SAMARA UNIVERSITY

COLLEGE OF ENGINEERING & TECHNOLOGY

CHEMICAL ENGINEERING DEPARTMENT

PROCESS INDUSTRIES & CONTROL

PROCESS DYNAMICS & CONTROL, PROCESS INDUSTRIES

AUTHOR
ABDULKADER MOHAMMED AWOL

April 2023

SEMERA UNIVERSITY 1
CHEMICAL ENGINERING DEPARTMENT
 GRADUATE ATTRIBUTES AND PROGRAMME GOALS
Graduate profile is a description of attributes (knowledge, skill and attitude) which the program aspires for its
students to be attained. In line with this conceptual framework chemical engineering program has more or less
the same graduate profiles as it is drawn from three different curricula. Chemical engineering program has the
following key occupational tasks and responsibilities that should be attained by graduates.
 Involving in the plant layout, design, construction and operation of industrial plants.
 Conducting economic and technical feasibility studies of chemical and process industries,
 Modeling process, design and evaluation by using appropriate computer programs,
 Designing, testing and commissioning processes, equipment and plants.
 Managing troubleshoots and solving problems to optimize the production processes;
 Overseeing the construction, modification, operation and maintenance of pilot plants, processing units
or processing plants;
 Acting as liaison between plant engineering personnel and equipment suppliers.
 preparing tender document, bid evaluation, coordinating the industrial construction projects;
 Ensuring efficient, optimum, safe and environmentally responsible plant operation; establishing and
conducting quality control programs; operating and assessment procedures and control strategies to
ensure consistency and adhere to standards;
 Frontally work with control and instrumentation specialists, supervision of and cooperation with other
engineering personnel;
 Participating and advising industry and governmental bodies regarding environmental policies and
standards;
 Teaching undergraduate Chemical Engineering Courses and assisting advanced courses.
 Working in multidisciplinary environment as well as - especially under the conditions of globalization-
in international cooperation or business;
 Coordinating research and development activities;
 Working in sustainable energy technologies and energy optimization systems;
Generally Chemical Engineering graduates should have basic scientific, technical, ethical, communication
and leadership skills wherever they work and pursue their further study

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 MODULE AIMS
The aim of this module is to assist the students for the preparation of the exit exam for the two courses from
identified courses which are matched to the competencies and learning outcomes of the program

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SECTION I: INTRODUCTION
SECTION CONTENTS & OBJECTIVES
Section Contents
The following contents are included in this section:
 Introduction of process control
 The benefits of process control
 Process control system
 Design elements of a control system
 Process control examples
 Classification of the variable in a chemical process
 Self-Check Questions
Section Objectives
After completing this section, you will be able to:
 Define process control
 Identify the needs & importance for process control
 Analyze design questions & formulate the problems that must be solved
Introduction to process control
What does chemical process mean?
Process, as used in the terms process control and process industry, refers to the
methods of changing or refining raw materials to create products. The raw
materials, which either pass through or remain in a liquid, gaseous, or slurry
state during the process, are transferred, measured, mixed, heated or cooled,
filtered, stored, or handled in some other way to produce the end product.
What is process dynamics?
Process dynamics is a study of the transient behavior. No process operates at
a steady state, because essentially all external variables change.
Why process dynamics?
As the chemical processes proceeded, all key variables changing continuously,
sometimes with small fluctuations and other times in response to major
changes i.e. almost all chemical processes are dynamic.

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Thus, the process design must consider systems that respond to external
disturbances and maintain the process operation in a safe region that yields
high-quality products in a profitable manner. The emphasis on good operation,
achieved through proper process control systems, requires a thorough
knowledge of the dynamic operation.
What is a process control?
Process control is the use of process dynamics for the improvement of process
operation and performance or it is the use of process dynamics to alleviate the
effect of undesirable (unstable) process behaviors. Process control in process
industries refers to the regulation of all aspects of the process.
The benefits of process control
Considering all the benefits that can be realized through process control, it
is well worth the time and effort required to become familiar with the
concepts and practices used in the field.
The benefits of process control are explained as
1. Safe process/plant operation: Personnel and Equipment.
Plant operating conditions should always be within allowable limits.
Example if a reactor designed to operate at a temperature up to 100oC,
we should have a control system that will maintain the temperature
below this value.
2. Production specification: it refers to both quantity and quality of the
final products. For e.g., we may require the production of 2 million
pounds of ethylene/ day, of 99.5% purity, from an ethylene plant.
3. Environmental regulations: government laws may specify the
characteristics of the effluents from a plant be within certain limits.
Example amounts of SO2 that a plant can eject to the atmosphere and
the quality of water returned to a river or a lake.
4. Operational constraints: various types of equipments used in a
chemical plant have constraints inherent to their operation. Such
constraints should be satisfied throughout the operation of a plant.

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CHEMICAL ENGINERING DEPARTMENT
 For example, tanks should not overflow or go dry; distillation columns Self-assesment activities’
should not be flooded: the temperature/pressure in a catalytic reactor 1. What does the term process

should not exceed an upper limit since the catalyst will be destroyed. mean in process industry &

5. Economics: it should be as economic as possible in its utilization of raw process control contexts?

materials, energy, capital and human labor. Thus, it is required that the 2. Which one is the example of

operating conditions are controlled at given optimum levels of process industry

minimum operating cost, or maximum profit; etc. All the above A. Power

requirements dictate the need for process control to guarantee the B. Oil & gas

satisfaction of the operational objectives. C. Satellite

D. Sugar
Process control systems:
Control systems are used to maintain process conditions at their desired E. B & D
values by manipulating certain process variables to adjust the variables of 3. Why almost all chemical
interest. A control system is required to compensate for the influence of processes are dynamic?
external disturbances such as changes in feed flow rate, feed conditions, 4. Why we control a
product specifications, ambient temperature and so on. A control system is manufacturing process?
then designed, which responds to variations in the measured variables and A. For Safe operation
manipulates variables to control the process. B. For Better quality
Conceptually the control systems can be explained the following general C. To reduce cost &
manner (Fig. 17.2.). The controller compares the measurement signal of the maximize profit
controlled variable to the set point (the desired value of the controlled D. To meet the regulation
variable). The difference between the two values is called the error. E. All
𝐸𝑟𝑟𝑜𝑟 = (𝑆𝑒𝑡𝑝𝑜𝑖𝑛𝑡 𝑣𝑎𝑙𝑢𝑒) − (𝑀𝑒𝑎𝑠𝑢𝑟𝑒𝑚𝑒𝑛𝑡 𝑠𝑖𝑔𝑛𝑎𝑙 𝑜𝑓 𝑐𝑜𝑛𝑡𝑟𝑜𝑙𝑙𝑒𝑑 𝑣𝑎𝑟𝑖𝑎𝑏𝑙𝑒) 5. What is a process control
Depending upon the magnitude and sign of the error, the controller takes system?
appropriate action by sending a signal to the final control element, which A. system to keep the parameters
provides an input to the process to return the controlled variable to the set point at zero value
B. system to maintain the
parameters constant
C. system to keep the parameters
at highest value
D. system to check the
temperature
Figure 17.2. Generalized process control system

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The concept of using information about the deviation of the system from its 5. Select a system from daily-
desired state to control the system is called feedback control. Information life activities, and identify,
about the state of the system is “feedback” to a controller, which utilizes determine its possible control
this information to change the system in some way. The type of control objective, classify its
system shown in Fig. 17.2 is termed a closed-loop feedback control system. variables, and develop
possible control system.
Closed-loop refers to the fact that the controller automatically acts to return
6. Imagine you are in a cabin in
the controlled variable to its desired value. In contrast, an open-loop system
front of a small fire on a cold
would have the measurement signal disconnected from the controller, and
winter evening. You feel
the controller output would have to be manually adjusted to change the
uncomfortably cold, so you
value of the controlled variable. An open-loop system is sometimes said to
throw another log into the
be in manual mode as opposed to automatic mode (closed-loop). Negative
fire. In this scenario, the
feedback is the most common type of signal feedback. Negative refers to
process variable is
the fact that the error signal is computed from the difference between the
temperature.
set point and the measured signal. The negative value of the measured signal
True or false?
is “fed back” to the controller and added to the set point to compute the error
Design element of a control system
1. Define Control Objective
2. Select Measurements
3. Select manipulated variables
4. Select the Control Configuration
5. Develop a process model
6. Design the Controller
Define Control Objective
The control objectives may have to do with:
 Suppressing the influence of external disturbances: the objective might
be to regulate a key component in the plant
 Optimizing the economic performance of a plant: to minimize energy
consumption while meeting product quality specifications
 Ensuring the stability of the process (removing flooding, overflow or
go dry etc.), or combination

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Select Measurements: What variables must be measured to monitor the
performance of a chemical plant?
Select manipulated variables
The choice of appropriate manipulated variables should affect performance
of control systems significantly. In general the manipulated variables:
 Should have direct and strong effect on the controlled variables
 Be simple to adjust.
For example, flow rates can be adjusted easily with a control valve
Select the Control Configuration
It is the determination of information structure for measured and controlled
variables. For example, pairing of controlled and manipulated variables.
There are three most common types of control configurations
 Feedback/corrective:
It uses direct measurements of the controlled variables to adjust the values
of the manipulated variables.
 Its advantage is taking of corrective action regardless of the source of
the disturbance.
 Taking the corrective action after the deviation of controlled variable
from the set point considered as its disadvantage.

Figure 17.4: Feedback control system

 Negative feedback—in negative feedback, the error is the difference

between the set point and the measured variable (this is usually the
desired configuration).
 Positive feedback—in positive feedback, the measured temperature is
added to the set point. (This is usually an undesirable situation and
frequently leads to instability.)

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Feedforward/predictive: Uses direct measurements of the disturbances to
adjust the values of the manipulated variables. For example, to achieve
desired room temperature - set the hot water flow based on the measured
outside temperature and a model of the heat loss of the house.
As its advantage, if all sources of the disturbances are known and these
values can be measured accurately we can perfectly control.
Disadvantages: No corrective action for unmeasured disturbances.

Figure 17.5: Feedforward control system

Inferential: uses secondary measurements, since the controlled variables

are unmeasured, to adjust the values of the manipulated variables. The
estimator uses the values of the available measured outputs, along with the
material & energy balances that govern the process, to compute
mathematically (estimate) the values of the unmeasured controlled
variables.
Unmeasured input = f (secondary measurements)

Figure 17.6: Inferential control system

Process control examples

Process control examples from daily life activities:
1. The cruise control on an automobile. The purpose of a cruise control is
to maintain the speed of the vehicle (the controlled variable) at the
desired value (the set point) despite variations in terrain, hills, etc.
(disturbances) by adjusting the throttle, or the fuel flow to the engine
(the manipulated variable).

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2. The home hot water heater also another example. The control system on 7. Simple level control
the hot water heater attempts to maintain the temperature in the tank at Consider the process system shown
the desired value by manipulating the fuel flow to the burner (for a gas in fig.17.7. The inlet flow comes
heater) or the electrical input to the heater in the face of disturbances from an upstream process, and may
such as the varying demand on the heater early in the morning, as it is change with time. The level in the
called upon to provide water for the daily showers. tank must be kept constant in spite
A third example is the home thermostat. This control system is designed to of these changes. If the outlet flow
maintain the temperature in the home at a comfortable value by is simply set equal to the inlet flow,
manipulating the fuel flow or electrical input to the furnace. The furnace the tank may overflow or run empty
control system must deal with a variety of disturbances to maintain (b/s of flow measurement errors)
temperature in the house, such as heat losses, doors being opened and
hopefully closed, and leaky inefficient windows. The furnace must also be
able to respond to a request to raise the desired temperature if necessary.
For example, we might desire to raise the temperature by 5 oC , and we
would like the system to respond smoothly and efficiently.
Process control examples from process industries:
Simple level control
A possible control system for the liquid flow is introduced as shown in Figure 17.7. a) Liquid holding tank

figure 17.7b. The level controller (LC) looks at the level (monitoring). If the
level starts to increase, the LC sends a signal to the output valve to vary the
output flow (change). This is the essence of feedback control.

Figure 17.7. b) Liquid level control system

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Tank heater control system 8. Tank Heater System
The operation of the heater is disturbed by external factors like changes in Consider the tank heater system
the feed flowrate and temperature (Fi and Ti). If nothing changed, then after shown in Figure 17.9a. A liquid
attaining T = Ts and V=Vs, we could leave the system alone without any enters the tank with a flowrate Fi
supervision and control. It is clear though that this cannot be true since Ti (ft3/min), and a temperature Ti
and Fi are subject to frequent changes. Consequently, some form of control (oF), where it is heated with
action is needed to alleviate the impact of the changing disturbances and steam (having a flowrate Fs,
keep T and V at the desired values. lb/min). Let F and T be the
One way to accomplish the first objective is by measuring the outlet flowrate and temperature of the
temperature T, comparing it to the desired value call the set point. The outlet stream leaving the tank. The tank
temperature is the measured variable. Any deviation from the set point can is considered to be well stirred,
be corrected by adjusting the control valve to change the steam flow to the which implies that the
stirred tank heater. The steam flow rate is the manipulated variable. temperature of the effluent is
equal to the temperature of the
liquid in the tank.
Keeping the effluent
temperature, T and the volume of
the liquid in the tank, V at
desired values of Ts and Vs,
respectively, are the operational
Figure 17.9b Feedback temperature control system for tank heater

A possible control system to keep T = Ts when Ti or Fi changes in stirred objectives of this heater.

tank heater is shown in Figure 17.9b. This configuration is a basic feedback

control loop. A sensor such as a thermocouple measures the temperature T
of the liquid in the tank.
Then T is compared with the desired value Ts yielding a deviation e=Ts -T.
This sensor is usually connected to transmitter, which amplifies the output
from the sensor and sends it to a controller. The value of the deviation e is
sent to a control mechanism, which decides what must be done in order for
Figure 17.9a Stirred tank heater
the temperature T to return back to the desired value Ts. The controller
compares the signal with the set point and decides the action necessary to
maintain the desired temperature.

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The controller then sends a signal to the final control element, which is the 9. For the process described as
control valve in this case, to adjust the steam flow rate accordingly. The figure below
control valves acts as a variable resistance in the steam line since the flow
rate depends on the valve stem or plug position. To regulate flow, the flow
capacity of the control valve varies from zero when the valve is closed to a
maximum when the valve is fully opened.
This control system that measures the variable of direct importance (T in
this case) after a disturbance had its effect on it, is called feedback control
system. The desired value Ts is called the Set Point and is supplied
externally by the person in charge of production. Where:
 𝐹𝑖 , 𝐹𝑜 : Tank inlet and outlet
Classification of the variable in a chemical process
Variables associated with a chemical process are divided into two groups. mass flows
1. Input variables–denotes the effect of the surrounding on the chemical  𝑇𝑖 , 𝑇𝑜 : Tank inlet and outlet
process. temperatures
2. Output Variables –denotes the effect of the process on the surroundings.  𝐹𝑐 : cooling jacket mass
The input variables can be further classified into the following category flow
1. Manipulative (adjustable) variable-If there, valves can adjusted freely  𝑇𝑐𝑖 , 𝑇𝑐𝑜 : cooling jacket inlet
by the human operator or control mechanism. and outlet temperatures
2. Disturbances- If there, values are not the result of adjustment by an  ℎ: Tank liquid level
operator or a control system.
Identify & classify the
The output variables are also classified as
variables
1. Measured: If there, values are known by directly measuring them.
2. Unmeasured: If they are not or cannot be measured directly.
According to their measurability the disturbance are 1) measured, 2)
Unmeasured disturbance

Figure- process variables

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 Self-Check Questions
1. If the level of a liquid in a tank must be maintained within 5m of 50m, what
is the liquid’s set point?
A. 45m
B. 55m
C. 5m
D. 50m
2. ____________________ is a sustained deviation of the process variable
from the set point.
3. A load disturbance is an undesired change in one of the factors that can
affect the setpoint. True or false?
4. Automatic control systems are control operations that involve human action
to make adjustment. True/ false?
5. What is the position of the valve if e =0, e > 0, e < 0
A. The controller opens the valve
B. The controller closes the valve
C. the controller does nothing
D. All
6. For proper feedback in a process control element, it is required to
measure________
A. set point
B. control variable
C. comparator
D. error
7. In feedback control, the measurement is taken only from output parameters.
True/ False
8. A process variable is a condition that can change the process in some way
True/False
9. Measurement, comparison & adjustment are the three tasks associated with
any control loop. True/False

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10. Under what circumstances does an open control loop exist? Select all
options that apply.
A. Process variable is not measured
B. Process variable is not compared
C. Process variable is measured and compared to a setpoint
D. Action is taken without regard to process variable conditions
E. Action is taken with regard to process variable conditions
11. What type of control configuration takes action in response to measured
deviation from setpoint?
Feedback/ Feedforward control configuration
12. What type of control configuration anticipates and controls load
disturbances before they can impact the process variable?
Feedback control configuration/ Feedforward control configuration

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SECTION II: DEVELOP A DYNAMIC MODEL
SECTION CONTENTS & OBJECTIVES
Section Contents
The following contents are included in this section:
 Introduction
 A Systematic approach for model development
 Degrees of freedom analysis
Section Objectives
After completing this section, you will be able to:
 Introduced modeling requirements for process control
 Construct useful models
Introduction
Motivation for Process Modeling
Develop understanding of process
 a mathematical hypothesis of process mechanisms
Match observed process behavior
 useful in design, optimization and control of process
Why dynamic modeling?
In order to control a chemical process first we need to understand the
process behavior. Therefore, a dynamic modeling is required for
understanding of process behavior. The knowledge of dynamic behavior is
formalized in dynamic model (mathematical models). Dynamic modeling,
investigates the process response to various input changes with time. For
process control problems, dynamic models are derived using unsteady-state
conservation laws. Dynamic models of chemical processes consist of
ordinary differential equations (ODE) and/or partial differential equations
(PDE), plus related algebraic equation. We will consider only two classes
of dynamic process models state-space models AND input- output models
State-space models can be derived directly from the general conservation
equation:
Accumulation = (Inlet – Outlet) + (Generation – Consumption)

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Written in terms of differential equations relating process states to time.
They occur in the “time domain”
Input-output models completely disregard the process states. They only give
a relationship between process inputs and process outputs.
They occur in the “Laplace domain”

What kind of model do we need?

Models can be classified based on how they are obtained
Experimental vs Theoretical
Experimental
 No process or other data required (theoretically)
 More complex but provides understanding
 In principle excellent extrapolation (scale-up) properties
 Can predict new phenomena (in principle)
 To design the control system before the process has been constructed
It is usually given in terms of a set of mathematical equations (differential,
algebraic) whose solution yields the dynamic or static behavior of the
chemical process
Theoretical
 based on actual/observed input and output variables
 Simpler model form
 Some parameters (coefficients) are identified based on observed
variables. These coefficients typically have no physical meaning
Easier to manipulate and it is time and effort consuming

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Dynamic vs Steady state
Dynamic:
 Process variables are a function of time.
 Control requires dynamic model
 involve ordinary differential equations
Steady state:
 process variables are not a function of time
 useful for design calculation
 involve algebraic equations
Lumped vs Distributed
Lumped:
 (Almost) perfect mixing
 Characterized by a single independent variable (time)
 a system properties do not depend on the position within the system
 steady-state models involve algebraic equations, and dynamic models
involve ordinary differential equations
Distributed
 Imperfect mixing will result in different operating conditions at
different points even at the same time
 existence of distributions of conditions over spatial domains
 the properties depend on position
 Involves partial differential equations
Linear vs Nonlinear
Linear
 basis for most industrial control, simpler model form, easy to identify
& easy to design controller
 poor prediction, adequate control
Nonlinear
 reality, more complex and difficult to identify
 need state-of-the-art controller design techniques to do the job better
prediction & control

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Batch vs Continuous
Batch
 Feedstock for each processing step (i.e., reaction, distillation) are
charged into the equipment at the start of processing; products are
removed at the end of processing
 Batch processes are intrinsically dynamic –conditions within the
equipment vary over the duration of the batch
Continuous
 Involve continuous flows of material from one processing unit to the
next
 Usually designed to operate at steady-state;
 due to external disturbances, even continuous processes operate
dynamically
A Systematic Approach for Developing Dynamic Models
Identify modeling objectives
 end use of model (e.g. control)
Prepare information
 Draw a schematic diagram of the process and label all process variables.
 List all of the assumptions involved in developing the model. The model
should be no more complicated than necessary to meet the modeling
objectives.
 Determine whether spatial variations of process variables are important.
If so, a partial differential equation model will be required.
Formulate the model
 Write appropriate conservation equations (mass, component, energy,
and so forth).
 Introduce equilibrium relations and other algebraic equations (from
thermodynamics, transport phenomena, chemical kinetics, equipment
geometry, etc.)

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Determine the solution Self-assessment activities’
 Perform a degrees of freedom analysis to ensure that the model 1. Consider the liquid holding tank

equations can be solved. system shown in fig.20.1.

 Solve model equations A liquid enters the tank with a

Check the validity of the model flowrate Fi (ft3/min). Let F be

 compare to process behavior the flowrate of the stream

leaving the tank. The tank cross-
Degree of freedom analysis
The degree of freedom of a processing system are independent variables sectional area and the liquid
that must be specified in order to define the process completely. density considered constants.
Desired control of a process will be achieved when and only when all the Keeping the tank level at
degree of freedom have been specified. The arbitrarily specified variables desired level is a modeling
are the degree of freedom and there is given by the following relationship. objective.
NF = NV-NE i. Develop the model
NE:- no. of independent equation i.e differential or algebraic equation.
NV=no. of independent variables ii. Determine the degrees of
NF=no. of degree of freedom freedom for the system
A degrees of freedom analysis allows modeling problems to be classified
according to the following categories:
 Case 1. If NF = 0, then we have NE = Nv The equation yields unique
solution. ⟹ the process is exactly specified.
 Case 2. If NF > 0, then we have more variables than equations. Multiple
solutions result from the equations since we can specify arbitrarily NF of
Figure 20.1 liquid holding tank system
the variables. In this case, we say that the process is underspecified by
NF equations, (i.e. we need NF additional equations in order to have a
unique solution).
 Case 3. If NF < 0, then we have more equations than variables and in
general there is no solution to the NE equations. In this case we say that
the system is over specified by NF equations i.e., we need to remove NF
equations in order to have a solution for the system.

