Unit Operations II Lab Manual - 2019

An-Najah National University
Chemical Engineering Department

Unit Operation 2 Laboratory (10626468)
Instructor:
Dr. Abed Al-Raheem Abu Safa

Dr. Husni Odeh
Eng. Majd Shhade
Eng. Maha Fuqha
1
Preface:
In view of the increase emphasis placed on safe, efficient plant operation, it is only natural that
the subject of process control has become increasingly important in recent years. Without
computer- based process control system it would be impossible to operate modern plants safely
and profitably while satisfying product quality and environmental requirements. Thus, it is
important for chemical engineering to have an understanding of both the theory and practice of
process control.
The primary objective of process control is to maintain a process at the desired operating
conditions safely and efficiently.
Set of process control experiments will be studied in this lab. The study of these experiments will
strengthen the understanding of process control and will aid the students to be more familiar with
the practical process control operations.
The manual presents detailed descriptions of experiments. The arrangement and organization
provide a convenient means of giving instruction on handling the equipments. The use of the
equipments is not limited to the experiments described; the instructor can feel free to make
variations. Moreover, the manual presents guidelines for preparation of laboratory reports.
The author is grateful to his students, namely: Mrs. Wisal Khderat, Mrs. Aseel Qafaf at An-
Najah National University and Eng. Azza Abu Asab, who helped in typing this manual
2
Table of content
Preface
Instruction for Preparing the Laboratories Report
Safety Regulations
pH Control
Pressure Control
Flow Control
Temperature Control
Level Control
Distillation Control
Tunning
Dynamics of stirred tanks
Simulink
Gas absorption
Liquid Liquid Extraction
Distillation
Evaporation
Solid Liquid Extraction
Steam distillation
3
Department of Chemical Engineering
Unit Operations Lab. II (10626468)
Total Credits 1
major compulsory
Prerequisites P1 : Unit Operations Lab. I (10626339) OR Unit Operations (10626362)
Course Contents
This Lab course provides chemical engineering students with a unique opportunity to apply the principles
learned in the unit operation and process control courses. Skills for accurate data collection, analysis and
communication are developed
Student Outcomes
Intended Learning Outcomes (ILO's) Contribution
(SO's)
1 Design& conduct experiments, as well as to analyze & interpret data B 70 %
obtained when conducting experiments.
2 Communicate effectively by writing technical reports about each G 10 %
conducted experiment in unit operation lab.
3 Use the techniques, skills & modern engineering tools necessary for K 10 %
engineering in order to present and calculate the operational parameters
based on experimental data of equilibrium using excel spread sheets
and related software.
4 Show An understanding of professional & ethical responsibility during F 10 %
performing the experiments and in writing the reports.
Textbook and/ or Refrences
Text book: Laboratory manuals
References:
1- C.J. Geankoplis, Transport processes and unit operation, 3rd Edition.
2- Seborg D.E., Edgar T.F., and Mellichamp D.A., Process Dynamics and Control, Wiley, 2004.
3- Robert E. Treybal, 3rd Edition, Mass transfer operations McGraw-Hill Book Company
Assessment Criteria Percent (%)
Reports 35 %
Laboratory Work 15 %
Final Exam 50 %
Course Plan
Week Topic
1 Introduction to laboratory, safety of used materials and equipment
2 Hydrodynamics measurements on packed column, dry column and water/air system
3 Gas absorption experiments
4 Batch distillation
6 Liquid/liquid extraction Experiments: distribution coefficient
7 Basic operation of liquid /liquid absorption column.
8 Midterm examination
4
9 Level control
10 Pressure control
11 Temperature control
12 Flow control
13 pH control
14 controller tuning
15 control configuration of distillation column control
16 Final examination
5
Instruction for Preparing the Laboratories Report
The formal report must be prepared according to the following outline:
Evaluation Criteria Grade

Abstract
answers of the questions: “What did you do? How did you do it? What did you 15
find?”
Introduction and theory
Sufficient,Clear and complete statement of objectives. 10
Procedure
Procedure sufficiently described. 5
Description of Appartus
main items, how it work 5
Experimental Results
Results analyzed correctly. Experimental findings adequately and specifically 20
summarized, in graphical, tabular, and/or written form.
Discussion
Crisp explanation of experimental results. Comparison of theoretical
predictions to experimental results, including discussion of accuracy and 20
error analysis in some cases.
Conclusions and Recommendations
Conclusions summarize the major findings from the experimental results
with adequate specificity. Recommendations appropriate in light of 4
conclusions. Correct grammar.
References and Nomenclature
Complete and consistent bibliographic information that would enable the 2
reader to find the reference of interest.
Appendices
Appropriate information, block diagram and sketch of the control loop 10
Appearance
Title page is complete, organization and neatness. 9
Total
100
6
1. Title Page
The title page should be separate from the rest of the report. It should contain:
a. The name of the experiment
b. The name of the course
c. The date when experiment was done
d. The name of the writer and his/her co-worker, ID number, and his/her group
number
e. The name of the instructor to whom the report is submitted
f. The date of submission report
2. Abstract
The abstract should be informative, and should be written in about three to five sentences. It
should over all phases of investigation. It must include the following:
a. An introductory statement about the subject matter

b. Briefly describe what was done
c. Present some selected results (numerical values, if possible)
d. If possible, present some percentage errors in experimental results in comparison
with theoretical values.
While writing the abstract, it should be kept in mind that you should not refer to any graph and
table.
3. Theoretical Background
This section should include the theory behind the experiment. It should also contain all those
equations, which are used to acquire a certain result. Theoretical correlation, which is used for
comparison with experimental results, should also be included.
4. Procedure
Here, you should briefly describe the actual step by step procedure you followed in running the
experiments and form the theoretical knowledge. It should be written in your own words.
5. Description of apparatus
This section should include a brief description of apparatus used in the experiment, include its
principle and application.
7
6. Results
The results should be presented in the form of tables and/or graphs. The tables should contain the
results obtained from experiments and from theoretical knowledge. Comparison should be
presented in terms of percentage, e.g. percent deviation.
7. Discussion of Results
In this section you should discuss your experimental results. Show how you make comparison
with the values obtained theoretically. Also discuss the deviation of experimental results from
theoretical values. The possible source of errors should be mentioned. If the results are obtained
in terms of graphs, then interpret them.
8. Conclusion and Recommendation
Conclusions are the series of numbered sentences, which answer the questions posed in the end
of each experiment. Conclusions should also include the errors between the experimental and
theoretical values. What you have learned from the experiment should be mentioned as well.
Recommendations are the proposals for future work, e.g. suggested changes in equipment, study
of new variables, or possible experiments in relative fields. Like the conclusions, numbers
usually lists the recommendations, and each consists of only a sentence or two.
9. Literature cited
Here, you should list books, journals, articles, etc. used in writing your report and analyzing the
experiments. The reference should be completed (name of the book, author, volume, date of
publications, pages, etc.) References should be arranged alphabetically.
10. Nomenclature
The symbols, which are used in the report, should be defined in the nomenclature in alphabetical
order. The accompanying definitions must include proper units.
11. Appendices
All appendices and graphs should be attached at the end of the report.
12. Organization and Neatness
The students must organize their reports in a manner earlier. It is required/encouraged to use
EXCEL, any available graphics software packaged to draw graph. The neatness will include how
the students has written the report.
8
Safety Regulations
1. Wear suitable lab coat, suitable gloves and safety glasses or goggles should be worn
whenever there is potential for contact with particulate debris, dust or corrosive or toxic
materials.
2. Confine long hair and loose clothing when in the laboratory.
3. Know the location of the fire extinguisher, eye wash, safety shower and first aid kit in
your lab and know how to use them.
4. Determine the potential physical and chemical hazards, and the safety precautions that
apply to your apparatus before beginning.
5. No unauthorized laboratory work should be carried out in the absence of the instructor.
6. Never leave unattended an experiment that is in progress.
7. Review the safety and health hazard data of all chemicals used in the laboratory.
8. Notify your instructor immediately after any injury, fire or explosion, or spill.
9. If chemicals come into contact with your skin or eyes, flush immediately with copious
amounts of water and consult with your instructor.
‫قواعد السالمة المهنية في مختبر التحكم بالعمليات‬

.‫يجب استخدام المالبس الواقية والنظارات والكمامات أثناء تشغيل األجهزة‬ -1
.‫تعرف على أماكن مغسلة العيون والدش وطفاية الحريق قبل البدء باي عمل داخل المختبر‬ -2
.‫قبل استخدام أي جهاز يرجى قراءة التعليمات الخاصة به بدقة واإلنتباه الى إشارات السالمة الخاصة بالجهاز‬ -3
.‫يمنع تشغيل األجهزة داخل المختبر دون الرجوع للمشرف‬ -4
.‫ يرجى قراءة تعليمات السالمة الخاصة بالمادة بدقة‬،‫في حالة استخدام أي مادة كيماوية‬ -5
.‫ يجب غسل المنطقة المصابة بالماء باستخدام مغسلة العيون أو الدش‬،‫في حالة مالمسة أي مادة كيماوية للجسم أو العيون‬ -6
:‫أنتبه‬
.‫معظم األجهزة تحتوي أسطح ساخنة‬ •
.‫ال تعبث بالمحابس والوصالت‬,‫يوجد أجهزة تعمل بضغط هواء مرتفع‬ •
9
II. Safety Regulations in Unit Operation Lab.
1. Wear lab coat in the laboratory, and wear gloves, safety glasses or goggles whenever
you work require it. as in the case of contact with particulate debris, dust or
corrosive or toxic materials.
2. Confine long hair and loose clothing when you are in the laboratory.
3. Know the location of the fire extinguisher, eye wash, safety shower and first aid kit in
your lab and know how to use them.
4. Determine the potential physical and chemical hazards, and the safety precautions
that apply to your apparatus before beginning.
5. No unauthorized laboratory work should be carried out in the lab, and don’t start
the any work with the absence of the instructor.
6. Never leave unattended an experiment that is in progress.
7. Review the safety and health hazard data of all chemicals used in the laboratory.
8. Notify your instructor immediately after any injury, fire or explosion, or spill.
9. If chemicals come into contact with your skin or eyes, flush immediately with
copious amounts of water and consult with your instructor.
‫قواعد السالمة المهنية في مختبر وحدات صناعية‬

.‫ يجب استخدام المالبس الواقية والنظارات والكمامات أثناء تشغيل األجهزة‬-1
10
‫تعرف على أماكن مغسلة العيون والدش وطفاية الحريق قبل البدء بأي عمل داخل المختبر‪.‬‬ ‫‪-2‬‬
‫قبل استخدام أي جهاز يرجى قراءة التعليمات الخاصة به بدقة واالنتباه إلى إشارات السالمة الخاصة بالجهاز‪.‬‬ ‫‪-3‬‬
‫يمنع تشغيل األجهزة داخل المختبر دون الرجوع للمشرف‪.‬‬ ‫‪-4‬‬
‫في حالة استخدام أي مادة كيماوية‪ ،‬يرجى قراءة تعليمات السالمة الخاصة بالمادة بدقة‪.‬‬ ‫‪-5‬‬
‫في حالة مالمسة أي مادة كيماوية للجسم أو العيون‪ ،‬يجب غسل المنطقة المصابة بالماء باستخدام مغسلة العيون أو الدش‪.‬‬ ‫‪-6‬‬
‫يجب أخذ االحتياطات الالزمة أثناء تشغيل جهاز ‪ Liquid Extraction‬الحتوائه على مواد سامة وخطرة‪.‬‬ ‫‪-7‬‬
‫أنتبه‪:‬‬
‫يوجد أجهزة توليد بخار ذات ضغط وحرارة مرتفعة‪ ،‬ال تعبث بالمحابس والوصالت‪.‬‬ ‫•‬
‫معظم األجهزة تحتوي أسطح ساخنة‪.‬‬ ‫•‬
‫هناك أبخرة وغازات متصاعدة من األجهزة قد تكون سامه أو قابله لالشتعال‪.‬‬ ‫•‬
‫يمنع استخدام اللهب المباشر في عمليات التسخين‪.‬‬ ‫•‬
‫‪11‬‬
Part one
Control lab
12
Exp # 1
pH Control
1.1- THEORITICAL BACKGROUND:
pH control is a common issue in many industrial processes. The basic idea to control the pH
variations in some liquid flow, usually making the pH as close to 7 as possible. This influent
liquid flows into a tank, where it is mixed with an amount of a concentrated reagent to alter its
pH. If the effluent is acidic with a pH of 4, the reagent would be basic with a pH larger than 10.
The reagent is more concentrated than the effluent, since it is desirable to as little volume to the
effluent as possible.
The pH is controlled in a tank - the iffluent flows into the top of the tank, and the reagent is also
added to the top of the tank. The tank is well-stirred so that the pH is uniform throughout the
tank. The effluent is pumped out the bottom of the tank, as shown in the figure below.
Figure 1.1
Note that pH is a very difficult control problem due to the non-linearities. This example
simplifies the problem somewhat to highlight some points about control system design in
general.
13
From elementary mass balance considerations, it can be shown that an appropriate state space
model for the strong acid-strong base system is
………………. (1)
Where
Co(t) : excess hydrogen ion concentration in the effluent stream (mol/L)

