Chemical Engineering 4L02, PC-3: pH Control

09/05/01 Copyright 2001 by McMaster University 1

CHEMICAL ENGINEERING 4L02

PROCESS CONTROL LABORATORY
PC-3: pH CONTROL


TABLE OF CONTENTS

Section Page

I. Laboratory Relevance and Goals 2
II. Resources 2
III. Preparation Prior to the First Laboratory 2
IV. Preliminary Tasks 3
V. Initial Learning Regarding Laboratory Equipment 6
VI. Required Tasks for Modelling and Control 7
A. Empirical Model Identification and Pressure Control 8
B. Empirical Model Identification and Flow Control 9
C. pH Control 9
D. Self-Directed Learning 9
E. Summary Report 9
VII. Major Laboratory Tasks and Schedule 9
VIII. References 10







Office hours Telephone email
Instructor: Y. Samyudia J HE 336
09.00 4.00
Ext. 23273 samyudi
Teaching Assistant: J . Flores-Cerillo J HE 370B Ext. 27429 floresj
time
p
r
o
g
r
e
s
s
1 2 3 5 (number is lab session)
M id-project review
SDL Proposal
M id-project Quiz, 10%
Preliminary
Report
Full Report
submitted
Quiz on preparation
Chemical Engineering 4L02, PC-3: pH Control
09/05/01 Copyright 2001 by McMaster University 2
Process Control Laboratory on pH Control


I. Laboratory Relevance and Goals

The pH of liquids affects important behavior, such as reaction rates, vapor-liquid equilibrium, and
corrosivity. In addition, the instrumentation used in the laboratory demonstrates a range of
typical control equipment. Therefore, you will gain useful experience in process control by
working with this equipment. In addition, the required tasks for this laboratory enable you to
apply principles and practice that you learned in your process control course to a real (not
simulated) physical process.

This laboratory has the following goals, which are in addition to the general goals
presented in the course outline.

Understand instrumentation in typical control loops
Perform empirical modelling and controller tuning for a complex cascade and multiloop
system.
Gain experience with digital equipment for implementing the PID feedback algorithm
Define and perform a Self-Directed Learning investigation

II. Resources

The basic references for this laboratory are given in the References section of this document. As
you encounter questions during the laboratory, you will need to gather information from other
published material in the library, on the WEB, and from suppliers of industrial control equipment.
Naturally, you are encouraged to ask questions of the TA and instructor, but you will be expected
to search and find information available in public references.


III. Preparation Prior to the First Laboratory Session

To make the best use of your time in the laboratory, you will need to prepare before the first
session. This laboratory involves the following technologies and equipment.

Principles of pH
Empirical modelling of process dynamics
Feedback control using a proportional-integral-derivative controller in single-loop and
cascade control
Measuring pressure, flow and pH
Manipulating the opening of a control valve
Digital control

You should (1) read this document thoroughly and (2) review material on the topics highlighted
above. Your group can share the responsibility for learning these topics and teaching all other
members of the group.


Chemical Engineering 4L02, PC-3: pH Control
09/05/01 Copyright 2001 by McMaster University 3


IV. Preliminary Tasks

Before you begin performing experiments, you need to understand the equipment and how to
operate it safely. To assist you, a schematic is given in Figure 1; please note that this schematic is
far too simple to serve as a piping and instrumentation drawing. You should begin your first
session by performing the following tasks.

A. Safety Learn the safety procedures from the TA, ask questions, and complete the safety form
when you are convinced that you can operate the equipment safely and know how to
respond to likely emergencies. Note that eye protection is required in the laboratory.

B. Equipment operation The TA will instruct you on how to startup and shutdown the
equipment. The procedures are summarized in Tables 1 and 2. Please be sure that you
understand these instructions.

C. Process equipment The TA will explain the basic equipment involved in the laboratory. It
is your responsibility to understand all equipment, i.e., be able to explain the purpose and
physical principles for every element in the equipment. During the first session, you
must collect information and prepare a sketch of the equipment.




















Figure 1. Overview Display for the pH control system.
(by Andrew Poyton in 2001)
At the beginning of the first laboratory session, you will write a short quiz to test your
preparation. The quiz will constitute 5% of the laboratory grade.
You are required to provide a piping and instrumentation (P&I) diagram of the
laboratory equipment in your report. Each group needs to prepare only one
drawing; a copy of this drawing must appear in the reports from each group
members.
Chemical Engineering 4L02, PC-3: pH Control
09/05/01 Copyright 2001 by McMaster University 4

Table 1. Instructions for Starting up the pH Experiment.