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Solutions for self-assessment activity 1
i. Developing a model
For control applications:
Modeling objectives is to describe process dynamics based on the laws of
conservation of mass, energy and momentum.
General balance equation:
rate of
Flow 𝐹𝑙𝑜𝑤 𝑅𝑎𝑡𝑒 𝑜𝑓
{ accumulation of } = { }−{ }+{ }
in 𝑜𝑢𝑡 𝑝𝑟𝑜𝑑𝑢𝑐𝑡𝑖𝑜𝑛
fundamental quantity
Conservation of Mass
{rate of mass accumulation} = {rate of mass in} − {rate of mass out}
Total mass balance
𝑑𝑚 𝑚 𝑚
⟹ 𝑑𝑡 = ( 𝑡 ) − ( 𝑡 )
𝑖𝑛 𝑜𝑢𝑡
𝑑(𝜌𝐴ℎ) (𝜌𝑉) (𝜌𝑉)
⟹ =( ) −( )
𝑑𝑡 𝑡 𝑖𝑛 𝑡 𝑜𝑢𝑡
𝑑(ℎ) 𝑑(ℎ)
⟹𝜌𝐴 = 𝜌(𝐹𝑖𝑛 − 𝐹𝑜 ) = 𝐴 = 𝐹𝑖𝑛 − 𝐹𝑜
𝑑𝑡 𝑑𝑡

Now we need to ensure that the model equation can be solved.

ii. Degree of freedom determination
NF = NV-NE
NV = 3 [h, Fi, Fo]
𝑑(ℎ)
NE = 1 [𝜌𝐴 = 𝜌(𝐹𝑖𝑛 − 𝐹𝑜 )]
𝑑𝑡
NF = 3-1 = 2
We have more unknowns (2) than equation (1)
⟹ NF > 0 ⟹ NV > NE
⟹ 2> 0
We have two unknown variables [NF], which can specify arbitrarily and
multiple solutions will be obtained.
⟹ the process is underspecified by NF (2) equations
⟹ we need 2 additional equations in order to have a unique solution
The process variables are classified as: 1 output: h & 2 Inputs: Fin, F
There exists a solution for each value of the inputs Fi & F

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CHEMICAL ENGINERING DEPARTMENT
Solution for self-assessment activity 2 2. Consider the tank heater system
Model equation shown in Figure 17.9a. A liquid
When V-is constant; we will consider only energy balance) enters the tank with a flowrate Fi
Conservation of energy: The general law of energy conservation is also (ft3/min), and a temperature Ti
called the First Law of Thermodynamics. It can be expressed as: (oF), where it is heated with steam
𝑛𝑒𝑡 rate of ℎ𝑒𝑎𝑡 𝑎𝑑𝑑𝑖𝑡𝑖𝑜𝑛 (having a flowrate Fs, lb/min). Let
rate of 𝑒𝑛𝑒𝑟𝑔𝑦 rate of 𝑒𝑛𝑒𝑟𝑔𝑦 𝑖𝑛 rate of 𝑒𝑛𝑒𝑟𝑔𝑦 𝑜𝑢𝑡
{ }={ }−{ } + { to the system from }
accumulation by convection by convection
𝑡ℎ𝑒 𝑠𝑢𝑟𝑟𝑜𝑢𝑛𝑑𝑖𝑛𝑔𝑠 F and T be the flowrate and
𝑛𝑒𝑡 rate of 𝑤𝑜𝑟𝑘
+ {performed the system } temperature of the stream leaving
𝑏𝑦 𝑡ℎ𝑒 𝑠𝑢𝑟𝑟𝑜𝑢𝑛𝑑𝑖𝑛𝑔𝑠
For these reasonable assumptions, the energy balance can be written as the tank.
𝑑𝐸 𝑑(𝑈+𝐾+𝑃) 𝑑𝐻 The tank is considered to be well
⟹ 𝑑𝑡
= 𝑑𝑡
= 𝑑𝑡
= ∑𝑖−𝑖𝑛𝑙𝑒𝑡 𝜌𝑖 𝐹𝑖 ℎ𝑖 − ∑𝑗−𝑜𝑢𝑡𝑙𝑒𝑡 𝜌𝑗 𝐹𝑗 ℎ𝑗 ± 𝑄 ± 𝑊
stirred, which implies that the
Where:
temperature of the effluent is equal
ℎ𝑖 , ℎ𝑗 = specific enthalpy/enthalpy per unit mass (𝐻 = 𝑚𝐶𝑃 ∆𝑇 ⟹ 𝐻⁄𝑚 = ℎ𝑖 )
to the temperature of the liquid in
Q = rate of heat transfer to the system the tank. Keeping the effluent
E=the total energy of a thermodynamic system, E is the sum of its internal temperature, T and the volume of
energy, kinetic energy, and potential energy: 𝐸 = 𝑈 + 𝐾 + 𝑃 the liquid in the tank, V at desired
It is appropriate to make two assumptions: values of Ts and Vs, respectively,
 Changes in K and P can be neglected because they are small in are the operational objectives of this
comparison with changes in internal energy (U). heater. The fundamental quantities
 The net rate of work can be neglected because it is small compared to whose values provide the
the rates of heat transfer and convection. information about the heater are:
𝑑𝑈𝑖𝑛𝑡 𝑑𝐻
= = 𝐻̇𝑖𝑛 − 𝐻̇𝑜𝑢𝑡 + 𝑄 [Since it is a liquid system U = H] the total mass of the liquid in the
𝑑𝑡 𝑑𝑡

𝑑𝑈𝑖𝑛𝑡 𝑑𝑇 𝑚𝐶𝑑𝑇 𝑚𝐶𝑑𝑇 tank & the total energy of the

= 𝜌𝑉𝐶 =( ) −( ) +𝑄
𝑑𝑡 𝑑𝑡 𝑡 𝑖𝑛 𝑡 𝑜𝑢𝑡 material in the tank
𝑑𝑇
𝜌𝑉𝐶 = 𝐹𝐶(𝑇𝑖 − 𝑇𝑟𝑒𝑓 ) − 𝐹𝐶(𝑇𝑜 − 𝑇𝑟𝑒𝑓 ) + 𝑄
𝑑𝑡
Assume that 𝑇𝑟𝑒𝑓 = 0,
𝑑𝑇
𝜌𝑉𝐶 = 𝐹𝐶(𝑇𝑖 − 𝑇𝑜 ) + 𝑄
𝑑𝑡
The process model often also includes algebraic relations often called
constitutive equations.
Figure 17.9a. Stirred tank heater

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CHEMICAL ENGINERING DEPARTMENT
 They are included to provide sufficient equations for a completely specified
model. Some examples of constitutive equations are:
Heat transfer: 𝑄 = ℎ𝐴(∆𝑇)
𝐸⁄
Chemical reaction rate: 𝑟𝐴 = 𝑘0 𝑒 − 𝑅𝑇 𝐶𝐴

Equation of state: 𝑃𝑉 = 𝑛𝑅𝑇

Degrees of freedom
3 parameters: 𝜌, 𝑉, 𝐶
4 variables: 𝑇𝑜 , 𝑇𝑖 , 𝐹, 𝑄
1 equation
⟹NF = 4 – 1 = 3
Can we solve this equation
The process variables are classified as:
1 output variable: T
3 input variables: Ti, F, Q
There exists a solution for each value of the inputs Ti, F, Q
Self-Check Questions

1. Water is entering a storage tank at a temperature 𝑇0 and flow rate 𝑄0 and leaving at a flow
rate Q and temperature T. There are negligible heat losses in the tank. The area of cross-
section of the tank is 𝐴0 . The model that describes the dynamic variation of temperature
of water in the tank with time is given as:
A. 𝑄0 (𝑇0 − 𝑇) = 𝐴0 ℎ(𝑑𝑇⁄𝑑𝑡)
B. 𝑄0 𝑇0 − 𝑄𝑇 = 𝐴0 ℎ(𝑑𝑇⁄𝑑𝑡)
C. 𝑄(𝑇0 − 𝑇) = 𝐴0 ℎ(𝑑𝑇⁄𝑑𝑡)
D. 𝑄(𝑇0 − 𝑇) = 𝐴0 (𝑑𝑇𝐻⁄𝑑𝑡)

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CHEMICAL ENGINERING DEPARTMENT
SECTION III Analysis of Dynamic Behavior of
Chemical Processes
SECTION CONTENTS & OBJECTIVES
Section Contents
The following contents are included in this section:
 Tools needed to analyze dynamic behavior of a typical processing
systems; it includes Laplace Transform & Transfer Functions Model
 Dynamic Behavior of First-Order Systems
 Dynamic Behavior of Second-Order Systems
 Self-Check Questions
Section Objectives
After completing this section, you will be able to:
 To analyze the static and dynamic behavior of processing systems
 To identify process characteristics which shape the dynamic response
for a variety of processing units
 To design effective controllers

Tools used for process dynamic behavior analysis

Laplace Transform (LT):
It is a mathematical tool, which can significantly reduce the effort required
to solve & analyze linear differential equation models. A major benefit is
that this transformation converts ordinary differential equations to algebraic
equations, which can simplify the mathematical manipulations required to
obtain a solution or perform an analysis. It offers a very simple & elegant
analytical method to solve the linear or linearized differential equations,
which are result from a mathematical modeling of processes. The LP also
allows: Simple development of input-output models which are very useful
for control purposes & straightforward qualitative analysis of how chemical
processes react to various external influences
Most of chemical engineering processes are modeled by nonlinear
equations. However, linear techniques are very valuable and of great
practical importance for the following reasons

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CHEMICAL ENGINERING DEPARTMENT
 There is no general theory for the analytical solution of nonlinear Self-Check Questions
differential equations, and consequently no comprehensive analysis of 1. Offers a very
simple and elegant analytical
nonlinear dynamic systems.
method to solve the linear or
 A nonlinear system can be adequately approximated by a linear near
linearized differential equations.
some operating conditions.
2. Which one of the following
 Significant advances in the linear control theory permit the synthesis
statement is correct about LT?
and design of every effective controllers even for nonlinear processes. A. It applies for linear model only
Definition: B. It is analytical tool
Consider the function𝑓(𝑡). The Laplace transform 𝑓(𝑠) of the function 𝑓(𝑡) C. It allows to develop TF model
is defined as follows: D. all
∞
𝐿[𝑓(𝑡)] = 𝑓(̅ 𝑠) = ∫ 𝑓(𝑡)𝑒 −𝑠𝑡 𝑑𝑡
0

Note: The L operator transforms a time domain function f(t) into an s

domain function, 𝑓(𝑠).
Where f(s) is the symbol for the LT and s is a complex variable: s = a + bj,
𝑗 = √−1
Inverse Laplace Transform, L-1
By definition, the inverse Laplace transform operator, L-1, converts an s-
domain function back to the corresponding time domain function:
𝐿−1 [𝑓(𝑠)] = 𝑓(𝑡), for t ≥ 0
Laplace Transforms of Common Functions:
Constant Function
Let f(t) = a (a constant). Then from the definition of the LT,
∞ ∞
𝑎 𝑎 𝑎
𝐿(𝑎) = ∫ 𝑎𝑒 −𝑠𝑡 𝑑𝑡 = − 𝑒 −𝑠𝑡 | = 0 − (− ) =
0 𝑠 0 𝑠 𝑠
Step Function
The unit step function is widely used in the analysis of process control
problems
0 𝑓𝑜𝑟 𝑡 < 0
It is defined as: S(𝑡) = {
1 𝑓𝑜𝑟 𝑡 ≥ 0
The LT of unit step function is the same as that obtained for the constant
1
above when a = 1: L[𝑆(𝑡)] = 𝑠

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CHEMICAL ENGINERING DEPARTMENT
Exponential Functions
Consider 𝑓(𝑡) = 𝑒 −𝑏𝑡 where b > 0. Then,
∞ ∞
1 ∞
𝐿[𝑒 −𝑏𝑡 ] = ∫ 𝑒 −𝑏𝑡 𝑒 −𝑏𝑡 𝑑𝑡 = ∫ 𝑒 −(𝑏+𝑠)𝑡 𝑑𝑡 = [−𝑒 −(𝑏+𝑠)𝑡 ]0
0 0 𝑏+𝑠
1
=
𝑠+𝑏
Laplace Transforms of Derivatives
The transform of a first derivative of f is important because such derivatives
appear in dynamic models:
∞
⟹𝐿[𝑑𝑓 ⁄𝑑𝑡] = ∫0 (𝑑𝑓 ⁄𝑑𝑡)𝑒 −𝑠𝑡 𝑑𝑡
𝑑𝑓
⟹𝐿 [ 𝑑𝑡 ] = 𝑠𝑓(𝑠) − 𝑓(0), 𝑓(0) 𝑖𝑠 𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑐𝑜𝑛𝑑𝑖𝑡𝑖𝑜𝑛 𝑎𝑡 𝑡 = 0

Proof: Integrating by parts,

𝑑𝑢 = 𝑑𝑓, 𝑣 = 𝑒 −𝑠𝑡
∞
⟹𝐿[𝑑𝑓 ⁄𝑑𝑡] = 𝑢𝑣]∞
0 − ∫0 𝑢𝑑𝑣
∞
= 𝑓(𝑡)𝑒 −𝑠𝑡 ]∞
0 − ∫ (−𝑠𝑓(𝑡)𝑒 −𝑠𝑡 )𝑑𝑡
0
∞
𝐿[𝑑𝑓 ⁄𝑑𝑡] = 𝑠 ∫ 𝑓(𝑡)𝑒 −𝑠𝑡 𝑑𝑡 − 𝑓(0) = 𝑠𝑓(𝑠) − 𝑓(0)
0

Similarly, for higher order derivatives:

𝑑𝑛 𝑓
𝐿[ ] = 𝑠 𝑛 𝑓(𝑠) − 𝑠 𝑛−1 𝑓(0) − 𝑠 𝑛−2 𝑓 (1) (0) − ⋯ − 𝑠𝑓 (𝑛−2) (0)
𝑑𝑡 𝑛
− 𝑓 (𝑛−1) (0)
dk f
where: n is an arbitrary positive integer and f (k) (0) = dtk |
t=0

Laplace Transform of Integrals

𝑡 1
𝐿 [∫0 𝑓(𝑡)𝑑𝑡] = 𝑠 𝑓(𝑠), where f(s) = L[f(t)]
𝑡 𝑡 𝑡
Proof: 𝐿 [∫0 𝑓(𝑡)𝑑𝑡] = ∫0 [∫0 𝑓(𝑡)𝑑𝑡] 𝑒 −𝑠𝑡 𝑑𝑡 (integrating by part)

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CHEMICAL ENGINERING DEPARTMENT
 Laplace Transforms of Some Basic Functions:

Function Laplace Transform

Constant, for f(t) = a 𝑎⁄

𝑠
Exponential, For 𝑓(𝑡) = 𝑒 𝑎𝑡 /𝑒 −𝑎𝑡 1⁄ 1
(𝑠 − 𝑎) / ⁄(𝑠 + 𝑎)

Ramp function, f(t) = at 𝑎⁄

𝑠2
𝑡2 2⁄
𝑠3
Laplace transform of derivatives 𝑑𝑓(𝑡)
𝐿[ ] = sf(s) − f(0)
𝑑𝑓(𝑡)⁄ 𝑑𝑡
𝑑𝑡 𝑑2 𝑓(𝑡)
2
𝑑 𝑓(𝑡)⁄ 𝐿[ 2
] = 𝑠 2 𝑓(𝑠) − 𝑠𝑓(0) − 𝑓 ′ (0)
𝑑𝑡 2 𝑑𝑡
𝑡
Laplace transform of Integrals, 1
𝑡 𝐿 [∫ 𝑓(𝑡)𝑑𝑡 ] = 𝑓(𝑠)
∫0 𝑓(𝑡)𝑑𝑡 0 𝑠

Important Properties of Laplace Transforms

Final Value Theorem:
It can be used to find the steady-state value of a closed loop system
(providing that a steady-state value exists.
Statement of FVT:
lim 𝑦(𝑡) = lim[𝑠𝑦(𝑠)]
𝑡→∞ 𝑠→0

providing that the limit exists (is finite) for all where Re (s) denotes the real
part of complex variable, s.
Solution for self-assessment activity 3
5𝑠+2
Then,𝑦(∞) = lim 𝑦(𝑡) = lim [(5𝑠+4)] = 0.5
𝑡→∞ 𝑠→0

Initial Value Theorem:

lim 𝑓(𝑡) = lim [𝑠𝑓(𝑠)]
𝑡→0 𝑡→∞

Solution for self-assessment activity 4

Using IVT
(𝑠−1)(𝑠+1)
lim 𝑓(𝑡) = lim [𝑠𝑓(𝑠)] = lim 𝑠 [𝑠(𝑠+3)(𝑠−4)] =1
𝑡→0 𝑡→∞ 𝑡→∞

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CHEMICAL ENGINERING DEPARTMENT
Procedure for the Solution of ODEs using Laplace Transforms 3. Determine the final value of
1. Take the L of both sides of the ODE. the following function
2. Rearrange the resulting algebraic equation in the s domain to solve 5𝑠 + 2
𝑦(𝑠) =
for the L of the output variable, e.g., Y(s). 𝑠(5𝑠 + 4)

3. Perform a partial fraction expansion. 4. Determine the initial value

4. Use the L-1 to find y(t) from the expression for Y(s). [find f(t=0).] of the following

Solution for self-assessment activity 5 function

(𝑠−1)(𝑠+1)
First, take L of both sides of the eqn. 𝑓(𝑠) = 𝑠(𝑠+3)(𝑠−4),
5(𝑠𝑦(𝑠) − 1) + 4𝑦(𝑠) = 2⁄𝑠, 5. Solve the ODE,
Rearrange, 𝑑𝑦
5 𝑑𝑡 + 4𝑦 = 2, y(0) = 1
5𝑠+2
𝑦(𝑠) = 𝑠(5𝑠+4),

Take L-1,
5𝑠+2
y(t) = L-1[𝑠(5𝑠+4)]= 𝑦(𝑡) = 0.5 + 0.5𝑒 −0.8𝑡

Partial Fraction Expansions (PFE)

Basic idea about PFE:
Expand a complex expression for y(s) into simpler terms, each of which
appears in the Laplace Transform table.
Then you can take the L-1 of both sides of the equation to obtain y(t).
𝑝(𝑠)
Assume that the LT of an unknown function y(s) is given by: 𝑦(𝑠) = 𝑞(𝑠)

where p(s) and q(s) are polynomials in s of order m and n respectively,

where m<n. q(s) is called the characteristic polynomial of the function y(s)
The factors of the characteristic polynomial correspond to the roots of the
characteristic polynomial set equal to zero. Once the factors are obtained,
the Laplace transform is then expanded into partial fractions.
In general we will distinguish two cases;
Polynomial q(s) has n distinct (all different) roots, real (no repeated roots)
or complex
𝛼
⟹ 𝑞(𝑠) = ∏𝑛𝑖=1(𝑠 + 𝑏𝑖 ) , expand as: 𝑦(𝑠) = ∑𝑛𝑖=1 𝑠+𝑏𝑖
𝑖

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CHEMICAL ENGINERING DEPARTMENT
Polynomial q(s) has multiple real roots (repeated roots (e.g., b1 = b2 = -3)) 6. Solve the following equation
𝛼 𝛼 𝛼
⟹ 𝑞(𝑠) = (𝑠 + 𝑏)𝑛 , expand as: 𝑦(𝑠) = 𝑠+𝑏
1 2
+ (𝑠+𝑏)2
𝑛
+ ⋯ + (𝑠+𝑏) 𝑛
using PFE:
𝑠+5
𝑝(𝑠) y(𝑠) = 𝑠2 +5𝑠+4
Constants are given by: 𝛼𝑖 = (𝑠 + 𝑏𝑖 ) ]
𝑞(𝑠) 𝑠=−𝑏𝑖
7. A process is described by a
After expanding and computing the values of the constants, the inverse
third-order ODE:
Laplace transform of every partial fraction will be determined. Then; the
𝑦⃛ + 6𝑦̈ + 11𝑦̇ + 6𝑦 = 1,
unknown function y(t) is given by:
all initial conditions are zero
𝛼
𝑦(𝑡) = 𝐿 −1 [𝑦(𝑠)]
=𝐿 −1
[∑𝑛𝑖=1 𝑠+𝑏𝑖 ] Show that the steady-state result
𝑖

Solution for self-assessment activity 6 in the time domain is the same

The denominator can be factored into a product of 1storder terms, (s + 1)(s + 4) as applying the final value
This transform can be expanded into the sum of two partial fractions: theorem.
s+5 a b
= s+1 + s+4, where coefficients a and b have to be determined
(s+1)(s+4)

To find a:
s+5 4
Multiply both sides by s + 1 and let s = -1⟹ a = s+4| =3
s=−1

To find b:
s+5 1
Multiply both sides by s + 4 and let s = -4⟹ b = s+1| = −3
s=−4

It has only real roots

4⁄ 1⁄
3 3
Substitute numerical values ⟹ 𝑦(𝑠) = 𝑠+1 − 𝑠+4

Take L-1 of both sides:

4⁄ 1⁄
L−1 [y(s)]
=L −1
[ 3 ]−L [ 3 ]
−1
s+1 s+4
4 1
⟹ 𝑦(𝑡) = 3 𝑒 −𝑡 − 3 𝑒 −4𝑡

Solution for self-assessment activity 7

Take LT of both sides and solve for y(s)
1 1
𝑦(𝑠) = =
𝑠(𝑠 3 + 6𝑠 2 + 11𝑠 + 6) 𝑠(𝑠 + 1)(𝑠 + 2)(𝑠 + 3)
⟹it has a distinct real roots- after factorize the denominator

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CHEMICAL ENGINERING DEPARTMENT
Perform the PFE: 8. Multiple roots. Consider the
1 𝑎 𝑏 𝑐 𝑑 LT,
𝑦(𝑠) = = + + +
𝑠(𝑠 3 + 6𝑠 2 + 11𝑠 + 6) 𝑠 𝑠 + 1 𝑠 + 2 𝑠 + 3 1
𝑥(𝑠) = (𝑠+1)3 (𝑠+2)
1 1 1 1
Solve for coefficients to get, a = 6 , b = − 2 , c = 2 , d = − 6

(For example, find a, by multiplying both sides by s and then setting s = 0.)
1⁄ 1⁄ 1⁄ 1⁄
6 2 2 6
Substitute numerical values ⟹ 𝑦(𝑠) = − 𝑠+1 + 𝑠+2 − 𝑠+3
𝑠

Take L-1 of both sides:

1⁄ 1⁄ 1⁄ 1⁄
L −1 [y(s)]
=L −1
[ 6 −1
]−L [ 2 −1
]+L [ 2 ]−L [ 6 ]
−1
s s+1 s+2 s+3
1 1 1 1
⟹ 𝑦(𝑡) = 6 − 2 𝑒 −𝑡 + 2 𝑒 −2𝑡 − 6 𝑒 −3𝑡

The FVT:
1 1 1 1 1 1
𝑦(∞) = lim [ − 𝑒 −𝑡 + 𝑒 −2𝑡 − 𝑒 −3𝑡 ] = lim [ 3 2
]=
𝑡→∞ 6 2 2 6 𝑠→0 (𝑠 + 6𝑠 + 11𝑠 + 6) 6
Solution for self-assessment activity 8
1 𝑎 𝑏 𝑐 𝑑
Perform PFE ⟹ 𝑥(𝑠) = (𝑠+1)3 (𝑠+2) = 𝑠+1 + (𝑠+1)2 + (𝑠+1)3 + 𝑠+2

Compute the constants: a, b, c and d

Step 1: First, compute for the value of d, this constant corresponds to
distinct roots: multiply both sides by s + 2 and then set s + 2 = 0, s = -2 &
find that d = -1
Step 2: Compute c: multiply both sides by (𝑠 + 1)3 and then set s = -1
1 (𝑠+1)3 𝑑
⟹ (𝑠+2) = 𝑎(𝑠 + 1)2 + 𝑏(𝑠 + 1) + 𝑐 + , and find that c = 1
𝑠+2

Step 3: Compute b: multiply both sides by (𝑠 + 1)2

1 c (s + 1)2 d
= a(s + 1) + b + +
(s + 1) (s + 2) (s + 1) s+2
Then, setting s = -1, the term involving the constant c becomes infinite
Therefore, an alternative procedure is needed to compute c
Differentiate both sides of the equation found in step 2 with respect to s and
1 (𝑠+1)2 (2𝑠+5)𝑑
take ⟹− (𝑠+2)2 = 2𝑎(𝑠 + 1) + 𝑏 + (𝑠+2)2
,

Then set s = -1 & find that b = -1

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CHEMICAL ENGINERING DEPARTMENT
Step 4: To compute a, differentiate the above equation once again
2 (𝑠2 +5𝑠+7 )2(𝑠+1)𝑑 9. Which statement is incorrect
⟹(𝑠+2)3 = 2𝑎 + and set s = -1 and find that a = 1
(𝑠+2)3
about Transfer Functions (TF)
1 −1 1 −1
⟹𝐿−1 [𝑥(𝑠)] = 𝐿−1 [𝑠+1] + 𝐿−1 [(𝑠+1)2 ] + 𝐿−1 [(𝑠+1)3 ] + 𝐿−1 [𝑠+2]
Model?
1 A. Can be used to determine
⟹𝑥(𝑡) = 𝑒 −𝑡 (1 − 𝑡 + 2 𝑡 2 ) − 𝑒 −2𝑡
the dynamic behavior of a
Transfer Functions (TF) Model
process after changes in
It also called Input-output model is an alternative model form based on
input variables.
Laplace Transforms. It is completely disregard the process states. It only
B. It is disregard the process
give a relationship between process inputs and process outputs. It occur in
state
the “Laplace domain”. The model can be used to determine the dynamic
C. It occur in time domain
behavior of a process after changes in input variables. It also plays a key
D. A & B
role in the design and analysis of control systems. A TF model characterizes
the dynamic relationship of two process variables, a dependent variable (or
output variable) and an independent variable (or input variable). For
example, in a continuous chemical reactor, the output variable could be the
exit concentration and the input variable a feed flow rate. Thus, the input
can be considered to be a "cause" & the output an "effect." Transfer function
models are only directly applicable to processes that exhibit linear dynamic
behavior, such as a process that as can be modeled by a linear ODE.
Definition of the Transfer Function: The TF is the ratio of the output
(response function) to the input (driving function) under the assumption that
all initial conditions are zero. Let G(s) denote the transfer function between
an input, x, and an output, y. Then, by definition
𝑌(𝑠) Laplace transform of the output, in deviation form
𝐺(𝑠) = 𝑋(𝑠) = ,
Laplace transform of the input, in deviation form

where 𝑌(𝑠) = 𝐿[𝑦(𝑡)] 𝑎𝑛𝑑 𝑋(𝑠) = 𝐿[𝑥(𝑡)]

If the TF of a system is known, the output or response can be studied for
various forms of inputs with a view toward understanding the nature of the
system. If the TF of a system is unknown, it may be established
experimentally by introducing known inputs and studying the output of the
system.

