Laboratory Manual

For

Advanced Chemical Engineering Lab (CHC510)

AY: 2021-22

Department of Chemical Engineering

Indian Institute of Technology (ISM), Dhanbad
Index

S.No. Name of the Experiment Page

No.
1. Study the physical properties of complex fluids flow behavior of 05
surfactant/polymer solutions for industrial application
2. Measurement of fluid flow 10
3. Determination of the heat transfer coefficient in drop wise & film wise 24
condensation
4. Performance of a Calandria Evaporator 29
5. Isothermal batch reactor (determination of activation energy) 36
6. RTD in packed bed reactor (PBR) 47
7. Simple binary distillation 56
8. Adsorption studies 61
9. Study of proportional (P) controller using computer-controlled level trainer 66
10 Study of proportional -integral (PI) controller using computer-controlled flow 74
trainer
11. Study of proportional-integral-derivative (PID) controller using computer- 82
controlled temperature trainer

2
Lab Safety Rules

Things to Do
• Be on time. Follow all written and verbal instructions carefully
• Conduct yourself in a responsible manner at all times in the laboratory
• Store your backpacks in the place mentioned by the Instructor and /or TA
• Familiarize yourself with all labs procedure before doing lab experiments
• Bring your lab notebook and an open mind to every lab
• Be aware of others in the lab. Areas of the room may be crowded at times and you
should take care not to disturb the experiments of others in the lab
• Be aware of all the safety devices
• Dress properly during a laboratory activity. Personal protective equipment (PPE),
such as gloves, safety glasses and lab coats, is an important factor in your safety
when working in the laboratory. Proper PPE should be worn during laboratory
experiments
• Keep clutter to a minimum. Work areas should be kept clean and tidy at all times
• Inform the instructor and/or TA if there is a problem. You will have their immediate
attention if you have cut yourself (even if you consider it minor), if something broke
and needs cleaning up, or if you are on fire
• Use extreme care when handling sharp objects
• Heated glassware remain very hot for a long time, picked up with caution. Use tongs
or heat protective gloves if necessary
• Read the chemical safety information (MSDS).
• Keep all materials away from open flames
• Dispose of all chemicals, broken glass and other lab materials as directed
• Always be sure that electrical equipment is turned in the "OFF" position before
plugging it into an electrical socket
• Always Turn OFF all electrical switches of the equipment before leaving laboratory
• Report ALL incidents, accidents, injuries, hazards or chemical spills to the instructor
(no matter how trivial it seems)
• Wash your hands before you leave the lab for the day

3
Things Not to Do
• DO NOT eat, drink beverages, chew gum in the lab
• DO NOT touch any equipment, chemicals, or other materials in the laboratory area until
you are instructed to do so.
• NEVER do any experiment on your own and NEVER work in the lab alone
• NEVER use electrical instrument around water
• DO NOT use the mobile
• NEVER smell, taste or touch chemicals
• DO NOT work with chemicals until you are sure of their MSDS that includes some
awareness of their flammability, reactivity, toxicity, and disposal.
• NEVER return unused chemicals to the original container/bottle
• DO NOT casually dispose of chemicals down the drain
• NEVER use chipped, cracked, or dirty glassware.
• DO NOT panic
• NEVER leave the lab without washing your hands

4
EXPERIMENT NO. 01: FLOW BEHAVIOR OF COMPLEX FLUIDS

AIM: Study the physical properties of complex fluids flow behavior of surfactant
/polymer solutions for industrial application.
OBJECTIVES:
❖ To prepare surfactant/polymer systems and determine the physical
properties of
these polymeric/surfactant systems.
❖ To evaluate rheological flow models for polymeric/surfactant systems.

Chemical/apparatus required- Rheometer, sample (surfactant/polymer

solutions), distilled
water
THEORY:
Science of flow and deformation of matter (liquid or solid) under the effect of an
applied force. A rheometer is a lab device used to measure how liquid suspension
or slurry flows in response to applied forces.it is used for those fluids which cannot
be defined by a single value of viscosity and therefore require more parameters to
be set and measured than is the case for a viscometer. It measures the rheology of
the fluid. There are two distinctively different types of rheometers. Rheometers
that control the applied shear stress or shear strain are called rotational or shear
rheometers, whereas rheometers that apply extensional stress or extensional strain
are extensional rheometers. Rotational or shear type rheometers are usually
designed as either a native strain-controlled instrument (control and apply a user-
defined shear strain which can then measure the resulting shear stress) or a native
stress-controlled instrument (control and apply user-defined shear stress and
measure the resulting shear strain). A rheometer is a device used to measure the

5
rheological properties of materials; rheology being defined as the study of the flow
and deformation of matter, which describes the interrelation between force,
deformation and time.
Unlike a viscometer, which can only measure the viscosity of a fluid under a
limited range of conditions, a rheometer is capable of measuring viscosity and
elasticity of non-Newtonian materials under a wide range of conditions. Some of
the most important properties that can be measured using a rheometer include
viscoelasticity, yield stress, thixotropy, extensional viscosity, creep compliance
and stress relaxation behaviour, as well as process-relevant parameters such as die
swell, melt fracture.
In general, either the fluid remains stationary and the object moves through
it. or the object is stationary, and the fluid moves past it. the drag caused by the
relative motion of fluid and surface is a measure of viscosity. The flow conditions
must have viscosity value of Reynolds number less than 2100 for laminar flow.
Rotational viscometer uses the idea that torque required to turn on an object in a
fluid is a function of the viscosity of that fluid. They measure the torque required
to rotate a disk or bob in a fluid at a known speed.

Block diagram of Rheometer.

6
PRINCIPLE:
The fluid is sheared in a narrow gap between concentric cylinders, parallel plates
or a cone and a plate. The viscosity is defined as the ratio of the shear stress and
the shear rate. The stress is related to the torque and the shear rate to the angular
velocity. One of these quantities is preselected the other is measured, depending on
the set-up of the instrument (controlled stress / controlled strain). A great variety of
tools is available to cover a large viscosity and shear rate range. Elastic material-
functions can be obtained from axial forces acting perpendicular to the plane of
shear in cone-plate or plate-plate geometry. Rotational rheometers allow for
numerous experimental modes controlling either shear rate, shear deformation or
shear stress.
PROPERTIES WHICH CAN BE MEASURED:
1) Dynamic viscosity 6) temperature
2) Shear rate 7)time
3) Shear stress 8)kinematic viscosity
4) Speed 9)fixed point
5) Torque 10)deformation

Rotational Rheometer

7
PROCEDURE:
➢ Turn on the rheometer/viscometer.
➢ Turn on the thermostat water bath. The setpoint should be between 20 to
30°C (the bath is used only as a thermal reservoir).
➢ Turn on computer, start the rheoplus program on computer.
➢ In toolbar press the icon “device”, which is a symbol of “rheometer”.
➢ In the control panel tab in the new window, press initialize to start.
➢ Put your desired tool.
➢ In control panel tab, press “set zero gap”.
➢ Set “default program”.
➢ Press “start” to begin adjustment.
➢ In the control panel tab, lift position high enough to put your sample (60
mm recommendable).
➢ Put your sample on plate.
➢ Set temperature.
➢ In the control panel tab, lift position.
➢ Press measuring position to go to measuring distance.
➢ Remove entered sample.
➢ The status column in your data table is good indication of reliability of
measurement.

After measurements are done:

✓ Lift the position to clean the plate.
✓ Clean the plate with distilled water or organic solvents (if needed).
✓ Exit rheoplus program.
✓ Take off the tool and clean it with water.
✓ Turn off device, thermostat bath and the computer.

8
OBSERVATION TABLE

S.NO Time Viscosity Shear rate Shear stress torque

RESULT/DISCUSSION:

OBSERVATION:

QUESTIONNAIRE:
Q1. What is the function of Rheometer?
Q2. What are rheological flow behaviour fluids?
Q3. Describe the working procedure of Rheometer?

9
EXPERIMENT NO. 2: MEASUREMENT OF FLUID FLOW

INTRODUCTION:

Flow measurement is an important topic in the study of fluid dynamics. It must

be made in chemical plants, refineries, power plants, and any other place where
the quality of the product or performance of the plant depends on having a
precise flow rate. Flow measurements also enter into our everyday lives in the
metering of water and natural gas into our homes and gasoline into our cars.
There are many instruments used in flow measurements. In this experiment, we
are going to use the following devices:
1. Venturi.
2. Orifice plate.
3. Rotameter.

OBJECTIVES:

This experiment aims to:

1. Familiarize students with some common devices and methods used in

measuring flow rate.
2. Each flow measurement device will be compared to the standard method of
using the catch-tank and stopwatch to measure the flow rate.
3. Determine the energy loss incurred by each of these devices.
4. Determine the energy loss arising in a rapid enlargement and a 900 elbow

10
APPARATUS:

The Flow Measurement apparatus. Water from the Hydraulic Bench enters
the equipment through a Venturi meter, which consists of a gradually
converging section, followed by a throat, and a long gradually diverging
section. After a change in cross-section through a rapidly diverging section, the
flow continues along a settling length and through an orifice meter. This is
made from a plate with a hole of reduced diameter through which the fluid
flows. The water then continues around a bend and up through a rotameter-type
flowmeter. The rotameter is a transparent tube of gradually diverging cross
section in which the “float” takes an equilibrium position; the vertical position
of the float is a measure of the flow rate.
After the rotameter, the flow returns via a control valve to the hydraulic
b
e
n
c
h

w
h
ere the flow rate can be measured using the catch-tank and a stopwatch.

THEORY:

For steady, adiabatic flow of an incompressible fluid along a stream tube, as

11
shown in figure (3), Bernoulli's equation between points 1 and 2 can be written
in the form:
P1 V12 P V2
+ + z1 = 2 2 + z2 + H12 − − − − − − − −(1)
pg 2 g pg 2 g

Where:
P
= Hydrostatic Head
pg
V2 volumetric flow rate Q
= Kinetic Head, (V is the mean velocity; V = =
2g cross sectional area of tube A
z = Potential Head
P V2
+ + z = Total Head
pg 2 g

The head loss H12 may be assumed to arise as a consequence of the vortices
in the stream. Because the flow is viscous a wall shear stress exists and a
pressure force must be applied to overcome it. The consequent increase in flow
12
 work appears as an increase in internal energy, and because the flow is viscous,
the velocity profile at any section is non-uniform.

