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SCHOOL OF CHEMICAL ENGINEERING

EKC 453 PLANT DESIGN & ECONOMIC

PLANT DESIGN FOR THE PRODUCTION OF PHTHALIC


ANHYDRIDE FROM O-XYLENE

TASK 2

GROUP 18

GROUP MEMBERS:

1. MUHAMMAD SHAFIZRUDDIN FIRDAUS BIN FAZLI KU 129098

2. MUTHU KUMAR A/L GANESON 129102

3. NURUL ATIKAH BINTI SAIFULQAHAR 129123

4. ZAHIRA BINTI MOHAMED MALIK 129138

SUPERVISOR : PROFESSOR DR. BASSIM H. HAMEED

DATE OF SUBMISSION : 19TH APRIL 2019


Table of Contents
LIST OF TABLE ................................................................................................................... iii
LIST OF FIGURES ................................................................................................................ iv
GANTT CHART ...................................................................................................................... 1
WORK DISTRIBUTION AND EXECUTION OF TASK .................................................. 2
CHAPTER 1: PIPING AND INSTRUMENTATION DIAGRAM (P&ID) ....................... 4
1.1 Process Control Loops for Equipment ............................................................................. 4
1.1.1 Mass Transfer Equipment .................................................................................... 4
1.1.1.1 Distillation Column, T-01 and its Auxiliary................................................. 4
1.1.2 Heat Transfer Equipment ........................................................................................ 10
1.1.2.1 Heat Exchanger, E-01 ...................................................................................... 10
1.1.2.2 Heat Exchanger, E-02 ...................................................................................... 12
1.1.2.3 Heat Exchanger, E-03 ...................................................................................... 14
1.1.2.4 Heat Exchanger, E-04 ...................................................................................... 16
1.1.2.5 Switch Condenser, SC-01 ................................................................................ 18
1.1.3 Reactor .................................................................................................................... 21
1.1.3.1 Multi-Tubular Reactor, R-01 ........................................................................... 21
1.1.4 Auxiliary Equipments ............................................................................................. 24
1.1.4.1 Centrifugal Pump, P-01, P-02 and Storage Tank ............................................. 24
1.1.4.3 Centrifugal Compressor, C-01 ......................................................................... 26
1.2 Summary of Control Loop for Each Equipment ....................................................... 28
1.3 Plant Layout Drawing .................................................................................................... 30
1.3.1 Description of Plant Layout .................................................................................... 30
1.3.2 Plant Layout ............................................................................................................ 35
1.4 Selection of Instrumentation and Equipment ................................................................. 36
1.4.1 Selection of Sensors and Calibration / Maintenance of Sensors............................. 36
1.4.2 Selection of Valves and Calibration / Maintenance of Control Valves .................. 46
1.5 Control Loop Simulation via ASPEN Dynamic ............................................................ 51
1.6 Piping and Instrumentation Diagram (P&ID) for The Whole Plant .............................. 54
CHAPTER 2: ENGINEERING ETHICS IN PLANT DESIGN ....................................... 60
2.1 Ethics Problem ............................................................................................................... 60
2.2 Code of Ethics ................................................................................................................ 63
2.2.1 The Institution of Engineers Malaysia (IEM) ......................................................... 64

i
2.2.2 Boards of Engineers Malaysia (BEM) .................................................................... 66
2.2.3 American Institute of Chemical Engineer (AIChE)................................................ 68
2.2.4 American Petrolem Institute (API) ......................................................................... 70
2.3 Ethics in Environment, Safety and Health Problems. .................................................... 72
2.4 Ethics in Design Project ................................................................................................. 74
2.4.1 Teamwork and Time Constraints ............................................................................ 74
2.4.2 Constraint of Data and References ......................................................................... 76
2.5 Case Study: Pasir Gudang chemical spill [1] ................................................................. 77
CHAPTER 3: PLANT RISK ASSESSMENT ANALYSIS ................................................ 80
3.1 Lists of Hazardous Substances....................................................................................... 80
3.2 List of Equipment Handling High Inventory of Hazardous Substances ........................ 83
3.3 Possible Hazard Derived Identification and Risk Evaluation ........................................ 84
3.3.1 Hazards Possibility, Consequences Analysis .......................................................... 84
3.3.2 Risk Evaluation Classification ................................................................................ 85
3.3.3 Classified Hazard Identification and Risk Evaluations .......................................... 87
3.4 Possible Hazards and Risk Analysis .............................................................................. 94
3.4.1 MSExcel Hazard Analysis ...................................................................................... 94
3.4.2 ALOHA Incident Analysis ..................................................................................... 95
3.4.3 Comparation between MSExcel calculation and ALOHA software .................... 106
3.5 Mitigations and Strategy Recommendations ............................................................... 107
3.6 Plant Start-Up and Shut-Down Sequence .................................................................... 111
3.6.1 Start Up and Shut Down Procedure for Reactor, (R-01) ...................................... 111
3.6.2 Start Up and Shut Down Procedure for Distillation Column, (T-01) ................... 114
3.6.3 Justification of Plant Start-Up and Shut-Down Procedures .................................. 116
3.6.4 Comparison with Industry on SOP Preparation .................................................... 119
3.7 Plant Emergency Shutdown ......................................................................................... 122
3.8 Alarm System for Major Unit Operations ................................................................... 123
3.8.1 Temperature Alarm ............................................................................................... 125
3.8.2 Pressure alarm ....................................................................................................... 126
3.8.3 Level Alarm .......................................................................................................... 126
3.8.4 Alarm System for Multi-Tubular Reactor, R-01................................................... 127
3.8.5 Alarm System for Switch Condenser, SC-01 ....................................................... 129
3.8.6 Alarm System for Distillation Column, T-01 ....................................................... 131
3.9 Comparison with Industry on SOP Preparation and Alarm System Setting ................ 133

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3.9.1 Standard Operating Procedure (SOP) ................................................................... 134
3.9.2 Shut-Down Procedure ........................................................................................... 134
3.9.3 Alarm System........................................................................................................ 135
REFERENCES ..................................................................................................................... 137
APPENDIX ........................................................................................................................... 140
Appendix A: Meeting Minute ............................................................................................ 140

LIST OF TABLES

Table 1: Summary of Control Loops for Distillation Column, T-01 7


Table 2: Summary of Control Loops for Heat Exchanger, E-01 11
Table 3: Summary of Control Loops for Heat Exchanger, E-02 13
Table 4: Summary of Control Loops for Heat Exchanger, E-03 15
Table 5: Summary of Control Loops for Heat Exchanger, E-04 17
Table 6: Summary of Control Loops for Switch Condenser, SC-01 20
Table 7: Summary of Control Loops for Multi-Tubular Reactor, R-01 23
Table 8: Summary of Control Loops for Centrifugal Pump, P-01 25
Table 9: Summary of Control Loops for Centrifugal Compressor, C-01 27
Table 10: Control loops summary list 28
Table 11: Justifications of Plant Layout 31
Table 12: Hazard Possibility 84
Table 13: Hazard severity 85
Table 14: Risk assessment criteria 86
Table 15: Suggested Criteria 86
Table 16: Commissioning Procedures 117
Table 17: Trigger values for reactor alarm systems 127
Table 18: Corrective actions after triggering reactor alarms 128
Table 19: Trigger values for switch condenser alarm systems 130
Table 20: Corrective actions after triggering of switch condenser alarms 130
Table 21: Trigger values for distillation column alarm systems 132
Table 22: Corrective actions after triggering of distillation column alarms 132

iii
LIST OF FIGURES

Figure 1: P&ID Drawing for Distillation Column, T-01 4


Figure 2: P&ID Drawing for Heat Exchanger, E-01 10
Figure 3: P&ID Drawing for Heat Exchanger, E-02 12
Figure 4: P&ID Drawing for Heat Exchanger, E-03 14
Figure 5: P&ID Drawing for Heat Exchanger, E-04 16
Figure 6: P&ID Drawing for Switch Condenser, SC-01 18
Figure 7: P&ID Drawing for Multi-tubular Reactor, R-01 21
Figure 8: P&ID Drawing for Centrifugal Pump, P-01 24
Figure 9: P&ID Drawing for Centrifugal Compressor, C-01 26
Figure 10: Plant Layout Phthalic Anhydride Production 35
Figure 11: Calibration Pressure Transducer 42
Figure 12: Initial Condition Before Any Changes 52
Figure 13: Pressure Controller is Changed to 5 bar 53
Figure 14: SOP for Industrial Distillation Column 121
Figure 15: Protection Layer of Process 124

iv
GANTT CHART

18/03 - 24/03 25/03 - 31/03 01/03- 07/03 08/04 - 14/04 15/04 - 19/04
SCOPE OF PROJECT Week 1 Week 2 Week 3 Week 4 Week 5
Planning and execution of the project
1.0 Piping & Intrumentation Diagram (P&ID)
P & ID diagram of
equipment
Mass transfer equipment
Reactors
Heat transfer equipment
Auxiliary
Summary of control loop
Plant layout
Sensor and valve
selection
P & ID diagram of
whole plant
Control structure
Analysis (ASPEN
Dynamic)
2.0 Engineering ethics in plant design
Ethical problem
Code of ethics
Ethic in design project
Ethic in environmental
safety and health
3.0 Plant risk assessment analysis
Identify possible hazard
Risk assessment analysis
(Excel & Aloha)
Recommendation of
mitigation strategies
Plant start up and shut
down procedure
4.0 Checking and
compiling
5.0 Task submission

1
WORK DISTRIBUTION AND EXECUTION OF TASK

A. Piping and Instrumentation Diagram Date


1.1 Piping and Instrumentation Diagram (P & ID) Legend Muthu 16/3/2019
1.2 Piping and Instrumentation Diagram (P & ID) ALL 16/3/2019
1.3 Summary of Control Loops Utilized in Equipment Zahira & 16/3/2019
1.4 Proposed Plant Layout Atikah
1.4.1 Site Selection Justification Shafiz 18/3/2019
1.4.2 Plant Layout Zahira 18/3/2019
1.5 Selection of Sensors Shafiz 16/3/2019
1.6 Selection of Valves Shafiz 16/3/2019
1.7 Control Structure Analysis via ASPEN Dynamics
1.7.1 Reactor
1.7.1.1 Temperature and Flow Control Muthu 20/3/2019
Loop Muthu 20/3/2019
1.7.1.2 Set Point Change Analysis for
Temperature Muthu 20/3/2019
1.7.1.3 Set Point Change Analysis for Flow Atikah 26/3/2019
1.7.2 Justification on ASPEN Dynamics
Analysis
A. Engineering Ethics
2.1 Ethical Problems Zahira 27/3/2019
2.2 Codes Effect Atikah 27/3/2019
2.3 Safety and Health Problem Shafiz 27/3/2019
2.4 Correct Practise Muthu 27/3/2019
B. Plant Risk Assessment Analysis

2
3.1 List of Hazardous Chemicals Shafiz 29/3/2019
3.2 List of Equipment Used Atikah 29/3/2019
3.3 Possible hazard Derived Identification and Risk
Evaluation Atikah 30/3/2019
3.3.1 Hazard Possibility and Consequence Analysis
Classification Shafiz 30/3/2019
3.3.2 Risk Evaluation Classification Muthu &
Zahira 1/4/2019
3.3.3 Classified Hazard Identification and Risk Zahira 1/4/2019
Evaluations Muthu 1/4/2019
3.4 Possible Hazards and Risk Analysis
3.5 Mitigation Strategy Recommendations Shafiz 3/4/2019
3.6 Plant Start-Up and Shut-Down Procedure Shafiz 3/4/2019
3.6.1 Reactor Shafiz 3/4/2019
3.6.1 Distillation Column
3.6.3 Justification of Plant Start-Up and Shut-Down Atikah 3/4/2019
Sequence Zahira 10/4/2019
3.6.4 Emergency Shut Down Procedure
3.7 Alarm Systems for Major Unit Operations
3.7.1 Temperature Alarm System
3.7.2 Level Alarm System Muthu 10/4/2019
3.7.3 Pressure Alarm System
3.7.4 Summary of Alarm System

3
CHAPTER 1: PIPING AND INSTRUMENTATION DIAGRAM (P&ID)

1.1 Process Control Loops for Equipment


1.1.1 Mass Transfer Equipment
1.1.1.1 Distillation Column, T-01 and its Auxiliary

Figure 1: P&ID Drawing for Distillation Column, T-01

4
The distillation column must have an effective control strategy as a separation unit. To achieve the

product composition and follow the design, temperature, pressure and level must be monitored and

controlled. The composition of the top and bottom product is indirectly controlled by controlling

the temperature and pressure in the column using the vapor liquid equilibrium thermodynamics

relationship calculated during the design task.

The top pressure and temperature of the column is controlled by using cascade control loop. The

pressure and temperature of the column are controlled by manipulating the inlet cooling water to

the condenser. TIC is used as master control loop and PIC as slave controller in cascade control

scheme due to the dynamics of the process. Fail-opened control valve is used to avoid pressure

built up and runaway temperature in case of control valve malfunction or under maintenance, and

a bypass valve is prepared to allow manual control.

A pressure safety valve with 15% safety margin is installed as an additional precaution to handle

any overpressure possibilities due to slow dynamics of the pressure regulating system. High

pressure alarm are installed as safety precaution to notify the operator if the pressure build up in

the column. In order to achieve the desired product composition, the reflux ratio must be controlled,

thus ratio control system are installed at the reflux drum to control the reflux ratio. The feedforward

ratio control scheme will control the desired reflux ratio by manipulating the flowrate of the outlet

stream. The ratio control used PID controller due to its dynamic process. Fail-opened control valve

is used to avoid exceed the flowrate ratio in case of control valve failure or under maintenance, a

bypass valve is prepared to allow manual control.

For the bottom of the column, the temperature is controlled by feedback control system. The

temperature of the bottom product is controlled by manipulating the inlet flowrate of the

superheated steam into the reboiler. PID controller is selected as TIC because temperature control

is a slow dynamic system. Fail-closed control valve is used to avoid runaway temperature in case

of control valve failure and a bypass valve is prepared for manual control. The liquid level in the

5
column is controlled by feedback control system. The liquid level in the column is controlled by

manipulating the outlet flowrate of the bottom product. The liquid level in the reboiler is controlled

by level controller is used at the bottom of the column to regulate the flowrate of product into the

reboiler to avoid any runaway reaction. PI controller are used as level controller LIC.

6
Table 1: Summary of Control Loops for Distillation Column, T-01

Control Loop Temperature Flow Pressure


Objective 1. To maintain the temperature at the To maintain the reflux ratio of To maintain the column pressure
structured packings zone and the column T-01 to indirectly control at 1.01 bar and avoid over
bottom. the purity of distillate pressure of T-01
2. To maintain the temperature of product
phthalic anhydride at 283.8 °C

Controlled Variables 1. Temperature of liquid at the top, Flowrate of distillate Pressure near the top of column
packings zone. T-01
2. Temperature of liquid at bottom
Manipulated 1. Flowrate of SC-01 effluent Flowrate of distillate Cooling water flowrate
Variables 2. Flowrate of steam inlet
3. Flowrate of cooling water supply
Disturbances  Temperature and composition of the Flowrate of reflux  Temperature build up in the
SC-01 effluent (feed inlet to column). structured packings due to
 Heat released from the exothermic exothermic reaction
reaction  Temperature of steam inlet.
 Temperature of steam inlet.

