National Institute of Technology Calicut Department of Chemical Engineering

National Institute of Technology Calicut

--------------------------- An Institution of National Importance --------------------------
NITC CAMPUS P.O., KERALA – 673 601, INDIA

Department of Chemical Engineering

CH2092E

HEAT AND MASS TRANSFER LABORATORY

Name: __________________________

CH2092E Heat and Mass Transfer Laboratory

National Institute of Technology Calicut Department of Chemical Engineering

CH2092E Heat and Mass Transfer Laboratory

National Institute of Technology Calicut Department of Chemical Engineering

National Institute of Technology Calicut

--------------------------- An Institution of National Importance --------------------------
NITC CAMPUS P.O., KERALA – 673 601, INDIA

Department of Chemical Engineering

CH2092E

HEAT AND MASS TRANSFER LABORATORY

LABORATORY RECORD

Name: _____________________________________________________________

Semester: _____IV__________ Slot: _______________ Year: 2024 - 2025 Winter

Roll No.:____________________________________________________________

Certified that this is the bonafide record of the work done in CH2092E Heat and Mass
Transfer Laboratory of this department at National Institute of Technology Calicut, by

Mr/Miss: ____________________________________________

Place: _____________________
Faculty Incharge
(Signature with Date)

CH2092E Heat and Mass Transfer Laboratory

National Institute of Technology Calicut Department of Chemical Engineering

CH2092E Heat and Mass Transfer Laboratory

National Institute of Technology Calicut Department of Chemical Engineering

INDEX

S. Name of Experiment Date Page Marks Remarks

No No.

10

LIST OF EXPERIMENTS IN MANUAL

1. Composite wall
2. Forced convection
3. Stefan-Boltzmann constant
4. Shell and tube heat exchanger
5. Pool boiling
6. Vapor in air diffusion
7. Simple distillation
8. Adsorption isotherm
9. Forced draft dryer
10. Ternary liquid equilibrium

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Experiment No.: 9 Date: 19th March 2025

HEAT TRANSFER THROUGH COMPOSITE WALL

AIM

Study thermal conduction through a wall made of composite materials

OBJECTIVE

To determine the total resistance of a composite wall and plot the temperature gradient
along the composite wall

INTRODUCTION

If the temperature varies with location in some stationary medium be it a solid or a fluid,
then a “temperature gradient” is said to exist in that medium. Energy in transit due to
such a temperature gradient is called conduction heat transfer. The degree of
temperature variation within a conducting medium is quantified using the mathematical
tools of vector calculus; in particular, the magnitude of the temperature gradient is found
from the derivative of temperature with respect to distance, and the gradient points in the
direction of steepest temperature increase. In this laboratory exercise, you will study
conduction heat transfer in detail, exploring the relationship between heat flux and
temperature gradient, geometrical effects, composite structures, and interfacial
resistance.
This mode of heat transfer is extremely important in industry, with applications in
automotive systems, aerospace systems, chemical and materials processing, electronics
cooling, space conditioning and environmental control, and medicine. In order to
concentrate on the fundamentals of conduction, your experiments will be restricted to
one-dimensional, steady state conditions, where the heat transfer occurs in only a
single coordinate direction and is independent of time.
Heat is always transferred when the temperature difference exists between two bodies.
There are three basic modes of heat transfer:

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Conduction involves the transfer of heat by interactions of atoms or molecules of a

material through which the heat is being transferred.
Convection involves the transfer of heat by mixing and motion of macroscopic portions
of fluid.
Radiation or radiant heat transfer involves the heat transfer by electromagnetic
radiation that arises due to the temperature of the body.

THEORY

In conduction heat transfer problems, the object being studied is usually a solid.
Convection problems involve a fluid medium. Radiation heat transfer problems involve
either solid or fluid surfaces, separated by a gas, vapor, or vacuum. There are several
ways to correlate the geometry, physical properties, and temperature difference of an
object with the rate of heat transfer through the object. In conduction heat transfer, the
most common means of correlation is through Fourier’s Law of Conduction. The law, in
its equation form, is used most often in its rectangular or cyclic. Let's assume that we
have a combination of different materials put together to form a composite structure like
the composite wall. Let's also assume that the cross- sectional area normal to the flow of
heat transfer is constant and the periphery is insulated so that heat flow is
one-dimensional. Taking only one of the slabs for now, the heat transfer is governed by
Fourier's Law: cyclic form (pipes and cylinders), both of which are presented below.
Fourier’s Law

The fundamental relation between the heat flux, q  , and the temperature gradient, ∇T,

for conduction heat transfer in an isotropic medium is

q  = − kT (1)

where, k (W/(m.K)), is an important property of the material called the thermal

conductivity. This relationship is based on observations, and as such we refer to it as
“phenomenological”; it is named Fourier’s Law

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Thoughtful inspection of Fourier’s Law can tell you a lot about conduction heat transfer.
Namely, the conductive heat flux is a vector—it has a magnitude and direction. The
magnitude of the conductive heat flux is proportional to the temperature gradient, and its
direction is coincident with the temperature gradient. Since the temperature gradient is
in the direction of maximum temperature change, the heat flux is in the direction of
maximum temperature change; i.e., it is perpendicular to the isotherms. The minus sign
means the conduction heat flux is in the direction of decreasing temperature. Many
engineers regard Fourier’s law as defining the thermal conductivity; this is a healthy
point of view that you may find useful.
In Cartesian (x, y, z) and cylindrical (r, Φ, z) coordinates, Fourier's Law is expressed as,

q q y ˆ qz  T ˆ T ˆ T 
q  = iˆ x + ˆj +k = −kT = −k  iˆ + j +k  (2)
Ax Ay Az  x y z 

where qx, is the heat transfer rate in the x-direction, , is the thermal conductivity of the
T
material, Ax is the cross-sectional area of the material normal to the x-direction, and
x
is the temperature gradient in the x-direction.
One-Dimensional Conduction in a Cartesian System
Consider the situation shown in Figure 1, where a cylinder of constant cross-sectional
area has a high temperature T1 imposed on its left end and a lower temperature T2 on its
right end.

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Assuming negligible heat loss from the cylinder periphery and that the x-coordinate is
aligned with the cylinder axis, the heat transfer and temperature gradient will occur in
the x-direction only (i.e., heat transfer is by one-dimensional conduction). For steady
state conditions (∂T/∂t = 0) with no heat generation, the heat diffusion equation becomes

dq x
=0 (3)
dx

d  dT 
 =0 (4)
dx  dx 

The first form states that under these conditions the heat flux, q x is a constant,
independent of x. If the thermal conductivity can be assumed to be constant, the second
form reduces to

d 2T
=0 (5)
dx 2

This can be integrated twice to obtain the general form of the temperature distribution.

T ( x) = C1 x + C2 (6)

Applying boundary conditions T(0) = T1, at the left and T(L) = T2 at the right end gives

T2 − T1
C2 = T1 and C1 = (7)
L

Substituting into the general solution for T(x):

T ( x) − T1 x
= (8)
T2 − T1 L

This result demonstrates the well-known finding that for steady one dimensional heat
conduction through a plane wall with constant thermal conductivity and no volumetric
heat generation, the temperature varies linearly with x.
Now using Fourier’s law to relate the heat flux to the temperature gradient

Q dT − k (T1 − T2 )
q x = = −k = (9)
Ax dx L

qx, is the heat transfer rate in the x-direction , and A, is the cross-sectional area normal to
the x-direction.

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Substituting this equation into the solution for T(x), the temperature distribution may
also be expressed in the form

qx
T ( x) = T1 − x (10)
kA

In analogy with Ohm’s law for electrical resistance R elec =∆E/I, the thermal resistance is
defined as the ratio of the driving potential ΔT to the corresponding transfer rate qx. For
steady heat transfer through a plane wall, the thermal resistance for conduction is
therefore given by

T1 −T 2 L
Rcond = = (11)
qx kA

Equivalent Resistance Method:

There is an analogy between the conduction of electricity and the conduction of heat.
Since electrical resistance is associated with the conductance of electricity, there is also a
thermal resistance associated with the conduction of heat. Composite fluids and solids
behave much like series and parallel combinations of resistors in an electrical circuit.
Using this approach we can add up the thermal resistances to find the overall resistance
and heat transfer coefficient.
It is possible to compare heat transfer to current flow in electrical circuits. The heat
transfer rate may be considered as a current flow and the combination of thermal
conductivity, thickness of material, and area as a resistance to this flow. The temperature
difference is the potential or driving function for the heat flow, resulting in the Fourier
equation being written in a form similar to Ohm’s Law of Electrical Circuit Theory. If
the thermal resistance term Dx/k is written as a resistance term where the resistance is
the reciprocal of the thermal conductivity divided by the thickness of the material, the
result is the conduction equation being analogous to electrical systems or networks. The
electrical analogy may be used to solve complex problems involving both series and
parallel thermal resistances. The student is referred to Figure 2, showing the equivalent
resistance circuit. A typical conduction problem in its analogous electrical form is given
in the following example, where the "electrical" Fourier equation may be written as
follows.
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DATA:
Wall thickness of composite slab = 0.045 m
Bakelite:
Diameter = 25 cm
Thickness = 10 mm
Brass:
Diameter = 25 cm
Thickness = 10 mm
Mild Steel:
Diameter = 25 cm
Thickness = 25 mm

OBSERVATION TABLE:

S Voltage Current Temperature (℃)

No. (V) (I)
T1 T2 T3 T4 T5 T6 T7 T8
1 100 0.35 45 45 44 44 37 37 36 36
2 110 0.39 50 50 49 49 40 40 39 39
3 120 0.43 57 57 56 56 44 44 43 43

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Figure 2: Equivalent resistance for thermal conduction through a composite wall

We now must introduce the concept of thermal resistance for conduction. Resistance in
general is defined as the ratio of driving potential over the transfer rate. As transfer rate
goes to zero, the resistance becomes infinite and, similarly, as the driving potential goes
to zero, resistance fails to exist. By using Fourier's Law and the definition of resistance,
we can derive the thermal resistance for conduction as

LA L L
Rcond = + B + C
k A A k B A kC A

APPARATUS DESCRIPTION:
The apparatus consists of a central heater sandwiched between two sheets. Three types
of slabs are provided both sides of heater, which forms a composite structure. A small
hand press frame is provided to ensure the perfect contact between the slabs. A
dimmerstat is provided for varying the input to the heater and input measurements are
carried out by a voltmeter and an ammeter. Thermocouples are embedded between
interfaces of the slabs, to read the temperature at the surface.