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CHEMICAL ENGINERING DEPARTMENT
Solution for self-assessment activity 10 10. Consider a simple processing
Determining the Transfer Function: system with a single input and a
To determine its TF, take LT of the dynamic equation of the system: single output (Fig.20.4a).
𝑑𝑛 𝑦 𝑑𝑛−1 𝑦 𝑑𝑦
𝑎𝑛 + 𝑎𝑛−1 + ⋯ + 𝑎1 + 𝑎0 𝑦 = 𝑏𝑓(𝑡)
𝑑𝑡 𝑛 𝑑𝑡 𝑛−1 𝑑𝑡
Using zero initial conditions. Then, rearrange it and will find:
Figure 20.4a. Single i/p & a single o/p process
𝑦̅(𝑠) 𝑏
= = 𝐺(𝑠) The dynamic behavior of the process is
̅
𝑓(𝑠) 𝑎𝑛 𝑠 𝑛 + 𝑎𝑛−1 𝑠 𝑛−1 + ⋯ + 𝑎1 𝑠 + 𝑎0
described by the differential equation;
G(s) is called the transfer function of the system and in a simple algebraic
𝑑𝑛 𝑦 𝑑𝑛−1 𝑦 𝑑𝑦
form; it relates the output of a process to its input (Figure 20.4b) 𝑎𝑛 𝑛
+ 𝑎𝑛−1 𝑛−1
+ ⋯ + 𝑎1
𝑑𝑡 𝑑𝑡 𝑑𝑡
Block diagram: + 𝑎0 𝑦 = 𝑏𝑓(𝑡)

The block diagram of TF model which relates the output of a process to its where f(t) and y(t) are the i/p & o/p of

input shown in figure 20.4b the process, respectively. Assume that

the system is initially at steady state.
Determine its TF and block diagram
11. If the process has two inputs,
Figure 20.4b. Block diagram of TF
𝑓1 (𝑡) and 𝑓2 (𝑡) as shown in
Solution for self-assessment activity 11
figure 20.5a,
Determine its LT & rearrange it
𝑏1 𝑏2
𝑦̅(𝑠) = 𝑎 ̅ (𝑠) ̅ (𝑠)
𝑠 𝑛 +𝑎 𝑠 𝑛−1 +⋯+𝑎 𝑠+𝑎 𝑓1 +𝑎 𝑠 𝑛 +𝑎 𝑠 𝑛−1 +⋯+𝑎 𝑠+𝑎 𝑓2
𝑛 𝑛−1 1 0 𝑛 𝑛−1 1 0

or equivalently, Figure 20.5a. Two input and a single

output process
𝑦̅(𝑠) = 𝐺1 (𝑠)𝑓1̅ (𝑠) + 𝐺2 (𝑠)𝑓2̅ (𝑠), where
𝑏1 𝑏2
Its dynamic model is
𝐺1 (𝑠) = 𝑎 𝑛 +𝑎 𝑛−1 +⋯+𝑎 𝑠+𝑎 𝑎𝑛𝑑 𝐺2 (𝑠) = 𝑎 𝑛 +𝑎 𝑛−1 +⋯+𝑎
𝑛𝑠 𝑛−1 𝑠 1 0 𝑛𝑠 𝑛−1 𝑠 1 𝑠+𝑎0 𝑑𝑛 𝑦 𝑑𝑛−1 𝑦
𝑎𝑛 + 𝑎 𝑛−1 +⋯
𝐺1 (𝑠) and 𝐺2 (𝑠) are the two TFs which relate the output of the process to 𝑑𝑡 𝑛 𝑑𝑡 𝑛−1
each one of its two inputs. 𝐺1 (𝑠) relates the output, y(s) to the first input 𝑑𝑦
+𝑎1 + 𝑎0 𝑦
𝑑𝑡
𝑓1̅ (𝑠) and 𝐺2 (𝑠) relates the output ,y(s) to the second input 𝑓2̅ (𝑠)
= 𝑏1 𝑓1 (𝑡) + 𝑏2 𝑓2 (𝑡)
⟹𝐺1 (𝑠) = 𝑦(𝑠)⁄𝑓1̅ (𝑠) 𝑎𝑛𝑑𝐺2 (𝑠) = 𝑦(𝑠)⁄𝑓2̅ (𝑠)
with the same initial conditions,
The block diagram of these relationships are shown as a Fig.20.5b
Determine transfer function of the
system in algebraic & block
diagram.

Figure 20.5b. TF Block diagram a system with one output and two input

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CHEMICAL ENGINERING DEPARTMENT
Solution for self-assessment activity 12 12. Consider the mathematical
Determining its TF: model of the stirred tank heater
Take the Laplace transforms of both sides and rearrange for T’(s) in terms of deviation variables
1⁄ 𝐾 shown below. Develop its TF
′ (𝑠) 𝜏 ′
𝑇 = 𝑇 𝑖 (𝑠) + 𝑇 ′ (𝑠)
𝑠+𝑎 𝑠 + 𝑎 𝑠𝑡 and express in block diagram
Defining the two transfer functions: 𝑑𝑇 ′ 1
+ 𝑎𝑇 ′ = 𝑇′𝑖 + 𝐾𝑇′𝑠𝑡
𝑇 ′ (𝑠) 𝑇 ′ (𝑠) 𝑑𝑡 𝜏
𝐺1 (𝑠) = 𝑇 ′ (𝑠), and 𝐺2 (𝑠) = 𝑇 ′ . Then,
𝑖 𝑠𝑡 (𝑠) 1 1 𝐹 𝑈𝐴
Where 𝑎 = 𝜏 + 𝐾, 𝜏 = 𝑉𝑖 , K = 𝑉𝜌𝑐𝑡
′ (𝑠) (𝑠)𝑇 ′ (𝑠)𝑇 ′
𝑇 = 𝐺1 𝑖 (𝑠) + 𝐺2 𝑠𝑡 (𝑠)
𝑝

Transfer Function b/n 𝑻′ (𝒔) and 𝑻′ 𝒔𝒕 (𝒔):

Suppose 𝑇𝑖 is constant at the steady-state value.
Then, 𝑇𝑖 (𝑡) = 𝑇̅𝑖 ⟹ 𝑇 ′ 𝑖 (𝑡) = 0 ⟹ 𝑇 ′ 𝑖 (𝑠) = 0
𝑇 ′ (𝑠) 𝐾
Thus, = 𝑠+𝑎
𝑇 ′ 𝑠𝑡 (𝑠)

Transfer Function b/n 𝑻′ (𝒔) and 𝑻′ 𝒊 (𝒔)

Suppose that 𝑇 ′ 𝑠𝑡 is constant at its steady-state value: 𝑇 ′ 𝑠𝑡 (𝑠) = 0
𝑇 ′ (𝑠) 1⁄
Thus, rearranging; 𝑇 ′ (𝑠) = 𝑠+𝑎𝜏
𝑖

Block diagram:
The block diagram for the tank heater G1(s) relates the temperature of the
liquid in the tank to that of the inlet stream, while G2(s) relates the
temperature of the liquid in the tank to that of the steam.

Figure: TF Block diagram a tank heater that relate its output temperature with two inputs

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CHEMICAL ENGINERING DEPARTMENT
Properties of Transfer Function Models:
TF clearly shows some important properties of the system
Order: The order of the system is the highest derivative of the output
variable in the defining differential equation, when expressed as a
combination of all individual equations.
For transfer functions of physical systems, the order can be easily
determined to be the highest power of s in the denominator.
Pole: A pole is defined as a root of the denominator of the TF; thus, it is the
same as a root of the characteristic polynomial. By analyzing the poles we
can obtained:
1. The stability of the system
2. The potential for periodic transients
Zero
A zero is a root of the numerator of the transfer function. Zeros do not
influence the exponents, but they influence the constants in the exponential
term (𝐴𝑒 −𝑎𝑡 -A is a constant). Thus, the numerator changes the weight
placed on the various exponential terms.
This demonstrates that the numerator of the transfer function cannot affect
the stability of the system modelled by the transfer function, but it can have
a strong influence on the trajectory followed by variables from their initial
to final values. Example to demonstrate the effect of numerator zeros:
3𝑠 + 1 1
𝐺(𝑠) = =
(3𝑠 + 1)(2.5𝑠 + 1) 2.5𝑠 + 1
The numerator zero cancelled one of the poles, with the result that the
second-order system behaves like a first-order system.

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CHEMICAL ENGINERING DEPARTMENT
Dynamic Behavior & Characteristics 13. The transfer function of a first
In analyzing process dynamic and process control systems, it is important order system is
to know how the process responds to changes in the process inputs A. 𝐾𝑝 ⁄(𝜏𝑝 𝑠 + 1)]
Dynamic Behavior of First-Order Systems B. 𝐾𝑝 ⁄𝜏𝑝 𝑠
First-order system is one whose output, y(t), is modeled by a first order,
C. 𝑠⁄(𝜏𝑝 𝑠 + 1)
linear differential equation
𝑑𝑦
D. None of these
𝑎1 𝑑𝑡 + 𝑎0 𝑦 = 𝑏𝑓(𝑡), where f(t) is the input.
14. By analyzing the first order
If 𝑎0 ≠ 0, then the above eqn. yields, processes parameters, we can say
𝑎1 𝑑𝑦 𝑏
+ 𝑦 = 𝑓(𝑡) that they are characterized by:
𝑎0 𝑑𝑡 𝑎0
A. Their capacity to store
𝑎1 𝑏
Define 𝑎 = 𝜏𝑝 , = 𝐾𝑝 𝑎𝑛𝑑 𝑡𝑎𝑘𝑒
0 𝑎0 material
𝑑𝑦 B. Their capacity to store
𝜏𝑝 + 𝑦 = 𝐾𝑝 𝑓(𝑡)
𝑑𝑡 energy
𝜏𝑝 is process time constant and 𝐾𝑝 is the steady state gain
C. The resistance associated
If y(t) and 𝑓(𝑡) are in terms of deviation variables around a steady state,
with the flow of mass in
then the initial conditions are: y(0) = 0 and f(0) = 0 reaching its capacity
𝑑𝑦
Determine the TF of the first-order system: 𝜏𝑝 + 𝑦 = 𝐾𝑝 𝑓(𝑡) D. The resistance associated
𝑑𝑡

𝑑𝑦 with the flow of energy in

𝐿 [ 𝜏𝑝 + 𝑦] = 𝐿[𝐾𝑝 𝑓(𝑡)] = 𝜏𝑝 𝑠𝑦(𝑠) + 𝑦(𝑠) = 𝐾𝑝 𝑓(𝑠)
𝑑𝑡 reaching its capacity
𝑦(𝑠)( 𝜏𝑝 𝑠 + 1) = 𝐾𝑝 𝑓(𝑠) E. All
𝑦(𝑠) 𝐾𝑝
= 𝐺(𝑠) =
𝑓(𝑠) 𝜏𝑝 𝑠 + 1
The standard first order transfer function is given by;
𝑦(𝑠) 𝐾𝑝
𝐺(𝑠) = =
𝑓(𝑠) 𝜏𝑝 𝑠 + 1
The important characteristics of the standard form are as follows:
The denominator must be of the form 𝜏𝑝 𝑠 + 1. The coefficient of the s term
in the denominator is the system time constant 𝜏𝑝 . The numerator is the
steady-state gain 𝐾𝑝

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CHEMICAL ENGINERING DEPARTMENT
The parameters the first-order system are:
 τ - time constant (is a measure of the time necessary for the process to 15. Choose the first order system
adjust to a change in the input) from the following:
 𝐾𝑝 -steady state gain (is the steady state change in output divided by the A. Liquid storage tank
sustained change in the input). It characterizes the sensitivity of the B. Stirred tank heater
output to the change in input C. Tank in series
Process Examples: D. A & B
Liquid storage E. All

𝑑(ℎ)
𝜌𝐴 = 𝜌(𝐹𝑖𝑛 − 𝐹)
𝑑𝑡
Since the system is storage tank F has to control in the way, which the tank
will hold the liquid.
If the output flow rate controller is designed to act proportional to the level
(F α h). Then F = βh
𝑑(ℎ)
𝜌𝐴 = 𝜌(𝐹𝑖𝑛 − βh)
𝑑𝑡
𝜌𝐴 𝑑(ℎ) 𝜌
= 𝐹𝑖𝑛 − h
β 𝑑𝑡 β
𝑑ℎ′
𝜏𝑝 + ℎ′ = 𝐾𝑝 𝐹𝑖𝑛
𝑑𝑡
Its TF becomes
ℎ′(𝑠) 𝐾𝑝
=
𝐹′𝑖𝑛 (𝑠) 𝜏𝑝 𝑠 + 1
Therefore, it is first order system

35
CHEMICAL ENGINERING DEPARTMENT
Stirred Tank heater 16. The dynamic response of a first
𝑑𝑇 order model of unit step
𝜌𝑉𝐶 = 𝐹𝐶𝑝 𝜌(𝑇𝑖 − 𝑇𝑜 ) + 𝑄,
𝑑𝑡
𝑑𝑇 change, magnitude A is
𝜌𝑉𝐶𝑝 = −𝜌𝐹𝐶𝑝 𝑇𝑜 + 𝑄, [if 𝑇𝑜 = 0]
𝑑𝑡 −𝑡⁄
𝜏𝑝
𝑉 𝑑𝑇 1
A. 𝑦(𝑡) = 𝐴𝐾𝑝 (1 − 𝑒 )
= −𝑇𝑜 + 𝜌𝑉𝐶 𝑄,
𝐹 𝑑𝑡 𝑝 −𝑡⁄
𝜏𝑝
B. 𝑦(𝑡) = 𝐾𝑝 (1 − 𝑒 )
𝑑𝑇𝑜 ′
𝜏𝑝 = +𝐾𝑝 𝑄 − 𝑇𝑜 , 𝐾𝑝
𝑑𝑡
C. 𝑦(𝑠) = 𝜏 𝑓(𝑠)
𝑇𝑜 ′(𝑠) 𝐾𝑝 𝑝 𝑠+1
=𝜏 ,
𝑄′(𝑠) 𝑝 𝑠+1 D. All
Therefore, it is first order system 17. The transfer function of a
Input response of first order model 𝐾𝑝
process is . If a step
𝜏𝑝 𝑠+1
Step input:
change is introduced into the
A sudden change in a process variable can be approximated by a step change
0, 𝑡 < 0 system, then the response will
of magnitude, A: 𝑓(𝑡) = {
𝐴, 𝑡 ≥ 0 be
If A = 1, we have a “unit step change”.
The dynamic response of a first order model of step change:
𝐴
L[f(t)] = L[A] = f(𝑠) = 𝑠
𝑦(𝑠) 𝐾𝑝
The transfer function of first order model is 𝐺(𝑠) = 𝑓(𝑠) = 𝜏
𝑝 𝑠+1

𝐾𝑝
𝑦(𝑠) = 𝑓(𝑠)
𝜏𝑝 𝑠 + 1
𝐴
Since f(𝑠) = 𝑠 , the output 𝑦(𝑠) is
𝐾𝑝 𝐴 𝐴𝐾𝑝 𝐴𝐾𝑝
𝑦(𝑠) = = − and inverse transform gives the solution,
(𝜏𝑝 𝑠+1) 𝑠 𝑠 𝜏𝑝 𝑠+1

−𝑡⁄
𝜏𝑝
𝑦(𝑡) = 𝐴𝐾𝑝 (1 − 𝑒 )
If the step change in f(t) were of a unit step ( A = 1), then the response would
−𝑡⁄
𝜏𝑝
be 𝑦(𝑡) = 𝐾𝑝 (1 − 𝑒 )

36
CHEMICAL ENGINERING DEPARTMENT
What do us looking for? 18. The static gain and time
Process Gain: Steady-State Response, 𝐾𝑝 constant of the process with a
15
As t → ∞ y(t) increases exponentially to a new steady state (ultimate value transfer function G(s) = 2𝑠+4
of the output) 𝐾𝑝 for a unit step change in the input, or 𝐴𝐾𝑝 for a step of are
size A, as t → ∞, y(t) → A𝐾𝑝 A. 1, 0.5
−𝑡⁄
𝑦(𝑡) = lim 𝐾𝑝 (1 − 𝑒 𝜏𝑝
) B. 3.75,0.5
t→∞
C. 2.75, 1
𝐾𝑝 ∆(Output) 𝑦(𝑡)
lim = 𝐾𝑝 = = D. 6.32, 1
𝑠→0 𝜏𝑝 𝑠 + 1 ∆(Input) 𝐴
19. What is the response of the
A process with this property is called self-regulating.
system with a transfer function
Process Time Constant, 𝜏𝑝
15
At 𝑡 = 𝜏𝑝 , the output response is, 𝑦(𝑡) = 0.632𝐴𝐾𝑝 G(s) = 2𝑠+4 for step change if

It is often used to estimate the time constant from experimental data. input is 5?
It can be used to determine the response of any typical first-order system, A. 𝑦(𝑡) = 18. 75(1 − 𝑒 −2𝑡 )
independently of the particular values of A, 𝐾𝑝 and 𝜏𝑝 . After a time interval B. 𝑦(𝑡) = 5(1 − 𝑒 −2𝑡 )

equal to the process time constant (t = τ), the process response is still only C. 𝑦(𝑡) = 6.32(1 − 𝑒 −2𝑡 )
63.2 percent complete. When the time elapsed is 2τ; 3τ; 4τ; 5τ the response D. None
is 86, 95, 98 and 99 percent respectively. 20. What is the ultimate value of

Large 𝜏𝑝 means a slow response ⟹Small 𝜏𝑝 means a fast response the response with a transfer
15
Small 𝜏𝑝 means ⟹ t → ∞ ⟹ the response is 99% function of G(s) = 2𝑠+4?

It does approximate the final steady-state value when t = 5τ . A. 5

Solution for self-assessment activity 18 B. 6.32
15 15⁄ 15 2 C. 18.75
4
G(s) = 2𝑠+4 = 2𝑠⁄ ⟹ 𝐾𝑝 = = 3.75 & τ=4 = 0.5
4+1 4
D. 1
Solution for self-assessment activity 19
5 𝑦(𝑠) 15 15 15 5
𝑓(𝑡) = 5 ⟹ f(s) = 𝑠 , = 2𝑠+4 →𝐲(𝐬) = 2𝑠+4 𝑓(𝑠) = 2𝑠+4 (𝑠 )
𝑓(𝑠)

After Partial Fraction Expansion, PFE

𝑦(𝑡) = 18. 75(1 − 𝑒 −2𝑡 ). Alternatively, we can substitute the parameters
in the response of a first order model of step change
−𝑡
⁄1⁄
𝑦(𝑡) = 5 ∗ 3.75 (1 − 𝑒 2) = 18. 75(1 − 𝑒 −2𝑡 )

37
CHEMICAL ENGINERING DEPARTMENT
Solution for self-assessment activity 20
Ultimate value of the response
t → ∞, 𝑦(𝑡) = 18. 75(1 − 𝑒 −2𝑡 ) = 18.75 or
We can check the result with the final value theorem,
75 75
lim sy(s) = lim [𝑠 ]= = 18.75
𝒔→𝟎 𝒔→𝟎 𝑠(2𝑠 + 4) 4
Ramp Input response
Industrial processes often experience “drifting disturbances”, i.e., relatively
slow changes up or down for some period of time.
The rate of change is approximately constant. We can approximate it as:
0 𝑡<0
𝑓(𝑡) = 𝐴𝑡, 𝑓(𝑡) = {
𝑎𝑡 𝑡 ≥ 0
Ramp a set point to a new value rather than making a step change.
Feed composition & catalyst activity are examples of ramp response
The dynamic response of a first order model of ramp change:
If the input f(t) is a ramp function with amplitude A, Its TF is
𝐴
f(t) = At ⟹ 𝑓(𝑠) =
𝑠2
𝐴 𝐴𝐾
Since f(𝑠) = 𝑠2 , the output 𝑦(s) is 𝑦(s) = (𝜏𝑠+1)𝑠2

Performing a partial fraction expansion yields:

𝑐1 𝑐2 𝑐3 𝐴𝐾
𝑦(s) = + 2+ =
𝑠 𝑠 𝜏𝑠 + 1 (𝜏𝑠 + 1)𝑠 2
−𝐴𝐾𝜏 𝐴𝐾 𝐴𝐾𝜏
𝑦(s) = + 2 +
𝑠 𝑠 𝑠 + 1⁄𝜏
−𝑡⁄
𝑦(t) = −AK𝜏 + 𝐴𝐾𝑡 + 𝐴𝐾𝜏𝑒 𝜏

−𝑡⁄
𝑦(t) = KA𝜏 (𝑒 𝜏 − 1) + 𝐾𝐴𝑡

For large values of time (t >> 𝜏)

𝑦(t) = KA(𝑡 − 𝜏)
This eqn. implies that after an initial transient period, the ramp input yields
a ramp output with slope equal to KA, but shifted in time by the process
time constant, 𝜏

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CHEMICAL ENGINERING DEPARTMENT
Dynamic Behavior of Second-Order Systems 21. The transfer function of a
A model that leads to a second order differential equation second order system is
2
𝑑 𝑦 𝑑𝑦 A. 1⁄(𝜏 2 𝑠 2 + 2𝜀𝜏𝑠 + 1)
𝑎2 2
+ 𝑎1 + 𝑎0 𝑦 = 𝑏𝑓(𝑡), 𝑎2 ≠ 0 𝑎𝑛𝑑 𝑦(0) = 𝑦′(0) = 0
𝑑𝑡 𝑑𝑡
B. 1⁄(𝜏 2 𝑠 2 + 2𝜏𝑠 + 1)
is usually rearranged to take the forms
2 2
C. 1⁄(𝜏 2 𝑠 2 + 2𝜀𝜏 + 1)
𝑑 𝑦 𝑑𝑦 𝑑 𝑦 𝑑𝑦
𝜏2 2
+ 2𝜀𝜏 + 𝑦 = 𝐾𝑓(𝑡) 𝑜𝑟 2
+ 2𝜀𝜔𝑛 + 𝜔𝑛2 𝑦 = 𝐾𝜔𝑛2 𝑓(𝑡) D. None of these
𝑑𝑡 𝑑𝑡 𝑑𝑡 𝑑𝑡
𝑎 𝑎 𝑏 1
Where 𝜏 2 = 𝑎2 ; 2𝜀𝜏 = 𝑎1 ; 𝐾 = 𝑎 ; 𝜔𝑛 =
0 0 0 𝜏

The corresponding Laplace transforms are

𝑦(𝑠) 𝐾 𝑦(𝑠) 𝐾𝜔 2
𝐺(𝑠) = 𝑓(𝑠) = 𝜏2 𝑠2 +2𝜀𝜏𝑠+1 𝑜𝑟 = 𝑠2 +2𝜀𝜔 𝑛𝑠+𝜔2 Where K-Process steady
𝑓(𝑠) 𝑛 𝑛

-state gain, 𝜏 = Process time constant/natural period of oscillation, 𝜀 =

Damping coefficient/ratio, 𝜔𝑛 =natural (undamped) frequency
A second order transfer function can arise physically when
Two process of first-order connected in series

𝑦(𝑠) 𝐾1 𝐾2 𝐾
𝐺(𝑠) = = =
𝑓(𝑠) (𝜏1 𝑠 + 1)(𝜏2 + 1) (𝜏1 𝑠 + 1)(𝜏2 + 1)
We will consider the second order transfer function,
𝑦(𝑠) 𝐾
𝐺(𝑠) = 𝑓(𝑠) = 𝜏2 𝑠2 +2𝜀𝜏𝑠+1 as the standard form

Step response of Second-Order Processes

Assume the general form
𝐾𝑃
𝑦(𝑠) = 𝑓(𝑠)
𝜏2𝑠2
+ 2𝜀𝜏𝑠 + 1
𝐾𝑃 𝐴
For a step change of magnitude A, 𝑓(𝑠) = 𝐴⁄𝑠 ⟹ y(𝑠) = 𝑠(𝜏2 𝑠2 +2𝜀𝜏𝑠+1)

The form of the response of y(t) will depend on the location of the two poles
in the complex plane (depends on value of damping constant)
Roots of the characteristic polynomial (𝜏 2 𝑠 2 + 2𝜀𝜏𝑠 + 1 = 0):
−2𝜀𝜏 ± √4𝜀 2 𝜏 2 − 4𝜏 2 𝜀 √𝜀 2 − 1
= − ±
2𝜏 2 𝜏 𝜏

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CHEMICAL ENGINERING DEPARTMENT
A stable process (or system) requires 𝜀 > 0 since we need τ > 0 to be 22. When the damping co-efficient
physically meaningful. The value of 𝜀 provides a measure of the amount of (ξ) is unity, the system is
damping (to diminish progressively in oscillation/vibration) in the system, A. Overdamped
i.e., completely determines the degree of oscillation in a process response B. Critically damped
after a perturbation. There are three different forms of answer to this C. Underdamped
equation for the way output varies with time –depends on value of damping D. Highly fluctuating
constant. The system can be over, critically or under damped. The important 23. The closed loop pole of a stable
issue in determining the form of the roots is the value of the square root second order system could be
term and this is determined by the value of the damping factor, ε A. Both real and positive
a) 𝜺 > 1(Over-damped) B. Complex conjugate with
 Two distinct real roots will obtain positive real parts
 System has an exponential behavior. This describes an output, which does C. Both real and negative
not oscillate but dies away with time D. One real positive and the
 The output takes longer than critical damping to reach the steady state value other real negative
 As time tends to infinity, the output becomes steady ⟹Sluggish(slow) response
b) 𝜺 = 1 (Critically-damped)
 The transition between over damped and under damped.
 The square root term is zero
 Both roots are real and both the same (Two equal real roots)
 Faster than over damped
 Output does not oscillate but dies away with time (the output just
gradually approaches the steady state value).
c) 0 < 𝜺 < 1 (Under-damped)
 The output is oscillates but the closer the damping ratio to 1 the faster the
amplitude of the oscillations diminishes.
 The square root term does not have a real value
 Two complex conjugate roots
 The response is fast initially, then overshoots & decays to steady state with
oscillations
 Oscillating response (the damping is attenuated as decreases)
d) 𝜺 ≤ 0 (Not-damped). Unstable (the oscillation amplitude grows indefinitely)
Note: Chemical processes are typically overdamped or critically damped

40
CHEMICAL ENGINERING DEPARTMENT
Characteristics of an Underdamped Response
Let us use as reference the underdamped response shown in the figure
below, in order to define the terms used to describe an underdamped
response.

