INTRODUCTION GENERALE...........................................................................................................................

4
MANIPULATION N°1 : EVAPORATION........................................................................................................... 5
INTRODUCTION........................................................................................................................................ 6
MANIPULATION N°2 : LE SECHAGE............................................................................................................... 6
AIM:.......................................................................................................................................................... 6
INTRODUCTION:....................................................................................................................................... 6
DESCRIPTION:........................................................................................................................................... 6
THEORY:................................................................................................................................................... 7
EXPERIMENTAL PROCEDURE:................................................................................................................... 7
MANIPULATION N°3 ASTM DISTILLATION..................................................................................................... 8
INTRODUCTION........................................................................................................................................ 8
Working Principle:.................................................................................................................................... 9
EXPERIMENTAL PROCEDURE:................................................................................................................... 9
Apparatus Used:....................................................................................................................................... 9
MANIPULATION N°4: FLOW THROUGH PIPE............................................................................................... 17
Aim of the Experiment:........................................................................................................................... 17
Calculations :.......................................................................................................................................... 18
Reference............................................................................................................................................... 19
MANIPULATIUS N°5: DETERMINATION OF VISCOSITY OF ORGANIC SOLVENT............................................20
Objective:............................................................................................................................................... 20
Theory:................................................................................................................................................... 20
Temperature Dependence of Viscosity............................................................................................ 21
Determination of unknown composition................................................................................................ 22
Materials Required:................................................................................................................................ 22
Reagents:................................................................................................................................................ 22
Procedure:.............................................................................................................................................. 23
Observations and Calculations:............................................................................................................... 23
Results:................................................................................................................................................... 24
Points to Remember while Performing the Experiment in a Real Laboratory:........................................24
References:............................................................................................................................................. 24
Books:..................................................................................................................................................... 24
Webliography:........................................................................................................................................ 24
Image Source:......................................................................................................................................... 24
MANIPULATION N°6 GAS ANDLIQUID ABSORPTION...................................................................................25
AIM......................................................................................................................................................... 25
THEORY................................................................................................................................................... 25
Constant Parameters.............................................................................................................................. 28
 Books:..................................................................................................................................................... 29
MANIPULATION N°7 HEAT TRANSFER CONDUCTION AMRITA....................................................................29
Aim:........................................................................................................................................................ 29
Apparatus:.............................................................................................................................................. 29
Theory:................................................................................................................................................... 30
Applications:........................................................................................................................................... 31
Performing Simulation:........................................................................................................................... 31
Simulator Controls.................................................................................................................................. 32
Procedure for Simulation........................................................................................................................ 32
Procedure for Real lab............................................................................................................................ 33
Observations and Calculations................................................................................................................ 33
Result:.................................................................................................................................................... 34
References:............................................................................................................................................. 34
Books:..................................................................................................................................................... 34
Webliography:........................................................................................................................................ 34
MANIPULATION N°8 HEAT TRANSFER RADIATION AMRITA........................................................................34
Aim:........................................................................................................................................................ 34
Apparatus:.............................................................................................................................................. 34
Theory:................................................................................................................................................... 35
Relationship between Absorptivity and Emissivity:................................................................................. 36
Working.................................................................................................................................................. 37
Applications............................................................................................................................................ 37
Procedure:................................................................................................................................................. 37
Variable Region:................................................................................................................................... 37
Measurement Region:.......................................................................................................................... 37
Procedure for Simulation........................................................................................................................ 38
Procedure for Real lab............................................................................................................................ 38
Observations and Calculations:............................................................................................................... 38
Result..................................................................................................................................................... 39
References:............................................................................................................................................. 39
Books:..................................................................................................................................................... 39
Webliography:........................................................................................................................................ 39
MANIPULATION N°9 BATCH REACTORS...................................................................................................... 40
CONCLUSION.............................................................................................................................................. 40
INTRODUCTION GENERALE

Le raffinage de par sa définition consiste à transformer et à traiter le pétrole brut en

produits à hauts valeurs ajoutés. Pour ce faire, l’ingénieur fait appelle à plusieurs techniques.
Ces dernières sont basées sur les phénomènes de transferts de chaleurs et de matières, de
mécanique des fluides, de PVT …

Sous l’appellation Opération Unitaire. La problématique de la maîtrise par l’élève

ingénieur des opérations sus évoquées est à l’origine de cette unité d’enseignement
« opérations unitaires en laboratoire ». Nous traiterons entre autre la distillation ASTM, les
transferts de chaleurs par radiation et conduction, le génie de la réaction chimique…

MANIPULATION N°1 :

INTRODUCTION

MANIPULATION N°2 : LE SECHAGE

AIM:

To determine the drying characteristic for rotary dryer.