FLOW MEASUREMENT:

1. Ventury meter:

A Venturi Meter is a device used for measuring the rate of a flow of a fluid flowing
through a pipe. It consists of three parts:
(i). A short conversing part
(ii). Throat
(iii). Diverging part

A Venturi Meter apparatus is based on Principle of Bernoulli’s equations. The

principle of apparatus is that, by reducing the cross section area of flow passes,
pressure difference is created and the measurement of pressure difference enables
the determination of the discharge through the pipe.

13
 A Venturi meter consists of an inlet section followed by a convergent cone,
a cylindrical throat and a gradually divergent cone.

By knowing the pressure difference across the inlet section and the throat,
discharge can be calculated by the formula:

a1a2 2gh

Qa= Cd * a12 − a22

Consider a venturimeter fitted in a horizontal pipe through which a fluid is

flowing (say water), as shown:

Let d1= diameter at inlet

p1= pressure at inlet
v1= velocity of fluid at inlet
a1= area at inlet section= ∏*d12/4
And d2, p2, v2, a2 are corresponding values at throat section (2).

Applying Bernoulli’s equation at both the inlet and throat section, and
considering the pipe to be horizontal,
The theoretical discharge Q is,

a1a2 2gh

a12 − a22
Qt=

14
 Qact= Cd*Qt

Where, Cd = Co-efficient of venturimeter and its value is less than 1.

Such that the diameters (bores) of the meter at (A) and (B) are 26 mm and
15 mm respectively.

2. Orifice meter:

An Orifice Meter is also a device used for measuring the rate of flow
of a fluid through a pipe. It also works on the same principle as that of venturi
meter. It consists of a flat circular plate which has a circular sharp edged hole
called orifice, which is concentric with the pipe. The orifice diameter is kept
generally 0.5 times the diameter of the pipe, though it may vary from 0.3 to 0.8
times the pipe diameter.

The principle of apparatus is that, by reducing the cross section area of flow
passes, pressure difference is created and the measurement of pressure
difference enables the determination of the discharge through the pipe.

15
An orifice meter is another device used for measuring the discharge through
pipes. Orifice meter works on the same principle as that of venturimeter i.e. by
reducing the cross sectional area of the passes a pressure difference between
the two sections is developed and the measurement of the pressure difference
enables the determinations of the discharges through the pipe.

An orifice meter consists of a flat circular plate with a circular hole called
orifice, which is concentric with the pipe axis. The discharge through the
orifice meter can be calculated by the formula

a1a2 2gh

a12 − a22
Qact=Cd*

Qact=Cd*Qt

Consider an orificemeter fitted in a horizontal pipe through which a fluid is

flowing (say water), as shown:
Let d1=diameter at inlet
p1=pressure at inlet
v1=velocity of fluid at inlet
a1=area at inlet section= ∏*d12/4
And d2, p2, v2, a2 are corresponding values at downstream section (2).

Applying Bernoulli’s equation at both the upstream and downstream section,

and considering the pipe to be horizontal,
The theoretical discharge Qt is,

16
 a1a2 2gh

a12 − a22
Qt=

Qact= Cd* Qt

Where, Cd = Co-efficient of orificemeter and its value is less than 1.

With the apparatus provided, the diameter (bore) at (E) is 50mm. At (F), the
water diameter (not the bore) is 20 mm

3. Wide-angled diffuser:

The inlet to the diffuser may be considered to be at (C) and the outlet at (D).
Applying equation (1):

PG VG2 PH VH2
+ = + + H GH − − − − − − − −(10)
pg 2 g pg 2 g

4. Right-angled bend:

The inlet to the bend is at (G) where the pipe bore is 51.9 mm and outlet is at
(H) where the bore is 40 mm. Applying equations (1):

PG VG2 PH VH2
+ = + + H GH − − − − − − − −(11)
pg 2 g pg 2 g

The outlet kinetic head is now 2.8 times the inlet kinetic head.

17
STANDARD DATA:

Venturimeter upstream diameter 26mm

Venturimeter converging Angle 14 degree
Venturimeter Throat diameter 15mm
Venturimeter diverging Angle 21 degree
Pipe diameter 26mm
Sudden enlargement pipe diameter 50mm
Orifice diameter 20mm
Density of water ρw 1000 kg/𝑚3

EXPERIMENTAL PROCEDURE:
Part 1: Flow measurements and head losses

1. Make sure the air purge valve is closed.

2. Close the control valve of the flow measurement apparatus fully, then
open it by about 1/3.
3. Switch on the hydraulic bench pump
4. Slowly open the hydraulic bench valve until water starts to flow. Allow
the flow measurement apparatus to fill with water
5. Open the bench valve fully, and then close the control valve of the flow
measurement apparatus
6. Open the valve of the flow measurement apparatus (1/4 turn ONLY)
7. Connect the hand pump to the air purge valve and pump until all the
manometers read approximately 330 mm

18
8. Dislodge any entrapped air from the manometers by gentle tapping with
the fingers
9. Check that the water levels are constant. The levels will rise slowly if the
purge valve is leaking
10.Open the apparatus valve until the rotameter shows a reading of
approximately 10 mm.
11.When a steady flow is maintained measure the flow with the hydraulic
bench as follows:
a. Direct the outlet of your experiment to the volumetric tank
b. Start your stopwatch as soon as the water level in the volume
indicator reaches 0.
c. Stop your stopwatch when the level in the volume indicator
reaches 10
12.Record the readings of the manometers in table (1)
13.Repeat steps 10-12 for 10 tests. Increase the opening of the apparatus
valve such that the rotameter reading is increased in steps of 10 mm.

19
OBSERVATION TABLE:

1 2 3 4 5 6 7 8
A
B
Manometer C
Levels D
E
F
G
H
Rotameter (cm)
Water W (kg)
Time T (seconds)
Mass Flow Venturi
Rate m Orifice
(kg/s) Rotameter
Weight
Tank
∆H/Inlet Venturi
Kinetic orifice
Head Diffuser
Elbow

20
CALCULATIONS

➢ Actual discharge,

R1 − R2
R=
100 , m = _ _ _ _ _ _ _ _ _ _ _m

A R 3
Q= m / sec =
t _ _ _ _ _ _ _ _ _ _ _m3/sec

➢ Head losses m of water, (Hf)

h1 − h2
h= ,m =
100 _ _ _ _ _ _ _ _ _ _ _m
 
H f = h m − 1
 w , m = _ _ _ _ _ _ _ _ _ _ _m

➢ Cross- section area, 𝑚2


a= d 2 , m2 =
4 _ _ _ _ _ _ _ _ _ _ _m2

➢ Velocity of fluid/s

Q
V = , m / sec =
a _ _ _ _ _ _ _ _ _ _ _m3/sec

21
NOMENCLATURE:

A = Area of measure tank, m2

V = velocity of fluid/s
R = rise of water level in measuring tank, m
R1 = final level of water in measuring tank, cm
R2 = initial level of water in measuring tank, cm
h = manometer difference, m
h1, h2 = man metric reading at both points, cm
hf = head losses, m of water.
Q = discharge, m2 /s
T = time taken for r, sec
ρw = density of water,

PRECAUTION AND MAINTENANCE INSTRUCTIONS:

1. Never run the apparatus if power supply is less than 180 volts & above
230volts
2. Never fully close the delivery valve & by-pass valve at a time.
3. To prevent clogging of moving parts, run pump at least once in a for night.
4. Always use clean water.
5. If apparatus is not in use for more than one month, drain the apparatus
completely.
6. Always keep the apparatus free from dust.

22
TROUBLESHOOTING:

1. If pump gets jam, open the back cover of pump & rotate the shaft manually.
2. If pump gets heat up, switch OFF the main power for 15 min & avoid
closing the flow control valve at a time during operation.

REFERENCES:

1. Ychengel j. cembala, “fluid mechanics”, 2nd ed. Mc grew hill, ND,2007,

page 329.
2. Dr.P.N.Modi & P.N.seth, “Hydraulics & fluid mechanics including
mechanics,”15th ed., rajinder Kumar Jain, ND, 2005, page 458-459.

23
EXPERIMENT NO. 3: DETERMINATION OF THE HEAT TRANSFER
COEFFICIENT IN DROP WISE & FILM WISE CONDENSATION

OBJECTIVE: To study heat transfer in the process of condensation.