1. Verify that both feed tanks contain sufficient liquid for the duration of the experiment,
which is 50L of acid and 100L of base.
2. Verify that the water inlet valves and the drain outlet valves to/from the feed tanks are
closed.
3. Open the valve on the instrument airline at the back of the equipment.
4. Open the water valve to dilute the effluent as it enters the drain.
5. Switch on the power to the experimental equipment; the orange LED will light up.
6. Open the pH Control program by double clicking the pH Control.exe icon on the
desktop. The program will load and begin to run. There is no reason to stop the
program at any time during the experiment.
7. Perform a 3-point calibration on the pH sensor using the buffer solutions provided.
8. Set both Bronco II DC drives, which control the pump speeds, on manual and
stop modes. Set the dials to about 50%. These are located at the top of the equipment
panel.
9. Make sure all controllers are in the manual mode (OFF).
10. Make changes to the valve positions to ensure they are working properly by changing
the controller outputs (both FCs and both VCs) in manual and observing the stem
positions; then, set them all to 50%.
11. Flip the switch on one of the Bronco II drives from stop to start (the switch must be
held up until the pump starts spinning). When the pump is running, flip the manual
switch to automatic, at which point the pump will stop. Repeat for the other pump.
12. Switch the pressure controllers to automatic or on, and enter the desired set point
values for each (see Table 3). Allow them to achieve steady state.
13. Adjust the acid and base large control valves (VCs outputs) to achieve nearly the
desired flow rates.
14. Close the bottom outlet valves on both tanks, and close the valve on the second
neutralization tank about halfway, so the liquid level is high enough for the probe to be
inserted. Turn on the mixers once the liquid level is at least 1 inch.
15. Clean off the pH probe with distilled water and insert it into the second tank.
16. Manually adjust both large valves (VC outputs) until you are close to the desired flows.
Then, switch both flow controllers into automatic.
Table 2. Instructions for Shutting Down the pH Experiment.

1. Place all controllers in manual or off
2. Set the pressure controller outputs (motor speeds) to zero percent.
3. After the pressures have decreased, close the acid and base large and small control
valves.
4. Switch the pumps off
5. Turn off the tank mixers.
6. Open the bottom outlet valves from both neutralization tanks.
7. Close the instrument air valve.
8. Close the water dilution valve to drain.
9. Remove the pH probe and place it in its storage medium.
10. Exit the LabView program using the x in the top right corner of the window, and turn
off the display.
11. Turn off the power to the experimental equipment; the orange LED with go off.
12. Clean the areas around the computer and experimental equipment.
Chemical Engineering 4L02, PC-3: pH Control
09/05/01 Copyright 2001 by McMaster University 5


The drawing should include the process from the feed tanks to the effluent drain. See
Austin (1979), Weaver (1986) and Woods (1995) for examples of these drawings.

D. Control equipment Sensors, displays, valves, and control calculation equipment are
essential for automatic process control. You should thoroughly understand this
equipment. As background, you can refer to the discussion of the feedback control loop
elements given in Chapter 7 of Marlin (2000) and much more detail provided in Andrew
and Williams (1979-1982).

The digital controller is based on the following continuous PID formulation.

I
dt
t dCV
T dt E t E
T
t E K K t MV
t
f
d
I
c sense
+

,
_

0
) (
' ) ( ) ' (
1
) ( ) (
with
E(t) = SP(t) CV
f
(t)
CV
f
(t) = The filtered value of the measured variable. The filter time constants are
quite fast, so that the effect is about 1-2 seconds of filtering.
K
sense
= determines the sign of the feedback; this is determined by the direct
(reverse) acting switch. (See Marlin (2000), Chapter 12)
K
C
= the controller gain. This must be positive. The units are controller
output/CV in engineering units.
T
I
= the integral time (minutes)
T
d
= the derivative time (minutes)
MV(t) = the controller output in units of (1) 0-100% if sent to a valve or (2) the
secondary CV range if sent to a secondary in cascade.

The integral mode differs from the standard algorithm by the term (E), which is unique
to the LabView software. The term is defined in the following equation.

1
]
1

+

range
2
2
SP
) t ( E
1
1
) E ( with SP
range
=Sp
max
SP
min


This term has the effect of reducing the integral mode when the error is large.

The controller is executed at a constant period of 1 second. Since this is very fast, the controller
functions essentially as a continuous controller.

Also, the data is stored at a period of 1 second. You must remember to begin data storage before
an experiment. Should you decide that the data is worthwhile, you can store in on the disk. Later,
you will be able to import the data into Excel for plotting and calculations.

You will operate the equipment using the displays provided by the LabView software. You have
an overview display that enables you to observe all key process variables and make most required
changes to process operation. In addition, you have a separate display for every controller; you
can change controller parameters, such as tuning constants, using these screens. Examples of
these displays are given in Figures 1 and 2.
Chemical Engineering 4L02, PC-3: pH Control
09/05/01 Copyright 2001 by McMaster University 6




















Figure 2. Example of a Loop Detail display for the pH control system.