INTRODUCTION:

The rotary dryer is a type of industrial dryer employed to reduce or minimize the liquid
moisture content of the material by bringing it in direct contact with a heated gas. The dryer is
made up of large rotating cylinder which slopes slightly so that the discharged end is lower
than the material feed end in order to convey the material under gravity. Material to be dried
enters the dryer and as the dryer rotates, the material is lifted up by a series of internal fins
lining the inner wall of the dryer. When materials fall back to the bottom, it passes through the
hot gas stream. In the experiment, the gas stream moves towards the feed end from the
discharge end (counter current flow). Also the material passes through the length of the dryer
at nearly the wet - bulb temperature. Single pass and three pass rotary dryers are ideal for high
moisture, friable, free-flowing products. The Aeroglide Rotary dryer is the choice for high
throughput capacity applications involving high moisture, friable, free-flowing commodity
products and by-products. A rotating drum and strategically positioned flights combine to lift
and shower product evenly through the air stream. Thermostatically controlled discharge air
temperature assures precise final moistures and great sensitivity to varying product
conditions. Single-pass or three-pass configurations are available to match product
characteristics. Heating options include steam, gas, oil, thermal oil and auxiliary biomass
burner system.

DESCRIPTION:

A rotary dryer consists of a cylindrical shell, set with its axis at a right angle to the horizontal
and mounted on rollers so that it can be rotated. The material to be dried is fed to the high end
of the dryer and, by rotation of the dryer, usually assisted by internal shelves of flight

Is gradually advanced to the lower end where it is discharged. The source of heat for a rotary
dryer is usually the hot air that circulates through the dryer. The characteristic dimensions are:

Rotary dryer ID = D =110 mm = 0.11 m

Dryer length = 1500 mm = 1.5 m

Pre - heating of air using 1.5 KW heater (2 nos)

Air flow rate measurement by a pitot tube

Solid feed: By a screw conveyor

Inlet / Outlet air temperature by a hygrometer.

EXPERIMENTAL SETUP :
THEORY:
Consider a rotary continuous counter current dryer fed with a non - porous material
having all moisture as unbound moisture. As the material enters the dryer, it is first
heated to the drying temperature. It will then pass through the length of dryer at nearly the
wet – bulb temperature and theoretically at the end of the dryer, the material shall be
discharged as dry material nearly at the wet bulb temperature.

EXPERIMENTAL PROCEDURE:
1. Set the pre - heating temperature for air.
2. Fill the feed hopper with wet solid.
3. Measure the initial moisture content of the feed.
4. Start the dryer in rotary motion.
5. Allow the wet solid to flow through the dryer by starting the screw conveyor at the pre
fixed speed.
6. At steady state record the following:
a) Air flow rate (Orifice meter, manometer reading and convert it to volumetric flow rate and
mass flow rate) = GG
b) Air temperature at inlet = tG1
c) Air temperature at outlet = tG2
7. Repeat the above steps for at least 4 gas flow rates.
ASSUMPTIONS:
1. No heat loss from the dryer.
2. Heat is supplied only from the air, not by conduction from the dryer shell.
3. All the moisture present is free moisture.
4. There is no evaporation of moisture in the preliminary heating period.
5. Drying proceeds at a constant wet - bulb temperature until desired amount of water has
been removed.
MANIPULATION N°3 ASTM DISTILLATION
INTRODUCTION 

Distillation is the method of separating the components of a solution which depends upon the
distribution of the substances between a gas and a liquid phase. Distillation may be done in
two ways:

 1. Production of vapor by boiling the liquid mixture to be separated and condensing the vapor
without allowing any to return to the still, there is no reflux. 

2. Returning a part of condensate to the still under such conditions that this returning liquid is
brought into intimate contact with on their way to condenser. 

The distillation column consists of several trays, which allow the simultaneous travel of liquid
down the tray and vapor up the tray, allowing mixing of the two phases and therefore
equilibrium.  

The liquid mixture that is to be processed is known as the feed. The feed-tray divides the
column into a top (enriching or rectification) section and a bottom (stripping) section. 

The vapor moves up the column, and as it exits the top of the unit, it is cooled by a condenser.
The condensed liquid is stored in a holding vessel known as the reflux drum. Some of this
liquid is recycled back to the top of the column and this is called the reflux. 

The condensed liquid that is removed from the system is known as the top product or
distillate.

The aim of this experiment is determination of boiling range characteristics of petroleum

product by using ASTM distillation. ASTM Distillation is  a standard Test Method for
Distillation of Petroleum Products at Atmospheric Pressure.
       Working Principle: 

It is based on the principle of differential or simple distillation. A batch of liquid is charged

to a still fitted with some sort of heating device. The charge is boiled slowly and the vapors
are withdrawn as rapidly as they form to a condenser where they are liquefied and the
condensate is collected in the receiver.

EXPERIMENTAL PROCEDURE: 

1. The distillation flask is filled with 100 ml of sample. 

2. Water in the cooling bath is replaced and cleaned properly for effective cooling. Ice is
placed in the cooling bath for removal of heat produced.

3. The distillation flash and the receiving cylinder are fitted to the input and output of the
cooling bath by connecting pipe. Thermometer is inserted to distillation flask. 

4. To reduce evaporation loss due to leakage, the various joints in the arrangement (such as
distillation lfask - connection pipe and cooling bath output - receiving cylinder) are sealed
properly using some paper. 

5. After all arrangements are completed, heater is switched on and heat is supplied at constant
and standard rate for proper vaporization.

6. The temperature is noted when first drop of liquid condensed is received at the receiving
cylinder. After that temperature for each 5 ml rise in volume of distillate is noted.

7. Final boiling point temperature is noted when no further liquid is received at the cylinder,
though heat is supplied at the same rate. Then we stop heating and final volume is recorded.

