that point by
simple/ordinary distillation technique is not possible.
In such cases, complete separation by ordinary fractionation may be impossible
The constituents of binary azcotrope are separated by:-
 adding a third component to the binary mixture and
 changing the system pressure.
The third component added to a binary azeotrope usually form a low boiling azeotrope with one or
both of the feed components and usually withdrawn as the overhead product/ distillate.
The third component added to break the binary azeotrope to effect its separation into the pure
components is called as an entrainer.
Methods of Distillation
The following are the common methods of distillation.
1. Differential or Simple distillation,
2. Flash or equilibrium distillation, and
3. Continuous multistage rectification or fractionation.
Differential or Simple Distillation

In this distillation technique a known quantity of a liquid mixture is charged into a still or jacketed
kettle. The jacket is provided for heating the mass in the still with the help of steam. The mass is boiled
slowly.
Vapors formed are withdrawn and fed to a condenser where they are liquefied and collected in a
receiver as a distillate.

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In the earlier stage of distillation, vapors leaving the still are richest in the more volatile
component and the distillation proceeds the liquid in the still becomes lean with respect to the more
volatile component.
The composition of the less volatile component thereby increases and hence the boiling point
increases. The product (distillate) from such units can be collected in several receivers, called cuts, to give
products of various purities over the length of distillation period.
The distillation is continued till the boiling point of the liquid reaches a predetermined value and
the contents of the still are finally removed as residual liquid containing majority of the less volatile
component.
As the composition of the vapor issuing from distillation and that of the liquid remaining in it
changes during the course of operation, the mathematical approach should be differential.
Let. F- Amount of liquid mixture (A+B) in kg.mol.
D - Amount of distillate in kg.mol
W- Amount of residual liquid in the still in kg.mol
XF - Mole fraction of A in the feed to the still.
yDavg -Mole fraction of A in the distillate,
XW - Mole fraction of A in the residual liquid.

Let 'L' be the kg mole of liquid in the still at any time during the course of distillation and let & be the
mole fraction of 'A' in the liquid. Let a very small amount dD kg, mol of the distillate of the composition
'y' in equilibrium with the liquid is vaporized. Then the composition and the quantity of liquid decreases
from x to x-dx and L to L-dl respectively.

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The above equation is known as Rayleigh equation. It is used to etermine F, W, XF or xw when three of
these are known. RHS of the above quation is evaluated graphically by plotting -) as an ordinate and x as
the scissa and determining the area under the curve between x = x F; and X-Xw. The require data for x and
y are taken from the vapor - liquid equilibrium.

Problem-3 (Rayleigh's Equation)

An ethanol-water mixture containing 18 mole% of ethanol is differentially distilled at 1 atm, pressure and
the mixture is reduced to maximum ethanol concentration of 6 mole%. Determine the composition of
distillate.

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Flash or Equilibrium Distillation:

Flash distillation is normally carried out in continuous manner. In this method a liquid mixture is
partially vaporized; the vapor and liquid are allowed to attain equilibrium and finally withdrawn
separately.
Feed is heated in a tubular heat exchanger.
The hot liquid mixture is then fed to a separator via a pressure reducing valve whereby the
pressure is reduced and vapor is formed at the expense of liquid adiabatically.

The liquid is withdrawn from the bottom of the separator and the equilibrium vapor leaves the
separator from the top which is then liquefied in a condenser.

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Flash distillation is commonly used in petroleum industry. handling multicomponent system in the
pipe stills.
Consider one mole of a liquid mixture, having x mole fraction of more volatile component, is fed
to a flash distillation unit.
Let f be the fraction of the feed that is vaporized and is of composition y
Then (1-f) will be the moles of the residual liquid obtained.

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Vacuum Distillation (Low-Pressure Distillation)

The temperature of distillation of many natural products such as separation of vitamins from
animal and fish oils as well as separation of many synthetic industrial products such as plasticizers may
not exceed 200 to 300°C to avoid chemical decomposition, where the vapor pressures of the substances
may be a fraction of mmHg. The conventional distillation equipments are not suitable for such
separations. In the distillation of above materials, the pressure, corresponding temperature and time of
exposure of material to the distillation temperature must kept low to avoid thermal decomposition.
Vacuum distillation is suitable for hese types of heat sensitive materials. The most commonly used
vacuum istillation is molecular distillation.
Molecular Distillation
This is a form of distillation at very low pressure conducted industrially at absolute pressure of the order
of 0.003 to 0.03 mmHg, suitable for heat sensitive materials described above.

