ChE 4L02

Process Control Laboratory

pH SYSTEMS

FALL 2002



Office hours Telephone Email
Instructor: Y. Samyudia J HE 345A
9:00-4:00, M-F
Ext. 23273 samyudi
Teaching Assistant: R. Baker J HE 370B Ext. 27429 bakerr



CONTENTS


I. Laboratory Relevance and Goals

II. Preparation Prior to the First Laboratory

III. Safety and Equipment

IV. Start-up and Shut-down Procedures

V. Preliminary Tasks

VI. Process Modeling and Control

A. Empirical Model Identification and Pressure Control

B. Empirical Model Identification and Flow Control

C. pH Control

D. Self-Directed Learning

E. Summary Report

VII. Major Laboratory Tasks and Schedule

Resources

References







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 modeling and controller tuning for a complex cascade and
multi-loop system.
Gain experience with digital equipment for implementing the PID feedback
algorithm
Define and perform a Self-Directed Learning investigation


1. 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 modeling 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

You should (1) read this document thoroughly and (2) review material on the topics
highlighted above. You should review/ learn the process reaction curve method and
a statistical-based parameter estimation method, since you will use both in this
laboratory. Your group can share the responsibility for learning these topics and
teaching all other members of the group.


Before the first laboratory session, you will need to answer a short quiz to test
your preparation. The quiz will be posted in the web and constitute 5% of the
laboratory grade.
2. Safety and Equipment

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. 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.

C. Control Station
A LabVIEW-based computer control has been developed for this experiment.
You just turn on the computer and double click the pH labViews icon so that
the following diagram will appear in your computers monitor. The TA will
explain the main function of this station.















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.
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) CVf(t)
CVf(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.
Ksense = determines the sign of the feedback; this is determined by the
direct (reverse) acting switch. (See Marlin (2000), Chapter 12)
KC = the controller gain. This must be positive. The units are
controller output/ CV in engineering units.
TI = the integral time (minutes)
Td = 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 SPrange = Spmax SPmin

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.





















3. Start-up and Shut-down Procedures

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.


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. After determining the controller parameter, 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.
4. Preliminary Tasks

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.
5. What type of valve body (globe, ball, diaphragm, etc.) is used for the large
acid? Is this a good choice?
6. How much stiction and hysteresis exists in the large acid valve
performance?
7. Describe the dynamic response of the large acid valve.
8. 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?
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?

You are required to provide written answers to these questions after the first
lab session. These answers will count for 5% of your laboratory grade.

5. Process Modeling 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

i. Determine the dynamic behavior of the system and tune the pressure
controller,
ii. Determine the dynamic behavior of the system and tune the flow controller
iii. Implement pH control, and
iv. 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.



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

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%
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.

B. Empirical Model Identification and Flow Control

For each flow system, determine the models between the small 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.
5. A set point change of 0.50 pH units.
6. A change in the base flow rate of -75 liters per minute.
7. 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.

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.
E. Summary Report



3. 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 pH-system laboratory
Timing Ungraded activity Graded activity Tasks by completion
Before 1st session Read Laboratory
documentation
Review relevant
technology
5% Quiz on
preparation,
which is posted
in the web (*)
Prepare for 5%
Quiz
Experimental
plant
1
st
session Safety training
Equipment
orientation
5% Quiz as the
answers to the
questions in this
module
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 (**)
5% Mid-Lab
Review
Feedback control
experiments
3
rd
session 5% summary
reports
Complete SDL
task
One week after 3
rd

session
Submit final
report

* Cover understanding of this document, relevant theory, and initial experimental plan
** Cover equipment principles, theory, and initial results from modeling experiments







At the end of each your Lab session, you must submit a preliminary report
that summarizes your experiment design and collected data. The reports (3
preliminary reports for 3-lab sessions) are submitted to the TA and will
count for 5% of your laboratory grade.
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.


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.