Rise time, tr: It is defined as the time required for the response to reach its
final value for the first time or amount of time to first cross the steady state
level. The smaller the value of 𝜀, the shorter the rise time, i.e. the faster the
response of the system, but at the same time the larger the value of the
overshoot
Peak time, tp: amount of time to reach the first peak/is the time required
−𝜋𝜀
for the output to reach its first maximum value. 𝑡𝑃 = √1−𝜀2

Response/Settling time, ts: is defined as the time required for the process
output to reach and remain inside a band whose width is equal to ±5% of
the total change in y. The term 95% response time sometimes is used to refer
to this case. In addition, values of ±1% sometimes are used.
Overshoot ratio, OS: amount that first oscillation surpasses the steady state
level relative to the steady state change. OS = a/b (% overshoot is 100a/b).
The overshoot is a function of, and it can be shown that is given by the
−𝜋𝜀
following expression: 𝑂𝑆 = exp(√1−𝜀2 )

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CHEMICAL ENGINERING DEPARTMENT
Effect of damping factor on overshoot and decay ratio. Overshoot increases
with decreasing 𝜀 while as 𝜀 approaches 1 the overshoot approaches zero
(critically damped response)
Decay ratio, DR: fractional size of successive peaks. DR is a measure of
how rapidly the oscillations decreasing.
DR = c/a, where c is the height of the second peak
The decay ratio can be `shown to be related to the damping factor 𝜀 through
−2𝜋𝜀
the equation: (𝑂𝑆)2 = exp(√1−𝜀2 )
Period of Oscillation (P): is the time between two successive peaks or two
successive valleys of the response.
To find the period of the oscillation, P use the well-known relationships
𝜔 = 2𝜋𝑓 & 𝑓 = 1⁄𝑃 where f = cyclical frequency. Thus,

2𝜋𝜏 √1 − 𝜀 2
𝑃= , 𝑤ℎ𝑒𝑟𝑒 𝜔 =
√1 − 𝜀 2 𝜏
Natural Period of Oscillation: A second-order system with 𝜀 = 0, is a
𝐾 𝐾
system free of any damping. Its TF is 𝐺(𝑠) = 𝜏2𝑠2+1 = 1 1 i.e. it has
(𝑠−𝑗 )(𝑠+𝑗 )
𝜏 𝜏

two purely imaginary poles and it will oscillate continuously with a constant
1
amplitude, & 𝜔𝑛 = 𝜏 .
2𝜋
The corresponding cyclical period, Pn, is given by𝑃𝑛 = = 2𝜋𝜏. This
𝜔

property of the parameter 𝜏 that gave its name.

Remark:
 Our objective during the design a controller will be the proper selection
of the corresponding 𝜀 & 𝜏 values, so that the overshoot is small, the rise
time short, the decay ratio small, and the response time short.
 We will realize that it will not be possible to achieve all these objectives
for the same values of 𝜀 & 𝜏 , and that an acceptable compromise should
be defined. Good understanding of the underdamped behavior of a 2nd
order system will help tremendously in the design of efficient controllers.

42
CHEMICAL ENGINERING DEPARTMENT
Solution for self-assessment activity 24 24. For the following system
A second order transfer function can arise physically when
 Two process of 1st-order connected in series. E.g. two heated stirred-
tanks in series
 Processing system with a controller: Presence of a controller induces Determine the:
oscillatory behavior. E.g. Feedback control system a. Transfer function of standard
Thus, this process is arise from two first order processes connected in series form of second order system
a) The system transfer function in standard form b. Natural period of oscillation
1⁄ c. Static gain
𝑦(𝑠) 1∗2 2 12
G(s) = = = = 25. Consider the following transfer
𝑓(𝑠) (4𝑠 + 8)(𝑠 + 3) 4𝑠 2 + 20𝑠 + 24 1 𝑠 2 + 5 𝑠 + 1
6 6 function; subject to a unit step
b) Natural period of oscillation 𝜏 2 = 1⁄6
input change (assume time
c) Static gain 𝐾𝑃 = 1⁄12
units are minutes):
Solution for self-assessment activity 25
5
System parameters 𝐺(𝑠) =
4𝑠 2 + 0.8𝑠 + 1
5
From the given transfer function; 𝐺(𝑠) = 4𝑠2 +0.8𝑠+1 we can find Find the system parameters a)
a) 𝐾𝑃 = 5 process gain, 𝐾𝑃 b) process
b) 𝜏 2 = 4 ⟹ 𝜏 = 2 time, 𝜏 c) 𝜀
0.8 0.8
c) 2𝜀𝜏 = 0.8 ⟹ 𝜀 = = = 0.2 26. Let a transfer function:
2𝜏 4
9
Solution for self-assessment activity 26 𝐺(𝑠) =
𝑠2 + 2𝑠 + 9
a) Natural period of oscillation, 𝜏 Determine
9 1 1 1
𝐺(𝑠) = 2 = ⟹ 𝜏2 = ⟹ 𝜏 = a. Natural period of oscillation
𝑠 + 2𝑠 + 9 1 𝑠 2 + 2 𝑠 + 1 9 3
9 9 b. Static gain & Damping coefficient
b) Static gain, 𝐾𝑃 & Damping coefficient, 𝜀
c. Overshoot, Decay ratio
2 2⁄9 2⁄9 1
𝐾𝑃 = 1, 2𝜀𝜏 = ⟹ 𝜀 = = = d. Period of oscillation
9 2𝜏 2⁄ 3
3
c) Overshoot, Decay ratio e. Natural and angular frequency
−𝜋𝜀 −2𝜋𝜀
𝑂𝑆 = exp ( ) , DR = (𝑂𝑆)2 = exp( ) f. Nature of response
√1 − 𝜀 2 √1 − 𝜀 2
d) Period of oscillation 𝑃 = 2𝜋𝜏 2
√1−𝜀
g. The peak time
√1−𝜀 2
e) Natural and angular frequency; 𝜔𝑛 = 1𝜏, 𝜔 = 𝜏
1
f) Nature of response 𝜀 = 3 ⟹0 < 𝜀 < 1 (Under-damped)
𝜋𝜏
g) The peak time P = T = 2𝑇𝑃 ⟹ 𝑇𝑃 = √1−𝜀2

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CHEMICAL ENGINERING DEPARTMENT
 Self-Check Questions
1. A control system has the following transfer function
[(𝑠 − 1)(𝑠 + 1)]
𝑓(𝑠) = ⁄[𝑠(𝑠 − 2)(𝑠 + 4)]

The initial value of the corresponding time function is

A. 1
B. 1/8
C. 7/8
D. -1
2. In a single tank system, the transfer function of _______ __to
inlet flow rate is 1⁄(𝑡𝑠 + 1)
A. Outlet flow rate
B. Level
C. Both (a) & (b)
D. Neither (a) nor (b)
3. The inverse Laplace transform of the function 𝑓(𝑠) = 1⁄𝑠(1 + 𝑠) is
A. 1 + 𝑒 𝑡
B. 1 − 𝑒 𝑡
C. 1 + 𝑒 −𝑡
D. 1 − 𝑒 −𝑡
4. A system with a double pole at the origin is unstable since the corresponding
term in the time domain
A. Is a constant
B. Grows exponentially with time
C. Grows linearly with time
D. Decays linearly with time
5. A stable system is the one
A. For which the output response is bounded for all bounded input
B. Which exhibits an unbounded response to a bounded input
C. Which satisfies the conditions for a servo problem
D. None of these

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CHEMICAL ENGINERING DEPARTMENT
6. Number of poles in a system with transfer function 1⁄(𝑠 2 + 2𝑠 2 + 1 is
A. 2
B. 5
C. 3
D. 1
7. Which of the systems having the following transfer function is stable?
A. 1⁄(𝑠 2 + 2)
B. 1⁄(𝑠 2 − 2𝑠 + 3)
C. 1⁄(𝑠 2 + 2𝑠 + 2)
2 +2𝑠−1)
D. 𝑒 (−20𝑠)⁄(𝑠
8. In a single tank system, the transfer function of level to inlet flow rate is
A. ℎ⁄𝜏𝑠
B. ℎ⁄(1 + 𝜏𝑠)

C. 1⁄𝜏𝑠
D. None of these
9. Identify an unbounded input from inputs whose transfer functions are given
below
A. 1
B. 1⁄𝑠
C. 1⁄𝑠 2
D. 1⁄𝑠 2 + 1
10. A system with a double pole at the origin is unstable since the corresponding
term in the time domain
A. Is a constant
B. Grows exponentially with time
C. Grows linearly with time
D. Decays linearly with time

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CHEMICAL ENGINERING DEPARTMENT
11. Time constant is the
A. Time taken by the controlled variable to reach 63.2% of its full change
B. Same as transportation lag
C. Same as dead time
D. Time required by the measured variable to reach 63.2% of its ultimate change
12. For an input forcing function,𝑥(𝑡) = 2𝑡 2 , the Laplace transform of this
function is
A. 2⁄𝑠 2
B. 4/ s 2 4⁄𝑠 2
C. 2⁄𝑠 3
D. 4⁄𝑠 3
13. A process is initially at steady state with its output y = 1 for an input u = 1.
The input is suddenly changed to 2 at time t = 0. The output response
is 𝑦(𝑡) = 1 + 2𝑡. The transfer function of the process is
A. 2/s 2⁄𝑠
B. 1 + (2⁄(𝑠 2 )
C. 1 + (2⁄𝑠)
D. (1⁄𝑠)[1 + (2⁄𝑠)]
14. The closed loop pole of a stable second order system could be
A. Both real and positive
B. Complex conjugate with positive real parts
C. Both real and negative
D. One real positive and the other real negative
15. Which of the systems having the following transfer function is stable?
A. 1⁄(𝑠 2 + 2)
B. 1⁄(𝑠 2 − 2𝑠 + 3)
C. 1⁄(𝑠 2 + 2𝑠 + 2)
2 +2𝑠−1)
D. 𝑒 (−20𝑠)⁄(𝑠

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CHEMICAL ENGINERING DEPARTMENT
16. The unit step response of the transfer function 1⁄(𝑠 2 + 2𝑠 + 3)
A. Has a non-zero slope at the origin
B. Has a damped oscillatory characteristics
C. Is overdamped
D. Is unstable
17. The second order system with the transfer function 4⁄(𝑠 2 + 2𝑠 + 4) has a
damping ratio of
A. 2.0
B. 0.5
C. 1.0
D. 4.0
18. In second order underdamped system,
A. Decay ratio = overshoot
B. Decay ratio = (overshoot) 2
C. Overshoot increases for increasing damping co-efficient
D. Large damping co-efficient means smaller damping

47
CHEMICAL ENGINERING DEPARTMENT
SECTION IV: FEEDBACK CONTROL
SECTION CONTENTS & OBJECTIVES
Section Contents
The following contents are included in this section:
 Introduction to feedback control
 Control loop elements
 Effect of the control loop elements on dynamic response
Section Objectives
After completing this section, you will be able to:
 discuss the notion of feedback control loop & describe their
elements
 identify the types of feedback controllers
 examine the effect of different types of feedback controllers on the
response of a chemical process

INTRODUCTION TO FEEDBACK CONTROL

Consider the generalized process shown in Figure 21. l. It has an output y,
a potential disturbance d and an available manipulated variable m.
The system shown is known as open loop. When the value of d or m
changes, the response of the system is called open-loop response

Figure 21.1. Process block diagram

A feedback control action takes the following steps:

 Measures the value of the output (flow, pressure, liquid level,
temperature, composition) using the appropriate measuring device.
Let 𝑦𝑚 be the value indicated by the measuring sensor. [Measurement]
 Compares the indicated value 𝑦𝑚 , to the desired value 𝑦𝑠𝑝 (set point) of
the output. Let the deviation (error) be 𝜀 = 𝑦𝑠𝑝 − 𝑦𝑚 . The value of the
deviation 𝜀 is supplied to the main controller. [Comparison]
 The controller in turn changes the value of the manipulated variable m
in such a way as to reduce the magnitude of the deviation 𝜀. [Action]

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CHEMICAL ENGINERING DEPARTMENT
Usually, the controller does not affect the manipulated variable directly but
through another device (usually a control valve) which is known as the final
control element. The feedback control action can be summarized
pictorially as

Figure 21.2. Feedback Loop

The feedback-controlled system shown in the figure 21.2 is called closed

loop. When the value of d or m changes, the response of system is called
the closed-loop response. The origin of the term closed-loop is evident from
the fig.21.2.
Note: the feedback control system consists
Sensor: monitors some property of system and transmits signal back to
controller
Controller:
 software component implements math
 hardware component provides calibrated signal for actuator
Actuator:
 physical (with dynamics) process triggered by controller
 directly affects process
Types of Feedback Controller: The controller is located between the
measuring device and the final control elements (see fig. 21.2).
Function of the controller:
To receive the measured output signal 𝑦𝑚 (t) and after comparing it with the
set point 𝑦𝑠𝑝 to produce the actuating signal c(t) in such a way as to return
the output to the desired value 𝑦𝑠𝑝 .

49
CHEMICAL ENGINERING DEPARTMENT
Therefore, the input to the controller is the error 𝜀(𝑡) = 𝑦𝑠𝑝 − 𝑦𝑚 (𝑡) while
its output is c(t).
The various types of continuous feedback controllers differ on the way they
relate 𝜀(𝑡) to c(t).
There are three basic types of feedback controllers;
 Proportional (P),
 Proportional-integral and
 Proportional-integral-derivative
Proportional (P) Controller:
In feedback control, the objective is to reduce the error signal to zero
where 𝜀(𝑡) = 𝑦𝑠𝑝 − 𝑦𝑚 (𝑡).
Its controller (actuating) output is proportional to the error, i.e.
𝑐(𝑡) = 𝐾𝑐 𝜀(𝑡) + 𝑐𝑠
Where: 𝑐(𝑡) - Controller Output
Kc = controller proportional gain and
𝑐𝑠 = controller bias signal (i.e. its actuating signal when 𝜀=0).
A P-controller is described by the value of its proportional gain Kc
The key concepts behind proportional control are the following:
 The controller gain can be adjusted to make the controller output
changes as sensitive as desired to deviations between set point and
controlled variable;
 The sign of Kc can be choose to make the controller output increase (or
decrease) as the error signal increases.
For proportional controllers, bias 𝑐𝑠 can be adjusted, a procedure referred to
as manual reset. The bias 𝑐𝑠 is the value of 𝑐(𝑡) at [e (t )=0] when the
process disturbances are at their expected values The bias value is assigned
at the controller design level, and remains fixed once the controller is put in
automatic
𝑐(𝑡) = 𝑐𝑠 = 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡-at the nominal steady state

50
CHEMICAL ENGINERING DEPARTMENT
In order to derive the transfer function for an ideal proportional controller
(without saturation limits), define a deviation variable 𝑐′(𝑡) as
𝑐 ′(𝑡) = 𝑐(𝑡) − 𝑐𝑠 ⟹ 𝑐′(𝑡) = 𝐾𝑐 𝜀(𝑡)
𝑐′(𝑠)
The transfer function for proportional-only control: = 𝐺𝑐 (𝑠) = 𝐾𝑐
𝜀(𝑠)

An inherent disadvantage of proportional-only control is that a steady-state

error (offset) occurs after a set-point change or a sustained disturbance. It is
attractive for control applications where offsets can be tolerated because of
its simplicity.
For example, in some level control problems, maintaining the liquid level
close to the set point is not as important as merely ensuring that the storage
tank does not overflow or run dry.
Proportional-Integral Controller (or PI-Controller)
Most commonly, it is known as proportional-plus-reset controller.
The P controller cannot remove offset because the only way to change the
controller bias during non-nominal operations is to cause e  0
The rationale behind a PI controller is to set the “actual” bias different
from𝑐𝑠 , thus letting the error be zero
Its actuating signal is related to the error by the equation,
𝐾𝑐 𝑡
𝑐′(𝑡) = 𝐾𝑐 𝜀(𝑡) + ∫ 𝜀(𝑡)𝑑𝑡 + 𝑐𝑠
𝜏𝐼 0
where 𝜏𝐼 is the integral time or reset time in minutes.
Initially c(t) is 𝐾𝑐 𝜀(𝑡) (the contribution of the integral term is zero).
After a period of 𝜏𝐼 minutes, the contribution of the integral term is
𝐾𝑐 𝜏𝐼 𝐾𝑐
∫ 𝜀(𝑡)𝑑𝑡
𝜏𝐼 0
= 𝜏𝐼
𝜀𝜏𝐼 = 𝐾𝑐 𝜀 i.e. the integral control action has "repeated"

the response of the proportional action.

This repetition takes place every 𝜏𝐼 minutes and has lent the name to the
reset time. Therefore, "reset time is the time needed by the controller to
repeat the initial proportional action change in its output."

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CHEMICAL ENGINERING DEPARTMENT
The integral action causes the controller output c(t) to change as long as an which is
error exists in the process output. Therefore, such a controller can eliminate proportional to
even small errors. the rate of change
Note that until e  0, the manipulated input keeps on changing because of in the error. Due
the presence of the integral term. to this property,
The change in c(t) will stop only when e = 0. the derivative
The corresponding transfer function for the PI controller is: control action is
1 sometimes
𝐺𝑐 (𝑠) = 𝐾𝑐 (1 + )
𝜏𝐼 𝑠 referred to as
Reset Windup "anticipatory
An inherent disadvantage of integral control action is a phenomenon known control".
as reset windup or integral windup. Recall that the integral mode causes the The major
controller output to change as long as e(t*) ≠ 0 in PI Eq. drawbacks of
When a sustained error occurs, the integral term becomes quite large and the derivative
the controller output eventually saturates. Further buildup of the integral control action
term while the controller is saturated is referred to as reset windup or are the
integral windup following:
Proportional-Integral-Derivative (or PID Controller)  For a
In the industrial practice, it is commonly known as proportional plus-reset- response
plus-rate controller. with
If the error is increasing very rapidly, a large deviation from the set point constant
may arise in a short time and sluggish processes tend to cycle. The rationale non-zero
behind derivative action is to anticipate the future behavior of the error error it
signal by considering its rate of change gives no
The output of the controller is given by, control
𝐾𝑐 𝑡 𝑑𝜀 action
𝑐(𝑡) = 𝐾𝑐 𝜀(𝑡) + ∫ 𝜀(𝑡)𝑑𝑡 + 𝐾𝑐 𝜏𝐷 + 𝑐𝑠
𝜏𝐼 0 𝑑𝑡
since
where 𝜏𝐷 is the derivative time in minutes. 𝑑𝜀⁄ =
𝑑𝑡
With the presence of the derivative term,(𝑑𝜀⁄𝑑𝑡) the PID controller anticipates
0.
what the error will be in the immediate future and applies a control action  For a noisy
response

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CHEMICAL ENGINERING DEPARTMENT
 with almost zero error, it can compute large derivatives and thus yield
large control action, although it is not needed.
The transfer function of a PID controller is:
1
𝐺𝑐 (𝑠) = 𝐾𝑐 (1 + + 𝜏𝐷 𝑠)
𝜏𝐼 𝑠
Features of Controller modes:
Proportional (P) Controller action
 Accelerates the process response by gain increases
 Produces steady state deviation (offset)
 Of-set decreases as gain increases
PI Controller
 Eliminates the steady state deviation (eliminate offset)
 Responses are sluggish with long oscillations
 Increasing gain Kc makes more oscillatory and leads to instability
PID Controller
 Anticipates the future error
 Introduces the stability effect

The Dynamic Behavior of Feedback Controlled Processes:

We will analyze the dynamic behavior of a process, which is controlled by
a feedback control system when (1) the values of the disturbance (load) d,
or of (2) the set point 𝑦𝑠𝑝 change.
Study of process dynamics focused on uncontrolled or Open loop processes
Observe process behavior as a result of specific input signals

y(s
m(s) y(s
PROCESS

In process control, we are concerned with the dynamic behavior of a

controlled or Closed-loop process

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CHEMICAL ENGINERING DEPARTMENT
The Closed-loop Response and Block diagram:

Figure 21.3: Generalized closed-loop system

Basic hardware components of a feedback control loop are the following:
 Process being controlled: the material equipment where the physical
or chemical operations take place (tanks, heat exchangers, reactors etc.).
 Measuring instruments or sensors: like thermocouples (for
temperature), bellows or diaphragms (for pressure or liquid level),
orifice plates (for flow), gas chromatographs or various types of
spectroscopic analyzers (for composition), etc.
 Transmission lines: used to carry the measurement signal from the
sensor to the controller and the control signal from the controller to the
final control element. These lines can be either pneumatic (compressed
air or liquid) or electrical.
 Controller: it also includes the function of the comparator. This is the
unit with logic that decides by how much to change the value of the
manipulated variable. It requires the specification of the desired value
(set point).
 Final control element: usually a control valve or a variable-speed
metering pump. This is the device that receives the control signal from
the controller and implements it by physically adjusting the value of the
manipulated variable
For each of its four components: process, measuring device, controller
mechanism and final control element, should be viewed as a physical
system with an input and an output we can write the corresponding transfer
function relating its output to its inputs.

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CHEMICAL ENGINERING DEPARTMENT
For control, we need to identify closed-loop dynamics due to two problems
or processes based on type of input
Servo process: the disturbance does not change (d = 0) and the set point
changes (𝑦𝑠𝑝 ≠ 0). The input is the set point 𝑦𝑠𝑝 that changes.
The objective is to cause the output to track the changing set-point.
Regulatory process: the disturbance changes(d ≠ 0) while set point does
not change (𝑦𝑠𝑝 = 0 ).
The task is to counteract the effect of external disturbances in order to
maintain the output at its constant set point.
In particular, if we neglect the dynamics of the transmission lines, we have:
̅ (𝑠) + 𝐺𝑑 (𝑠)𝑑̅ (𝑠)
Process: 𝑦̅(𝑠) = 𝐺𝑝 (𝑠)𝑚
Measuring Device: 𝑦̅𝑚 (𝑠) = 𝐺𝑚 (𝑠)𝑦̅(𝑠)
Controller Mechanism:
Comparator: 𝜀̅(𝑠) = 𝑦̅𝑠𝑝 (𝑠) − 𝑦̅𝑚 (𝑠)
Control action: 𝑐̅(𝑠) = 𝐺𝑐 (𝑠)𝜀̅(𝑠)
̅ (𝑠) = 𝐺𝑓 (𝑠)𝑐̅(𝑠)
Final Control Element: 𝑚
where 𝐺𝑝 , 𝐺𝑑 , 𝐺𝑚 , 𝐺𝑐 and 𝐺𝑓 are the transfer functions between the
corresponding inputs and outputs.
Figure 21.8 below shows the block diagram for the generalized closed-loop
system and it is nothing else but a pictorial representation of the four
components equations.