8. The residue is cooled, and measured using a measuring cylinder. Thus subtracting from
total volume to volume distillate we get the loss.

Apparatus Used: 
1. Distillation Flask

2. Cooling Bath

3. Heater

4. Thermometer

5. Receiving cylinder to collect distillate.

The following data are obtained by performing the experiment

Initial boiling point of the product = 540C

Volume percent distilled     Temperature 0C

10 65
15 69
20 74
25 78.5
30 83.5
35 90
40 94.5
45 100
50 104.5
55 109
60 114
65 119.5
70 125.5
75 133
80 141.5
85 155
90 173
92 150

Final boiling point  of the product = 1730C

Volume distilled = 92 ml

Residue left = 2 ml

Evaporated = 6 ml

 A plot of volume percent distilled and temperature can be plotted as shown below:

Discussions:

1. The boiling range gives the information on the composition, the properties and the
behaviour of the fuel during storage and use. 

2. The distillation characteristics of hydrocarbons have an important effect on their safety and
performance.

3. Volatility is the major determinant of the tendency of a hydrocarbon mixture to produce

potentially explosive vapor.

Applicable literature:
A comparison between Indian gasoline specification for BS - IV and our experimental result
is given below:

  Our result BS - IV
IBP (0C) 54 38
FBP (0C) 173 210
Residue (ml) 2 2
Recovery up to  (700C) 10-15 10-45
Recovery up to  (1000C) 75 70

Finally, we can also convert out ASTM data obtained from the experiment into TBP data as
follows:

1. Firstly a probability chart is plotted on which all points connecting IBP, ASTM 10 %, and
ASTM 20 %…… ASTM end point shall lie on a straight line. In other words, knowing any
two ASTM temperatures at any two volume % values, the entire ASTM data for the product
can be
estimated.

Table1: ASTM‐TBP correlation data from Edmister method. 

Table2: End point correlation data. Data sets represent fractions whose cut point starts at 200
of TBP or lower (Set A); 300 of (Set B); 400 of (Set C); 500 of (Set D).
2. The ASTM temperatures of the product can be converted to the TBP using Edmister
correlation table 1 given in the next tab (Expt calc 2).

 3. It is assumed that the 50 % TBP of the crude matches with the 50 % TBP point of the
products. Eventually, the 50 % ASTM can be converted to obtain 50 % TBP point for the
products (other than the residue).
MANIPULATION N°4: FLOW THROUGH PIPE

Aim of the Experiment:

1. To determine the frictional losses encountered in a hydraulically smooth pipe under

gglaminar and turbulent flow situations.
2. To determine the effect of Reynolds number on Fanning friction factor for laminar and
turbulent flow situations in a hydraulically smooth pipe. Verify the correlations for
laminar flow and turbulent flow (Blasius correlation and Nicurdse’s correlation)

Apparatus required: CCL4,Hgmanometer.

Procedure:

1. Keep the valve leading to the smooth pipe open and valves leading to other lines
closed.
2. Keep the bypass valve completely open and the main valve completely closed. Switch
on the pump.
3. Connect a CCL4 manometer, to the pressure taps across the smooth pipe. Ensure that
no air bubbles present and height in both the limbs of manometer are the same.
4. Set a flow rate of water through the pipe by opening the main valve and throttling the
bypass valve suitably using the rotameter.
5. Note down the rotameter reading and manometer reading after a steady state is
attained.
6. Increase the flow rate of water by opening the main valve and throttling the bypass
valve suitably and repeat step 4 and 5.
7. Use mercury manometer for higher flow rates.
8. Take eight readings with CCL4 manometer as well as with Hg manometer.

Data:
Diameter of the pipe= D =        m
Length of the pipe= L =        m

Density of water = =        kg/m3

Viscosity of water = =cp=       kg/ms

3
Density of CCl4 = 1600 kg/m
Density of Hg = 13600 kg/m3
Observations:
Sl No. Rotameter Manometer Reading
Reading LPM
 ∆Hm cm

Calculations :

1. ∆Hm is cm of manometric fluid

2. Volumetric flow rate, Q = m3/s

3. Pressure drop in m of water

4. Cross sectional area of the pipe A =

5. Average velocity through the pipe = V=Q/A = m/s
6. Reynolds number = NRe = =

7. Friction factor f is calculated using f Blasius equation:

8. Friction factor

9. Nicurdse’s correlation:
 10.

Plot fexpt vs NRe on log-log graph. Compare them.

To verify Nicurdse’s correlation:

on a semi log graph

Find the slope and intercept.

Compare with Nicurdse ’s correlation.

Discuss on effect of Reynolds number on friction factor.

 Reference
  Additional Resources 1. Warren Lee McCabe, Julian Cleveland Smith, Peter Harriott ,Unit
operation of chemical engineering , 5th Edition,1993 2. Coulson and Richardson, Chemical
Engineering Volume I Pargamon Press 3rd edition.1977 3. Walter L. Badger and Julius T.
Banchero, Introduction to Chemical engineering.. Tata McGraw-Hill book Edition 1997,India
4.Perry's Chemical Engineers' Handbook (7th Edition) Edited by Perry, R.H.; Green, D.W. ©
1997 McGraw-Hill 5.A. S. Foust, Principles of Unit Operations, 2nd ed. John Wiley and
Sons, Inc., 1980 6.Industrial Instrumentation by Donald P Eckman, Wiley Eastern Publication
7.Lecture notes by M.Subramanian http://www.msubbu.in/ln/fm/
MANIPULATIUS N°5: DETERMINATION OF VISCOSITY OF
ORGANIC SOLVENT

Objective:
• Determine the absolute viscosity of organic liquids.