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APPARATUS:

SPECIFICATIONS:
Electricity Supply: 1 Phase, 220 V AC, 2 Amp.
Table for set-up support.

TECHNICAL DETAILS:
Slab assembly arranged symmetrically provided on both sides of heater.
Slab Material and Slab Size:
Cast Iron : 250 mm diameter & 20 mm thick.
Bakelite : 250 mm diameter & 15 mm thick.
Press Wood : 250 mm diameter & 12 mm thick.
Heater : Nichrome wire.
CONTROL PANEL COMPRISING OF
Digital Voltmeter : 0-300 Volts.
Digital Ammeter : 0-2 Amp.
Variac : 0-230 V, 2 Amp.
Digital Temp. Indicator : 0-200 °C, with multi-channel switch
Temperature Sensors : RTD PT-100 type.

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EXPERIMENTAL PROCEDURE:
1) See that plates are symmetrically arranged on both sides of the heater plates.
2) Operate the hand press properly to ensure perfect contact between the plates.
3) Close the box by cover sheet to achieve steady environmental
4) Start the supply of heater by varying the dimmerstat. Adjust the input to desired value
5) Take readings of all the thermocouples at an interval of 10 minutes until fairly steady
temperatures are achieved and rate of rise is negligible.
6) Note down the reading in observation table.

PRECAUTIONS:
1) Keep the dimmer stat at zero before switching on the power supply.
2) Do not disturb the thermocouples while testing.
3) Do not increase the power supply above 150 V.
4) Increase the voltage slowly.

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MODEL CALCULATIONS:
S. No.: 1

Mean temperature readings:

TA = (T1 + T2)/2 = (45+45)/2 = 45 ℃

TB = (T3 + T4)/2 = (44+44)/2 = 44 ℃

TC = (T5 + T6)/2 = (37+37)/2 = 37 ℃

TD = (T7 + T8)/2 = (36+36)/2 = 36 ℃

Area of the plates, A = πd2/4, where d is diameter of the plates

A = π × 0.252 / 4 = 0.04906 m2

Heat supplied Q = V × I (Watts) = 100 × 0.35 = 35W

Heat flux q” = Q/A (W/m2) = 35/0.04906 = 713.4121 W/m2

Average total thermal resistance, Rtotal = (TA – TD)/q”

= (45-36)/713.4121

= 1.2615 x 10-2 m2K/W

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LA L L
Equivalent resistance method: Rcond = + B + C
k A A k B A kC A

QL A
For mild steel, k A = W/mK = (35*25*10-3 )/(0.04906) *(45-44)
A(TA − TB )

kA = 17.8353 W/mK

QL B
For Bakelite, k B = W/mK = (35*10*10-3 )/(0.04906) *(44-37)
A(TB − TC )

kB = 1.01916 W/mK

QLC
For Brass, k C = W/mK = (35*10*10-3 )/(0.04906) *(37-36)
A(TC − TD )

kC = 7.1341W/mK

Rtotal = (25*10-3 )/ (0.04906*17.8353) + (10*10-3 )/ (0.04906*1.0191) +

(10*10-3 )/(0.04906*7.1341) = 0.25715 Km2/W

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GRAPH:

Plot temperature in y-axis and thickness or length of the wall along x-axis

DISTANCE V/S TEMPERATURE

100V 110V 120V
60

50

40
TEMPERATURE IN OC

30

20

10

0
0 25 35 45
DISATNCE IN MM

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RESULTS:

The heat transfer through a composite wall through conduction has been investigated.
The temperature vs length of the walls has been plotted. The average total resistance of
the given composite wall has been found to be 0.25715 Km2/W.
The thermal conductivity of the three materials namely Bakelite, Brass and Mild Steel
are 1.01916 W/mK, 7.1341 W/mK and 17.8353 W/mK respectively for calculations
number 1.

DISCUSSION:

1. This experiment helps us to determine which material has a higher or lower rate

of heat dissipation.

2. With higher temperature difference, the heat flux also increases.

SAFETY PRECAUTIONS:

1. Avoid direct contact with hot surfaces – The composite wall can reach high
temperatures; use heat-resistant gloves if handling components.

2. Allow components to cool before touching – After the experiment, let the system
cool down before disassembling.

3. Use heat insulation – To minimize heat loss and accidental burns, ensure proper
insulation around the heated sections.

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Experiment No.: Date:

FORCED CONVECTION
AIM
To determine the heat transfer coefficient for a forced convection setup and verify the
Dittus – Boelter equation.
INTRODUCTION:
In many practical situations, we invariably deal with flow of fluids in tubes e.g. boiler,
super heaters and condensers of a power plant, automobile radiators, water and air
heaters or coolers etc. the knowledge and evolution of forced convection heat transfer
coefficient for fluid flow in tubes is essentially a prerequisite for an optional design of all
thermal system.
Convection is the transfer of heat within a fluid by mixing of one portion of fluid with
the other. Convection is possible only in a fluid medium and is directly linked with the
transport of medium itself. In forced convection, fluid motion is principally produced by
some superimposed velocity field like a fan, blower or a pump.
THEORY:
The essential ingredients of forced convection heat transfer analysis are given by

Newton's Law of Cooling, Q = kA(Tw − T ) = hAT

The rate of heat Q0 transferred to the surrounding fluid is proportional to the object's
exposed area A, and the difference between the object temperature Tw and the fluid
free-stream temperature T∞.
The constant of proportionality h is termed the convection heat-transfer coefficient.
Other terms describing h include film coefficient and film conductance. The Dittus –
Boelter correlation (1930) is a common and particularly simple correlation useful for
many applications. This correlation is applicable when forced convection is the only
mode of heat transfer; i.e., there is no boiling, condensation, significant radiation, etc.
The accuracy of this correlation is anticipated to be ±15%.
The Dittus- Boelter equation, has two forms as follows:

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Nu = 0.023 Re0.8 Pr0.4, for ‘heating’ (temperature of wall > temperature of fluid)
Nu = 0.026 Re0.8 Pr0.3, for ‘cooling’ (temperature of wall < temperature of fluid)

Forced Convection apparatus

SPECIFICATIONS:
Test pipe = 33 mm internal diameter, 500 mm long
Diameter of pipe = 22 mm
Cd = 0.64
Cross sectional area of pipe = 8.3 × 10-4 m2

OBSERVATIONS:
S. Hw Voltage Current T1 T2 T3 T4 T5 T6 T7
No (cm) (V) (A) (℃) (℃) (℃) (℃) (℃) (℃) (℃)

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FORCED CONVECTION APPARATUS:

The apparatus consists of a blower unit fitted with the test pipe. The test section is
surrounded by a Nichrome band heater. Four thermocouples are embedded on the test
section and two thermocouples are placed in the air stream at the entrance and exit of
the test section to measure the air temperature. Test pipe is connected to the delivery
side of the blower along with the orifice to measure flow of air through the pipe. Input
to the heater is given through a dimmerstat and measured by meters.
It is to be noted that only a part of the total heat supplied is utilized in heating the air. A
temperature indicator with cold junction compensation is provided to measure
temperatures of pipe wall at various points in the test section. Airflow is measured
with the help of orifice meter and the water manometer fitted on the board.

PROCEDURE:
1. Switch ON the mains system
2. Switch ON the blower.
3. Adjust the flow using gate valve to a desired difference in the manometer level.
4. Start heating the test section with the help of dimmerstat and adjust the desired
heat input with the help of Voltmeter (125 V) and Ammeter.
5. Take readings of all the seven thermocouples after the steady state is reached.
6. Note down the heater input.
7. Repeat the experiment for different air flow rate or power rates

PRECAUTIONS:
1. Keep the dimmer stat at zero position before switching ON the power supply.
2. Increase the voltmeter gradually.
3. Do not stop the blower in between the testing period.
4. Do not disturb thermocouples while testing. Operate selector switch of the
thermocouple gently. Don’t exceed 200 Watts
5. Operate selector switch of the temperature indicator gently.

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CALCULATIONS: S. No. _________

ρa0 =

ρa =

Ta = (T1 + T7)/2 =

Ts = (T2 + T3 + T4 + T5 + T6)/5 =

ha = hw × (ρw/ρa) =

ao = π do / 4 =

Q = Cd × ao × √(2gha) (m3/s) =

ma = Q × ρa =

ap = π dp2 / 4 =

v = Q / ap (m/s) =

q = ma Cp (T7 – T1) (W) =

A = π×D×L (m2) =

ε = 0.4

q1 = σεA(Ts4 – Ta4) (W) =

Actual heat loss = Qconv = q – q1 =

Heat transfer coefficient, hexpt = Qconv / (A(Ts – Ta)) =

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NOMENCLATURE:

ρao Density of air at 273 K

ρa Density of air at inlet temperature

ρw Density of water at room temperature

ha Head of air

hw Head of water

Q Volumetric flow rate of air

Cd Coefficient of discharge of orifice = 0.64

Cp Specific heat of air at ambient temperature

μ Dynamic viscosity of air at ambient temperature = 19.05×10-6 Ns/m2

do Diameter of orifice = 22 mm

ao Cross section area of orifice

ap Cross section area of pipe

ma Mass flow rate of air

v Velocity of air

q Heat gained by air

D Internal diameter of test pipe = 33 mm

L Length of the test pipe = 500 mm

A Lateral surface area of test pipe

ε Emissivity of test pipe

q1 Heat loss by radiation

σ Stefan Boltzmann constant = 5.672×10-8 W/m2K4

Ts Surface temperature

Ta Ambient temperature

hexpt Experimental heat transfer coefficient

htheo Theoretical heat transfer coefficient

k Thermal conductivity of air at ambient temperature

NRe Reynolds number

Nu Nusselt number

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NPr Prandtl number

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Dittus – Boelter equation verification:

Here, Ts _________ Ta, hence we use

Nu = __________NRe______ NPr______

Dv  a
N Re = =


Cp
N Pr = =
k

Nu =

htheo = Nu k / D =

S No Q (m3/s) v (m/s) hexpt (W/m2K) htheo (W/m2K)

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RESULTS:

The heat transfer coefficient has been found from experiments and theoretical
expression of Dittus Boelter equation. The error is about _________ %.
The experimental heat transfer coefficient is about ________________ W/m2K.

