1.

Introduction

pH control systems are pivotal part of regulating the pH range of the wastewater that is
discharged from industrial and commercial sites. Usually the pH effluent limits in
discharging the wastewater to the environment will be around 6-10. The process employed in
stabilizing pH is known as neutralization. This chemical process uses acid or base to produce
a neutral solution. The pH neutralization system consists of a couple of liquid streams acid
and base and the stream are used respectively according to the need of the system.[1] For
example, if the system’s pH is lower than the set-point pH, basic stream will be used while on
the contrary, if the system’s pH is higher than the set-point, acidic stream will be used. The
pH control can be tricky as the problem can arise not only from the control system but also
from the chemical equilibrium and sometimes even in the kinetics of the neutralization
process itself. The challenge of pH control is to maintain the system’s pH as close to the set-
point pH. Buffering capacity is also a challenge when it comes to fine-tuning a pH control
system. As the pH deviates slightly from the set-point, small amounts of acid or base will be
continuously added to bring back the pH to its set-point. Here the control system’s response
time is tested as, late response could cause huge amount of acid/base being used, which in
return does more damage than a batch of unbuffered sample. The amount of liquid being
added is usually regulated by a control valve which receives the input from the controller or it
can also be operated manually. A proportional integral derivative (PID) control loop feedback
system is the common type of controller used in the industry. The controller can be used for
so many different situations thus making it very robust. Proportional action corrects the error
from the system by sending a change in the input directly proportional to the control error.
The integral action on the other hand eliminates offset and the derivative action quickens
corrective response thus stabilizing the system quicker.[2]
2. Literature Review

The textile industry in general consumes enormous quantities of water and large
volumes of wastewater obtained from various stages of textile production. Nowadays, due to
the lower efficiency of chemical operations in conjunction with the spillage of chemicals,
significant pollution occurs and leaves an adverse impact on the discharged wastewater
treatment process. Neutralization is a type of process often used to control and maintain the
pH of wastewater to prevent pollution upon discharge. However, it is hard to control the pH
process with an excellent and robust performance due to its non-linearity’s, time-varying
properties and sensitivity on small disturbances when working near the equivalence point.
Therefore, more reliable, accurate, efficient and flexible control systems are required for pH
neutralization process [2].

When it comes to pH neutralization process, the control is highly challenging. This is

because the process is characterized by high nonlinearities and changing process dynamics
which are usually difficult to model. These factors degrade the performance of the system.
Therefore, many researchers are trying to introduce and implement robust control
methodologies for modelling and control of pH processes. [3]. In process control industries,
PID controllers are the mostly used owing to their simple design and tuning. The most
important and crucial task while designing the controller is proper tuning of its parameters.
To dates, Ziegler-Nichols (ZN) tuning is the most widely accepted method for determining
the parameters of PID controllers.

The Ziegler-Nichols tuning method was developed by John Ziegler and Nathaniel
Nichols in 1942, and it remains a widely used and unique technique for tuning controllers that
utilizes integral, proportional and derivative actions in the industrial sector. As for control
system performance, the in close-loop format is normally measured by applying a step
function as the set point command variable continued by measuring the response of the
process variable. In general, the response is observed and studied by measuring defined
waveform characteristics. These are rise time, percentage overshoot, settling time, steady-
state error [4]. The PID controller sole function is mainly on the comparison between the
reference input signal and output signal of the control system mainly to effect the control
action. The difference which is termed the error signal is the basis on which the controller
depends for required performance. The Ziegler-Nichols design method is one of the most
popular methods used in process control solely to evaluate and know the parameters for a
PID controller. Not only that but, Ziegler-Nichols tuning method as a whole is a trial and
error method which is based on sustained oscillations introduced by Ziegler and Nichols.
Known for its unique continuous cycling method, Ziegler-Nichols method is widely used in a
myriad of applications. Also, using However, ZN-PID's are found to be satisfactory for first-
order processes with small dead-time even in the presence of load disturbances, but under set-
point change and long dead-time, it fails to keep the process within acceptable limit [3].
Diving in the industrial sector, the PID human tuning method is normally applied in
machinery tuning is Ziegler Nichols (ZN) tuning method, known as the ZN-PID tuning
method. But this PID controller tuning method is ineffective in ways such as during the
control of nonlinear and complex system with varied parameters, large inertia and large
delay, as it tends to give a very higher overshoot, higher rise time and higher settling time in
the system operation. These disturbances, due to the nonlinearity of the system under control
cause the controller to produce poor responses at the output, leading to poor system
performance. The limitations in this ZN-PID tuning method could be overcome by using
other fine tuning methods such as Cohen-Coon-PID (CC-PID) or others to drive the system
plant [4].