Theory: 

The internal property of a fluid for its resistance to flow is known as viscosity. In 1844
Hagen–Poiseuille did their work concerning the interpretation that liquid flow through tubes
and he proposed an equation for viscosity of liquids. This equation is called Poiseuille’s
equation.

   ---------- (1)
Where η is called the viscosity coefficient, t is the time of flow of liquid, V is the volume of
the liquid, P is the hydrostatic pressure, and L is the distance travelled by the liquid during
time t. In the honour of Hagen–Poiseuille the unit of viscosity is called the Poise (P). The
official SI unit for absolute viscosity is kg/m s (or Pascal-seconds, Pa s).
 
 Viscosity can be measured using a viscometer. The different types of viscometer are as
follows:

1. Ostwald viscometer
2. Falling sphere viscometer
3. Falling piston viscometer
4. Oscillating piston viscometer
5. Vibrational viscometers
6. Rotational viscometers
7. Bubble viscometer

Ostwald viscometer is a commonly used viscometer, which consists of a U-

shaped glass tube held vertically. For more accurate measurements it is held
in a controlled temperature bath. It is also known as a glass capillary
viscometer. A liquid is allowed to flow through its capillary tube between
two etched marks and the time of flow of the liquid is measured using a stopwatch.
In an Ostwald viscometer the measured distance the liquid travels, L, will be always a
constant; the radius, r will always be a constant; and by procedure the volume of liquid, V will
also be constant. Equation (1) can then be simplified to: 
     Ostwald viscometer
 
                     
--------- (2)  

Where K is a constant and 

  
 The hydrostatic pressure is P proportional to the density of the fluid being measured. In our
experiment we will be measuring the mass of equal volumes of liquid so that the viscosity
will be proportional to the masses measured. Therefore we have the relation:
 
--------- (3)
 
Where K and t are defined above and m is the mass of the liquid.
For finding the viscosity of liquids it is important to calibrate the viscometer using a reference
liquid. Water is a commonly used reference liquid. The viscosity of water at 30.0 °C is 0.8007
centipoise (cP). Knowing the values for the reference liquid and relation (3), we get:
 

---------- (4)
 
Where: ηr is viscosity coefficient of the reference sample (water), mr is the mass of the
reference sample, and tr is the time flow of the reference sample. Note that K cancels out. The
other variables are the viscosity coefficient, mass, and time flow of the sample respectively.
 
With an Ostwald viscometer we can measure the time flow of a liquid (mass can be measured
using standard laboratory procedures, e.g. a relative density bottle and a scale) and determine
its viscosity by solving equation (4) for η.

------------ (5)

Temperature Dependence of Viscosity

In 1889 Arrhenius expressed an equation for temperature dependent chemical reaction rates.
Since then, many temperature dependent chemical and physical processes have been found to
behave in accordance with Arrhenius-like equations. For the viscosity of many liquids, the
viscosity decreases as the temperature increases in accordance with the following equation:

------ (6)
 
Where A is a constant known as the Arrhenius constant, Eη is the activation energy for flow, R
is the ideal gas constant, and T is the temperature of the liquid using an absolute scale (almost
always K — the units of Eη and R and T should be chosen so that the ratio is dimensionless, A
will have the same dimensions as η, in our case cP). A plot of η vs. 1/T should be linear and
have a slope equal to Eη /R if the liquid’s viscosity exhibits Arrhenius-like behaviour.  
Determination of unknown composition

Using an Ostwald viscometer, we can also calculate the unknown composition of a mixture.
The viscosities of mixtures of different known compositions are measured and a graph is
plotted with viscosity against the compositions of the different mixtures. From the graph, the
composition of the unknown mixture corresponding to the viscosity can be determined.

Materials Required: 

1. Ostwald viscometer
2. Beaker
3. Wash bottle
4. Stop watch
5. Sucker
6. Pipette
7. Electronic balance
8. Hot Air gun 

Reagents:

1. Chromic acid
2. Acetone
3. Toluene
4. Nitrobenzene
5. Water 
Procédure:

To determine the coefficient of viscosity of organic liquids. 

1. Select the liquid from the list.

2. Click on the button "Fill the liquid".
3. Click "Start" button. (Note: DO NOT use "Start" button on the stopwatch)
4. Click "Stop" button on stopwatch when liquid reaches "label D". (Mark "Show Label"
for seeing the labels)
5. Note the flow time on the stopwatch.
6. Calculate the Viscosity coefficient of the liquid.