The above figure shows a device which is used industrially for accomplishing a molecular distillation.
The feed is introduced continuously at the bottom of the inner surface of the rotor, a rotating conical
shaped surface. The rotor may revolve at speeds of 400 to 500 rpm. A thin layer of liquid feed. 0:05 to 0-1
m thick, then spreads over the inner surface and travels rapidly to the upper periphery under the action of
centrifugal force.
Heat is supplied to the liquid through the rotor by radiant electrical heaters, and the vaporized
material is condensed upon the water cooled condenser This is maintained at temperatures sufficiently
low to prevent reevaporation or reflection of vaporized molecules.

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The residue liquid is caught in the collection gutter at the top of the m and the distillate is drained
from the collection troughs on the condenser. Each product is pumped from the still body immediately so
as to maintain low pressure in the still. The residence time of the substance in the still is as low as I
second or less, and 8 to 95% separation can be achieved in this method.
Continuous Rectification:
Rectification is commonly encountered in industrial practice as it is possible to get almost pure
product by this method.
The enrichment of the vapor stream as it passes through the column in contact with reflux is
termed as rectification.
*. In this separation method, part of the condensed liquid is returned back as reflux and maximum
enrichment of more volatile component in the vapor is obtained by successive partial vaporization and
condensation by multi stage contact of the vapor and the liquid.
This is achieved in a single unit called as a fractionating column.
Fractionating Column:
The construction of a rectification column is as shown in the following figure.

A fractionating column or fractionator consists of

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1. a cylindrical shell divided into sections by a series of perforated trays,

2. a reboiler and
3. a condenser
The liquid mixture to be separated is introduced in the cylindrical column more or less centrally.
The column itself is divided into two sections as rectifying section and stripping section.
The section above the feed plate or tray is called the rectifying section, wherein the vapor is
washed to remove the less volatile component with the liquid returned to the column from the top known
as reflux.
The rectifying section is also called the enriching section as the feed is enriched in this section,
owing to which the top product or distillate is richer in the more volatile component than the feed.
The portion below the feed plate including feed plate is called the stripping section, wherein the
liquid is stripped off more volatile component by the rising vapor.
Perforated trays are gas-liquid contacting devices on which gas/vapor and liquid streams are
brought into intimate contact for mass transfer to occur.
The vapors are generated in the reboiler (generally steam heated) and are fed to the bottom of the
column.
The liquid removed from the fractionator rich in the less volatile component is called as bottom
product.
The vapor issuing from the top of the column is fed to the condenser where latent heat is removed
with the help of circulating a coolant through the condenser.
A part of the condensed liquid is returned to the column (reflux) and the remaining part is
withdrawn as the top product or distillate which is rich in more volatile component.
As we move up the column, the vapor becomes richer and richer in the more volatile component
as we move down the column; the liquid becomes richer and richer in less volatile component.
As the liquid is at its bubble point and the vapor is at its dew point. temperature is maximum at the
bottom and minimum at the top.

Dimensionless Numbers in mass transfer and its significance

The following are the important dimensionless numbers used in mass transfer:-
 Schmidt number,
 Lewi's number, and
 Sherwood number
Schmidt Number
It is defined as the ratio of momentum diffusivity to mass diffusivity. Mathematically.
Momentum Diffusivity μ
Sc = mass Diffusivity

= μ / ρ DAB

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Significance:
 Analogous to Prandtl number of Heat transfer
 Used in fluid flows in which there is simultaneous momentum and mass diffusion.
 It is also the ratio of fluid boundary layer to mass transfer boundary layer thickness
 To find mass transfer coefficient using Sherwood number Schmidt number is needed.
Lewi's Number
It is defined as the ratio of heat diffusivity to mass diffusivity. Mathematically,
k
Thermal Diffusivity μ ( ) k Schmidt number
ρ Cp
Le = = = =
mass Diffusivity DAB ρCpDAB Prandtl number