AIM: To find heat transfer coefficient for drop-wise & film-wise condensation
process.
INTRODUCTION:
In all applications, the steam must be condensed as it transfers heat to a cooling
medium, e.g. Cold water in the condensers of a generation station, hot water in a
heating clarifier, sugar solution in a sugar refinery etc. During condensation very
high heat fluxes are possible and provided the heat can quickly transferred from the
condensing surface to the cooling medium, heat exchangers using steam can be
compact and effective.
THEORY:
Steam may condense on a surface in two distinct modes, known as film wise and
drop wise condensation. For same temperature between the steam and surface
dropwise condensation is much more effective than film wise condensation and for
this reason, the former is desirable although in practical plants, it rarely occurs for
prolonged period.
Film wise condensation: Unless specially treating, most materials are wet table and
as condensation occurs as film condensate spreads over the surface. The thickness
of the film depends upon a number of factors, e.g. the rate of condensation, the
viscosity of the fluid, the surface orientation and nature.
Fresh vapor condenses on to the outside of the film and heat is transferred by
conduction through the film to metal surface beneath, as the film thickness
increases it flows downward drips from the low points leaving the film intact and
at an equilibrium thickness. The film of liquid is a barrier to the heat transfer and

24
its resistance accounts for most of the difference between the effectiveness of the
film wise and drop wise condensation.
Drop-wise condensation: By specially treating the condensing surface, the contact
angle can be changed and the surface become not wettable. As steam condense, a
large number of generally spherical beads cover the surface. As condensation
proceeds, the beads become larger, coalesce, and then strike downwards over the
surface. The moving bead gathers on the static beads along its downward in its tail.
The bare surface offers very little resistance to the transfer of heat and very high
heat fluxes are therefore possible. Unfortunately, due to nature of material used in
construction of condensing heat exchangers, filmwise condensation is normal.
EXPERIMENTAL SETUP:
The equipment consists of a metallic container in which steam generation
takes place. The lower portion houses suitable electric heater for steam generation.
A cover is provided for filling water. The glass cylinder houses two water cooled
copper condensers, one of which is chromium coated to promote drop wise
condensation and other is in its natural state to give film wise condensation. A
pressure gauge is provided to measure steam pressure. Separate connections of two
condensers for passing water are provided. One Rota meter is provided to measure
flow rate of water through the condenser. A multi-channel digital temperature
indicator is provided to measure temperature of steam, condensers, and water inlet
and outlet from condenser.
SPECIFICATIONS:
1. Condensers- one chromium plated for drop wise condensation and one
having natural finish for film wise condensation. Both condensers are
identical in construction. Dimensions:
Outer diameter: 20.4 mm
Inner diameter: 20 mm

25
 Length: 150 mm
Material: Copper
2. Main unit: M.S. fabricated construction comprising of test section and steam
generator. Test section is provided with glass cylinder for visualization of
the process. It also houses Rota meter and necessary piping and valves to
connect any one condenser in operation
3. Steam generator: Suitable for above experiment with electric heater.
4. Instrumentation:
a) Multy-channel digital temperature indicator with cold junction
compensation with thermocouples. Range 0 to 300°𝐶.
b) Rota meter to measure flow rate of water flowing through
condenser. Range 10 to 100 Lph.
c) Pressure gauge to measure steam pressure. Dial type, range 0 to
2.1 kg/cm2
5. Control panel: Separate control panel to house temperature indicator,
necessary switches, steam generator etc.

PROCEDURE:
1) Fill up the water in steam generator by opening the valve
2) Switch ON the heater switch.
3) After filling the water close to the top cover of steam generator. Start water
flow through one of the condensers which is to be tested and note down the
water flow rate in Rota meter. Ensure that during measurement, water is
flowing only through the condenser under test.
4) Slowly steam generation will start in the steam generator of the unit and as
the steam rises to the test section, gets condensed and falls down in the
cylinder.

26
 5) Depending upon type of condenser under test drop wise or film wise
condensation can visualized.
6) If the water flow rate is low then steam pressure is changed then
condensation will occur at more or less atmospheric pressure.
7) Observations like temperature, water flow rate, pressure, are noted down in
the observation table at the end of each test.

FORMULAE:-
Heat loss from steam :Qs =Ms .θ
Heat taken by cold water: Qw = Mw .Cp.(T5-T4)
Average heat transfer: Q= (QS+QW) /2
Inside heat transfer coefficient:Hi = Q/(Ai.∆Tm )
Outside heat transfer coefficient:Ho= Q/(Ao.∆Tm)
Experimental overall heat transfer coefficient: 1/Uex= 1/hi+ (Di/Do).(1/ho)
Nusset number: Nu = 0.023 (Re)0.8 (Pr)0.4
Theoritically heat transfer coefficient:1/Uth= 1/hi + (Di/Do).(1/ho)

OBSERVATION TABLE:

SI.No. Water Steam Time Temperature

flow rate condense (min) T1 T2 T3 T4 T5 T6 T
(lph) d 7

(ml)
Film 1
wise 2

27
Drop 1
wise 2

RESULTS: Do calculations and report all the results that you have obtained in
your experiment and write down the discussions in your journal.

CONCLUSIONS: Compare the experiment heat transfer coefficient that you have
obtained for different conditions.

PRECAUTIONS:
1. Do not start heater supply unless water is filled in the steam generator.
2. Operate all the switches and controls gently.
3. Never allow steam to enter the cylinder unless the water is flowing through
condenser.
4. Always ensure that the equipment is earthed properly before switching on the
supply.

QUESTIONS:
1. What is condensation? How does it occur?
2. What is the difference between film and drop wise condensation? Which is a
more effective mechanism of heat transfer?
3. Consider film condensation on a vertical plate. Will the heat flux be higher at
the top or at the bottom of the plate? Why?

28
EXPERIMENT NO. 4: PERFORMANCE OF A CALANDRIA
EVAPORATOR

OBJECTIVE: To concentrate the solution carbonate using Calandria evaporator.

AIM: To determine an overall heat transfer coefficient for the evaporator.
INTRODUCTION:
Evaporation deals with the concentration of a non-volatile solute from a
solution by the removal of required amount of volatile solvent. Usually the solvent
is water. By vaporizing a part of the solvent, useful product i.e. the concentrated
solution or thick liquor is produced and the vapor is discarded. This is usually done
before crystallizing or drying the material, or to reduce the volume for transport or
storage.
THEORY:
For heat transfer from the condensing steam to the boiling solution, the
overall heat transfer coefficient is found from the equation:
𝑄 = 𝑈𝐴∆𝑇
The temperature difference ∆𝑇 is the difference between the temperature at which
the steam condenses at the shell side pressure, and the temperature at which the
solution boils at the tube side atmospheric pressure.
∆𝑇 = 𝑇𝑠 − 𝑇𝑤
The area could be taken as either the inside or outside surface area of the tubes.
The inside area is chosen because the greatest resistance to heat transfer is on this
side. The area of the central downcomer is included, but the area of the tube plates
is excluded.
𝐴 = 𝑛(𝜋𝐷𝑙)𝑡𝑢𝑏𝑒 + (𝜋𝐷𝑙)𝑑𝑜𝑤𝑛𝑐𝑜𝑚𝑒𝑟
Heat flow from the steam to solution:
The heat flow is expressed in Watts (W) and calculated from an energy balance on

29
the feed and the two outgoing streams which are:
Product stream i.e. a saturated hot liquid phase leaving the evaporator.
Condensate i.e. a saturated vapor leaving the evaporator, then being
condensed and cooled.
Then the steady state energy balance (neglecting the losses) is:
𝑄 = 𝑤𝑝 ℎ𝑝 + 𝑤𝑣 ℎ𝑣 − 𝑤𝑓 ℎ𝑓
Q will be in Watts and corresponding units of overall heat transfer coefficients will
be, 𝑊 ⁄𝑚2 𝐾
Material balance:
At steady state, you would expect: 𝑤𝑓 = 𝑤𝑝 + 𝑤𝑣 (this should check out
within ±5%)
EXPERIMENTAL SETUP:
Present evaporator is a vertical short tube type evaporator with stainless steel
tubes. A central downcomer is provided. The feed solution (to be evaporated) is
fed near the top end of the tubes, flows down through the downcomer and rises
through the tubes due to density difference. It circulates up through the tubes by
natural convection, and some of the water is vaporized in the tubes. The liquid and
vapor separate in the vapor space above. The vapor is passed through the
condenser and collected as vapor condensed at the end of the condenser, while
liquid returns through the central downcomer to the bottom space before again
rising through the tubes. The water level in the evaporator is maintained nearly at
constant level by supplying a continuous feed and adjusting the product flow at the
bottom of the evaporator. The amount of water evaporated is estimated by
measuring the rate of water collected at the base of the rate of water collected at the
base of the condenser.
The heat used to evaporate the water, comes from steam from the steam

30
boiler provided at the base of the assembly. It enters the (shell side) space around
the tube bundle where it loses heat, condenses and collects at the bottom of the
shell space. The condensate drains out through a steam trap (which permits
condensed steam but not the live steam to pass through it). Flow rate of feed is
recorded from the readings of Rota meter in LPH. Bottom product flow can be
obtained with the help of measuring cylinder and stop watch. Densities of feed and
product are measured by using specific gravity bottles at ambient conditions.

Sensor positions are as follows:

T1 = Steam inlet temperature
T2 = Feed inlet temperature
T3 = Liquid temperature in vessel
T4 = Temperature of vapor entering to condenser
T5 = Condensed steam temperature
T6 = Water inlet temperature
T7 = Water outlet temperature
UTILITIES REQUIRED:
Water supply 5 LPM and drain
Electricity supply: 1 Phase, 220 V AC, 6 kW
Chemicals: 𝑁𝑎2 𝐶𝑂3
EXPERIMENTAL PROCEDURE:
1. Fill the feed tank with solution (~ 5 wt %) up to ¾ height.
2. Switch on the power supply to the steam generator (keep steam supply
closed) and attain the desired steam pressure.
3. Introduce the feed in to the evaporator by opening the Rota meter needle
valve at the maximum. Fill the evaporator.

31
4. Direct the steam into the shell side of the evaporator by opening the steam
valve. Heat the liquid in the evaporator till observes boiling in the glass-
viewing window. Adjust the steam rate at the desired level in the steam
jacket. Now allow fresh feed to enter by opening the feed valve and
adjusting the feed rate at the desired level.
5. Open the product valve and adjust the flow rate of product such that the
liquid level in the evaporator remains steady by observing it through front
window glass.
6. Wait till steady state is achieved. (Temperature and flow rates do not vary
with time). It may take about one hour.
7. During this one hour record the following at 15 minutes interval:
Product density, product concentration, weight of water vapor evaporated
(𝑤𝑣 ), feed rate, product rate, boiling temperature of liquid in the evaporator
(𝑇𝑤 ), condenser water outlet temperature (𝑇𝑤𝑜 ), cooling water flow rate to
the condenser (𝐹𝑤𝑐 ), shell side steam pressure gauge reading (𝑃𝑠 ).

CLOSING PROCEDURE:
1. Close the inlet feed valve.
2. Close the steam supply by switching off the electric supply to the steam
generator.
3. Wait till residual vapor is condensed.
4. Drain Calandria, concentrated and condensate receivers.
5. At last close the cooling water supply to the condenser.