E. Calibration Due to the length of this experiment, we have calibrated the sensors for you.
(You can buy Andrew Poyton a free pizza for his hard work!)


V. Initial Learning Regarding Laboratory Equipment

One of your important learning goals is to understand all elements in a control loop. Control
equipment is not perfect, so that you should understand its actual behavior and how the behavior
influences the dynamic performance of control systems. In this section, you will investigate the
behavior of individual elements before you consider the integrated control loop. To answer these
questions, you will have to review the equipment carefully, locate information in references, and
perform simple empirical tests.

A. Control valve Answer the following question about the control valve that can be
manipulated by the feedback controller.
1. What type of valve body (globe, ball, diaphragm, etc.) is used for the large acid?
Is this a good choice?
2. How much stiction and hysteresis exists in the large acid valve performance?
3. Describe the dynamic response of the large acid valve.
4. The acid flow is influenced by two valves, large and small. What is the
advantage of this approach? Why is it especially advantageous for pH control?
You are required to provide written answers to these questions in Appendix A of your
laboratory report. These answers will count for 10% of your laboratory grade.
Chemical Engineering 4L02, PC-3: pH Control
09/05/01 Copyright 2001 by McMaster University 7
B. The pH is measured.
1. What is the physical principle of the sensor? What reproducibility and accuracy
should we expect?
2. Where is the sensor located? Discuss the advantages and disadvantages for this
location.
C. Flow Measurement Acid and base flows are measured for use in flow controllers.
1. The acid and base flows are measured by sensors using different principles.
Describe the principles for each.
2. Which sensor do we expect to provide better accuracy? What is the expected
accuracy of each? What is the cost for each?


VI. Required Tasks for Process Modelling and Control

The goal of this laboratory is to develop a control system to maintain the effluent pH near its set
point. The typical operating conditions in the process are given in the following. The flow of the
base represents the product stream that must be neutralized; you are not allowed to adjust this
stream to achieve pH control. The acid flow is the utility stream that can be adjusted to achieve
pH control.

When you have completed the startup procedure, the process will be in operation near the desired
conditions in Table 3. All automatic control will be off or in manual, and the data storage
will be off.

You will perform typical tasks to

A. Determine the dynamic behavior of the system and tune the pressure controller,
B. Determine the dynamic behavior of the system and tune the flow controller
C. Implement pH control, and
D. Perform a self-directed study proposed by your group and accepted by the instructor.

However, chemical engineers should always apply their process knowledge when involved in
process operations and control. Therefore, you should review the principles of the pH process
before beginning this experiment.



Table 3. Typical operating conditions for the pH Experiment

Measurement Controller output
Acid Pressure, P1 6 psig Acid pump 50%
Base Pressure, P2 3 psig Base Pump 80%

Acid flow, F1 250 mL/min Acid vales large 20%
small 50%
Base flow, F2 500 mL/min Base valves large 55%
Small 50%
Chemical Engineering 4L02, PC-3: pH Control
09/05/01 Copyright 2001 by McMaster University 8

A. Empirical Model Identification and Pressure Control

Engineers use models, either qualitative or quantitative, for nearly every task in plant design and
operation. Since fundamental models are time consuming to develop and require data that might
not be available, we often build models based on experimental data; these are termed empirical
models. You should review/learn the process reaction curve, since you will use it in this
laboratory. When performing these experiments, manipulate the valve using the PC-based
LabView system; observe the results on the screen graphs, and save worthwhile data for later use.

1. For each flow system, determine the models between the pump speed and pressure using
the process reaction curve method.
a. Design the experiment and justify the design
b. Perform the design and evaluate the data (review 3P03 for data evaluation)
c. Estimate the model parameters and discuss the accuracy of your results

2. For each flow system, tune the feedback controller.
a. Calculate the tuning constants
b. Implement, test, and fine tune




Important Data storage

You can observe the dynamic responses on the real-time screen plots provided by the LabView
program. However, you cannot plot these directly or manipulate the data for calculations.
Therefore, we have provided the ability to save data to a file. Please remember to follow the
following instructions.

1. The data storage is initially off and will not store data until you take action
2. You can begin to store data by changing the save data switch to ON. (You should
not leave this on at all times, because you will store a very large file and you will not
be able to easily find the relevant data.)
3. After you have completed an experiment, you can stop saving data. The program will
prompt you to store the data. If you believe that the data will be useful, save the data.
We recommend that you use the .xls extension, so that the data in saved as an Excel
spreadsheet.
4. Be sure to give the file a meaningful name so that you distinguish the data from
different experiments.
5. Do not run any other programs at the same time that you are running LabView. You
can copy to a floppy if you want to use the file in Excel during the lab period.
6. You can open the Excel file and plot and perform calculations. When you save the file
after modification, BE SURE to save as an Excel spreadsheet this will require you to
change the default Save as type!
7. You should not include the data listings in your lab report. However, you must retain
the data in case the instructor has questions.