Significance:
 Ratio of thermal diffusivity to mass diffusivity
 Used in fluid flows with simultaneous heat and mass transfer by convection.
 It is also the ratio of Schmidt number to Prandil number.
Sherwood Number
It is also called the mass transfer Nusselt number) is a dimensionless mber used in mass-transfer
operation. It represents the ratio of be convective mass transfer to the rate of diffusive mass transport
It is defined as follows,
Convective mass transfer rate h Schmidt number
Le = = =
Diffusion rate D/L Prandtl number

Where
L - is a characteristic length (m)
D - is mass diffusivity (m²s-1)
h- is the convective mass transfer film coefficient (ms)
Significance
Analogous of Nusselt number in heat transfer or Sherwood number is nusselt number for mass
transfer.

UNIT-4

FUNDAMETALS OF DISTILLATION
Distillation- relative volatility- boiling point diagram- Raoult's law –azeotropic mixture- maximum and
minimum boiling azeotropes – simple or differential distillation- Rayleigh's equation- flash distillation –
vacuum distillation- continuous multistage rectification- boiling point diagram and equilibrium diagram–
construction of boiling point and equilibrium diagram for a binary system using vapour pressure data.
Dimensionless numbers in mass transfer and its significance- Schmidt number, Lewis number, and
Sherwood number (Brief description only).

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PART – A

Q.NO QUESTIONS CO Map BT MARKS

1 Define distillation? CO 4 Re 3

2 What is boiling point diagram? CO 4 Re 3

3 Define bubble point and dew point? CO 4 Re 3

4 State Raoults’s law. CO 4 Re 3

5 Define Dalton’s law? CO 4 Re 3

6 Define relative volatility ? CO 4 Re 3

7 What is Q-line? CO 4 Re 3

8 Write down the Rayleigh equation ? CO 4 Re 3

9 Write the overall material balance equation in simple distillation ? CO 4 Re 3

10 What is the advantage of vacuum distillation? CO 4 Re 3

11 What is Azeotrope? CO 4 Re 3

12 Explain maximum and minimum boiling azeotropes with example. CO 4 Re 3

13 Expalin Schmidt number and Sherwood number. CO 4 Un 3

14 Write the different between more , less volatile ? CO 4 An 3

15 Define entrainer ? CO 4 Re 3

16 What is fractional distillations with example ? CO 4 Re 3

PART-B
1 i) Derive Rayleigh’s equation. ii) Explain in detail Flash distillation. CO 4 Ap 14
i) Explain in detail about Boiling point diagram. ii) Explain in detail vacuum CO 4 Un 14
2
distillation
Discuss in detail about the construction of boiling point diagram and CO 4 UN 14
3
equilibrium diagram.
4 Write in detail about vacuum distillation and its significance. CO 4 Re 14

5 Explain with neat diagram about flash distillation? CO 4 Re 14

Explain with a neat sketch the construction and operation of continuous CO 4

6 Re 14
fractionating column.

Explain with a neat sketch the construction and operation of Simple CO 4

7 Re 14
distillation?

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UNIT-V
DESIGN AND TECHNIQUES OF DISTILLATION COLUMN
CALCULATION OF NUMBER OF TRAYS
The theoretical/ideal stages plates required for a given degree of separation can be obtained by:
 McCabe-Thiele method
 Lewis-Sorel method
 Ponchon-Savarit method.
McCabe-Thiele Method:
It is a graphical procedure of obtaining theoretical plates. The following assumptions are made in
this method.
Assumptions:
 Constant molal heat of vaporization,
 No heat loss, and
 No heat of mixing.
 Consider the rectification column shown in the following figure, where plates are numbered
serially from the top down.
 Consider the nth plate from top in the cascade. The plate n-1 is immediately above the plate n and
the plate n+1 is immediately below the plate n.

Material balance over ideal plate

 On every plate, the two different fluid streams not at equilibrium are brought into intimate contact,
mass transfer takes place, phases are separated, and finally the two fluid streams leave the plate in
equilibrium with each other.

