EXPERIMENT NO: 9 CHEMICAL AND ANALYTICAL SYSTEM: pH PROCESS CONTROL To identify the major components of the pH control system. To start-up the plant systematically. To study the process analytical measurement of pH. To study pH control using PID controller. To tune the PID controller using the open loop method. | KEYWORDS pH process, Neutralization process, PID control | 1. INTRODUCTION | Chemical and Analytical Process Control Training System, Model WA921, involves two chemical processes. They are (i) neutralization process and (ii) Demineralization process. 1.1 Neutralization Process: ‘An acid is reacted with alkali and the end point of this Neutralization process is at pH = 7. | If the acid is in excess quantity (pH below 7) or if the alkali is in excess quantity (pH above 7), it is brought to pH =7 by regulating the alkali flow rate. A batch of strong acid (for example, sulphuric acid) and a batch of strong alkali (for | example, sodium hydroxide) are prepared in sufficient quantity and concentration. The acid is pumped by a metering pump P52 And this flow rate can be manually set. The reaction between the acid and alkali takes place in the tank W53. The correct amount of alkali is regulated via a metering pump P51 by the PID controller PHICS1 to bring back the pH to 7. fessssiue Alll our experiments will be limited to reduced time constant and short dead time. We only use the small capacity tank W53 and the large tank TS3 is only used as a downstream mixing tank. 1.2 Demineralization Process: The discharge from the neutralization process now goes to the second process for total dissolved solids removal, The demineralization process will remove them by ion- exchange in a packed column filled with resin. The resin is a mixed bed of both cation and anion exchanger. UniKL-MICET Experiment (CPB 30004 — Process Dynamics and Control Laboratory periment]2. EXPERIMENTAL EQUIPMENT The experimental equipment is the Chemical and Analytical Process Control Training System, Model WA921 (Figure 13.1). 2.1 PROCESS PLANT Tank T52 contains a dilute solution of sulphuric acid. This represents acid waste. By manually setting the pump rate of P52, the waste discharge can be changed. This is done manually by changing the 0-100% stroke length at the circular knob-dial of pump P52. Tank TS1 contains a dilute solution of Sodium Hydroxide. This represents the reagent to neutralize the acid waste discharged. The flow rates can be manipulated by the 4-20 mA signal from the controller PHICS1, regulating the number of strokes per minute (spm) of the metering pump PS1. The acid and the alkali are injected into the suction of the recirculating pump PS3A and pumped into the measuring well W53. The overflow from W53 flows into the tank 53, The piping to W53 and T53 can be arranged in two different ways. This gives rise to two schemes, where one of them give rise to a reduced time constant and short time delay. 2.2 INSTRUMENTATION AND CONTROL SYSTEM ‘The following is a list of instruments and control systems used in WA921 SENSORS PHESI : _ pH sensor element, submerged in measuring well W53 CESI —: Conductivity sensors element, submerged in Tank T54 DOESI Dissolved Oxygen sensors element, submerged in Tank TS4 ORPES1 Oxidation reduction Potential sensors element, submerged in W53 INDICATOR-TRANSMITTERS PHITS! : Indicating pH transmitter cirsi Indicating conductivity transmitter DOITS1 : Indicating Dissolved Oxygen transmitter ORPITS1 : Indicating ORP transmitter CONTROLLERS A panel controller PHICS1/CICS1 configured with one PID and two ON/OFF controllers PHICS! : pH control, PID PHICSI1 : pH control, ON/OFF CICS1 : Conductivity control, ON/OFF UniKL-MICET Experiment CPB 30004 — Process Dynamics and Control Laboratory ———_———————————— |RECORDER PHCRSI : 3 Pen Recorder FINAL CONTROL ELEMENTS PSI : Metering pump, for PID control of