DISCUSSION:

SAFETY AND PRECAUTIONS:

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Experiment No.: Date:

STEFAN BOLTZMANN CONSTANT

AIM
Determine the Stefan – Boltzmann constant using a heat transfer by radiation setup

INTRODUCTION:
Thermal radiation is electromagnetic radiation generated by the thermal motion of
charged particles in matter. All matter with a temperature greater than absolute zero
emits thermal radiation. The energy transfer by conduction and convection requires
some material carrier, but the transfer of energy by radiation can take place in a vacuum
without a material carrier between the heat source and the receiver.
A black body is an idealized physical body that absorbs all incident electromagnetic
radiation. Because of this perfect absorptivity at all wavelengths, a black body is also the
best possible emitter of thermal radiation, which it radiates incandescently in a
characteristic, continuous spectrum that depends on the body's temperature. At
Earth-ambient temperatures this emission is in the infrared region of the electromagnetic
spectrum and is not visible. The object appears black, since it does not reflect or emit
any visible light.
Absorptivity: If the amounts of radiation energy absorbed, reflected, and transmitted
when radiation strikes a surface are measured in percentage of the total energy in the
incident electromagnetic waves. The total energy would be divided into three groups,
they are called Absorptivity (α), Reflectivity (ρ), and Transmissivity (τ), with α+ρ+τ = 1.
Absorptivity: It is the fraction of irradiation absorbed by a surface.
Reflectivity: It is the fraction reflected by the surface.
Transmissivity: It is the fraction transmitted by the surface.
A body is considered transmit some of the radiation waves falling on its surface. If
electromagnetic waves are not transmitted through the substance it is therefore called
opaque. When radiation waves hit the surface of an opaque body, some of the waves are
reflected back while the other waves are absorbed by a thin layer of the material close to
the surface. For engineering purposes all materials are thick enough to be considered as
opaque, reducing α + ρ = 1.
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The emissivity of a material (usually written ε or e) is the relative ability of its surface to
emit energy by radiation. It is the ratio of energy radiated by a particular material to
energy radiated by a black body at the same temperature. A true black body would have
ε = 1 while any real object would have ε < 1. Emissivity is a dimensionless quantity.
Stefan Boltzmann law:
The Stefan–Boltzmann law, also known as Stefan's law, states that the total energy
radiated per unit surface area of a black body per unit time (known variously as the
black-body irradiance, energy flux density, radiant flux, or the emissive power) q , is
directly proportional to the fourth power of the black body's thermodynamic
temperature T (also called absolute temperature):

q = AT 4

where,
q = rate of heat transfer (W)
σ = 5.67 × 10-8 W/m2K4, Stefan Boltzmann constant
A = surface area of the emitting body (m2)
The Planck law gives the intensity radiated by a blackbody as a function of frequency (or
wavelength). Let a blackbody have temperature T. Let be the energy density per unit

solid angle so that dE = u v ()dVdv

Then the blackbody radiates at a frequency with spectral energy density

2h 3
u v () = 3
c exp( h /( kT )) − 1

where h is Planck's constant, c is the speed of light, and k is Boltzmann's constant.

Wien’s Displacement law:
The wavelength corresponding to the peak emission in various black body spectra are
function of temperature. Wien's displacement law states that there is an inverse
relationship between the wavelength of the peak of the emission of a black body and its
temperature. i.e. λmax = b/T
where, λmax is the peak wavelength in meters and
b is constant of proportionality called Wien’s displacement constant = 2.8976 × 10-3 mK

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Figure 1. Depicting Wien’s displacement law

Kirchhoff’s Law:
An object at some non-zero temperature radiates electromagnetic energy. If it is a perfect
black body, absorbing all light that strikes it, it radiates energy according to the
black-body radiation formula. More generally, it is a "grey body" that radiates with some
emissivity multiplied by the black-body formula. Kirchhoff's law states that:
At thermal equilibrium, the emissivity of a body (or surface) equals its absorptivity.

EXPERIMENTAL APPARATUS:
The apparatus consist of a water heater jacket of hemisphere shape, where a hemisphere
is surrounded by hot water. A copper test disc is fitted at the center of jacket. The hot
water is obtained from hot water tank, fitted to the panel in which water is heated by an
electric heater. The hot water is taken around the hemisphere, so that hemisphere
temperature rises. The test disc is then inserted at the center. Thermocouples are fitted
inside hemisphere to find the average hemisphere temperature. Another thermocouple is
fitted at the center of the test disc to measure the temperature of the test disc. A timer
with a small buzzer is provided to note down the disc temperature at the time interval of
5 sec.
When the blackened disc is inserted at the centre of the hemisphere, heat is transferred to
the disc from hemisphere by radiation and its temperature begins to rise and from
temperature rise rate (it is be the intervals of 5 seconds) Using this data, Stefan –
Boltzmann constant is determined

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Figure 2: Stefan Boltzmann apparatus

OBSERVATIONS:
Time (s) T4 (℃) Time (s) T4 (℃) Time (s) T4 (℃)

0 70 140

5 75 145

10 80 150

15 85 155

20 90 160

25 95 165

30 100 170
35 105 175
40 110 180

45 115 185
50 120 190

55 125 195

60 130 200
65 135

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PROCEDURE:
1. Ensure that all the valves are closed except the overflow valve on the test setup
2. Ensure that copper disc is pulled down and water is present in the top water tank
3. Heat the water in top water tank to about 80℃ as measured by thermocouple T5
4. Open the gate valve very slowly so that water flows from hot water tank and fills
around the hemisphere. Close the gate valve immediately if hot water overflows
5. Measure the temperatures on hemisphere using thermocouples T1, T2 and T3
6. Change reading to T4 and Push the copper test disc up to reach the centre
7. Note temperature T4 every five seconds until about 200 seconds
8. Pull the copper test disc down to its original position
9. Once the water around the hemisphere has cooled, drain it and refill the top tank
EQUATIONS:
According to Stefan –Boltzmann law, energy radiated by a body per unit area per unit
time is given by
R = εσT4, where R is energy radiated per unit area per time
ε = emissivity of the material
σ = Stefan –Boltzmann constant = 5.67 x 10-8 W/m2K4
T = temperature in Kelvin scale.
For a black body emissivity =1, hence, R = σ T4
In the given experiment set up the net heat transfer to the disc per second is
∆Q/∆t = m CpdT/ dt = σA[Th4 –Td4]
From the above equation,

mC p dT / dt
=
A(Th4 − Td4 )

m = mass of the disc only

Cp = specific heat of material of the disc
dT/dt = slope of the temperature –time graph of the hemisphere
A = area of the disc
Th = steady state temperature of the hemisphere in Kelvin
Td = steady state temperature of the disc in Kelvin
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Temperature reading of three thermocouples on the hemisphere

T1 (℃) T2 (℃) T3 (℃)

CALCULATIONS:

T1 + T2 + T3
Hemisphere temperature = + 273.15 = = _______ K
3

Initial disc temperature = T5 sec = _____________ K

m, mass of the disc = 5.2 g = ________________ kg

d, diameter of the disc = 20 mm

A, area of the disc, m2 = πd2/4 = = ____________

Cp specific heat capacity of disc material = ________________

Slope, dT/dt from graph = ___________________

mC p dT / dt
= =
A(Th4 − Td4 )

GRAPH:
Plot the temperature T (in ℃) in y-axis and time t (in seconds) in x-axis.

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RESULTS:

Heat transfer in a black body radiation setup was studied and the Stefan Boltzmann

constant was calculated as _________________, which has error of ___________ %

from expected value of 5.67 × 10-8 W/m2K4.

DISCUSSION:

SAFETY PRECAUTIONS:

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CH2092E Heat and Mass Transfer Laboratory Page No.

National Institute of Technology Calicut Department of Chemical Engineering

Experiment No.: Date:

SHELL AND TUBE HEAT EXCHANGER

AIM

To determine the heat transferred between the hot and cold fluid flowing through a shell
and tube heat exchanger. Determine the internal and external overall heat transfer
coefficients of heat transfer for this setup. Determine the temperature efficiencies.