Liquid Mass (g) Density (g/cm3)

Water 25.06 1.002
Toluene 21.55 0.862
Nitrobenzene 30.01 1.200

Observations and Calculations:

Flow Time (sec)
Solvents
i Ii Mean
Water      
Toluene      
Nitrobenzene      

Room temperature = 30oC

Mass of water = 25.06 g

Mass of Toluene = 21.55 g

Mass of Nitrobenzene = 30.01 g

Time of flow of water=...........................sec

Time of flow of Toluene=......................sec

Time of flow of Nitrobenzene =............sec

Absolute viscosity of water,  = 0.8007 centipoise

Absolute viscosity of the Toluene, =........................centipoise

Absolute viscosity of the Nitrobenzene, =...............centipoise

Results: 

1. Absolute viscosity of the Toluene = .......................centipoise

2. Absolute viscosity of the Nitrobenzene =..............centipoise 

Points to Remember while Performing the Experiment in a Real Laboratory:

1. Always wear lab coat and gloves when you are in the lab. When you enter the lab,
switch on the exhaust fan and make sure that all the chemicals and reagents required
for the experiment are available. If they are not available, prepare the reagents using
the components for reagent preparation.
2. Make sure to clean all your working apparatus with chromic acid and distilled water
and ensure that all the apparatus are free from water droplets while performing the
experiment.
3. Make sure to calibrate the electronic weigh balance before taking the measurements.
4. Ensure that the stop watch and hot air gun are working properly.
5. Clean all glassware with soap and distilled water. Once the experiment is completed
recap the reagent bottles. Switch off the light, and exhaust fan before leaving the lab.
6. Discard the used gloves in a waste bin.

References: 
Books: 

1. Advanced practical physical chemistry Dr.  J.B Yadev

2. Practical chemistry O.P Pandey, D.N Bajpai,  S.Giri
3. Essentials of physical chemistry Arun Bahl, B.S Bahl, G.D Giri
4. A. Halpern and J. Reeves, Experimental Physical Chemistry, 1988, Scott and
Foresman.

Webliography:

1. www.ias.ac.in/initiat/sci_ed/resources/chemistry/Viscosity.pdf
2. en.wikipedia.org/wiki/Viscosity
3. physics.info/viscosity/

Image Source:

1. upload.wikimedia.org/wikipedia/commons/thumb/3/3e/Ubbelohde.jpg/100px-
Ubbelohde.jpg
MANIPULATION N°6 GAS ANDLIQUID ABSORPTION

AIM

The object of this experiment is to study gas liquid absorption in an absorption column:-

         1. The reaction of carbon dioxide when it is contacted with sodium

hydroxide solution.

         2. To compare the performance of a packed column (continuous

process) with a bubble column (semi-batch process).

         3. To observe the effect of different flow rates on the performance of

the two columns.

THEORY

This exercise deals with the mass transfer operation known as gas
absorption in which a soluble gas is absorbed from its mixture with an
inert gas by means of a liquid in which the solute gas is more or less
soluble.

A common apparatus used in gas absorption is packed tower, an example

of which is shown in figure (1). The device consists of a cylindrical column,
or tower, equipped with a gas inlet and distributing space at the bottom; a
liquid inlet and a distributor at top; gas and liquid outlets at the top and
bottom respectively; and a supported mass of inert solid shapes, called
tower packing
The inlet liquid which may be pure solvent or a dilute solution of some
solute (may or may not be same gas) in the solvent is distributed over the
top of the packing by distributor and, in ideal operation, uniformly wets
the surfaces of the packing. The solute containing gas enters the
distributing space below the packing and flows upward through the
interstices in the packing counter current to the flow of liquid. The packing
provides large area of contact between liquid and gas and encourages
intimate contact between phases. At ideal steady state condition, for a
specified flow rates of liquid and gas phase, the extent of absorption will
not changed with passage of time. In case of absorption in semi-batch
process as shown in figure (2), the extent of absorption increases with
passage of time as more and more gas is passed through the same liquid.

The absorption column in the experimental setup was packed with raschig
rings. They provide a large surface area within the volume of the column
for the interaction between liquid and gas and also enhance the contact
time between liquid and gas. The liquid phase is preferably sodium
hydroxide solution of known concentration (not more than 2 N), enters
from the top and the mixture of carbon dioxide and air (inert solvent for
gaseous phase), enters from the bottom of the column. Thus we have
counter-current flow column.NaOH is passed in excess of the theoretical
requirement in the column.

The reaction which takes place in absorption column and the bubbling pot
is:

When the samples from the absorption column and bubbling pot are
titrated with HCl, first end-point is obtained using a Phenolphthalein
indicator.

Moles of bicarbonate ion are equal to the moles of carbonate ion present.
Also, the moles of H+ ion reacted is equal to the sum of moles
of OH- and CO32- ions.

Second end-point is obtained using the Methyl Orange indicator which

helps us in determining the total moles of bicarbonate ion (and hence the
carbonate ions) present.

SIMULATOR
Constant Parameters

Parameters that remain constant throughout experiment and to be used in calculation

Concentration of HCl = 1 M
Volume collected for titration =10 ml
Time of run of experiment =10 min
Volume of NaOH initially in Bubbling Pot = 3 l

PROCEDURE

1) Prepare 20 liter of 1N NaOH solution in a feed tank.

2) Check the concentration of the feed solution by titration against 0.1 N HCl.

3) Fill the bubbling pot with 3 liters of above prepared solution. 

4) Check the concentration of the bubbling pot solution by titration against 0.1N HCl.