Cohen-Coon (CC) tuning methods of PID controller is an extension to the Ziegler-

Nichols (ZN) methods [5]. This tuning method is a method based on the ZN type tuning
algorithm which referring to the first order plus dead time model [4]. Usually, ZN method
shows a slow steady state response but in order to overcome the limitation of ZN method, CC
tuning method is introduce [5]. In Cohen-Coon method, it gives better advantages in term of
reduction in energy consumption which resulted the reduction also occur in output cost. This
is due to the CC methods which has low percentage overshoot and setting time [4].
Moreover, in term of controller error, the CC tuning control technique shows less error
occurred compared to ZN method for each step size and each range. This occurred due to the
ability for coping up the dynamic disturbance [5].The Cohen-Coon tuning rules work well on
processes where the dead time is less than two times the length of the time constant and can
even be stretched further if process demands. However, the major problem arise in Cohen-
Coon parameters is that they tend not to be very robust which if there is a small change in the
process parameters, it can cause the closed-loop system become unstable and lead to
oscillatory closed loop behaviour [6].
 2.1. Cohen –Coon (CC) Tuning Methods

Cohen-Coon (CC) tuning methods of PID controller is an extension to the Ziegler-Nichols

(ZN) methods [5]. This tuning method is a method based on the ZN type tuning algorithm
which referring to the first order plus dead time model [7]. Usually, ZN method shows a slow
steady state response but in order to overcome the limitation of ZN method, CC tuning
method is introduce [5]. In Cohen-Coon method, it gives better advantages in term of
reduction in energy consumption which resulted the reduction also occur in output cost. This
is due to the CC methods which has low percentage overshoot and setting time [7].
Moreover, in term of controller error, the CC tuning control technique shows less error
occurred compared to ZN method for each step size and each range. This occurred due to the
ability for coping up the dynamic disturbance [5].The Cohen-Coon tuning rules work well on
processes where the dead time is less than two times the length of the time constant and can
even be stretched further if process demands. However, the major problem arise in Cohen-
Coon parameters is that they tend not to be very robust which if there is a small change in the
process parameters, it can cause the closed-loop system become unstable and lead to
oscillatory closed loop behavior [6].

3. Application of Chemical pH Process Control

3.1. Milk and Diary Industry

Chemical pH process control system plays an essential role for controlling and measuring pH
in milk and diary processing to meet their regulatory requirements. The purposes of controlling pH
are to prevent causing health problems to consumers and produce product with consistent well defined
properties as well as at optimal cost. Small changes in pH may bring significant impact to flavour,
consistency and shelf-life of product due to the logarithmic nature of measurement. For example, the
difference between pH 6 and pH 5 signify that a ten-fold increase in acid concentration and a change
of 0.3 signifies a doubling of acid concentration. Therefore, controlling pH value is very important in
milk and diary processing especially in manufacturing cheese and butter [8].

The quality of milk that used for cheese processing must be excellent and its pH value is the
crucial parameter to determine whether the cheese will be soft or hard. During cheese preparation,
souring of milk and cream maturation, the pH value must be maintain in the range of 4.1 to 5.3 in
order to slow down the growth and multiplication of pathogen. Moreover, with butter production,
cooling of cream can start only after pasteurization at a very strict pH of 6.70 to 6.85 to produce sweet
butter while citric acid extracts are only added to acidify the cream to pH 4.6 to 5.0 for producing sour
butter. Thus, constant pH measurement and controlled addition of buffering agents are vital for
assuring reliable milk and diary product quality [8].

3.2. Wastewater Treatment

pH process controlling is important for wastewater treatment as it enables separation of waste

from water during treatment process. Most of wastewater treatment is focusing on removing heavy
metals and organic compound from effluent by chemically adjusting pH. In acidic condition, the
excess of positive hydrogen or metal ions have nothing bond with and float in water while at a basic
condition the excess hydroxide ions bond with metal ions to form metal hydroxide and they can be
removed through filtering or settling [9].

Furthermore, pH of water can be used to kill off microorganism in wastewater. Most of the
microorganism is familiar in condition of neutral or basic. Hence, to kill the microorganism the pH
value should be controlling in acidic condition break down the cell as well as slowing their growth.
After a wastewater treatment cycle the pH must be raised back to neutral by adding chemicals [9].

4. Problem Statement

Nowadays in many industrial sectors and processes, the control of pH is a very crucial
step to be figured out mainly because of its ability and function which is significantly needed
in many industrial applications. Therefore, the development of appropriate strategies which
monitors and controls pH is definitely required. From the existing WA 921 Chemical Process
Control equipment, an improvement and alteration to the experimental setup either process-
wise or equipment wise is muchly needed to obtain a smooth and a stable response towards
any possible disturbances or variation in the pH system.
5. Methodology
5.1. Flow Chart

Meet the technician in-charge for briefing of unit operation given

Understand the process control unit operation and know all the equipment involved in
the experiment

Meet supervise lecturer for the experiment to find out the things needed for the
proposal of experiment

Do group discussions and distribute works accordingly in order to complete the

proposal

Meet the lecturer for the approval of the experiment proposal

Conduct the experiment and run scientific study based on two methods which are
Ziegler Nichols method and Cohen-Coon method
 Do calculations and determine the most suitable method PID controller tuning
method to use in chemical pH process control

Meet lecturer for the approval of data obtained and to continue next step

Do discussion for the lab report and distribute work accordingly

Submission of the lab report

5.2. Procedure

A. Determination of PID tuning parameter of the process model.

1. Weigh 20g of sodium hydroxide (NaOH) pellets and dissolve it in 500ml of water.
2. Measure 30ml of hydrochloric acid (HCl) (37wt%) and mix it with 500ml of water.
Make sure the acid is added to water and not the other way around.
3. Add the dissolved sodium hydroxide and hydrochloric acid into T51 and T52
respectively.