7
Control Structure 1. Single loop control with PI feedback Ratio controller with PID Singe loop control with PID
controller for PIC feedforward controller for FIC feedback controller for PIC

Additional  Pressure relief valves with 10% safety margin, venting out gaseous substances of the column and reflux drum to
Considerations avoid rupture of the structures during event of over-pressurization.
 Fail-open control valve for the case of pressure and reflux ratio control to enable condensation of vapor product
to continue and avoid overflow in reflux drum in case of failure
 Fail-close control valve for the case of temperature control to avoid temperature build up in column from
uncontrolled exothermic reaction in case of failure
 Alarm system for low and high detection for column pressure, liquid level in both sump and reflux drum, and
temperature with additional high-high alarm for temperature of column.
 Drain valve is installed at the bottom of the column and reflux drum to drain accumulated liquid for maintenance
works and shut down purpose.
 By-pass valves are installed parallel to all the control valves for manual control during maintenance works or failure of
control valves Backup sumps are installed for standby purpose in case of malfunction of the servicing sump.
 Alarm system for low and high detection for level.

8
Control Loop Level Flow

Reflux Drum Column sump


Objective To maintain the liquid level in reflux To maintain the liquid level of To maintain the flowrate of
drum, V-02. sump of the T-01. steam inlet to the reboiler, E-06.

Controlled Variables Liquid level in reflux drum Liquid level of sump Flowrate of steam inlet to
reboiler

Manipulated Flowrate of reflux back to column Flowrate of bottom liquid product Steam inlet flowrate
Variables

Disturbances Flowrate and liquid fraction of condensed  Temperature in the column  Pressure of steam inlet
stream from condenser, E-05  Temperature of reboiled vapor  Temperature of steam inlet.
from reboiler

Control Structure Single loop control with PID feedback Single loop control with PID Single loop control with PID
controller for LIC feedback controller for LIC feedforward controller for FIC

9
1.1.2 Heat Transfer Equipment
1.1.2.1 Heat Exchanger, E-01

Figure 2: P&ID Drawing for Heat Exchanger, E-01

10
E-01 is used to heat up the steam supply before being proceed to the R-01. Steam is

supplied to the heat exchanger to increase the temperature of the air. Temperature of the outlet

stream is the variable that is going to be controlled to get the desired specification. Alarm is

installed to warn the operator if there is any undesirable condition occur so that immediate

action can be taken to avoid accident or damage to other equipment. High and low temperature

alarm is used to sense high temperature in the heater that may lead to explosion. Feedback

controller is used to control the temperature outlet of heat exchanger. The temperature control

valve use PI controller to eliminate the disturbances in the system.

Table 2: Summary of Control Loops for Heat Exchanger, E-01

Control loop Temperature

Objectives To control the temperature of the outlet of heat exchanger

Controlled variable Temperature outlet of heat exchanger.

Manipulated variable Inlet flow rate of steam supply to the shell side.

Disturbances Inlet temperature of heat exchanger feed.


Inlet flow rate of air.

Control structures Single loop, PID controllers with feedback control strategy.

Additional  For plant safety and the quality control of the production, high and
considerations low temperature alarms are installed.
 Temperature transmitter is installed to monitor the changes of the
temperature.
 Regular maintenance is needed to prevent any leakage from occur.

11
1.1.2.2 Heat Exchanger, E-02

Figure 3: P&ID Drawing for Heat Exchanger, E-02

12
Feed stream into the heater E-02 consists of O-Xylene which are used to react with air

in reactor. To control the system, feedback control schemes is applied. Hence, a temperature

control loops are proposed at the outlet process stream of this heater. Temperature control loop

with the aim to measure the temperature before going into multi-tubular reactor, R-01 in which

the operating condition must be at 300⁰C. For safety purpose, high alarms, low alarm as well

as by-pass valves are installed in case of maintenance.

Table 3: Summary of Control Loops for Heat Exchanger, E-02

Control Loop Temperature

Objective To control the outlet process liquid temperature at

Controlled Variable Outlet temperature of Heat Exchanger

Manipulated Variable Flow rate of steam supply

Disturbances  Inlet temperature of heat exchanger feed.


 Inlet flow rate of O-Xylene

Control Structure Single loop, PID controllers with feedback control strategy.

Additional Considerations  For plant safety and the quality control of the production,
high and low temperature alarms are installed.
 Temperature transmitter is installed to monitor the changes
of the temperature.
 Regular maintenance is needed to prevent any leakage from
occur.

13
1.1.2.3 Heat Exchanger, E-03

Figure 4: P&ID Drawing for Heat Exchanger, E-03

14
The main function of the control loop system in heat exchanger is to maintain the outlet

process liquid (reactor products) temperature at desired value. This can be achieved by

controlling the exit temperature of the hot fluid in response to variations of the operating

conditions (P.Sivakumar, 2012). The controlled variables in this control loop system are tube-

side outlet temperature. The manipulated variable is the flow rate of cooling water on the shell-

side. While the main disturbances are flow rate and temperature of reactor products in S8 on

tube side.

Feedback control configuration is chosen to maintain the outlet product temperature.

The PID controller is used to measure the temperature of outlet product of heat exchanger by

using temperature indicator and controller (TIC). Temperature transmitter (TT) measures the

outlet product temperature and sends electrical signal to TIC which is then compares the

measured temperature with its set point and sends electrical signal to I/P converter. The I/P

converter converts the electrical signal to a corresponding pneumatic signal used to accurately

position the control valve.

Table 4: Summary of Control Loops for Heat Exchanger, E-03

Control Loop Temperature


Control Objective To maintain the outlet process liquid (reactor products)
temperature at desired value from 300˚C to 45 ˚C.

Controlled Variable Tube-side outlet temperature

Manipulated Variable Cool water flow rate on the shell-side

Disturbance Flow rate and temperature of reactor products in S9 on tube side.

Control Structure Single loop, PID controller, feedback control strategy

Additional Considerations Availability of by-pass for control valve for maintenance.

15
1.1.2.4 Heat Exchanger, E-04

Figure 5: P&ID Drawing for Heat Exchanger, E-04

16
The main function of the control loop system in heat exchanger is to maintain the outlet

process liquid (Phthalic Anhydride and Maleic Anhydride) temperature at desired value. This

can be achieved by controlling the exit temperature of the hot fluid in response to variations of

the operating conditions (P.Sivakumar, 2012). The controlled variables in this control loop

system are tube-side outlet temperature. The manipulated variable is the flow rate of steam on

the shell-side. While the main disturbances are flow rate and temperature of reactor products

in S11 on tube side.

Feedback control configuration is chosen to maintain the outlet product temperature.

The PID controller is used to measure the temperature of outlet product of heat exchanger by

using temperature indicator and controller (TIC). Temperature transmitter (TT) measures the

outlet product temperature and sends electrical signal to TIC which is then compares the

measured temperature with its set point and sends electrical signal to I/P converter. The I/P

converter converts the electrical signal to a corresponding pneumatic signal used to accurately

position the control valve.

Table 5: Summary of Control Loops for Heat Exchanger, E-04

Control Loop Temperature


Control Objective To maintain the outlet process liquid (reactor products) temperature at
desired value from 45˚C to 250.17 ˚C.

Controlled Variable Tube-side outlet temperature

Manipulated Variable Steam flow rate on the shell-side

Disturbance Flow rate and temperature of Phthalic Anhydride and Maleic Anhydride
in S12 on tube side.

Control Structure Single loop, PID controller, feedback control strategy

Additional Availability of by-pass for control valve for maintenance.


Considerations

17
1.1.2.5 Switch Condenser, SC-01

Figure 6: P&ID Drawing for Switch Condenser, SC-01

18
The main objective is to sustain the temperature and flow of the process fluid from the

outlet of the switch condenser. Stream temperature can be controlled via manipulating the

flowrate of inlet stream in the Temperature Indicator Control (TIC) inside the control room.

The higher the flowrate of the medium entering the tube side, the faster the rate of heat transfer

between the oil and the process fluid. Thus, this will help to maintain the outlet process fluid

temperature at the desired range. Therefore, the temperature control must be taken into serious

consideration to prevent the occurrence of extreme temperature changes in this equipment

because exceeding the operating temperature of the process fluid might obstruct the

performance of the subsequent processes.

To ensure the safe operation of the switch condenser at the desired temperature, useful

control systems were applied. Oil is supplied to the shell side of the switch condenser to

maintain the outlet temperature of the process fluid. The temperature transmitter (TT) that

mounted on the pipeline of the switch condenser inlet stream measures the process fluid (tube

side) temperature and sends electrical signal to TIC which is then converted to pneumatic signal

by convert it to control the opening and closing of the valve that mounted onto the alarm

system. For the alarming purposes, high alarms were installed in this unit due to the high

sensitivity of the switch control. If the temperature of the switch condenser inlet goes to unusual

temperature or flow, the alarm will be functioning and alert the operator or engineer in charge

within 5 minutes.

Flow controller is applied in the process as well to ensure the flow can be monitor

during the purging of the gas or before transferring to the heat exchanger (E-04). A pneumatic

signal at valve VC-340 is placed in order to control the signal. Thus, the signal will be send off

to the control room via electric signal at FIC. Thus, the flow of the major product and the minor

product can be controlled and observe during the production. Since the switch condenser

19
consisted of 3 condensers inside it, the coolant is an oil and it heat up the oil to cool down the

switch condenser. It is important to observe the temperature and the flow inside this switch

condenser because this equipment can be classified as a sensitive equipment.

Table 6: Summary of Control Loops for Switch Condenser, SC-01

Control Loop Flow Temperature

To ensure that the outflow of the To maintain the temperature since

switch condenser does not exceed the switch condenser can be


Objective
the limits. considered as a sensitive

equipment.

Fluid flow of the outflow of the The temperature inside the

Controlled Variable Switch Condenser (SC-01) in pipeline before entering Switch

stream 10 Condenser (SC-01)

Flow rate of outflow by-product Temperature of the incoming


Manipulated Variable
fluid.

 Fluctuations of feed in  The existence of Eddie’s

Disturbances pipeline Current in the stream.

 Air Turbulent flow

Control Structure Single loop system, PI controllers with feedback control strategy

 Installation of high alarms system


Additional Considerations
 Regular maintenance to ensure no corrosion and leakage happen.

20
1.1.3 Reactor
1.1.3.1 Multi-Tubular Reactor, R-01

Figure 7: P&ID Drawing for Multi-tubular Reactor, R-01

21
Our proposed plant consists of single packed bed reactor whereby inlet stream contains

O-Xylene and air from the feed as our raw material while the outlet streams consist of desired

product which is Phthalic Anhydride and together with other by-products such as maleic

anhydride, carbon dioxide, carbon monoxide, oxygen, nitrogen and water. The reaction inside

this reactor takes place at 300 ⁰C and also 1 bar. Salt water flows inside the reactor for

continuous heat removal and to maintain the reaction temperature. 2 different variables have

been identified in this control strategy that plays significant role in terms quality and safety

aspect of the product and plant. This include temperature and flow.

Cascade control structure is used in the system to maintain the operating temperature

of reactor at 300 ⁰C. The temperature of the reactor is controlled by regulating the flowrate of

salt water supply. Feedback control structure is introduced in the system to maintain the

temperature of reactor at 300°C since it is an isothermal reactor. Flow transmitter and flow

control device is used as slave controller whereas temperature control loop serves as master

loop. The control valve for salt water supply is fail-open valve as the coolant must be

continuously supplied to the reactor to ensure the isothermal conditions. Temperature sensors

and transmitters are installed to measure the temperature of the reactor to observe the reactor

temperature profile. However, it should be note there are disturbance variable of the inlet

flowrate temperature of O-Xylene and air that could not be controlled. It is also important to

highlight that the reaction is highly exothermic, therefore the rate of reaction is also considered

as disturbance to our control strategy. Fail-opened control valve is used to avoid temperature

build up in case of failure. Alarm system is installed to alert the operation personnel in case the

temperature is higher or lower than desirable temperature of 300oC.

Flow rate control loops are installed at the reactor’s inlet; S-3 and S-6 respectively

to make sure the inlet flow rate of reactant of the reactor are at the desired set point. A fail-

22
closed control valve also is used to avoid excessive amount of reactant which could

increase the pressure inside the reactor indirectly.

Since this reactor operates at 1.0 bar, a pressure transmitter with high alarm is

installed to maintain the reaction’s pressure. As a safety feature, a fail-opened control

valve is used to prevent pressure building up inside the reactor R-01.

Table 7: Summary of Control Loops for Multi-Tubular Reactor, R-01

Control Loop Temperature Flow rate


To maintain the temperature in the To maintain amount of air and O-
Objective Xylene
reactor at 300oC
Controlled Temperature of reactor R-01 Inlet flow rate of the reactor, R- 01
Variable(s)
Manipulated Inlet salt water supply flowrate Inlet flow rate of the raw
Variable(s) material, S-3 and S-6.

 Temperature of inlet stream of Temperature of the raw material


stream, S-3 and S- 6.
Disturbances reactor
 Rate of reaction
PID controller with cascade control  Ratio control to control the flow
Control rate of reactants.
strategy
Structure  PID controller with feedback
control strategy.
 Install alarm for detection of high and low temperature.
 By-pass available for control valve maintenance purpose.
Additional
 Manual on-off valve is installed at the relative control valve for ease of the
consideration
maintenance of the control valve.
 Pressure relief system with 15% margin to avoid pressure build-up.

23
1.1.4 Auxiliary Equipments
1.1.4.1 Centrifugal Pump, P-01, P-02 and Storage Tank

Figure 8: P&ID Drawing for Centrifugal Pump, P-01

24
The flow and level of the liquid O-Xylene in the storage tank, TK-01 is to be controlled

by regulating the flowrate of the feed entering the acid storage tank in order to ensure the level

of the liquid O-Xylene. A drainage valve is used to avoid overflow of the feed in case of failure.

As for the additional considerations, alarm systems are added to detect any undesired changes

in flows. The controller valve that manipulates the inlet flow rate of o-xylene is a type of fail-

close valve. The installation is essential to ensure that in the case of controller valve failure,

the inlet flow of the reactant will be stopped, preventing the liquid o-xylene from over-flowing.

This concept is also used for P-02.

Table 8: Summary of Control Loops for Centrifugal Pump, P-01

Control Loop Flow

To ensure that the incoming feed does not exceed the


Objective maximum or go to below that the minimum limits.

Fluid flow of the incoming feed into the O-Xylene tank


Controlled Variable (TK-01)
Liquid flow rate of incoming O-Xylene.
Manipulated Variable

 Fluctuations of feed in liquid O-Xylene tank


Disturbances  Turbulent flow in the tank
Single loop system, PI controllers with feedback control
Control Structure strategy
 Installation of high- and low-level alarms.
 Install drainage system at the bottom of the acid storage
Additional Considerations tank to ease cleaning process and to avoid overflow.
 Regular maintenance to ensure no corrosion and leakage
happen.

25
1.1.4.3 Centrifugal Compressor, C-01

Figure 9: P&ID Drawing for Centrifugal Compressor, C-01

26
No control system in this unit but the Pressure Transmitter (PT) is placed to control the

compressor motor from the pressure flow in pipeline as the operating pressure of the centrifugal

compressor is at ambient condition from the input stream. No control valve at this unit. Pressure

indicator and temperature indicator is placed at the pipeline to indicate the pressure and

temperature before entering the Heat Exchanger, E-01.