Figure 21.8 block diagram for the generalized closed-loop system

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CHEMICAL ENGINERING DEPARTMENT
The series of block between the comparator and the controlled output, i.e.
𝐺𝑐 , 𝐺𝑓 and 𝐺𝑝 constitutes the forward path, while the block 𝐺𝑚 is on the
feedback path between the controlled output and the comparator, If
𝐺 = 𝐺𝑐 𝐺𝑓 𝐺𝑝 then figure 3.9 below shows a simplified but equivalent
version of the block diagram.

Figure 21.9 Simplified block diagram of generalized closed-loop system

Algebraic manipulation of the above equations (control components TF)

yields:
̅ (𝑠) = 𝐺𝑓 (𝑠)𝑐̅(𝑠)
𝑚
̅ (𝑠) = 𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)𝜀̅(𝑠)------------------------(since 𝑐̅(𝑠) = 𝐺𝑐 (𝑠)𝜀̅(𝑠))
𝑚
̅ (𝑠) = 𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)[𝑦̅𝑠𝑝 (𝑠) − 𝑦̅𝑚 (𝑠)]------(since 𝜀̅(𝑠) = 𝑦̅𝑠𝑝 (𝑠) − 𝑦̅𝑚 (𝑠))
𝑚
̅ (𝑠) = 𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)[𝑦̅𝑠𝑝 (𝑠) − 𝐺𝑚 (𝑠)𝑦̅(𝑠)]------(since 𝑦̅𝑚 (𝑠) = 𝐺𝑚 (𝑠)𝑦̅(𝑠)
𝑚
Substitute in to
̅ (𝑠) + 𝐺𝑑 (𝑠)𝑑̅ (𝑠)
𝑦̅(𝑠) = 𝐺𝑝 (𝑠)𝑚
Yields
𝑦̅(𝑠) = 𝐺𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)[𝑦̅𝑠𝑝 (𝑠) − 𝐺𝑚 (𝑠)𝑦̅(𝑠)] + 𝐺𝑑 (𝑠)𝑑̅ (𝑠)
Rearrange as input-output form (general closed loop response)
𝐺𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)
𝑦̅(𝑠) = 𝑦̅ (𝑠)
1 + 𝐺𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)𝐺𝑚 (𝑠) 𝑠𝑝
𝐺𝑑 (𝑠)
+ 𝑑̅(𝑠)
1 + 𝐺𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)𝐺𝑚 (𝑠)
This equation gives the closed-loop response of the process. We notice that
it is composed of two terms.

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CHEMICAL ENGINERING DEPARTMENT
The first term shows the effect on the output of a change in the set point
while the second constitutes the effect on the output of a change in the load
(disturbance). The corresponding transfer functions are known as closed-
loop transfer functions. In particular
𝐺𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)
Servo problem at [d(s) =0] is 𝑦̅(𝑠) = 1+𝐺 𝑦̅𝑠𝑝 (𝑠) and the
𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)𝐺𝑚 (𝑠)

feedback controller acts in such a way as to keep y close to the changing

𝑦̅𝑠𝑝 (𝑠). The transfer function for servo problem is:
𝑦̅(𝑠) 𝐺𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠) 𝐺
𝐺𝑠𝑝 = = =
𝑦̅𝑠𝑝 (𝑠) 1 + 𝐺𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)𝐺𝑚 (𝑠) 1 + 𝐺𝐺𝑚
Regulatory problem at [𝑦̅𝑠𝑝 (𝑠) = 0] is:
𝐺𝑑 (𝑠)
𝑦̅(𝑠) = 𝑑̅ (𝑠)
1 + 𝐺𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)𝐺𝑚 (𝑠)
The feedback controller tries to eliminate the impact of the load changes
and keep y at the desired set point. The transfer function for regulatory
problem is:
𝑦̅(𝑠) 𝐺𝑑 (𝑠) 𝐺𝑑 (𝑠)
𝐺𝑙𝑜𝑎𝑑 = = =
𝑑̅(𝑠) 1 + 𝐺𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)𝐺𝑚 (𝑠) 1 + 𝐺𝐺𝑚 (𝑠)
The block diagram is further simplified as the figure 3.10 shows

Figure 21.10. Simplified block diagram

Remark:
The closed-loop overall transfer functions𝐺𝑠𝑝 𝑎𝑛𝑑 𝐺𝑙𝑜𝑎𝑑 depend on the
dynamics of the measuring sensors, controllers and final control elements.
Consequently, the closed-loop response for set point or load changes
depends on the dynamics of these elements whose selection becomes
therefore critical.

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CHEMICAL ENGINERING DEPARTMENT
 Effect of P-control on the response of a controlled process
The closed-loop response of a process is given by the eqn.
𝐺𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠) 𝐺𝑑 (𝑠)
𝑦̅(𝑠) = 1+𝐺 𝑦̅𝑠𝑝 (𝑠) + 1+𝐺 𝑑̅ (𝑠)
𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)𝐺𝑚 (𝑠) 𝑝 (𝑠)𝐺𝑓 (𝑠)𝐺𝑐 (𝑠)𝐺𝑚 (𝑠)

To simplify the analysis assume that 𝐺𝑚 (𝑠) = 1 and 𝐺𝑓 (𝑠) = 1

Also, for a proportional controller 𝐺𝑐 (𝑠) = 𝐾𝑐
𝐺𝑝 (𝑠)𝐾𝑐 𝐺 (𝑠)
⟹ 𝑦̅(𝑠) = 1+𝐺 𝑦̅𝑠𝑝 (𝑠) + 1+𝐺 𝑑(𝑠) 𝐾 𝑑̅(𝑠)
𝑝 (𝑠)𝐾𝑐 𝑝 𝑐

Self-Check Questions
1. The transfer function for a proportional plus reset controller is
1
A. 𝐺𝑐 (𝑠) = 𝐾𝑐 (1 + 𝜏 𝑠)
𝐼

B. 𝐺𝑐 (𝑠) = 𝐾𝑐 (1 + 𝜏𝐼 𝑠)
𝐾
C. 𝐺𝑐 (𝑠) = 𝜏 𝑐𝑠
𝐼

D. 𝐺𝑐 (𝑠) = 𝐾𝑐 𝜏𝐼 𝑠
2. If response of a control system is to be free of offset and oscillation, the
most suitable controller is
A. Proportional controller
B. Proportional-derivative (PD) controller
C. Proportional-integral (PI) controller
D. Proportional integral-derivative (PID) controller
3. Response of a linear control system for a change in set point is called
A. Frequency response
B. Transient response
C. Servo problem
D. Regulator problem
4. The offset introduced by proportional controller with gain Kc in response
of first order system can be reduced by
A. Reducing value of Kc
B. Introducing integral control
C. Introducing derivative control
D. None of the above

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CHEMICAL ENGINERING DEPARTMENT
5. The transfer function for a PID controller is (where, τ i is the integral (reset)
time and τD is the derivative time.
A. 𝐾𝑐 (1 + 𝜏𝐼 𝑠 + 𝜏𝐷 𝑠) ∗ 𝑠
1
B. 𝐾𝑐 (1 + 𝜏 𝑠 + 𝜏𝐷 𝑠)
𝐼

1
C. 𝐾𝑐 (1 + 𝜏𝐼 𝑠 + (𝜏 𝑠))
𝐷𝑠

D. None of these
6. Reset time is called also ________ time.
A. Dead
B. Integral
C. Derivative
D. None of these
7. For the block diagram shown below: The characteristic equation is

A. 𝜏𝐼 𝑠(𝜏𝑃 𝑠 + 1) + 𝐾𝐶 ∗ 𝐾𝑃 (𝜏1 𝑠 + 1)𝑒 −𝜏𝐷𝑠 = 0

B. (𝜏𝑚 𝑠 + 1)(𝜏𝑃 𝑠 + 1) + 𝐾𝑚 ∗ 𝐾𝑃 𝑒 −𝜏𝐷𝑠 = 0
C. 𝜏𝐼 𝑠(𝜏𝑚 𝑠 + 1)(𝜏𝑃 𝑠 + 1) + 𝐾𝐶 ∗ 𝐾𝑃 𝐾𝑚 (𝜏1 𝑠 + 1)𝑒 −𝜏𝐷 𝑠 = 0
D. (𝜏𝑚 𝑠 + 1)(𝜏𝑃 𝑠 + 1) + 𝐾𝐶 ∗ 𝐾𝑚 𝑒 −𝜏𝐷𝑠 = 0

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CHEMICAL ENGINERING DEPARTMENT
SECTION V: PROCESS INDUSTRIES
SECTION CONTENTS & OBJECTIVES
Section Contents
The following contents are included in this section:
 Introduction to process industry
Section Objectives
After completing this section, you will be able to:
 provide basic knowledge about Industrial chemical process
Introduction to process industry
A chemical process industry involves the chemical processing of the raw
materials into useful and profitable products. These products are used both
as consumer goods and as intermediates for further chemical and physical
modification to yield consumer products. We can make a chemical process
industry by increasing the yield (desired product) and decreasing the
conversion (all consumer good and intermediate products). A chemical
process industry involves the physical operation and the chemical
conversion. There are many objective of a chemical process industry like as
to make pure product and reduce the by-product by increasing the desired
product. However, its main objective is to reduce the cost of the final
product. The final cost can be reduced by increasing the yield and using
material and energy balances.
The yield of any reaction is the amount of the desired product and the
conversion can be defined as in a multi pass system or process the total
product produce in a single pass is called as conversion. The cost of the
product can be reduce if conversion is equal to the yield means the amount
of by product and intermediate product is minimum and the amount of
desired product is maximum. It can be one by changing the operating
conditions of the reaction, process or system. For example, in the production
of ammonia gas by using the Haber process the yield of ammonia is only
14% and the conversion (unreacted nitrogen and hydrogen) is 86% if this
conversion is reduced by converting the single pass system into the multi

60
CHEMICAL ENGINERING DEPARTMENT
pass system then conversion can be decreased and yield can be increased
and the cost of the final product can be reduced. The yield of ammonia can
be also increased by changing the operating conditions i.e. by increasing the
pressure the production of ammonia is also increased. If we optimize the
conditions then yield will be equal to the conversion and the area of plant
decreased 4 to 5 times a capital cost (starting investment) also decreased.
Material balance also effect the final cost of the product in the material
balance will check that the raw material has good quality its treatment level
properties should be good. If material is pure then cost is automatically
reduced if it is impure then cost is increased for making the raw material
pure. The distribution of the material in the system also affects the final cost
of the product. For example, formally we use the cracker in oil refinery butt
now a day we use thermal cracker because fuel is expensive for cracker then
coal for thermal cracker. Similarly formally, we use the dry process for the
production of cement, which is expensive, but now we use the wet process,
which is less expensive, the dry process.
The requirement of energy to run a process plant also effect the cost of the
final product for example oil and gas fuel is expensive then the coal so now
a day our engineers are work to convert the plants in our country from oil
and gas to coal to reduce the cost of the final product.
Processes in chemical process industry: There are two main processes in
a chemical process industry. Both have their advantages and disadvantages
in a chemical process industry.
 Batch Process
 Continuous Process
Batch Process:
Batch process is used where low production rate is required. In a batch
process precise measurement are required for example one could add 1ml
of a 1% solution to 100,000L. Its labor and maintenance cost is high. In
batch process, it is difficult to maintain the operating conditions.
Temperature control is main issue in the batch process.

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CHEMICAL ENGINERING DEPARTMENT
In this process per unit cost is high as production rate is low. The simple
form of a batch reactor is a beaker. This process is used in the
pharmaceutical industry, cosmetic industry and paint industry etc.
Continuous Process:
Continuous process is used where high production rate is required. In a
continuous process no precise measurement are required because we add
the raw material continuously and run in the ranges. This process is also
flexible in operating condition. In this process per unit cost is low as
production rate is high. In the continuous process, the labor cost and
maintenance cost is low as production rate is high. This process is used in
the cement industry, paper industry and caustic soda industry etc.
Chemical process control and instrumentation: Today in the modern era
of science and technology almost every industry is operate on digital system
which is also called as piping and instrumentation system by which a single
person can run a plant by using controlling software and devices.
Process Flow Diagram (Charts Sheets): To represent a process of any
plant process flow diagrams are used they have two major types one is
called PFD diagram or block diagram in this diagram process and
equipment’s are shown by the simple blocks that what is input, what is
output, what is the operating condition and what is the energy requirements.
The 2nd type is called piping and instrumentation diagram (P&ID) in this
diagram proper piping and instrumentation is shown by the proper symbols.
It is more proper and difficult diagram than PFD diagram.
Some industries have also manual system until now a days but the labor cost
of the manual system is high as compared to the piping and instrumentation
system.

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CHEMICAL ENGINERING DEPARTMENT
SECTION VI: TYPICAL PROCESS INDUSTRIES
SECTION CONTENTS & OBJECTIVES
Section Contents
The following contents are included in this section:
 Introduction to process industry
Section Objectives
After completing this section, you will be able to:
 provide basic knowledge about Industrial chemical process

NITROGEN INDUSTRIES
Ammonia Production
Introduction
Ammonia is compound of nitrogen and hydrogen with formula NH3. At
standard temperature and pressure, ammonia is a gas. It is toxic and
corrosive to some materials and has a characteristic pungent odor. It is used
commercially can be anhydrous ammonia or an aqueous solution of NH3
and water referred to as ammonium hydroxide. Anhydrous ammonia must
be stored under pressure or at low temperature to remain a liquid.
Uses of Ammonia
 Serving as a fertilizer ingredient like urea, ammonium nitrate
 It can be used directly as a fertilizer by forming a solution with
irrigation water, without additional chemical processing
 It can be used in the production of nitric acid
 Used as a refrigerant-because of its good thermodynamics properties
 It also sometimes added to drinking water along with chlorine to
form chloramines a disinfectant
 It used to manufacture many other chemicals compounds like HCN,
explosives etc.

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CHEMICAL ENGINERING DEPARTMENT
Ammonia Synthesis Self-assessment activities
Steam Reforming Process Ammonia is synthesized using?

Overall Conversion A. Contact Process

B. Steam Reforming
The theoretical process conversion, based on methane feedstock are given
Process
in the following approximate formulae
C. A & B
0.88CH4 + 1.26𝐴𝑖𝑟 + 1.24𝐻2 𝑂 → 0.88CO2 + 1.26𝑁2 + 3𝐻2
D. None
𝑁2 + 3𝐻2 ⇆ 2𝑁𝐻3
Block Diagram of ammonia synthesis using steam reforming process

Figure 3.1 Ammonia synthesis

Steps in ammonia synthesis

Feedstock Desulphurization
Most of the catalysts used in the process are sensitive to sulfur and sulfur
compounds. The feedstock normally contains up to 5mg/Nm3 (normal m3)
as sulfur compounds.

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CHEMICAL ENGINERING DEPARTMENT
The feedstock is pre heated to 350-400oC and then treated in a
desulphurization vessel, where the sulfur compounds are hydrogenated to
H2S, Typically using a Cobalt molybdenum catalyst and then adsorbed on
pelletized ZnO.
𝑅 − 𝑆𝐻 + 𝐻2 → 𝐻2 𝑆 + 𝑅𝐻
𝐻2 𝑆 + 𝑍𝑛𝑂 → 𝑍𝑛𝑆 + 𝐻2 𝑂
In this way, sulfur is remove to less than 0.1-ppm sulfur in the gas feed. The
ZnS remains in the adsorption bed. The hydrogen for the reaction is usually
recycled from the synthesis reaction.
Steam Reforming
Primary Reforming
The gas from desulphurizer is mixed with process steam. Mixture is then
heated further to 500-600 oC before entering the primary reformer. The
primary reformer consist of a large number of high nickel-chromium alloy
tubes filled with nickel containing reforming catalyst. The overall reaction
is highly endothermic.
The composition of the gas leaving the primary reformer is given by the
close approach to the following chemical equilibria
𝐶𝐻4 + 𝐻2 𝑂 ⇆ 𝐶𝑂 + 3𝐻2 − − − − − − − ∆𝐻 = 206𝑘𝐽/𝑚𝑜𝑙
𝐶𝑂 + 3𝐻2 𝑂 ⇆ 𝐶𝑂2 + 𝐻2 − − − − − − − ∆𝐻 = −41𝑘𝐽/𝑚𝑜𝑙
Natural gas or other fuel supplies the heat for the primary reforming process.
Secondary Reforming
Upto 85% hydrocarbon feed is reformed in the primary reformer because of
the chemical equilibria at the actual operating conditions. The temperature
must be raised to increase the conversion. This is done in the secondary
reformer by internal combustion of the part of gas with process air, which
also provides the N2 for the final synthesis gas
𝐻2 + 𝐴𝑖𝑟𝑁2 + 𝐻2 𝑂
The process gas is cooled 350-400 oC in a waste heat boiler.

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Shift Conversion
Process gas form the secondary reformer contains 12-15% CO (dry gas
bases) and most of the CO is converted in the shift section according to the
reaction
𝐶𝑂 + 3𝐻2 𝑂 ⇆ 𝐶𝑂2 + 𝐻2 − − − − − − − ∆𝐻 = −41𝑘𝐽/𝑚𝑜𝑙
In the High Temperature Shift Conversion (HTS), the gas is passed through
a bed of iron oxide/chromium oxide catalyst at around 400C, where the CO
content are redused to 3%(dry gas base), limited by shift equilibrium at the
actual operating temp. The gas from HTS is further cooled to increase the
conversion and through the Low Temp. Shift (LTS) converter. The LTS
converter is filled with a zinc oxide based catalyst and operated at about
200-220oC. The residual CO content in converted gas is 0.2-0.4%(dry gas
base).
CO2 Removal
The process gas from LTS converter contains mainly H2, N2 , CO2 and the
excess process steam. The gas is cooled and most of the excess steam is
condensed before it enters the CO2 removal System.
The CO2 is removed in a chemical or physical absorption process. The
solvent used in chemical absorption processes are mainly aqueous amnie
solution (Mono Ethanolamine (MEA)), Activated Methyl Di-Ethanolamine
(AMDEA) or hot potassium carbonate solutions. Physical solvents are
glycol, di-methyl ethers (selexol), Propylene carbonate and other.
Methanation
The small amount of CO and CO2 , remaining in the synthesis gas, are
poisonous for the ammonia synthesis catalyst and must be removed by
conversion of CH4 in the methanation
𝐶𝑂 + 3𝐻2 → 𝐶𝐻4 + +𝐻2 𝑂
𝐶𝑂2 + 4𝐻2 → 𝐶𝐻4 + 2𝐻2 𝑂
The reaction take place at around 300oC in the reactor filled with a nickel
containing catalyst.

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CHEMICAL ENGINERING DEPARTMENT
Methane is an inert gas in the synthesis reaction, but the water must be
removed before entering the convertor. This is done by cooling and
condensation downstream of the methanator.
Synthesis Gas Compression
After mathanation the gas pressure is 27kg/cm2 and temperature is 364oC.
This gas is pressurized to 151Kg/cm2 as required by the synthesis reaction.
Ammonia Synthesis
The synthesis of ammonia is takes place on an iron catalyst at pressure
usually in the range 100-250bar and temperature 350-550oC
𝑁2 + 3𝐻2 ⇆ 2𝑁𝐻3 − − − − − − − − − ΔH = − 46 kJ/mol
Only 20-30% is reacted per pass in the reactor due to the Unfavorable
equilibrium conditions. The ammonia that is formed is separated from the
recycle gas by cooling/ condensation, and unreacted is substituted by the
fresh make up synthesis gas, thus maintain the pressure. In addition to that,
extensive heat exchanger is required due to exothermic reaction.
NH3 Purification
Conventional reforming with methanation as the final purification step
produces a synthesis gas containing inerts (methane and argon) in quantities
that do not dissolve in the condensed Ammonia. The major part of these
inerts are removed by taking out a purge stream from the loop. The purge
gas is scrubbed with water to remove ammonia before being used as fuel or
before being sent for hydrogen recovery.
Energy Conservation
Conservation and reuse of heat is so vital that it has been said that an
ammonia plant is really a steam generating plant that incidentally produces
ammonia. Much more steam than ammonia is made 4:1
SULPHUR AND SULPHURIC ACID
SULFUR
Sulfur is one of the most important and basic raw materials in the chemical
process industries. It exists, in nature both in the free and combined states
in ores such as pyrite, FeS2.

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CHEMICAL ENGINERING DEPARTMENT
Beside its most important application in the manufacture of sulfuric acid Pure sulfur can be obtained by
(90%), sulfur is used extensively in explosives, refrigerants, rubber, pulp, mining. True/False
and paper. Sulfur is mostly manufactured in
Sulfur Manufacturing Process the form of
Sulfur is obtained as elemental sulfur from sulfur dioxide and from A. SO2
hydrogen sulfide. Pure sulfur is mined but the sulfur dioxide comes from B. H2S
the roasting of sulfide ores and the hydrogen sulfide is removed from C. H2SO4
industrial gases. D. A & B
Pyrites source The usual concentrated sulfuric
Iron pyrites containing 40-45% s are roasted and must be purified by dust acid is
removal, cooling, scrubbling, filtering and drying by concentrated acid A. 87%
scrubbling to removal dust, moisture and catalyst poisons. B. 98%
Smelter sources C. 100%
SO2 obtained by roasting non-ferrous sulfide ores such as zinc, lead and D. 67%
copper given same treatment as pyrites gas. Why the chemical industries
Waste H2SO4 produce the 98% concentrated
FeSO4 from iron and steel pickle liquors and H2SO4 from petroleum refinery sulfuric acid?
operations are roasted to recover SO2 A. It is difficult to produced
H2S sources 100% concentrated
H2S is recovered by scrubbling various fuel and refinery gases with B. The 98% grade is more
ethanoalmies followed by hot stripping. The sulfide gas is burned as in stable for storage
reaction under sulfur. C. A & B
SULFURIC ACID D. None of the above
USES Sulfuric acid is synthesized
It uses in fertilizer, and leather production, dyeing of fabrics, paper using?
production, ore processing, wastewater processing, nitration – production A. Contact Process
B. Steam Reforming
of explosives, acid batteries, dehydrating agent
Process
FORMS
C. Chamber process
Although 100% sulfuric acid can be made, this loses SO3 at the boiling point
D. A & B
to produce 98.3% acid. The 98% grade is also more stable for storage,
making it the usual form for "concentrated" sulfuric acid.

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CHEMICAL ENGINERING DEPARTMENT
Other concentrations of sulfuric acid are used for different purposes. Some
common concentrations are: 10%, dilute sulfuric acid for laboratory use,
33.5%, battery acid (used in lead-acid batteries), 62.18%, chamber or
fertilizer acid and 98%, concentrated
PRODUCTION PROCESSES
Raw Material
So2 and Catalyst most widely used catalyst is vanadium pentoxide dispersed
on a porous carrier in pellet form.
Process description
Theoretical process description: the process can be classify as contact
process and chamber process. Both processes are based on SO2.
Chamber process was developed first (1746) but produced acid of
concentration less than 80%. Contact process yields 98% H2SO4 and higher
which can be diluted, if necessary.
Contact Process
In the first step, sulfur is burned to produce sulfur dioxide.
S(s) + O2(g) → SO2(g)
Air- SO2 gas containing 7 -10% SO2 and 11 – 14% O2 is preheated by
converter gas, if necessary and sent to first stage reactors of steel
construction. This is the high temperature (500-600OC) stage, contains 30%
of total catalyst and converts about 80% of SO2. The converter product is
cooled by heat exchange at 300OC and fed to a second stage where total
yield is increased to 97% by operating at 400-450OC for favorable
equilibrium.
Then SO2 is oxidized to sulfurtrioxide using oxygen in the presence of a
vanadium (V) oxide catalyst.
2 SO2 + O2(g) → 2 SO3(g) (in presence of V2O5)
For SO2/SO3 systems, the following methods are available to maximize the
formation of SO3:-
Removal of heat – a decrease in temperature will favor the formation of
SO3 since this is an exothermic process

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CHEMICAL ENGINERING DEPARTMENT
Increased oxygen concentration
Removal of SO3 (as in the case of the double absorption process)
Raised system pressure
Selection of the catalyst to reduce the working temperature (equilibrium)
Finally the sulfur trioxide is treated with water (usually as 97-98% H2SO4
containing 2-3% water) to produce 98-99% sulfuric acid.
SO3 (g) + H2O(l) → H2SO4(l)
Directly dissolving SO3 in water is impractical due to the highly exothermic
nature of the reaction. Mists are formed instead of a liquid. Alternatively,
the SO3 is absorbed into H2SO4 to produce oleum (H2S2O7).
H2SO4(l) + SO3 → H2S2O7(I)
Oleum is reacted with water to form concentrated H2SO4.
H2S2O7(I) + H2O(I) → 2 H2SO4(I)
High yield product gases are cooled to 150oC by water and air heat
exchanges, and absorbed in oleum fed at a rate to allow not over a 1% rise
in acid strength. Final scrubbling is done with a lower strength (97%) acid.
Oleum concentrations up to 40% can be made by tower absorption. Higher
strength oleum up to 65% is prepared by distilling 20% oleum
Absorption of SO3
Sulphuric acid is obtained from the absorption of SO3 and water into
H2SO4 (with a concentration of at least 98%).
The efficiency of the absorption step is related to:-
 The H2SO4 concentration of the absorbing liquid (98.5-99.5%)
 The range of temperature of the liquid (normally 70°C-120°C)
 The mist filter
 The temperature of incoming gas
 The co-current or counter-current character of the gas stream in the
absorbing liquid
Single absorption process
In the contact process, elemental sulfur is melted, filtered to remove ash,
and sprayed under pressure into a combustion chamber.