Cu(t) : excess hydrogen ion concentration of the reagent (mol/L)
Ci(t) : excess hydrogen ion concentration in the influent stream (mol/L)
u(t) : flow rate of the reagent (L/s)
q(t) : flow rate of the influent stream (L/s)
V : volume of the tank (L)
Normally, the reagent concentration is constant, and we control the effluent pH by varying the
reagent flow. Note that the concentrations are excess concentrations, meaning that they measure
the concentration of hydrogen ions in excess to that found in water. We can convert an excess
concentration C to pH using the following formula.
……………………………. (2)
From this formula, we can see that an excess concentration of 0 gives a pH of 7 (which is the pH
of water, as expected). Also, negative excess concentrations correspond to basic pH, and positive
excess concentrations correspond to acidic pH.
NOTE: The reader should already be aware that if a weak acid or weak base is used, the titration
curve will be substantially different. The differential equation (1) represents the dynamic
equation for a strong acid-strong base titration curve. For any other acid-base combination (e.g.
weak acid-strong base), the system model will be substantially different, as will equation (2) for
finding concentration from pH. The graph below shows the titration curve for a strong acid-
strong base system.
14
Figure 1.2 The titration curve for a strong acid-strong base system
1.2- TECHNICAL CHARACTERISTICS
Figure 1.3 pH control system
15
• AISI 304 stainless steel framework
• Electronic pH transmitter, range 0-14 pH, 4-20 mA output signal, code pHT1 ( n° 1)
• 2 gear pumps, AISI 316 stainless steel execution, code G1 and G2 (n° 12)
• 2 variable area flow meters, glass and stainless steel execution, range 0-20 l/h, code FI1 and
FI2 (n° 3 and 6)
• Microprocessor PID controller, 4-20 mA input and output signals, accuracy ± 0.1%, complete
with serial card RS 232 ( n° 9)
• 2 AISI 316 stainless steel feed tanks, capacity 13 liters, code D1 and D2 ( n° 2)
• AISI 316 stainless steel collection tank, capacity 26 liters, code D3 (n° 7)
• AISI 316 stainless steel reactor complete of 0÷600 rpm variable speed stirrer (n° 4), capacity 3
liters, code R1 (n° 5)
• AISI 316 stainless steel connection lines and valves
• 2 measurement terminals for the 4-20 mA signal at the controller input (n° 10)
• 2 measurement terminals for the 4-20 mA signal at the controller output (n° 11)
• Electrical supply light (n° 8)
• Painted carbon steel electrical board with synoptic of the plant and E.L.C.B.
1.3- OPERATING PRINCIBLE

In this unit, the PID control is carried out on the pH inside the reactor R1. The control device
consists in the pump G1 that, according to the signal coming from the PID controller, adjusts the
flow rate of the basic solution at the input of the reactor and consequently the pH.
The flow rate of the acid solution is fixed adjusting the flow rate of the pump G2.
The control loop can be described as follows: the electronic transmitter, pHT1, measures the pH
in the reactor R1 and sends the PID electronic controller a 4-20 mA electrical signal proportional
to 2 - 12 pH.
In practice (Fig. 1.4):
- If the pH = 2, the output signal from the transmitter is 4 mA (zero).
- If the pH = 12, the output signal from the transmitter is 20 mA.
- For intermediate values the output signal from the transmitter will be proportional to pH; e.g. at
pH = 7 the output signal from the transmitter will be equal to 12 mA.
16
Figure 1.4
The signal sent by the transmitter pHT1 to the PID controller is compared to the set point value
set on the controller. A this point, the controller sends a 4-20 mA signal to the output, function
(PID) of the shift between the value of the process variable and the set point. This electrical
signal is converted by an electronic card into voltage so that it controls the rpm (and so the flow-
rate) of the pump G1.
Fig. 1.5 shows the proportionality between the electrical output signal of the PID controller and
the rpm of the pump G1.
Figure 1.5
17
The 4-20 mA signals at the input and output to the PID controller can be measured with a
milliammeter using the proper terminals set on the board.
The controller is pre-set in PI mode (proportional + integrative + derivative).
1.4- INSTALLATION
• Shut off the valves V1, V2, V3, V4, V5, and V6
• Connect the electrical board to the single-phase + G electrical line (n° 1)
• Connect the plant to the serial port COM1 of the P.C. with the serial cable (n° 2)
• Insert the E.L.C.B. (n° 3)
1.5- STOP
- Switch the selectors of G1, G2 and M1 in position “0”
- Drain the tanks and all the lines of the plant
- Wash using distilled water tanks, reactor and all the lines of the plant
- Insert the pH electrode in the protection cap filled with buffer solution at pH = 7
1.6- EXRECISE
• Set:
Gain = 0.5
I = 0.5 min
D = 0.0 min
• Set the set point to the 50% (pH = 7)
• The process variable will reach the set point value with regular behaviour. This indicates that
the Gain and integrative time values are valid (Figure 1.6)
18
Figure 1.6
• Try to increase the flowrate of acid solution increasing the output of 2nd loop to 30%
• Consequently, the output of 1st loop increase (from 20% up to 35%) and the process variable
will reach the set point value with regular behavior At this point, you can carry out a test
excluding the integrative action or the derivative action.
1.7- SAFETY
• During the experiments, take care in wearing the necessary protections:

- laboratory coat
- goggle
- laboratory glove
• Before any maintenance operation, disconnect the plant from the electrical mains.
19
Table1 RAW DATA SHEET
Time (sec) Process Variable Set Point Gain Integral Derivative
20
Exp #2
Pressure Control
2.1- INTRODUCTION
The unit enables to study the automatic pressure control using a line provided with a tank, a
control valve, a pressure transmitter and a PID controller.
The line is pressurized using compressed air. The plant is provided with specific supervision
software, Mod. SWPCB/EV, that enables the use from P.C. The bench can be connected in series
with Mod. FCB/EV.
Figure 2.1
21
Fig. 2.2
• Pneumatic control valve, AISI 316 stainless steel execution, DN 15, Cv = 2.3, code PV1 (n° 1)
• Electronic pressure transmitter, AISI 316 stainless steel execution, range 0÷6 bar, output signal
4÷20mA, code PT1 (n° 3)
• AISI 304 stainless steel tank, code D1 (n° 4)
• PID microprocessor controller, input and output signals 4÷20mA, accuracy ±0.1%, complete
with serial card RS 232 (n° 6)
• Electropneumatic converter, 4÷20mA/0.2÷1 bar (inside the switchboard)
• Safety valve calibrated at 9 bar (n° 10)
• AISI 304 and 316 stainless steel connecting lines and valves
• Bourdon spring pressure gauge, range 0÷6 bar (n° 2)
• Pressure gauge 0÷2.5 bar on switchboard
• Power supply light (n° 7)
22
• 2 measurement terminals for the 4-20 mA input signal of the controller (n° 8)
• 2 measurement terminals for the 4-20 mA output signal of the controller (n° 9)
• Plastic silencer (n°5)
• Painted carbon steel electrical switchboard complete with synoptic of the plant and E.L.C.B.
2. 3- OPERATING PRICIBLE
In this unit, the PID control is carried out on the air pressure inside the piping with possibility to
insert a capacity into the circuit consisting in the tank D1. The control device consists in a
pneumatic valve that, according to the signal coming from the PID controller, adjusts the
compressed air flow rate at the system’s input. The electronic transmitter PT1, measures the
pressure in the line and sends an electrical signal 420 mA to the PID electronic controller
proportional to 06 bar. In practice (fig. 2.3):
- If the pressure is null, the output signal from the transmitter is 4mA (zero).
- If the pressure is 6 bar, the output signal from the transmitter is 20 mA.
- For intermediate pressure values, the output signal from the transmitter will be proportional to
the pressure; e.g. at 3 bar, the output signal from the transmitter is 12mA.
Fig. 2.3
The signal sent by the transmitter PT1 to the PID controller is compared to the set-point value set
on the controller. At this point the controller sends a signal 4-20 mA to the output, function
(PID) of the shift between the value of the process variable and the set-point. Such electrical
23
signal is converted by an electropneumatic converter into pneumatic signal controlling the
opening level of the valve.
The following graphs show:
• Fig. 2.4: the proportionality between the electrical output signal of the PID controller and the
pneumatic output signal of the electropneumatic converter (I/P).
Fig. 2.4
•Fig. 2.5: the proportionality between the output signal of the electropneumatic converter (0-2-
1 bar) and the opening level of the valve (0-100%).
Fig. 2.5
24
The signals 4−20 mA and the input and output of the PID controller can be measured with a
milliammeter using the proper terminals set on the board. The pneumatic signal at the output of
the I/P converter can be read directly on the pressure gauge set on the board.
The controller is set at the factory to PI mode (proportional + integrative) as in the pressure
control the derivative action is generally not used.
2.4- INSTALLATION
• Shut off valves V1, V2, V4 and V6.

• Open valve V3 and partially valve V5.
•Connect the electrical board to the electrical mains (n° 2)
• Connect the electrical board (n° 1) to the compressed air line with the provided pipe
(complete with quick connections); the air pressure must be at max. 1.5 bar and not less than 1.2
bar.
• Connect the valve V1 to the 6 bar compressed air line (n° 5).
• Connect the plant to the serial port COM1 of the P.C. with the proper serial cable (n° 3).
• Insert the E.L.C.B (n° 4).
2.5- STOP
• Shut off valve V1

• Switch off the E.L.C.B.
•Depressurize all lines through valve V5.
25
2.6- EXERCISE
• Set:
Gain= 1.0
I=0.5 min
D=0
• Set the set-point to the 40% (approx. 2.40 bar, full scale 6 bar).
• The process variable will reach the set-point value with regular behavior. This indicates the
Gain and Integrative time (I) values are valid.
Figure 2.6
In the pressure control, the derivative time must be null, i.e. the controller operates in PI mode
(the controller is programmed in PI mode); the derivative time introduction, in fact, gets the
regulating action worse.
• Increase the gain to 3
• Disturb the system setting the set-point to the 50% (or by shutting or opening valve V5).
• You can note that, with the set gain value, the pressure control is impossible.
However, inserting the tank D1 into the circuit (the volume of the system increases noteworthy),
there is a quick softening of the oscillations until the set-point value is reached. The tank D1
26
substantially acts as shock absorber). At this point a test can be carried out excluding the
integrative action,
• Set:
• Gain = 1.0
• Set the set-point to the 40% (approx. 2.40 bar considering that the full scale is 6 bar).
• The process variable will get near the set-point value never reaching it: a constant shift in time
called OFF SET will remain.
2.7- SAFTY
• Before any maintenance operation, disconnect the system from the electrical supply.
• Use compressed air at the maximum pressure of 6 bar as process fluid.
27
28
Exp #3
Flow Control
3.1- INTRODUCTION
The unit Mod. FCB/EV can be used to study the automatic flow-rate control through the typical
system composed of calibrated diaphragm, control valve, differential pressure transmitter and
PID controller. The process fluid can be water or air. The system is provided with a specific
supervision software, mod. SW – FCB/EV, that provides the P.C. control. The bench can be
connected in series with Mod. PCB/EV or in parallel
to the other automatic control units (Mod. LCB/EV and TCB/EV).
Fig. 3.1
29
• Pneumatic control valve, AISI 316 stainless steel execution, DN 15, Cv = 2.5, code FV1 (n° 4)
• Electronic differential pressure transmitter, range 0-1000 l/h of water and 30 Nm3/h of air,
transmitter calibration 0-500 mmH2O, 4- 20 mA output signal, code FT1 (n° 3)
• Variable area flow meter, range 100-1000 l/h, code FI2 (n° 2)
• Calibrated diaphragm, AISI 316 stainless steel execution, d = 10.9 mm (n° 11)
• Microprocessor controller, PID type, 4-20 mA input and output signals, accuracy ± 0.1%,
complete with serial card RS 232 (n° 6)
• Electropneumatic converter 4-20 mA/0.2-1 bar (inside the swtichboard)
• Bourdon spring pressure gauge, range 0-6 bar (n° 1)
• AISI 304 and 316 stainless steel valves and connection lines
• Safety valve, calibration at 9.3 bar, code PSV1 (n° 12)
• Silencer in plastic material (n° 5)
• Pressure gauge, 0 - 2.5 bar (n° 10)
• 2 measurement terminals for the 4-20 mA signal at the controller input (n° 8)
• 2 measurement terminals for the 4-20 mA signal at the controller output (n° 7)
• Power supply light (no. 9)
• Painted carbon steel electrical board with plant synoptic and E.L.C.B.
The operating principle of the equipment can be described as follows.

The fluid, crossing the calibrated diaphragm, causes a pressure drop
proportional to the flow rate.
The phenomenon is described by the following equation:
30
where:
Δp = pressure drop on the diaphragm
A1 = pipe section
A2 = calibrated hole section
ρ = fluid density
In case of turbulent motion of the fluid, the last equation is written as follows:
Where Cd is the discharge coefficient and ranges between 0.6 (turbulent flow) and 1 (laminar
flow). The electronic transmitter FT1 measures the pressure drop Δp (in mmH2O), extracts the
square root of the measured value, and sends the PID electronic controller a 4-20 mA electrical
signal proportional to √Δp and so to the flow rate.
In practice (Fig. 3.2):
- If the flow is null (Δp = 0, Q = 0 l/h,) the output signal to the transmitter is 4 mA (zero).
- If the flow rate is maximum (Δp = 500 mmH2O, Q = 1000 l/h,) the output signal to the
transmitter is 20 mA.
- For intermediate flow rate values, the output signal from the transmitter will be proportional to
the flow rate; e.g. at 500 l/h the output signal from the transmitter will be equal to 12 mA.
31
L/h
Fig. 3.2
The signal sent by the transmitter FT1 to the PID controller is compared to the set point value set
on the controller. At this point, the controller sends the output a 4-20 mA signal, function (PID)
of the shift between the value of the process variable and the set
point. This electrical signal is converted by an electropneumatic converter into a pneumatic
signal controlling the valve opening degree. The following graphs report:
Fig. 3.3: the proportionality between the electrical signal at the output of the PID controller and
the pneumatic signal at the output of the electropneumatic converter (I/P).
Fig. 3.3
32
Fig. 3.4: the proportionality between the output signal of the electropneumatic converter (0.2-1
bar) and the valve opening degree (0- 100%).
Fig. 3.4
The 4-20 mA signal at the input and output of the PID controller can be measured with a
milliammeter using the proper terminals (Fig. 3.1 – no.7 and 8) set on the board.
The output signal to the I/P converter can be read directly on the pressure gauge (Fig. 3.1 – no.
10) set on the board. The controller is pre-set to PI mode (proportional + integral) as the
derivative action is not generally used in the flow rate control.
3.4- INSTALLATION
• Shut off the valves V1, V2, V3, V4, V6 and V7