pH PHSVS51 : Electric solenoid valve, for ON/OFF controller PHICS11 PHCV51 : Pneumatic control valve for PHSV51 CSVS51 _: _Bleciric solenoid valve, for ON/OFF controller CICS11 ccys! Pneumatic control valve for CSVS1 CSV52 Electric solenoid valve, for ON/OFF controller CICS1 PS4A Air operated pump for CSV52 ANNUNCIATORS PHAHS1 : pH at W53 exceeds the preset High alarm limit PHALSI : pH at W53 below the preset Low alarm limit CAHS1 : Conductivity at T54 exceeds the preset High alarm limit LALS1—: Level in TS1 below the Low limit LALS2 : Level in T52 below the Low limit 3. EXPERIMENTAL PROCEDURES 3.1. IDENTIFICATION OF MAJOR COMPONENTS OF THE PLANT Walk around the test rig, identify and mark them in the blank P&I Diagram provided (Figure 13.2) TSI Tank that contains dilute solution of alkali, NaOH TS2 Tank that contains a dilute solution of sulphuric acid (HzS0.) ws3 A small reaction tank 153 Downstream Tank to reduce large fluctuations in pH of the exit stream PHESI pH Electrode PHITS1 Indicating pH transmitter PHICS1 pH controller, PID PHCRS1 pH recorder PSI Metering pump for alkali PS2 Metering pump for acid PS3A Pump for mixing and feeding the acid and alkali into tank WS3 UnikKL-MICET Experiment 7 CPB 30004 ~ Process Dynamics and Control Laboratory iPS3B Recirculation pump to keep the contents of tank T53 uniformly mixed 3.2 START-UP PROCEDURES. The following steps constitute the START UP procedure. These steps must be carried out whenever you start a new experiment, 1) Make sure the tank 51 is filled with dilute solution of NaOH (0.01N). 2) Make sure the tank T'52 is filled with dilute solution of H:SOs (0.01N).. 3) The plant drainage system should be opened. 4) Close the bottom drain valves of tanks TS1, T52, T53, T54 and TSS. Also shut the bottom drain valve of W53. 5) Fill the tanks T53, T54 and W53 with water up to the level of their gravity discharge pipes (overflow pipes). 6) Important NOTE: The tanks W53 and TS4 must NEVER be empty, to preserve the analytical sensors. 7) Switch ON the mains power supply at the electrical cubicle. 8) All the pumps have their own power supply. Do not switch them on yet. 9) If there is any ANNUNCIATOR coming on, press the ACKNOWLEDGE, button to silence the buzzer. 10) Open the suction valves of all the pumps, namely, P51, P52, P53A, P53B and PS4B. 11) Switch ON the pumps P51 and P52 at the electrical cubicle and also the red STOP/START switches on the pumps also. 12) Start also the pumps P53A, P53B and P54B. 13) Check that PHICS1 is in Manual (M) mode with its MV = 100%. 14) Set the knob dials of pumps P51 and P52 at 100%. 15) _ Set the frequency in stroke per minute (spm) of both the pumps P51 and P52 as follows: Change the window display to Freq page using the ‘i’ pushbutton. Check the pump P51 display page is at “Analog, 180 freq” and the pump P52 display page is at “Manual, 100 freq”. Otherwise, reset to 100 using Up and Down arrow pushbutton. 16) Connect and regulate the air supply at the air regulators (IAS) 17) Tum the selector switch at the front of the electrical cubicle to “PANEL, SCADA”. 18) Check all the analyzer electrodes are immersed. 19) Identify the manual valves MV1, MV2, MV3 and MV4, Shut the valves MV1 and MV4. Open the valves MV2 and MV3. UniKL-MICET CPB 30004 ~ Process Dynamics and Control Laboratory eee20) 21) 22) The recorder is preset at fast speed (500 mm/Hz). To start/stop the recorder chart drive, open the swing cover and press ‘RCD’ button at the front of the recorder. The red pen represents the pH as % of 2-12 pH. Practice operating the PID controller. Lear to change the controller set point (SV), transfer from Auto (A) to Manual (M) mode and vice versa and operate the controller output (MV) manually, Learn to change the PID controller parameter values i.e., PBI %, TII sec, and TDI sec. 3.3 ANALYTICAL MEASUREMENT OF pH 1) Make sure that the start-up procedure of section 3.2 is carried out correctly. 