B. Startup procedure

1. Fill T53 with water using hose until overflow hole.

2. Valve V2, V4, V7, V17, MV2, MV3, MV4 is opened and valve V1, V3, V5, V8,
V13, V15 is closed.
 3. The main power supply is turned on.

C. Obtaining the process response

1. Measure and record the pH of the sodium hydroxide and hydrochloric acid.
2. Calculate the concentration of the sodium hydroxide and hydrochloric acid.
3. Set P52’s frequency and stroke length to 100rpm and 50% respectively.
4. Set P51’s stroke length to 20%.
5. Set the controller setpoint to 7. Switch PHIC 51 to manual mode.
6. P51, P52 and P53 is switched on. Observe the pH of system to reach a steady state
value.
7. Increase P51’s stroke length to 70%. Record the response in PHIC 51.
8. Analyze the response graph to determine the PID controller parameters.

D. Response of Closed-loop Control System.

1. Switch on P52.
2. Set P52’s frequency and stroke length to 100rpm and 50% respectively.
3. Set the controller setpoint to 7. Switch PHIC 51 to automatic mode.
4. Set the PID values of Cohen Coon in PHIC 51.
5. Switch on P52 and P53.
6. Observe and wait for the pH reach 5.
7. Start P51.
8. Record the response in PHCR 51.
9. Repeat Experiment D using Zeigler-Nichols method.
 5.3. Formula of Calculation

Process Model:

∆y
K=
∆x

K e−θs
G=
τs+1

PID controller settings [10], [11] :

PID Ziegler Nichols method Cohen Coon method

parameters
Kc 0.5 K cu 1 τ 4 td
() ( + )
K t d 3 4τ

τI Pu τd
2 (
t d 32+6
τ )
td
13+ 8
τ
τD Pu 4td
8 2td
( 11+
τ )
Where K, gain

Pu, ultimate gain

K cu , ultimate gain

τ , effective time constant of first order response

t d, dead time
6. Reference

[1] T. K. Gustafsson, B. O. Skrifvars, K. V. Sandström, and K. V. Waller, “Modeling of pH for

Control,” Ind. Eng. Chem. Res., vol. 34, no. 3, pp. 820–827, 1995.

[2] R. Babu and R. Swarnalath, “Comparison of Different Tuning Methods for pH Neutralization
in Textile Industry,” J. Appl. Sci., vol. 17, no. 3, pp. 142–147, 2017.

[3] K. Bingi, R. Ibrahim, M. N. Karsiti, T. D. Chung, and S. M. Hassan, “Optimal PID control of
pH neutralization plant,” 2016 2nd IEEE Int. Symp. Robot. Manuf. Autom. ROMA 2016, 2017.

[4] E. Joseph, E. A. Amnim, C. Regd, and M. Tech, “Cohen-Coon PID Tuning Method : A Better
Option to Ziegler Nichols-Pid Tuning Method,” vol. 9, no. 5, pp. 33–37, 2018.

[5] R. Sen, C. Pati, S. Dutta, and R. Sen, “Comparison Between Three Tuning Methods of PID
Control for High Precision Positioning Stage,” Mapan - J. Metrol. Soc. India, vol. 30, no. 1,
pp. 65–70, 2014.

[6] A. K. Mehta and R. Swarnalatha, “Performance evaluation of conventional pid control tuning
techniques for a first order plus dead time blending process,” J. Eng. Sci. Technol., vol. 13, no.
11, pp. 3593–3609, 2018.

[7] E. Joseph, “Cohen-Coon PID Tuning Method: A Better Option to Ziegler Nichols-Pid Tuning
Method,” Online), vol. 9, no. 5, pp. 33–37, 2018.

[8] “The Importance of pH in Food Quality and Production,” SPER SCIENTIFIC, 2015. .

[9] T. Brand, “The Importance of pH in Wastewater Treatment,” ADVANCED Chemical Systems,

2019. .

[10] M. F. B. M. NORIS, “COMPARISON BETWEEN ZIEGLER-NICHOLS AND COHEN-

COON METHOD FOR CONTROLLER TUNINGS MOHD FADZLI BIN MOHD NORIS A
thesis submitted in fulfillment of the requirements for the award of the degree of Bachelor of
Chemical Engineering Faculty of Chemical & Natural,” no. November, 2006.

[11] D. E. Serborg, T. F. Edgar, D. A. Mellichamp, and F. J. D. III, Process Dynamics and Control,
Third Edit. John Wiley & Sons, Inc., 2011.