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 Thus, the plate under consideration will receive a liquid Ln-1 moles/hr of composition Xn-1 and a
vapor Vn+1 moles/hr of composition yn+1 from plate n-1 and n+1 respectively.
 The liquid stream Ln moles/hr of composition xn and the vapor stream Vn moles/hr of composition
yn leave this plate for plates n+1 and n-1 respectively in equilibrium with each other.
 In the above figure liquid and vapor streams enter a tray, are equilibrated, and leave.
A total material balance gives,
Vn+1+Ln-1=Vn+Ln ---------- (1)
Component balance;
Vn+1Yn+1+Ln-1Xn-1=VnYn +LmXn ---------(2)
 The compositions yn and xn are in equilibrium and the temperature of the tray n is To. If T. is
taken as datum, it can be shown by a heat balance that the sensible heat differences in the four
streams are quite small if heats of solution are negligible
 Hence only latent heats in the streams Vn+1 and Vn are important. Since molar latent heats of
chemically similar compounds are almost the same, V. V. and LL. Therefore we have constant
molal overflow in the tower.
Equations for Enriching Section
The following figure (a) shows the distillation - tower section above the feed, the enriching
section.

Material balance and operating line for enriching active (a) Schematic TOwer
The vapor from the top tray having a composition y passes as the condenser, where it is condensed
so that the resulting liquid is at boiling point.
The total reflux stream L mol/hr and distillate D mol/hr have the same composition, so y1=xD
Since equimolar overflow is assumed, L1= L2 = Ln and V₁ =Vn = Vn+1
Making material balance over the dashed-line section in the aber figure.

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The above equation is a straight line on a plot of vapor composition versus liquid composition. It relates
the compositions of two streams passing in each other and is plotted in the above figure (b).
The slope is Ln / Vn+1 or R / (R + 1). It intersects the y = x line (45" diagonal line) at x = xD. The
intercept of the operating line at x = 0 is y = xD / (R + 1).
The theoretical stages are determined by starting at xD and stepping off the first plate to x1. then y2
is the composition of the vapor passing the liquid x1. In a similar manner, the other theoretical trays are
stepped off down the tower in the enriching section to the feed tray.
Equations for Stripping Section:
The stripping section of the distillation tower is as shown in the following figure.

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Making total material balance over the dashed line section in the above figure.
Vm+1=Lm-W -------------- (7)
Making balance on component A,

Again the theoretical stages for the stripping section are determined by starting at xw, going upto
yw, and then across to the operating line and so on.

Graphical procedure to determine the number of theoretical trays:

By material balance evaluate the terms D, W and L etc. Draw the equilibrium curves and the
diagonal with the help of x - y data given. If relative volatility is given, generate the x-y data.
Draw the operating line of the rectifying section through the point (xD, xD) on the diagonal line
and with an intercept equal to xD /(R+1) or slope equal to R /(R+1)
Draw the operating line of the stripping section through the point (x L on the diagonal and with the slope
equal to Lm / Vm+1

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Construction of number of stages

*. Starting from the point (XD, XD) on the diagonal, draw a horizontal line to meet the equilibrium curve
at point 'a'. drop a vertical from point 'a' to meet the operating line at point 1.
Proceed in this way that is constructing the triangles (representing the stages) between the
equilibrium curves and the operating line of rectifying section, till we are above the point of intersection
of two operating lines. Once we cross this point of intersection, construct the triangles between the
equilibrium curve and the operating line of the stripping section i.c. dropping verticals on the operating
line of the stripping section.
Proceed in the same manner till we reach exactly or cover the point (XW,XW)
Count the triangle constructed between XD and XW. each triangle on x-y diagram represents a
theoretical plate.
If the number of triangles are 'n', then 'n' represents the theoretical number of plates including
reboiler and 'n-1' represents the number of theoretical plates in the column to achieve a desired degree of
separation.
Limitations of McCabe-Thiele Method:
It is not used when the relative volatility is less than 1.3 or greater than 5.
It is not used when more than 25 theoretical stages/ plates are required, and
It is not used when the operating reflux ratio is less than 1.1 times the minimum reflux ratio.
Total Reflux:
In distillation of binary mixture A and B, the feed conditions, distillate composition, and bottom
composition are usually specified and the number of theoritical trays are to be calculated.
However, the number of theoritical trays needed depends upon the operating lines.
To fix the operating lines, the reflux ratio R = Ln/D at the top of the column must be set.
One of the limiting values of reflux ratio is that of total reflux, or R= ∞. Since R = Ln/D.