SPECIFICATION:

Evaporator: Material Stainless Steel, OD-30cm, with central down take of

32
 10cm Dia,
Feed Tank: Material Stainless Steel, Capacity 20 Ltrs
Flow measurement: Rotameter 2 Nos. (One each for feed arid cooling water)
Feed Circulation: By compressed air (optional: using mini compressor)
Steam Generator: Made of Stainless Steel provided’ with Pressure & Level
Gauge, Safety valve and drain etc. & insulated with ceramic wool and
cladding with Aluminum foil.
Piping: Stainless Steel and PVC, size ¼”
Condenser: Shell & Tube type made of Stainless Steel
Product tank: Made of Stainless Steel, capacity 10 Ltrs.
Heater: Nichrome wire heater.
Water supply tank: Made of Stainless Steel, capacity 100 Ltrs. (for
condenser).
Pump: FHP capacity
Temperature Sensors: RTD PT-100 type

Control panel of:

Digital Temperature Controller: 0-199.9°C (For Steam Generator)
Digital Temperature Indicator: 0-199.9°C with multi-channel switch
On/Off switch, Mains Indicator etc.

FORMULAE:
1. Mass flow rate of feed: 𝑊𝐹 = 𝑤𝑓 × 𝜌𝑓 , g/s
2. Mass flow rate of product: 𝑊𝑃 = 𝑤𝑝 × 𝜌𝑝 , g/s
3. Mass flow rate of condensed vapor: 𝑊𝑉 = 𝑤𝑣 𝜌𝑣 , g/s
4. Heat transfer area: A = 𝑛(𝜋𝐷𝑙)𝑡𝑢𝑏𝑒 + (𝜋𝐷𝑙)𝑑𝑜𝑤𝑛𝑐𝑜𝑚𝑒𝑟 , m2

33
 𝑄
5. Heat transfer coefficient: 𝑈 = , 𝑊 ⁄𝑚 2 ℃
𝐴×∆𝑇

6. Heat balance: 𝑄 = 𝑤𝑝 ℎ𝑝 + 𝑤𝑣 ℎ𝑣 − 𝑤𝑓 ℎ𝑓
7. Mass balance: 𝑤𝑓 = 𝑤𝑝 + 𝑤𝑣
8. Economy = Amount of water vaporized (kg) / Amount of steam used (kg)
OBSERVATIONS:
Data:
Number of tubes in Calandria, n =
Outer diameter of tube =
Inner diameter of tube =
Tube length =
Downcomer outer diameter =
Calibration curve for sugar solution at 30 ℃
Conc. 0 10 12 14 16 18 20 25 30
(% w/v)
Density
g/ml

Plot density vs concentration on a simple graph and obtain a straight line.

Feed density =
Feed concentration from the calibration curve =
OBSERVATION TABLE:
SI. Time Product P, lph 𝑊𝑒𝑣 𝑇𝑤 𝑇𝑤𝑖 𝑇𝑤𝑜 𝐹𝑤𝑐 𝑇𝑠
No (min) density lph ℃ ℃ ℃ lph ℃
1 0
2 15
3 30

34
4 45
5 60

RESULTS: Report all the results that you have obtained in your experiment and
write down the discussions in your journal.
CONCLUSIONS: Using the results obtained from your experiment comment on
the heat transfer coefficient of the evaporator.
Precaution:
i. Use the stabilize AC single phase power supply only.
ii. Do not disturb any electrical connections of the experimental setup.

QUESTIONS:
1. Define evaporator capacity and economy.
2. Write down the enthalpy balances for the single effect evaporator
3. Explain enthalpy – concentrations diagram.

35
EXPERIMENT NO. 5: ISOTHERMAL BATCH REACTOR
(DETERMINATION OF ACTIVATION ENERGY)

AIM: To study of a non catalytic homogeneous reaction in an isothermal batch

reactor.
To determine the rate constant (k) for the given saponification reaction of ethyl
acetate in aqueous sodium hydroxide solution.
To determine the effect of temperature on k and determine the activation energy.
THEORY:
A batch reactor is a closed system with no input and output streams. A batch
reactor can operate under the following conditions:
Isothermal (temperature of reaction mass remains constant)
Perfectly mixed (composition of the reaction mixture is uniform throughout)
Constant volume (volume of the reaction mixture within the reactor remains
constant; there is no appreciable change in the density of reaction mass)
In a homogeneous reaction, all the reactants remain in single phase. The rate of
reaction for such a reaction is expressed as:
Moles of Product formed per unit volume of reaction mixture per unit time.
For a first order unidirectional reaction A Product
Rate of reaction can also be expressed as moles of A disappearing per unit volume
per unit time
Also - rA = KCA = K NA / V
Combining these two equations yield.
ln NA = ln NA0 - kt
NA = NA0 e – kt
Or, in terms of Concentrations

36
CA = CA0 e – kt
And
NA0 = No of moles of A at t = 0
NA = No of moles of A at t = t
For second order unidirectional reaction
2A Product
If we plot 1/CA Vs t we must get a straight line with slope = k and intercept = 1/C A0
For second order reaction:
A+ B Product
(If NA0 = NB0 then NA = NB for all t)
It reduces to 2A product
Degree of conversion X is defined as:

Equation

And NB = NB0 – NA0 X for NA0 NB0

Equation

The effect of concentration on the rate of reaction is generally determined

experimentally in a batch reactor by studying the rate of reaction at constant
temperature
The interpretation of the kinetic data involves a trial and error procedure. A
kinetic model is first assumed and the experimental observed conversion – time
rate is matched with the selected model. The reaction rate constant is a strong
function of reaction temperature. The temperature dependence of k is expressed in
terms of Arrhenius equation: k = A exp(-EA/RT)
A = frequency factor of Arrhenius constant
EA = Activation Energy
R = gas law constant
37
This equation can be written in the form:

ln k = lnA – EA/(RT)
A plot of ln k Vs 1/T shall yield EA and A.

In case of second order reversible reaction with CA0 = CB0 Equation

Equation

XAe = fractional conversion at

equilibrium Saponification of Ethyl
acetate & NaOH
CH3COOC2H5OH+NaOH CH3COONa + C2H5OH
88g 40 82 46
B + A C + D

Description

A batch reactor is closed system with no input and output streams. A batch
reactor can operate under conditions like isothermal (Temperature of reaction
Mass remains constant), perfectly mixed (composition of reaction mixture is
38
uniform throughout), and constant volume (volume of the reaction mixture within
the reactor remains constant, there is no appreciable change in the density of
reaction mass). This set – up is used to study a non – catalytic homogeneous
reaction under isothermal condition. The set up consists of a reactor fitted in a
constant temperature water bath. One stirrer is fitted for mixing the reactants in
reactor and other is fitted in water batch to keep the uniform temperature
throughout in the bath. The temperature of bath can be maintained from ambient
to 900C with the help of Digital temperature indicator cum controller. Samples
can be taken out with the help of a sampling pipette.
Volume of reactor = 2.815
lt Volume of bath = 14.3lt
Reactor stirrer =100rpm

Bath stirrer = 100rpm

Temperature controller – ambient to 2000C with 10C

resolution Utilities required
1. Water supply

2. drain

3. electricity supply 1 phase 220V AC,1.5kw

4. Instruments, laboratory glass ware and chemicals required for analysis as

per the system adopted.

Chemicals:
1. N/10 NaOH

2. N/10 HCl

3. N/10 Ethyl acetate (8.8gms of ethyl acetate in 1 lits of water), indicator

(phenolphthalein)

39
EXPERIMENTALPROCEDURE:

1. Prepare a solution of N/10 ethyl acetate by mixing 8.8gms (or 9.8ml at

200C) of ethyl acetate in 1L of solution.

2. Prepare a solution of N/10 NaOH by dissolving 4gms / 1L of solution

3. Prepare a solution of N/10 HCl

4. Use phenolphthalein as indicator

5. Take 6Nos of 250ml beakers and put 20ml of N/10HCl in each beaker

6. Take N/10 NaOH in the burette

7. Adjust the temperature of water bath at250C

8. If the volume of reactor is 1L then take 400ml each of N/10 CH3COOC2H5

and N/10 NaOH in two separate flasks and keep these in the water bath for
about 15min
9. Transfer these solutions quickly in the batch reactor. Start immediately the

mixer and the stopwatch

10. At regular intervals of 3-5min withdraw 100ml of reaction mixture and put

it in the marked beakers containing N/10HCl. Take at least 6 samples at

regular intervals of time.
11. Transfer the solution from beakers to the conical flasks, and titrate the

excess N/10 HCl in each flask using N/10 NaOH from burette and
phenolphthalein as indicator

12. Record the reaction temperature

13. Equilibrium conversion can be determined at reaction time of ½hr

14. In order to study the effect of temperature on k the above steps may be

repeated at temperature = 350C and 500C. all the reactants must be

40
 preheated in the water batch before mixing in thereactor.