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CHEMICAL ENGINERING DEPARTMENT
The sulfur is burned in clean air that has been dried by scrubbing with 93 to
99 percent sulfuric acid. The gases from the combustion chamber cool by
passing through a waste heat boiler and then enter the catalyst (vanadium
pentoxide) converter.
Usually, 95 to 98 percent of the sulfur dioxide from the combustion chamber
is converted to sulfur trioxide, with an accompanying large evolution of
heat. After being cooled, again by generating steam, the converter exit gas
enters an oleum tower that is fed with 98 percent acid from the absorption
system. The gases from the oleum tower are then pumped to the absorption
column where the residual sulfur trioxide is removed.
Dual absorption process
In the dual absorption process the SO3 gas formed in the primary converter
stages is sent to an inter pass absorber where most of the SO3 is removed to
form H2SO4. The remaining unconverted sulfur dioxide is forwarded to the
final stages in the converter to remove much of the remaining SO2 by
oxidation to SO3, whence it is sent to the final absorber for removal of the
remaining sulfur trioxide.
CHLOR-ALKALI INDUSTRIES
The important products of the Chloro-alkali industry are caustic soda, soda The method used to produce
ash, poly vinyl chloride (PVC), hydrochloric acid, calcium chloride, both sodium hydroxide and
chlorine and bleaching powder etc. and their main raw material is brine, chlorine is
which is the saturated solution of sodium chloride salt. A. Electrolysis
Chlorine-caustic soda B. Contact Process
Electrolysis is a method used in the production of both caustic soda C. Chamber process
(sodium hydroxide) and chlorine. D. None
Caustic soda production
Process Description:
Caustic soda is produced through the following processes (cells)
1. Mercury process (88% of total),
2. Diaphragm Process (7%),
3. Membrane Process (4%)

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CHEMICAL ENGINERING DEPARTMENT
1. Mercury process
The operation of the mercury cell is different from the other cells. It has
electrolyzer and decomposer portions both have anodes and cathodes
separately. Mercury is hanging in the cell and act as a cathode in hanging
form and two anodes are used.

Figure 5.1 mercury cell

The brine break in the sodium ions and chloride ions. Chloride ions released
as in the form of chlorine gas.
In electrolyzer sodium ions are combined with the mercury to form sodium
amalgam (Na-Hg) and chloride ions are released in the form of the chlorine
gas. This amalgam is send to the decomposer where water is already present
in the form of hydrogen ions and hydroxide ions.
Here sodium from amalgam combine with the hydroxide ions to form
caustic soda and hydrogen ions are released in the form of hydrogen gas.
Mercury cell is made of stainless steel (SS) coated with rubber.
2. Diaphragm Process
Using this process we can produced 12 % concentrated caustic soda. The
formation of unreacted sodium chloride is its disadvantage. The diaphragm
cell contains anode and cathode compartments. Both are made of magnesite
and diaphragm wall is made of non-asbestos material.

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CHEMICAL ENGINERING DEPARTMENT
Add (80%-90%) saturated brine and water into the diaphragm cell. It will
produce sodium ions, chloride ions, hydrogen ions and hydroxide ions.

Figure 5.2 diaphragm cell

At anode chloride, ions are combining to form chlorine gas. At the cathode,
hydrogen ions are combining to form hydrogen gas. Caustic soda (12%
concentrated) and unreacted sodium chloride (14%) is formed as products.
3. Membrane Process:
The membrane cell is same as the diaphragm cells but in here, the selective
permeable membrane replaces diaphragm wall. In the membrane cell, the
anode is made of titanium and cathode is made of nickel. The membrane is
called as selective permeable membrane because it allows only sodium ions
to pass through it so the leakages of chloride ions are reduced. The caustic
soda concentrated using evaporator. The chlorine and hydrogen gas produce
in this process are send to the hydrochloric acid furnace where they react
which each other to form hydrochloric acid.

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 Figure 5.3 membrane cell

AGRO-CHEMICAL INDUSTRIES
Fertilizer industry
Introduction
Fertilizers are compounds given to plants with the intention of promoting
growth; they are usually applied either via the soil, for uptake by plant roots,
or by foliar feeding, for uptake through leaves. It is now known that at least
16 plant-food elements are necessary for the growth of green plants. These
plant-nutrients are called essential elements. In the absence of any one of
these essential elements, a plant fails to complete its life cycle, though the
disorder caused can, however, be corrected by the addition of that element.
Fertilizers application and the use of suitable fertilizers are recommended
for higher crop yields in productive farming.
Needs fertilizers
Increasing agricultural production by area increasing process is no longer
possible as cultivable land left over is only marginal.
Further a considerable cultivable land is being diverted year after year for
industrial purpose and housing etc. hence self-sufficiency in food lies in
increasing the yield per unit area per unit time through adoption of modern
agricultural technology.

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CHEMICAL ENGINERING DEPARTMENT
Hence, there is need for an efficient use of fertilizers as major plant nutrient
resource in enhancing the farm productivity.
Fertilizers can be divided into macronutrients or micronutrients.
There are three macronutrients:
 nitrogen,
 potassium, and
 phosphorus,
Which are consumed in high quantities and normally present as whole
number percentages in plant tissues. There are many micronutrients, and
their importance and occurrence differ from plant to plant. In general, most
present from 5 to 100 parts per million (ppm) by mass. Examples of
micronutrients are as follows: boron (b), calcium (ca), copper (cu),
magnesium (mg), iron (fe), molybdenum (mo), and zinc (zn).
Classification of Fertilizers
Natural fertilizers
These include both plant and animal bi-products. They contain low quantity
of nutrients as compared to synthetic fertilizers.
Synthetic fertilizers
Synthesized materials are also called artificial, and mainly contains the
three primary ingredients of nitrogen (n), phosphorus (p) and potassium (k),
which are known as n-p-k fertilizers or compound fertilizer. The mass
percent nitrogen is reported directly. However, phosphorus is reported as
diphosphorus pentoxide (P2O5), and potassium is reported as potash or
potassium oxide (K2O), consequently, an 18-51-20 fertilizer would have
18% nitrogen as n, 51% phosphorus as P2O5, and 20% potassium as K2O.
If nitrogen is the main element, they are often described as nitrogen
fertilizers.
Nitrogen: it is very important nutrient for plants and it seems to have the
quickest and most pronounced effect. In the case of nitrogenous fertilizers,
nitrogen may be in the ammonical, nitrate (or a combination thereof) or
amide form.

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CHEMICAL ENGINERING DEPARTMENT
Ammonical form of nitrogen is contained in fertilizers like ammonium
sulphate, ammonium chloride, etc. nitrate nitrogen is contained in fertilizers
like ammonium nitrate, calcium ammonium nitrate, etc. The amide nitrogen
is contained in urea.
Phosphorus: it is the second fertilizer element, it is an essential constituent
of every living cells and for the nutrition of plant and animal, it takes active
part in all types of metabolism of plant. Phosphorus plays an important role
in energy transformations and metabolic processes in plants.
Potassium: it plays an important role in the maintenance of cellular
organizations by regulating permeability of cell membranes and keeping the
protoplasm in a proper degree of hydration. It activates the enzymes in
protein and carbohydrate metabolism and translocation of carbohydrates
and imparts resistance to plants against fungal and bacterial disease.
Urea
Urea is white crystalline solid. It is manufactured in prilled as wellas
granular form. The prilled and granular fertilizers are white in color, free
flowing, readily soluble in water and both contain 46% nitrogen. Because
of its high solubility, it is suitable for solution fertilizers and foliar
application. It is not explosive so easy to transport.
Uses of urea
It is used:
 As a solution fertilizer and foliar application due to good solubility.
 As protein food supplement
 In making utensils in the form of melamine.
 As an ingredient in tooth whitening products, dish soap.
 As a raw material for the manufacture of plastics.
Production of urea
General process involving in urea production are:
 once through process
 partial recycle process
 total recycle process

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CHEMICAL ENGINERING DEPARTMENT
Main reactions in the production of urea are:
2NH3+ CO2 = NH2COONH4
NH2COONH4 = NH2CONH2 + H2O
Once through process
The once-through process is the simplest of the three types.
Liquid ammonia and carbon dioxide are sent to the reactor. The carbamate
strippers steam heat the effluent to remove unreacted ammonia and carbon
dioxide, with the stripped effluent containing approximately 80% urea.
While this process is the simplest of the urea processes, it is tried to the co-
production of some other material, e.g. ammonium sulphate, ammonium
nitrate, nitric acid, for which ammonia can be used.
Partial recycle process
The partial-recycle method a portion of the unreacted ammonia and carbon
dioxide present in the off-gas recycles back to ammonia reactor. Recycling
reduces the amount of input ammonia required. With this method, the
amount of unreacted ammonia that is about 15% of that generated by the
once-through process.
Total recycle process
In the total recycle process, the unreacted ammonia and carbon dioxide from
the off-gas are returned to the urea reactor (conversion is 99%).
The total recycle process can be divided into:
 Hot gas mixture recycle
 stemicarbon urea stripping process
Hot mixture recycle process
In this process, mixture of CO2 and NH3 is recycled back to urea reactor.
The carbamate is decomposed in one or more decomposers, each having a
lower pressure than the previous one. so pressure is reduced and all evolved
gases must be recompressed to the reactor pressure and this is too expensive.
Stemicarbon urea stripping process
The most popular method designed to minimize the use of energy is by
stripping with CO2.

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CHEMICAL ENGINERING DEPARTMENT
The process involves following steps:
1. reaction of NH3 and CO2
2. stripping with CO2
3. partial condensation of NH3 and CO2
4. rectification column
5. evaporating
6. prilling and granulating

Figure 6.1 stemicarbon urea stripping process

PAPER AND PULP INDUSTRY

Introduction
Pulp is a lignocellulosic fibrous material. It is prepared by chemical or
mechanical separation of cellulose fibers from wood, fiber crops or waste
paper. The wood fiber sources required for pulping are, “45% sawmill
residue, 21% logs and chips, and 34% recycled paper. A mixture of
cellulose material, such as wood, paper, and rags, ground up and moistened
to make paper.

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CHEMICAL ENGINERING DEPARTMENT
Pulp and paper mills are highly complex and integrate many different
process areas including wood preparation, pulping, chemical recovery,
bleaching, and papermaking to convert wood to the final product. The final
product often determines processing options and the type of wood
processed.
The pulp for papermaking may be produced from virgin fiber by chemical
or mechanical means or may be produced by the re-pulping of paper for
recycling. Wood is the main original raw material. Paper for recycling
accounts for about 50 % of the fibers used but in a few cases straw, hemp,
grass, cotton and other cellulose-bearing material can be used. Paper
production is basically a two-step process in which a fibrous raw material
is first converted into pulp, and then the pulp is converted into paper. The
harvested wood is first processed so that the fibers are separated from the
unusable fraction of the wood, the lignin. Pulp making can be done
mechanically or chemically. The pulp is then bleached and further
processed, depending on the type and grade of paper that is to be produced.
In the paper factory, the pulp is dried and pressed to produce paper sheets.
Post-use an increasing fraction of paper and paper products is recycled.
Non-recycled paper is either land filled or incinerated.

Figure 7.1: pulp and paper making process

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CHEMICAL ENGINERING DEPARTMENT
Process Descriptions
Pulp production process
Sulfite Pulp
The sulfite process produces wood pulp, which is almost pure cellulose
fibers by using various salts of sulfurous acid to extract the lignin from
wood chips in large pressure vessels called digesters. The salts used in the
pulping process are either sulfites (SO32−), or bisulfites (HSO3−),
depending on the pH. The counter ion can be sodium (Na+), calcium
(Ca2+), potassium (K+), magnesium (Mg2+) or ammonium (NH4+).
Kraft Pulp
The kraft process (also known as kraft pulping or sulfate process) is a
process for conversion of wood into wood pulp consisting of almost pure
cellulose fibers. It entails treatment of wood chips with a mixture of sodium
hydroxide and sodium sulfide, known as white liquor that breaks the bonds
that link lignin to the cellulose. Steps involved in the Kraft process are as
follows: 1) Impregnation, 2) Cooking, 3) Blowing, 4) Screening, 5)
Washing and 6) Bleaching
Impregnation:
Common wood chips used in pulp production are 12–25 millimeters (0.47–
0.98 in) long and 2–10 millimeters (0.079–0.394 in) thick. The chips
normally first enter the pre-steaming where they are wetted and preheated
with steam. Cavities inside fresh wood chips are partly filled with liquid and
partly with air. The steam treatment causes the air to expand and about 25%
of the air to be expelled from the chips
Cooking:
The wood chips are then cooked in pressurized vessels called digesters.
Some digesters operate in a batch manner and some in a continuous process.
There are several variations of the cooking processes for both the batch and
the continuous digesters.

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CHEMICAL ENGINERING DEPARTMENT
Digesters producing 1,000 tons or more of pulp per day are common
The solid pulp (about 50% by weight of the dry wood chips) is collected
and washed. At this point, the pulp is known as brown stock because of its
color. The combined liquids, known as black liquor (because of its color),
contain lignin fragments, carbohydrates from the breakdown of
hemicellulose, sodium carbonate, sodium sulfate and other inorganic salts.
Blowing:
The finished cooked wood chips are blown by reducing the pressure to
atmospheric pressure. This releases a lot of steam and volatiles
Screening:
Screening of the pulp after pulping is a process whereby the pulp is
separated from large shives, knots, dirt and other debris. The accept is the
pulp. The material separated from the pulp is called reject.
The screening section consists of different types of sieves (screens) and
centrifugal cleaning. The sieves are normally set up in a multistage cascade
operation because considerable amounts of good fibres can go to the reject
stream when trying to achieve maximum purity in the accept flow
Washing:
The brown stock from the blowing goes to the washing stages where the
used cooking liquors are separated from the cellulose fibers. Normally a
pulp mill has 3-5 washing stages in series. Pulp washers use counter current
flow between the stages such that the pulp moves in the opposite direction
to the flow of washing waters
Bleaching:
In a modern mill, brown stock (cellulose fibers containing approximately
5% residual lignin) produced by the pulping is first washed to remove some
of the dissolved organic material and then further delignified by a variety of
bleaching stages

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CHEMICAL ENGINERING DEPARTMENT
Paper production process
The following are steps for the production of paper
1. Stock preparation
2. Beating and refining
3. Filling and loading
4. Sizing
5. Coloring
6. Sheet forming, pressing and drying
1. Stock preparation
Paper making pulps are conveniently handled as aqueous slurries so that
they can be conveyed, measured, subjected to desired mechanical
treatments and mixed with non-fibrous additive
2. Beating and refining
This type of treatment is used to improve the strength and other physical
properties
3. Filling and loading
Filling process is carried out to make the paper making furnish. For this
purpose, mostly pigments are used. Fillers can improve brightness, opacity,
softness, smoothness and ink receptivity.
4. Sizing: It is the process of adding material to the paper in order to render
the sheet more resistant to penetration by liquids.
5. Coloring
The color of most papers and paperboards that are made from pulp is
achieved by addition of dyes and other colored components
6. Sheet forming, pressing and drying
Sheet forming
Commonly Cylinder machines are used for sheet forming. Fourdriniers are
used as standards in industry to produce all grades of paper. They vary 1-10
m in width and may be >200 m long

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CHEMICAL ENGINERING DEPARTMENT
Sheet pressing
The sheet leaving the wet contains almost 4 parts of water per part of fiber.
For this sheet are pressed between rotary presses.
Sheet drying
At a water content of 1.2-1.9 parts of water per part of fiber, mechanical
means for drying are not feasible, for this evaporation, drying process is
applied.
FERMENTATION TECHNOLOGY
Introduction
Industrial fermentation is the intentional use of fermentation by
microorganisms such as bacteria and fungi to make products useful to
humans. Fermented products have applications as food as well as in general
industry. Some commodity chemicals, such as acetic acid, citric acid, and
ethanol are made by fermentation. The rate of fermentation depends on the
concentration of microorganisms, cells, cellular components, and enzymes
as well as temperature, pH and for aerobic fermentation oxygen. Product
recovery frequently involves the concentration of the dilute solution. Nearly
all commercially produced enzymes, such as lipase, invertase and rennet,
are made by fermentation with genetically modified microbes. In some
cases, production of biomass itself is the objective, as in the case of baker's
yeast and lactic acid bacteria starter cultures for cheese making.
There are five major groups of commercially important fermentation
processes:
 Production of microbial cells (biomass) e.g. single cell protein (SCPs),
Bakers’ Yeast, Lactobacillus, E. coli etc.
 Production of microbial enzymes e.g. catalase, amylase, protease,
pectinase etc.
 Production of microbial metabolites e.g.
 Primary metabolites: ethanol, citric acid, glutamic acid, lysine,
vitamins e.t.c
 Secondary metabolites: all antibiotics fermentations

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CHEMICAL ENGINERING DEPARTMENT
  Production of recombinant proteins e.g. insulin, interferon, hepatitis B
vaccine, streptokinase
 Transformation (chiral catalysts) e.g. phenylacetylcarbinol, steroid
biotransfromation
These types are not necessarily disjoint from each other, but provide a
framework for understanding the differences in approach. The organisms
used may be bacteria, yeasts, molds, animal cells, or plant cells. Special
considerations are required for the specific organisms used in the
fermentation, such as the dissolved oxygen level, nutrient levels, and
temperature.
General overview of industrial fermentation
In most industrial fermentations, the organisms are submerged in a liquid
medium; in others, such as the fermentation of cocoa beans, coffee cherries,
and miso, fermentation takes place on the moist surface of the medium.
There are also industrial considerations related to the fermentation process.
For instance, to avoid biological process contamination, the fermentation
medium, air, and equipment are sterilized. Foam control can be achieved by
either mechanical foam destruction or chemical anti-foaming agents.
Several other factors must be measured and controlled such as pressure,
temperature, agitator shaft power, and viscosity. An important element for
industrial fermentations is scale up. This is the conversion of a laboratory
procedure to an industrial process. It is well established in the field of
industrial microbiology that what works well at the laboratory scale may
work poorly or not at all when first attempted at large scale. It is generally
not possible to take fermentation conditions that have worked in the
laboratory and blindly apply them to industrial-scale equipment. Although
many parameters have been tested for use as scale up criteria, there is no
general formula because of the variation in fermentation processes. The
most important methods are the maintenance of constant power
consumption per unit of broth and the maintenance of constant volumetric
transfer rate.

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CHEMICAL ENGINERING DEPARTMENT
Phases of microbial growth:
When a particular organism is introduced into a selected growth medium,
the medium is inoculated with the particular organism. Growth of the
inoculum does not occur immediately, but takes a little while. This is the
period of adaptation, called the lag phase. Following the lag phase, the rate
of growth of the organism steadily increases, for a certain period—this
period is the log or exponential phase. After a certain time of exponential
phase, the rate of growth slows down, due to the continuously falling
concentrations of nutrients and/or continuously increasing (accumulating)
concentrations of toxic substances. This phase, where the increase of the
rate of growth is checked, is the deceleration phase. After the deceleration
phase, growth ceases and the culture enters a stationary phase or a steady
state. The biomass remains constant, except when certain accumulated
chemicals in the culture lyse the cells (chemolysis). Unless other
microorganisms contaminate the culture, the chemical constitution remains
unchanged. If all of the nutrients in the medium are consumed, or if the
concentration of toxins is too great, the cells may become scenescent and
begin to die off. The total amount of biomass may not decrease, but the
number of viable organisms will decrease.
Fermentation Medium:
The microbes used for fermentation grow in (or on) specially designed
growth medium which supplies the nutrients required by the organisms. A
variety of media exists, but invariably contains a carbon source, a nitrogen
source, water, salts, and micronutrients. In the production of wine, the
medium is grape must. In the production of bio-ethanol, the medium may
consist mostly of whatever inexpensive carbon source is available.
Carbon sources are typically sugars or other carbohydrates, although in the
case of substrate transformations (such as the production of vinegar) the
carbon source may be an alcohol or something else altogether.

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CHEMICAL ENGINERING DEPARTMENT
For large scale fermentations, such as those used for the production of
ethanol, inexpensive sources of carbohydrates, such as molasses, corn steep
liquor, sugar cane juice, or sugar beet juice are used to minimize costs. More
sensitive fermentations may instead use purified glucose, sucrose, glycerol
or other sugars, which reduces variation and helps ensure the purity of the
final product. Organisms meant to produce enzymes such as beta
galactosidase, invertase or other amylases may be fed starch to select for
organisms that express the enzymes in large quantity.
Fixed nitrogen sources are required for most organisms to synthesize
proteins, nucleic acids and other cellular components. Depending on the
enzyme capabilities of the organism, nitrogen maybe provided as bulk
protein, such as soy meal; as pre-digested polypeptides, such as peptone or
tryptone; or as ammonia or nitrate salts. Cost is also an important factor in
the choice of a nitrogen source. Phosphorus is needed for production of
phospholipids in cellular membranes and for the production of nucleic
acids. The amount of phosphate which must be added depends upon the
composition of the broth and the needs of the organism, as well as the
objective of the fermentation. For instance, some cultures will not produce
secondary metabolites in the presence of phosphate.
Growth factors and trace nutrients are included in the fermentation broth for
organisms incapable of producing all of the vitamins they require. Yeast
extract is a common source of micronutrients and vitamins for fermentation
media. Inorganic nutrients, including trace elements such as iron, zinc,
copper, manganese, molybdenum and cobalt are typically present in
unrefined carbon and nitrogen sources, but may have to be added when
purified carbon and nitrogen sources are used.
Fermentations which produce large amounts of gas (or which require the
addition of gas) will tend to form a layer of foam, since fermentation broth
typically contains a variety of foamreinforcing proteins, peptides or
starches.

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To prevent this foam from occurring or accumulating, antifoaming agents
may be added. Mineral buffering salts, such as carbonates and phosphates,
may be used to stabilize pH near optimum. When metal ions are present in
high concentrations, use of a chelating agent may be necessary.
Production processes
Biomass production
Microbial cells or biomass is sometimes the intended product of
fermentation. Examples include single cell protein, baker’s yeast,
Lactobacillus, E. coli, and others. In the case of single-cell protein, algae
are grown in large open ponds, which allow photosynthesis to occur. If the
biomass is to be used for inoculation of other fermentations, care must be
taken to prevent mutations from occurring.
Production of extracellular metabolites
Microbial metabolites can be divided into two groups: those produced
during the growth phase of the organism, called primary metabolites and
those produced during the stationary phase, called secondary metabolites.
Some examples of primary metabolites are ethanol, citric acid, glutamic
acid, lysine, vitamins and polysaccharides. Some examples of secondary
metabolites are penicillin, cyclosporin A, gibberellin, and lovastatin.
Primary metabolites
Primary metabolites are compounds made during the ordinary metabolism
of the organism during the growth phase. A common example is ethanol or
lactic acid, produced during glycolysis. Citric acid is produced by some
strains of Aspergillus niger as part of the citric acid cycle to acidify their
environment and prevent competitors from taking over. Glutamate is
produced by some Micrococcus species, and some Corynebacterium
species produce lysine, threonine, tryptophan and other amino acids. All of
these compounds are produced during the normal "business" of the cell and
released into the environment. There is therefore no need to rupture the cells
for product recovery.