Chemical Engineering 4L02, PC-3: pH Control
09/05/01 Copyright 2001 by McMaster University 9

B. Empirical Model Identification and Flow Control

1. For each flow system, determine the models between thesmall valve and the flow, and
tune the flow controller using the same method as in (1) and (2) above.

C. pH Control

After parts A and B, we have stabilized the flows, but we have no automatic control of the
effluent pH. In this laboratory, you will implement a feedback controller to control pH by
manipulating the acid flow rate. This is a cascade design! (Its time to review cascade control if
its a little fuzzy after the summer.)

1. Discuss advantages for the cascade design.
2. Perform a process reaction curve experiments at several ranges of the effluent pH, e.g., 4,
5.5, 7, 8.5 and 10. Why would we want to investigate various operating conditions?
Compare your results with the theoretical titration curve.
3. Calculate the tuning at three conditions and explain differences.
4. Implement the pH controller and evaluate the dynamic performance for the following
changes.
a. A set point change of 0.50 pH units.
b. A change in the base flow rate of -75 liters per minute.
5. Discuss strengths and weaknesses of the control system that you have designed. These
issues should provide some ideas for the SDL exercise.

D. Self-Directed Learning

In this section, you will define a knowledge-based learning goal that is related to this laboratory.
By knowledge-based, we mean a goal directed to improving your understanding of process
dynamics and control technology (not group skills, communication skills, etc.).


Your plan should include a program of investigation to achieve the goal. The program
can include experimental, theoretical, and literature tasks; it must include some experimentation.
Prepare a clear and concise explanation of your goal and the program for investigation.

In your final laboratory report, briefly explain why you selected these goals and how you
designed the experimental program, as well as specific conclusions based on the investigations.

E. Summary Report



You must submit your proposed SDL goal to the instructor or TA for approval before
you begin this part of the laboratory. The explanation must be presented during the mid-
laboratory review (2
nd
session), if not discussed and approved earlier.
At the end of your Lab, you must submit a short report that summarizes your experiment
design and collected data to TA.
Chemical Engineering 4L02, PC-3: pH Control
09/05/01 Copyright 2001 by McMaster University 10
VII. Major Laboratory Tasks and Schedule

Guidance on the key tasks and when they should be completed is given in Table 4. Students can
rearrange some of the tasks; however, the graded activities cannot be rescheduled. Students are
encouraged to discuss topics with the TA and instructor at any time. They can propose their SDL
project before the second session, if they want.


Table 4. Guidance for PC-1 Laboratory
Timing Ungraded activity Graded activity Tasks by completion
Before 1st session Read Laboratory
documentation
Review relevant
technology
Prepare for 5%
Quiz
Experimental
plant
1
st
session Safety training
Equipment
orientation
5% Quiz on
preparation (*)
Sketch of
equipment
Collect data for
dynamic models
Between 1
st
and 2
nd
Calculate model
parameters
Complete P&I
Drawing
2
nd
session Mid-lab review
meeting
Define SDL task
5% Quiz (**) Feedback
control
experiments
3
rd
session Submit summary
report
Complete SDL
task
One week after 3
rd

session
Submit final
report

* =covers understanding of this document, relevant theory, and initial experimental plan
** =covers equipment principles, theory, and initial results from modelling experiments


VIII. References


Andrew, W. and H. Williams, Applied Instrumentation in the Process Industries, Gulf
Publishing, Houston, Volume I, 1979; Volume II, 1980; Volume III, 1982.
Austin, D., Chemical Engineering Drawing Symbols, Halsted Press, London, 1979.
Hough, M., E. Wood, and T. Marlin, Instrumentation Principles, available at
www.pc-education.mcmaster.ca (March 2001).
Hoyle, D., Designing for pH Control, Chemical Engineering, p. 121, November 8, 1976.
Marlin, T., Process Control (2
nd
Edition), McGraw-Hill, New York, 2000.
(or, Marlin, T., Process Control (1
st
Edition), McGraw-Hill, New York, 1995)
McMillan, G., pH Control, A Magical Mystery Tour, InTech, 69-76, Sept. 1984.
Vendors, Notebook on laboratory equipment available in laboratory room (Do not remove!).
Weaver, R., Process Piping Drafting (3
rd
Edition), Gulf Publishing, Houston, 1986.
Woods, D., Process Design and Engineering Practice, Prentice Hall, Englewood Cliffs, 1995.