• Open the valve V5
• Connect the electrical board to the single-phase + G electrical supply (Fig. 3.1 – n° 2)
• Connect the electrical board to the compressed air line using the provided pipe (complete with
quick connections); the air pressure must be at max. of 1.4 bar (Fig. 3.1 – n° 1) and not less than
1.2 bar.
• Connect the installation to the water line with the provided rubber pipe (Fig. 3.1 – n° 4) using
metal hose clamps to fix it to the hose connector; the line water flow rate must be about 1000 l/h
33
• In case air is to be used as process fluid, connect the system to the compressed air line at 6 bar
through the valve V2 (Fig. 3.1 – n° 5) using the proper provided pipe (complete with quick
connections).
• Connect the plant to the serial port COM1 of the P.C. with the serial cable (Fig. 3.1 – n° 3)
• Connect the valve V5 to a drain by means of a rubber pipe (Fig. 5.2)
• Insert the E.L.C.B.
3.5- STOP THE SYSTEM
• Shut off the valve V3

• Disconnect the E.L.C.B.
In case of long period of inactivity:
• Open the exhaust valve V5, the valve V7, the valve FV1 and the valve V1
• Drain the line
3.6- EXERCISES
Process fluid: Water

• Set:
Gain = 0.2
I = 0.3 min
D=0
• Set the set point to the 50% (500 l/h about, full scale 1000 l/h) (Fig.3.5)
• Wait until the process variable reaches the set point value.
34
Fig. 3.5
• Wait until the process variable reaches the set point value. As you can note, the gain and
integrative time values are valid. In the flow rate control, the derivative time must be null, i.e. the
controller operates in PI mode; the introduction of the derivative time, in fact, makes the
controlling action worse.
• Perturbate the system by closing and opening the valve V5
• You can note that the flow rate control is impossible with the set gain value.
Process fluid: Air
• Set:
Gain = 0.2
I = 0.3 min
D=0
• Set the set point to the 50% (full scale 30 Nm3/h about)
35
Fig. 3.6
• Wait for the process variable to reach the set point value.
Fig. 3.7
36
• Set the controller with the single action P and take the set point to the 30%.
Fig. 3.8
As you can note, in absence of integrative action there is a permanent off–set of the process
variable in respect to the set point.
3.7- SAFETY
• Before any maintenance operation, disconnect the plant from the electrical mains.
• In case compressed air is used as process fluid, keep the valve V3 always closed.
37
38
Exp #4
Temperature Control
4.1- INTRODUCTION
General guidelines for temperature control loops are difficult to state because of the wide
variety of process and equipment involving heat transfer and there different time scales. For
example, the temperature control problems are quite different for heat exchangers, distillation
columns, chemical reactors and evaporators. The presence of time delay and/ or multiple thermal
capacitances will usually place a stability limit on the controller gain. PID controllers are
commonly employed to provide more rapid response that can be obtained with PI controllers.
Heat exchanger is good examples for temperature control, figure (1) illustrate a set up of the heat
exchanger. It is required to heat the process fluid to a specific temperature (T2) by adjusting the
inlet flow rate of the steam. If the out let temperature of the process fluid decreases then the
temperature transmitter will measure it and send an electrical signal to temperature controller
that will compute the error and give appropriate action to inlet steam valve. Finally steam flow
will increase and inherently T2 will increase.
TT TC
Figure 4.1
39
Fig. 4.2

• Pneumatic control valve, AISI 316 stainless steel execution, DN 15, Cv = 0.13, code TV1 (n°
2)
• RTD Pt100 with AISI 316 stainless steel sheath, code TT1 (n° 8).
• Microprocessor controller, PID type, 4-20 mA output signals, accuracy ± 0.1%, complete with
serial card RS 232 (n° 6)
• Electropneumatic converter 4-20 mA/0.2-1 bar (inside the switchboard)
• AISI 304 and 316 stainless steel connection lines and valves
• Pressure gauge 0 - 2.5 bar (n° 4).
• Electrical supply light (n° 5)
• Painted carbon steel electrical board with synoptic of the plant and E.L.C.B.
40
In this unit, the PID control is made on the output temperature of the hot current coming from the
plate heat exchanger E1. The control device consists in a pneumatic valve that, according to the
signal coming from the PID controller, adjusts the cold current flow-rate.
The temperature measurement is carried out by means of an RTD which operating principle can
be summed up as follows. The electrical resistor of a conductor generally increases with the
temperature, so from the resistor measurement, obtained with a bridge
circuit, you can find out the temperature of the ambient with which a resistor is in thermal
balance. The instruments of this kind have the double advantage to be very accurate and very
simple and are used in industrial devices with direct reading as well as in temperature
measurements with the maximum accuracy (in these cases a wire of pure platinum is used as
resistor, in the temperature range between —258 °C and 900 ºC).
The RDT is composed of a very thin metal wire, wound around a small porcelain cylinder and
included into an insulating sheath. The wire, that represents the thermometric substance, is
connected to a proper electrical circuit created to provide a measurement of the resistance with
the maximum accuracy. The RTDs are indicated according to the atomic element that constitutes
the wire and according to the zero degree resistance; e.g., the most used ones are the Pt100:
platinum RTDs from 100 to 0°C. 4 wires normally exit from the RDT: two primaries for the
current and two secondaries for the voltmeter.
The relation that enables to measure the resistance from the temperature is:
where R0 is the resistance of the material at 0°C and  is a coefficient the most common values of
which we report on a table:
41
Qualities:
• It is a stable instrument so it is always precise and quite accurate;
• It is strong;
• It changes very slowly in time and so it must not be calibrated continuously;
• It has an electrical output, for this reason, it is particularly recommended for industrial accuracy
measurements.
42
Defects:
• It is quite expensive;
• It needs auxiliary instruments;
•The heating by Joule effect can be consistent (the dissipated heat is
• It has a thermal inertia as it is not too small (it is more proper for industrial uses). The RTD
TI1 measures the temperature and sends the electronic PID controller a signal in Ohm
proportional to it.
• If the temperature is 0 degrees, the signal of the Pt100 is equal to about 100 Ω;
• If the temperature is 100 degrees, the signal of the Pt100 is equal to 138.5 Ω; for intermediate
temperature values the output signal from the Pt100 will be proportional. The signal in Ω is
converted by the PID controller into °C and compared with the fixed set-point value. At this
point, the controller sends a signal of 4-20 mA across the output, function (PID) of the shift
between the value of the process variable and the set point. Such electrical signal is converted by
an electropneumatic converter into pneumatic signal that controls the valve opening degree. The
following graphs shows:
• Fig. 4.3: the proportionality between the output electrical signals of the PID controller and the
pneumatic output signal of the electropneumatic converter (I/P)
Fig. 4.3
43
• Fig. 4.4: the proportionality between the output signal of the electropneumatic converter (0.2-1
bar) and the valve opening degree (0-100%).
Fig. 4.4
The 4-20 mA signals at the output of the PID controller can be measured with a milliammeter
using the proper terminals set on the board. The output signal from the I/P converter can be read
directly on the pressure gauge set on the board.
4.4- INSTALLATION
• Shut off the valves V1, V4 and V6
• Open the valves V2, V3, V5
• Connect the electrical board to the single-phase + G electrical supply (Fig. 5.1 – n° 2)
• Connect the electrical board to the compressed air line with the provided pipe complete with
quick connections (Fig. 5.1 – n° 1); the air pressure must be at max. of 1.5 bar and not less than
1.2 bar.
• Connect the unit to the tap water with the rubber pipe provided using metal hose clamps to fix
it to the hose connector (Fig. 5.1 – n°4); the line water flow rate must be about 300 l/h
• Connect the system to the thermostatic bath with the provided pipes respecting the direction of
the adhesive arrows set on the pipes.
44
• Fill the tank of the thermostatic bath with distillated water or with silicon oil (with viscosity
around 100 mm2/s); with silicon oils (specific heat = ½ water specific heat) the temperature set
on the thermostatic bath is reached more quickly.
• Switch on the thermostatic bath and fix the temperature e.g. to 50 °C (see related technical
manual).
• Connect the system to the serial port COM1 of the P.C. with the serial cable (Fig. 5.1 – n° 3).
• Connect the valve V5 to a drain by means of the provided rubber pipe and metallic clamp
• Insert the E.L.C.B. (Fig. 5.1 – n° 5)
4.5- Stop of the system

• Shut off the valve V2.
• Switch off the thermostatic bath.
• Disconnect the E.L.C.B. set on the electrical control board.
In case of long period of inactivity:
• Drain all lines of the unit.
45
4.6- EXERCISES
No.1
• Set the thermostatic bath at 50 °C
• Set:
Gain = 3.0
I = 0.4 min
D = 0.1
• Set the set point e.g. to 45°C.
Fig. 4.5
• Wait for the process variable to reach the set point value. As you can note the gain, integrative
and derivative time values are valid as the temperature control is good.
• Exclude the integrative action from the controller.
• Change the set point, e.g. 40°C.
• The process variable will get near the set point value never reaching it: a constant shift in time
called OFF SET will persist.
• Reintroduce the integrative action on the controller and set I = 0.3 min; the off set will be
quickly canceled.
46
No.2
• Set:
Gain = 3.0
I = 0.4 min
D = 0.1
• Set the set point e.g. to 45°C.
• While the process variable tends to reach the set point, increase the Gain, e.g. to 6.0; you will
observe an increase of the inclination of the graph of Out (controller output) in time as the gain
has been increased.
When the value of gain is too high, the controller output starts to oscillate.
4.7- SAFETY
• Before any maintenance operation, disconnect the plant from the electrical mains
47
48
Exp#5
Level Control
5.1- THEORITICAL BACKGROUND:
The liquid-level control system shown in the following figure. The liquid level is
measured and the level transmitter (LT) output is sent to a feedback controller
(LC) that controls liquid level by adjusting volumetric flow rate q2. A second inlet
flow rate q1 is the disturbance variable. If the inlet flow rate q1 is decreased the
level in the tank will drop , the level transmitter (LT) output will be sent to the
controller , the controller will compare between the measuring value and the set
point value to evaluate the error, depending on the error the controller will give
appropriate action to the final control element and in our case the controller will
send an electrical signal to I/P transducer which change the electrical signal to
pneumatic action to the valve (final control element) to adjust the manipulated
variable q2 (increase it) to reach the set point value of the level.
Assume:
1. The liquid density ρ and the cross-sectional area of the tank A are constant.
2. The flow-head relation is linear, q3 = h/R.
3. The level transmitter, I/P transducer, and control valve have negligible
dynamics.
49
Consider the unsteady-state mass balance for the tank contents:
Substituting the flow-head relation, q3 = h/R, and introducing deviation variables

gives
Thus, we obtain the transfer functions
50
Where Kp = RA. Note that Gp(s) and Gd (s) are identical because q1 and q2 are
both inlet flow rates and thus have the same effect on h.
Fig. 5.1

• Pneumatic control valve, AISI 316 stainless steel execution, DN 15, Cv = 1.25, code LV1 (n°3)
• Differential pressure electronic transmitter, AISI 316 stainless steel execution, range 0 - 500
mmH2O, output signal 4-20 mA, code LT1 (n°2)
• Variable area flow meter, range 100-1000 l/h, code FI2 (n° 1)
• Microprocessor controller, PID type, 4-20 mA input and output signals, accuracy ± 0.1%,
complete with serial card RS 232 (n°7)
• Electropneumatic converter, 4-20 mA/0.2-1 bar (inside the switchboard)
• Transparent plastic tank, capacity 5 litres, code D1 (n° 9)
• Power supply light (n° 5)
• 2 measurement terminals for the 4-20 mA input signal of the controller (n° 6)
51
• Pressure gauge, range 0÷2.5 bar (n° 4)
• AISI 304 and 316 stainless steel valves and connection lines
• Painted carbon steel electrical switchboard complete with synoptic of the plant and E.L.C.B.
In this unit, the PID control is made on the water level inside the tank D1. The control device
consists in a pneumatic valve that, according to the signal from the PID controller, adjusts the
inlet water flow rate to the tank and consequently the level. The electronic transmitter, LT1,
measures the pressure at the base of the tank (directly proportional to the level) and sends the
PID electronic controller a 4-20 mA electrical signal proportional to 0 - 500 mmH2O.
In practice:
- If the level is null, the output signal from the transmitter is 4 mA (zero).
- If the level is to 500 mm, the output signal from the transmitter is 20 mA.
- For intermediate values, the output signal from the transmitter will be proportional to the level;
e.g. at 250 mm the output signal from the transmitter will be equal to 12 mA.
Fig. 5.2
The signal sent by the transmitter LT1 to the PID controller is compared to the set point value set
on the controller. At this point, the controller sends a 4-20 mA signal to the output, function
(PID) of the shift between the value of the process variable and the set point. This electrical
52
signal is converted by an electropneumatic converter into a pneumatic signal that controls the
valve opening level. The following graphs show:
• The proportionality between the output electrical signal of the PID controller and the pneumatic
output signal of the electropneumatic converter (I/P).
Fig. 5.3
• Fig. 5.4: the proportionality between the output signal of the electropneumatic converter (0.2-1
bar) and the opening level of the valve (0-100%).
Fig. 5.4
53
The 4-20 mA signals at the input and output of the PID controller can be measured with a
milliammeter using the proper terminals set on the board. The pneumatic output signal from the
I/P converter can be read directly on the pressure gauge set on the board. The controller is pre-set
to PID mode (proportional + integral + derivative).
5.4- INSTALLATION
• Close valves V1,V2, V3 and V4