Table 9: Summary of Control Loops for Centrifugal Compressor, C-01

Control Loop Flow

To ensure that the incoming feed of the air does not exceed
Objective the maximum or go to below that the minimum limits of the
compressor.
Power rate of the compressor motor
Controlled Variable

Pressure rate of incoming air.


Manipulated Variable

 Fluctuations of feed in centrifugal compressor


Disturbances  Air Turbulent flow
No control loop
Control Structure

 Installation of pressure indicator and temperature


Additional Considerations indicator

27
1.2 Summary of Control Loop for Each Equipment

The following table summarized the control loops each equipment:

Table 10: Control loops summary list

Equipment Code Control loop Control Structure Objective


To ensure that the incoming feed of the air does not
Compressor C-01 Pressure No control loop exceed the maximum or go to below that the minimum
limits of the compressor.
To ensure that the incoming feed does not exceed the
Centrifugal Pump P-01 Pressure FB PID Single loop
maximum or go to below that the minimum limits.
To ensure that the incoming feed does not exceed the
Centrifugal Pump P-02 Pressure FB PID Single loop
maximum or go to below that the minimum limits.

Temperature FB PID Cascade loop To maintain the temperature in the reactor at 300oC
Mutitubular reactor R-01
Pressure
FB PID Ratio controller To maintain amount of air and O-Xylene
Flow rate
E-01 Temperature FB PID Single loop To control the temperature of the outlet of heat exchanger
E-02 Temperature FB PID Single loop To control the outlet process liquid temperature at 300 oC
To maintain the outlet process liquid (reactor products)
E-03 Temperature FB PID Single loop temperature at desired value from 300˚C to 45 ˚C.
Heat Exchanger
To maintain the outlet process liquid (reactor products)
E-04 Temperature FB PID Single loop temperature at desired value from 45˚C to 250.17 ˚C.

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To ensure that the outflow of the switch condenser does
Flow rate FB PID Single loop not exceed the limits.
Switch Condenser SC-01

To maintain the temperature since the switch condenser


Temperature FB PID Single loop
can be considered as a sensitive equipment.
To maintain the temperature at the structured packings
FB PID Cascade loop
zone and the bottom.

Temperature To maintain the temperature of product phthalic

FB PI Single loop anhydride at 283.8 °C

Distillation
T-01 To maintain the reflux ratio of column T-01 to indirectly
Column
Flow FB PID Ratio controller control the purity of distillate

To maintain the column pressure at 1.01 bar and avoid

Pressure FB PID Single loop over pressure of T-01

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1.3 Plant Layout Drawing

1.3.1 Description of Plant Layout

The Phthalic Anhydride plant is planned to build at Gebeng Intergrated Petrochemical

Complex (GIPC) which is in Gebeng, Pahang Malaysia. With the strategic location, GIPC will

give benefits to development of the chemical industry in Malaysia. The main aspects that taken

into consideration of choosing GIPC as location to build the Phthalic Anhydride plant are:

1. Utilities

Present of high availability of water and electricity resources for the production

process of the proposed plant.

2. Labor

Skilled labor are highly available for conducting the operation and maintenance of the

proposed plant.

3. Location and transportation

A location of proposed plant is convenient and logistic as it located a few kilometers

away from Kaneka Kuantan port terminal and the road systems are highly accessible.

4. Job opportunity

Provides job opportunities for local community around the outskirts of Gebeng.

A plant layout with a proper arrangement of building or facilities is important to ensure the

safety and smooth-running plant to occur. The process units and auxiliary buildings should be

laid out to give the most potential economical flow of materials and employees around the site.

Hazardous substances should be isolated away from other buildings. Evacuation path is

provided in the plant layout to lead the employees correctly toward the assembly point in case

30
of emergency which is located near the side gate of the plant at a safe distance away from

process units and hazardous chemicals in plant as well as at the downwind location to avoid

gas emission effects from prevailing wind. The justification for the locating of the units and

buildings is provided in the table below.

Table 11: Justifications of Plant Layout

Building /facility Justification(s)

Security office The security office is located near the main gate. Its function as

place for security offices to discuss and handle security issues and

management. As well as to monitors the trucks, visitors or outsiders

that enters the plant.

Security booth Security booths are located at all gates of the plant. Its function is to

provide security checks and inside access to workers, incoming

clients, transport trucks and outsiders entering the plant.

Assembly point A place for all the workers to gather during the case of emergency

when evacuating the building.

Car park The car parking lots are located near the main gate and car owners

are advised to reverse park to ensure rapid exit from the plant.

Parking area also can be use as reversed assembly area for workers

personnel in the case of emergency as it is close to these locations.

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Administration Building The buildings are isolated away from the production line as well as

and Cafe hazardous materials and located near the main entrance of plant for

the ease of customers or visitors service and safety issues. Since, the

buildings are located within proximity of the assembly point and the

main gate to ease evacuation procedures during emergency case.

Medical Facility Medical building is located near to plant area to provide medical

service immediately once needed.

Emergency Water Tank It functions as water reservoir for emergency purpose.

Utility Facilities It provides utilities for the auxiliary services needed in the operation

such as electricity, steam (for process heating), cooling water and

water for general use. As well to give an easy access of running

pipes to and from process units.

Emergency Power Generator To provide back-up supply of electricity in case of electricity supply

cut or during emergency purpose which requires the use of

electricity.

Fire Station and Fire Water A fire station and fire water tank are placed near the plant area to

Tank extinguish hazardous fire during accident or emergency.

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Research and Development A center for researchers to carry out research on improve the

(R&D) Centre production process.

Process Control Department Control building is positioned at a strategic location so that the

process control engineer can monitor the overall plant from the

building. Control room is situated adjacent to plant area to save cost

in signal wiring. It is located near to assembly area in order to make

sure workers able to run for their lives if there is any emergency or

accidents.

Process control room is located just beside the plant to monitor the

overall plant. It is located just beside reaction unit since they require

more intimate attention from the operator than the other units.

Immediate monitoring can be provided if there is any run-over

reaction happening.

Quality Control Department The department is located near the production lines to allow fast

analyses on the quality of products and other chemicals. Immediate

actions can be taken if necessary.

Warehouse The warehouse located near to production process to make

transportation easier for raw material and located not far from the

main gate to ease the delivery of the products for sale. It also

provides space for storing raw materials and products before

distributing them.

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Workshop The workshop provides maintenance services for any unit

operations or machines. Sufficient space must be provided in the

workshop to permit access for heavy lifting of the equipment.

Product Storage Product storage is temporary storage for the products and to provide

transfer of the products. It is situated right next to the final process

unit thus reducing much conveyer cost.

Loading and Unloading To provide secure and efficient area for loading and unloading of

Sites things from trucks. It situated next to product storage and warehouse

where near to main gate and side gate respectively. As well as to

make loading and unloading of the works easier.

Wastewater treatment The wastewater treatment located near the production process to

ease up the treatment of wastewater produce from all equipment.

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1.3.2 Plant Layout

Figure 10: Plant Layout Phthalic Anhydride Production

35
1.4 Selection of Instrumentation and Equipment

1.4.1 Selection of Sensors and Calibration / Maintenance of Sensors

The table below shows the selection of sensors use in Phthalic Anhydride production Plant.

Parameter Sensor Selection Brand Justification

Temperature Type T Thermocouple Techno Instruments Type T Copper-Constantan Thermocouple is

chosen for our plant as it is stable at lower

temperatures and the recommended temperature

range for this type of thermocouple is -270 oC to 400


o
C. Thermocouple is made up of stainless steel,

suitable for any liquid application, lower cost and a

durable sensor.

Pressure Pressure Transducer TE Connectivity (TE) The Pressure Transducer which is chosen for our

plant since, the particular sensor is designed to

measure pressure under a wide variety of

36
conditions, including hostile environments and

temperatures up to 150 oC. The sensor has excellent

temperature stability, high accuracy, able to produce

faster response and also results in long term

performance.

Flow Flow Sensor (gas) – Ultrasonic Greyline Instruments This sensor is chosen because the sensor is typically

Gas Meter SFM6.1 Corporation mounted on the outside of pipe and it is also

unaffected by the abrasive gas or harsh chemicals.

It is also continuously measures the flow and

portrays the data in the form of charts and tables for

easier understanding of the user. This unit also may

benefit the industry in terms of maintenance cost as

it does not require one.

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Flow Sensor (liquid) – Icenta Controls LTD The sensor is a flexible and comprehensive sensor

Electromagnetic Flow Sensor program, which is deliverable in a wide range of

(SITRANS F M MAG 3100P) sizes. In additional to that, SITRANS F M

electromagnetic flow sensor is also widely used in

industries such as process industries and chemical

industries. This unit also possess excellent chemical

resistance during high process temperature, suitable

for reactor equipment.

Level Level Sensor (solid) – Radar Endress+Hauser Levelflex FMP50 is the instrument for basic

Level Sensor (Levelflex FMP50) applications in liquids which do not place high

demands on temperature and pressure ranges or

chemical resistance. Particularly in basic supply or

storage applications as well as utility processes

FMP50 is the best choice. Levelflex FMP50 guided

radar can be used for continuous level measurement

38
of liquids, pastes and slurries. The sensor also has

highest reliability due to new Multi-Echo Tracking

evaluation.

Level SSensor (liquid) – Siemens In the plant, level sensor is used to detect the level

Capacitance Level Transmitter of liquid in a vessel such as in vacuum evaporator

(Pointek CLS300) and falling film evaporator. The level transmitter

chosen which the capacitance level transmitter is an

ideal for standard chemical industry applications.

The particular sensor is also to operate under heavy

solids applications where abrasive materials occur

as in the mining industry It is also idea for detecting

liquids, solids, slurries, foam and interfaces in

demanding conditions where high pressure and

temperatures are present.

39
Calibration and Maintenance of Sensors

Temperature Sensor

Thermocouple

Calibration [1]

Plot voltage-temperature curve

1. Fill the thermo bath container with water and switch on the thermo bath.

2. Heat up the water up 30℃ and turn on the thermocouple.

3. Connect the thermocouple one end to each lead of the multimeter. The multimeter

should be able to measure up to 1 microvolt.

4. Next, place one junction of the thermocouple into the water and let the voltage to

stabilize. Record the voltage value from multimeter.

5. Then, rises the water temperature up to 35℃ and record the voltage value. Repeat this

step for each 5℃ increases of water temperature from 35 to 60℃.

6. Measure the room temperature and find the voltage value for the thermocouple at room

temperature. The voltage value is added to each value that are recorded in steps 4 and

5.

7. Use suitable curve-fitting method to find the best fit line of the recorded data. The slope

line should provide the voltage increase for each degree of temperature increase.

40
Maintenance [2]

i. Prevent excessive bending of thermocouples.

ii. Avoid cold work on thermocouple as it can decreases the thermocouple insulation

resistance at certain points and causing short circuits or lowering the accuracy.

iii. Use protection tubes on thermocouple for corrosive atmospheres.

iv. The protection tube should always be inspected when changing thermocouples such as

cracks, pinhole, contamination and discoloration.

v. Place the thermocouple away from heating element.

vi. Record the causes of failure and life span for each thermocouple to help track down the

potential problem.

41
Pressure Sensor

Pressure Transducer

Calibration [3]

Figure 11: Calibration Pressure Transducer

1. Remove the electronics module cover to allow the excess for transducer terminal.

2. Set the switch settings for different input-output configuration to achieve the desired

input-output range.

3. If the control device in the control loop is being used as current source, connect the

control device to the pressure transducer as shown above otherwise, disconnect the

device and connect the current source to the transducer incorporating a current meter to

monitor the calibration operation as shown above.

4. Make sure the supply pressure to the pressure transducer is at least 20 psig.

5. Adjust the input current to the low mA DC value e.g. 4mA in the case of a 4 to 20 mA

output calibration.

42
6. Ensure that the output pressure of the pressure transducer is 0.2 bar or 3 psig. If not,

trace the ZERO adjustment screw and adjust the ZERO potentiometer until the output

pressure is 0.2 bar or 3 psig. Note ZERO and SPAN adjustment screw are noticeably

visible and labelled.

7. Next, adjust the input current to the high mA DC value e.g. 20mA in the case of a 4-20

mA input calibration.

8. Make sure the output pressure is at 1 bar or 15 psig. If not trace the SPAN adjustment

screw and adjust the SPAN potentiometer until the output pressure is 1 bar or 15 psig.

9. Repeat steps 5 to 8 until the output pressure of the pressure transducer is within the

referenced accuracy requirement stated by the manufacturer without further adjustment.

10. If other current source is used, disconnect the current source and reconnect the control

device. Now, the pressure transducer is ready to be in operation.

Maintenance [4]

Regularly check the pressure transducer pressure connections for leaks and tighten as needed.

Also, keep all electrical connections between the system and components free of water and

spray.

Flow sensor (gas)

Calibration [5]

1. Gases are measured by flow meters that consist of one or two tubes that vibrate as gas

passes through it creating Coriolis effect.

2. It is done to measure the volume flow, mass flow, standard flow and density.

3. This way it can avoid errors from possible air bubbles in the tube and have more

accurate and dependable measurements.

43
Maintenance [6]

1. Remove the flow meter from the line. Remove excess piping from meter.

2. Thoroughly wipe off the entire flow meter surface using mild detergent or isopropyl

alcohol.

3. Remove the inlet cap from the flow meter, noting the sequence of disassembly for later

reference.

4. The internal parts are secured with a retaining ring. Remove the retaining ring and the

internal wetted parts from the flow meter.

5. Place all parts on a clean work surface. Clean and inspect all parts. Replace any that

appear worn of damaged.

6. Check inlet port O-ring for damage and replace if required.

7. Reassemble spring, then piston assembly and retaining ring into flow meter.

8. Install metering cone plate assembly, retaining spring and secure with inlet cap.

9. Reinstall meter to the line.

Level sensor

Calibration [7]

1. Set up the guided level sensor, communicator, power supply and multimeter.

2. Check the configuration of the lower range value (0% level, 4 mA) and high value

(100% level, 20 mA).

3. Fill the level sensor chamber with water up to 0% level. Read the level measurement in

the communicator. Set this condition as 0% level through communicator.

4. Read the mA output of the sensor by using a multimeter. Adjust through the

communicator so that the output of the sensor is 4 mA.

44
5. Fill the level sensor chamber with water up to the 100% level. Read the level

measurement in the sensor communicator. Set this condition as 100% level through the

communicator.

6. Read the mA output of the sensor by using a multimeter. Adjust through the

communicator so that the output of the sensor is 20 mA.

Maintenance [8]

1. Remove the level sensor from the water circuit compartment.

2. Detach the cap from the level sensor, add about 500 ml of deionized water and reattach

the cap of the sensor.

3. Shake the sensor in all directions to wash the inner part.

4. Detach the cap and empty the sensor.

5. Repeat steps 2 to 4 for three times.

6. Reinstall the level sensor in the water circuit compartment as before.

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1.4.2 Selection of Valves and Calibration / Maintenance of Control Valves

The table below shows the advantages and justification of selection valve use in Phthalic Anhydride production Plant.

Types of Valve General Functions/Advantages Justification


Diaphragm Valve The diaphragm valve utilizes a flexible diaphragm that  Excellent control of the flow of fluid
connected to a compressor by a stud which is molded into containing suspended solids.
the diaphragm. The compressor is moved up to increase  Applied in the control of the flow for low
the flow while it is lowered to stop the flow. pressure gas and liquid including slurries and
viscous liquid.
 Suitable for hazardous chemical.
Gate Valve This mechanism mostly to function as fully open or fully  Can be used as isolation valve during
close. To prevent fluid hammer which is detrimental to maintenance for pumps and control valve as
the piping systems, this valve enables slow operation. it can fully open or closed.
Positive seal is provided for the valve at the fully closed
condition.