INTRODUCTION:

A heat exchanger is a piece of equipment built for efficient heat transfer from one
medium to another. The media may be separated by a solid wall, so that they never mix,
or they may be in direct contact. Shell and tube heat exchanger is a class of heat
exchanger designs. It is the most common type of heat exchanger in oil refineries and
other large chemical processes, and is suited for higher-pressure applications. This type
of heat exchanger consists of a shell (a large pressure vessel) with a bundle of tubes
inside it. One fluid runs through the tubes, and another fluid flows over the tubes
(through the shell) to transfer heat between the two fluids. The set of tubes is called a
tube bundle, and may be composed by several types of tubes: plain, longitudinally
finned, etc. In this way, waste heat can be put to use. This is an efficient way to conserve
energy. Heat exchangers with only one phase (liquid or gas) on each side can be called
one-phase or single-phase heat exchangers. Two-phase heat exchangers can be used to
heat a liquid to boil it into a gas (vapor), sometimes called boilers, or cool a vapor to
condense it into a liquid (called condensers), with the phase change usually occurring on
the shell side. There are also single pass, and multi pass exchangers, based on the
number of passes of the shell side or tube side liquids.
We apply the same formula of Q = m Cp ΔT to their shell and tube side fluids.
Qe = mH C pH (THi − THo )
Qa = mC C pC (TCo − TCi )

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Here,
Qe = heat emitted by the hot fluid (W)
mH = mass flow rate of the hot fluid (kg/s)
CpH = specific heat of the hot fluid at its average temperature (J/kg K)
THi = inlet temperature of the hot fluid (K)
THo = outlet temperature of the hot fluid (K)
Qa = heat absorbed by the cold fluid (W)
mC = mass flow rate of the cold fluid (kg/sec)
CpC = specific heat of the cold fluid at its average temperature (J/kg K)
TCo = outlet temperature of the cold fluid (K)
TCi = inlet temperature of the cold fluid (K)
The average temperature is:

THi + THo TCi + TCo

Tavg , H = and Tavg ,C =
2 2

The temperature efficiencies are calculated as

THi − THo TCo − TCi

H =  100 and C =  100
THi − TCi THi − TCi

The mean temperature efficiency is calculated as

 H + C
m =
2

The logarithmic mean temperature difference is

T1 − T2
Tln =
 T 
ln  1 
 T2 
where, ΔT1 = THi – TCo and ΔT2 = THo – TCi
The overall heat transfer coefficient is defined by the formula

Qe
U=
ATln

where, A is the area of heat transfer (m2) and Q is heat emitted from the hot fluid (W)

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APPARATUS DESCRIPTION:
The apparatus is a shell and tube heat exchanger itself. It has an external heater
attached to it, to heat the hot flow water. The liquids used in both the sides of the
apparatus id water. Thus, water is heated and sent into the hot water inlet at point 2,
shown in Figure 1. Cold water is sent into the cold water inlet at point 1. Similarly, the
hot water is removed from the hot water outlet at point 4. And the cold water is
removed from the cold water outlet at point 3.
The hot water flows in the tubes, and the cold water flows in the shell. The baffles are
provided to promote the counter flow of the shell side liquid. The hot fluid is heated to
a constant temperature by an external heater. The cold fluid is let directly from the tap.
To measure the temperatures, there are four thermo couples at the points 1, 2, 3, 4.
Their readings respectively give the temperatures TCi, THi, TCo, THo. To measure the
flow rate of the hot and cold fluids, two rotameters are fixed to the apparatus. One
measures the flow rate of the cold fluid as it enters, and the other measures the flow
rate of the hot fluid as it leaves. There is also a control valve and a bypass valve to
control the flow of the hot water. There is an indication panel where the readings of the
thermocouples can be read.
PROCEDURE:
1. Fill water in the water bath and switch on the heaters.
2. Adjust the required temperature of hot water.
3. Adjust the control valve. Allow hot water to recycle in bath through by pass
switching on the magnetic pump.
4. Start flow of cold water through annulus and set the exchanger to counter flow.
5. Measure the flow rate of cold water and hot water by using rotameter or beakers.
6. Keeping the flow same, wait till steady state condition is reached (30 minutes).
7. Record the temperature of the hot water and cold water side and also the flow
rate accurately.
8. Now change the flow of the cold water using the control valve.
9. Repeat the procedure again

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Figure 1: Shell and tube heat exchanger

DATA:
Internal area of the tube (Ai) = 3.187×10-3 m2
External area of the tube (Ao) = 4.827×10-3 m2
External diameter of the tube (d0) = 16 mm
Internal diameter of the tube (di) = 13 mm
Diameter of the shell (ds) = 220 mm
Length of the shell (L) = 500 mm
Number of tubes (N) = 24

OBSERVATIONS:
S. Hot Water Cold Water
No V mL t (s) THi ℃ THo ℃ V mL t (s) TCi ℃ TCo ℃

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SAMPLE CALCULATIONS:
S. No._____________

Tavg,H = ρH at Tavg,H = _____________ kg/m3

Tavg,C = ρC at Tavg,C = _____________ kg/m3

Mass flow rate, mH = = ___________ kg/s

Mass flow rate, mC = = ___________ kg/s

Amount of heat transferred,

QH = mH × CPH × (THi – THo) = = ____________ kW

QH = mH × CPH × (THi – THo) = = ____________ kW

Average of actual heat transferred, Qavg = (QH+QC)/2 =

ΔT1 = THi – TCo =

ΔT2 = THo – TCi =

ΔTLMTD = = _____________ K

Uo = Qavg/(Ao ΔTLMTD) =

= =_____________ W/m2K

Ui = Qavg/(Ai ΔTLMTD) =

= =_____________ W/m2K

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Efficiencies are calculated as

ηH =

ηC =

ηm =

For Hot Fluid

Tavg ℃ ρH kg/m3 CpH kJ/kg mH kg/s QH kW

For Cold Fluid

Tavg ℃ ρC kg/m3 CpC kJ/kg mC kg/s QC kW

Overall Results

S. No. ΔTm ℃ Qavg kW Uo Ui ηH ηC ηm

W/m2K W/m2K

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RESULTS:
The heat transfer between the hot and cold fluid flowing through a _______ current

shell and tube heat exchanger has been investigated. Using log mean temperature, the

average internal and external overall heat transfer coefficients were determined to be

__________________ and _________________ respectively. The mean temperature

efficiency was found to be ____________

DISCUSSION:

SAFETY PRECAUTIONS:

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Experiment No.: 3 Date: 19th March

2025

CRITICAL HEAT FLUX IN POOL BOILING OF WATER

AIM
To study the heat transfer during boiling phenomena and determine the critical heat flux
in pool boiling of water.

THEORY:
The general boiling is a convection process involving a change is phase from liquid the
vapour. Boiling may occur when a liquid is to contact with a surface maintained at a
temperature higher than the saturation temperature of the liquid of heat is added to a
liquid from a submerged solid surface. The boiling process is referred to as pool boiling.
In this process the vapour produced may form bubbles, which glows and subsequently
detach them from the surface, rising to the free surface due to buoyancy effects.

PROCEDURE:
1. Distilled water is to be taken in the container.
2. The heaters are to be completely submerged.
3. The heater coil and best heater wire are connected across the studs and electrical
connections are made.
4. Heater coil is switched ON and left ON till the required bulk temperature of water
reaches the desired value.
5. Then bulk heating coil is switched OFF and the test heater is switched ON.
6. The boiling phenomenon on wire is observed, by varying the voltage across it using
the dimmerstat.
7. As the voltage is increased further and a point is reached when wire breaks (keep
rigorous note of the current) and at this point the voltage and current are to be noted
8. Change the nichrome wire and repeat with different bulk temperature

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Figure
OBSERVATION TABLE:
S. No TWater (℃) Voltage V (V) Current I (A) Q (W) qE (W/m2)

1 80 36 5.27 3.48*106 9.37*107

2 90 32 4.90 2.73 *106 8.935* 107

3 100 27 3.57 1.67 *106 8.642* 107

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APPARATUS DESCRIPTION:

The apparatus consists of 5 L borosil container. An immersion heater is fixed in a

circular plate. The complete set is connected in the top of the container. The heater is
completely submerged in the distil water of the container.

SPECIFICATIONS:

Length of the nichrome wire, L = 100 mm

Diameter of the nichrome wire, d = 0.183 mm

FORMULA:

 ( l −  v )g 
1/ 4

Theoretical value of critical heat flux, qT = 0.18hlv  v  

  v2 
VI
Experimental value of heat flux, q E = Q / A =
A

hlv = latent heat of vaporization = 2257 kJ/kg

ρv = density of vapour
ρl = density of liquid
σ = surface tension of water =(75.69 – 0.1413T – 0.0002985T2)nN/m (T in ℃)
g = acceleration due to gravity
A = surface area of wire = πdL

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GRAPH:
Plot qE in y-axis and temperature in x-axis

SAMPLE CALCULATION:
S. No.: 3

A = 3.14*D*L = 3.14*0.183*10-3 *100*10-3

= 5.7491*10-5 m2

= 27*3.57/(5.7491*10-5 )

=1. 6766 *106 W/ m2

= 8.642 *107 W/m2.

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RESULTS:

We have successfully studied the boiling heat transfer phenomena and determined the
critical heat flux of pool boiling at 60 ℃, 80 ℃ and 100 ℃. The variation is also
plotted as a graph.

DISCUSSION:

1. We investigated about pool boiling in water

2. We observed different regimes of pool boiling while heating the wire

3. As the bult temperature increases, the current required to break the wire

decreases. (Since Boiling heat transfer coefficient increases with temperature,

less energy is required to break the wire). Also, Leidenfrost effect leads to
overheating.

SAFETY PRECAUTIONS:

1. When changing nichrome wire, avoid touching the heating element and hot
water.
2. Turn off main switch before changing the wire.

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Experiment No.: Date:

VAPOUR IN AIR DIFFUSION

AIM

Study of the effect of temperature on the diffusion coefficient

OBJECTIVE

To determine the diffusion coefficient of an organic vapour (Acetone) in air

INTRODUCTION

Diffusion is concerned with the movement of individual molecules through a substance

by virtue of their thermal energy. The phenomenon of molecular diffusion ultimately
leads to a completely uniform concentration of substances throughout a solution which
may initially have been non uniform. So this equipment is very helpful in determining
the diffusion coefficient of an organic vapour. We can also study the effect of
temperature on the diffusion coefficient.

