UNIVERSITI MALAYSIA PERLIS

PUSAT PENGAJIAN KEJURUTERAAN ALAM SEKITAR School of Environmental Engineering

EAT 449

ENVIRONMENTAL PROCESS CONTROL AND INSTRUMENTATION

Title : pH Control in Fermentation Process Lecturer : Dr. Fahmi Muhammad Ridwan Group members
LIEW JEUN YANG THENMOLHI A/P RAVINDER ROSNAH BINTI HAMID NUR FALAHI BINTI MOHAMMED

No.matric
101130420 101131300 101131123 111131334

Content

Chapter 1 : Introduction

1.1 Background 1.2 pH monitoring devices 1.3 Background of fermentation in plants 1.4 pH control

Chapter 2: Process control and instrumentation

Chapter 3 : Process Description and modeling 3.1 Process Description 3.2 Process Modelling Chapter 4 : Process control Design 4.1 Equation for acid, 4.2 Equation for alkaline , 4.3 Calculation part 4.4 Characteristic equation 4.5 Routh Array 4.6 Root locus Chapter 5 : Conclusion References

CHAPTER 1 INTRODUCTION

1.1 BACKGROUND In the general aspects of process control, there are also focuses on process control applications in the chemical process industries (CPI) and biotechnology industries. The chemical process industries represents a range of industries that are use processing units to produces a wide range of products such as hydrocarbon fuels, petrochemical products, concrete, pharmaceutical products, paper products, man made fibers and films, agrochemical products and ceramics. Biotechnology is the technology that uses microbial species or any other living organisms or part of them to produce useful products (Atkinson et al, 1992).

Fermentation is a another type of chemical process and its also engineering that help in the development and regulation of biological processes. There are possibilities in applying ideas and techniques developed for more conventional chemical system (Gaden, JR., et al, 1959). There are three types of fermentation methods such as batch fermentation, fed batch fermentation processes and continuous fermentation. The batch fermentation can be refers as a partially closed system and requires materials are loaded onto the fermenter, decontaminated before process starts and then removed at the end. The regulation of batch fermentation process variables are temperature, dissolved oxygen and the traces which determined by initial conditions (micobiological basis). Fedbatch fermentation is a production technique which lies between batch and continuous fermentation which related to the presence of production of high concentrations of substrates. The presence of concentration can be avoided by limiting the amounts that required in biochemical production (R.M. Dekkers, 1979)

In addition, the control process of variables which we distinguishing between batch and fed-batch / continuous fermentation are similar with closed loops cases such as temperature, pH and possible dissolved oxygen.

Figure 1 shows typical industrial fermentation and typical process measurements that are availables. The typical measurements can be differentiate as on-line and off-line. The industrial fermenter control can be divided into three categories such as on-line environmental control (examples: pH and temperature), off-line environmental-control (examples: nutrient concentration and precursor concentration) and off-line organism state control (examples: biomass concentration and hyphal length distribution) (Gary A. Montague et al)
.

1.2 pH monitoring devices A pH measurement is a determination of the activity of hydrogen ions in an aqueous solution. Many important properties of a solution can be determined from an accurate measurement of pH, including the acidity of a solution and extent of a reaction in the solution. Many chemical processes and properties, such as the spees of a reaction and the solubility of a compound, can also depend greatly on the pH of a solution. In application ranging from industrial opertaions to biological processes, it is important to have an accurate and precise measurement of pH. Most modern pH electrodes consist of a single combination reference and sensing electrode instead of separate electrodes. This type of pH electrode is much easier to use and less expensive than electrode pair. A combination electrode is functionally the same as an electrode pair.

Figure 2 (a) glass electrode (b) combined electrode

Any pH electrode requires both a sensing electrode and a reference electrode. The sensing electrode consists of a thin hydrogen permeable membrane containing a solution and electrode. The membrane of the sensing electrode allows hydrogen to slowly pass, creating a positive voltage across the membrane. The voltagecreated in this electrode is then compared to the voltage in the refences electrode. The voltage difference between the two electrode is then used to determine the pH of the unknown solution using the Nernst equation. E(pH) = E(constant) + (2.3* RT/nF) * log [H+] (5)

Where: E (pH) = Voltage difference between sensing electrode and Reference electrode (V) E (constant) = Voltage difference in a solution with pH = 7 (V) R = Gas Constant (8.314 J/K*mole) T = Temperature in Kelvin (K)

n = Number of Valence Electrons per Mole (1 for H+) F = Faradays Constant (96500 J/V * mole e-)

1.3 Background of fermentation in plants

A typical batch fermentation process starts with sterilization so that all micro-organisms found in the mash and reactor are completely destroyed. The mash heated in the fermenter or a special cooking vessel by injecting live steam or by means of steam coils set in the vessel. Holding the temperature at 121C (250 F) for 30 miunutes is usually adequate to destroy all living organism in the mash. However dome processes require higher temperature, as shown in figure 2 which a heating/cooling jacket maintains the temperature of the fermentor.