Screw-Down Valve This valve is more related to the bypass manual control of  Provide the alternative flow when the main
the flow rate of fluid. Besides, it is employed by fully control valve is under maintenance.
close or fully open the stream manually when there is

46
malfunction to the automatic control system. It is also  Installed parallel with control valve to bypass
being useful during the process start-up and shut-down through a control valve when it is necessary.
because it provides a tight seal when it is closed.

Drainage Valve This valve is used to control the overflow in the  Provide alternative flow when the equipment

equipment by manual control of the flow rate of the fluid. level overflow.

It is employed by fully closed or fully open the stream

manually when there is malfunction.

Control valves in the Phthalic Anhydride production plant with their respective failure positions are listed in the table below:

Failure Position Justifications


Fail-Closed This type of control is used in switch condenser with heating process. When it fails, it will be closed
fully automatically to stop the flow of heating medium. This can prevent overheating which may
vaporize the process solid and eventually lead to explosion.
Fail-Opened This type of control is used in reactor with cooling process. When it fails, it will be open fully
automatically to allow continuous flow of cooling medium. This can prevent overheating especially in
exothermic reaction.

47
Calibration and Maintenance of Control Valves

Calibration [9, 10]

Control valves requires regular calibration to reduce the response time due to disturbance or

changes that happen in the process line of the plant. The calibration procedures of a control

valve are as follows:

i. Ensure that the supply gauge shows the maximum pressure to line. After connecting

the input test pressure regulator to the positioner.

ii. Move the flapper assembly to the mid of range of the operating quadrant beam and

apply pressure to the valve positioner. A minor nozzle height adjustment should be

performed to make the desired input signal value correspond to the starting point of the

travel.

iii. Apply an input signal equal to the low value of the input signal. The signal range in our

plant I assumed to be 3 to 15 psig, thus lowest input value of 3 psig must be set. Loosen

the nozzle locknut and adjust the nozzle pin to set the output zero.

iv. Insert an input signal equal to the high value of the signal range e.g. this case is 15 psig

and observe the actuator stem travel. Move the flapper assembly to a higher number on

the beam (increase the steam travel) if the stem travel is shorter than the expected range.

Move the flapper assembly to a lower number on the beam (decrease the travel) if the

desired stem travel occurs before the input signal reaches 15 psig.

v. Repeat the above steps until the correct travel is achieved.

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Maintenance [11]

In-service inspection and periodical maintenance are two type of maintenance process

that are commonly practice and perform in a plant. In-service inspection is a test or series of

tests performed on a frequency established by the manufacturer based on prior experience with

the system/equipment/component or upon engineering analysis of the probable failure rate for

the equipment. This type of maintenance is suitable for process that encountered any

disturbances due to the malfunction of control valves. The operators should proactively check

for any leakages or dead band issues in the control valve. Microprocessor based diagnostic

tools, ValScope-PRO can provide assistances to operators to detect problems such as dead band

or stickiness and perform a root cause analysis on the complete control system. Therefore, the

inspection and maintenance can be done by the operators without shutting down the whole

plant.

Periodical maintenance is a scheduled maintenance that carried out at regular interval of time.

The following steps must be taken account during the scheduled maintenance:

i. Make sure no air leak between the diaphragm case and diaphragm.

ii. Make sure no process fluid is leaking from the bonnet and flanges.

iii. Make sure the yoke clamp bolt is not loose.

iv. Make sure no air leak from the actuator’s air pipe.

v. Make sure no loose bolts on the stem connector that connects the actuator stem to the

valve stem.

vi. Make sure the actuator stem and valve stem are not warped and show no sign of

damage.

vii. Ensure the valve operation is smooth and valve lift is correct.

49
viii. Make sure the control valve does not generate any abnormal sound or vibration.

ix. Ensure the gland packing section does not leak. If the control valve has a lubricator,

occasionally lubricate and tighten the gland packing section.

x. If the Control valve has a manual handwheel, check that the pointer of the operation

nut conforms with the AUTO position and that the hand-wheel is locked.

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1.5 Control Loop Simulation via ASPEN Dynamic

ASPEN Dynamic Analysis for Multi-Tubular Reactor (R-01)

Pressure control loop

The steady state simulation that was done is Aspen Plus V10 is converted into

Dynamic mode and run via ASPEN Dynamic. Additional information which is the

dimensions of the reactor are provided to the software for this simulation. ASPEN Dynamic

allow user to simulate real time behaviour of the system. Pressure controller has been

incorporated in our reactor to control the pressure of gases inside the reactor to avoid

explosion in the reactor. The controller work by detecting the pressure of gases inside the

reactor and control the output flowrate.

Stream labelled as “7” indicates the feed input which consist of o-xylene and air.

Stream labelled as “8” indicates the product outlet which consist of phthalic anhydride,

51
maleic anhydride, carbon monoxide, carbon dioxide, water vapor, nitrogen, oxygen and

unreacted o-xylene.

The primary objective of this loop is to control the pressure inside the reactor. A

dynamic simulation with a setpoint change is illustrated in the figures below.

Figure 12: Initial Condition Before Any Changes

It is an initial result when the system does not change. The response shows that the

pressure (2.55 bar), mass flow rate (1418.40 kmol/hr) and temperature (300˚C) remain constant

throughout the first 2 hours when the time is paused at 2 hours.

52
Figure 13: Pressure Controller is Changed to 5 bar

The process was run with initial set point value of 2.55 bar and it is the initial steady

state level for the reactor. After 2 hours of running the process, a set point change was

introduced to the system. The pressure controller is given a new set point which is 5 bar. There

was a sudden increase in temperature which is from 300 ˚C to 314 ˚C. It also results a small

drop in the flowrate which is from 1418.40 kmol/hr to 1414.40 kmol/hr. For a moment of time

it can be seen from figure (2) that the controller reduced its output to hold the feed inside the

reactor before increasing it back to maintain the pressure. However, both the temperature and

flowrate returned to its initial values and reached a steady state. Therefore, no oscillation is

observed in the controller dynamic after that.

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1.6 Piping and Instrumentation Diagram (P&ID) for The Whole Plant

The P & ID drawings of Phthalic Anhydride production plant are divided into mainly 5 parts as

listed below:

i. P & ID for Compressor, Pump and Heat Exchanger

ii. P & ID for Multi-tubular Reactor and Auxiliaries

iii. P & ID for Switch Condenser and Auxiliaries

iv. P & ID for Distillation Column and Auxiliaries

v. Symbols, Abbreviations and Legends.

** Kindly refer the following pages for the P & ID drawings.

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55
56
57
58
59
CHAPTER 2: ENGINEERING ETHICS IN PLANT DESIGN

2.1 Ethics Problem

Ethics problem occurs when a condition that requires a person and organization to choose

between alternatives solution that either to be evaluated as ethical (right) or unethical (wrong).

For ethical problems to be arise this might be due to encounter of limitation of data as well as

during decision making session for the design tasks.

During the progress in completing the plant design tasks that given, we encounter lack

of data that are not available in the recommended reference books such Coulson & Richardson

Chemical Engineering Design Handbooks, Perry Chemical Engineering Handbooks, and

Chemical Engineering Design: Principles, Practice and Economics of Plant and Process Design

which are required to perform the design calculations. Thus, the lack information is then being

search through either literature review or by utilizing Aspen Plus software to find the required

physical and chemical data. Even when there are still lacking information, we conducted a

discuss to solve the problem by making logical assumptions and rationalizing them through

proper justifications.

One of problem that we encountered during completion of the design task is the

simulation of switch condenser using Aspen Plus solution. Due to absent of switch condenser

equipment in ASPEN, we cannot run the simulation. Thus, we are not able to design the switch

condenser using Aspen Plus. Besides that, we also encountered problem in designing unit

operation which are not covered during lectures. For instance, we faced some difficulties in

60
designing the switch condenser because we have limited knowledge about this unit operations.

However, we decided to search for extra information from the book in library or internet besides

seeking advice from supervisor to solve this problem.

Moreover, another ethical problem that we encounter is during the performance of

equipment costing using Aspen Plus Economic Analysis. The equipment sizing would never

meet our design specification after a series of accurate equipment mapping procedure since they

are auto-sized by Aspen software. Thus, the costs computed from the Aspen Economic Analysis

at this step would not be reliable. Therefore, we choose to stick with manually calculated each

cost of equipment’s as this method is more accurate.

We can save more time on solving the problem that we encounter by sharing with our

supervisor as they are more experience. We should be seeking advice from the lecturers who

had taught us on the related subject. As it can help to ease the difficulties that occurs during task

completion. After all the design project is conducted in a limited period, hence some assumptions

have been made for us to complete the tasks given.

As a future engineer, moral duty is undeniable dominant to be respected and practiced

by all of us in designing the plant. Discussion should be conducted with every team member as

it one of the examples of ethical duty. Every group member should be able to give out opinions

before critically choose the right selection to design the unit without involving any ethical issues.

Discussion among the group members could make the group address the hassle and preserve the

progress up-to-date. In short, engineers should usually uphold and develop the integrity, honour

61
and dignity of the engineering career by way of the use of their expertise and abilities for the

improvement of human welfare.

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2.2 Code of Ethics

Code of ethics, also recognized as the Professional Conduct Code, is important as a

trademark of professionalism for engineers. It is a document outlining the business or

organization's mission and values, how professionals are supposed to address issues, the ethical

principles based on the core values of the organization, as well as the standards to which the

professional will be held. It defines the basic requirement of qualifying as an engineer while

setting the limit and edge during a competitive working environment that can ensure the

professional's ultimate benefit. Four sets of Code of Ethics are discussed in this section and are

published by:

1. The Institution of Engineers Malaysia (IEM)

2. Boards of Engineers Malaysia (BEM)

3. American Institute of Chemical Engineers (AIChE)

4. American Petroleum Institute (API)

Since the proposed plant is located in Malaysia, IEM and BEM would be the most associated

institutions whereby the Code of Ethics should always be strictly adhered to. However, AIChE's

Code of Ethics would be a good practice for all chemical engineers about global requirements.

63
2.2.1 The Institution of Engineers Malaysia (IEM)

Original Source: IEM Official Website (Retrieved on 6th April 2019) [12]

Malaysia's Engineering Institution, better known as the IEM. It is an experienced

professional society that serves more than 16,000 members in Malaysia, overseas and the

communities they work in. It was established in 1959 and in 1962 was admitted to the

Commonwealth Engineers Council. The institution is a professional engineering qualifying body

in Malaysia.

The following Professional Conduct Regulations shall be made by the Council in accordance

with Section IX of the Bylaws. ' Member ' means a member of any grade specified in Section II

of the Bylaws in these regulations, and ' employer ' includes ' client '.

1. A member shall at all times take care to ensure that his work and the products of his work

constitute no avoidable danger of death or injury or ill health to any person.

2. A member shall take all reasonable steps to avoid waste of natural resources, damage of the

environment, and wasteful damage or destruction of the products of human skill and

industry.

3. A member shall take all reasonable steps to maintain and develop his professional

competence by attention to new developments in science and engineering relevant to his

field of professional activity and, if he is an employer, shall encourage his professional

employees to do likeness.

4. A member shall not undertake responsibility as professional engineer which he does not

believe himself competent to discharge.

5. A member shall accept personal responsibility for all work done by him or under his

supervision or direction and shall take all reasonable steps to ensure that persons working

64
under his authority are competent to carry out the tasks assigned to them and that they accept

personal responsibility for work done under the authority delegated to them.

6. A member called upon to give an opinion in his professional capacity shall to the best of his

ability, give an opinion that is objective and reliable.

7. A member whose professional advice is not accepted shall take all reasonable steps to ensure

that the person overruling or neglecting his advice is aware of any danger which the member

believes may result from such overruling or neglect.

8. A member shall not make any public statement in his capacity as a professional engineer

without ensuring that his qualification to make such a statement and any association he may

have with any party, which may benefit from his statement are made known to the person or

persons to whom it is directed.

9. A member shall not, in self-laudatory language or in any manner derogatory to the dignity

of the profession advertise or write articles for publication, nor shall he authorize any such

advertisement or article to be written or published by any other person.

10. A member shall not recklessly or maliciously injure or attempt to injure, whether directly or

indirectly, the professional reputation, prospects or business of another engineer.

11. A member shall inform his employer in writing of any conflict between his personal interest

and faithful service to his employer.

12. A member shall not improperly disclose any information concerning the business of his

employer or of any past employer.

13. A member shall not accept remuneration in connection with professional services rendered

to his employer other than from his employer or with his employer's consent; nor shall he

receive directly or indirectly any royalty, gratuity or commission on any article or process

65
used in or for the purposes of the work in respect of, which he is employed unless or until

such royalty, gratuity or commission has been authorized in writing by his employer.

14. A member shall not improperly solicit work as an independent adviser or consultant, either

directly or by an agent, nor shall he pay any person, by commission or otherwise, for the

introduction of such work.

15. A member acting as an independent adviser or consultant shall not be the medium of payment

made on his employer's behalf unless so requested by his employer; nor shall he place

contracts or orders in connection with work on, which he is employed, except with the

authority of and on behalf of his employer.

2.2.2 Boards of Engineers Malaysia (BEM)

Original Source: BEM Official Website (Retrieved on 6th April 2019) [13]

The Board of Engineers Malaysia (BEM) is a statutory body established with perpetual

succession and a common seal under the 1967 Registration of Engineers Act, which can sue and

be sued. It was created in August 23, 1972. In addition to facilitating the registration of

engineers, Malaysia's boards of engineers play an important role in determining and regulating

the behavior and ethics of the engineering profession. They hear and determine disputes

concerning the professional conduct or ethics of registered engineers or appoint a committee or

arbitrator or arbitrators to hear and determine disputes of this kind.

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The guidelines for Code of Professional Conduct are outlined as the following:

1. A Registered Engineer shall always hold paramount the safety, health and welfare of the

public.

A Professional Engineer shall approve and sign those engineering documents that he

has prepared or directly supervised on preparation only. He shall certify satisfactory on

a completion of work that he has supervision on the construction and installation of the

work and it has accomplished the requirements of the engineering design and

specifications. A Registered Engineer cannot reveal any information without the

permission of client or employer except as it is required by law or affects public safety.

He also has to know the violation of engineering code and Local Authorities regulations

shall report to appropriate professional bodies and public authorities if relevant.

2. A Registered Engineer shall undertake assignments only if he is qualified by education

and experience in the specific technical fields in which he is involved.

A Professional Engineer shall not sign any document which he lacks competence

or not prepared under his direction and control. He shall not sign and stamp the

documents for an entire project unless each technical section of the project is signed and

stamped by the qualified engineer.

3. A Registered Engineer shall issue public statements only in an objective and truthful

manner.

A Registered Engineer should be honest in professional reports and include all

relevant data in the reports which is updated. He should only express technical opinions

which he has competence and knowledge of the facts. He should not issue any technical

matter that is inspired or paid by other interested parties.

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4. A Registered Engineer shall act for each employer or clients as faithful agent or

executor.