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Vn+1=Ln+D
Then very large, as is the vapor flow Vn. This means that the slope R/(R+1) of the enriching operating
line becomes 1.0 and operating lines of both sections of the column coincide with the 45° diagonal line,
as shown in figure.

Number of plates for total reflux condition

The number of theoritical trays required is obtained as before by stepping off the trays from the
distillate to the bottoms.
This give the minimum number of trays that can possibly be used to obtain the given separation.
In actual practice, this condition can be realized by returning all the overhead condensed vapor V1
from the top of the tower back to the tower as reflux, that is, total reflux. Also, all the liquid in the
bottoms is reboiled.
Hence, all the products distillate and bottoms are reduced to zero flow, as is the fresh feed to the
tower.
This condition of total reflux can also be interpreted as requiring infinite size of condenser,
reboiler, and tower diameter for a given feed rate.

Minimum Reflux Ratio:

The minimum reflux ratio is defined as the reflux ratio Rm that will require an infinite number of
trays for the given desired separation of XD and XW.
This corresponds to the minimum vapor flow in the tower, and hence the minimum reboiler and
condenser sizes.
This case is shown in figure as follows;

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Number of plates for minimum reflux condition

If R is decreased, the slope of the enriching operating line R/(R+1) is decreased and the
intersection of this line and stripping line with the q line moves later from the 45° line and closer to the
equilibrium line.
As a result, the number of steps required to give a fixed xD and xW increases.
When the two operating lines touch the equilibrium line, a "pinch poin at y' and x' occurs, where
the number steps required becomes infinite
The slope of the enriching operating line is as follows from the above figure, since the line passes
through the points x', y' and xD (y = xD)

Number of plates for minimum reflux condition with inflection

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Optimum Reflux Ratio:

Any reflux ratio between infinite reflux ratio requiring minimum number of plates and minimum
reflux ratio requiring infinite number of plates is a workable system which requires finite stages for a
desired degree of separation.
At minimum reflux ratio, as infinite number of plates are required, the fixed cost is also infinite
while the cost of heat supply to the reboiler and the condenser coolant is minimum.
As the reflux ratio is increased, the number plates decreases and the fixed cost decreases at first,
passes through a minimum and then increases as with higher reflux ratio the diameter of the column and
sizes of reboiler and condenser increase.
The operating cost increases continuously as the reflux ratio is increased as it is directly
proportional to (R+1).
At total reflux, though the number of plates are minimum, the cost of heat supply to reboiler and
condenser coolant is maximum and also large capacity reboiler are needed.
The total cost which is the sum of the fixed cost and operating cost also decreases to a minimum
and then increases with reflux ratio. The optimum reflux ratio occurs at appoint where the sum of the
fixed cost and the operating cost is minimum.
The optimum reflux ratio is defined as that reflux ratio at which the sum fixed cost and operating
cost is minimum.
As a rough approximation, the optimum reflux ratio is usually 1.1 to 1.5 times the minimum reflux ratio.

Optimum reflux ratio

q-line:
We can represent the condition of feed by the quantity q, which is defined as
Heat needed vaporize 1 mole of feed at entering conditions
= --------- (1)
Molal latent heat of vaporization

If the feed enters at its boiling point, the numerator of the above equation is same as the
denominator, and q = 1. The above equation can be written in terms of enthalpies;
Hv −Hf
q= Hv −Hl

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Where,
HV = Enthalpy of feed at the dew point,
HL =Enthalpy of feed at the boiling point or bubble point
HV = Enthalpy of feed at its entrance conditions.
Value of q based on five different feed conditions
If the feed enters as vapor at the dew point; q=0
For cold liquid feed; q> 1.0,
For liquid at its bubble point/boiling point/saturated liquid feed; q = 1.0,
For super-heated vapor; q <1.0, and
For the feed being partially vapor q lies between 0 and 1.0 (0 < q< 1.0)
We can also look at q as the number of moles of saturated liquid produced on the feed plate by
each mole of feed added to the tower.
The following figure, shows the relationship between flows above and below the feed entrance.

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Setting y =x in equation (9), the intersection of the q- line equation with the 45° line is y=x=xF,
where x is the overall composition of feed.
In the following figure, the q-line is plotted for various feed conditions are shown.