5) Set the flow rate of NaOH solution to 10 L/H.(you can set any point from slider)

6) Set the flow rate of carbon dioxide gas to 90 L/H. (you can set any point from slider)

7) Set the flow rate of air to 30 L/H.

8) Take sample at 10, 20, 30 minutes from column outlet and bubbling pot outlet.

9) Titrate the sample collected, using phenolphthalein indicator against 0.1N HCl.

10) titrate the same sample, using methyl orange indicator against 0.1 N HCl

11) Calculate the balance on NaOH and CO2.

Books:

1. Treybal, R.E., 1980. Mass-transfer operations, McGraw-Hill.

2. McCabe, W.L., Smith, J.C. & Harriott, P., 2005. Unit operations of chemical
engineering, McGraw-Hill.

MANIPULATION N°7 HEAT TRANSFER CONDUCTION

AMRITA
Aim:  

1. To find the thermal conductivity of a material by the two slabs guarded hot plate method.
2. To find the thermal resistance of the sample.

Apparatus:

A circular main heater plate (MH) is surrounded by an annular guard heater plate (GH) with a
narrow air gap in between. Each heater is made up of electrical resistance wire sandwiched
between two copper plates. Thermocouples are fixed to the plates to measure their surface
temperatures.
Two identical circular slabs of the material to be tested are placed on either side of and in
good thermal contact with the heater plates. On the outer sides of the two slabs, in good
thermal contact, are two circular water-cooled slabs whose surface temperatures can also be
monitored with thermocouples (Fig 1).
The purpose of the guard heater is to prevent heat loss from the edge of the main heater by
maintaining the temperature outside the main heater at the same temperature as the main
heater. This ensures that all heat lost from the main heater flows through the test slabs.

         
Theory:

The theory of heat transfer seeks to predict the energy transfer that may take place between
material bodies as a result of temperature difference. This energy transfer is defined as heat.
The three modes by which heat can be transferred from one place to another are conduction,
convection and radiation.
In conduction, heat is carried by means of collisions between rapidly moving molecules closer
to the hot end of a body of matter and the slower molecules closer to the cold end. Some of
the kinetic energy of the fast molecules passes to the slow molecules, and as a result of
successive collisions, heat flows through the body of matter from the hot end to the cold end.
Solids, liquids, and gases all conduct heat. Conduction is poorest in gases because their
molecules are relatively far apart and so interact less frequently than in solids and liquids.
Metals are the best conductors of heat because some of their electrons are able to move about
relatively freely and can interact frequently by collisions.
Without the guard heater, cooler air surrounding the edge of the main heater would be heated
by conduction and convection. Thus some of the heat supplied to the main heater would be
carried away by the surrounding air.

With the guard heater in place and adjusted to the same temperature as the main heater, the air
in the gap between is maintained at the temperature of the main heater, so no heat is lost at the
edge of the main heater. All heat lost from the main heater must flow into the test slabs.

Consider one dimensional heat conduction (Fig 2). The rate at which heat is conducted
through a slab of a particular material is proportional to the area A of the slab and to the
temperature difference ΔT between its sides and inversely proportional to the slab's thickness
d.

The amount of heat Q that flows through the slab in the time t is given by

Rate of conduction                                                       

 And thus                                                                                 

(1)

Where ΔT = T1 – T2, and k is the thermal conductivity of the material, is

a measure of its ability to conduct heat. The SI unit of k is Wm-1K-1.

Thermal conductivity: Note that a heat flow rate is involved, and the numerical value of the
thermal conductivity indicates how fast heat will flow. In general, thermal conductivity is
strongly temperature dependent. It has the units of watts per meter per Kelvin. Heat transfer
by conduction in a solid can be realized through the support of phonons, electrons and
photons. The individual contributions of these carriers widely depend on material and its
temperature. Thermal conductivity is thus a second order tensor, but in a material with cubic
isotropy it reduces to a scalar. It is an intensive property (changing the amount of material
does not change its thermal conductivity) and is a function of both pressure and temperature.

The thermal resistance R of a layer of a material of thickness d and of thermal conductivity k

is given by

                                                                                                       . (2)
The greater the value of R, the greater the resistance to the flow of heat.

Applications: 

Heat transfer has wide applications for the proper functioning of thermal devices and systems.
This principle is used to solve many problems in thermal mechanics.

1. Heat exchangers.
2. Building construction works.
3. Thermal energy storage devices.
4. Heat transfer in human body.
5. Thermopile and infrared thermometer.
6. Thermal resistance in electronics like thermal diode or thermal rectifier.
7. Used in laser cooling, radiative cooling, magnetic cooling, etc.
 

Performing Simulation:

 
Simulator Controls

1. The Choose Material combo box is used to select the material for the test slab.
2. The Diameter of the material slider is used set the diameter of the portion of the test slab
in contact with the main heater, in cm
3. The Thickness of material slider is used to set the thickness of the test slab, in cm.
4. The Coldwater temperature slider is used to set the temperature ( in degrees Celsius) of
the water flowing inside the outer plates.
5. The White knobs in simulator can be rotated by clicking side arrows to adjust the voltage
and corresponding current, which can be used to calculate input power.
6. The MH-GH Switch is used to set either main heater (MH) or guard heater (GH) voltage
and current as shown on the meters. Note: For the simulator to be powered on, the voltage for
both heaters must be the same.
7. The Power on button switches on the power after the initial adjustments are done.
8. The Temperature indicator is used to read the temperature at the positions of the various
thermocouples. After a steady state is reached (when the timer shows 20 minutes), click the
arrows on either side of the knob to read temperatures T1 to T8 in degrees Celsius.