A Registered Engineer should reveal all conflicts of interest that could affect his

service. He should not accept any compensation and financial from more than one

party for services on the same project unless it is agreed by all interested parties. He

should not accept any valuable consideration from outside agents. He cannot make

decision on services which are provided by him or his organization. He should not

accept a contract from a body which his organization served as a member of that body.

5. A registered engineer shall conduct himself honourably, responsibly, ethically and

lawfully to enhance the honour, reputation and usefulness of the profession.

A Registered Engineer shall not misrepresent his qualifications and exaggerate

his responsibility. He should not offer any contribution that may influence the award of

a contract. He should not offer gift or pay a commission in order to secure work. He

should check the accuracy of facts and data before he signs any documents. He should

not be a medium of payment made unless it is requested by his client.

2.2.3 American Institute of Chemical Engineer (AIChE)

Original Source: AIChE Official Website (Retrieved on 6th April 2019) [14]

The Board of Directors of the American Institute of Chemical Engineers has adopted this

Code of Ethics to which it expects its members to comply with their professional conduct and

to which each applicant attests by signing their application for membership. Members of the

American Institute of Chemical Engineers shall uphold and promote the integrity, honor and

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dignity of the engineering profession by: being honest and impartial and serving their employers,

clients and the public with fidelity; striving to enhance the skills and prestige of the engineering

profession; and to use their knowledge and skills to improve human well - being. Members are

required to achieve these goals:

 Formally advise their employers or clients (and consider further disclosure, if warranted)

if they perceive that a consequence of their duties will adversely affect the present or

future health or safety of their colleagues or the public.

 Accept responsibility for their actions, seek and heed critical review of their work and

offer objective criticism of the work of others.

 Hold paramount the safety, health and welfare of the public and protect the environment

in performance of their professional duties.

 Issue statements or present information only in an objective and truthful manner.

 Act in professional matters for each employer or client as faithful agents or trustees,

avoiding conflicts of interest and never breaching confidentiality.

 Treat all colleagues and co-workers fairly and respectfully, recognizing their unique

contributions and capabilities by fostering an environment of equity, diversity and

inclusion.

 Perform professional services only in areas of their competence.

 Build their professional reputations on the merits of their services.

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 Continue their professional development throughout their careers and provide

opportunities for the professional development of those under their supervision.

 Never tolerate harassment.

 Conduct themselves in a fair, honourable and respectful manner.

2.2.4 American Petrolem Institute (API)

Original Source: API Official Website (Retrieved on 6th April 2019) [15]

You agree that you will always perform audit services on behalf of the API:

 Conduct your business in accordance with all applicable laws, regulations, auditing

standards and ethical standards of conduct,

 Adhere to facility safety standards and general industrial safety standards to protect your

health and well-being,

 Conduct yourself in a professional manner at all times during the course of the contracted

assignment,

 Avoid any personal relationships, activities, or financial affairs that may influence your

performance or create the appearance of a conflict of interest or an actual conflict of

interest,

 Use adequate safeguards to prevent the disclosure of any confidential information,

 Observe high ethical standards of conduct to ensure that the integrity of API’s programs

is protected,

 Immediately disclose to API any actual, potential or perceived conflicts, and

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 Immediately disclose to API any offers of bribes or other improper or unethical attempts

to influence your decision-making.

You, your immediate family or other members of your household shall not use your position as

an auditor to avoid any potential or perceived conflict of interest to:

 Offer any services to a facility or a company affiliated with a facility that you have

audited in the past 24 months or that you have been assigned to audit, where such services

would be provided by yourself, your immediate family members, or a company that you

or your immediate family members work for, contract with, or otherwise have a direct

or indirect financial interest in, or any affiliate of such a company. For purposes of this

code, your immediately family includes, but is not limited to, any member of your

household, your spouse, your parents, your children, or your siblings.

 Discuss future employment opportunities with any facility or a company affiliated with

a facility that you have audited in the past 24 months or that you have been assigned to

audit.

 Accept or solicit from any facility, which you or your company have audited or been

assigned to audit, any money or anything else of value for yourself, your family, your

friends, any company or organization in which you or your immediate family member

has a direct or indirect financial interest, or any affiliate of such a company or

organization. “Anything else of value” includes, but is not limited to, cash, gifts,

hospitality, services, commission, rebates, discounts, loans, vacations, event tickets,

entertainment, trips, or other items of value. A “financial interest” includes any

ownership stake, employment agreement, or independent contracting or consulting

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arrangement. Ownership of publicly traded securities does not itself constitute a

“financial interest” in a company under this policy.

 Give any gifts, money or anything else of value to any API employee or their immediate

family members.

 Otherwise use your position as an auditor to seek an improper benefit from a facility or

company affiliated with a facility.

2.3 Ethics in Environment, Safety and Health Problems.

In accordance to the Board of Engineers Malaysia (BEM) and the Institution of

Engineers Malaysia (IEM), the ethical codes proposed by these bodies highlight the importance

of safety, health and welfare of the public and protect the environment in performance of their

professional duties. In all aspects, plant safety should be given utmost priority to ensure safety

and efficient operation of the plant without any major negative impacts to the health and

environmental condition. In our proposed plant, the highest temperature and pressure recorded

are 353 ºC and 2 Bar. Generally, the operating conditions of each equipment are carefully

inspected and precautionary steps were undertaken in the designing of high operation condition

equipment in safe manner. In relation to that, safe operation of the plant is always taken into

consideration even in the choice of method to be implemented in producing safe anhydride

product. Other than that, utilization of one distillation unit in our plant instead of two distillation

unit further indicates our sincere concern in minimizing the use of hazardous materials as well

as our intention in maintaining the welfare of the labour and the cost.

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Inevitably, our plant also ensures zero waste were produced via using switch condenser

units with the aid of fume chamber to further eliminate off the unwanted by-product before shift

back into the main operation system. This act able to minimize the environmental waste loads

and ensures clean gases were emitted to the atmosphere as outlined by Statement (2) of the

IEM’s Code of Ethics. Generally, installation of these equipment is sustainable in terms of costs

and natural resource consumption. Such acts comply with the regulations set by the Department

of Environment (DOE). Moreover, all the equipment in our plant are also housed together to

further make sure that the excessive chemicals do not escape into the air and pollute the

surroundings. On the contrary, appropriate process control systems especially flow and pressure

controls alongside indicators and alarms were also installed in our plant to maximize the safety

of the plant operation.

Furthermore, the process controller such as pressure controller and temperature

controller and safety system such as relief valve and drainage system were also installed to alert

the workers regarding the changes and disturbances in process flow. For example, we have

indicator and alarm for both low temperature and high temperature in our reactors to alert the

workers nearby if there is any sudden change in temperature and relatively proper mitigation

measures able to be taken quickly without any delay, since plant safety is the main concern for

an ethical engineer and for the public safety regarding to the production of anhydride product.

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2.4 Ethics in Design Project

There are always problems encountered as for any project in the world. We stumbled

into several humps on the road throughout the tenure of our entire plant design project. The

issues faced are discussed as in the following subsections with reference and representation of

the published Code of Ethics.

2.4.1 Teamwork and Time Constraints

Engineering bodies and firms will receive an intake of registry applications in the nearest

future. We were all assigned to be upcoming engineers with numerous tasks and assignments

that had to be submitted before the deadline had been exceeded. A sense of time and project

management is nurtured as we strive to perform such tasks within the time allocated for our

assignments and projects. In the real world, as time is money, these qualities are an important

practice. There was no violation of ethical codes throughout the duration of the assigned design

tasks as each member played an active role in the development of ideas and initiations of

solutions as well as in discussions and meetings.

As the Code of Ethics draws guidelines for conducting a chemical engineer and at all

times upholds one's professionalism, any issues faced or incurred must be resolved without side-

tracking from the ethical codes outlined. These solutions must also be carried out with the help

of adequate knowledge and technical skills in engineering. For each task, an average of 4 weeks

was spent. As such, it was vital that both time and project management skills were applied, and

their importance was emphasized to ensure that the tasks were performed within the specified

timeframe.

Statement (5) of the IEM Code of Ethics indicates that we, as future engineers, are

required to carry out the tasks assigned by the task leader in a professional manner and to uphold

74
our responsibility. Similar practice is mentioned in the API codes whereby we should carry out

all tasks in a professional manner. However, care must be taken when it comes to the ability

and competency to undertake a certain task or assignment. BEM's Code of Ethics means the

importance of undertaking a task only within one's ability and competency. A thorough

evaluation must be carried out from time to time in order to evaluate one's competency.

Statement (6) of IEM’s Code of Ethics suggests that an engineer should be able to

provide and assert an opinion within his expertise. Such an opinion must be reliable and highly

relevant to the participating active discussion. Although the Code of Ethics of both IEM and

BEM is more focused on self-development, as a chemical engineer-to-be, team work is

extremely crucial. Referring to AIChE's Code of Ethics, emphasis must be placed on fostering

an atmosphere of equity, diversity and inclusion through respect and fair treatment for colleagues

and colleagues. As a result, an exposure to the practical environment is served through the

current plant design project tasks, celebrating diversity and highlighting the form of teamwork.

Referring to Statement (5) of BEM’s Code of Ethics, a task must be performed in an

honourable, responsible, ethical and lawful manner that upholds the honour, reputation and

usefulness of the profession. While the current project for plant design does not involve real cash

flow, personal interests are a major roadblock in making decisions that come to the real world.

Strict notice must be reiterated to ensure that no decision should be made by personal interests.

Task leaders shall equally distribute all workload without taking into account any prior personal

preference and feelings.

With reference to the Code of Ethics of API, any personal relationships, activities, or

financial affairs should be avoided as it is possible to influence one's performance and cause

conflict of interest. All members are required to carry out the designated plant design task and

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must be able to maintain their professionalism in any discussion, problem solving, judgment and

decision making.

2.4.2 Constraint of Data and References

The most frequently encountered problem with our plant design was the lack of data and

resources available for calculations and justifications of design. Proper data research with

relevant and reliable references is essential for a design project to be reliable. Throughout the

tenure of our design projects, countless journals, books, publications and reference text books

have been studied with hopes of acquiring the necessary calculation resources and methods, as

well as providing a set of data for use in information analysis, comparisons and justifications.

Referring to Statement (6) of IEM’s Code of Ethics, all members of the design team should be

able to provide a relevant and reliable opinion on their professional ability. Applying this

statement to our team contributes to a successful and fruitful discussion on the path. That

statement was also relevant in the design project during the design phase of the equipment.

Because our manufacturing process required physical and chemical data for proper equipment

design, literatures were scouted abundantly and software such as ASPEN Plus was used for

proper data acquisition.

Brainstorming with the design team makes it possible to milk ideas and test whether that

milk is fresh or spoiled, meetings with the supervisor assigned help a lot. Our supervisor not

only monitors our progress, but also tests our proposed theories and corrects them to reaffirm

our project's proper continuity. The supervisor also eased the difficulty of our problems by

recommending solutions or offering a more comprehensive view of the problem from a different

perspective.

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Issues also arisen during the ASPEN Plus simulation required for the plant design

justification. Unfortunately, our proposed plant involves the use of switch condenser which is

not included in the ASPEN Plus equipment models. Thus, attempts were done to create a user-

defined equipment model in ASPEN Plus with combinations of other software for the

simulation. The attempt though, failed. However, it was beyond our understanding and

knowledge. This could lead to new areas of study in the future. Such a thing is in line with

Statement (3) of IEM’s Code of Ethics.

2.5 Case Study: Pasir Gudang chemical spill [16, 17, 18]

Recently, the Malaysian government has identified the chemical waste that was illegally

dumped into a river in Johor Baru on Thursday (March 7). Two directors of a used tyre

processing company were charged to 15 charges each, over their alleged involvement in the

Pasir Gudang chemical pollution case. Their company, P Tech Resources, was also slapped with

15 charges at the Sessions Court in the Malaysian state of Johor. Singaporean Wang Jin Chao,

34, and Malaysian Yap Yoke Liang, 36, are accused of failing to notify the authorities about the

generation of scheduled wastes within 30 days. They are also accused of failing to conduct

periodic air quality monitoring and maintain records for manufacturing processes. The illegal

dumping of chemical waste in Pasir Gudang's Sungai Kim Kim caused a wave of poisoning

cases that affected over 2,770 people. All 111 schools in the city were ordered to shut down as

a massive clean - up operation was started by the authorities. In order to determine the

concentration and movement of harmful gases, an expert on atmospheric science and climate

change urged the authorities to continuously monitor the air in not only Pasir Gudang but also

other nearby areas.

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Dr Mohd Shahrul Mohd Nadzir, a senior lecturer at the Faculty of Science and

Technology at Universiti Kebangsaan Malaysia, said that emitting more gases from the

chemicals dumped into river was not impossible. The eight chemicals, identified from water

samples taken from Sungai Kim Kim, are methane, hydrogen chloride, acrylonitrile, acrolein,

benzene, toulena, xylene and limonene. Explaining that the adverse effects of any pollutant are

influenced by its atmospheric lifespan, he said: "A gas such as methane with a longer lifespan

will have no effect on humans as long as its concentration in the air is below the level specified

by NIOSH (National Institute for Occupational Safety and Health), i.e. 1,000 ppm (parts per

million; exposure to methane over a period of eight hours). On the other hand, acrylonitrile may

have an atmospheric lifespan of only 18 hours, but it has carcinogenic effects, he warned, adding

that high concentrations of this substance in the air may pose a danger to humans. The current

hot weather makes the situation more challenging as it caused the chemicals to evaporate easily

and react with other substances in the air, leading to higher concentrations of the substances

created through these chemical reactions. Meanwhile, the wind direction is also crucial because

it dictates gas movement to other areas. People living in the affected areas are advised to wear a

proper mask, for example, the 3M 7502 Respirator 6001, that can filter the gases permeating in

the air and not to remain outdoors for too long.

Referring to the IEM Code of Ethics as stated in Statement (1) “A member shall at all

times take care to ensure that his work and the products of his work constitute no avoidable

danger of death or injury or ill health to any person. This is referring to the person in charge who

should take responsibility to notify the authorities about the generation of scheduled wastes

within 30 days and to conduct periodic air quality monitoring and maintain records

for manufacturing processes. It is essential to establish a planning to anticipate the long term

problem of the waste generation. If a problem occurs, spillage of chemicals or wastes into a river

78
are not the solution. In Statement (5) IEM’s Code of Ethics, it is read that “A member shall

accept personal responsibility for all work done by him or under his supervision or direction,

and shall take all reasonable steps to ensure that persons working under his authority are

competent to carry out the tasks assigned to them and that they accept personal responsibility

for work done under the authority delegated to the”. Similarly, in this case, the employees whom

are responsible for conducting periodic air quality monitoring and maintaining records

for manufacturing processes, should have been well aware of the problem, the risks and long

term effects of their solution. As the fault of the incident was identified, the personnel involved

should step up and claim responsible for their actions. The above codes have not been followed

and a catastrophic incident has followed. It could have prevented the incident if the engineers

could predict the long - term effects of dumping the wastes and chemicals into the river. The

best solution is to send the chemical and wastes to chemical waste treatment as hazardous

waste can be treated by chemical, thermal, biological, and physical methods. Finally, the

employees do not have to choose between safety and production as safety comes first.

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CHAPTER 3: PLANT RISK ASSESSMENT ANALYSIS

3.1 Lists of Hazardous Substances

The following table summarized the hazardous chemicals involved in our Phthalic Anhydride production plant.