THEORY

If two gases are inter-diffusing with a continual supply of fresh gas and removal of the
products of diffusion, this diffusion reaches an equilibrium state with constant
concentration gradients. This is known as steady state diffusion. If also there is no total
flow in either direction the rates of diffusion of A and B, N A and NB are equal but have
opposite sign.
As per Dalton’s law, the total concentration of the two components CA and CB is constant

dC A dC
=− B
dx dx

Then using the integrated form of the Fick’s Diffusion equation

D D
NA = ( PA1 − PA2 ) = N B = ( PB1 − PB 2 )
RTx RTx
where PA1 and PA2 are the partial pressures of A at the boundaries of the zone of diffusion
and x is the distance over which diffusion occurs., CA = Molar concentration of A,
kmol/m3.

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NOMENCLATURE

CB = Molar concentrations of B, kmol/m3

CT = Total molar concentration, kmol/m3
CBM = Log mean concentration of CH3-CO-CH3, kmol/m3
DAB = Diffusion coefficient, m2/s
MA = Molecular weight of CH3-CO-CH3 (component A), kg/kmol
P = Total Pressure, kN/m2
R = Gas Law Constant, kN m/kmol K
T = Operating temp, K
VP = Vapour pressure of the evaporating liquid, kN/m2
x = Final height from the top end of the tube after time θ, cm
x0 = Initial height from the top end of the tube, cm
x0 – x = Drop in liquid (CH3-CO-CH3) level in time θ, cm
θ = Time of evaporation, s
ρl = Density of CH3-CO-CH3, kg/m3
S = slope of graph s/cm

Figure 1 Experimental Setup

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In the case where gas A is diffusing through stagnant gas, B (non-diffusing) the flow
carries both components in proportions to their partial pressure

The total transfer of A is the sum of this proportion of the flow and the transfer by
diffusion

This is the expression used for the experimental determination of vapour diffusion
coefficients in gases by evaporation from a liquid surface in a narrow bore tube and
measuring the fall of the level of this surface. The distance of the liquid surface below
the open end of the tube is measured before and after evaporation over a definite period.
If the variation in level is small, then arithmetic mean of these two readings is taken as
the value of x. In case there is an appreciable change of level, the value of x is
determined by the integration between the initial and final readings of the level.

The rate of evaporation is thus given by:

Integration of this expression yields:

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DATA
P = ____________________ kN/m2
R = ____________________ J/mol K
MA = ____________________ kg/kmol
ρl = ____________________ kg/m3 at T = ______________
ρl = ____________________ kg/m3 at T = ______________

OBSERVATIONS
T = ___________________ K x0 = ______________ cm
x, cm
S. No θ, s (x0 – x), cm θ/(x0 – x), s/cm
3 decimals
1 300

2 600

3 900

4 1200

5 1500

6 1800

T = ___________________ K x0 = ______________ cm
x, cm
S. No θ, s (x0 – x), cm θ/(x0 – x), s/cm
3 decimals
1 300

2 600

3 900

4 1200

5 1500

6 1800

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Usually, x0 will not be measured accurately nor is the effective distance for diffusion, x,
at time θ. However, accurate values of (x – x0 ) are available, hence we rewrite Equation
(2) as:

CB1 shall be equal to CT.

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CALCULATIONS:

Calculation of vapour pressure, VP (N/m2) of acetone at temperature, T:

C2
ln( VP) = C1 + + C3 ln T + C4T C5 (T in K)
T

where,
C1 = 69.006 C2 = −5599.6
C3 = −7.0985 C4 = 6.2237 x 10-6
C5 = 2

VP of Acetone (at T = _______) =

= _____________ kN/m2

VP of Acetone (at T = _______) =

= _____________ kN/m2
GRAPHS:
Find the slope S from the plot of θ /(x0 − x) in y-axis vs (x0 − x) in x-axis

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Effect of temperature and pressure on the coefficient of diffusion, D is expressed as:

D = Const. T1.5/P
D can be determined by drawing a curve of DP vs. T.

DESCRIPTION

The equipment consists of a T tube made of glass, placed in a constant temperature water
bath. The temperature of the bath is controlled by the DTC. Air pump is used to supply
the air, passed through the T tube. Volatile component is filled in the T tube and air
passed over it by the pump and change in the level is seen by the sliding microscope.

PROCEDURE

1. Clean the apparatus and make it free from dust.

2. Fill 3/4th water bath with water.
3. Set the water bath temperature at the desired level (35 °C and 50 °C) and wait till
the bath attains the set temperature. Note the steady temperature of the bath.
4. Fill the T-tube with Acetone (CH3-CO-CH3) up to within two centimeters of the
top of the capillary leg. Note down the initial diffusion height of liquid in the
capillary
5. Make the connection with the air or vacuum pump and allow a gentle current of
air to flow over the capillary.
6. Record the height of liquid (x) in the capillary after every min
7. Repeat the steps 1 through 5 for different water bath temperatures.
8. Use different organic liquids like ethanol, toluene, CCl4, hexane etc. and tabulate
the results and discuss.

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For T =

P
CT = =
RT

(VP) A
CA =  CT =
P

From graph, S =

C B1 = CT =

P − (VP) A
CB2 =  C B1 =
P

C B1 − C B 2
C BM = =
C 
ln  B1 
 CB2 

 AC BM
D AB = =
2M A SC ACT

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For T =

P
CT = =
RT

(VP) A
CA =  CT =
P

From graph, S =

C B1 = CT =

P − (VP) A
CB2 =  C B1 =
P

C B1 − C B 2
C BM = =
C 
ln  B1 
 CB2 

 AC BM
D AB = =
2M A SC ACT

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RESULTS:

The effect of temperature on diffusion coefficient has been studied. The values of
diffusion coefficient at different temperatures are:

DAB at T = ____________ = ________________________ m2/s

DAB at T = ____________ = ________________________ m2/s

DISCUSSIONS:

SAFETY PRECAUTIONS:

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Experiment No.: Date:

SIMPLE DISTILLATION
OBJECTIVE
To verify Rayleigh’s equation for simple distillation of methanol-water mixture.
To verify material balance equation, FxF = DyD,avg + WxW

APPARATUS

1. Simple distillation apparatus.

2. Density bottle
3. Measuring cylinder (10 mL)
4. Burette (2 No.s)
5. Conical flask (100 mL)

CHEMICALS
1. 50 mole% methanol-water mixture.

2. Pure methanol
THEORY

Distillation is a method of separating the components of a solution. This makes use of

the fact that when part of a liquid mixture is vaporized by addition of heat, the
composition of the new phase may be different from the composition of the original
solution. Let us consider the addition of heat at constant pressure to a completely
miscible liquid mixture A and B. The temperature of the mixture rises. If it had been pure
A, the vapour pressure of A rises with increases in temperature and finally equals the
pressure at which the operation is carried out. If further heat is added, this is utilized in
converting A from liquid to vapour state at a constant temperature. Similar is the case for
a component for liquid B also. In other words, we can say that a pure Component has
only one degree of freedom at the two-phase equilibrium condition. But when there are
two components, phase rule suggests two degrees of freedom for the same situation,
which means that there is a range temperature through which the transition from liquid to
vapour state occurs. The temperature at which vaporization starts is called ‘bubble point’
and the temperature at which the vaporization ends is called ‘dew point’.

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Figure 1: Simple Distillation experimental setup

OBSERVATIONS:

Specific Gravity Bottle + Bottle + Bottle +

Item
Bottle Feed Distillate Residue

Weight (g)

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In the figure, the mole fraction of more volatile component (here A) is used to denote the
compositions of the mixtures. Consider the mixture to be initially in the liquid phase
denoted by point G. On addition of heat, the temperature of the mixture rises. Let us
consider that two components, the state of the system have reached point H when the
vapour pressure of the solution equals the constant pressure exerted. The liquid mixtureis
at the point of vaporization, or the liquid mixture has reached its bubble point. When
more heat is added, the temperature further rises to point P. Now the system exists in two
phases; a liquid phase represented by point L and a vapour phase represented by point K.
The composition of the liquid phase suitably changed so that the vapour pressure of the
solution is equal to the pressure maintained. This is the property made use of in
distillation to effect a separation between A and B. On further addition of heatthe state of
the system reaches point M where the mixture gets completely vaporized. The system at
this state said to beat at its dew point. The bottom line is saturated liquidline and the top
curve is the saturated vapour curve. Vapour phase K and liquid phase L coexist and
hence they said to be in equilibrium. While the mole fraction of A in the liquid phase is
denoted by x, the mole fraction of A in the vapour phase in equilibrium which is denoted
by y*. If there is a separation by distillation, y* has to be different from x.

Differential or Simple distillation

With reference to the figure, let us consider that the state of the system has reached the
point H. A drop of vapour forms which has compositions represented by J. By some
method this vapour is removed from the vessel in which the equilibrium distillation is
carried out and is condense elsewhere. The composition of liquid phase moves up along
the saturated liquid line. Addition of more heat forms more vapour, but all vapour is
removed from the region of distillation immediately on the formation. The process of
distillation is stopped when the composition of the liquid phase has changed to the extent
required. In practice, this can only be approximated since,
• Removal of differential amounts if vapour makes the process infinitely slow.
• Entrainment cannot be fully avoided.
• There will be cooling and condensing of the vapour before removal from the
region of distillation.