Procedure for Simulation

1. Choose the material from combo box.

2. Using the sliders, fix a particular diameter for the portion of the test slab in contact with the
main heater, and a thickness for the entire slab.
3. Adjust the cold water temperature using the slider.
4. Using the white knobs, fix the value of same voltage and current for both main heater (MH)
and guard heater (GH). With the MH-GH switch set to MH, use white MH knob to set the
voltage and current for the main heater. Then click the MH-GH switch to GH and use the
white GH knob to set the voltage and current for the guard heater to the same values you set
for the main heater.
5. Click the Power On switch to power the unit on.
6. After a steady state is reached (20 minutes in the timer), use the temperature indicator to
read and note down T1, T2, T3, T4, T5, T6, T7 and T8.

7. Using the work sheet and the equations from the theory page, calculate the thermal
conductivity of the test slab. Note: since the main heater is in contact with a test slab on both
sides, the area A in equation

(1)  

where d is the diameter of the MH, not , as might first be assumed.

Procedure for Real lab

The procedure for the real lab is quite similar. The main differences are (1) the guard heater
can be set to a slightly different temperature, as needed, to keep the temperature of the main
heater uniform, and (2) the calculations can be extended to allow for and/or find the
dependence of k on ΔT.

 Observations and Calculations

Mean temperature at the surface of the specimen on the heater side,

=            °C

Mean temperature at the surface of the specimen on cold plate side,

=                              °C

Area of heat transfer,

=                       m2

In above equation, d is the diameter of the specimen

Heat transferred,    
    

Δx is the thickness of the specimen

Thermal conductivity                                                                                k =              Wm-1K-1 

Result: 

Thermal conductivity of the given specimen by conduction =                        Wm-1K-1 

References: 
Books:

1. Jiji, Latif. Heat Conduction. Berlin: Springer, 2009.

2. Holman, J. Heat transfer in SI units. New Dehli: McGraw-Hill, 2008
3. James R. Welty, Charles E. Wicks, Gregory Rorrer - 2009 - 776 pages
4. Pitts, Donald. Schaum's outline of theory and problems of heat transfer. New York: McGraw-
Hill, 1998.

Webliography:

1.  en.wikipedia.org/wiki/Thermal_conduction
2.  www.engineeringtoolbox.com/conductive-heat-transfer-d_428.html
3.  www.bbc.co.uk/schools/gcsebitesize/science/aqa_pre_2011/energy/heatrev1.shtml

MANIPULATION N°8 HEAT TRANSFER RADIATION

AMRITA

 Aim:

Heat Transfer by Radiation

1. To compare heat transfer between different material surface and the black body
surface by radiation.
2. To find the emissivity of different material surface.
 Apparatus:

Emissivity measurement apparatus: The experimental set up consists of two circular

aluminum plates identical in size provide with heater coils at the bottom Fig.1

It is kept in an enclosure so as to provide

undisturbed natural convection surroundings. The
heat input to the heaters is varied by two
regulators and is measured by an ammeter and
voltmeter. Each plate is having three
thermocouples; hence an average temperature is
taken. One thermocouple is kept in the enclosure
to read the chamber temperature. One plate is
blackened by a layer of enamel black paint to
form the idealized black surface whereas the other
plate is the test plate. The temperatures of the
plates are measured by using thermocouples.

Theory:

In radiation, energy is carried by the electromagnetic waves emitted by every object. In

general, radiation is a volumetric phenomenon. This is because the electrons, atoms and
molecules of all solids, liquids and gases above absolute zero temperature are in constant
motion and hence energy is constantly emitted, absorbed and transmitted throughout the entire
volume of the matter.

The radiation from a surface is emitted in all possible directions. A body at a temperature
above absolute zero emits radiation in all directions over a wide range of wavelength. The
amount of radiation from the surface of a body at a given temperature and at a given
wavelength depends on the material of the body and nature of its surface. A concept of an
idealized surface has been made which are perfect emitter and absorber of radiation. This
ideal surface is known as a black body.

A black body or ideal radiator is a body that emits and absorbs at any temperature the
maximum possible radiation at any given wavelength.

A black body has the following features           

1. At a specified temperature and wavelength a black body emits more radiation energy
than the real one.
 2. It absorbs all
incident radiation
regardless of
wavelength and
direction
3. It emits radiation energy
uniformly in all
direction. That is black
body is a diffuse emitter
the term ‘diffuse’ means
independent of
direction.

Depending on type of surface, the reflected radiation is specular or diffuse. A smooth and
polished surface is more specular while the rough surface is more diffuse.
The fraction of incident energy absorbed by the surface is called the absorptivity. For a black
body it is equal to one.
Actually black body do not exist in nature through its characteristics are approximated

by a hole in a box filled with highly absorptive material. The emission spectrum of such a
black body was first fully described by Max Planck.