• Open valve V5
• Connect the electrical control board to the single-phase + G electrical line, (n° 2)
• Connect the electrical board to the compressed air line using the provided pipe,complete with
quick connections (n° 1); the air pressure must be at max. 1.4 bar and not less than 1.2 bar.
• Connect the plant to the serial port COM1 of the P.C. with the serial cable (n° 3)
• Connect the installation to the water line with the provided rubber pipe (n° 1) using metal hose
clamp to fix it to the hose connector; the line water flow rate must be about 1000 l/h
• Connect valves V5 and V6 to a drain by means of the provided rubber pipe using metal hose
clamps to fix it to the hose connectors (n° 1 and 2).
• Connect the E.L.C.B. (n° 4)
5.5- STOP
• Close valve V2
• Disconnect the E.L.C.B.
• Empty the tank D1 and all lines from the water
5.6- EXERCISE
• Set:
Gain = 2.0
I = 1 min
D = 0.5 min
• Set the set point to the 50% (250 mm bar about, full scale 500 mm)
54
• The process variable will reach the set point value with regular behavior. This indicates that the
Gain, derivative and integrative time values are valid (Fig.5.5)
5.7- SAFETY
• Before any maintenance operation, disconnect the plant from the electrical mains
Fig. 5.5
• Switch the loop in manual mode
• Set the setpoint at 60%
• Switch the loop in automatic mode
• You can note that, with the set gain value, the level control is impossible.
At this point, you can carry out a test excluding the integrative action or the
derivative action.
55
56
Exp #6
Distillation Control
6.1- THEORETICAL BACKGROUND
The process of distillation should be familiar to most readers. The basic concept is that we can
separate a mixture of two pure liquids with different boiling points by heating the mixture to a
temperature between their respective boiling points. For example, water boils at 100°C and
ethanol boils at around 83°C at atmospheric pressure. If we heat the mixture to say 92°C, the
ethanol will boil and be transformed into vapor (which is collected and condensed) while the
water will remain as a liquid. This phenomenon is usually quantified by the relative volatility of
the two components.
A distillation column is used to make this process more efficient. A schematic diagram of a
distillation column is shown below.
The distillation column itself is made up of a series of stacked plates. A liquid feed containing
the mixture of both liquids enters the column at one or more points. The liquid flows over the
57
plates, and vapor bubbles up through the liquid via holes in the plates. As liquid travels down the
column, vapor comes in contact with it many times (due to the multiple plates). This is the
critical process in distillation columns. The liquid and vapor phases are brought into contact
because as one molecule of higher boiling material converts from vapor to liquid phase by
energy release, another molecule of the low boiling material utilizes the free energy to convert
from liquid to vapor phase.
The base of the distillation column contains a large volume of liquid, which is mostly the liquid
with higher boiling point (in our example, this would be water). Out of the base flows some of
this liquid, some of which is heated in the reboiler and returned to the column. This is called the
boil up, and is labeled V. The remaining liquid is the bottom product, labeled B.
Some vapor escapes from the top of the column and is returned to a liquid state in the condenser.
Some of this liquid is returned to the column as reflux L, and the remainder is the top product or
distillate D.
Vapor and liquid phases on a given plate approach thermal, pressure and composition
equilibrium to an extent depending upon the efficiency of the plate
6.1.1 Design of Columns

The design of multistage columns for binary mixtures can be accomplished graphically, via
equilibrium curves. This is called the McCabe-Thiele Method. Equilibrium curves plot the
volatility of components in a mixture; that is, the proportion of species 1 in the vapor phase (y1)
compared with the proportion of species 1 in the liquid phase (x1). The figure below shows two
common curves: curve A is a species with normal volatility, and curve B is a system with a
homogeneous azeotrope. The curves allow us to determine y1 from x1 given constant temperature
and pressure.
58
The azeotrope indicates that a component that is more volatile at low x1 becomes less volatile at
high x1 (above the azeotrope). This limits the separation that can be achieved between
components.
As an example, for an ethanol-water mixture, there is an azeotrope at x1 = 0.8943 (for pressure of

101.3 kPa and temperature of 78.15 °C) thus the maximum distillate composition that can be
achieved is xd = 0.8943. The distillate cannot have higher purity than this value from binary
separation.
The McCabe-Thiele Method allows the designer to determine the number of trays needed to
distil a mixture to the required purity. As well as the equilibrium curve, other factors such as the
feed quality (i.e. the thermal condition of the feed, which could be sub cooled, saturated,
superheated etc), the ratio of liquid to vapor flow and the proportion of species 1 in the feed are
used in distillation column design.
Based on these calculations, and the required spacing between plates, the theoretical height of the
column can be determined. For example, for a certain configuration the required number of trays
for an ethanol-water mixture may be 60. At a spacing of 25 cm, this will give a height of 15 m.
This may be excessive, and so the usual practice is to set the number of trays and then set the
reflux ratio L/D. e.g. for our example the number of trays are set to 12, and the reflux ratio is
then set to 5 (5×12 = 60). Thus only 1/5th of the product is being drawn out at any time, which
means that product is recirculating through the column about five times.
Thus it is important to have a fixed reflux ratio in steady state. The optimum feed tray can also
be determined using this method.
6.1.2 Pressure drop over the distillation column:

The total pressure drop across each tray is the sum of that caused by the restriction of the holes in
the sieve tray, and that caused by passing through the liquid (foam) on the top of the tray.
As the velocity of the vapors passing up the column increases then so does the overall pressure
drop. Varying the boil-up rate, which is done by varying the power input to the reboiler, controls
the velocity. Under conditions with no liquid present, the sieve trays will behave like an orifice
in that the pressure drop will be proportional to the square of the velocity.
The readings of the pressure drops over the rectifying (above the feed plate) and the stripping
(below the feed plat) sections will be taken by opening valves V6 and V7 on the manometer.
6.1.3 The boil-up rate:

Can be measured by operating valve V3 so that all the condensate is diverted into a measuring
cylinder and the time observed to collect a set quantity.
6.1.4 Equilibrium condition

The system will be have reached an equilibrium condition when the T1, T2, T3, T4, T5, T6, T7
and T8 are constant.
59
6.1.5 Refractometer
It is essential to have a convenient quick method of determining the composition of the binary
mixture taken from the various sample points on the equipment. Such a method involves the use
of a refractometer since the refractive index of these mixtures varies with composition.
6.1.6 PROPERTIES OF METHANOL AND WATER
Equilibrium Data For The Methanol- Water @ Atmospheric Pressure
Depend on % mole of Methanol
Liquid Vapor Temperature C

0 0 100
0.02 0.134 96.4
0.04 0.23 93.5
0.06 0.304 91.2
0.08 0.365 89.3
0.1 0.418 87.7
0.15 0.517 84.4
0.2 0.579 81.7
0.3 0.665 87.0
0.4 0.729 75.3
0.5 0.779 73.1
0.6 0.825 71.2
0.7 0.87 69.3
0.8 0.915 67.6
0.9 0.958 66
0.95 0.979 65
1 1 64.5
60
Equillibrium curve (methanol -water)
100
95
90
85
Tempreture (C)
80
75
70
65
60
55
50
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
x,y methanol
Equation for Equilibrium

y = -21.98x6 + 76.67x5 – 106.23x4 + 74.875x3 – 28.67x2 + 6.33x + .01
R2 = 0.9997
6.1.7 CALCULATION OF REFLUX
The minimum reflux can be calculated using the following equation:
xd − y f
R min =
yf − xf
Where:
Xd: the required distillation composition (liquid).
Yf: the vapor composition in equilibrium with xf.
Xf: the liquid feed composition
Then R required = 1.5Rmin
61
6.1.8 CALCULATION OF SET POINT
Set point: is the desired value and is supplied externally by the person in charge the production.
In determination of set point many of factors must be considered like:
1. The type of the system (binary or multi-component system).
2. The system operates at atmospheric pressure.
3. Depending on purity of methanol required the temperature of mixture at the top and
bottom was calculated (dew and bubble temperature).
6.1.9 DEW POINT AND BUBBLE POINT CALCULATION
6.1.9.1 Bubble point calculation

The basic equations for the bubble point are:
Nc Nc
 yi =  Ki xi = 1
i =1 i =1
Where:
K: is the ratio of mole fractions in the vapor and liquid at equilibrium.
yie
Ki =
xie
If Raoult’s law and Dalton’s law hold, values of KI can be calculated from the vapor pressure
and the total pressure of the system.
Pi
Ki =
P
P: total pressure.
Pi⁄: vapor pressure.
Procedure:
1. Assume Initial guess of Tmix.
2. Calculate vapor pressure of each component from Antoine equation:
B
ln P = A − (P in KPa, T in K)
C +T
Antoine constant
Component A B C
Methanol 16.4948 3593.39 -35.2249
water 16.5362 3985.44 -38.9974
3. Complete the following table:
62
Component Pi⁄ at Tguess Ki xi yI=xI Ki
Methanol
Water
4. If yI is too large try lower temperature.
6.1.9.2 Dew point calculation

The basic equations for the dew point are:
Nc Nc
yi

i =1
xi = 
i =1 K i
=1
Procedure:
1. Assume Initial guess of Tmix.
2. Calculate vapor pressure of each component from Antoine equation:
3. Complete the following table:
Component Pi⁄ at Tguess Ki yi xI=yi/Ki

Methanol
Water
4. If xI is too large try a higher temperature.

6.2- DISTILLATION CONTROL
In distillation control there are several requirements that must satisfy such as:
1. Safety.
2. Production specification: a plant should produce the desired amounts and quality of
the final products.
3. Environmental regulations.
4. Operational constrains.
5. Economics
The input variables can be further classified into the following categories:
1. Manipulated (or adjustable) variables: values can be adjusted freely by the human
operator or a control mechanism.
2. Disturbance: if their values are not the result of adjustment by an operator or a control
system.
At First the manipulated variables and disturbances and set point must be considered.
63
There are four values which are used to control, the flow rate of B (the bottom product), the
temperature of V (the boil up), the flow rate of L (the reflux) and the flow rate of D (the
distillate).
The system as shown above has four inputs and four outputs
Input Variables Output Variables

Distillate flow rate D Condenser level
Bottom product flow rate B Reboiler level
Reflux flow rate L Distillate composition
Steam flow
Bottom product composition
(which affects the temperature of V)
The overhead vapor VT is also generally considered an input variable and is mainly used to
control the column pressure. Since this is usually a self-regulating loop, we will ignore it in this
discussion.
Obviously, it is desirable to maximize the purity of the top and bottom products. Normally in
industry, the control variables are set manually by human operators. Some plants use automatic
control for only one product, and manual control for the other. Manual control can result in over
purification or loss of valuable product. These difficulties can be overcome by using dual
composition control, i.e. automatic control for both products.
There are some difficulties involved in designing a dual composition controller. In particular, the
system is both strongly nonlinear and strongly interactive. Also, the system has a very sluggish
response, and there are many problems with measuring the output variables (including dead
times for composition measurements).
Choosing the control structure is the most important step in designing a controller for the system.
The column pressure and reboiler and condenser levels must be controlled very carefully to
maintain stable operation. The control systems for these variables are called inventory
controllers. This leaves two degrees of freedom to control the top and bottom concentrations.
Deciding the control structure then amounts to choosing which two inputs will control the
compositions.
The most common is called the LV configuration, where the reflux flow rate L is used to control
the composition of the top product, and the boilup temperature V is used to control the
composition of the bottom product. In this case, the distillate flow rate D and bottom product
flow rate B are used to control the levels of the condenser and reboiler respectively. The
64
variables L and V are the ones most likely to be used by a manual operator to control the product
compositions.
Another common choice is the DV configuration, where the distillate flow rate D is used to
control the composition of the top product, and the boilup temperature V is used to control the
composition of the bottom product. For this configuration, the reflux flow rate L and bottom
product flow rate B are used to control the levels of the condenser and reboiler respectively.
USING A PID CONTROLLER WITH UOP3CC

The UOP3CC distillation column can be used for single loop process control demonstrations
using a PID process controller. It possible to configure 2 different control loops:
1. Reboiler power control from a column temperature (T7).
2. Reflux control from the top tray temperature (T1).
The object of the experiment can be:

1. Demonstrate a typical application of a PID process controller.
2. Observe the response of the process to a change in set point or disturbances.
3. Adjust the settings of the controller from optimum control of the process.
A PC microcomputer with GENESIS is available; the response of the process under PID control
can be monitored and logged using data logging screen.
6.2.1 REBOILER POWER CONTROL:
6.2.1.1 Procedure
1. Ensure that the reboiler power control selector switch is set to the “I/O PORT”.
2. Ensure that the reflux control and feed pump control selector switches are set to the
‘MANUAL “ position.
3. Select reboiler control from the main menu of the appropriate UOP3CC Genesis
application.
Reboiler power control from the tray temperature T7.
6.2.1.2 Open Loop System
• For such system the manipulated variableT7 allows to reach the steady state without using
controller.
•
65
Time (min) T7 (C)
• Plot T7 versus Time
6.2.1.3 Close Loop System
The controller setting for this control demonstration are listed below:
Initial value:
P 50%
I 4 RPM
D 0 MIN
Adjust the manual output from the controller until the tray temperature T7 has stabilized at the
required value then select AUTO to allow the controller to maintain T7.
66
Experiment May Be Performed To Establish:
1. Optimize the P, I, D settings.
2. The effect of disturbances
6.2.1.4 OPTIMIZE THE P, I, D SETTINGS.
6.2.1.4.1 Optimize The P Setting:
This part aims to study the response of P controller:
Feed pump RPM

Reflux ratio
Set point C
I 0
D 0
P= % P= % P= %
Time (min) T7 (C) Time (min) T7 (C) Time (min) T7 (C)
67
• Repeat the above steps with another values of P and observe the results.
6.2.1.4.2 Optimize The I Controller Setting:
This part aims to study the response of I controller:
Feed pump RPM

Reflux ratio
Set point C
P 0 %
I
D 0
I= I= I=

• Repeat the above steps with another values of I and observe the results.
68
6.2.1.4.3 Optimize The D Controller Setting:
This part aims to study the response of D controller:
Feed pump RPM

Reflux ratio
Set point C
P 0 %
I 0
D
D= D= D=

• Repeat the above steps with another values of D and observe the results.
69
6.2.1.4.4 Optimize The PI Controller Setting:
This part aims to study the response of PI controller:

Feed pump RPM
Reflux ratio
Set point C
P %
I
D 0
P= P= P=
I= I= I=

• Repeat the above steps with another values of PI and observe the results.
70
6.2.1.4.5 Optimize The PID Controller Setting:
This part aims to study the response of PID controller:
Feed pump RPM