The slope of the q-line is q/q-1, for example, for the liquid below the boiling point, q>1, and the
slope is >1.0 as shown.
The enriching section operating line are plotted for the case of a feed of part liquid and part vapor,
and the two lines intersect on the q line.
A convenient way to locate the stripping operating line is to first plot the enriching operating line
and the q-line. Then draw the stripping line between the intersection of the q line and enriching operating
line and the point y = x = xw
Feed tray location:
To determine the number theoritical trays needed in a tower, the stripping and operating lines are
drawn to intersect on the q line, as shown in the following figure.

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*. Starting at the top at xo, the trays are stepped off. For trays 2 and 3, the steps can go to the enriching
operating line, as shown in the figure (a). . At step 4 the step goes to the stripping line. A total of about 4.6
theoritical steps are needed. The feed enters on tray 4. ⚫. For the correct method, the shift is made on step
2 to the stripping line, as shown in the figure (b). . A total of only about 3.7 steps are needed, with the
feed on tray 2.
keep the number of trays to a minimum, the shift from the enriching to the stripping operating line should
be made at the first opportunity after passing the operating line intersection. *. In the figure (b) is part
liquid and part vapor, since 0 <q<1. Hence in adding the feed to tray 2, the vapor portion of the is
separated and added beneath plate 2 and the liquid added to the liquid to the above entering tray 2 *. If the
feed is all liquid, it should be added to the liquid flowing to tray 2 from tray above. *. If the feed is all
vapor, it should be added below tray 2 and join the vapor rising from the plate below.
Types of Trays used in Distillation Column
In tray towers three types of trays are used for gas liquid
Bubble cap tray/Plate
Sieve tray/Plate
Valve tray/Plate
Bubble cap tray:
Bubble cap tray is as shown in the following figure. In bubble cap tray, gas vapor flows through
riser, reverses flow under cap, moves down ward through the annular space between riser and cap, and
finally it bubbles into a pool of liquid through series of slots provided along the periphery of cap at
bottom.
Bubble cap disperses the gas phase into liquid as a fine bubbles, it prevents liquid drainage
through gas passage at low gas rates. The bubble cap columns can be operated with high and constant
stage efficiencies over wide range of vapor and liquid flow rates.
Bubble cap trays are costly and high pressure drop.

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Sieve tray:
This is very common type of tray used in tray tower, because its simplicity and its cost is low. In
sieve trays, hundreds of round perforation of size ranging from 3 to 12 mm are there for dispersing gas
into liquid, on a plate total area of perforation is ranges from 5 to 10% of the plate area. In sieve tray, the
liquid flows across the tray and gas passes vertically upward through the holes, in the form of bubbles
into liquid on plate. Gas flow through openings in the tray prevents down- flow of liquid the openings
(perforations) in plate.

Valve tray:
Valve plate is improved form of sieve tray, in which perforations in the metal sheet are covered with
liftable valves (caps). Valves are metal disc upto 38 mm diameter and are held in plate by means of legs,
which restricts the upward motion of valves. Valve provides variable orifices for gas flow i.e. opening
will be small at low gas rate and large at high gas rate. This weeping is reduced greatly with this plate at
low gas rates. Gas-liquid contact with valve plate is much better than in sieve plates.

Tray Efficiency
There are three types of tray efficiencies are used in the design of tray tower for distillation as follows;
a. Overall tray efficiency
b. Murphree tray efficiency
c. Point or local tray efficiency

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a. Overall tray efficiency (Eo)

It is defined as the ratio of the number of theoretical or ideal trays needed in an entire tower to the number
of actual trays used.
Number of ideal trays
Number of actual trays
For example, if eight theoretical steps are needed and the overall efficiency is 60%, the number of
theoretical trays is eight minus one reboiler, or seven trays. Then the ctual number of trays is
(7/0.60)=11.7 trays.

b. Murphree tray efficiency (EM)

It is defined as follows;
EM, Where, yn is the average actual concentration of the mixed vapor leaving the tray n as shown in the
figure below, yn+1 average actual concentration of the mixed vapor entering tray n, and yn is the yn the
concentration of vapor that would be in equilibrium with the liquid of concentration xn leaving the tray to
the downcomer.