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OBSERVATIONS
Volume of Volume Weight of mix Mixture Mole %
Mix
methanol of water + specific Density of
No
(ml) (ml) gravity bottle(g) (g/ml) Methanol

1 0 30 0.000

2 3 27

3 6 24

4 9 21

5 12 18

6 15 15

7 18 12

8 21 9

9 24 6

10 27 3

11 30 0 1.000

For S. No.: _____

VA  A
MA
xA = =
V A  A VB  B
+
MA MB

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The amount of liquid that is distilled can be related to the initial and final liquid phase
composition using an equation called Rayleigh’s equation. For a binary mixture of A and
B assume that at any time during the course of distillation there are L moles of liquid in
the still of composition x mole fraction of A and the amount of distillate ( =dL) of mole
fraction y* in equilibrium with the liquid, is formed. Let us denote the corresponding
change in the liquid phase composition by dx.
Let us determine the corresponding material balance for A

Lx = y * L + ( L − dL)( x − dx)

Expanding and neglecting dxdL, we get y * dL = Ldx + xdL

x
F
F
dL dx
= ln   =  *
L  W  xW y − x

where F and W are the total number of moles of liquid at any instant during distillation
having composition xF and xW respectively. This equation can be used to determine F, W,
xF, and xW for simple distillation when any three of these are known.
PROCEDURE
1. Add 300 ml of given methanol-water mixture in a simple distillation flask after
exactly measuring the volume using a measuring cylinder. Assemble the distillation
apparatus, start circulation of water through condenser and switch on the heating.
2. Take distilled water in one burette and methanol in another. Determine the specific
gravity of pure methanol. Clean and dry a 100 mL conical flask. Prepare a 10 % by
volume mixture of methanol and water in this by mixing 3 mL methanol with 27 mL
water and find out the specific gravity of this mixture.
3. Similarly, find the specific gravity values of several known compositions of
methanol-water mixtures. It is better to do the experiment in increasing percentages
of methanol and to shake the dry bottle between successive densitydeterminations so
that little amount of solution remain in the bottle and will not affect much.
4. When required amount of distillate (50 % of feed volume) has been collected, stop
heating and disassemble the apparatus. Measure the volume of distillate collected in
that of residue remaining using a measuring cylinder. Determine the specific gravity
of this solution also

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CALCULATIONS:
Volume of Methanol-Water mixture as feed =
Volume of distillate collected =
Volume of residue after distillation =
Molecular wt. of methanol =
Molecular wt. of water =
Density of water =( - )/25 = ____________ g/mL
Density of methanol =( - )/25 = ____________ g/mL
Density of feed mixture =( - )/25 = ____________ g/mL
Density of distillate =( - )/25 = ____________ g/mL
Density of residue =( - )/25 = ____________ g/mL

The equilibrium relation between Methanol (A) – Water (B) system at 1 atm :
𝟏
xA yA*
𝒚∗ −𝒙
0 0 -
0.02 0.1 12.5
0.04 0.2 6.25
0.06 0.3 4.17
0.09 0.4 3.23
0.14 0.5 2.78
0.22 0.6 2.61
0.3 0.66 2.78
0.4 0.73 3.03
0.5 0.78 3.57
0.6 0.82 4.54
0.7 0.87 5.88
0.8 0.92 8.33
0.9 0.96 16.67
1.0 1.0 -

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GRAPHS:

Plot the mixture density in y and methanol mole fraction in x-axis. Find xW, xF and yD,avg.

Plot 1/(y*-x) in y-axis and methanol mole fraction in x-axis. Find area under curve

between xW and xF.

From graph:

Mole fraction of methanol in the distillate, yD,avg =

Mole fraction of methanol in feed, xF, =

Mole fraction of methanol in residue, xW, =

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For feed, F

From graph, xF =

xF × Molecular weight of methanol

Mass fraction of methanol in feed =
xF × MWmethanol + (1 − xF ) × MWwater

Mass of feed, F = Volume of feed × Density of feed

mass of feed × mass fraction of methanol in feed

Moles of methanol in feed = Molecular weight of methanol

Mass fraction of water in feed = 1 – mass fraction of methanol in feed

mass of feed ×mass fraction of water in feed

Moles of water in feed =
molecular weight of water

Total moles in feed = moles of methanol in feed + moles of water in feed

= =

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For Distillate, D

From graph, xD = yD,avg =

yD,avg ×Molecular Weight of methanol
mass fraction of methanol in Distillate =
yD,avg ×MWmethanol +(1−yD,avg )×MWwater

Mass of Distillate = volume of distillate × Density of distillate

mass of distillate×mass fraction of methanol in Distillate

Moles of methanol in Distillate= =
molecular weight of methanol

Mass fraction of water in Distillate = 1 - mass fraction of methanol in Distillate

= =

mass of distillate×mass fraction of water in distillate

Moles of water in Distillate =
molecular weight of water

Total moles in Distillate, D = moles of methanol + moles of water in Distillate

= =

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For Residue, W

From graph, xw =
xw ×Molecular Weight of methanol
mass fraction of methanol in Residue =
xw ×MW of methanol+(1−xw )×MW of water

Mass of residue = volume of residue × density of residue

mass of residue×mass fraction of methanol in residue

Moles of methanol in Residue =
molecular weight of methanol

Mass fraction of water in Residue = 1 - mass fraction of methanol in Residue

mass of residue×mass fraction of water in residue

Moles of water in Residue =
molecular weight of water

Total moles in Residue, W = moles of methanol + moles of water in Residue

= =

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Material Balance:

F=D+W and FxF = DyD,avg + Wxw

Total moles in feed, F =

Total moles in distillate, D =

Total moles in residue, W =

LHS, F = ______________ moles and RHS, D + W = ______________ moles

Mole fraction of methanol in the distillate, y D,avg, =

Mole fraction of methanol in feed, xF, =

Mole fraction of methanol in residue, xW, =

Substituting the values in material balance we get,

LHS = F xF = = ______________ moles

RHS = D yD,avg + W xW = = ______________ moles

xF dx
The area under the curve between xF and xW gives the value of ∫x
W y∗ −x

From graph, area under the curve =

F
ln ( ) = =
W

Hence, the Rayleigh’s equation and material balance for the system has been verified.

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RESULTS:

The Rayleigh’s equation and material balances for the given methanol - water system

has been verified with errors present within allowable limits. The error in material

balance is about __________ %

DISCUSSION:

SAFETY PRECAUTIONS:

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Experiment No.: 6 Date: 5th March

2025

ADSORPTION ISOTHERM
OBJECTIVE
To verify the applicability of the Freundlich equation for adsorption of acetic acid on
activated carbon and to determine the value of constants k and n in the equation for
adsorption at room temperature.

APPARATUS
Reagent bottles, conical flasks, filtering funnel, burette, pipette, and volumetric flask

CHEMICALS REQUIRED
Acetic acid, activated carbon, 0.1N NaOH solution, Oxalic acid

THEORY
Adsorption isotherm exploits the ability of certain solids preferentially to concentrate
specific substances from solution to their surfaces. In this, components of either liquid or
gaseous solution may be separated from each other. Some applications of adsorption in
gaseous separations are de-humidification of air and other gases, removal of
objectionable odors of impurities from industrial gases, recovery of valuable solvent
vapours from dilute mixtures with air and other gases and fractionation of mixtures of
hydrocarbon gases containing such substances like methane, ethane, and propylene.
Typical liquid separation is the removal of moisture dissolved in gasoline,
decolourisation of petroleum products and aqueous sugar solution, removal of
objectionable taste and odour from water and fractionation of a mixture of aromatics and
paraffinic hydrocarbons.
Adsorption can be physical or chemical. Physical adsorption or Vander Waal’s
adsorption can be readily reserved and is the result of intermolecular forces of attraction
between solid and the substance adsorbed. The equilibrium partial pressure of the

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substance adsorbed equals that of contacting gas phase. This is lower than the vapour
pressure and so adsorption is not simple condensation. By lowering the pressure of gas
phase by raising the temperature, the adsorbate is readily removed or desorbed in
unchanged form, reversible adsorption is seen in liquids as well.

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OBSERVATIONS:
Room Temperature = 25 oC

Weight of acetic acid taken in 250 mL flask (F1) = 25 g

Normality of Oxalic Acid N1 = 0.1 N

Standardization of NaOH

Indicator: Phenolphthalein

Colour Change: Colourless to Pink Colour

Titre value of NaOH (ml) V1

S No. Volume of Oxalic Acid
Titre 1 Titre 2
(ml) V2
1 10 12.1 12.1

Average V1 = 12.1 ml

Preparation of mixtures

Bottle V12 Volume transferred V2B Volume from flask F2 m, Weight of

No. from F1 to F2 (mL) transferred to bottle (mL) Carbon added (g)
1 10 200 5

2 20 200 5

3 30 200 5

4 40 200 5

5 50 200 5

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Chemisorption or activated adsorption is the result of chemical interaction between the

solid and the adsorbed substance. The process is frequently irreversible and on
adsorption, the original substance will be found to have undergone a chemical change.
Chemisorption finds applications in catalysis. The usual adsorbents are fuller’s earth,
activated clays, bauxite, alumina, bone charcoal, decolourising carbon, gas adsorbent
carbon, silica gel,zeolites and metal alumino-silicates.
Adsorption equilibria
The amount of substance adsorbed depends on the concentration of the contacting gas or
liquid phase, the temperature, and pressure. A relationship between these variables is
called “adsorption equilibria”. Data on equilibria are essential for designing adsorption
unit. Equilibrium data plotted for a given temperature is called “adsorption isotherm”.

Figure Adsorption Equilibria

In liquid adsorption, isotherms are important since no appreciable volume changes of the
liquid occur which might be used as a measure of adsorption. Withdrawal of the solid
and weighing it, as can be done in the case of gases, will not distinguish between the
adsorbed liquid and that which is mechanically occluded. When adsorbent is mixed with
a binary solution, adsorption in both solute and solvent occurs.Since the total adsorption
cannot be measured, the relative or apparent adsorption can be determined instead. The
customary procedure is to treat a known volume of solution with a known weight of the
adsorbent. V cm3 of solution/g of adsorbent. As a result of preferential adsorption of
solute, the solute concentration of the solution is observed to fall from initial C0 to final
Ce in the liquid (C-concentration in g of solute per cm3 of solution).