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Secondary metabolites
Secondary metabolites are compounds made in the stationary phase;
penicillin, for instance, prevents the growth of bacteria, which could
compete with Penicillium molds for resources.
Some bacteria, such as Lactobacillus species, are able to produce
bacteriocins, which prevent the growth of bacterial competitors as well.
These compounds are of obvious value to humanswishing to prevent the
growth of bacteria, either as antibiotics or as antiseptics (such as gramicidin
S). Fungicides, such as griseofulvin are also produced as secondary
metabolites. Typically, secondary metabolites are not produced in the
presence of glucose or other carbon sources, which would encourage
growth, and like primary metabolites, are released into the surrounding
medium without rupture of the cell membrane.
Production of intracellular components
Of primary interest among the intracellular components are microbial
enzymes: catalase, amylase, protease, pectinase, glucose isomerase,
cellulase, hemicellulase, lipase, lactase, streptokinase and many others.
Recombinant proteins, such as insulin, hepatitis B vaccine, interferon,
granulocyte colony-stimulating factor, streptokinase and others are also
made this way. The largest difference between this process and the others
is that the cells must be ruptured (lysed) at the end of fermentation, and the
environment must be manipulated to maximize the amount of the product.
Furthermore, the product (typically a protein) must be separated from all of
the other cellular proteins in the lysate to be purified.
Transformation of substrate
Substrate transformation involves the transformation of a specific
compound into another, such as in the case of phenylacetylcarbinol, and
steroid biotransformation, or the transformation of a raw material into a
finished product, in the case of food fermentations and sewage treatment.

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Food fermentation
Ancient fermented food processes, such as making bread, wine, cheese,
curds, idli, dosa, etc., can be dated to more than seven thousand years ago.
They were developed long before man had any knowledge of the existence
of the microorganisms involved. Some foods such as Marmiteare the
byproduct of the fermentation process, in this case in the production of beer.
Ethanol fuel
Fermentation is the main source of ethanol in the production of Ethanol fuel.
Common crops such as sugar cane, potato, cassava and corn are fermented
by yeast to produce ethanol which is further processed to become fuel.

SUGAR PROCESSING
Introduction
Raw materials for sugar production are sugar cane -- a large tropical grass,
sugar beet root-a root crop in temperate zone of north and corn (only used
for sweeteners)
Sugar is produced in 121 Countries and global production now exceeds 120
Million tons a year. Approximately 70% is produced from sugar cane. The
remaining 30% is produced from sugar beet, a root crop resembling a large
parsnip grown mostly in the temperate zones of the north.
Sugar manufacturing industries can be categorized as:
Raw sugar manufacturing industries: raw sugar (brown in color and
unsuitable for direct consumption) is produced, and sent to refineries and
converted to refined sugar (white sparkling in appearance of high purity and
suitable for direct human consumption, pharmaceutical, beverages etc.).
This can be separate raw sugar or refined sugar manufacturing or an
integration of the two called as raw sugar factories-cum refineries, in which
raw sugar is produced from cane and refined sugar is manufactured in small
installed refinery units by processing the raw sugar.

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Plantation white sugar factories:-in these factories, white sugar is
manufactured directly from cane for direct consumption or industrial use
employing more complicated techniques in clarification of juice and so in
crystallization of sugar. Slightly produces a sugar containing higher
impurities than a sugar of refinery industries. Most sugar factories in
Ethiopia are a type of plantation white sugar factories.
Sugarcane is generally about 70% water, 15% fibrous material and the
remaining is dissolved solids. The major composition of sugarcane when
becomes matured we can observe clearly the following characteristics:
Sugarcane: 100%, Water: 70 to 73%, Fiber: 12 to 15%, Sugar (sucrose): 11
to 14% and Dissolved non-sugar solids: 2 to 3%
Sugar manufacturing process
The chemical formula for sucrose is C12H22O11. Under conditions of low pH
or under influence of certain enzymes like invertase sucrose is hydrolyzed
into two monosaccharide. Glucose and levulose in equimolecular
proportions according to equation: C12H22O11 + H2O C6H12O6 + C6H12O6
Sugar production from sugarcane uses several processes and unit operations
(a set of operations in which separation, mixing or conversion by reaction
takes place) this process is summarized for plantation white sugar
production in figure 10. 1.
The following are the main unit operations involved in manufacturing sugar
from sugarcane:
1. Cane preparation
2. Extracting of juice from sugarcane
3. Clarification of cane juice
4. Evaporation of juice
5. Sugar boiling or vacuum pans operation
6. Crystallization
7. Centrifuging (separation of mother liquor from crystal sugar)
8. Sugar drying, grading, packing and storing

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Figure 10.1 plantation white sugar production

Cane Preparation
The object of cane preparation is
 To cut cane into short pieces for feeding the mills
 To rupture the cells, without extracting juice.
The preparatory devices commonly employed and installed before the
milling tandem, are classified into three types:-

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 1. Knives, which cut the cane to pieces.
2. Shredders, which shred cut cane into long fine pieces.
3. Fibrizer, system combining the features of both (I) & (II),
Percentage of cells opened to the total, which is indicative of the extent of
cane preparation, is
1. 50-60% in the case of two sets of knives runs in the direction of carrier,
2. 85-90% with a combination of knives and shredder, while for unigrator
or fibrizor it would be 75-80%.
In the case of knives run in opposite direction to the flow of cane, the
preparation index can be 65-70% depending on whether one or both the sets
are revolving in reverse direction.
Cane kicker or equalizer: it is installed on the carrier to prevent excessive
cane being fed to cane leveler, which causes jamming of the leveler set. It
consists of a steel shaft directly coupled to a motor with arms or knives
mounted on it, running normally at 50-100 rpm. In reverse direction to the
flow of cane on the cane carrier. When arms or angles are secured to the
shaft, the rpm and power requirement are low but when knives are fitted
and rpm about 100 or so the power requirement is higher since some cutting
action is also envisaged along with maintaining uniform feed to knives,
which forms the main function of this piece of equipment. In some factories
before a shredder or a fibrizer an equalizer or leveler of the same design as
a cane kicker is installed after the cane has passed through first one or two
sets of knives to ensure even distribution of feed.
Cane knives
Cane preparation by knives essentially consists in disintegrating the hard
rind, and nodes, and breaking the cane to short pieces, which in effect
increases the mill capacity and efficiency of juice extraction. It consists of
forged steel shaft with cast steel hubs to which are secured knives in
different planes. The shaft supported on double row ball bearings is coupled
to a motor and revolves at about 600 rpm.

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Different designs of knives are adopted, some of which are of reversible
blade types, while some are of bent or circular type. The knives are made of
shock resisting steel with stellited edges. The knives are enclosed in M.S.
hoods attached to cane carrier frame and provided with bolted doors on top.
The pitch of the knives, i.e. the distance between two successive circles of
knife rotation, is usually about 50 mm. but is reduced to 25 mm. or lower,
while handling hard and thin canes in some sugar producing regions, by
increasing the cutting planes.
The first set of knives known as leveler is installed over the carrier with
clearance between the tips of knives and the carrier of 50-150mm. as it has
to chop whole cane; while with the 2nd set of knives which cuts the partially
cut cane from leveler the clearance is 30-50mm. This unit known as cutter
is located at a distance of about 5-6 m. from the leveler set on the carrier.
The efficiency of knives decided by the proportion of cut cane is dependent
to a large extent on the clearance, which can be varied by adjusting position
of knives and the motor.
Shredder
Shredder is essentially a hammer mill adapted to the function of sugarcane
pulverising and swing hammer type shredders of different designs are
common in sugar producing countries including
India. On forged steel shaft are fitted a number of steel discs to which are
attached hammers with hard faced tips, and provided with hardened bush at
the pin. The hammers revolve on pivots.
Shredders are housed in thick steel plates, with inspection door provided at
the discharge end. As the shredder starts rotating, the hammers are thrown
out radially by centrifugal force. The shredders rotate at 1000-1200 rpm.
and are usually directly coupled through flexible coupling to electric motor
or driven by steam turbines, the total installed power being about 20-26 HP
per ton fiber per hour, while actual mean-power consumption is 30-50%
lower than this. Feed to Shreddar is from top, which is pulverized between
the anvil bars, and rotating hammers.

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Influence of cane preparation:-
It is now an established fact that fine cane preparation is key to efficient
milling in as much as it exerts influence on mill extraction as well as
throughput. Fine preparation calls for higher power requirement for the
preparatory devices like shredders and fibrizers, but results in reduction of
power consumption at mills. In Australia great stress is laid on cane
preparation by employing heavy-duty shredders and the power consumed
for cane preparatory devices is very high around 70-90% of the total power
for mills whereas in Indian sugar mills the installed hp. For cane,
preparation is about 40-50% of the power of mill turbines.
Extraction of juice:

Figure 10.2 Extraction by mill

Figure 10.3 Tandem of Sugar mills

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CHEMICAL ENGINERING DEPARTMENT
Milling:
The prepared cane passes through a series of mills called a tandem or
millingtrain. These mills are composed of massive horizontal cylinders or
rolls in groups of three, one on the top and two on the bottom in the triangle
formation. The rolls are 50 –100 cm diameter and 1 –3 m long and have
grooves that are 2 –5 cm wide and deep around them. There may be
anywhere from 3 – 7 of these 3 roll mills in tandem, hence the name. These
mills, together with their associated drive and gearing, are among the most
massive machinery used by industry. The bottom two rolls are fixed, and
the top is free to move up and down. The top roll is hydraulically loaded
with a force equivalent about 500 t. The rolls turn at 2 – 5 rpm, and the
velocity of the cane through them is 10- 25cm/s. After passing through the
mill, the fibrous residue, from the cane, called bagassae, is carried to the
next mill by bagassae carriers and is directed from the first squeeze in a mill
to the second by turn plate.
In order to, achieve a good extraction, a system of imbibition is used,
bagassae going to the final mill is sprayed with water to extract whatever
sucrose remains; the resultant juice from the last mill is then sprayed on the
bagasse mat going to the next to last mill, and so on. The combination of all
these juices is collected from the first mill and is mixed with the juice from
the crusher. The result is called the mixed juice and is the material that goes
forward to make the sugar.
Imbibition
In order to extract as much as possible the sugar it contains, it is therefore
necessary to resort to artifice. Since this moisture content cannot be reduced,
the effort made is to replace by water the juice comprising it. This process
is called imbibition. With dry crushing, the limit of extraction is very soon
attained in practice. After first mill the moisture content of bagasse is
reduced to 60%; after second mill it will be about 50%and after third mill it
will not go far from 45%; that means, the maximum extraction possible with
simple pressure is attained.

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CHEMICAL ENGINERING DEPARTMENT
However, if at this stage the bagasse is sprayed with water, the water will
spread in the bagasse and dilute the juice that it contains; and then when
pressure is applied to the bagasse by the following mill and the bagasse is
compressed to its final moisture content, about 45%. However, this
moisture consists no larger of absolute juice but of diluted juice. Hence, the
sugar will have been extracted in place of the dilution water. This operation
may be repeated to obtain minimum sugar content of bagasse from the last
mill of the tandem.
Imbibition systems
Simple imbibition
The procedure in which water is added to the bagasse after each mill is
called simple imbibition. If the water is added at one point only, for
example, between the last two mills, it is called single simple imbibition. If
it is added at, two points between the last two mills and between penultimate
mills it is called double simple imbibition. Similarly, if it is applied at three
points, it is called triple simple imbibition, and so on.
Compound imbibition
Staring from single simple imbibition the diluted juice from last mill is
mostly water and it has been sent back before the preceding mill, this is
called double compound imbibition. If again the juice obtained from
penultimate mill is retuned before the previous mill, it is called triple
compound imbibition, and so on. This system will consume more water,
which has to be evaporated latter at evaporation plant.
Hot and cold imbibitions: it appears that temperature has a little effect up to
the neighborhood of 60-70oC. Above this point, the efficiency of imbibition
is slightly superior with hot water, the gain in the extraction reaching 0.4%
in most favorable cases. The material of cell wall of the cane, which is
impermeable only by osmosis, would be softened and water thus would
have direct access to juice contained in the cell.

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Advantages of hot imbibition
 Slight gain in extraction with hot water, some times rather difficult
to detect and often negligible.
 The mills do not take the feed as well with hot imbibition as with
cold.
 It is used to consume condensate from the latter vessels of multiple
effect and save cold water.
 Cane carries on its rind a certain quantity of wax, most of which is
found at the wax ing below the node. Most of the waxes melt at
temperature between 60-800C, and imbibition with hot water
increases the proportion of the wax passing in to the mixed juice.
But experiment has shown that there is no appreciable effect by
temperature of imbibition on the amount of wax in the mixed juice.
Bagasse:
The bagasse from the last mill is about 50-wt% water and will burn directly.
Diffusion bagasse is dripping wet and must be dried in a mill or some sort
of bagasse press. Most bagasse is burned in the boilers that run the factories
Juice Clarification:
The juice from either milling or diffusion is about 12 – 18% solids, 10 – 15
pol (polarization) (percent sucrose), and 70 – 85% purity. These figures
depend upon geographical location, age of cane, variety, climate,
cultivation, condition of juice extraction system, and other factors. As
dissolved material, it contains in addition to sucrose some invert sugar, salts,
silicates, amino acids, proteins, enzymes, and organic acids; the pH is 5.5 –
6.5. It carries suspension cane fibre, field soil, silica, bacteria, yeasts, molds,
spores, insect parts, chlorophyll, starch, gums, waxes, and fats. It looks
brown and muddy with a trace of green from the chlorophyll.
In the juice from the mill, the sucrose is inverting (hydrolyzing to glucose
and fructose) under the influence of native invertase enzyme or an acid pH.

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The first step of processing is to stop the inversion by raising the pH to 7.5
and heating to nearly 100oC to inactivate the enzyme and stop
microbiological action. At the same time, a large fraction of the suspended
material is removed by settling. The cheapest source of hydroxide is lime,
and this has the added advantage that calcium makes many insoluble salts.
Clarification by heat and lime, a process called defecation, was practiced in
Egypt many centuries ago and remains in many ways the most effective
means of purifying the juice.
Phosphate is added to juices deficient in phosphate to increase the amount
of calcium phosphate precipitate, which makes a floc that helps
clarification. When the mud settles poorly, polyelectrolyte flocculants such
as polyacrylamides are sometimes used. The heat and high pH serve to
coagulate proteins, which are largely removed in clarification.
The equipment used for clarification is of the Dorr clarifier type. It consists
of a vertical cylindrical vessel composed of a number of trays with conical
bottoms stackedone over the other. The limed raw juice enters the center of
each tray and flows towardthe circumference. A sweep arm in each tray
turns quite slowly and sweeps the settled mud toward a central mud outlet.
The clear juice from the top circumference overflows into a header.
Diffusion juice contains less suspended solids than mill juice. In many
diffusion operations, some or all of the clarification is carried out in the
diffuser by adding lime.
The mud from clarification is filtered on Oliver rotary vacuum filters to
recovery the juice. The mud mostly consists of field soil and very fined
divided fibre. It also contains nearly all the protein (0.5 wt% of the juice
solids) and cane wax. The mud is returned to the fields.
Although the clarification removes most of the mud, the resulting juice is
not necessarily clear.
The equipment is often run at beyond its capacity and control slips a little
so that the clarity of the clarified juice is not optimum. Suspended solids
that slip past the clarifiers will be in the sugar.

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CHEMICAL ENGINERING DEPARTMENT
Clarified juice is dark brown. The color is darker than raw juice because the
initial heating causes significant darkening.
Filtration process
 The clear juice from the Dorr Clarifiers is sent to evaporation plant
where as the muddy juice is sent to filtration process where as
maximum sugar (pol) as possible is recovered from the mud.
 Muddy juice conditioning for filtration
Mud: which is a filter aid is added and mixed with muddy juice in the -
mud mixer. The added up the stickiness of mud; gives it body and forms a
fibrous mat through which the filtrate will be drawn. The quantity of
bagacillo used is about the quantity of dry mud solids present.
Muddy juice heating: Viscosity of muddy juice and especially that of the
gums and waxes that have to pass through the filtering surface decreases as
the temperature increases. Therefore, filtering at high temperature is
preferable. 80 - 850C is recommended. Such high temperature also destroys
bacterial activity. The muddy juice is thus heated to the said temperature
range in the mud heater.
Liming: Alkaline juices filter better than acid or neutral juices. Hence the
pH of muddy juice has to be raised to 8 – 8.5. This is done by adding to
muddy juice.
Juice evaporation
Juice evaporation is to remove by far the greatest weight of material, water
from the clarified juice without effecting crystallization process. Hence, the
evaporation process is the process of concentrating juice from about 150
brix to 550-650 brix. Based on the concept of steam economy four
evaporator arrangements are realized.
1. Single effect evaporators
2. Single effect evaporators with vapor recompression
3. Multiple effect evaporators
4. Quadruple effect evaporators

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CHEMICAL ENGINERING DEPARTMENT
1. Single effect evaporators
The required capacity is so small. Steam is cheap. The vapor is so
contaminated that it cannot be reused.
2. Single effect evaporators with vapor recompression
The simplest means of reducing the energy requirements of evaporators in
compressing the vapor from the single evaporator so that the vapor can be
used as heating medium in the same evaporator. The pressure and
consequently the temperature of vapor from the evaporator is increased to a
certain extent (i.e., to the pressure and temperature that prevail in the heating
calandria of the evaporator) by the aid of a compressor.
3. Multiple -effect evaporators
Multiple effect evaporators are the principal means (arrangement) in use for
economizing on energy consumption. They can be double, triple, etc. As the
number of effects increases, energy (steam) saving increases, but the rate of
evaporation (which is minimum when the number of effects is greater than
five and maximum when the number of effects is three) decreases. The rate
of evaporation falls with the number of effects because the driving force,
log-mean temperature difference, for heat transfer decreases. Creating the
necessary vacuum in the multiple effect evaporators requires installation of
vacuum creating equipments called condensers. A condenser is equipment,
which creates vacuum.

Figure 10.4 multiple effect evaporators

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CHEMICAL ENGINERING DEPARTMENT
Sugar boiling and vacuum pans
The sugar boiling process commences with syrup from the multiple effects
at 65 – 70 bx. This material is further concentrated to a concentration of
780brix in which crystallization of sucrose begins.
The operation known in the sugar factory, as sugar boiling is essentially the
process of crystallization, which is carried out in single effect vacuum
evaporators designed for handling viscous materials and known as vacuum
pans. Thus, the vacuum pan is an evaporative crystallizer in which degree
of super saturation is controlled by evaporating the solvent as the solute
crystallizes out. The art of pan boiling requires skill and experience to make
crystals of required number and of predetermined size, character, free from
false grain and conglomerates or twined grain. Once the crystals are formed,
the boiling operation is conducted in such a way that grains already formed
only developed and that none of the existing grain is re-dissolved.
There are three types of vacuum pans used in sugar boiling, namely: The
coil pans, the calandria pans and combined calandria and coil type.
Essential requirements of pan boiling
1. Grain size: The number and size of grains should be such as to give
maximum crystal surface for sugar adsorption from the mother
liquor. The grains should be uniform in size.
2. Less power consumption: Sticky massecuite spins with difficulty,
which takes longer time and high, power at centrifugal.
3. Maximum rendement: As much sugar as possible must be separated
out in crystal forms. If the grains are too fine, they pass out of the
centrifugal liners with the mother liquor and give less rendement.
4. Number of boiling: This should not be increased unnecessarily by
the unwanted recirculation of sugar or molasses. It invites gradual
increase of non-sugars, and would require excess capacity at back
factory.

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The Boiling Scheme
The operation of sugar boiling is arranged with the aim of maximum sucrose
recovery as much as possible with the minimum quantity of total massecuite
boiled. Practically, it is not possible to exhaust the syrup of the crystallizable
sucrose in one operation.
Therefore, the operation of pan boiling is carried out in two, three or four
stages producing different grades of massecuite or strike.
Number of Boiling Stages – The number of boiling depends upon the
following:
The purity of syrup
 For syrup purities higher than 85%, four boiling stage is
recommended.
 For syrup purities between 82 and 85% three boiling stage may be
adopted.
 For syrup purities less than 82% only two boiling stage can do.
The purity drops between the massecuite and its molasses.
The purity drop is influenced by the following factors:
 The quality of the massecuite, if the massecuite contains false grain, the
purity drop will be less and poor
 The brix or concentration of the massecuite – The higher the brix of
massecuite, the greater (better) is the purity drop.
 The grade of massecuite – In high-grade massecuite, the purity drop is
smaller than the case of low-grade massecuite because of the richness
of the mother liquor.
 Grain size – The larger the grain size, the smaller is the purity drop.
 Cooling effects – When massecuite are cured hot, they give less purity
drop than when they are sufficiently cooled in crystallizers.
In sugar boiling, commonly three boiling scheme is followed.
1. A - massecuite – It is produced by dominantly boiling syrup.
2. B - massecuite – It is with A - molasses derived from A - massecuite.

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 3. C - massecuite – It is boiled with A molasses & B molasses derived
from B massecuite.
These three grades of massecuite produce sugar of different quality and
polarization. In earlier days, all these grades of sugars were used to be
bagged together. Today qualitative operations are performed to produce one
grade sugar to the market. This is done by turning low grade sugars in to
one superior grade of marketable sugar
Crystallization
In the pans boiling operation, crystallization is effected by evaporating
water from solution, whereas, in crystallization by cooling, crystallization
is by cooling the massecuite. The rate of crystallization is determined by the
degree of super saturation, temperature, crystal surface area and nature &
concentration of impurities. The viscosity is also influenced by the same
factors.
The limit to which the massecuite can be cooled depends upon the ability
of crystallizers to handle physically the material at high viscosities.
When cooling the massecuite, the viscosity increases. The increase of
viscosity again prevents deposition of sugar on the existing crystals. The
viscosity should be kept low at this stage as well.
If cooling is pushed rapidly, it induces the formation of false grain. So that
while lowering the temperature of the massecuite, care should be taken to
prevent formation of false grain. The formation of false grain in this stage
is very dangerous with the result that either the sugar will not be cured or
the grain will pass out through the centrifugal liners increasing losses. The
temperature of the massecuite on leaving the pan is in the range of 65 –
700C.
There are two types of crystallizers depending on their operation:
1. Batch crystallizers
2. Continuous crystallizers
Depending on the system of cooling, the batch and continuous crystallizers
are classified as:

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  air cooled crystallizers Sugar
 water cooled crystallizers conveying -
 vacuum cooled crystallizers wet
Centrifugal separation commercial
Massecuite leaving the crystallizers has to be separated into crystals and sugar is
molasses. The more efficient this separation, the more sucrose will be conveyed to
recovered as a sugar and less sucrose will be lost in molasses. The sugar
centrifugal operation is carried out in centrifugal machines, which are dryer/cooler
variously called: centrifuges, centrifugals or fugals. In the past batch, by screw
centrifugal machines were the only ones in use to any extent. However, in conveyers
recent years, continuous machines have been used to an increasing extent, (horizontal as
and are now extensively used, for low-grade massecuites. well as
Batch Centrifugal – It consists of a cylindrical basket designed to receive inclined screw
the massecuite to be treated. The basket is carried on a vertical shaft, which conveyers)
is driven from its upper end by a motor. while dried
The basket is pierced with a numerous holes to allow the molasses to escape. and cooled
It is provided with circumferential hoops to with stand the centrifugal force. white sugar is
The basket is lined with metal gauze, which serves to retain the sugar while conveyed by
allowing the molasses to pass through. The basket is open at the top to allow horizontal and
the massecuite to be fed into it and a bottom opening allows the sugar to be inclined belt
discharged when the machine is stopped. While the machine is running, that conveyers or
is during charging and spinning, the discharge opening is generally closed bucketed belt
by a cone of thin sheet metal. elevator.
Continuous Centrifugal - The continuous centrifugal machine runs with Sugar drying:
constant speed without stopping. The machine is fed continuously by the since it is
massecuite and cured sugar is discharged continuously at high speed. hygroscopic
Therefore, it avoids waste of time and power in frequent stopping and (absorbs
starting the machine and in charging and discharging it. The mechanical moisture &
construction is simpler as it eliminates braking devices and the necessary gets
control gear starting up. It requires less accelerating power. agglomerated)
Sugar drying, handling and bagging , the

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commercial sugar must be dried, cooled and stored in such a way that it
doesn’t absorb moisture from the atmosphere and lose moisture to the
surrounding. The Rotary Sugar Dryer-Cooler is used for drying and cooling
purpose.
Sieving and grading of sugar: The sugar obtained after drying and cooling
consists of a mixture of heterogeneous crystals and needs to be well sieved
and graded before it is marketed. The sieving is done through sifters, which
are of vibrating type (vibrating sugar screen).
Sugar Weighing & Bagging: from each 1250 quintals capacity sugar
reconditioning bins, digital weighing scales weigh the commercial sugar.
There are two weighing machines both of which automatically weigh sugar
and discharge to the bagging material. One of the sugar scales weigh 50kg
per dump whereas the other weighs 100kg per dump. After weighing, the
weighed sugar is dumped into pp - bags. The pp -bags are then sewed by
sewing machines (one sewing machine for each sugar scale) and transported
to warehouse by belt conveyers for storage.