A fermentation cycle can be divided into two phases are (a) the growth phase and (2) the production phase. During the growth phase, cells grow very slowly because its adapting to the reactor environment. After the adaption period, the cell culture grows exponentially, releasing enzymes as a byproduct of the metabolic process. During the production the molecular products are formed through a series of chemical reations catalyzed by the enzymes. For many fermentation processes, these two phases are con-current.

1.4 pH control

pH is the one of the most important chemical environmental measurements used to indicate the course of the fermentation process. It detects the presence of specific chemical factors that influence growth, metabolism and final product. For example, the pH of commercial mash of P.chrysogenum (penicillin production) should be closely monitored and controlled in both the growing phase and the production phase. Initiation of the growth phase, the ph of the mash is carefully maintained between 4.5 and 5.5, depending on the mash formulation. The range is set to ensure the most favourable condition for growth. The metabolism of glucose and rapid consumption of ammonia during this phase adversely affect

the medium by lowering the pH. If the medium is not adjusted, growth may be inhibited and the fermentation may take a long time to reach the optimal range required for penicillin production.

In the production phase, the organism starts to metabolize other sugars (lactose) and amino compounds because of the depletion of glucose. The liberation and accumulation of ammonia from the metabolism of amino compounds will cause the pH to slowly rise. The pH is allowed to about 7 and is controlled at this point until the end of production. Depending on the culture and several other factors, it has been found that the optimum range of penicillin production lies between 6.8 and 7.8. the pH is monitored and controlled in this range by the addition of sulfonic acid. Finally at the end of the fermentation, the pH rises and production stops. Figure 2 shows that the pH control loop implemented on a standard fermentor.

Figure 2

Chapter 2

Process control diagram and Instrumentation

pH is read by the measurement of an electric potential generated at a pair of electrodes, which are wetted by the sample stream. All pH instruments use a buffer solution, which is generally pumped to the electrodes in very small volumes by the controller. The solution must be replenished at intervals. 1. A needle valve and rotameter should be provided to adjust the flowrate past the electrodes so that it falls in the range required by the manufacturer. If necessary, a pressure reducing valve should be installed upstream of the needle valve to make the flowrate adjustment easier. 2. If the sensor element could become clogged with silt, a filter should be provided upstream. The sensor elements are generally very fragile, so flush lines should only be provided where the electrodes can be completely removed from service during flushing. 3. The liquid stream is contaminated with buffer solution during the measurement; the stream should be discharged to waste. 4. If the controller includes an alarm contact to warn of low buffer solution level, the contact should be tied into the alarm system to remind the operator to refill the controller. 5. The sense element must not be mounted far from the controller because of the very low-level signals involved. If necessary, the sample line should be routed to a location where the sense probe and the controller may be located near each other. 6. The controller should include a display, and should be installed so that the display is easily read.

Process control diagram to control pH

CHAPTER 3

PROCESS DESCRIPTION AND MODELLING

3.1

Process Description

The Reactor Tank The reactor tank is very crucial in this research as this is where the neutralization reaction process takes place and where the output measurements are taken. Figure shows the simplified diagram of the physical arrangement of the reactor tank and a photograph of the actual reactor tank on the pH neutralization pilot plant.

The reactor tank

The outlet point is positioned to provide a maximum storage volume for this tank of 80L. The minimum operating volume is 30L, as the agitator will not be able to mix the solution properly if the volume is smaller than this value. Thus most of the simulation and experimental results are based on a volume of mixing solution of approximately 80L. As shown in the figure, the pH meter (AT 122) and the agitator (AG 120) are installed near the acid feed stream inlet. The main purpose of this agitator is to mix both solutions completely and homogeneously. In addition to that, it will also accelerate the neutralization reaction process. The agitator produces some turbulence in the tank in order to mix the solution satisfactorily. The pH value from the online pH meter is also relatively consistent, indicating

that the agitator works adequately and its turbulence does not adversely affect the measured signals.

3.2

Process Modelling

The first principle that is applied is known as the conservation balance principle. The conservation balance equations that are commonly used in process control are the equations for conservation of material, energy and momentum. As far as this research is concerned the variables involved relate to the total liquid mass in the reactor tank and the principle of conservation of material is used in the derivation of the basic equations of the process. The general equation for the conservation of material for the pH process may be written as follows:

( (

) )

As described earlier, the volume V represents a constant volume of 80L of the reactor tank. The flowrates for the acid and alkaline streams are F1 and F2 respectively. The concentration for acid in tank is C1 and the concentration of alkaline in tank is C2.