Chemical and Physical Properties

Compound Mw Colour and Specific Toxic Properties Flammability Properties


Tm (oC) Tb (oC)
(kg/kmol) Phase Gravity

Phthalic  Irritating to the eyes,  It must be preheated


Anhydride respiratory system and human before ignition can occur.
skin.  React slowly with water
Colourless,
 Causing lower blood pressure. to form heat.
Clear to
148.10 1.20 131 295  Could decreased body weight  Vapor may form
amber, heavy,
and causing kidney explosive mixtures with
liquid
lymphocytosis. air.
 React violently with CuO
at elevated temperatures.

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Maleic 98.06 Colourless, 1.48 52.8 202  Irritating to the eyes, skin and  Heated above 300 oF in
Anhydride flakes, pallets, mucous membranes. the presence of various
molten  Substance can be absorbed materials may generate
into the body by inhalation. heat and CO2.
 Irritating to the nose and upper  Flammable in molten and
respiratory system such as vapor state.
conjunctivitis and  Dust cloud may be
photophobia. exploded by spark
Carbon 28.01 Odorless, 1.25 205 191  Inhalation causes central  May causing explosion in
Monoxide tasteless, nervous system damage and fire.
poisonous, asphyxiation.  Fire ignited by heat or
gaseous  Prolonged exposure to CO sparks.
may be fatal.
 Causing headache, tachypnea,
nausea, lassitude, dizziness,
confusion, hallucinations,
angina and syncope.

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 Causing death or
cardiovascular problem.
Carbon 44.01 Colourless, 1.21 -56.6 -78.5  Causing problem to  May be exploded when
Dioxide odorless and reproductive system and heated.
incombustible cardiovascular system.  Non-flammable gases.
gas  Causing headache, dizziness,  Non-Combustible gases.
restlessness, paresthesia,  Exploded when passes
dyspnea, sweating, malaise, over a mixture of
increase heart rate, cardiac powdered aluminum and
output, blood pressure and sodium peroxide.
coma.

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3.2 List of Equipment Handling High Inventory of Hazardous Substances

Remark: Only the reactor and mass transfer equipment handling the listed hazardous chemicals

at high inventory will be listed in this section.

Equipment Major Hazardous Operating Condition

Chemical Pressure (bar) Temperature (C)

Multi-Tubular Phthalic Anhydride 2.55 300

Reactor Maleic anhydride

(R-01) Oxylene

Carbon dioxide

Carbon monoxide

Switch Condenser Phthalic Anhydride 1.10 110

(SC-01) Maleic anhydride

Oxylene

Carbon dioxide

Carbon monoxide

Distillation Column Phthalic Anhydride 1.01 230

(T-01) Maleic Anhydride

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3.3 Possible Hazard Derived Identification and Risk Evaluation

Major hazards and the respective consequences are identified as coupled with possibility

and severity which lead to risk evaluation for level of acceptability.

3.3.1 Hazards Possibility, Consequences Analysis

The following possibility and consequence analysis are being done by identifying the

potential major hazards from each equipment within the production plant. The

categorization of the possibility and severity of the hazard has also been done included in

the following table:

Table 12: Hazard Possibility

Possibility Description

Level A Frequent • Likely to occur frequently

Level B Probable • Will occur several times in life of production

Level C Occasional • Likely to occur sometime in life of production

Level D Remote • Unlikely, but possible to occur in life of production

Level E Improbable • Unlikely, assume no occurrence

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Table 13: Hazard severity

Severity Description

• Death
Class I Catastrophic
• Loss of System

• Severe injury or morbidity

Class II Critical • Major damage to the system

• Major loss of production

• Minor injury or morbidity

Class III Marginal • Minor damage to the system

• Minor loss of production

• No injury or morbidity
Class IV Negligible
• No damage to the system

3.3.2 Risk Evaluation Classification

All the identified risk and its consequences have been assessed and evaluated. The

level of acceptance of each hazard has been discussed and outlined based on the

managerial review following the guidelines in the table below.

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Table 14: Risk assessment criteria

Frequency Severity
Catastrophi Critical (II) Marginal Negligible
c (I) (III) (IV)
Frequent 1A 2A 3A 4A

Probable 1B 2B 3B 4B

Occasional 1C 2C 3C 4C

Remote 1D 2D 3D 4D

Improbable 1E 2E 3E 4E

Table 15: Suggested Criteria

Risk Color Code Criteria


1A, 1B, 1C, 2A, 2B, 3A Unacceptable.
1D, 2C, 2D, 3B, 3C Undesirable (Management decision required).
1E, 2E, 3E, 4A, 4B Acceptable with review by management.
4C, 4D, 4E Acceptable without review.

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3.3.3 Classified Hazard Identification and Risk Evaluations

The following table classified hazard identification and risk evaluations involved in our Phthalic Anhydride production plant.

Equipment Major Possible Consequence Possibility Severity Level of Justifications /

hazardous hazard(s) Acceptance Safety Features

Chemical

Multi- C8H4O3 Overpressure Rupture of reactor Improbable Catastrophic 1E Equipped with pressure

Tubular C4H2O3 system (E) (I) relief system, proper

Reactor C8H10 Explosion due to high Remote Catastrophic 1D mechanical design.

R-01 CO2 pressure buildup of the (D) (I)

CO gases in the

anaerobic digester

Reactor leakage Fire and explosion could Remote Catastrophic 1D Require ignition source

occur due to biogas (D) (I) while plant area has

leakage. tight control on

ignition source tight

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control.

Emission of gases (CO, Improbable Marginal 3E Dilution of leaked

CO2) that might cause (E) (III) gas as plant area is

vision blurring, and etc.) open area.

Piping Leakage Fire and explosion could Occasional Catastrophic 1C Require ignition source

occur due to biogas (C) (I) while plant area has

leakage. tight control on

ignition source tight

control.

Switch
S C8H4O3 Overpressure The vessel might rupture Occasional (C) Catastrophic (1) 1C  Equipped with

Condenser C4H2O3 system due to the excess pressure pressure relief system,

SC-01 C8H10 developed inside the vessel. and proper mechanical

CO2 This can cause fire and design.

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CO explosion to occur due to

presence of PA and MA
 Temperature control
which a flammable
system also has been
chemical.
installed to maintain

the operating

temperature. Rapid

rise in temperature

also can cause

overpressure.

 The plant area has

tight control on

ignition source

89
Piping Leakage Fire and explosion could Occasional Catastrophic 1C The plant area has tight

occur due to PA and MA (C) (I) control on ignition

leakage. source.

Loss of cooling Release of volatile Remote (D) Critical (II) 2D Level indicators are

media in substances from column that installed in cooling

condenser are flammable and/or toxic. media to make sure

enough cooling media


Reaction occur with impurity
are available for
or other substances present
distillation process.
in connecting units

Distillation Phthalic Overpressure The vessel might rupture Occasional (C) Catastrophic (1) 1C  Equipped with

Column Anhydride system due to the excess pressure pressure relief system,

T-01 (PA) developed inside the vessel. and proper mechanical

Maleic This can cause fire and design.

90
Anhydride explosion to occur due to  Temperature control

(MA) presence of PA and MA system can be installed

which a flammable to maintain the

chemical. operating temperature.

Rapid rise in

temperature also can

cause overpressure.

 The plant area should

have tight control on

ignition source.

Piping leakage Fire and explosion could Occasional (C) Catastrophic (I) 1C  The plant area should

occur due to presence of PA have tight control on

and MA. ignition source

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 Requires maintenance

often.

 Leakage may occur

due to presence of PA

and MA which can

corrode the pipelines

over the years.

Column leakage Fire and explosion due to the Remote (D) Marginal (III) 3D

exposure of flammable gases  Installing leak

detectors can help

fasten the maintenance

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phase before it become

more serious.

 Dilution of leaked gas

as plant area is open

area.

Loss of cooling Release of volatile Remote (D) Critical (II) 2D  Level indicators are

media in substances from column that installed in cooling

condenser are flammable and/or toxic. media to make sure

enough cooling media


Reaction occur with impurity
are available for
or other substances present
distillation process.
in connecting units

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3.4 Possible Hazards and Risk Analysis
3.4.1 MSExcel Hazard Analysis
Downwind Concentration
Chemical: O-Xylene
Input Data
Rate Release 117.180kg/s
Wind Velocity 2m/s
Air Density 1205 g/m3
Molecular Weight 106 g/mol
Atmospheric Stability Day
Release Elevation 0.5m
Initial Concentration 100%
Release Type Continuous
Material Buoyancy Neutral
Ground Type Urban
Ground Level Concentration
High level hazard 900 ppm / 3964 mg/m3
Calculated Downwind Distance
High level hazard 457m / 499.88 yard

Chemical: Carbon Dioxide


Input Data
Rate Release 3813.34 kg/s
Wind Velocity 2 m/s
Air Density 1205 g/m3
Molecular Weight 44 g/mol
Atmospheric Stability Day
Release Elevation 0.5m
Initial Concentration 100%
Release Type Continuous
Material Buoyancy Neutral
Ground Type Urban
Ground Level Concentration
High Level Hazard 40000ppm / 73131mg/m3
Calculated Downwind Distance
High Level Hazard 647 m / 707.95 yard

Chemical: Carbon Monoxide


Input Data
Rate Release 606.67 kg/s
Wind Velocity 2m/s
Air Density 1205 g/m3

94
Molecular Weight 28g/mol
Atmospheric Stability Day
Release Elevation 0.5m
Initial Concentration 100%
Release Type Continuous
Material Buoyancy Neutral
Ground Type Urban
Ground Level Concentration
High Level Hazard 330 ppm / 384 mg/m3
Middle Level Hazard 83 ppm / 97 mg/m3
Calculated Downwind Distance
High Level Hazard 5944 m / 3.69 miles
Middle Level Hazard 14580 m / 9.06 miles

3.4.2 ALOHA Incident Analysis


The purging stream from switch condenser, SC-01 in Phthalic Anhydride plant are consists of

O-xylene, Carbon Dioxide and Carbo Monoxide. Since, they are being released to the

atmosphere without any pre-treatment, it might cause environmental and human health issue.

The exposure routes to the human body are mainly through inhalation, skin as well as eye

contact.

Therefore, the hazardous analysis for switch condenser, SC-01 is important to be carried out

for the sake of environment as well as human being. The following are steps involved to deal

with emergencies involving direct source using ALOHA software. The steps are as shown

below:

95
Step 1: Define location in ALOHA by using geographic coordinates of Gebeng, Pahang

[19, 20]

Step 2: Select Gebeng, Pahang, Malaysia as location.

96
Step 3: The pure chemical is defined as O-xylene.

97
Step 4: Fulfilled the atmospheric requirement from the data at 6.00 pm, Tuesday [21]

Step 5: The source choice is direct source, the amount of pollutant entering the

atmosphere is obtain from the previous mass balance.

98
Step 6: The last step where the threat zone is display and give result.

99
Result Summary:

100
From the result, it shows that Aloha Incident Analyst has performed the calculation to

determine the safety distances at specified range. Threat zone has been truncated at distance

almost 1000 yards limit. The IDLH limit represents the concentration of a chemical in the air

to which healthy adult workers could be exposed (if their respirators fail) without suffering

permanent or escape-impairing health effects [22]. Only a single threat zone is available

because there is only one IDLH value per chemical. At red zone, the exposure concentration is

900 ppm (IDLH) at distance range 986 yards from SC-01. In this zone, general population

including susceptible individuals could experience life-threatening health effects or even more

severe, death.

101
Carbon dioxide

From the result, it shows that Aloha Incident Analyst has performed the calculation to

determine the safety distances at specified range. Threat zone has been truncated at distance

102
greater than 1000 yards limit. The IDLH limit represents the concentration of a chemical in the

air to which healthy adult workers could be exposed (if their respirators fail) without suffering

permanent or escape-impairing health effects [23]. At red zone, the exposure concentration is

40000 ppm (IDLH) at distance range 1038 yards from SC-01. In this zone, general population

including susceptible individuals could experience life-threatening health effects or even more

severe, death.

Carbon monoxide

103
From the result, it shows that Aloha Incident Analyst has performed the calculation to

determine the safety distances at specified range. Threat zone has been truncated at distance of

6 miles limit. AEGLs estimate the concentrations at which sensitive individuals such as old,

104
sick, or very young people where will begin to experience health effects if they are exposed to

a hazardous chemical for a specific length of time (duration). For a given exposure duration, a

chemical may have up to three AEGLs values, each of which corresponds to a specific tier of

health effects. The AEGLs are divided into 3 stages as shows in next figure.

In Aloha, the AEGL-1, AEGL-2, and AEGL-3 values to generate a threat zone estimate where

yellow, orange, and red zones indicate areas where those values were predicted to be exceeded

at some point after the chemical release began. At red zone, the exposure concentration is

greater than 330 ppm (AEGL-3) at distance range 4.6 miles from SC-01. In this zone, general

population including susceptible individuals could experience life-threatening health effects or

even more severe, death. For orange zone, the concentration is greater than 83 ppm (AEGL-2)

at distance range of greater than 6 miles from SC-01. The general population in this zone are

susceptible in experiencing irreversible or other serious long-lasting adverse health effects or

an impaired ability to escape. Lastly, at yellow zone, the concentration is undefined and no

105
recommendation for the distance range from SC-01. The general population in this zone are

susceptible in experiencing notable discomfort, irritation, or certain asymptomatic non-sensory

effects which varies for everyone. However, the effects are not disabling and are transient and

reversible upon cessation of exposure [23].

3.4.3 Comparison between MSExcel calculation and ALOHA software

Summary of hazard analysis results for O-Xylene, Carbon Dioxide and Carbon Monoxide

downwind concentration.

Chemical: O-Xylene
Risk Level ALOHA Excel Deviation (%)
High 186 yards 499.88 yards 62.79

Chemical: Carbon Dioxide


Risk Level ALOHA Excel Deviation (%)
High 1038 yards 707.95 yards -46.62

Chemical: Carbon Monoxide


Risk Level ALOHA Excel Deviation (%)
High 4.6 miles 3.69 miles -24.66
Middle 6miles 9.06 miles 33.77

Downwind concentration of O-xylene, Carbon Dioxide and Carbon Monoxide hazard is

analysed by using manual calculation and ALOHA software as we want to know the hazard

threat upon on these chemicals that the plant purged from the switch condenser. The deviation

between the hazard analysis between Excel and ALOHA as shown in tables above. However,

the result shown for all risk level for both analysis methods are quite large in gap. Excel is

chosen as a reference due the ALOHA software have limitation in estimation the distance

above a certain distance range and the hazard analysis from Excel shows more conventional

result which can be consider as the worst-case condition.

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3.5 Mitigations and Strategy Recommendations

The table below shows the mitigation strategy proposed for each hazard [24].

Hazard Prevention and Mitigation Strategies

Fire 1. Water supplies

 A big water tank should be installed in the plant as a backup in

case any fire accident happens.

 Fire hydrants should be installed at section where flammable

material located.

2. Smoke/fire detectors and fire extinguishers

 Smoke detectors are installed on top of equipment and fire

extinguishers are installed at areas where equipment is located.

 This equipment should be tested and/or inspected regularly

 Training to workers/operators are taught on how to use a fire

extinguisher by safety department.

 Workers are not allowed to smoke around plant area.

3. Fire drill training

 Fire drill should be frequently practice involve all workers

includes top management. In this case, emergency evacuation

route should be taught to the workers.

 Every worker must know the location and right path to assemble

so that they can gather at that assembly point immediately if any

accident occurs.