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Titration of the filtered solution

Indicator: Phenolphthalein

Colour Change: Pink to Colourless

V3 Volume of V5 Volume Titre value of Acetic Acid

Bottle filtrate taken for V4 Makeup of NaOH V6 (mL)
No dilution (mL) Volume (mL) taken (mL) Titre 1 Titre 2
1 10 190 10 18.1 18.0

2 20 180 10 9 8.8

3 30 170 10 5.1 5.3

4 40 160 10 4.3 4.1

5 50 150 10 3.2 3.2

CALCULATIONS

Normality of given NaOH solution (N2) = V1 × N1 / V2 = 10*0.1/12.1

= 0.0825 N

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The apparent adsorption of solute, neglecting any adsorption of solvent is qe =

V(C0-Ce)/m g of solute adsorbed per gram of adsorbent. This is satisfactory for dilute

solutions where the fraction of the original solvent, which may be adsorbed, is small. For
dilute solutions, the adsorption isotherm may be described by an empirical expression,

V (C0 − Ce )
qe = = KCe1 / n
m
1
In linear form of Freundlich isotherm, can be written as ln qe = ln k + (n) ln Cewhere

k and n are constants at a particular temperature. It is to be noted that ‘n’ is

independent of units used and ‘ k ’ has units same as that used for C0 or Ce. Sometimes
this curve may show deviation from linearity. This may be due to appreciable
adsorption of the solvent or simply the general inapplicability of Freundlich isotherm.

PROCEDURE
1. Record the room temperature.

2. Weigh about 25 g of Acetic acid exactly in weighing bottle and transfer it

completely by repeated washings to a 250 ml volumetric flask (F 1) and make
up the volume with distilled water.
3. Pipette out 10 ml of this solution into another 250 ml volumetric flask (F2) and
the volume is made up.

4. Weigh about 5 g of activated carbon into reagent bottle (B 1) by differential

weighing.
5. Add 200 ml of solution from the flask (F2) to this bottle.

6. Repeat the same procedure with bottle numbers B2, B3, B4, B5 with the
difference that the volumes of solution pipette out from the flask F1 are 20 ml,
30 ml, 40 ml and 50 ml respectively.

7. Shake the bottles well for one hour using bottle shaker for adsorption to come
into equilibrium.
8. Prepare a standard solution of Oxalic acid (0.1 N) and use this to standardize
the supplied NaOH solution.
9. After 1 h shaking, filter the solution and titrate in the five bottles. Take the
solutions in the burette and titrate it against 10 ml NaOH.
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For Bottle No.: 1

Final equilibrium concentration attained,

NNaOH × V5 × Equivalent weight of acetic acid
Ce =
V6 × 1000
=0.0825*60.05*10/(18.05*1000)

= 0.002744 g/ml

Initial concentration of acetic acid taken in bottle,

weight of acetic acid taken (g) × V12 (mL)
C0 =
V𝐹1 (mL) × V𝐹2 (mL)
= 25*10/(250*250)

= 0.004 g/ml
V2B (C0 − Ce )
qe =
m
=200(0.004-.002744)/5

= 0.05024

ln Ce = ln(0.002744)

= -5.8983

ln qe = ln(0.05024)

= -2.9909

C0 Ce
3
Bottle V/m (cm of (g solute/ (g solute/
solution/ g qe ln Ce ln qe
No ml of ml of
adsorbent) solution) solution)
1 50 0.004 0.002744 0.05024 -5.8983 -2.9909

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2 50 0.008 0.005566 0.09736 -5.1910 -2.3293

3 50 0.012 0.009527 0.09892 -4.6536 -2.3134

4 50 0.016 0.011795 0.16821 -4.4400 -1.7826

5 50 0.020 0.015481 0.18071 -4.1681 -1.7109

GRAPH:

Plot ln qe in y-axis and ln Ce in x-axis

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CALCULATIONS:

From graph,

Slope = 1/n = 0.58620

Thus, n = 1.70588

Intercept = ln k = -0.85

Thus, k = 0.4274

Thus, Freundlich isotherm is qe = k Ce1/n i.e. qe = (0.4274) *Ce (0.5862)

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RESULTS:

The applicability of Freundlich isotherm for adsorption of acetic acid on activated

charcoal has been verified at room temperature and the Freundlich constant values are
found as

n = 1.70588

k = 0.4274

Thus, isotherm equation is: qe = (0.4274) *Ce (0.5862)

DISCUSSION:

The experiment aims to determine the relationship between the concentration of solute

in the liquid phase and amount absorbed into a solid at equilibrium. Data obtained is

fitted to Freundlich isotherm and has been verified within experimental accuracy.

SAFETY PRECAUTIONS:

1. Alway wear lab coat, safety goggles, and gloves to protect against chemical

spills and splashes.

2. Conduct experiment in a well-ventilated area, especially when working with

volatile hazardous chemicals.

3. Review the MSDS Sheet for Acetic acid and use appropriate PPF such as gloves

to prevent skin and eye irritation. In case contact with skin, immediately flush

the affected area under water for 15 mins

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Experiment No.: Date:

FORCED DRAFT TRAY DRYER

OBJECTIVE
To study the drying characteristics of a solid under forced draft condition.
AIM
To determine the drying rate of a solid under forced draft condition and determine the
critical moisture content.
INTRODUCTION
In many cases, drying of materials is the final operation in the manufacturing process,
carried out immediately prior to packaging or dispatch. Drying refers to the final
removal of water, and the operation often follows evaporation, filtration or
crystallization. Drying is carried out for one or more of the following reason:
1. To reduce the cost of transport.
2. To make a material more suitable for handling.
3. To provide definite properties.
4. To remove moisture this may otherwise lead to corrosion.
THEORY
Drying of solids is considered to occur in two stages, a constant rate period followed
by a falling rate period. In the constant rate period, the rate of drying corresponds to
the removal of water from the surface of the solid. The falling rate period corresponds
to the removal of water from the interior of the solid. The rate, in either case, is
dependent on:
- Flow Rate of Air.
- The Solid Characteristics.
- Tray Material.

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The rate of drying can be determined for a sample of a substance by suspending it over
an electronic balance in the duct. The weight of the drying sample can then be
measured as a function of time.

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NOMENCLATURE:
A = Drying surface area, m2
a0 = Area of orifice, m2
ap = Area of pipe, m2
D = Diameter, m
do = Diameter of orifice, m
dp = Diameter of pipe, m
G = Mass flow rate of air, kg/s
h = Head loss, m
N = Drying rate, kg/m2s
Nc = Constant drying rate, kg/m2s
W = Weight of moist solid, kg
R = Manometric difference, m
S = Weight of dry solid, kg
X = Moisture content of a solid, kg water / kg of dry solid
Xc = Critical moisture content, kg water / kg of dry solid
θ = Time, s
ρa = Density of air, kg/m3
ρw = Density of water, kg/m3

Let the weight of dry solid =S

Let the weight of dry solid + moisture = W
Then, kg of water/kg of dry solid =X
X = (W – S)/S
Drying Rate N (kg/s m2)
S X
N= −
A 
A = exposed surface area for drying, m²

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DESCRIPTION
The set up consists of an insulated double wall chamber. Inside the chamber, a tray is
attached directly to an electronic weighing balance, which is fitted on bottom outside
the chamber. Material for drying is placed in the tray and regular loss of weight is
monitored. Air from a blower passes through a heating chamber is used as a drying
agent. Flow control and bypass valve are fitted to regulate the airflow.
UTILITIES REQUIRED
1. Electricity Supply: Single Phase, 220V AC, 50 Hz, 5-15 amp. socket with earth
connection.
2. Bench Area Required: 0.75 m x 2 m.
3. Wet Solid.
EXPERIMENTAL PROCEDURE
1. Record the weight of tray alone. Then dry sand and tray.
2. Place the tray with solid inside the drying chamber.
3. Start the blower and fix the air flow rate and also its inlet temperature by adjusting
the energy regulator.
4. When the desired conditions of temperature and air velocity are reached (in about
10-15 min), weight the sample tray again and put known amount of water (6-8 mL) in
it to give desired initial moisture content.
5. Keep the tray gently in the drying chamber and start the stopwatch
6. Record the balance reading at every 3 minute interval for about 40 minutes.
7. Drying is assumed to be complete when at least 3 consecutive readings are
unchanged. The wet/dry bulb temperatures at the inlet and outlet of the drying chamber
and the air flow rate (manometer reading fixed across the orifice) are recorded at least
three times during the course of a run to give average operating conditions.
8. The same steps are repeated for other runs at different operating conditions like air
flow rate.

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Figure 1: Drying rate curve

OBSERVATIONS:

do =

dp =

d =

S =

Cd =

TDry,in =

TDry,out =

TWet,out =

ρw (at T = ________) =

ρa (at T = ________) =

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TABLE:
R = _____ cm
No. θ, s W, g X ΔX Δθ, s N, kg/m2s
1

10

11

12

13

14

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R = _____ cm
No. θ, s W, g X ΔX Δθ, s N, kg/m2s
1

10

11

12

13

14

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GRAPHS:

Plot the drying rate N (kg/m2s) vs moisture content X (kg of water/kg of dry solid) i.e.

drying rate curve. Mark the critical moisture content, Xc where drying rate starts to fall

CALCULATIONS:

ao = πdo2/4 =

ap = πdp2/4 =

A = πd2/4 =

 
H = R w − 1 =
 a 
C d  ao  a p   a  2 gH
G= =
a 2p − ao2

SAMPLE CALCULATION FOR θ = ________ min and R = ________ cm

W −S
X = =
S

S X
N =− =
A 

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RESULTS:

The drying rate curve has been plotted where the different regions of constant drying
region, varying drying regions, critical moisture content and equilibrium moisture
content have been marked.
The critical moisture content is ___________________ at _____________________

The critical moisture content is ___________________ at _____________________

DISCUSSION:

SAFETY PRECAUTIONS:

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Experiment No.: 8 Date: 17th March

2025

TERNARY LIQUID EQUILIBRIUM

OBJECTIVE
To draw the binodal solubility curve for the system Benzene (A) – Water (B) – Glacial
acetic acid (C) at room temperature and pressure.
APPARATUS
1. 50 cc burette (3 nos.)
2. 50 cc test tube (10 nos.)
3. specific gravity bottle
CHEMICALS
1. Glacial acetic acid
2. Distilled water
3. Benzene
THEORY
Consider the liquid extraction operation, where we are interested in separating acetic
acid from a mixture of acetic in water. The liquid is agitated with a liquid such as ethyl
acetate. Some of the acid but relatively less amount of water will enter the liquid phase.
So, the difference immiscibility of acetic acid and water in ethyl acetate and water is
taken advantage of in separating the mixture.
In all such operations, we see that
There are at least three substances and two-phases involved.
The two liquid phases finally reach equilibrium when they are kept in contact with
each other, for which sufficient length of time. Study the composition of two phases
which are in equilibrium with each other and each of which involves three components
called ternary liquid equilibrium.
All possible composition of three substances involved can be divided into two groups:
Compositions in which the ternary system exists as a single phase (three liquids
are completely miscible)
Compositions in which the system exists in two phases.