Problem-1
A continuous fractionating column is to be designed to separate 350 gm-moles per minute of a
binary mixture containing 40% (by weight) of benzene and 60% (by weight) of toluene. The top
product contains 97% (by weight) of benzene and the bottom product contains 98% (by weight) of
toluene. A reflux ratio of 3.5 is to be used. The feed is liquid entering at the column at its boiling
point.
(a). Determine the number of ideal plates
(b). Calculate the moles of top product and bottom product

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Feed is at its boiling point. Hence q-line (feed line) is

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From graph;
Number of ideal plates = 15 (including one reboiler)
(b). F-B+D, F-350 gm-mole/min
:. D 350-B
Fx = BX + DXD
350(0.44) B(0.023)+(350-B)(0.974)
By solving,
B=196.5 gm moles/min (Bottom product)
D=350-196.5=153.5 gm moles/min (Top product)

Azeotropic Distillation
This the special case of multi component distillation used for separation. of binary mixtures which
are either difficult or impossible to separate by ordinary fractionation.
If the relative volatility of a binary mixture is very lo, the continuous rectification of the mixture
to give nearly pure products will require high reflux ratios and correspondingly high heat requirements, as
well as towers of large cross section and number of trays.
In other cases the formation of a binary azeotrope may make it impossible to produce nearly pure
products by ordinary fractionation.

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Under these circumstances a third component, some times called an entrainer may be added to the
binary mixture to form a new low-boiling azeotrope with one of the original constituents, whose volatility
is such that it can easily be separated from the other original constituent. Example:
The following flow sheet describes the azeotropic separation of acetic acid - water solutions, using
butyl acetate as entrainer. *. Acetic acid can be separated from water by ordinary methods, but it will be
highly expensive due low volatility of constituents, hence azeotropic distillation is followed.
The normal boiling point of acetic acid is = 118.1°C and for water is = 100°C.
Butyl acetate is only slightly soluble in water and consequently forms heteroazeotrope with it
(boiling point is -90.2°C). *. Therefore, if sufficient butyl acetate is added to the top of the distillation
column (1) to form the azeotrope with all the water in the feed, the azeotrope can readily be distilled from
the high boiling acetic acid, which leaves as a reside product.
The heteroazeotrope on condensation forms two insoluble liquid layers, one nearly pure water but
saturated with ester, the other nearly pure ester but saturated with water.
The later is returned to the top of the column as reflux and is the source of the entrainer in the
column. *. The former can be stripped of its small entrainer content in a second column (2).

Extractive Distillation
This is a multi component distillation method similar in purpose to azeotropic distillation.

*. To a binary mixture which is difficult or impossible to separate by ordinary means a third component,
termed a solvent is added which alters the relative volatility of the original constituents, thus permitting
the separation. . The added solvent is, however, of low volatility and is itself not appreciably vaporized in
the fractionator. Example:

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Separation of toluene from paraffin hydrocarbons of approximately the same molecular weight is
either very difficult or impossible, due to low volatility or azeotropism yet such a separation is necessary
in the recovery of toluene from certain petroleum hydrocarbon mixtures.
Using isooctane (boiling point 99.3°C) as an example of a paraffin hydrocarbon.
The following figure shows that isooctane in this mixture is more volatile, but the separation is
obviously difficult. . In the presence of phenol (boiling point 181.4°C), however, the isooctane relative
volatility increases, so that, with as much as 83 mole percent phenol in the liquid, the separation from the
toluene is relatively easy.
A flow sheet for accomplishing this is shown in the above figure (b). where the binary mixture is
introduced more or less centrally into the extractive distillation tower (1).
Phenol as solvent is introduced near the top so as to be present in high concentration upon most of
the trays in the tower.
Under these conditions isooctane is readily distilled as an overhead product, while toluene and
phenol are removed as residue. *. The solvent recovery section of the tower, which may be relatively
short, serves to separate the phenol from the isooctane. *. The residue from the tower must be rectified in
the auxiliary tower (2).