2) Check the following: © Power supply is ON © Air supply pressure is set © The controller pHICS1 is in Manual (M) mode and its MV = 100% © Check the P/T Register page of pHICSI. P20 should be 0% always * Check the suction valves of pumps P51, P52, P53A, PS3B, P54A and P54B are fully opened. © Check the manual drain valve of all the tanks are fully shut © Check the air supply manual inlet valve located at PS4A is fully opened © Shut MV1 and MV4 and open MV2 and MV3. 3) Start pumps P53A, PS3B and PS4B. Verify there is flow in all the pumps. ‘These three pumps should be running throughout the experiment. 4) Start the pumps PS1 and P52. Make sure the pump green light is flickering. 5) Ensure the pump PS1 display “Analog, 180 + 2 Freq” and P52 display “manual, 100 Freq”. Otherwise, adjust them using the Up/Down arrow button. 6) Check the pH analyzer, pHITS1, is showing a pH value. 7) Start the recorder chart drive by pressing ON the “RCD” pushbutton of the recorder. Channel 1 (Red pen) reads pH. 8) When the analyzer reading is steady, record down the pH reading. Also record, the acid flow rate and the base flow rate in a Tabular Column. 9) Adjust the MV of the controller pHICS1 (Manual mode) and bring the pH to a steady value of about 7. 10) Stop P51 and P52 at the Start/Stop pushbuttons when the pH is about 7. Make sure the other pumps P53A, P53B and PS4B are running. 11) Again check the pH is about 7. 12) Start the alkali pump P51 at the pump Stop/Start pushbutton. Simultaneously make a mark on the chart paper (Red pen). * UnikL-MICET Experiment CPB 30004 ~ Process Dynamics and Control LaboratoryX) 2) 3) 4) UniKL-MICET ‘CPB 30004 ~ Process Dynamics and Control Laboratory Observe the chart response. There is no change in pH for sometime (Dead Time) and a sudden rise in the pH value followed by a gradual rise after pH is about 9.5. 13) Stop the pump P51 and wait for the response to become steady. 14) Now, start the acid pump P52 at the pump Stop/Start pushbutton. Make a mark on the Red trajectory of the record chart the instant the acid pump is started, Observe the chart response again. There is no change in pH for sometime (Dead Time) and a sudden fall in the pH value followed by a gradual fall below pH about 4.5. 15) Stop the pump P52 16) Extract the relevant portions of the chart recording. 3.4 PID CONTROL OF pH 1) Make sure that the START-UP procedure is followed. 2) Follow the steps (2) to (7) of Section 3.3. 3) Put the pH controller pHICS1 under Manual (M) mode. Access the PID values and set the trial values as follo PB =: 25%, TI = 60 secs, TD=15 secs Set the value for the set point SV = 7.0 Set GW1 = 0% and GGI = 1.0 for a linear controller. 4) Switch OFF the alkali pump PSI at the panel and switch ON the acid pump P52. Let the pH drop to about 4.0. 5) Note that all the five pumps are ON and the recorder chart drive is running. 6) — When the pH is just below 4, start the alkali pump P51 and switch the controller pHICS1 to Auto (A) mode. 7) Observe the PID controller response for its maximum overshoot and until it is almost steady at pH = 7.0 + 0.10 or better. 8) Attach the pH chart response as results of PID controller performance. 9) If time permits, repeat the experiment with different sets of PID controller parameters, 3.5 PID CONTROLLER TUNING USING OPEN LOOP METHOD Make sure that the START-UP procedure is followed. Follow the steps (2) to (7) of Section 3.3. To perform the open loop test, the pH value must be almost steady near its set point (pH = 7), with the controller in the Manual (M) mode. If the pH is not steady with in pH = 6.5 to 7.5, stabilize the pH by adjusting the manual control output, MV, of pHCS1. Experiment 910) When the pl is steady near its set point 7, note down the MV value of pHICS1. Mark the pH