4. Firewalls and fire doors

107
 A fire door is a door with a fire-resistance rating used as part of a

passive fire protection system to reduce the spread of fire or

smoke between compartments.

 Fire doors can be installed at chemical storage room. In case any

fire occurs in the room, the other part of the building can still be

protected.

5. Cleanup activities

 Cleanup activities should be done periodically in areas of

abandoned or collapsed structures, accumulated junk or debris,

and in areas that store flammable materials.

 Training to workers to handling flammable and explosive

materials

6. Education and awareness

 Workers should be educated on proper evacuation procedures,

such as wearing protective clothing (e.g., sturdy shoes, cotton or

woolen clothing, long pants, a long-sleeved shirt, gloves and a

handkerchief to protect the face); and choosing a route away

from fire hazards.

 Educate workers to differentiate between different type of fire

extinguishers.

Explosion 1. Explosion relief

 Safety device used to protect equipment or building against

excessive internal, explosion incurred pressure.

internal, explosion incurred pressure.

108
2. Inerting

 This technique prevents an explosive atmosphere developing in

the event of a leak through the addition of inert gas. By addition

of inert gas, the oxygen concentration is reduced below a certain

level, called the limiting oxygen concentration (LOC) thereby

preventing explosion. Inert gas should be spray in the chemical

storage room

3. Water deluge

 Water deluge can significantly reduce the explosion pressure

generated by a gas explosion. It has to be activated on gas

detection, rather than on detection of the start of the explosion,

and the gas velocities generated by the explosion have to be high

enough to break up the water droplets from the sprinklers into a

fine mist

4. Explosion Barriers

 Reduce the consequences of an explosion in a system by

confining it to just part of the system and thus preventing it

propagating throughout the entire system

 Applied to pipes and ducts or for a system comprising of two or

more interconnected vessels

Utility 1. Backup power

failure  Generators can be used for backup power at critical facilities for

example pump.

2. Lightning protection

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 Electrical and communications systems should be protected from

lightning strikes.

3. Trees Trimming

 Tree trimming is important to prevent electrical transmission lines

breakage. Besides. Tree trunks may fall down during raining

season or when there is strong winds, causing casualty to the

workers. Tree leaves will plug water drainage system.

Toxic 1. Control equipment

release  The gas leaked can be directed to chemical scrubbers for

treatment.

 Install a restricting orifice in a pipeline to restrict the flowrate if a

control valve should fail.

2. Double containment

 Double wall storage tanks or double co-axial distribution lines and

raceways can be used as an important measure against leaks of

toxic gases into occupational space

3. Personal Protective Equipment (PPEs)

 PPEs should be provided for the workers who work near equipment

that has probability of toxic release.

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3.6 Plant Start-Up and Shut-Down Sequence

The start-up and shut-down procedure of major units which include the Multi-Tabular Reactor

(R-01) and Distillation Column (T-01) are discussed in this chapter.

3.6.1 Start Up and Shut Down Procedure for Reactor, (R-01)

Standard Operating Procedure (SOP) Document No.: SOP-EKC453-01

Start-Up and Shut-Down Procedure of Effective Date: 1st April 2019

Multi-Tubular Reactor (R-01)

Prepared By: Muhd Shafizruddin Reviewed/Approved By: Nurul Atikah

GENERAL

Multi-Tubular Reactor is used to produce Phthalic Anhydride and Maleic Anhydride via

reaction between liquid O-Xylene and Air. The reactor unit operates at 2.55 bar and 300oC.

This reaction is crucial to obtain a good quality binder for the production. Salt water bath is

circulated at the shell side of the reactor to continuously remove the heat generated through

the reaction.

1.0 SAFETY

1.1 Continuous supply of salt water into the shell side to efficiently operate reactor

at optimum condition.

1.2 Material safety Data Sheet (MSDS) and Standard Operation Pressure (SOP)

should be updated and ready to be reached by authorized personnel.

1.3 Do not carry out any fire inducing activities near the reactor unit.

1.4 All personnel in the plant shall wear personal protective equipment (PPE) as

required by site policies or regulations and NIOSH.

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2.0 PRE-START UP CHECK

2.1 Ensure all the valves in the system are closed

2.2 Ensure there is no blockages and leakages in the pipeline system

2.3 Check the sensors as well as the alarm completely and make sure it is functioning

properly

2.4 Ensure the pressure testing, mechanical integrity testing and operational testing

are completed and acceptable.

2.5 Ensure the raw material storage tanks are filled, up to the desired level prior to

the reactor start-up

2.6 Ensure salt water supply is available with safety allowance considered

2.7 Ensure the chiller unit is functioning properly

3.0 START-UP

3.1 Make sure the drainage valves and by-pass valves are completely closed

3.2 Open the gate valve for salt water supply system and ensure the salt water at the

shell side reached a steady state.

3.3 Turn on the control system

3.3.1 Set all the control loops into manual mode

3.3.2 Set the desired set point value for controller TIC and FIC and then

switch the controllers to auto mode.

3.4 Open the feed valves to let the feed enter the pipe reactor

3.5 Control the feed flow rate of feed and salt water supply by monitoring with the

use of controller

3.6 Make sure the pressure regular indicator is maintained at 1 bar

3.7 Heat the reactor up to 50oC, then allow the system to reach steady state

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3.8 Allow rise of temperature of reactor to normal operating temperature. Control

system is used to monitor reactor temperature

3.9 Allow the system to reach steady state by checking on the flow, temperature and

pressure with the aid of the alarm

3.10 Allow automatic run of process with the help of the installed control system

4.0 SHUT-DOWN

4.1 Switch the control system to manual mode

4.2 Allow the system to cool down with the continuous supply of salt water

4.3 Once the system is cooled, open the gate valve to remove all the remaining

process fluid from the pipelines

4.4 Drain out all the process fluid left inside the reactor via the drainage valve. Care

should be taken during the removal of hazardous process fluid

4.5 Stop the salt water flow by fully closing gate valve

4.6 Ensure all the valves are closed before isolate the system. Purge all the vessel and

piping with inert nitrogen as cleaning steps.

5.0 EMERGENCY SHUT DOWN

5.1 The emergency shut down button should be pressed when the temperature of the

reactor reached above 84 oC and system get highly pressurized

5.2 Follow the emergency response plan as stated in Risk Management Plan (RMP)

5.3 Switch the control system to manual mode

5.4 Supply large amount of salt water to cool the reactor

5.5 Drain out all process fluid inside the reactor by opening drainage valve

5.6 Immediately inform all operators about the emergency

5.7 Evacuate the plant immediately

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3.6.2 Start Up and Shut Down Procedure for Distillation Column, (T-01)

Standard Operating Procedure (SOP) Document No.: SOP-EKC453-01


Start-Up and Shut-Down Procedure of Effective Date: 1st April 2019
Distillation Column (T-01)

Prepared By: Muhd Shafizruddin Reviewed/Approved By: Nurul Atikah

GENERAL
Distillation unit is used to separate top product and bottom product which is Maleic
Anhydride as the top product and Phthalic Anhydride as the bottom product. Only one
distillation unit is utilized in our plant. Thus, the operating condition of this unit is at 283.8oC
and 1 bar.
1.0 SAFETY
1.1 Material safety Data Sheet (MSDS) and Standard Operation Pressure (SOP)
should be updated and ready to be reached by authorized personnel.
1.2 Do not carry out any fire inducing activities near the distillation unit.
1.3 All personnel in the plant shall wear personal protective equipment (PPE) as
required by site policies or regulations and NIOSH.
2.0 PRE-START UP CHECK
2.1 Ensure all the valves in the system are closed
2.2 Ensure there is no blockages and leakages in the pipeline system
2.3 Check the sensors as well as the alarm completely and make sure it is functioning
properly
2.4 Ensure the pressure testing, mechanical integrity testing and operational testing
are completed and acceptable.
2.5 Ensure the raw material storage tanks are filled, up to the desired level prior to
the distillation unit start-up
2.6 Ensure continuous cool water supply is available with safety allowance
considered.
2.7 Ensure that emergency shutdown procedures were reviewed by the workers.

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3.0 START-UP
3.1 The column should be in total reflux at steady state with the initial valve setting
of Feed:0, Distillate: 0 and Bottoms:0.
3.2 Close all open valves.
3.3 Purge column with inert (Nitrogen) to the atmosphere through open valves. It is
used to pressuring up the system and then de-pressuring it. It is repeated several
times to get the air out.
3.4 Pressure up the system with inert again to check the leakage.
3.5 Open vent to the flare system to de-pressure the inert.
3.6 Allow the column to build pressure to near its normal operating pressure.
3.7 Make sure the condenser on the column is lined up to begin condensing liquid.
3.8 Once liquid has built in overhead accumulation drum above the minimum
operating level, turn on your reflux pump and reflux drum.
3.9 Put the distillation column on total reflux to begin building a level in the bottom
of the column.
3.10 Put heat on the reboiler once the level builds in the bottom to begin boil up
on the column.
3.11 Begin pumping out the overhead product and bottom product to keep the
system in mass balance and prevent the tower from flooding.
3.12 Open the inlet valve and wait until steady state is reached.
4.0 SHUT-DOWN
4.1 Turn the Reboiler Heater Control knob to zero.
4.2 Turn off the pumps.
4.3 Turn off the valve when the temperature of the distillate is below the boiling point
of the light component of the mixture.
4.4 Drain out all the process fluid left inside the column via the drainage valve.
Care should be taken during the removal of hazardous process fluid.
4.5 Ensure all the valves are closed before isolate the system. Purge all the vessel
and piping with inert nitrogen as cleaning steps.

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5.0 EMERGENCY SHUT DOWN
5.1 The emergency shut down button should be pressed when the temperature of the
distillation column reached above 84 oC and system get highly pressurized
5.2 Follow the emergency response plan as stated in Risk Management Plan (RMP)
5.3 Switch the control system to manual mode
5.4 Drain out all process fluid inside the column by opening drainage valve
5.5 Immediately inform all operators about the emergency
5.6 Evacuate the plant immediately

3.6.3 Justification of Plant Start-Up and Shut-Down Procedures

The plant start-up and shutdown procedures are truly vital for the efficient operation of the

plant without any considerable accidents and problem in anhydride production. Shutdown

method is one of the crucial part to ensure continuous operation of the plant in the upcoming

years. During the shutdown session, the maintenance works will be carried out and mechanical

equipment will be completely checked for any leakages and operation failure. Other than that,

proper plant start-up procedure allows the plant to operate in safe manner and will also able to

reduce the accidents especially in reactor unit. Thus, a proper and well-managed start-up and

shutdown sequences should be developed and followed by everyone for the safe plant

operation. Relatively, the following section mainly emphasizes regarding the factors in

designing the SOP for plant start-up and shut down.

As shown below, pre-check list covers the ultimate criteria to be focused on before proceeding

with the plant start-up and shutdown procedure. Commissioning Procedures as indicated in the

table below document a logical progression of steps necessary to verify that installed plant is

fully functional and fit for purpose. A general sequence of steps in commissioning may

typically include:

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Table 16: Commissioning Procedures

Criteria Description

System Configuration Check To trace all pipework and connections to verify the system

configuration and to ensure the plant is safe to be operated.

Instrumentation System Check To ensure that all instrumentation, alarm settings,

microprocessor signals and hardwire trips pertaining to the

installation are functional

Flushing and Cleaning of Lines To clean all items of pipework and the vessels that make up

and vessels with Water the installation.

Assessment of Auxiliary To verify the performance of all auxiliary equipment. This may

Equipment include pumps, fans, heat exchanges, condensers and etc.

Calibration of Vessels and To check the calibration and performance of all vessels and

Instrumentation instrumentation pertaining to the installation.

Start-Up Protocol To provide guidance for bringing the installation online

starting from an empty non-operational system.

Shut-Down Protocol To provide guidance for taking the installation offline starting

from a fully operational system.

Chemical Trials To verify the performance of the installation by simulating

‘live’ conditions by following standard procedures.

Raw Material Availability To ensure all the raw material are sufficient and at hand.

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 General Plant Start-Up Procedure

1. Ensure all valves in the system are closed.

2. Ensure the pressure relief vent line is securely connected to pressure relief valve and is

terminated properly.

3. Ensure the utility supplies are available.

4. Ensure the seal oil of all machineries is in normal level.

5. Ensure the vent and drain valves are closed.

6. Ensure all the pressure gauge isolation valves are slightly open while level isolation

valve.

7. Ensure the pressure testing, mechanical integrity testing and operational testing are

completed and acceptable.

8. Ensure that the piping, tower and vessel are cleaned and undesired fluid is purged out.

 General Plant Shut-Down Procedure

1. Ensure all the process stream inlet valves in the system are closed.

2. Allow the cooling down of the system.

3. Depressurize the system and drain out of liquid.

4. Ensure the vent and drain valves are closed.

5. Terminate the utility supplies.

6. Purge and clean the piping, tower and vessel prior isolation.

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3.6.4 Comparison with Industry on SOP Preparation
SOP for distillation column is available due to private and confidential issues, but it is

not clearly shown. Most of the equipment's SOP is not publicly disclosed and reserved for

copyright. It is however good to note that the procedures instruction is in a similar and arranged

format with the setting of the SOP and alarm system as prepared. By comparison, the

arrangement of the sequences is based on consideration of safety, properties of the equipment

and requirements of the process. The Armfield Inc.'s SOP document is attached as follows.

SOP of Distillation Column

119
120
Figure 14: SOP for Industrial Distillation Column

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3.7 Plant Emergency Shutdown

Shutdown is a complex process and is more than just switching off. Emergency

Shutdown is an event that, due to certain circumstances, could not be neglected by any chemical

plant with the following objectives:

1. To ensure the process in safe condition.

2. To avoid equipment damage.

3. To minimize hazardous chemical release.

4. To protect equipment when there is unexpected severe phenomenon.

The emergency shutdown will be initialized by situations such as:

 An electric power failure which stops the control process of the plant;

 Faults or damages in the mechanical equipment such as pumps, compressor,

motors etc.;

 Reflux Drum overflow;

 Flooding and Weeping of distillation column;

 Hazard identified alarm;

 Leakage and clogged connecting pipelines.

Safety counter measures that will be executed during such accidents occur:

1. Adhere to the Emergency Response Plan as informed in Risk Management Plan

(RMP);

2. Shut off feed supply to the equipment;

3. Shut off utility supply unless it is for room temperature cooling purpose such as

cooling water;

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4. Switch off auxiliaries related to the equipment such as pumps and compressors;

5. Shut off outlets of the equipment;

6. Isolate affected sections by shut off isolation valve; and

7. Alert the operators and evacuate from the emergency site instantly;

8. Plant can be tripped by the trigger of the alarm. Follow the normal shut down

sequence for emergency shutdown of each equipment.

Remark: The system must be return to normal operating condition as soon as possible after

emergency procedures are followed.

3.8 Alarm System for Major Unit Operations

Industrial alarm systems are very critical for the efficient and safe operation and control

of plants. Alarms are used to inform the operator about possible process deviations from the

normal so that the operator can take appropriate corrective action. From figure below, there are

multiple layers of protection to be conducted in a plant production line to prevent any undesired

incident from occurring as well as implementation of mitigations once the accidents occurred.

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Figure 15: Protection Layer of Process

Alarm system also have other several functions such as aid in monitoring the operating

process to be at optimal conditions for maximize the plant production and capable to warn as

well as to notify the operators immediately once the process runs out from the desired

operational range. A well-functioned and suitable alarm system plays crucial role in ease up

process production and allow the working plant to be in safe zone as they will be triggered once

the process is abnormal.