Standard Data

Reactor : Material stainless steel 304 grade, Volume

2.1 Lts(Approx)
Water Bath : Material stainless steel 304 grade, double wall,
insulated with ceramic wool
Heater : Nichrome wireHeater

Stirrers (2Nos) : stainless steel 304 grade impeller and shaft

coupled with FHPmotor
Stopwatch : electronic
Temperature sensor : RTD PT –
100type
Control panel comprises of Digital Temperature controller cum – indicator (
For Batch) = 0 – 1999.90C, RTD PT – 100 type
With standard make on/off switch, mains indicator fuse etc

The whole unit is assembled rigidly on a base plate and mounted on a

stand Most of the parts are powder coated and rest are painted with auto
paints

FORMULAE:

Degree of conversion XA = (CA0 – CA)/CA0

Amount of HCl taken as quench, HCl = VHCl*NHCl / 1000, gmol

Amount of HCl reacted with the un-reacted NaOH of the reaction sample =
HCLR = HCLO – (V* NNaOH)/1000), gmol

41
Concentration of unreacted NaOH in the reaction mixture, CA= (HCLR /
VSamp)*1000, gmol/L

Measurement data:

Time, t (min) CA Concentration of NaOH 1/CA

(gmole/L) (L/gmole)

0
-
-
-

Plot t Vs 1/CA

42
Slope = k, L/gmole – min

CA = concentration of NaOH in
gmole/L

t =time in min
Plot k Vs (1/T – 1/ T0), k –1 on a semi log graph
Slope = - EA/Rk, (L/gmole –min)

Intercept = K0

Express

K = k0E- EA/RT

Observations and Calculation Reaction:

k

A+B C+D (CA0 =CB0)

Reaction temperature=00C = 0K
Concentration of Ethyl acetate = N/10
Concentration of NaOH = N/10

43
Volume of Ethyl acetate taken
=400ml

Volume of Sodium Hydroxide = 400ml

Initial concentration of Ethyl acetate (B) in the mixture = 0.01N = C B0

(gmole/L) Initial concentration of NaOH (A) in the mixture = 0.01N = C A0
(gmole/L)

S. No Time, t Min. Concentration of unreacted NaOH in 1/CA

the

reaction mixture, CA (gmole/L)

Tabulate the time concentration data ( t Vs CA)

Determine the rate constant k by assuming the reaction to be of second order and
plotting 1/CA Vs t
1 1
kt
CA C A0

Draw a smooth curve through all the points

If the data points yield a straight line, the assumed order of 2 is

confirmed Slope = k (L/gmole –min)
Intercept =1/CA0 (L/gmole)

44
Tabulate k values at 3 or 4 different temperatures

S. NO k T, K T0, K (1/T – 1/T0), K -1

1 T1
2 T2
3 T3 T0
4 T4

T0 = (T1 + T2 + T3+T4)/4

Plot k Vs (1/T – 1/T0), K –1 on a semi log graph

𝐸𝐴
𝑆𝑙𝑜𝑝𝑒 =
𝑅

intercept = k0

Express, k = k0 e –EA/RT

45
PRECAUTIONS & MAINTANANCE INSTRUCTION:

1. Measure the exact volume of water and weigh the chemicals.

2. Always use clean water and good quality chemicals and standard solution

for titration
3. Use electronic balance for weighing of chemicals. Don’t mix the droppers

of different chemicals
4. Keep close all the drain valves and vent valve should open while filling

the reactant in feed tanks

5. Flow should not be disturbed during the experiments

6. Handle the chemicals carefully

7. Don’t ON heater switch before filling the water in the bath

There should be no air in the flow during experiment

TROUBLESHOOTING:
1. If any type of suspended particles are come in the rotameter. Remove the

rotameter clean the tube and fit that at its place.

2. if there is any leakage tight that part or remove that and fix that again after

wrapping Teflon tape

3. if rotameter fluctuating more than average tight control knob of that

(Procedure: two nuts are there lose first nut and tight the second lightly,
and then first also, both nuts are on rotameter)
4. if D.T.C display ‘1’ on display board it means sensor connection is not OK

tight that
5. if switch ON the heater but temperature can’t rise but panel LED is ON it

means bath had burned replace that

REFERENCE: Chemical Reaction Engineering by Octave Levenspiel, Chapter 2.

46
EXPERIMENT 6: RTD IN PACKED BED REACTOR (PBR)

OBJECTIVE: Study of a Non-Catalytic Homogeneous reaction in Packed Bed

Reactor.
AIM: To determine the reaction rate constant for saponification of ethyl acetate
with NaOH at ambient conditions.
INTRODUCTION:
A packed-bed reactor shown in figure. When a reactor is packed with catalyst, the
reacting fluid usually does not flow through the reactor uniformly. Rather, there
may be sections in the packed bed that offer little resistance to flow, and as a result
a major portion of the fluid may channel through this pathway. Consequently, the
molecules following this pathway do not spend as much time in the reactor as
those flowing through the regions of high resistance to flow. We see that there is a
distribution of times that molecules spend in the reactor in contact with the
catalyst.

Figure. Packed-bed reactor.

RTD in Batch and Plug-Flow reactors
The RTDs in plug-flow reactors and ideal batch reactors are the simplest to
consider. All the atoms leaving such reactors have spent precisely the same amount
of time within the reactors. The distribution function in such a case is a spike of
infinite height and zero width, whose area is equal to 1; the spike occurs at t = V/ν,

47
or Θ = 1. Mathematically, this spike is represented by the Dirac delta function:
𝐸(𝑡) = 𝛿 (𝑡 − 𝜏)
The Dirac delta function has the following properties:
0 𝑤ℎ𝑒𝑛 𝑥 ≠ 0
𝛿(𝑥) = {
∞ 𝑤ℎ𝑒𝑛 𝑥 = 0
∞
∫ 𝛿(𝑥)𝑑𝑥 = 1
−∞
∞
∫ 𝑔(𝑥)𝛿(𝑥 − 𝜏)𝑑𝑥 = 𝑔(𝜏)
−∞

To calculate τ the mean residence time, we get g(x) = t

∞ ∞
𝑡𝑚 = ∫ 𝑡𝐸(𝑡)𝑑𝑡 = ∫ 𝑡𝛿(𝑡 − 𝜏)𝑑𝑡 = 𝜏
0 0

But we already knew this result. To calculate the variance we set, g(t) = (t – τ)2,
and the variance σ2, is
∞
𝜎 = ∫ (𝑡 − 𝜏)2 𝛿(𝑡 − 𝜏)𝑑𝑡 = 0
2
0

All material spends exactly a time τ in the reactor, there is no variance.

The cumulative distribution function F(t) is
𝑡 𝑡
𝐹(𝑡) = ∫ 𝐸(𝑡)𝑑𝑡 = ∫ 𝛿(𝑡 − 𝜏)𝑑𝑡
0 0

The E(t) function is shown in figure (a), and F(t) is shown in figure (b).

48
Figure. Ideal plug-flow response to a pulse tracer input.
RTD in CSTR
In an ideal CSTR the concentration of any substance in the effluent stream is
identical to the concentration throughout the reactor. Consequently, it is possible to
obtain the RTD from conceptual considerations in a fairly straightforward manner.
A material balance on an inert tracer that has been injected as a pulse at time t = 0
into a CSTR yields for t >0
In – Out = Accumulation
𝑑𝐶
0 – νC = V
𝑑𝑡

Because the reactor is perfectly mixed, C in this equation is the concentration of

the tracer either in the effluent or within the reactor. Separating the variable sand
integrating with C = C0 at t = 0 yields
𝐶(𝑡) = 𝐶0 𝑒 −𝑡⁄𝜏
This relationship gives the concentration of tracer in the effluent at any time t.
To find E(t) for an ideal CSTR,
𝐶(𝑡) 𝐶0 𝑒 −𝑡⁄𝜏
𝑒 −𝑡⁄𝜏
𝐸(𝑡) = ∞ = ∞ =
∫0 𝐶(𝑡)𝑑𝑡 ∫0 𝐶0 𝑒 −𝑡⁄𝜏 𝑑𝑡 𝜏

49
Evaluating the integral in the denominator completes the derivation of the RTD for
an ideal CSTR given by Equations,
𝑒 −𝑡 ⁄𝜏
𝐸(𝑡) =
𝜏
𝐸(𝛩) = 𝑒 −𝛩
Recall Θ = t/τ and E(Θ) = τE(t).

Figure. E(Θ) and F(Θ) for an Ideal CSTR.

The cumulative distribution F(Θ) is
𝛩
𝐹(𝛩) = ∫ 𝐸(𝛩) 𝑑(𝛩) = 1 − 𝑒 −𝛩
0

The E(Θ) and F(Θ) functions for an Ideal CSTR respectively.

Earlier it was shown that for a constant volumetric flow rate, the mean residence
time in a reactor is equal to V/ν, or τ. This relationship can be shown in a simpler
fashion for the CSTR. Applying the definition of the mean residence time to the
RTD for a CSTR, we obtain
∞ ∞
1 −𝑡⁄𝜏
𝑡𝑚 = ∫ 𝑡𝐸(𝑡)𝑑𝑡 = ∫ 𝑒 𝑑𝑡 = 𝜏
0 0 𝜏
Thus, the nominal holding time (space time) τ = V/ is also the mean residence time
that the material spends in the reactor.
The second moment about the mean is a measure of the spread of the distribution
about the mean. The variance of residence times in a perfectly mixed tank reactor

50
is (let x = t/τ)
∞ ∞
2
(𝑡 − 𝜏)2 −𝑡⁄𝜏
𝜎 = ∫ 𝑒 𝑑𝑡 = 𝜏 ∫ (𝑥 − 1)2 𝑒 −𝑥 𝑑𝑥 = 𝜏 2
2
0 𝜏 0

Then σ = τ. The standard deviation is the square root of the variance. For a CSTR,
the standard deviation of the residence-time distribution is as large as the mean
itself!!

UTILITIES REQUIRED
1. Compressed air supply at 2 Bar,0.25CFM
2. Water Supply
3. Drain
4. Laboratory Glassware

CHEMICALS REQUIRED
5. 1N NaOH
6. N/20 HCl
7. Phenolphthalein indicator

EXPERIMENTAL PROCEDURE
• Fill the feed tank with water and connect compressed air line to the
apparatus.
• Place the syringe containing known amount of 1N NaOH at Tracer inlet
• Start the supply of water to the reactor at particular flow rate with the help of
rotameter
• Allow water to flow through the PFTR and attain steady state.
• Inject 1N NaOH into the system as a pulse signal from the tracer inlet.

51
 • At regular time intervals (say 1 minute), collect the samples at the outlet in
pre-marked beakers/measuring cylinders (about 20ml) until all tracer leaves
the vessel.
• Analyze these samples with N/20 HCl using phenolphthalein as indicator.
• Repeat the experiment for different flow rates.

SPECIFICATIONS
Reactor : Material stainless steel, capacity 0.7 Ltrs.
(Approx) (helical coiled tube type)
Feed Tank : Material stainless steel, capacity 20 Ltrs.
Feed Circulation : By compressed air
Flow measurement : Rotameter
Piping : Material stainless steel and PVC
Pressure Regulator : 0-2 Kg/cm2
Pressure Gauge : Bourdon type 0-2 Kg/cm2
Stop watch : Electronic
The whole unit is assembled rigidly on a base plate and mounted on a stand.
Most of the parts are powder coated and rest are painted with auto paints.