Reflux ratio
Set point C
P %
I
D

• Repeat the above steps with another values of PID and observe the results.
6.2.1.5 EFFECT OF EXTERNAL DISTURBANCE
In this section the effect of external disturbances must be studded

Type of disturbance must be studded:
71
1. Feed composition
2. Feed flow rate.
3. Reflux ratio.
6.2.1.5.1 Feed Composition
Set point C
Feed pump RPM
Reflux ratio
P %
I
D
Feed composition before change Methanol Water

Feed composition after change Methanol Water
6.2.1.5.2 Feed Flow Rate
Set point C
Reflux ratio
Feed pump before change RPM
Feed pump after change RPM
P %
I
D
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6.2.1.5.3 Reflex Ratio

Set point C
Feed pump RPM
Reflux ratio before change
Reflux ratio after change
P %
I
D
6.2.2 REFLUX CONTROL

6.2.2.1 Procedure:
73
1. Ensure that the reflux control selector switch is set to the “I/O PORT”.
2. Ensure that the reboiler power control and feed pump control selector switches are set to the
“MANUAL” position.
3. Select reboiler control from the main menu of the appropriate UOP3CC Genesis application.
Reflux control from tray temperature T1

1. Enter typical values in constant reflux controller:
Cycle time 10 secs.
Required ratio 4:1
Then select constant reflux and allow the column to stabilize.
2. Enter typical values in temperature proportional controller:

Cycle time 10 secs.
Required ratio 4:1
Rate of change 1.0/deg
Required temperature value to suit binary mixture (T1).
3. Select temperature proportional reflux control to allow the controller to maintain T1.
Experiment may be performed to establish

1. The effect of disturbances
2. Optimize the controller settings.
6.2.2.2 OPTIMIZE THE CONTROLLER SETTINGS

6.2.2.2.1 Optimize The Cycle Time
Set point C
Feed pump RPM
Power Input kW
Required ratio
Rate of change /deg
Cycle time before change sec.
74
Cycle time = sec. Cycle time = sec. Cycle time = sec.
Time (min) T1 (C) Time (min) T1 (C) Time (min) T (C)
• Plot T1 versus time

• Repeat the above steps with another values anther cycle time and observe the results.
6.2.2.2.2 Optimize Rate of Change
Set point C
Feed pump RPM
Power Input kW
Cycle time sec.
Required ratio
Rate of change before change /deg
75
Rate of change = deg. Rate of change = deg. Rate of change = deg.
Time (min) T1 (C) Time (min) T1 (C) Time (min) T (C)

• Repeat the above steps with another values anther rate of change and observe the results.
6.2.2.3 EFFECT OF EXTERNAL DISTURBANCE

In this section the effect of external disturbances must be studded
Type of disturbance:
4. Feed composition
5. Feed flow rate.
6. Power input
6.2.2.3.1 Feed Composition

Set point C
Feed pump RPM
Power Input kW
Cycle time sec.
Required ratio
Rate of change /deg
Feed composition initial Methanol . Water .

Feed composition after change Methanol . Water
76
6.2.2.3.2 Feed Flow Rate

Set point C
Power Input kW
Cycle time sec.
Required ratio
Rate of change /deg
Feed pump before change RPM
Feed pump after change RPM
6.2.2.3.3 Power Input

Set point C
Feed pump RPM
Cycle time sec.
Required ratio
Rate of change /deg
Power Input before change kW
Power Input after change kW
77
78
Exp #7
Tunning
Learning objectives
The learning objectives includes,
 How to identify low order process models from simple process reaction curve data
 Using a relay feedback experiment to adaptively tune simple process models
 How to tune PID controller using an inverse process model-based technique
 Understanding and using the idea of controller assessment based on classical performance
indices
7.1 Introduction
In model-based controller design, simple models are used to characterize the dynamics of a given
process. Based on the simple dynamic model obtained, the PID controller parameters are then
computed. For example, in the parametric Ziegler-Nichols tuning method, a process model of the
following form was assumed,
 Ke − s   Ke − s   K   e −s 
G p ( s) =    =  
 s + 1    s       s 
Where the process gain, the time-constant and the delay-time are denoted by K ,  , 
respectively. Identification of this simple model structure used the step response of the process as
shown in Figure 7.1. In process engineering this type of system response is termed a process
reaction curve or an S-curve and this is the origin of the name for the family of tuning methods.
79
Key
Process gain, K Delay-time,  Slope of tangent line, S
Figure 7.1 Process reaction curve of a system
The process reaction curve would be recorded and various response measurements made. As can
be seen on Figure 7.1, the process gain, K can be measured and the intersection of the tangent
line with the base line provides an estimate of the dead time,  . The slope of the tangent at the
inflection point on the S-curve can also be measured. This measured slope has the theoretical
formula, S = K /  . Although the PID tuning is based on an inherent process model with
parameters, K ,  ,  , the PID controller coefficients are computed from formula given in terms
of the measured values of K , S ,  . Modeling for controller design in this way is pretty rough
due to the need for a tangent line at the inflection point of the S-curve.
There are also quite a few methods in the literature which propose to model the S-shape step
response curve with the so called First-Order-Plus-Dead-Time (FOPDT) models or alternatively,
over-damped Second-Order-Plus-Dead-Time (SOPDT) models. Parametric methods to tune the
PID controllers have been presented in many different ways for the FOPDT model given by,
80
 Ke − s 
G p (s) =   . For example, tuning rules to minimize an integral performance index based
 s +1 
   
b c
on the FOPDT dynamics have been given in the forms, P = a  and P = a + b  , where
   
P is controller parameters (such as: kc ,  R , and  D ) to be tuned for a PID controller, and
a, b, c are regression constants. Furthermore, since the years of 80, the Internal Model
Control (IMC) theory has been used to formulate PID controllers. As a result, the need for simple
models is even more emphasized.
There are a few methods reported in the literature for identifying simple SOPDT models. In an
early work of Oldenbourg and Sartorius (1948), the model being identified is
 Ke− s 
G p ( s) =   , where the process gain, the two process time-constants and the
 ( 1 s + 1)( 2 s + 1) 
delay-time are denoted by K , 1 ,  2 ,  , respectively. From the response as shown in Figure
7.2, the initial delay-time  and the length of segments I1 and I 2 are measured.
Key
Process gain, K Delay-time,  Slope of tangent line, S
Figure 7.2 Process step response of a system
81
1 
Mathematically, the value of is related to 2 by the following equations:
I1 1
2
1   2 1 − 2 x
=  =x 1− x
I1   1 
1 2 2
x = , where x =
I1 I1 1
On the other hand, the point ( τ1 /I1 , τ 2 /I1 ) also satisfies the following:
τ1 τ 2 I 2
+ =
I1 I 2 I1
Consequently, based on the above equations and the measured segments, the two time constants
can be solved.
In an alternative method, Sundaresan et al. (1978) derived the following relation,

ln  
 = ( tm − m ) S =  e −  , where  = and  = 2  1
 −1 1
The value of tm is taken as the time at the inflection point of the response, and the quantity m is
computed from the integration of the following:


m =  [ y(t ) − y(t )]dt
0
As the input is a unit step change, y(t ) equals K (see as Figure 7.2). A plot of  versus  can
thus be prepared. Thus, by calculating the value of  from the response, the value of  can be
calculated, then, the two time constants and the dead time can be obtained from the following
formulas,
1
1 =  1−
/ S ,  2 =   1 , and  = m −  1 −  2
As mentioned, S is the slope of the tangent at the inflection point of the response.
Another method for identifying simple over-damped SOPDT models is found in an early text
book of Harriott (1964). The Harriott’s method is derived based on two observations from a class
82
1
of step responses of the process represented by the transfer function ,
(1s + 1)(1s + 1)
   0,1 . First, it is found that almost all the step responses mentioned reach 73 % of its final
steady state approximately at a time of 1.3 times 1 +  2 . For easy reference, this response
position and time are designated as y73 and t73 , respectively, as shown in Figure 7.3(a). Second,
at a time of 0.5(1 +  2 ), all the step responses separate from each other most widely. Again, for
easy reference, the time at 0.5(1 +  2 ) is designated as t* , and the corresponding response
position is denoted as y * . It is found that y * is a function of  1 ( 1 +  2 ) as shown in Figure
7.3(b). In other words, from the experimental response, the position of y73 is identified and the
t73 is read from the corresponding time. Upon having t73 , the value of t* can be calculated. From
this t* , the position of y * can be read from its step response again. When y * is found, the value
of  1 ( 1 +  2 ) can be obtained by making use of Figure 7.3(b), and the two time constants can
be computed.
(a)
(b)
83
Figure 7.3 (a) Step responses (b) Relation between y * and  1 ( 1 +  2 )
Key
Process time constants,  1 , 2 Response position at 73% complete, y73
Response time at 73% complete, t73 Time at 0.5(1 +  2 ) , t*
Response position at t* , y* Fractional constant,  : 0 ~ 1
The method as given above was originally formulated for systems without delay-time, but it can
be easily extended to include the estimation of delay-time by using the relationship for the area,
m given as,
m =  1 + 2 +
Thus, the parameters can be estimated from the following equation set,
t73
 = m−
1.3
 1   t −t 
1 =     73 0 
  1 +  2 at y* 
1.3 

  1  
  t73 − t0 
 2 = 1 −     

  1 +  2 at   1.3 
y* 
where t0 is the time at which the process begins to response initially.
84
All of the above methods for developing SOPDT models are characterized by the use of data
from the step responses instead of using whole sets of time series data of both input and output as
might typically occur for classical parameter estimation procedures. In this chapter, the focus
will be on developing a systematic procedure to identify these simple models from transient step
response curves or from relay feedback experiments. Following this, PID controllers will be
synthesized using these simple models and a proposed inverse-based method. This methodology
will not resort to rule-based methods based on optimization procedures.
85
Exp #8
Dynamic of Stirred Tanks
8.1 Introduction
A B
1 2 3
Figure 8.1 shows the schematics of the experimental set-up
Tank (A) and (B) contain water of differing salt concentration, and provide
solution at constant head. Item (C) is a three way valve which can be positioned to
select the flow from either tank (A) or (B). The solution passes through a rotameter
and then to first tank (1) in series. The overflow from this tank passes successively
to 2 and 3 tanks in series before being discharged. The tanks 1, 2 and 3 are stireed
continuously. A conductivity cell immersed in the solution is connected t a
conductivity bridge and a recorder.
86
8.2 Experimental Procedure:
1. Prepare NaCl solution (about 6 gm/l) in the big storage tank.

2. Fill the other storage tank with distilled water.
3. Adjust the zero of the recorder.
4. Place the three way valve such that the distilled water flows through the
tanks.
5. Start the pumps and adjust the flow to about 0.2 l/min.
6. Place conductivity meter in the first and second tanks.
7. Introduce a step change in concentration by shifting the position of the three
way valve such that saline water flows through the tank. Mark this time as
zero time on recorder.
8. Observe the recorder and wait for system to attain steady state (i.e. when
concentration becomes constant).
9. Introduce the change in reverse direction and again mark time equal to zero
on the recorder, then wait for the new steady state.
10.Increase the flowrate to 0.3 l/min. repeat steps 7 to 9.
11.Measure the liquid hold-up of each tank and record the flowrate for each
process step.
12.Switch off recorder agitator and pumps.
8.3 Experimental Programs:
1. Study dynamics of s stirred tank by subjecting the system to a step and

pulse input.
2. Study the dynamics of stirred tanks in series.
3. Demonstrate use of conductivity as a method of concentration
measurement.
8.4 Data analysis required
1. Derive the dynamic model equations for pulse input for the first and the
second tank.
2. Calculate the dead time for all process steps. Clearly indicate what
experimental results you are using to do this.
87
3. Convert the chart recorder readings into concentrations at different times.
The time is obtained by taking distances at different points and dividing
by the chart speed. Thence into deviation variables. Place results in
appropriate appendix. Note that the y-axis of the chart represents
conductivity and readings vary from 0-100 mV.
4. Calculate the time constant of the 1st tank by plotting ln(1-C1(t)/A) versus
(t-td) for all step changes.
5. Calculate the time constant of all the tanks for all step changes from the
volumetric and flow measurements and compare your time constant in
tank 1 with that that calculated from the previous step.
6. Plot C1(t) versus (t-td) both experimentally and theoretically for both step
and pulse inputs and compare the results.
7. Plot C2(t) versus (t-td) both experimentally and theoretically for both step
and pulse inputs and compare the results.
88
Exp #9
Simulink
9.1 Introduction to SIMULINK
Although the standard MATLAB package is useful for linear systems analysis,
SIMULINK is far more useful for control system simulation. SIMULINK enables
the rapid construction and simulation of control block diagrams. The goal of the
tutorial is to introduce the use of SIMULINK for control system simulation. The
version available at the time of writing of this textbook is SIMULINK 4, part of
Release 12 (including MATLAB 6) from MATHWORKS. The version that you are
using can be obtained by entering ver in the MATLAB Command Window.
The easiest way to learn how to use SIMULINK is to implement each step of the
tutorial, rather than simply reading it. The basic steps to using SIMULINK are
independent of the platform (PC, MAC, UNIX, LINUX…).
9.1.1 Background
9.1.2 Open-loop Simulations
9.1.3 Closed-loop Simulations
9.1.4 Developing Alternative Controller Icons
89
9.1.1 Background
The first step is to start up MATLAB on the machine you are using. In the Launch
Pad window of the MATLAB desktop, select SIMULINK and then the SIMULINK
Library Browser. A number of options are listed, as shown in Figure 9.1. Notice that
Continuous has been highlighted; this will provide a list of continuous function
blocks available. Selecting Continuous will provide the list of blocks shown in
Figure 9.2. The ones that we often use are Transfer Fcn and StateSpace.
90
Figure 9.1 SIMULINK Library Browser.
91
Figure 9.2 SIMULINK Continuous Blocks.
Selecting the Sources icon yields the library shown in Figure 9.3. The most
commonly used sources are Clock (which is used to generate a time vector), and
Step (which generates a step input).
92
Figure 9.3 SIMULINK Sources.
The Sinks icon from Figure 9.1 can be selected to reveal the set of sinks icons
shown in Figure 9.4. The one that we use most often is the To Workspace icon. A
variable passed to this icon is written to a vector in the MATLAB workspace. The
93
default data method should be changed from “structure” to “matrix” in order to
save data in an appropriate form for plotting.
Figure 9.4 SIMULINK Sinks.
9.1.2 Open-loop Simulations