Detect, Diagnose and Respond are three phases that involved from operators to reactor

to alarm trips. These phases should be fully understood and taken into consideration during the

designing of alarm trip system. For detect phase, operators must make sure that all alarms are

not been left out. Each operator should be assigned with minimum number of alarms to allow

the alarm performance to be optimize. Elimination of “nuisance” alarm is allowed according

to proper safety consideration. This can allow the operators to take care of higher priority alarm.

The misinterpretation of alarm alert should be avoided at all cost during diagnose phase. The

information for causes and corrective action should be easily access by the operators through

124
safety documents such as HAZOP, ETA and PHA. Operator can response and compensate the

consequences of the possible causes after the detection of any faulty has been alerted by alarm

system. Every incident can be documented in Alarm Response Procedures for future reference

to allow faster action will be taken.

A suitable alarm system can be designed for the proposed production plant by

considering the three phases. There are commonly four types of alarm installed for each alarm

system which are low low alarm, low alarm, high alarm and high high alarm. High high alarm

and low low alarm will respond when the measured parameter reaches ±10% of the required

level. Whereas, high alarm and low alarm will only be alerted when the measured parameter

reaches ±5% of the required level.

3.8.1 Temperature Alarm

The safety margin for temperature allowance is set to ±15% from the set point

temperature. The high and low temperature alarms will be triggered once the measurement

exceeds +10% and -10% from the operating temperature respectively. The operators will

conduct the troubleshooting step when the alarms are triggered, and the emergency shutdown

steps will be activated if the measurement reach ±15%.

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3.8.2 Pressure alarm

The safety margin for pressure allowance is similar to temperature alarm system as it

is set up to ±15% from the set point pressure. High pressure alarms were installed to alert the

operators when the pressure exceeds the +10% margins and low-pressure alarms will blare

when the pressure indicates -10% in which the operator should proceed to carry out the

troubleshooting steps. Upon constant monitoring, if the reading reach ±15%, the emergency

shutdown steps will occur.

3.8.3 Level Alarm

The safety margin for level allowance is set to ±10% from the level set point but it is

relatively small as compared to pressure and temperature due to the limitation of the tank height

designed. The high and low temperature alarms will be triggered once the reading exceeds +5%

and -5% from the operating temperature respectively. The operators will proceed toward

troubleshooting steps when the alarms are triggered, and the emergency shutdown steps will

be activated if the reading reach ±10%.

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3.8.4 Alarm System for Multi-Tubular Reactor, R-01

A. Temperature Alarm System

The temperature alarm systems connected to the multi-tubular reactor (R-01) is

important to alert the operating personnel about the abnormal or deviation occur in the reactor

of the plant.

Low temperature is not desired as it leads to deviation in reactor conversion and slow

down the reaction rate. High temperature is not favourable because it will lead to deviation in

reactor conversion and might triggers high explosion risk by runaway reaction of the oxidation

of O-Xylene due to its process is highly exothermic. There are four types of alarm been

installed, low low alarm, low alarm, high alarm and high high alarm. High alarm and low

alarm are triggered when the reactor temperature reaches ± 5℃ of the reactor operating

temperature. High high alarm and low low alarm is triggered when the reactor temperature

reaches ± 10℃ of the reactor operating temperature. High high alarm is used to trigger the

emergency shutdown system. The reason why there are no installation of pressure and flow

alarm systems because the feedback system of the temperature control loop will control the

flow rate of process fluid and the build-up of pressure is related in rising of temperature of

rector. So, when the temperature alarm trigged, it will inform the operator on the abnormality

occurs on the temperature of the reactor as well as the pressure.

Table 17: Trigger values for reactor alarm systems

Alarm Operating Trigger values for various alarm

System Condition Low High Low Low High High

Temperature 300℃ 285℃ 315℃ 270℃ 330℃

127
Table 18: Corrective actions after triggering reactor alarms

Alarm System Alarm triggered Corrective Action

Temperature 1. The reactor temperature is controlled by


Low
temperature control loop system.

2. Make sure to check and adjust the flow rate of

cooling salt water entering the reactor using bypass


High
valve VS-233.

1. Ensure to rise the temperature controller action.

2.Make sure to check and adjust the flow rate of

cooling salt water entering the reactor using bypass

valve VS-233.
High High
3. Press emergency shutdown button or automatic

trigger

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3.8.5 Alarm System for Switch Condenser, SC-01

A. Temperature Alarm System

The temperature alarm systems connected to the switch condenser (SC-01) is important

to alert the operating personnel about the abnormal or deviation occur in the switch condenser

of the plant. If the temperature is too high, it might cause the switch condenser to be

malfunction or broke down. This will lead to high maintenance cost as it will requires frequent

maintenance service. Besides that, the purity and amount of Phthalic Anhydride collected will

be affected if the temperature is too high. As low temperature is required to solidify the Phthalic

Anhydride above its solidification point. the There are three types of alarm been installed, low

alarm, high alarm and high high alarm. High high alarm, high alarm and low alarm are installed

at the input stream of the switch condenser while high alarm and low alarm are installed at the

output stream (stream 10) of switch condenser. High high alarm is triggered when the switch

condenser temperature reaches + 10℃ of its operating temperature. High high alarm is used to

trigger the emergency shutdown system. High alarm and low alarm are triggered when the

switch condenser temperature reaches ± 5℃ of its operating temperature.

B. Flow Alarm System

There are two flow alarm system been installed at the output stream of switch condenser

(stream 10). They function is to alert the operators about the fluctuation of flow rate occurring

at the output stream of the switch condenser before entering the next operating unit. High

alarm and low alarm are triggered when the flow rate reaches ± 5℃ of the its operating flow

rate.

129
Table 19: Trigger values for switch condenser alarm systems

Alarm Operating Trigger values for various alarm

System Condition Low High Low Low High High

Temperature 45℃ 42.75 ℃ 47.25℃ - 49.5℃

input

Temperature 45℃ 42.75℃ 47.25℃ - -

output

(Stream 11)

Flow 43.33 kg/s 45.50kg/s 41.16kg/s - -

Table 20: Corrective actions after triggering of switch condenser alarms

Alarm System Alarm triggered Corrective Action

Temperature Low 1. The switch condenser temperature is controlled by

temperature control loop system

High 2. Check and adjust the flow rate of process fluid

entering the switch condenser using bypass valve V-

338.

High High

1.Ensure to rise the temperature controller action.

2. Check and adjust flow rate of the process fluid

entering the switch condenser using bypass valve VS-

338.

130
3. Press emergency shutdown button or automatic

trigger

Flow Low 1. The switch condenser flow rate (stream 10) is

controlled by flow control loop system

2. Check and adjust the flow rate of process fluid

entering the heat exchanger, E-04 using bypass valve

VS-350.

3.8.6 Alarm System for Distillation Column, T-01

There are two alarm systems installed for the distillation column: pressure alarm system and

level alarm system.

A. Pressure Alarm System

Pressure alarm system is used to alert the operators upon the pressure fluctuation in the

distillation column. Pressure alarm system is required as pressure fluctuation in distillation

column cannot be tolerated. Low pressure is not desired as it leads to deviation in product

purity. High pressure is even not desired as it not only leads to deviation in product purity but

also brings high explosion risk caused by column overpressure. Three types of alarm are

installed: low alarm, high alarm and high high alarm. High alarm and low alarm are triggered

when the column pressure reaches ± 5% of the column operating pressure. High high alarm is

triggered when the column pressure reaches ± 10% of the column operating pressure. High

high alarm is used to trigger the emergency shutdown system too.

131
B. Level Alarm System

Distillation column base level alarm system is used to alert the operators upon the level

fluctuation at distillation column base. Distillation column base level alarm system is required

as level fluctuation at distillation column base cannot be tolerated. Low column base level is

not desired as possibly flooding occurs causing no liquid to be accumulated at column base.

High column base level is not desired as it possibly causes flooding of the column base liquid

back to the distillation column stage. Two types of alarm are installed: low alarm, high alarm.

High alarm and low alarm are triggered when the column base level reaches ± 5% of the column

base operating level.

Table 21: Trigger values for distillation column alarm systems

Alarm Operating Trigger values for various alarm

System Condition Low High Low Low High High

Pressure 1atm 0.95atm 1.05atm 1.1atm

Level 10.72m 10.18m 11.26m

Table 22: Corrective actions after triggering of distillation column alarms

Alarm System Alarm triggered Corrective Action

Pressure Low

1. The distillation column pressure is controlled by


High
pressure control loop system.

2.Make sure to check and adjust the flow rate of

cooling water entering distillation column using

bypass valve V-455.

132
High High

1. Rise up the pressure controller action

2.Make sure to check and adjust flow rate of cooling

water entering condenser using bypass valve V-455.

3. Break pressure safety valve to relieve the

distillation column overpressure.

4. Press emergency shutdown button or automatic

trigger.

Level Low

1. Level control on distillation column is controlled at

base level control loop system

2. Make sure to check and adjust the flow rate of

bottom product using bypass valve VS-463.

3.9 Comparison with Industry on SOP Preparation and Alarm System Setting

All the documentations on SOP, shutdown procedure and the alarm system setting

prepared in the previous section are in the same and appropriate format as the current

industrial requirement. The sequences arranged are done based on safety consideration and

process requirements. As attached below is the document from Lotte Chemical Titan (M)

Sdn. Bhd. All the content is private and confidential with copyright reserved

133
3.9.1 Standard Operating Procedure (SOP)

3.9.2 Shut-Down Procedure

134
3.9.3 Alarm System

135
136
REFERENCES

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Apr 2019].

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transducer/[Accessed 15 Apr 2019].

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2019].

6. https://www.instrumart.com/assets/Hedland-Air-Flowmeter-Manual.pdf[Accessed 15

Apr 2019].

7. https://instrumentationtools.com/level-transmitter-calibration-procedure/[Accessed 15

Apr 2019].

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2019].

9. https://www.instrumentationtoolbox.com/2017/03/how-to-calibrate-fisher-3582-

pneumatic.html[Accessed 15 Apr 2019].

10. https://automationforum.in/t/how-to-calibrate-pneumatic-control-valve-

positioner/2922[Accessed 15 Apr 2019].

11. https://instrumentationtools.com/installation-and-maintenance-of-control-

valves/[Accessed 15 Apr 2019].

12. Myiem.org.my. (2019). IEM. [online] Available at:

http://www.myiem.org.my/content/professional_conduct_and_discipline-68.aspx

[Accessed 5 Apr. 2019].

137
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http://bem.org.my/registration-of-engineers-act-1967-revised-2015- [Accessed 5 Apr.

2019].

14. Aiche.org. (2019). Code of Ethics. [online] Available at:

https://www.aiche.org/about/code-ethics [Accessed 5 Apr. 2019].

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https://www.api.org/~/media/certifications/apiauditorcodeposter_en.pdf?la=en

[Accessed 5 Apr. 2019].

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were-from-dumped-oil-waste-report[Accessed 14 Apr 2019].

17. https://www.channelnewsasia.com/news/asia/pasir-gudang-chemical-spill-singapore-

director-plead-not-guilty-11378254[Accessed 14 Apr 2019].

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crisis[Accessed 14 Apr 2019

19. https://www.latlong.net/c/?lat=3.975810&long=103.393000[Accessed 10 Apr 2019].

20. https://www.freemaptools.com/elevation-finder.htm[Accessed 10 Apr 2019].

21. https://www.windy.com/3.983/103.365?3.670,103.365,9,m:dLNai1r[Accessed 10 Apr

2019].

22. https://response.restoration.noaa.gov/oil-and-chemical-spills/chemical-

spills/resources/immediately-dangerous-life-health-limits-idlhs.html[Accessed 10 Apr

2019].

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spills/resources/acute-exposure-guideline-levels-aegls.html[Accessed 10 Apr 2019].

138
24. https://ehs.unl.edu/sop/s-chemical_haz_assessment_risk_min.pdf[Accessed 07 Apr

2019].

139
APPENDIX

Appendix A: Meeting Minute

Meeting Minute 1

Date : 19th March 2019


Time : 10.00am-11.00am
Venue : Anjung Ilmu, School of Chemical Engineering

Attendance : Muhammad Shafizruddin Firdaus Bin Fazli Ku


Muthu Kumar A/L Ganeson
Nurul Atikah Binti Saifulqahar
Zahira Binti Mohamed Malik

Agenda

1. Discuss the correction from previous report.


2. The meeting was continued by distributing the subtopic from Chapter 1 which is
planning/execution of the project.
3. Study about the P&ID, on how to install proper control loops (flow, temperature,
pressure, and level)
4. We plan to settle ethical part first since we need to settle our FYP report.
5. Distribute work within team members. For Part A Question 1, 2 and 3 each member
was given 3 equipment each to do the P&ID

Prepared by,

Muthu
Muthu Kumar A/L Ganeson

140
Meeting Minute 2

Date : 30th March 2019


Time : 9.00pm-10.30pm
Venue : Café Lembaran

Attendance : Muhammad Shafizruddin Firdaus Bin Fazli Ku


Muthu Kumar A/L Ganeson
Nurul Atikah Binti Saifulqahar
Zahira Binti Mohamed Malik

Agenda
1. Discussed our progress and problem identified during the progression of tasks

2. Study on how to run Aspen Dynamic Analysis on the distillation column.

3. Study on how to run the simulation for ALOHA

4. Investigate on how to choose and locate proper sensors for P&ID.

Prepared by,

Muthu
Muthu Kumar A/L Ganeson

141
Meeting Minute 3

Date : 4th April 2019


Time : 9.00pm-11.30pm
Venue : Café Lembaran

Attendance : Muhammad Shafizruddin Firdaus Bin Fazli Ku


Muthu Kumar A/L Ganeson
Nurul Atikah Binti Saifulqahar
Zahira Binti Mohamed Malik

Agenda
1. Briefly explain the progress on individual tasks

2. Discussed our progress and problem identified during the progression of tasks

3. Discuss and plan how to draw the plan layout for our plant

4. Focused on other task questions.

5. Distribute tasks for chapter 2, 3 and 4

Prepared by,

Muthu
Muthu Kumar A/L Ganeson

142
Meeting Minute 4

Date : 15th April 2019


Time : 9.00pm-11.30pm
Venue : Café Lembaran

Attendance : Muhammad Shafizruddin Firdaus Bin Fazli Ku


Muthu Kumar A/L Ganeson
Nurul Atikah Binti Saifulqahar
Zahira Binti Mohamed Malik

Agenda
1. Briefly explain the progress on individual tasks

2. Discussed our progress and problem identified during the progression of tasks

3. Discussed on the problems of unfinished tasks in Chapter 2, chapter 3 and Chapter 4.

4. Compiling the current tasks into words file.

Prepared by,

Muthu
Muthu Kumar A/L Ganeson

143
Meeting Minute 5

Date : 18th April 2019


Time : 9.00pm-11.30pm
Venue : Café Lembaran

Attendance : Muhammad Shafizruddin Firdaus Bin Fazli Ku


Muthu Kumar A/L Ganeson
Nurul Atikah Binti Saifulqahar
Zahira Binti Mohamed Malik

Agenda
1. Briefly explain the progress on individual tasks

2. Discussed our progress and problem identified during the progression of tasks

3. Editing, compiling and referencing the report.

Prepared by,

Muthu
Muthu Kumar A/L Ganeson

144

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