FORMULAE
1. Concentration of NaOH in sample,
𝑁1 𝑉1 40
Ci = × 𝑔𝑚/𝑚𝑙
𝑉2 1000

2. Experimental mean residence time,

∑ 𝐶 𝑡𝑖
τ= ∑ 𝑖
𝐶𝑖

52
 3. Theoretical mean residence time,
𝑉𝑅
τt=
𝑉𝑜

4. σθ2 = 2 (D/UL) - 2(D/UL)2(1- e UL/D)

OBSERVATIONS AND CALCULATIONS

For calculating the concentration of NaOH in the exit stream, take 10 ml of the
solution in titration flask. Add 2-3 drops of phenolphthalein and titrate against
N/20 HCl (taken in a burette).The end point is light pink.
Let the volume of N/20 HCl used = V1
Normality of N/20 HCl used = N1
Volume of sample taken = V2
V1N1 = V2N2
[V1 (N/20)] HCl = (10X N2) NaOH
Normality of NaOH in the solution, N2 = V1/200-gram eq/L
Concentration of NaOH = [(V1/200) X40.0] gram eq/L
Concentration of NaOH at exit = 0.2 V1 gm eq/L

Time Volume of Conc. Of ti X Ci t i2 X Ci

min N/20 HCl NaOH
used per 10ml gm/L, Ci
of Solution

𝛴Ci= 𝛴 ti X Ci= 𝛴 t i2 X Ci=

𝛴Ci =

53
𝛴 ti X Ci =
𝛴 ti2 X Ci =
τ = [𝛴 ti2Ci X 𝛴Ci]
σ2 = [𝛴 ti2Ci X 𝛴Ci] – τ2
σθ2 = σ2 / τ2
using the dispersion model:
σθ2 = 2 (D/UL) - 2(D/UL)2(1- e UL/D)
For an initial trial method, neglect the second term on RHS
2(D/UL) = σθ2
By hit and trial method (improve upon the previous values exact values of D/UL
is:
The dispersion number D/UL =
Theoretical mean residence time is
τt = VR/Vo, (L/LPM) → min
Calculate the experimental mean residence time is
τ = 𝛴 t E Δt = τ = [𝛴 tiCi X 𝛴Ci]
Compare τt and τ and discuss your results
To plot RTD curve (E curve)
Time Ci, gm/L Ei= 𝛴Ci θ= t/ τ Eθ = τ Ei
min Δt

Plot E curve, θ vs Eθ

54
NOMENCLATURE
θ = reduced time
E = activation energy
τ = Experimental mean residence time
τt = theoretical mean residence time
σθ = variance at time, θ
t = time
V1 = volume of N/10 NaOH
VR = Volume of reactor
Vo = Volumetric flow rate
D/UL = dispersion number

PRECAUTIONS AND MAINTENANCE INSTRUCTIONS

• Always use clean water, good quality chemicals and standard solutions
for titration.
• Keep close all the drain valves. Vent valve should open while filling the
water in feed tank
• Air pressure should not more than 1 Kg/cm2
• Flow should not be disturbed during the experiments
• Handle the chemicals carefully
• If any types of suspended particles are in the rotameter, stop the flow, the
drain the water tank and reactor. Fill the tank with clean water after
proper cleaning of feed tank and reactor.

55
 EXPERIMENT NO. 7: SIMPLE DISTILLATION

AIM:
To verify ‘Rayleigh Equation’ by conducting simple distillation of given binary
mixture (Ethanol + Water)
THEORY: Simple distillation is a process in which a binary mixture is distilled
batch-wise without giving any reflux. It is also known as differential distillation
because the composition of the liquid in the distillation still changes with time.
The liquid is heated slowly and the vapors are withdrawn as rapidly as they are
formed into a condenser, where the distillate is collected. The vapors which
form as soon as vaporization begins will be richest in the more volatile
component. Eventually, the vapors become leaner in more volatile component.

𝑋𝐹
𝐹 𝑑𝑋
ln ( ) = ∫
𝑊 𝑌−𝑋
𝑋𝑊

Where F = original moles charged

W = moles left in the still

xF = original composition &

x W = final composition of liquid

y* = composition of the component in vapor phase in equilibrium with the

liquid.

56
The above equation is known as Rayleigh equation. The integration part of
the equation is obtained graphically by plotting 1/(y* – x) versus x.

PREPARING CALIBRATION CHART:

Use the data from the experiment No: 01

EXPERIMENTAL PROCEDURE

1. Fill the Round bottom (RB) flask with known volumes of water and

ethanol (100 ml + 100 ml). Allow running water to flow through the
condenser.
2. Heat the still at a low heating rate till 2/3 of the liquid is distilled.

3. Cool the distillate and residue to room temperature and determine their

refractive indices and volume.

4. Using calibration chart note down the mole fractions of distillate and

residue ( xD ).

5. Plot 1/(y* – x) versus x by using equilibrium data given. (See last page)

6. Determine area under the curve between x w and xf which gives the RHS

part of the Rayleigh equation.

OBSERVATIONS AND CALCULATIONS

Weight of empty sp. gravity bottle, W1 = gm

Weight of empty sp. gravity bottle + water, W2 = gm

Weight of sp.gr. bottle + ethanol, W3 = gm

57
 O
Room temperature, TR = C
Density of water at TR =w = gm/cc

Density of ethanol at TR = ρe = gm/cc

Moles of feed, F = (VA * e )/MA + (VB *

w)/MB

MA and MB are molecular weight of methanol and water respectively

VA and VB are volume of ethanol and water added in the still.
Mole fraction of ethanol in the feed

𝑉𝐴 𝜌𝑔 /𝑀𝐴
𝑥𝑓 =
𝑉𝐴 𝜌𝑔
( 𝑀 ) + (𝑉𝐵 𝜌𝑊 )/𝑀𝐵
𝐴

Refractive index of ethanol = e =

Refractive index of water = w = Weight of a beaker = W4 = gm

Weight of a beaker + distillate W5 = gm

Volume of Distillate = VD = cc
Density of distillate = D = [(W5 – W1) / (W2 – W1)] * w, gm/cc
Mole fraction of distillate, xD = (from calibration chart)
Average molecular wt. of distillate, MD = x D MA + (1- xD ) MB

Moles of distillate, D = (VD * D)/MD = gm

moles Weight of a beaker + Residue W6 = gm
Volume of Residue = Vr = cc

Density of distillate = r = [(W6 – W1) / (W2 – 1)] *

58
w, gm/cc Mole fraction of residue, xW = (from

calibration chart)

Moles of Residue, W = F – D = ______ gm

moles

𝑋𝐹
𝑑𝑋
𝑟ℎ𝑠 = ∫
𝑋𝑊 𝑌−𝑋

59
EQUILIBRIUM DATA

x y* 1/(y* – x)
0 0
0.019 0.17
0.0721 0.3891
0.0966 0.4375
0.1238 0.4704
0.1661 0.5089
0.2337 0.5445
0.2608 0.558
0.3273 0.5826
0.3965 0.6122
0.5079 0.6564
0.5198 0.6599
0.5732 0.6841
0.6763 0.7385
0.7472 0.7815
0.8943 0.8943

RESULT

Plot the graph between 1/(y* – x) versus x and find the area under the curve
between x F to x W

60
EXPERIMENT NO. 8: ADSORPTION STUDIES

AIM
To Verify the Freundlich Equation by an adsorbing acetic acid on
activated carbon from an acetic acid solution and estimation of the
constants of the equation.
APPARATUS

Five stoppered bottles, conical flask, burette with stand, funnel,

pipette, measuring Jar.
CHEMICALS REQUIRED

Standard solution of Oxalic acid, Sodium hydroxide solution, acetic acid,

activated Charcoal and Phenolphthalein indicator.
THEORY

Freundlich adsorption isotherm:- ( for dilute solutions )

At a given temperature, the mass of a solute adsorbed by a solid

adsorbent at various amounts are given by the following empirical
relation.
C* = K [V(C0 – C* ) ] n

Where C0 = initial concentration of acetic

acid solution C* = equilibrium
concentration after adsorption V =
Volume of given solution / mass of
solid
K, n are constants at a given temperature for a given solute and
adsorbent.

61
 PROCEDURE

1. Prepare exactly 0.1 N Oxalic acid solution.

2. Take 5 reagent bottles and label them 1 to 5.

3. Weight separately and accurately 0.5, 1, 1.5, 2, 2.5 gm of activated

carbon and transfer it in to 5 reagent bottles in the same order.

4. Prepare solution of 0.1 N HCl and 0.1 N NaOH solutions.

5. Verify the Normality of NaOH by taking 10 ml of standard

Oxalic solution and titrating against it.

6. From this NaOH solution, find exactly the normality of HCl solution by

titration.

7. Carefully measure and transfer 50 ml of acetic acid solution of

known concentration (0.1N) to each reagent bottle.

8. Close the lids and keep the bottles in a shaker. Switch on the shaker

and operate it for about 30 minutes.

9. At which time the equilibrium is expected to reach between the

liquid and solid phases.

10. Remove the bottles from the shaker, filter the contents of each

bottle and collect the clear solution in to 5 separate 250ml conical

flasks also numbered 1 to 5.
11. From each of these solutions take 10 ml with pipette and titrate

against the previously standardized NaOH solution using

phenolphthalein indicator.

STANDARDISATION OF 1N NaOH:

62
Standard solution of Oxalic acid (1N) was prepared by dissolving 6.3g of
Oxalic acid in 100ml of water.
Wash 50ml burette and rinse with 1N NaOH. Pipette out 10ml of std. Oxalic
acid into conical flask and titrate it with NaOH in burette using
phenolphthalein indicator. The end point has been reached when the pale pink
color of the phenolphthalein persists for 30 seconds. There should be a one-
drop difference between when the solution is colourless and when it is pink. If
too much NaOH is added (that is, if you "over-shoot" the endpoint), discard the
solution and repeat the titration. A white piece of paper placed under the flask
will aid in the color detection.
Sl. No. Volume of Sodium Burette reading Volume of
hydroxide (ml) Oxalic
Initial Final
acid, (ml)

STANDARDISATION OF 1N HCl:

Wash 50ml burette and rinse with 1N NaOH. Pipette out 10ml of HCl into
conical flask and titrate it with NaOH in burette using phenolphthalein
indicator. The end point has been reached when a very light pink color persists
for at least 30 seconds.

