ChE 4L02

Process Control Laboratory


FALL 2005


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



Laboratory Relevance and Goals

The pH of liquids affects important process phenomena, 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 of pH dynamics and its controller tuning for a
complex cascade and multi-loop system.
• Gain experience with digital equipment for implementing the PID feedback
• 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 pH dynamics
• Feedback control using a proportional-integral-derivative (PID) 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 be asked some preliminary
questions to test your preparation. This test will be included as an
individual lab-performance in the preliminary report.
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

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 labView’s icon so that the
following diagram will appear in your computer’s 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

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.

t dCV
T dt E t E
t E K K t MV
c sense


− Ψ + ·

) (
' ) ( ) ' (
) ( ) (
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
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 Ψ(E), which is
unique to the LabView software. The term is defined in the following equation.



· Ψ
) t ( E
) 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
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 FC’s and both VC’s) 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 (VC’s 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
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.
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
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
B. The pH measurement.
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 during the
lab session. These answers should be included in your preliminary report.

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 Table
3. 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
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

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 ~100 mL/min Acid valves large 20%
small 50%
Base flow, F2 ~250 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
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
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! (It’s time to review
cascade control if it’s 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
5. A set point change of 0.50 pH units.
6. A change in the base flow rate of -30 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.

You must submit your proposed SDL goal to the instructor or TA for
approval before you begin the third week of your lab. The explanation must
be presented in the preliminary report, if not discussed and approved
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

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

Table 3. Guidance for the stirred tank heater laboratory
Timing Un-graded activity Graded activity Tasks by
Before 1st session • Read Laboratory
documentation (*)
• Review relevant
technology (**)

session • Safety training
• Equipment
• Answers to the
questions in this
• Sketch of P&ID
diagram of the
• Collect data for
dynamic models
Between 1
and 2
• Calculate model
• Complete P&I
session • Mid-lab review
• Identify a list of
SDL tasks
• Controller tuning
• Data analysis
• Draft for
session • Do your SDL task • Data analysis

• Complete SDL
∼Two weeks after 3

• Submit final

One week after the second week of each your Lab session, you must submit
a preliminary report that summarizes your experiment design, collected data
and answers to the assigned questions. The report together with the
proposed SDL experiment design is submitted to the TA and will count for
10% of your laboratory grade.
* Cover understanding of this document, relevant theory, and initial experimental plan
** Cover equipment principles, theory, and initial results from modeling experiments


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.


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 (March 2001).
Hoyle, D., Designing for pH Control, Chemical Engineering, p. 121, November 8, 1976.
Marlin, T., Process Control (2
Edition), McGraw-Hill, New York, 2000.
(or, Marlin, T., Process Control (1
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
Weaver, R., Process Piping Drafting (3
Edition), Gulf Publishing, Houston, 1986.
Woods, D., Process Design and Engineering Practice, Prentice Hall, Englewood Cliffs,

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