You now have enough information to generate an open-loop simulation. The
Clock, simout, step and Transfer function blocks can be dragged to a model
(.mdl) workspace, as shown in Figure 9.5a. Renaming the blocks and variables,
and connecting the blocks, results in the model shown in Figure 9.5b. The
transfer function studied is the Van de Vusse reactor (Module 5).
The s-polynomials in the process transfer function were entered by double-
clicking on the transfer function icon and entering the coefficients for the
94
numerator and denominator polynomials. Notice also that the default step (used
for the step input change) is to step from a value of 0 to a value of 1 at t = 1.
These default values can be changed by double-clicking the step icon. The
simulation parameters can be changed by going to the Simulation “pull-down”
menu and modifying the stop time (default = 10) or the integration solver
method (default
= ode45).
simout
Clock To Workspace
Simout
To Workspace1
1
simout
s+1
Step Transfer Fcn To Workspace2

a. Placement of function blocks
t
Clock
time
-1.117s+3.1472
s 2 +4.6429s+5.3821 y
step
input Transfer Fcn measured output
b. Renaming and connection of blocks
Figure 9.5 Development of an Open-loop Simulation.
The reader should generate simulations and observe the “inverse response”
behavior of the output with respect to a step input change. Use the subplot
command to place the process output (y) on the top plot, and the manipulated input
95
(u) on the bottom plot. Perform this now. If desired, change the default simulation
stop time by selecting the parameters “pull down” menu.
9.1.3 Feedback Control Simulation
The Math icon from Figure M2.2 can be selected, resulting in the functions shown
in Figure M2.6. Additional icons can be found by selecting the Simulink Extras
icon in Figure M2.1. Selecting the Additional Linear icon from this group yields
the set of icons in Figure M2.7. The most useful icon here is the PID Controller.
Any icon can be “dragged” into the untitled model workspace. In Figure M2.8 we
show the preliminary stage of the construction of a control block diagram, where
icons have been dragged from their respective libraries into the untitled model
workspace.
96
ks
7
Figure 9.6 SIMULINK Math.
97
Figure 9.7 SIMULINK Additional Linear.
The labels (names below each icon) can easily be changed. The default parameters for
each icon are changed by double clicking the icon and entering new parameter values.
Also, connections can be made between the outputs of one icon and inputs of another.
Figure M2.8b shows how the icons from Figure M2.8a have been changed and linked
together to form a feedback control block diagram. It should be noted that the form of
the PID control law used by the SIMULINK PID Controller icon is not the typical
form that we use as process control engineers. The form can be found by double-
clicking the icon to reveal the following controller transfer function representation
Gc(s)=P+1/s+Ds
98
while we normally deal with the following PID structure
gc(s)=kc(1+1/τIS+τDS)
so the following values must be entered in the SIMULINK PID Controller
p=kc I=kc/τI D=kcτD
The s-polynomials in the process transfer function were entered by double-clicking

on the transfer function and entering the coefficients for the numerator and
denominator polynomials. Notice also that the default step (used for the step setpoint
change) is to step from a value of 0 to a value of 1 at t = 1. These default values can
be changed by double-clicking the step icon. The simulation parameters can be
changed by going to the Simulation “pull-down” menu and modifying the stop time
(default = 10) or the integration solver method (default = ode45).
The controller tuning parameters of kc = 1.89 and tI = 1.23 are used by entering P =
1.89 and I = 1.89/1.23 in the default PID Controller block. The following plot
commands were used to generate Figure 9.9.
» subplot(2,1,1),plot(t,r,'--',t,y)
» xlabel('t (min)')
» ylabel('y (mol/l)')
» subplot(2,1,2),plot(t,u)
» ylabel('u (min^-1)')
99
Figure 9.9. Measured Output and Manipuated Input Responses to a Unit Step Setpoint
Change.
This brief tutorial has gotten you started in the world of SIMULINK-based control
block diagram simulation. You may now easily compare the effect of different tuning
parameters, or different formulations of a PID controller (“ideal” vs. “real”, for
example).
Let’s say you generated responses for a set of tuning parameters that we call case 1
for convenience. You could generate time, input and output vectors for this case by
setting:
» t1 = t;
» y1 = y;
» u1 = u;
100
after running the case 1 values. You could then enter case 2 values, run another
simulation, and create new vectors
» t2 = t;
» y2 = y;
» u2 = u;
then, compare the case 1 and case 2 results by:
» subplot(2,1,1),plot(t1,y1,t2,y2,'--')
» ylabel('y (mol/l)')
» subplot(2,1,2),plot(t1,u1,t2,u2,'--')
» ylabel('u (min^-1)')
which automatically plots case 1 as a solid line and case 2 as a dashed line. Similarly,
you could modify the controller type by placing a transfer function block for the
controller and using a “real PID” transfer function (this only differs when there is
derivative action).
Other Commonly Used Icons
Often you will want to simulate the behavior of systems that have time delays. The
Transport Delay icon can be selected from the Continuous library shown in Figure
9.2. The transport delay icon is shown in Figure 9.10. Our experience is that
simulations can become somewhat “flaky” if 0 is entered for a transport delay. We
recommend that you remove the transport delay block for simulations where no time-
delay is involved.
Transport Delay
Figure 9.10. Transport Delay Icon
101
Manipulated variables are often constrained to between minimum (0 flow, for
example) and maximum (fully open valve) values. A saturation icon from the
Nonlinear library can be used to simulate this behavior. The saturation icon is
shown in Figure 9.11.
Figure 9.11. Saturation Element
Actuators (valves) and sensors (measurement devices) often have additional

dynamic lags that can be simulated by transfer functions. These can be placed on
the block diagram in the same fashion that a transfer function was used to represent
the process earlier. It should be noted that icons can be “flipped” or “rotated” by
selecting the icon and going to the format “pull-down” menu and selecting Flip
Block or Rotate Block. The block diagram of Figure 9.8 has been extended to
include the saturation element and transport delay, as shown in Figure 9.12.
clock time
setpoint u
manipulated
step set point Sum PID Controller Saturation
Figure 9.12. Block Diagram with Saturation and Time-Delay Elements
The default data method for the “to workspace” blocks (r,t,u,y in Figure 9.12) must
be changed from “structure” to “matrix” in order to save data in an ppropriate
form for plotting.
102
9.1.4 Developing Alternative Controller Icons
It was noted earlier that the default SIMULINK PID controller block uses a
different form than that used by most process engineers. It is easy to generate new
PID controller blocks as shown below. The default PID controller icon is shown in
Figure M2.13a. This is “unmasked” to yield the diagram shown in Figure M2.13b.
Again, this has the form
Gc(s)=P+1/s+Ds
while we normally prefer the following PID structure
gc(s)=kc(1+1/τIS+τDS)
Of course, the two algorithms are related by
p=kc I=kc/τI D=kcτD
but it would be much less confusing to work with our standard form.
Summary
SIMULINK is a very powerful block diagram simulation language. Simple

simulations, including the majority of those used as examples in this textbook, can
be set-up rapidly (in a matter of minutes). The goal of this module was to provide
enough of an introduction to get you started on the development of open- and
closed-loop simulations. With experience, the development of these simulations
will become second-nature. It is recommended that you perform the simulations
shown in this module, as well as the practice exercises, to rapidly acquire these
simulation skills.
103
Part Two
Unit lab
104
Exp 1
GAS ABSORPTION COLUM
UOP7
105
1.1.SAFETY IN THE USE OF EQUIPMENT SUPPLIED BY ARMFIELD
Before proceeding to install commission or operate the equipment described in

this instruction manual we wish to alert you to potential hazards so that they may
be avoided.
Although designed for safe operation, any laboratory equipment may involve
processes or procedures which are potentially hazardous. The major potential
hazards associated with this particular equipment are listed below.
• INJURY FROM ELECTRIC SHOCK

Mains electrical supply to water pumps and air compressor
• INJURY FROM INCORRECT HANDLING

The equipment is heavy and must be handled properly when positioning.
Bottles of compressed gas (not supplied by Armfield) are heavy and must
be handled / stored correctly
• INJURY FROM MISUSE

Glass components are delicate and can break if mistreated
• INJURY OR DAMAGE TO CLOTHING FROM CORROSIVE FLUIDS

Dilute sodium hydroxide is used for gas analysis and is circulated through
the column for one of the teaching exercises
• RISK OF INFECTION DUE TO LACK OF CLEANLINESS

Water will stagnate if left in the sump tank or column. Water must be
changed at regular intervals
Accidents can be avoided provided that equipment is regularly maintained

and staff and students are made aware of potential hazards.
106
Armfield Ltd. suggests that a comprehensive list of Laboratory Safety
Precautions and Rules be made available to all laboratory users. Local laws or
regulations related to laboratory practice or laboratory safety must be
incorporated in these safety rules.
Please refer to the notes overleaf regarding the Control of Substances Hazardous
to Health Regulations.
Figure 1 UOP7 GAS ABSORPTION COLUMN
107
1.2.INTRODUCTION
The packed tower, in which two fluids flowing in opposite directions enable a
chemical component to be transferred from one fluid phase to the other, occurs
in almost all chemical plants. The process may be gas absorption, distillation,
solvent extraction or chemical reaction. Knowledge of the characteristics of both
fluid flow and of mass transfer in such towers is necessary for both plant
operators and designers.
The Armfield Gas Absorption Column has been designed to allow these studies
to be made and the instrumentation and layout enables students to follow both
the hydrodynamic characteristics in the absence of mass transfer, and also,
separately, to advise the performance of the mass transfer process involved in
gas absorption. The size of the equipment has been chosen so that teaching
exercises may be completed in a typical laboratory class period, while at the
same time being capable of demonstrating full-scale plant behavior.
Considerable attention is directed towards matters of safety that are of crucial
importance in the process industries.
This instruction manual gives details of all the laboratory services required for
operation of the column, together with commissioning procedures and
instructions for the many teaching exercises possible with the equipment.
108
1.3.DESCRIPTION
The packed absorption column is made of two 80 mm inside diameter clear

acrylic sections joined end to end to give a total column length of 1.4 m and is
installed vertically on a mild steel floor standing framework. The column is filled
with 10 mm x 10 mm glass Rashig rings (11) which is representative of the type
of packing used in gas absorption.
The liquid for the process is normally water and is stored in a 50 liter rectangular
sump tank (1). A valve (2) on the underside of the tank allows it to be drained for
cleaning. A float valve on the side of the tank supplies fresh water as required. A
centrifugal pump (15) is used to deliver the liquid to the top of the column (9)
where it falls by gravity through the packing before returning to the sump tank
via a 'U' trap that forms a liquid seal. A control valve C4 downstream of the 'U'
trap allows the head of water in the column to be varied. This valve is usually
fully open when the column is in use but can be partially closed to restrict the
flow of water returning back to the sump tank. Water can be drained from the 'U'
trap after use by opening the drain cock (16) at the bottom. A variable area flow
meter F1 gives a direct reading of the liquid flow rate entering the top of the
column. The flow of liquid can be varied using the control valve C1 above the
liquid flow meter.
The gas to be absorbed is normally carbon dioxide and would be taken from a
cylinder of compressed gas (not supplied by Armfield), located in a suitable
storage rack adjacent to the column. The gas is connected to a low pressure
regulator that is located at the rear of the vertical backboard. The gas passes
through a calibrated variable area flow meter F3 and is mixed with an air stream,
also via a calibrated variable area flow meter F2 from a rotary compressor (14).
The flow of air can be varied using the control valve C2 above the air flow meter.
The ratio of gas to air in the mixture entering the column is therefore known and
easily varied. Entering the base of the column, the gas mixture rises up through
the packed bed of Raschig rings (11) and is counter-currently contacted with the
109
liquid flowing down the column. Gas is prevented from escaping at the base of
the column by the liquid in the 'U' trap.
Tappings are provided at the base (13 with isolating valve), centre (12 with
isolating valve) and top (8) of the column to allow indication of pressure drop in
the two sections of column using a pair of 'U' tube manometers (3). These
tappings also provide a means of extracting samples of gas from the column for
analysis using the sampling syringe (7). The carbon dioxide content of the gas
samples is determined using a Hempl apparatus (5) and readings are indicated on
the scale (6). A sampling point (17) below the column allows analysis of the
liquid outlet stream. A sampling pipette S5 can be used to withdraw a sample of
liquid from the sump tank for analysis. The flow meters, manometers and gas
analysis equipment are all mounted on a vertical backboard at a convenient
height for operation.
The effluent gas leaves the top of the column via a cap with an overflow
arrangement (19 & 20). This arrangement ensures that any liquid is safely
returned to the sump tank if the column becomes flooded. When using a solution
of caustic soda (sodium hydroxide) in the column it is suggested that a suitable
container is located below the overflow to intercept any liquid that spills from
the top of the column. For safe operation the flooding characteristics of the
column should be evaluated using clean tap water. Caustic soda should not be
used for this series of tests.
110
111
Diagram showing details of the overflow arrangement and air pipework
112
1.4.COMMISSIONING
All numerical references in brackets relate to the diagrams on pages 11 and 12.
Clean tap water is used for safe commissioning of the equipment.
1. Fill the sump tank (1) with clean cold water by turning on the water
supply attached to the float valve.
2. Connect the electrical supply cable to the appropriate mains supply.
3. Prime the water manometers (3) with clean water until the meniscus in
both tubes is at mid height (250 mm on the scale).
4. Fill the Hempl gas analysis apparatus (5) with demineralised water up to
the '0' mark on the scale (6).
5. Connect a CO2 gas cylinder, fitted with a regulator, to the inlet regulator
on the equipment with a flexible tube, and set the cylinder regulator to
minimum pressure.
6. Open fully the gas flow control valve C3 that is incorporated on the gas
flow meter F3 (small, centre flow meter) and open the main gas cylinder
valve.
7. Increase the cylinder regulator output pressure to give maximum flow
reading on the gas flow meter then immediately close the main cylinder
valve to avoid wasting gas (the remainder of the commissioning will be
carried out using air and water). Close the gas flow control valve C3 on
F3.
8. Close the air C2 and water C1 flow control valves. Close the gas sampling
cocks (8, 12 and 13) on the absorption column. Check that the flow
control valve C4 in the discharge pipe from the 'U' trap into the sump tank
is fully open.
9. Switch on the air compressor (14) using the appropriate mains switch (4).
Check that the relief valve on the compressor operates - audible click with
air escaping. Gradually open the air flow control valve C2 and check that
air is delivered to the base of the column. Open the air flow control valve
fully and check that a maximum flow rate of 180 litres/min can be
113
obtained on flow meter F2. Adjust C2 to give a reading of 80 litres/min on
F2.
10. Switch on the water pump (15) using the appropriate mains switch (4).
Gradually open the liquid flow control valve C1 and check that water is
delivered to the top of the column. Adjust C1 to give a reading of 4
litres/min on F1. Adjust valve C4 if necessary to maintain a liquid seal in
the 'U' trap (close the valve until air does not escape via the 'U' trap).
11. Open the sample cocks at the base (13), middle (12) and top (8) of the
column. Check that the two water manometers (3) indicate the pressure
drop across the column (the connecting valves above the manometers
must be correctly set. Refer to the diagram on page G-1 for details).
12. Check that the Hempl gas analysis apparatus (5) operates correctly by
following the instructions in exercise A.
13. Close the air flow control valve C2 and switch off the air compressor.
Open valve C4 fully at the top of the 'U' trap. Open the liquid flow control
valve C1 fully and confirm that a maximum flow rate of 10 litres/min can
be obtained on flow meter F1. Switch off the water pump and close the
liquid flow control valve C1.
14. Drain the Hempl apparatus.
15. Drain the water seal by opening the small drain cock (16) at the bottom of
the 'U' trap beneath the column.
The equipment is now ready for use.
114
1.5.NOMENCLATURE
a = Effective interfacial area per unit packed column (cm-1)
A = Cross sectional area of the tower (m2)
Cc = Concentration of sodium hydroxide (g.moles/litre)
Cd = Concentration of dissolved 'free carbon dioxide' (g.moles/litre)
CN = Concentration of sodium carbonate ions (g.moles/litre)
F = Flow (litres/second)
G = Gas flow rate (g.moles/second)
Kog = Gas-side mass transfer coefficient (g.moles/second.cm2.atm)
L = Liquid flow (litre/second)
M = Molecular weight
P = Pressure (atm)
R = Mass transfer rate (g.moles/cm2.second)
T = Standard acid titration volume (ml)
VB = Volume of alkali solution added in liquid analysis (ml)
V1 = Volume of gas sample taken in Hempl apparatus (ml)