Sl. No. Volume of Sodium Burette reading Volume of HCl,

hydroxide (ml) (ml)
Initial Final

63
SAMPLE CALCULATION

Normality of initial acetic acid, N0 = 0.1 N

Normality of the bottle 1 filtrate, N1 = (Normality of NaOH x burette reading) /

10

N = Initial concentration of Acetic acid

C0 = N0 x equivalent weight of acetic

acid, Equilibrium concentrations of
filtrate after adsorption, C1* = N1 x
equivalent weight of acetic acid,
Kg acid / m3 solution

Weight of Volume
adsorbent of 0.1 N V, C* , V( C0 log[V (C0-
Bottle gm acetic Kg / m3 log C* – C*)]
m3/ Kg
No. acid, ml
C*)

1 0.5 50
2 1 50
3 1.5 50
4 2.0 50
5 2.5 50

GRAPH

The Freundlich adsorption isotherm over the small

concentration range is C* = K [ V( C0 – C* ) ] n
Log C* = Log K + n Log [ V( C0 – C* ) ]

64
Plot a graph between Log C* Vs Log [V (C0-C*)]. A straight line is drawn
fitting all the five points. Calculate the slope (n) and intercept (log K).

RESULT

1. A straight line obtained in the plot shows the validity of the Freundlich

adsorption isotherm over the concentration range studied.

2. The values of n and K are &

65
EXPERIMENT NO. 9: STUDY OF PROPORTIONAL (P) CONTROLLER
USING COMPUTER-CONTROLLED LEVEL TRAINER

AIM: To study the effect of proportional band (PB) on the response of the given
level system
OUTCOMES: After completing this experiment students are expected to know
▪ basic feedback control configuration using P-controller
▪ concept of PB or proportional gain and its effect on output
▪ hardware involve in direct digital control (DDC) system

EQUIPMENT: Level control trainer (DDC type)

THEORY:
An automatic control is essential in industrial operations for controlling pressure,
temperature, liquid level, concentration humidity, viscosity, and flow in the
process industries. Feedback control systems represent the control schemes
encountered most often in a chemical plant. Fig.1 represents a schematic of basic
feedback loop in which feedback is taken from output and fed in to input. It comes
between the measuring device and the final control element and generates
actuating signal, CO using error signal e(t) as input. There are three basic types of
feedback controllers
i. Proportional (P controller)
ii. Proportional- Integral (PI controller)
iii. Proportional- Integral -Derivative (PID controller)

Actuating output of P- controller is proportional to current error e (t):

𝐶𝑂(𝑡) = 𝐾𝑐 𝑒(𝑡) + 𝐶𝑠
and

66
 𝐺𝐶 (𝑠) = 𝐾𝑐
where KC = proportional gain of the controller and Cs = controller's bias signal
(i.e., its actuating signal when e = 0). If the error value is zero, then this
controller output is zero.

Fig. 1 Schematic of Basic Feedback Control Loop

A proportional controller is described by the value of its proportional gain K c, or

equivalently by its proportional band PB, where PB = 100/K c; The proportional
band characterizes the range over which the error must change in order to drive the
actuating signal of the controller over its full range. The larger the gain K c or
equivalently, the smaller the PB value, the higher the sensitivity of controller's
actuating signal to deviations e(t) will be.
This controller requires biasing or manual reset when used alone. This is because it
never reaches the steady state condition. It provides stable operation but always
maintains the steady state error between the process variable and set point, called
‘offset’. It is defined as the ultimate response, after t → ∞ , never reaches the
desired new set point. There is always a discrepancy called offset:
Offset = (new set point) - (ultimate value of the response)

67
The offset is characteristic effect of P-controller (see Fig. 2). It decreases as KC
becomes larger and theoretically: Offset → 0 when PB → 0
Speed of the response is increased when the proportional constant K c increases.
However, we will never use extremely large values of Kc (why?)

Fig. 2 Unit-step response for set point change

Description of Setup:
The role of the level controller is to determine the desired control action by sensing
the level of water column in the process tank with the help of a level transmitter by
producing current in the range of 4 to 20 mA. As per the desired level to be
attained in the process tank, a pneumatic control valve is opened or closed
(manipulated) by an I/P controller to minimize any error to maintain a steady level
in the process tank with the help of supervisory control and data acquisition
(SCADA) system.
The process setup consists (see Fig. 3 and 4) of supply water tank fitted with
centrifugal pump for water circulation. The rate of flow is regulated by the
pneumatic control valve. A level transmitter used for level sensing produces
current in the range of 4 to 20 mA proportional to the height of water column in the
water tank. The difference in desired level and current water level is computed.
Based on this information the controller determines the desired water level. The
process parameter (level) is controlled by microprocessor based digital indicating

68
controller which manipulates pneumatic control valve through I/P converter.

Specification:
▪ Level Transmitter: Type electronic, two wire, range 0-250 mm, output 4-
20 mA
▪ I/P converter: Input 4-20 mA, output 3-15 psig
▪ Control valve: Pneumatic (Air to close); Size: ¼ inch; Input: 3-15 psig
▪ Valve Characteristics: Linear
▪ Rotameter: 10-100 LPH
▪ Pump: Type submersible
▪ Process tank: Transparent, MOC: Acrylic, with 0-100 % graduated scale
▪ Air filter regulator: Range 0-2.5 kg/cm2

Fig. 3 A Schematic of the Level Control Trainer

69
Fig. 4 (a) Front View and (b) Back View of the Setup

PROCEDURE:
▪ Fill supply tank with distilled water and keep the pump inside the water.
▪ Switch on electric supply. Switch on Mains.
▪ Switch on the pump and ensure that flow through rotameter is above 100
LPH.
▪ Adjust the tank drain valve such that the tank level remains between 90 and
100%
▪ Confirm the reading on digital indicating controller is within ± 2%.
▪ Switch on the compressed air source and adjust the air regulator to set
supply air pressure at 2 kg/cm2

▪ Set the controller to manual mode by pressing the A/M key.

▪ Increase output of controller from 0 to 100% in steps of 25%. Check the
pressure on pressure gauge at the output of I/P converter is varying from 3-
15 psig and ensure that control valve operates from full open to fully close
position.

70
Start-up of software:
• Click on Start|All programs|Wonderware|InTouch|Yes to open InTouch
Application manager.
• Open “Level Control Trainer” under InTouch Application Manager
• Click “Ignore” under “WindowMaker” for License not available
• Click “Select All” and “OK” under “Windows to Open”
• Click on “Runtime” at Top Right corner under “Intouch- WindowMaker”
• Click “Ignore” under “WindowViewer” for License not available
• Click “OK” under “ WindowViewer” for Demo mode

FOR STUDY OF P-CONTROLLER

▪ Select P Mode option for control from software. (click on “Change Expt.”
Button, click on “Change”, Click on “P Mode” button.)
▪ Adjust the process value by switching the controller to manual mode to a
particular level (say 50 %) on the screen and apply output of the controller
as bias value. Change the proportional band to 100%. Switch the controller
to auto mode.
▪ Apply step change of 10% to set point.
▪ Switch the controller to manual mode. Decrease proportional band to half of
the previous value. With each decrease, obtain a new response of the step
change.
▪ Ensure that the set point changes are around the same operating point (say
50%).

71
OBSERVATIONS:

• From the data file stored observe the output response of the process and note
down the output and plot the response

• Observe the effect of proportional band values

CALCULATIONS:

Plot PV vs time for various PB values

Sl. Value of PB Offset amount

No.
1.
2.
.
.

Offset =

RESULTS:
Report the effect of proportional band values
Discuss the characteristics of the closed-loop response of the process.

72
QUESTIONS:
i. Define proportional band (PB) of a P-controller. Explain its physical
significance.
ii. What are the relative advantages and disadvantages of the proportional
control actions? What are its characteristic effects on the closed-loop
response of a process?
iii. Where can we use a P-controller in process industries?
iv. What are the weaknesses of a P-controller?

73
EXPERIMENT NO. 10: STUDY OF PROPORTIONAL INTEGRAL (PI)
CONTROLLER USING COMPUTER-CONTROLLED FLOW TRAINER

AIM: To study the effect of integral time on the response of the given process flow
system

OUTCOMES: After completing this experiment students are expected to know

▪ basic feedback control mechanism using PI-controller
▪ concept of integral time and its effect on response
▪ hardware involve in direct digital control (DDC) system

EQUIPMENT: Flow control trainer (a direct digital controller)

THEORY:
Feedback control systems represent the control schemes encountered most often in
a chemical process plant. Fig.1 represents a schematic of a basic feedback loop in
which feedback is taken from output and fed in to input. It comes between the
measuring device and the final control element and generates actuating signal, CO
using error signal e(t) as input. There are three basic types of feedback controllers
i. Proportional (P controller)
ii. Proportional- Integral (PI controller)
iii. Proportional- Integral -Derivative (PID controller)

Actuating output of PI- controller is proportional to current error e (t):

𝐾𝑐 𝑡
𝐶𝑂(𝑡) = 𝐾𝑐 𝑒(𝑡) + ∫ 𝑒(𝑡) 𝑑𝑡 + 𝐶𝑠
𝜏𝐼 0
and

74
 1
𝐺𝐶 (𝑠) = 𝐾𝑐 (1 + )
𝜏𝐼 𝑠
where KC = proportional gain of the controller, I = is the integral time constant
or reset time in minutes, and Cs = controller's bias signal (i.e., its actuating
signal when e = 0). Here,

the reset time is an adjustable parameter and is sometimes referred to as minutes

per repeat. The integral control action has "repeated" the response of the
proportional action. This repetition takes place every I minutes.