Emissivity of a surface is defined as ratio of the radiation emitted by the surface to the
radiation emitted by the black body at the same temperature.

If a sample is replaced by a black body of temperature of same area at same temperature,

under thermal equilibrium, the emissivity of the body is equal to the absorptivity.

Relationship between Absorptivity and

Emissivity:

Consider two flat infinite plates, surface A and surface B,

both emitting radiation towards one another. Surface B is
assumed to be an ideal emitter, εB= 1.

Surface A will emit radiation according to Stefan’s Boltzmann law as

         (1)
And will receive radiation as
        (2)
Net heat flow from surface A will be
   (3)
Now suppose that the two surfaces are at exactly same temperature then, εA = αA
Emissivity of surface will depend on the material of which it is composed.
The radiation emitted per unit area per unit time from the surface of a body is called its
emissive power. The ratio of emissive power of a body to the emissive power of a black body
is called emissivity.
Heat emitted by the black body per unit area, (4)
Heat emitted by the test plate per unit area, (5)
εb Emissivity of the black plate.
εp Emissivity of the test plate
σ Stefan-Boltzmann constant = 5.67×10-8 W m-2K-4
Tb Black body temperature in Kelvin
Tc Chamber temperature in Kelvin
Tp Test plate temperature in Kelvin
Qb = Qp since input power to the two plates is same and conduction heat loss are also same.

Emissivity,   (6)

Working

The same amount of power input is given to both test plate and black plate. After achieving steady
state temperature for black plate, it continuously emits radiations and this radiation is completely
absorbed by the test plate. But its emit radiation is slightly less than the black body because
emissivity depends on nature of the material.  

Applications

1. In lasers
2. Microwave ovens
3. Solariums
4. Mobile telephones
5. MRI devices in the magnetic field
6. Industrial heaters

Procedure :
Variable Region:

1.  Choose material - This can be used to select the specimen plate.

2.  Diameter of the specimen- Used to vary the diameter of the specimen in centimeter.
3.  Thickness of the specimen- Used to change the thickness of the specimen in
centimeter.
4.  Chamber temperature- This is used to change the temperature in the evacuated
chamber in degree Celsius.

Measurement Region:
White knobs in simulator- This knob can be rotated by right clicking side arrows and
thereby adjusting the voltage and corresponding current which is given as input power.

Tuning Switch- Used to turn either Black plate (BP) or Test plate (TP) and thereby can
change the corresponding voltage and current for  both the plates.

Note: Power should be given for both the plates must be same.

Power on button- Using this button we can switch on the power when all the initial
adjustments were done.

Temperature indicator in the simulator- After steady state of temperature is reached (20
minutes in timer). Adjusting the knob by clicking the side arrows in the indicator, thereby T1
to T7 temperature on thermocouples can be noted in degree Celsius.

 Procedure for Simulation

1. Choose a particular material to perform simulation.

2.  Fix the value of diameter and thickness of the plate.

3. The temperature is given to the chamber using the slider «chamber temperature".

4. Using tuning switch and white knob, fix the voltage and corresponding current for black
plate and test plate.

5. Note the value of temperature T1, T2, T3, T4,T5,T6,T7 using temperature indicator.

6. Calculate the value of emissivity for a given test plate using equations.

Procedure for Real lab

 Using emissivity apparatus, the power is given to carry out the experiment using voltmeter
and ammeter. After steady state is reached,(2 hours), Using stop watch, every half an hour,
the temperature in the temperature indicator is noted. Using trial and error method, T 1,T2, T3,
T4, T5, T6, and T7  are noted. Calculate the value of emissivity for a given test plate using
equations.
Observations and Calculations:

Heat emitted by the black body,        

                                     W

Heat emitted by the test plate,                                                                       

W

εb Emissivity of the black plate and it is equal to 1

εp Emissivity of the test plate
σ Stefan-Boltzmann constant = 5.67×10-8 W m-2K-4

=..........................K

= ...................K

                                            K         

Qb = Qp since input power to the two plates is same and conduction heat loss are also same.
Emissivity of the specimen plate,                                                                                                 

Result

Emissivity of test plate surface =

References:

Books:

1. Siegel, Robert. And John Howell. Thermal Radiation Heat Transfer. London: Taylor
& Francis Group, 2001.
2. Keith, Frank et.al. Principles of Heat Transfer. City: CL-Engineering, 2010.
3. White, Guy. And Philip Meson. Experimental Techniques in Low-Temperature
Physics. Oxford Eng.: Clarendon, 2002.

Webliography:

 www.engineeringtoolbox.com/radiation-heat-transfer-d_431.html

 www.efunda.com/formulae/heat_transfer/radiation/overview_rad.cfm

 www.biocab.org/Heat_Transfer.html

MANIPULATION N°9 BATCH REACTORS

CONCLUSION

Arrive au terme de ce travail qui portait sur les opérations unitaires en laboratoire, force est
de constater que, leur connaissance est capitale pour toute personne désirant devenir
ingénieur. Nous notons que la tache ici accomplie ne donne un travail complet sur les
opérations unitaires utilisées en raffinage et en pétrochimie. Ces techniques de séparations,
de transformations et de traitements sont également utilisées dans d’autres domaines tels
que l’agro-alimentaire, la pharmaceutique etc.