115
V2 = Corresponds to amount of gas absorbed in Hempl apparatus (ml)
X = Mole fraction of component in liquid phase
Y = Mole fraction of component in gas phase
Subscripts
T = Total
i = Inlet conditions to column
o = Outlet conditions to column
N = Rate of absorption (g.moles/second)
116
1.6. INDEX TO TEACHING EXERCISES
EXERCISE A
To measure the absorption of carbon dioxide into water flowing down
the packed column, using the gas analysis equipment provided.
EXERCISE B
To calculate rate of absorption of carbon dioxide into water from analysis of liquid
the solutions flowing down the packed column.
EXERCISE C
To calculate rate of absorption of carbon dioxide into caustic soda solutions from
analysis of liquid solutions flowing down the packed column.
EXERCISE D
To show that the amount of carbon dioxide removed from the air stream equals the
amount taken up by a liquid stream of caustic soda solution.
EXERCISE E
Determination of Overall Mass Transfer Coeffcient (Kog).
EXERCISE F
To determine the air pressure differential across the dry column as a function of
the air flow rate.
EXERCISE G
To examine the air pressure differential across the column as a function of air flow
rate for different water flow rates down the column.
117
1.6.1. EXERCISE A
1.6.1.1.OBJECT OF EXERCISE:
To measure the absorption of carbon dioxide into water flowing down the
tower, using the gas analysis equipment provided.
Obtaining gas sample from gas sample from the top of the column
Obtaining a Gas Sample from the Middle of the Column
118
1.6.1.2.EQUIPMENT REQUIRED:
1. Carbon dioxide cylinder with integral pressure regulator, connected to

regulator R on gas inlet on the apparatus.
2. Approximately 300ml of 1.0 molar caustic soda solution with safety

gloves and goggles. Small funnel and tubing for filling analysis
equipment.
1.6.1.3.PROCEDURE:
1. First fill the two globes of the absorption analysis equipment on the left
of the panel with 1.0 Molar caustic soda. Wear gloves and goggles
while doing this. Adjust the level in the globes to the '0' mark on the
sight tube, using drain valve Cv into a flask to do this. (See step A in
sketch overleaf).EQUIPMENT SET-UP:
2. Turn on the mains water supply to the sump tank. Fit the drain pipe to
the water return from the column so that water is not returned to the
sump tank.
3. With gas flow control valves C2 and C3 closed, start the liquid pump
and adjust the water flow through the column to approximately 4
litres/minute on flowmeter F1 by adjusting control valve C1.
4. Start the compressor and adjust control valve C2 to give airflow of

approximately 25 litres/minute in flowmeter F2.
5. Carefully open the pressure regulating valve on the carbon dioxide

cylinder, and adjust valve C3 to give a value on the flowmeter F3
approximately one half of the air flow F2. Ensure the liquid seal at the
119
base of the absorption column is maintained by, if necessary,
adjustment of control valve C4.
6. After 5 minutes or so of steady operation, take samples of gas from the

top and middle sample points. (Refer to the appropriate diagram for
details of the valve positions.) Analyse these consecutively for carbon
dioxide content in these gas samples as shown in the accompanying
sketch and following notes.
Diagrams relating to Steps A to F can be found on page A-4.
7. Flush the sample lines by repeated sucking from the line, using the gas
piston and expelling the contents of the cylinder to atmosphere. Note
that the volume of the cylinder is about 100 cc. Three full volumes of
the gas piston is sufficient. (Steps B and C).
8. With the absorption globe isolated and the vent to atmosphere closed,
fill the cylinder from the selected line by drawing the piston out slowly
(Step B). Note volume taken into cylinder V1, which should be
approximately 20ml for this particular exercise (see WARNING note
below). Wait at least two minutes to allow the gas to come to the
temperature of the cylinder.
10. Isolate the cylinder from the column and the absorption globe and vent
the cylinder to atmospheric pressure. Close after about 10 seconds (Step
D).
11. Connect cylinder to absorption globe. The liquid level should not
change. If it does change, briefly open to atmosphere again.
12.
Wait until the level in the indicator tube is on zero showing that the
pressure in the cylinder is atmospheric.
13. Slowly close the piston to empty the cylinder into the absorption globe.
Slowly draw the piston out again (Steps E and F).
120
Repeat steps E and F until no significant change in level occurs. Read
the indicator tube marking = V. This represents the volume of the gas
sampled.
WARNING: If the concentration of CO2 in the gas sampled is greater than

8%, it is possible to suck liquid into the cylinder. This will ruin
your exercise and takes time to correct. Under these
circumstances, do not pull the piston out to the end of its travel.
Stop it at a particular mark, eg. V1 = 20 on the coarse scale, and
read the fine scale.
13. Once the final value has been read from the scale, slowly close the
piston to empty the cylinder into the absorption globe. Reposition the
valves as shown in step G to allow the globe to equilibrate with
atmosphere.
WARNING: It is important to follow the above steps closely in order to take

representative gas samples and to achieve reproducible results.
Deviation from the above can lead to erroneous results.
121
122
1.6.1.4.READINGS AND CALCULATIONS:
A) CO2 content of gas samples:
From use of Hempl apparatus, volume fraction of CO2= V2

V1
For ideal gases, volume fraction = mole fraction = Y. Check that the sample
taken from the inlet to the absorption column should give the same value of CO2
fraction as that indicated by the inlet flowmeters.
B) Calculation of amount of CO2 absorbed in column from analysis of

samples at inlet and outlet.
From analysis with Hempl apparatus, volume fraction of CO2 in gas stream at
inlet
If Fa is litres/second of CO2 absorbed between top and bottom,
123
Note: Litres/second can be converted to g.moles/second as follows:-
absorbed CO2
g.moles/second
The assumption implicitly made here is that the volume flow is not affected by
the pressure drop through the column as this drop should be small in
comparison with atmospheric pressure. In Exercise D, a correct solution to this
problem is made.
124
1.6.2. EXERCISE B
To calculate rate of absorption of carbon dioxide into water from analysis of

liquid solutions flowing down absorption column.
1.6.2.2.EQUIPMENT SET-UP:
1.6.2.3.PROCEDURE:
1. Turn on the mains water supply to the sump tank and allow the tank to
fill. Ensure that the water outlet from the column is fitted with the drain
pipe and not the pipe that returns water to the tank.
and adjust the water flow through the column to approx. 6 litres/minute
on flow meter F1 by adjusting flow control valve C1.
125
3. Start the compressor and adjust control valve C2 to give an air flow of
approx. 10% of full scale on flow meter F2.

cylinder, and adjust valve C3 to give a value on the flowmeter F3
approx. one half of the air flow F2 Ensure the liquid seal at the base of
the absorption column is maintained by, if necessary, adjustment of
control valve C4.
5. After 5 minutes of steady operation, take samples at 10 minute intervals

from the mains water inlet and from S4. Take 150ml samples at known
times in each case. Analyse the samples according to the procedure
detailed below.
Analysis of Carbon Dioxide Dissolved in Water

Note: Water used for absorption should be deionised as presence of dissolved
salts affect the analysis described below. If tap water is used, no metal ions
should be present in greater quantities than 1.0 mg/litre and pH should be just
alkaline: 7.1 to 7.8.
Chemical Solutions Needed

a) Phenolphthalein indicator prepared from carbon dioxide-free
distilled water ie. A. R. grade.
b) Standard 0.0277M sodium hydroxide solution, prepared by
diluting 27.70ml 1M caustic soda standard solution to 1 litre
with carbon dioxide free distilled water. Prepare daily and
protect from carbon dioxide in the atmosphere by keeping in a
stoppered Pyrex bottle.
c) Standard 0.01M sodium bicarbonate solution, prepared by
dissolving approximately 0.1 gram of anhydrous sodium
bicarbonate in carbon dioxide free distilled water to 100ml.
126
1.6.2.4.Procedure
1. Take a water sample from the mains water inlet, approximate

volume of 150ml, or from liquid outflow point S4.
2. Discharge the sample at the base of a 100ml graduated cylinder,

flicking the cylinder to throw off excess liquid above the 100ml
mark.
3. Add 5-10 drops of phenolphthalein indicator solution a) above; if

the sample turns red immediately, no free CO2 is present. If the
sample remains colorless, titrate with standard alkali solution b)
above. Stir gently with a glass rod until a definite pink color
persists for about 30 seconds. This color change is the end point
- note volume VB of alkali solution added.
For best results, use a color comparison standard, prepared by

adding the identical volume of phenolphthalein solution a) to
100ml of sodium bicarbonate solution c) in a similar graduated
cylinder.
127
1.6.2.5. Calculation
The amount of free CO2 in the water is calculated from:
Readings to be taken :
CALCULATIONS:
128
1.6.3. EXERCISE C
To calculate rate of absorption of carbon dioxide into caustic soda solutions

from analysis of liquid solutions flowing down absorption column.
129
1.6.3.3.PROCEDURE:
1. Fill the sump tank at the base of the column to approximately three-
quarters full with 0.2M caustic soda solution. The preparation of this
requires great care and GLOVES AND GOGGLES MUST BE WORN.
Use standard 1M caustic soda solution from normal laboratory supplies
and add with care to the sump tank, eg. first add 30 litres of tap water to
the sump tank, followed by successive additions of 1M caustic soda
until a total volume of 7.5 litres of 1M caustic soda has been added,
giving 37.5 litres of 0.2M.
and adjust the flow of caustic soda through the column to
approximately 3 litres/min on flowmeter F1 by adjusting control valve
C1 .
3. Start the compressor and adjust valve C2 to give an air flow of

approximately 30 litres/minute on flowmeter F2.
CAUTION: As the solution used in this exercise is caustic it is

essential that the column is not allowed to flood. The air supply
should be turned off immediately if any liquid is present in the
clear tube above the top of the column.