Fig. 1 Schematic of Basic Feedback Control Loop

The integral action causes the controller output CO(t) to change as long as a
non-zero error exists in the process output. Therefore, such a controller can
eliminate even small errors or offset but it can cause the response to become
more oscillatory to set point changes. The qualitative effects of changing
individual controller settings are shown in Fig.2.

75
 (a)

Fig.2. Proportional-integral control: (a) effect of integral time, (b)

effect of controller gain
Description of Setup:
The role of the level controller is to determine the desired control action by sensing
the level of water column in the process tank with the help of a level transmitter by
producing current in the range of 4 to 20 mA. As per the desired level to be
attained in the process tank, a pneumatic control valve is opened or closed
(manipulated) by an I/P controller to minimize any error to maintain a steady level
in the process tank with the help of supervisory control and data acquisition
(SCADA) system.
The process setup (see Fig. 3 and 4) consists of supply water tank fitted with
centrifugal pump for water circulation. The rate of flow is regulated by the
pneumatic control valve. A level transmitter used for level sensing produces
current in the range of 4 to 20 mA proportional to the height of water column in the
water tank. The difference in desired level and current water level is computed.
Based on this information the controller determines the desired water level. The
process parameter (level) is controlled by microprocessor based digital indicating
controller which manipulates pneumatic control valve through I/P converter.

76
Specification:
• Differential pressure transmitter: Type capacitance, two wire, range 0-
200mm, output 4-20 mA sq. root.
• I/P converter: Input 4-20 mA, output 3-15 psig
• Control Valve: Pneumatic type, Size: ¼ inch, Input: 3-15 psig; Air to
close; Characteristics: Linear
• Rotameter: 10-100 LPH
• Pump: Fractional horse power, type submersible
• Supply Tank: SS304
• Flow Measurement: Orifice meter
• Air filter regulator: range 0-2.5 kg/cm2
• Pressure gauge: range 0-2.5 kg/cm2, range 0-7 kg/cm2

Fig. 3. A Schematic of the Flow Control Trainer

77
 Fig. 4 (a) Front View and (b) Back View of the Setup

PROCEDURE:
▪ Fill supply tank with distilled water and keep the pump inside the water.
▪ Switch on electric supply. Switch on Mains.
▪ Switch on the pump and ensure that flow through rotameter is above 100
LPH.

▪ Confirm that flow signal reading is displayed at controller (For 100 LPH
flow the reading should be @100%. If not, remove air from the pressure
signal connections of Flow transmitter by loosening vent plugs provided on
it).

▪ Ensure that air regulator is fully open by rotating anticlockwise. Switch on

the compressed air source and adjust the Air regulator to set supply air
pressure at 25 psig.

▪ Set the controller to manual mode by pressing the A/M key.

78
 ▪ Increase output of controller from 0 to 100% in steps of 25%. Check the
pressure on pressure gauge at the output of I/P converter is varying from 3-
15 psig and ensure that Control valve operates from full open to fully close
position.

▪ Switch on the computer and execute the software.

START-UP OF SOFTWARE:
• Click on Start|All programs|Wonderware|InTouch|Yes to open InTouch
Application manager.
• Open “Flow Control Trainer” under InTouch Application Manager
• Click “Ignore” under “WindowMaker” for License not available
• Click “Select All” and “OK” under “Windows to Open”
• Click on “Runtime” at Top Right corner under “Intouch- WindowMaker”
• Click “Ignore” under “WindowViewer” for License not available
• Click “OK” under “ WindowViewer” for Demo mode

FOR STUDY OF PI-CONTROLLER

▪ Select PI Mode option for control from software. (click on “Change Expt.”
Button, click on “Change”, Click on “PI Mode” button.)
▪ Select PID controller. Set the proportional band. Set derivative time to 0 sec
and integral time 6000 sec, which will cut off the derivative action and
widen the effect of integral action.

▪ Set the set point to desired flow value (@70%). Allow the process to reach
at steady state. Record the steady state error.

79
 ▪ Switch the controller to manual mode. Reduce the integral time to half of the
previous value. Switch to Auto mode and apply step change (+/- 10%) to the
set point. Note the response of the system.

▪ Repeat above step to observe the effect of changes in Integral setting.

OBSERVATIONS:

• From the data file stored observe the output response of the process and note
down the output and plot the response
• Observe the effect of reducing integral time on offset and on the response of
the process.

CALCULATIONS:

Plot PV vs time for various I

Sl. Value Value Offset Oscillation/Overshoot Rise Time

No. of PB of I amount,
if any
Increase/decrease Faster/slower/no
effect
Increase/decrease Faster/slower/no
effect
Increase/decrease Faster/slower/no
effect

80
RESULTS:
Report the effect of integral time values for a fixed PB value.
Discuss the characteristics of the closed-loop response of the process.

QUESTIONS:

i. What is the transfer function of a PI- controller?

ii. Define reset time and reset rate, and explain their importance.
iii. What are the relative advantages and disadvantages of the integral control
actions? What are its characteristic effects on the closed-loop response of a
process?
iv. Where can we use a PI-controller in process industries?

81
EXPERIMENT NO. 11: STUDY OF PROPORTIONAL-INTEGRAL-
DERIVATIVE (PID) CONTROLLER USING COMPUTER-CONTROLLED
TEMPERATURE TRAINER

AIM: To study the effect of derivative time on the response of the given process
system

OUTCOMES: After completing this experiment students are expected to know

▪ basic feedback control configuration using PID controller
▪ concept of various feedback parameters and their effect on output
▪ hardware involve in direct digital control (DDC) system

EQUIPMENT: Temperature control trainer (DDC type)

THEORY:
Feedback control systems can be designed to achieve specific behavior of the
output variable, for example (i) to keep the output variable within a tightly
constrained range, irrespective of changes in the environment, and (iii) to reduce
the influence of process changes, etc. It allows a system dynamic response to be
modified without changing any system components. Fig.1 represents a schematic
of a basic feedback loop in which feedback is taken from output and fed into input.
It comes between the measuring device and the final control element and generates
actuating signal, CO using error signal e(t) as input. There are three basic types of
feedback controllers:
i. Proportional (P controller)
ii. Proportional- Integral (PI controller)
iii. Proportional- Integral -Derivative (PID controller)

82
The PID controller is by far the most common control algorithm. With the
presence of the derivative term, a PID controller anticipates what the error will be
in the immediate future and applies a control action which is proportional to the
current rate of change in the error.

Actuating output of PID- controller is related to current error e (t) as:

𝐾𝑐 𝑡 𝑑𝑒(𝑡)
𝐶𝑂(𝑡) = 𝐾𝑐 𝑒(𝑡) + ∫ 𝑒(𝑡) 𝑑𝑡 + 𝐾𝑐 𝜏𝐷 + 𝐶𝑠
𝜏𝐼 0 𝑑𝑡
and
1
𝐺𝐶 (𝑠) = 𝐾𝑐 (1 + + 𝜏𝐷 𝑠)
𝜏𝐼 𝑠
where KC is proportional gain of the controller, I is the integral time constant
or reset time in minutes, D is the derivative time and Cs is controller's bias
signal (i.e., its actuating signal when e = 0). In this case, all three values Kc , I,
and D can be adjusted in the controller.

Fig. 1 Schematic of Basic Feedback Control Loop

83
 The qualitative effects of changing proportional gain and derivative time
settings are shown in Fig.2.
(a) (b)

Fig.2. PID control: (a) effect of gain (b) effect of derivative time

Description of Setup:
Temperature control trainer (Fig. 3 & 4) is designed for understanding the basic
temperature control principles using PID controller. The process setup consists of
heating tank fitted with solid state relay (SSR) controlled heater for on-line heating
of the water. The flow of water can be manipulated and measured by rotameter.
Temperature sensor (RTD) is used for temperature sensing. The process parameter
(Temperature) is controlled by microprocessor based digital indicating controller
which manipulates heat input to the process. These units along with necessary
piping and fitting are mounted on support frame designed for tabletop mounting.
The controller can be connected to computer through ethernet port for monitoring
the process in SCADA mode.

Specification:
• Temperature sensor: Type RTD, PT100

84
 • Heating control Proportional power controller: Solid state relay (SSR),
Input 4-20 mA, Capacity 50 A.
• Heater Type: Electrical 2 coil, Capacity 3 KW
• Rotameter: 6-60 LPH
• Process tank: SS304, Capacity 0.5 lit, insulated

Fig. 3. A Schematic of the temperature control trainer

Fig. 4 (a) Front View and (b) Back View of the Setup

85
PROCEDURE:
▪ Switch on electric supply. Switch on Mains.
▪ Adjust rotameter flow rate to 40 LPH.
▪ Switch on the heater.
▪ Double click on Apex_Process_Trainers icon on the desktop
▪ Click Select Experiment, select PID mode and click Start
▪ Switch the controller to manual mode.
▪ Set the proportional band, integral time and derivative time.
▪ Change the controller to Auto mode. Apply step change by 2 to 3% to the set
point and observe the response of the process.
▪ Keeping the proportional band, PB and integral time constant, I change the
derivative time, D and observe the response of the process for step change
for each change in setting.

OBSERVATIONS:

• From the data file stored observe the output response of the process and note
down the output and plot the response
• Compare the steady state response of the PID controller for various
derivative time

86
CALCULATIONS:
Plot PV vs time for various D values
Sl. Value Value Offset Oscillation/Overshoot Rise Time
No. of PB of I amount,
if any
Increase/decrease Faster/slower/no
effect
Increase/decrease Faster/slower/no
effect
Increase/decrease Faster/slower/no
effect

RESULTS:
Plot the steady state responses of the PID controller for various derivative time but
for fixed PB and I values.

Discuss the characteristics of the closed-loop response of the process.

QUESTIONS:
i. What is the transfer function of a PID controller?
ii. Define derivative time and explain their importance.
iii. What are the relative advantages and disadvantages of the derivative
control actions? What are its characteristic effects on the closed-loop
response of a process?
iv. Discuss the effects of Kc, I and D on the closed-loop response of a
process controlled with PID.
v. Where can we use a PID-controller in process industries?

87