trend (Red pen) at the recorder chart and instantly step change the MY by about 10 to 20%, Note the new MV and the step change in MV. Observe patiently the pH response at the recorder, till it reaches @ new steady state, ‘Temporarily stop both the alkali and the acid pumps P51 and P52, and stop the recorder chart drive. Take out the recorder chart to analyze its open loop step response. Design the PID controller using Ziegler Nichols formula. e Draw the steepest tangent to the slope of the step response trajectory to intersect the baseline to define the dead time (DT). Using a ruler, measure intersetfnce in mim between the point of intersection and the instant when the change in MV was effected. © The dead time in time units is given by Dead Time =: Distance in mm. - 3600 sec Record chart speed, 500mm/Hr Hr «The slope ofthe steepest tangent gives the Response Rate (RR) The process gain Ky is equal to the maximum change in the pH divided by ‘the change in the manual controlled variable, MV. The time constant of the process, 7, is equal to the response rate (RR) divided by the maximum change in pH. «The controller settings by Ziegler-Nichols formulae are: 100 12 DT jo aor, f= PB% = DTxRR eee Perform steps (3) to (7) of Section 3.4 with the above designed controller parameter values. 4, RESULTS ‘The report must contain: ‘The P&I Diagram with all the major components marked. ‘A detailed report on start-up procedure. Observations made in Section 3.3 as given in Table 1: Table 1 Si. | Acid Pump, P52 Base pump, P51 pH No. at Steady state Stroke | Stroke Stroke] Stroke Digital | Chart paper length | Frequency | length _| Frequency in% UniKL-MICET Pie CPB 30004 — Process Dynamics and Control Laboratory«two portions of the pH chart records. steepest tangent against the slope of the pH chart response (Red trend) to {the time axis (the initial steady pH value). Use a ruler to measure in mm, the = between the intersection and the ‘mark’ for the start of the pump P52/P51. Chart distance in mm 3600 sec Record chart speed, 500 mnV/Hr Hr {5 dead time in seconds. sec at rising slope (due to alkali addition) sec at falling slope (due to acid addition). Submit the report along with the pH chart responses of the PID controller used in Section 3.4, Discuss on the response. © From Section 3.5, report the gain, time constant and dead time of the process. © The values of the PID controller parameters designed. © The pH chart response of the PID controller used. Discuss on the response. 5. DISCUSSIONS Based on your observation, comment/discuss on the following statements. 1) The definition of pH. 2) The pH scale runs from 0 to 14. But when you conduct the experiment, the lowest pH that you can observe with only acid is around 2 and the highest pH with only alkali is about 12. Explain the reasons why you can not go below the minimum or above the maximum pH observed. 3) State the reasons why pH control is difficult compared to any other composition control. 4) The pH reaction process presents extreme non-linearity. Discuss on this. 5) Discuss on the fail-safe mode of the control valves, UniKL-MICET Expeimen CPB 30004 ~ Process Dynamics and Control Laboratory . 4Coughanowr, D.R., Process Systems Analysis and Control, 2" Ed., McGraw Hill, 1991, 2) Seborg, Dale. B, Edgar, T.F. and D.A. Mellichamp, Process Dynamics and Control, 2" Ed., John Wiley and Sons, 2004. 3) Stephanopoulis, G., Chemical Process Control: An Introduction to Theory and Practice, Prentice Hall, 1984. 4) Luyben, W.L., Process Modelling, Simulation and Control for Chemical Engineers, 2" Ed., McGraw Hill, 1990. 5) Smith, C.A., and Coripio, B.A., Principles and Practice of Automatic Process Control, John Wiley & Sons, 1985. 6) Chemical and Analytical Process Control Training System, Model WA921, Laboratory Manual. 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