The non-reactant components in the system are for acid and for alkaline. = [ H2SO4] + [HSO-4] + [SO-24] = [Na+]

The next step is to identify and derive the electroneutrality condition of the nonreactant components. Based on the principle of electroneutrality all solutions are electrically neutral. There is no solution containing a detectable excess of positive or negative charge because the sum of positive charges equals the sum of negative charges. The total electro neutrality condition is, [ ] [ ] [ ] [ ] [ ]

The equilibrium constant expressions that apply to the acid-base system, i. Water (H2O) Kw = [H+] [OH-] ii. Sulphuric acid (H2SO4) [ [ ][ ][ ] ]

The quantity Kw (the constant value for the ionic product of water), is equal to 1.0 x 1014. There are two acid dissociation constants for sulphuric acid K1= 1.0 x 103 and K2=1.2 x 10-2 since sulphuric acid falls under category of a diprotic acid, having two equilibrium points or dissociation points. However for this case, the first point is negligible as the first dissociation constant, K1 is too large. Theoretically the titration curve for this acid-base reaction process will only show one break point or equilibrium point.

The pH scale is a measure of the hydrogen ion concentration, thus the pH value can be calculated by using the equation below. [ pH equation, [ a1 = K1 + a2 = K1 + K1K2 Kw K1 a3 = K1K2 + K1Kw 2K1K2 a4 = - K1K2Kw ] [ ] [ ] [ ] ]

Chapter 4

Process control Design

4.1 Equation for acid,

= F1C1 - (F1 + F2)

) ( )

S [(s) (0)] =

) ( )

(s) [S +

]=

+ (0)

(s) =

( )
( )

(s) =

* (

+
)

( )[ )

. Equation for acid (1)

4.2 Equation for alkaline,

= F2C2 - (F1 + F2)

) ( )

S [(s) (0)] =

) ( )

(s) [S +

]=

+ (0)

(s) =

( )
( )

(s) =

* (

+
)

( )[ )

. Equation for alkaline (2)

4.3 Calculation part Assume that :V = 80 l F1 = 300 l/h F2 = 350 l/h =3 C1 = 0.5 M C2 = 0.5 M = 11

For acid,

Gp =

* ( * ( + [

+
)

( )* ) ]

= = = So,

Kp = 0.5 tp = 0.1

For alkaline,

Gp =

* ( * ( + [ )

+
)

( )* ) ]

= = = So ,

Kp = 1.7 tp = 0.1

Gs , Ks = = = 1.14 Assume time delay , ts = 3 Gs = Ga = 1 Gc = Kc

4.4 Characterisation Equation

(Kc) ( Ga) (Gp) (Gs) + 1 = 0 (Kc) (1) ( )( )+1=0

( ( ( Kc +

)(

) ) ) =0 ( )

4.5 Routh Array n

A1 = = =

) (

A2 = 0

= 3.15 0.05Kc

B1 =

[(

)(

B2 = 0

= 1+ Kc

Therefore ,

=(

3.15 0.05 Kc 0 -0.05 Kc -3.15 Kc 63

1 + Kc 0 Kc -1

4.6 Root Locus Kc 0 -2 -1 2 4 R1 -0.33 0.3 -10.17 + 1.82i -1.19 -13.22 R2 -10 -10.31 -10.17-1.82i -6.79 -3.33 R3 -10.31-2.53i 0 -12.35 -3.78

Chapter 5

Conclusion

A fermenter is a vessel which does not permit contamination but provides conditions necessary for the maximum production of the desired product. The use of software sensors, which combine signals already available on-line with mathematical models, should be a valuable tool for process development. The possibility to obtain more information throughout the process using software sensors, without sampling and off-line analysis, generates a demand for efficient tools for data evaluation by muitivariate analaysis and data presentation. In conclusion , it is important to recognize the major advances in biosensors technology and how much instruments contribute to the overall control scheme. A significant conclusion is that in order to achieve improved control, process must become more computerized in their operation. The levels of computerization of bioprocess plants are very low compared to their chemical equilkvalent and in order to improve operability, this problem must be rectified. Greater computer application leading to improved data .

References and Appendices

1. Atkinson, R., Baulch, D.L.,Cox, R.A.,Hampson, R.F.,Kerr,J.A.r and Troe,J., 1992, Evaluated kinetic and photochemical data for atmospheric chemistry supplement IV Atmos.Environ., 26A, No.7, 1187-1230 2. Gaden, E.L., Jr.Chem & Ind (Rev.) (1955) , 154 3. Gary A.Montague, A.J.M., and John R Bush (1966). Considerations in Control Scheme Development for Fermentation Process Control, IEEE Control Systems Magazine , C30(88) 4. R.M. Dekkers, State Estimeation of a Fed-Batch Fermentation Process, Proc.1st IFAC on Modelling and Control of biotechnical Processes, Helsinki, Pergamon Press, pp.201-211,1979.