CEMENT TECHNOLOGY
Introduction
Cement is a product material obtained by calcination of calcareous (a
material containing lime) and argillaceous (a material which contain silica)
materials. According to (specification stand as) ASTM (American standard
testing material) “Cement is defined as a product obtained by pulverizing
(crushing followed by grinding) clinkers to which no addition has been
made except H2O.”
Properties of Cement
Composition: Chemically cement is a mixture of Silicates, Aluminates like
aluminoferrites with some amount of MgO and gypsum.
Various complexes which are contained in cement are
 (2CaO.SiO2) Di Calcium Silicate (C2S) 22-24%
 (3CaO.SiO2) Tri Calcium Silicate (C3S) 50-58%
 (3CaO.Al2O3) Tri Calcium Aluminate (C3A) 10-11%

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  (4CaO.Al2O3.Fe2O3) Tetra Calcium Aluminoferrite (C4AF) 8-9%
 (6CaO.Al2O3.Fe2O3) Hexa Calcium Aluminoferrite (C6AF) traces
 MgO <5%
 Gypsum (CaSO4.2H2O) 4-5%
Oxides of cement: the following are various oxides of cement
 CaO 60-66%
 Total silica 20-15%
 Combined silica/active silica
 Uncombined or inert silica
 Alumina (Al2O3) 3-8%
 Fe2O3 1-5%
 MgO <5% & Alkalies <5%
Color
The gray color in cement is due to presence of complexes of Ferric ions in
O.P.C (ordinary Portland cement). White cement is produced from those
raw materials which contain extremely low conc. of Iron & even like low
conc. of Iron is converted from Fe+3to Fe+2 (which can be done by
reducing or maintaining atmosphere in the kiln) & eventually the product
appears to be white.
Raw materials used in the production of O.P.C:
Lime stone, Clay and Gypsum
Limestone: Limestone on calcinations gives CaO that is an essential
component of all the complexes (silicates, aluminates and aluminoferrites)
present in cement. Limestone is available in two lime forms.
High lime: high lime is that lime stone which on calcination gives CaO of
greater than 90% purity. It contain Magnesia (MgO) less than 5% and rest
of the impurities may be alumina, Fe2O3 ,SiO2.
Low lime: Low lime means the limestone, which on decomposition yields
CaO of less than 90% purity.
Alumina & MgO is present to an extent of greater than10%. Dolomite rich
in MgCO3 should not be used in the manufacture of Portland cement.

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Clay
The complexes such as silicates, aluminates & aluminoferrites all contain
SiO2, & Al2O3. These are added into O.P.C by clay. • Ordinary clay found
in the area close to the mines of limestone have high quality clay.
The clay need for all production of O.P.C should meet the following
requirements.
1) It must be high in silica contents
2) Comparatively low in the amounts of Al2O3
3) Low in the amount of alkalis
In case if clay does not conform to the required specifications of oxides then
the clay has to be beneficiated before use.
Gypsum
When H2O is added into the cement & it is not thoroughly mixed then
tricalciumaluminate picks up H2O and rapidly hardens. This phenomenon
is called as flash setting. The flash setting in cement is retarded by the
addition of Gypsum, which forms the following complex
(3CaOAl2O3.3CaSO4.31H2O). The time of hardening of cement is
increased. Thus, the Gypsum containing cement gets hardened in
comparatively longer period of lime.
Fuel
Prior to 1971 the cement industry used furnace oil as fuel in cement
industry. As an higher energy consuming industry in which energy is
required for crushing, grinding, mixing & running of various units.
However, after 1971 the majority of the cement industries was switched
over to natural gas.
In the past few years, the importance of natural gas was realized for the
production of petrochemicals and the cement plants were converted into
furnace oil fired units now most of the cement industry is being switched
over to using coal, as a fuel.
Water-If cement is produced by wet process, large quantity of H2O is
needed. The H2O should not be saline in nature.

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 Production Process
Cement production involves following steps
1. Crushing & grinding of clay and lime stone.
2. Mixing of ground raw material to obtain an almost homogeneous mass.
3. Transportation of material ground raw materials to rotary kilns &
burning of raw materials to clinkers.
4. Grinding of clinkers in the presence of CaSO4 .2H2O
Step no 3 & 4 are as like on all the cement plants however step no 1 & 2
may be carried out in two ways.
 The crushed materials is ground & mixed in the presence of H2O to
obtain slurry containing 40%H2O &60% solids. This method is
called as wet method.
 If the crushed material is ground & mixed in absence of H2O & dry
homogenized mass is fed into the kiln for burning. The process is
called as dry process.
Comparison between wet and dry processes:
No. Wet process Dry process

1 Soft raw material is used Hard or soft, any type of raw material
is used for the production of cement.

2 The crushed material is ground The crushed material is ground in dry

in the presence of H2O to form &the feed given to the kiln is in the
a slurry paste. The slurry is than form of dry powder.
fed in to the rotary kiln for the
manufacture of cement

3 Grinding is done in rotary ball The grinding is conducted in the

mills in the presence of H2O to roller mill which combines grinding
obtain slurry of ground lime drying as well as classification. In
stone & clay that roller mills particles of dried size
are collected through a classification.

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4 Fuel consumption is comparatively Since water has not to be
more as the slurry added in the rotary evaporated so less fuel cons
kiln is 30-40%H2O and 60-
70%solids. Substantial amount of heat
is used in evaporation of H2O

5 Exposure to the effect of heat is for a Exposure to the effect of heat is

longer period and hence the operating less & hence the operating life
life of the lining of the kiln is less. of the lining of the kiln is more.

6 The length of the rotary kiln is more The length of kiln is usually
which may be between 300- 400 ft about 150 ft which may in some
usually and it may be sometime even cases be 250 ft.
as long as 500 ft.

7 The cost of insulation is high. The cost of insulation of kiln is less.

8 Thermal efficiency is higher as the Thermal efficiency in the kiln is

flue gases leave the kiln at about less as the gases leaving the
1000C. rotary kiln are about 300oC.

9 The loss of raw material in the form of The loss of the raw material in
dust contained in the flue gas coming the form of dust is much higher
out of the kiln is less. It amounts to and about 15% raw material is
about 1.5% of the clinker produced. lost with the flue gas coming
out of the kiln.

10 The dust particles leaving with the flue Dust contained in the flue gas is
gas are recovered by installing recovered in the same way as in
scrubbers, cyclone separators and by wet process.
installing high-density electrical
precipitators.
11 The recovery of heat from the flue The heat recovery in dry process is
gases is less. 20% more in this process.

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Crushing & grinding of clay and limestone
The limestone and the clay needed for the production of cement as
excavated from the quarries are crushed to approximately a particle size of
100mm using crushers, which are called as the primary crushers.
The secondary crusher installed in the same area crushes the limestone and
the clay to obtain a particle size of about 10mm.
In the wet process, the crushed lime and clay is fed into a rotary grinding
ball mill in the presence of water. The grinding is carried out using the
technique of close circuit.
Mixing of ground raw material to obtain an almost homogeneous mass
The lime and clay obtained from the classifier is received in a correcting
tank where the composition w.r.t. limestone and clay is adjusted. The slurry
should contain 65-70% limestone and 30-35% clay in it. In case any of the
two is less in quantity, the difficulty is made up by adding required quantity
of deficient material.
Then slurry containing corrected limestone and clay is pumped to a dark
thickener where excess of water of any is removed which in turn is reused
for grinding in the ball mill. The slurry obtained from the dark thickener
should contain 30-40% water and 60-70% of the solids. This slurry is then
introduced into the kiln for pyro processing (heat treatment).
Transportation of ground raw materials to rotary kilns & burning of
raw materials to clinkers
Construction and working of the rotary kiln:
The pyro-processing of slurry obtained in the wet method and the dry
ground raw materials in the dry process is carried out in a rotary kiln. It is
made from sheets of plain carbon steel riveted together to obtain a shell.
In the old versions, the rotary kiln tapered towards the top. Now a day’s
large no. of cement industry is using rotary kiln of uniform internal
diameter.

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CHEMICAL ENGINERING DEPARTMENT
In the old versions, the rotary kiln was placed in a way that it made an angle
of 15 degrees with the horizontal, which facilitates the movement of
material from the feed end tothe discharge end.
Construction and working of the rotary kiln:
Now days the inclination of shell with the horizontal has been reduced to
about 5-6 degrees. To facilitate then movement of the material from feed
end to the discharge end, chains are installed inside the rotary kiln.
The kiln rotates in the clockwise direction by standing at the discharge end.
The revolutions of the kiln about its axis ranges between half to one rpm in
some cases, while in the others it may be 1-3 rpm.
This depends upon the size of the kiln which may be 300- 400 ft in case of
wet process and up to 150 ft in dry process. From the feed end to the
discharge, end the total time taken for the movement of material is between
2-3 hours. The temperature maintained inside the rotary kiln ranges between
300-1400 degree Celsius in dry process and 100-1400 degree Celsius in wet
process. At elevated temperature, calcium oxide behaves as a very strong
base and it can attach the material of construction of the shell of rotary kiln.
It is therefore necessary to take appropriate measure to increase the working
life of rotary kiln. For this purpose, lining is provided on the interior of the
shell of rotary kiln.
Merits of Lining in rotary kiln
A lining provided in the rotary kiln has the following merits:
The chemical attack of calcium oxide leading to corrosion of material of
construction of shell be eliminated.
The lining used is of a refractory material which processes very low thermal
conductivity hence heat losses from rotary kiln to atmosphere would be
reduced. The ordinary firebricks which contain a very high percentage of
silica cannot be used for the purpose of lining as silica contained in it may
react with CaO to form CaSiO2 which may solidify inside the kiln forming
rings which may obstruct the movement of material inside the kiln from the
feed end to discharge end.

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CHEMICAL ENGINERING DEPARTMENT
Usually high aluminium bricks produced from bauxite are used for the
purpose of lining. In the old version of the rotary kiln the lining of 9 inches
were provided from first 100 ft staring from discharge end whereas the next
110ft was lined with 7 inches thick brick of bauxite. Now days the kiln
usually processes a uniform lining.
Temperature Zones of Rotary kiln
Temperature Range Working
100-300 0C Evaporation of water. This zone shall not be
existed in dry process.
300-600 0C Evaporation of combined water means
chemically bound water.
Decomposition of carbonate starts.
400-800/900 0C Burning of organic matter.
600-900oC Volatilization of alkalis.
Volatilization of chlorides.
Evolution of CO2 from CaCO3 and the existence
of free CaO start.
900-12000C In this zone, main reaction between lime and clay
takes place which is further subdivided into the
following:
900-11000C (Formation of tricalcium aluminate
and tetracalcium aluminoferrite.)
1100-12000C (Max. formation of tricalcium
aluminate and dicalcium silicate.)
1250-12800C Commencement of liquid formation.
1280-14000C Further formation of molten mass and the
formation of main constituent of cement i.e.
tricalcium silicate. In this range most of CaO from
the decomposition of lime stone gets associated to
form various complexes.

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CHEMICAL ENGINERING DEPARTMENT
Figure 11.1 kilning

Clinker Formation
The product obtained due to high melting temperature is converted into the
form of circular balls called as clinkers, which vary in this size between 1/8
to 3/8 inches, the clinkers are collected in a cooler where they are cooled
using a draft of cold air. Wet air gets heated to 700-8000C and used in the
burning of fuel in the rotary kiln. The flue gases leaving at the feed end pass
through an integrated system of scrubbers, cyclone separator and electrical
precipitators to recover the dust particles of the raw material.
Grinding of the clinkers:
The clinkers are ground in the presence of 4-5% gypsum to obtain fine
powder, which may confirm to the following specification:
ASTM
The 78% of the ground material should pass through 200-mesh sieve.

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CHEMICAL ENGINERING DEPARTMENT
Figure 10.3 the cement manufacturing processes

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CHEMICAL ENGINERING DEPARTMENT
LEATHER PROCESSING
Introduction
Skin/Hides-from cows, pigs, goats, and sheep; exotic animals such as
alligators, ostriches, and kangaroos
Products- (footwear, garments, gloves, bags, wallet, travel goods, etc)
This sector is the second largest foreign exchange earner to the country next
to coffee.
According to an industry survey conducted by the Ethiopian export
promotion agency, most tanneries are operating only 30 to 90% of their
capacity due to different reasons including limited supply of raw materials,
outdated equipment and machineries, lack of market information, and low
quality standards to fulfill the stringent international market requirement.
Tanning process
The processing of hides and skins into leather is a fascinating procedure that
requires a precise combination of many chemical and mechanical
operations.
Major divisions of the leather sector
Tanneries
Total no of tanneries are 33, of which 2 of are under investment. 23 of them
are owned by local investors and 10 of them are owned by foreigner
investors from Italy, China, UK, India, Sudan, Turkey.
Around 6000 workers are employed.
They have a capacity of 50 million pieces of skin and 5 million hides per
year
They are located in Addis Ababa and other four regions.
Finished Leather
More than 100 million square feet of finished leather produced annually. Of
which 72 million is from sheep and goatskin and 30 million is from
cowhide.
More than 60 million square feet from sheep and goat and 10 million from
cow is exported annually.

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CHEMICAL ENGINERING DEPARTMENT
There is a possibility of producing up to 500 million square feet at present
capacity of tanneries..
Quality finished leather manufacturers like Farida and United Vasan of
India are producing in Ethiopia.

Tannery
Tannery operations can be broadly divided
Beam house operations
Tanning operations
Post-tanning and
Drying and finishing operations
Beam house operations
Before tanning the main important operations for leather manufacturing are
done in beam house. Beam house operations consists of soaking, liming,
de-liming, bating, pickling, de-pickling, and degrease(if necessary).

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Trimming and weighing
First of all the selected tannable hides and skins are trimmed to remove the
tail, shoulder, flanks, neck and trimmable portions correctly. Then weighed
correctly
Reception: salted skins are temporarily stored. The application of salt
(NaCl) is done outside the factory to preserve the skins from decay.
All hides are weighed for calculating the amount of needed chemicals.
Soaking: it is carried out to allow salted skins to re-absorb any water, which
may have been lost after flaying, to clean the hides and skins(removal of
dung, blood, salt, air, etc), and
To remove inter-fibrillery material.
The process of soaking
Pre-soaking (dirt soaking): in dirt soaking, 300-400% of water is used to
remove the unwanted materials
Main soaking: the purpose of main soaking is to re-hydrate the material. In
this operation, water, non-anionic wetting agent (0.2% concentrated), soda
ash (0.2% concentrated) and preservative (0.5% concentration) are used.
Final soaking: only water is used for the washing of purpose.
The Treatment Process
Preparation for tanning (Steps 1 - 4)
The main chemical processes carried out by the tanner are the unhairing,
liming, tanning, neutralising and dyeing.
Step 1 - Unhairing
The keratin of hair and wool is subject to attack by alkali, which will break
(by hydrolysis) the sulphur-sulphur bond in the cystine linkage of the
keratin. The hair is attacked first at the root, where it is in its immature form.
After a certain time of being steeped in a solution of alkali (sodium or
calcium hydroxide) and a reducing agent, normally sodium sulphide, the
hair roots are dissolved, and the hair may be removed and saved.

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CHEMICAL ENGINERING DEPARTMENT
In the processing of sheep and lambskins, the solution of alkali and sulphide
is applied on the inside of the skin, allowing the solution to penetrate
through the skins, attacking the wool roots, which can then be removed by
'pulling' them from the skin
Step 2 - Liming
The process of liming is a combination of chemical and physical action on
the skin structure. The chemicals involved are similar to those in the
unhairing operation. A solution of lime and sodium sulphide is used and the
skins are immersed in this solution for whatever time is necessary to
produce the desired effects. The process of un-hairing is taken to completion
during the liming process, and there is appreciable modification of the
collagen due to the action of alkali.
Liming objectives
To remove hairs, hooves, nails, and other keratinous materials.
To remove some of the inner fibrillary soluble proteins like mucins etc
To swell up and to split up the fibers to the desired extent
To remove the natural grease and fats
To bring the collagen to a proper conditions for satisfactory tanning
Hydrolysis is continued by the enzyme process and further dissolution of
unwanted material occurs. The main fibrous network is then cleaned up and
the swelling is reduced.
Step 3 - Deliming and Bateing
After the strong alkaline action, the skin structure is further opened up
during the deliming and bateing process.
Bateing is an enzyme digestion process which continues the cleaning up
process begun by the alkaline action. Bateing is carried out at pH 9-10. This
is achieved by treatment with acid salts (ammonium chloride or ammonium
sulphate) or carbon dioxide until the desired pH is reached.

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Step 4 - Pickling
The main acidification process is that of pickling. The skins are agitated in
a solution of salt and sulphuric acid until they are at or near equilibrium at
a pH value of 3.0 - 3.5.
Objectives of Pickling
 To bring the de-limed and bated pelts to a required degree of acidity
before chrome tannage
 To reduce the pH
 To modify the fiber structure
 To preserve the leathers and to achieve the special effect
Step 5 Tanning
The process of tanning
The tanning or stabilising process can be carried out as noted before, by
means of vegetable, mineral or synthetic tanning materials. The vegetable
and synthetic tanning materials are largely anionic in nature and are
essentially similar in their action on skin protein. Chemically they are
complex mixtures and their chemistry is not well understood. The vegetable
tans fall into two main classes.
Hydrolysable tans - complex esters of phenol, carboxylic acids and
polyhydroxyphenols
Condensed tannins - mixtures of products of varying degrees of
polymerisation, containing several molecules of catechin or catechinlike
compounds
There are two main features of chromium chemistry which enable it to act
as a tanning agent.
Firstly, the complexes formed are of intermediate stability, and thus
exchange of coordinating ligands can take place comparatively easily.
Secondly, chromium has the ability to form polynuclear complexes in
which Cr-O-Cr bridges are involved.

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CHEMICAL ENGINERING DEPARTMENT
Step 6 - Neutralising, Dyeing and Fat Liquoring
After tannage, leather must be neutralised to remove unwanted acids to
prevent deterioration during the drying process, and to prepare the leather
for the next stages in processing: dyeing and fat liquoring.
Neutralising is often carried out using mild alkalis which have some effect
on the chromium complex (sodium formate is a good example).
Next is dyeing, using a variety of dyestuff types. Commercial dyes are
essentially mixtures of chemical compounds which can be fixed (combined)
to the material to be dyed and which have appreciable resonance within the
molecule giving color.
Fat liquoring is the process in which 'tanned' fibers are treated with reactive
oils, which attach themselves to the fibrous structure, and lubricate them so
that they can move readily in relation to one another, producing a soft,
supple leather.
Step 7 - Drying
Finally, as water is removed from the system, the chemical condition is
stabilized and the final properties of the leather are determined.
Step 8 - Finishing
Finishing consists of applying a surface coating - pigments or dyes bound
in an organic (acrylic, butadiene or polyurethane) or protein (casein)
medium. This enhances the natural qualities of the skin and covers such
defects as scars, horn damage, seed scars etc., as may be present.
Tanneries and Environment
The leather industry is a chemical processing industry. Processing is largely
carried out in a water medium and as such, there is potential for a number
of environmental concerns.
The main waste products originating from leather processing are hair or
wool, salts, alkali (lime), sulphides, acids, chromium salts and dye-stuffs.
Hair and wool are useful by-products, the hair being used for felt
manufacture and wool for clothing and carpeting.

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CHEMICAL ENGINERING DEPARTMENT
Any excess of acid or alkali can be readily and cheaply neutralised. The two
components of normal tannery effluent which are difficult to deal with are
sulphides and chromium salts. Each is undesirable for different reasons.
Solutions of sulphides in neutral or acidic conditions liberate significant
quantities of hydrogen sulphide, which has a strong and objectionable smell
(like rotten eggs) and is quite toxic - a potential hazard for sewerage
workers. The main objection to sulphide, however, is its corrosive action on
the sewer fabric. The sulphuric acid erodes the sewer walls by forming
sulphates of the calcium, aluminium and iron found in concrete. Besides
being readily soluble, these salts expand as they are formed and cause
crumbling of the aggregates in the concrete.
Chromium
Chromium salts are undesirable for two reasons. Firstly, they can have a
poisoning effect on the micro-organisms used for sewage treatment.
Secondly, they are precipitated as chromium hydroxide at neutral and near
neutral pH's, meaning that they persist into the sludge from the sewage
treatment plants. This gives a build-up of chromium (III) hydroxide in the
sludge, which is undesirable as sludge is commonly used as a fertilizer.
Tannery effluents are discharged in an alkaline condition. Under these
circumstances any chromium present is in the form of chromium hydroxide,
a light, finely divided precipitate, which is very difficult to remove.
Treatment consists of the addition of more alkali and trace quantities of
polyelectrolyte flocculating agents. This aggregates the finely divided
particles and greatly improves the rate of sedimentation so the chromium
hydroxide can be removed in a normal settling operation, or by dissolved
air flotation.
However, because of the limited world supply of chromium, it is necessary
to develop means by which chromium tanning materials are recycled. What
tanning liquor is lost can be made alkaline and the chromium hydroxide
separated and recovered by re-acidification. The chromium sulphate so
produced is suitable as a tanning solution.

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Self-Check Questions
1. Which manner is a chemical or biochemical plant not operated in?
A. Continuous
B. Batch-wise
C. Semi-continuous
D. Discontinuous
2. When is a separation process not required in a manufacturing process?
A. When there is a decomposition reaction
B. When there is a complete conversion
C. When the byproducts are in form of gases
D. When the reaction is reversible
3. If only 5% of Ethylene is converted to Ethylene glycol, why is there a
need of separation process?
A. To feed more reactant to the reacting mixture
B. To remove the ethylene glycol formed
C. To recover the unreacted Ethylene Glycol
D. To start an intermediate reaction
4. Which of the following is a condition of operation for biochemical
plant?
A. Metallic catalyst
B. Chemical catalyst
C. Elevated temperature
D. Non-pathologic state of the organism
5. During the production of ammonia low temperature is required. The
advantages of low temp. could be
A. slow only
B. better yields only
C. better quality
D. slow and better yields

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CHEMICAL ENGINERING DEPARTMENT
6. The factories which produce fertilizers usually have plants of
A. ammonia production
B. nitric acid production
C. ammonium nitrate production
D. All of above
7. The only condition for nitrogen based fertilizers is that they must be
soluble in
A. acid
B. base
C. water
D. alkalis
8. The ideal pulp for the manufacture of paper should have high __________
content.
A. Cellulose
B. Lignin
C. Both (a) & (b)
D. None of these
9. Production of alcohol by fermentation of molasses is a/an __________
process.
A. Anaerobic
B. Aerobic
C. Endothermic
D. Both (b) and (c)
10. Sulfuric acid solution having a specific gravity of 1.20 at room
temperature is used mainly for the
A. Fertilizer manufacture
B. Car battery solution
C. Synthesis of oleum
D. Water treatment

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11. During the absorption of HCl gas in water (to produce liquid HCl), the
gas is kept above dew point to
A. Increase the rate of absorption
B. Avoid corrosion
C. Reduce the cooling water circulation rate
D. None of these
12. With increase in temperature, the equilibrium constant at constant
pressure (Kp) for oxidation of sulphur dioxide
A. Increases
B. Increases linearly
C. Decreases
D. Decreases linearly

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REFERENCES
1. Donald R. Coughanowr Steven E. LeBlanc Process Systems Analysis and Control, 3 rd Ed., McGraw-Hill
Chemical Engineering Series (2009)
2. [T.K. Nguyen Chemical and Materials Engineering Cal Poly Pomona (Winter 2014)]
3. George Stephanopoulos, CHEMICAL PROCESS CONTROL, An Introduction to Theory and Practice,
2002, Prentice-Hal of India.
4. Romagnoli, Jose A. Introduction to Process Control. s.l.: CRC press, 2006.
5. Jacob A. and et al. Chemical Process Technology, 2nd ed.
6. James A. Kent, Handbook of Industrial Chemistry and Biotechnology. 12th ed.

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