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Figure1: Ternary liquid equilibrium data represented on equilateral triangular

coordinates

(a) (b)
Figure 2: (a) Type I system and (b) Type II system

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Hence in liquid extraction design, it is important to determine the compositions at

which the system changes from a completely miscible into a two-phase system. If all
compositions of the ternary liquid system can be represented on a graph paper, the
boundary between miscible and immiscible regions can be represented by a curve. This
curve is called a binodal curve.
At a given condition of temperature and pressure, the composition of one phase
automatically fixes the composition of another phase in equilibrium with it. Lines
joining points representing compositions of the two phases in equilibrium are called tie
lines which must be determined experimentally. However, this is out of scope for the
present experiment.
Graphical representation on equilateral triangular coordinates
Suppose the components are denoted using letters A, B, and C. The same letter will be
used to indicate the quantity of a solution or mixture on a phase diagram. The
concentration of ternary liquid system can be plotted on equilateral triangle coordinates.
It is the property of an equilateral triangle that sum of perpendicular distances from
any point within the triangle to three sides equals the altitude of the triangle. We may,
therefore, let the altitude represent 100% composition and distance to the three sides
the percents or fractions of the three components. With reference to Figure 1, each
apex of the triangle represents one of the pure components as marked. The
perpendicular distance from any point such as K to the base AB represents the
percentage of C in the mixture at K, the distance to the base CB, the percentage of A.
The following are some of the properties of this graphical representation. If R g of
a mixture at point R is added to the E g of a mixture at E, the new mixture can be
represented by the point M which lies on the straight line RE, such that

R lineME x E − x M
= = (1)
E lineRM xM − x R

where xE, xM, and xR represent the compositions of any one component in mixture E,
M, and R respectively. Similarly, if a mixture at M has been removed from it a mixture
of composition E, the new mixture is on the straight-line EM extended in the direction
away from E and the location of this at R is given by Equation 1.
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OBSERVATIONS:
No. Benzene Acetic Water No. Benzene Acetic Water
(ml) Acid (ml) (ml) (ml) Acid (ml) (ml)
1 6.6 9 1 10 1 9 0.1

2 3.6 8 2 11 2 8 0.2

3 1.7 7 3 12 3 7 0.3

4 1.4 6 4 13 4 6 0.4

5 1.2 5 5 14 5 5 0.6

6 0.9 4 6 15 6 4 0.9

7 0.6 3 7 16 7 3 1.5

8 0.4 2 8 17 8 2 2.6

9 0.3 1 9 18 9 1 6.1

Weight of specific gravity bottle = 17.16g

Weight of specific gravity bottle + water = 42.55g

Weight of specific gravity bottle + acetic acid = 43.74g

Weight of specific gravity bottle + benzene = 39.15 g

CALCULATION:

Density of water = (42.55-17.16) g/25 g/mL

= 1.0156 g/mL

Density of acetic acid = (39.15-17.16) g/25 g/mL

= 1.0632 g/mL

Density of benzene = (43.74-17.16) g/25 g/mL

= 0.8796 g/mL

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Different types of ternary liquid systems:

1. Two pairs completely soluble –one pair partially soluble;
Example 1: Water (A)-Chloroform (B)-Acetone (C)
Example 2: Benzene (A)-Water (B)-Acetic acid (C)
Liquid C dissolves completely in A and B, but A and B dissolve only to a limited
extent in each other. At a particular temperature and pressure, as shown in Figure 2a. L
and K represent a saturated liquid mixture of A and B. Curve LRPEK is the binodal
solubility curve. Any mixture outside the curve will be a homogeneous solution of one
liquid phase. A ternary mixture underneath the curve, such as M, will form two
insoluble saturated liquid phases of equilibrium compositions indicated by R (A-rich)
and E (B-rich). The line joining these equilibrium compositions is called a tie line. And
the plot at which the tie line ends is called plait point.
2. One pair completely soluble - 2 pairs partially soluble.
Example: Chlorobenzene (A)-Water (B)-Methyl Ethyl Ketone (C)
A and C are completely soluble while pairs A-B and B-C compositions may show
limited solubility. With reference to figure 4.3, mixtures such as mixture M are inside
the heterogeneous area and exist as two phases, the compositions of which are given
by points R and E. Line RE is a tie line. Curves KRH and IHEL are ternary solubility
curves and the mixtures outside the band between these curves form homogeneous
single-phase liquid solutions.

PROCEDURE

1. Report the temperature at which the binodal solubility curve is drawn.

2. Wash the test tubes with water, alcohol or acetone and perfectly dry it by blowing
hot air.
3. Clean the burettes. Distilled water is taken in burette 1, benzene in burette 2 and
glacial acetic acid in burette 3.
4. Prepare 9 mixtures of varying compositions in h test tubes by mixing 1 cc of water
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National Institute of Technology Calicut Department of Chemical Engineering

with 9 cc of acetic acid, 2 cc of water with 8 cc of acid and so on.

5. To each mixture add benzene from the bottle drop by drop till turbidity appears
which indicates light traces of separation of a new phase.

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National Institute of Technology Calicut Department of Chemical Engineering

TABLE:
No. Weight Fraction No. Weight Fraction

Benzene Acetic Acid Water Benzene Acetic Acid Water

1 0.3542 0.5838 0.0619 1 0.0528 0.5749 0.3722

2 0.2310 0.6206 0.1482 2 0.1363 0.6590 0.2046

3 0.1247 0.6210 0.2542 3 0.2273 0.6413 0.1312

4 0.1054 0.5464 0.3480 4 0.3254 0.5900 0.0845

5 0.0921 0.4642 0.4435 5 0.4260 0.5149 0.0590

6 0.0710 0.3818 0.5470 6 0.5311 0.4279 0.0408
7 0.0648 0.2946 0.6566 7 0.6379 0.3304 0.0315

8 0.0331 0.2005 0.7662 8 0.7512 0.2270 0.0216

9 0.0252 0.1015 0.8732 9 0.8717 0.1170 0.0111

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6. Note down the volume of benzene added to the mixture

7. Wash the test tubes with water and some volatile liquid like alcohol or acetone and
dry it by blowing hot air.
8. Prepare 9 mixtures of varying compositions by taking 1 mL benzene and 9 mL
acetic acid, 2ml benzene and acetic acid taken in each is now taken down.
9. Add water drop by drop till turbidity appears.
10. To determine points L and K with reference to figure take 10 mL of benzene in a
clean dry test tube and find out the volume of water needed to make this turbid and
take 10 cc of water in a clean dry test tube and find out the volume of benzene needed
to make this turbid.
11. Find specific gravity of benzene, water and acetic acid using specific gravity bottle.

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National Institute of Technology Calicut Department of Chemical Engineering

Sample Calculations:
For Mixture 1 ( S.No. : 9):

Weight Fraction of Benzene = 0.3*0.8796/ (0.3*0.8796 + 1*1.0632 + 9*1.0561)

= 0.0252

Weight Fraction of Acetic Acid = 1*1.0632/ (0.3*0.8796 + 1*1.0632 + 9*1.0561)

= 0.1015

Weight Fraction of Water = 9*1.0561/ (0.3*0.8796 + 1*1.0632 + 9*1.0561)

= 0.8732

GRAPH:
Plot the weight fractions on a ternary graph with different markers for 1-9 and 10-18.

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National Institute of Technology Calicut Department of Chemical Engineering

CH2092E Heat and Mass Transfer Laboratory Page No.

National Institute of Technology Calicut Department of Chemical Engineering

RESULTS:

The binodal solubility curve for benzene - water - glacial acetic acid system has been
drawn at room temperature and pressure. From the shape of the binodal curve, we
observe that the system is of Type I, where 2 components are only partially miscible,
and 3rd is miscible with both. The binodal solubility curve exhibits a teardrop shape,
with the immiscibility region lying inside the curve.

DISCUSSION:

1. The experiment identified the immiscibility region, plotted the binodal curve,

and determined tie lines connecting coexisting phases

2. Temperature changes, measurement errors, and incomplete phase separation is

influencing the accuracy of equilibrium data.

3. This experiment is essential for liquid-liquid extraction, solvent selection, and

chemical separation processes in industries like pharmaceuticals and

petrochemicals.

SAFETY PRECAUTIONS:

1. Wear gloves, goggles, and lab coats to prevent exposure to toxic or corrosive
solvents. Work in a well-ventilated area or fume hood.

2. Symbols on Benzene and Acetic Acid bottles indicate that both are flammable,
and they are toxic and cause skin irritation respectively.

3. Handle pipettes, burettes, and separators carefully to avoid breakage. Dispose of

chemical waste properly.

4. Keep flammable solvents away from heat sources. Use spill trays and have a fire
extinguisher ready.

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