Steam Distillation
Steam distillation is used- for separation of a high boiling component from the non-volatile
impurities, for separation of a high boiling mixture into different fractions, wherein the decomposition of
material if we use direct distillation, and in cases where vaporization temperature cannot be reached by
steam heat.
Steam distillation is especially adopted for heat sensitive materials; this kind of materials can be
separated by reducing the partial pressure of the volatile component.
This can be done by making use of an inert vapor that decreases the temperature of distillation,
steam is generally used for this purpose, because steam is immiscible with organic compounds, also it
provides required heat for vaporization and it readily available.
A typical steam distillation set up for purification of organic compounds is shown in the following
figure.

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The impure mixture together with some water is placed in a round bottom flask, which is then connected
to steam generator on one side and a water condenser at other side.
The mixture in the flask is heated and a current of steam passed into it. Steam picks up the volatile
substance from the mixture and passes into the condenser.
The distillate collected in the receiver consists of a mixture of water and the organic substance.
The distillation is stopped when the droplets or the solid particles of the organic substance cease to appear
in the condenser.
The distillate is then treated to recover the organic substance by a suitable method. In case it is a solid, the
substance may be separated by filtration, if it is a liquid, it can be separated by means of separating
funnel.
Steam distillation is employed in industry for the recovery of various essential oils from plants and
flowers.
It is also used in the manufacture of aniline and turpentine oil.
In steam distillation, the composition of vapor produced may be obtained from
Where ma-mass of component being recovered
m- mass of steam
MA-Molecular weight of component being recovered Mn- Molecular weight of steam
PA & PB- Partial pressure of component to be recovered and steam respectively.
P-Total pressure

UNIT-5
DESIGN AND TECHNIQUES OF DISTILLATION COLUMN
Tray towers - calculation of number of trays - McCabe Thiele method - Assumptions in McCabe-Thiele
method -Graphical procedure to determine the number of theoretical trays -total reflux - minimum reflux -
optimum reflux- q line –values of q based on five different feed conditions-operating lines – feed tray
location.- Types of distillation column trays- Types of plate efficiencies- Overall efficiency and Murphree
plate efficiency.
Azeotropic distillation - Extractive distillation - Steam distillation.
PART – A

Q.NO QUESTIONS CO Map BT MARKS

1 Define McCabe Thiele method? CO 5 Re 3

2 What are the methods for calculating the number of trays in distillation column? CO 5 Re 3

3 Write the theoretical stage separation method? CO 5 Re 3

4 What are the limitations of McCabe Thiele method? CO 5 Re 3

6 Write any three assumptions made in McCabe - Thiele method? CO 5 Re 3

8 What is Operating line and q-line? CO 5 Re 3

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9 What is Total reflux? CO 5 Re 3

10 Define minimum reflux ratio? CO 5 Re 3

11 Define optimum reflux ratio? CO 5 Re 3

12 Define Azeotropic distillation with example? CO 5 Re 3

13 Write any three application of Azeotropic distillation. CO 5 Re 3

16 Define extractive distillation with example? CO 5 Re 3

17 Define steam distillation and its use? CO 5 Re 3

19 Define azeotropic distillation and its use. CO 5 Re 3

20 What is the use of mc-cabe method? CO 5 Re 3

21 Draw the graphical diagram of total reflux ratio? CO 5 Re 3

22 Why steam is chosen for steam distillation? CO 5 Re 3

23 Write the types of reflux ratio? CO 5 Re 3

24 Write the types of trays used in distillation columns? CO 5 Re 3

25 Write the types of trays efficiency? CO 5 Re 3

26 Define overall tray efficiency? CO 5 Re 3

27 Define murphree plate tray efficiency? CO 5 Re 3

PART-B
Derive Mc-Cabe Thiele method to determine the number of plates in distillation
1 CO 5 Ap 14
column.

i) Explain in detail Azeotropic distillation.

2 CO 5 Un 14
II) Explain in detail the values of q for five different feed conditions.

3 Explain with details on Types of tray used in distillation columns? CO 5 Un 14

What is q-line? Discuss in detail about various values of q. (ii) Discuss about
4 CO 5 Re 14
murphree plate efficiency and overall efficiency.

5 Explain with Azeotropic distillation and their applications? CO 5 Un 14

6 Explain with Extractive distillation and their applications? CO 5 Un 14

7 Explain with Steam distillation and their applications? CO 5 Un 14

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