cylinder and adjust valve C3 to give a flow of 3 litres/minute on
flowmeter F3. Ensure the liquid seal at the base of the absorption
column is maintained by, if necessary, adjustment of control valve C4.
5. After 15 minutes of steady operation, take samples at 20 minute

intervals simultaneously from S4 and S5. Take 250ml samples at known
times in each case. Analyse both samples according to the procedure
detailed overleaf.
130
Analysis of Carbon Dioxide Dissolved in Caustic Soda/Sodium Carbonate
Solutions
Theory:
The absorption of carbon dioxide from mixtures with air into caustic solutions
is characterised by the overall reaction (for most conditions) as:
CO + 2 NaOH → Na2CO3 + H2O
Under the conditions chosen for the absorption exercises, the amount of CO
removed from the air stream can be estimated from the amounts of NaOH and
NA2CO3 in the liquid samples, as virtually no 'free' CO2 will remain unreacted
in the liquid.
In using titration techniques of analysis, acid is first used to neutralise the

caustic soda and at the same time converts all sodium carbonate to bicarbonate.
Continuation of the titration with acid then neutralises all bicarbonate. The
total concentration of carbonate can thus be determined, and hence the amount
of CO2 absorbed deduced.
Solutions Needed:
1. Phenolphthalein indicator prepared from carbon dioxide-free distilled

water.
2. Methyl orange indicator similarly prepared.
3. One litre of standardised 0.20M hydrochloric acid.
4. One litre of 5% by weight of barium chloride solution.
131
1.6.3.4.Procedure:
a) Take a 250ml sample of liquid from the absorption column liquid outlet
or sump tank (as directed in the exercise) into a conical flask. Pipette
two 50ml portions of this into two separate conical flasks.
b) Flask 1 - Add a drop of phenolphthalein solution 1) to the contents and
titrate until the pink color just disappears with the standard hydrochloric
acid 3) Note the volume of acid added - T1, which is that needed to
neutralize all hydroxide and convert carbonate to bicarbonate. Then add
a drop of methyl orange 2) to the flask and continue to titrate with
standard acid 3) until the end point is found. Note the total acid added to
this second end point - T2, which represents neutralization of all
bicarbonate as (T2 - T1).
c) Flask 2 - Add about 10% more than the value of (T2 - T1) of the barium
chloride solution 4), to the flask contents and shake well. This
precipitates out all the original carbonate in the sample as barium
carbonate. Now add two drops of phenolphthalein solution 1) and titrate
against the standard acid solution 3) to the end point. Note the volume
of acid added - T2, which represents that needed to neutralize only the
original caustic soda. (T2 - T3) represents the difference between total
acid required for carbonate and hydroxide, and that required for
hydroxide alone.
Overall: NA2CO3 + 2 HCl ∧ 2NaCl + H2O + CO2
It is advisable to repeat all of the above to check reproducibility
1.6.3.5.Calculations of Sample Composition
a) Concentration of NaOH in original sample:

Cc = T3 x 0.2M (gra moles/litre)
b) Concentration of NACO in original sample:

CN = 2 − T3
T
x 0.2M x 0.5 50
132
c) Amount of CO2 removed from air mixture:
During a time interval, or between the top and bottom of the column, C N will
increase as CO2 is absorbed in equi-molar proportions, while Cc should
decrease in twice-molar proportions.
Calculations:
The amount of CO2 absorbed across the column as measured from

samples taken simultaneously from the sump tank feeding the column
top and at the bottom outlet, is given by:-
CO2 absorbed = liquid flow rate x [(CN)o - (CN)i]
(gram-moles/sec) (litres/sec) (gram-moles/litres)
1
= Liquid flow rate x 2 [(Cc)i - (Cc)o]
Similarly, over a time period θ seconds after a first sample is taken from
the sump S5:-
133
1.6.4. EXERCISE D
To show that the amount of carbon dioxide removed from the air stream
equals the amount taken up by a liquid stream of caustic soda solution.
1.6.4.2.SUMMARY OF THEORY
134
1.6.4.3.PROCEDURE:
The same procedure should be followed as for Exercise C, except that

gas samples at the inlet and outlet, as described in Exercise A, are to
be taken as well.
As the liquid composition is slowly changing as progressive

absorption of CO2 takes place, the steady state can only be
approximated by taking samples as close to each other in time as
possible.
Thus, after 5 minutes of circulating liquid and gases at the pre-set rates, take
1. a gas outlet sample, to give Yo,
2. a liquid outlet sample from the point S4 as soon after 1) as possible,
3. a liquid sample from the sump tank at S5 at the same time,
4. inlet gas sample, which should be constant and therefore can

be taken last. READINGS TO BE TAKEN:
135
COMMENTS SYMBOL UNITS QUANTITY
From flowmeter litres/min Air flow rate
(Divided by 60) F2 litres/sec ∴ air flow rate
From flowmeter litres/min CO2 flow rate
F3 litres/sec CO2 flow rate
From flowmeter litres/min Caustic soda flow rate
Li = Lo litres/sec Caustic soda flow rate
From Hempl analysis Yo vol. fraction CO2 outlet concentration
From Hempl analysis Yi vol. fraction CO2 inlet concentration
(should equal F2/F3+F2)
Liquid Samples: outlet
From Exercise C T1(o) m Titration with HCl
Procedure
T2(o) ml Titration with HCl
T3(o) ml Titration with HCl
Liquid Samples: inlet =
sump
From Exercise C T1(i) ml Titration with HCl
Procedure
T2(i) ml Titration with HCl
T3(i) ml Titration with HCl
Assumed equal to outlet P mm H Barometric pressure
Pressure
From manometer mm H2O Column pressure drop
P mm Hg Pressure at base of column
P+
13.6
θi C Temperature of feed gas
θi + 273 K Temperature of feed gas
136
1.6.4.4.SAMPLE CALCULATION:
Readings: Comments:
F2 = 0.40 litres/second
F3 = 0.052 litres/second Flowmeter readings divided by 60
L = 0.051 litres/second
Yo = 0.032
Yi = 0.111
From Hempl apparatus readings (Use
F3 0.052 0.111 for Yi)
0.
1
1
and Y 5
F2
F3 0.40 0.052
T1 (o) = 33.2 ml
T2 (o) = 50.9 ml As in exercise C, 0.20M HCl used in
T3 (o) = 35.0 ml titrations of 50ml sample.
T1 (i) = 48.4 ml
T2 (i) = 47.2 ml As in exercise C, 0.20M HCl used in
T3 (i) = 45.0 ml titrations of 50ml sample.
P = 759 mm Hg Lab. Barometer
P = 100 mm
H2O 100
= 7.35 ≈ 7mm Hg
13.6
θi = 19 C 292 K
137
Calculations:
138
1.6.5. EXERCISE E
Determination of Overall Mass Transfer Coefficient (Kog).
1.6.5.2.SUMMARY OF THEORY:
The familiar equation for packed tower absorption is
where Y* is the mole fraction of gas in equilibrium with the liquid

at any point in the tower and where Y is the bulk mole fraction; A
is the cross-sectional area of the tower; H is the packing height and
a is the specific area of packing/unit volume of packing.
For dilute gases in an otherwise inert gas stream, the above

equation can be simplified:-
The right hand side of this equation is difficult to integrate and Kog
is more simply (but less accurately) evaluated from the definition
of Kog as:
139
1.6.5.3.PROCEDURE:
The exercise is conducted as for Exercise D, except that the liquid

analyses may be omitted as the gas analysis alone can determine
the rate of absorption [as in Exercise A].
1.6.5.4.RESULTS AND CALCULATIONS:
1) N is calculated as in Exercises A and D.
2) a is specific area of packing/unit volume of tower, which for

9mm Raschig rings is 440 m2/m3.
4) A.H. is volume of the column.

= volume of tower
5) Partial pressures (of CO2):

Partial pressure = mole fraction x total pressure
Partial pressure = volume fraction x total pressure
∴ Using results of Exercise C:
140
5) Mass transfer coefficient:-
141
1.6.6. EXERCISE F
To determine the air pressure differential across the dry column as a function
of the air flow rate.
No additional equipment is required for this exercise
142
1.6.6.3.PROCEDURE:
1. The column must be dried by passing the maximum air flow until all
evidence of moisture in the packing has disappeared.
2. Set valves V1, V2 and V3 as shown in the diagram so that differential

pressures in the top and bottom sections of the column are indicated on
the two water manometers.
Take manometer readings of pressure differential across the column for a range
of air flow rates. The total pressure differential is the sum of the differential
across the top and bottom halves of the column, ie. add the readings from the
two water manometers.
READINGS TO BE TAKEN:
AIR FLOW RATE (l/min)
PRESSURE DIFFERENTIAL (mmH20)
1.6.6.4.RESULTS:
Plot the pressure differential as a function of air flow rate on log-log graph
paper and establish the relationship between these variables.
143
1.6.7. EXERCISE G
To examine the air pressure differential across the column as a function of air
flow rate for different water flow rates down the column.
No additional equipment is required for this exercise.
Note: For safe operation this exercise must not be performed using caustic soda
in the sump tank (used in previous exercises).
144
1.6.7.3.PROCEDURE:
1. Fill the sump tank to three-quarters full with tap water. Set valves V1,
V2 and V3 as shown on the diagram so that differential pressures in the
top and bottom sections of the column are indicated on the two water
manometers.
2. Switch on the water pump and set C1 to give a flow rate of say 3
litres/minute down the column.
3. After about 30 seconds close C1, switch off the pump and allow the
column to drain for 5 minutes.
Measure the air pressure differential across the wet column as a function of the
air flow rate.
Measure the air pressure differential across the column as a function of the air
flow rate for different water flow rates up to say 5 litres/minute, noting the
appearance of the column at each setting.
145
Pressure Differential (mm water)

Air flow 1/m
Water 180
flow l/m 20
0
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
9.0
10.0
The range of possible air flow rates will decrease with increasing water flow
rate due to onset of 'flooding' of the column, which should be noted.
1.6.7.4.RESULTS:
Pressure differential should be plotted as a function of air flow rate on log-

log graph paper for each water flow rate. It may be necessary then, to take
more readings in order to define precisely the transition points on the
resulting graphs.
146
Exp.# 2
LIQUID/LIQUID EXTRACTION
UNIT
1
2.1.SAFETY IN THE USE OF EQUIPMENT SUPPLIED BY ARMFIELD
Before proceeding to install commission or operate the equipment described in this

instruction manual we wish to alert you to potential hazards so that they may be
avoided.
Although designed for safe operation, any laboratory equipment may involve processes
or procedures which are potentially hazardous. The major potential hazards associated
with this particular equipment are listed below.
_ INJURY THROUGH MISUSE

_ INJURY FROM ELECTRIC SHOCK
_ INJURY FROM INCORRECT HANDLING
_ POISONING FROM TOXIC MATERIALS
_ INJURY FROM CORROSIVE LIQUIDS
_ RISK OF INFECTION THROUGH LACK OF CLEANLINESS
_ DAMAGE TO CLOTHING
Accidents can be avoided provided that equipment is regularly maintained and staff and
students are made aware of potential hazards. A list of general safety rules is included
in this manual, to assist staff and students in this regard. The list is not intended to be
fully comprehensive but for guidance only.
Please refer to the notes overleaf regarding the Control of Substances Hazardous to
Health Regulations.
2
2.2.INTRODUCTION
Many processes in chemical engineering require the separation of one or more of the
components of a liquid mixture by treating the mixture with an immiscible solvent in
which these components are preferentially soluble. In some cases purification of a
liquid may be the function of the process, in others the extraction of a dissolved
component for subsequent processing may be the important aspect. An example of the
former is the preparation of pure organic liquids from products of the oil industry.
Liquid/liquid extractions may also be used as energy-saving processes by, for example,
eliminating distillation stages. It is possible, of course that the substance of interest may
be heat-sensitive anyway and that distillation is accordingly an unacceptable process.
The rate at which a soluble component is transferred from one solvent to another will
be dependent, amongst other things on the area of the interface between the two
immiscible liquids. Therefore it is very advantageous for this interface to be formed by
droplets and films, the situation being analogous to that existing in packed distillation
columns. The Armfield Liquid/Liquid Extraction Unit takes the form of a vertically-
oriented packed column which may be operated either, by filling the column with water
and allowing a solvent to flow down the column over the packing, or filling the column
with solvent and allowing water to flow up the column over the packing. In either case
the process is continuous, both liquids being pumped into the column. Sensing
electrodes at the top and bottom of the column determine whether the column is filled
with water or with solvent. This is achieved by sensing and maintaining the position of
the water level at the appropriate height. A solenoid valve controlling the flow of
solvent under gravity from the column is operated by the sensing electrode system.
A distillation unit with a fractionating column is included to allow the reclamation of

solvent where appropriate.
3
2.3.DESCRIPTION
All numerical references relate to the Equipment Diagram on page 11 and the
Component System Diagram on page 12 and in the experimental section of this manual.
All letter coded references relate to the Control and Instrumentation System Diagram
on page 13 and in the experimental section of this manual.
The equipment is mounted in a floor-standing, welded steel framework (8) fitted with
adjustable feet (12). The frame contains an extra cross-member (9) at the front and a
similar one at the rear to allow the use of a fork-lift truck. The glass liquid/liquid
extraction column (19a & 19b) is fitted with enlarged end sections (14), (25), which are
closed by stainless steel plates (13), (26), the lower one being bolted to the framework
and supporting the column. The four sections of the column proper and the two end
plates are all fastened together with flanges (15), the joints between the sections being
sealed with moulded PTFE gaskets. The column is filled with Raschig rings which are
supported on a perforated stainless steel plate (16) fitted between the bottom enlarged
portion and the lower section of the column. Water for the column is stored in the
supply tank (37) (L2) from where it is pumped by the centrifugal pump (4), through an
air bleed valve (5) (V3), a flow control valve (23) (C1) and a flowmeter (24) (F1) to an
injector (28) mounted in the baseplate and with its exit about 150mm above the plate.
Water leaves the top of the column through a pipe, and is collected in a polythene tank
(40) (L1).
All storage tanks for solvent are constructed in stainless steel. The organic solvent
supply tank (3) (L5) provides the feed for the solvent metering pump (43) (F2), the
pumping rate of which is varied by a stroke adjustment knob (1) and indicated by a dial
calibrated from 1 – 10 where 10 is the maximum flow (nominally 380ml/min at 50Hz).
Pumped solvent enters the top of the column via an injector similar to that fitted at the
base for the water (28). A sampling and drain cock (2) (V6) is fitted in the solvent feed
line.
4
NOTE: The stroke adjustment knob on the metering pump must only be adjusted
when the pump is running. The smaller clamping knob must be unscrewed before
making an adjustment then tightened again when the adjustment knob is in the
required position (scale is calibrated 1 – 10).
A 3-way valve (V8) at the discharge of the solvent pump allows the flow from the
pump to be collected in a calibrated vessel (not supplied) so that the pump can be
calibrated. Calibration is
recommended so that a known flow of solvent through the column can be set
(procedure is described in the experimental section of this manual).
Solvent from the base of the column is returned under gravity to the receiver vessel
(36) (L3) via a pipeline (27) which is also fitted with a solenoid valve (6) (C3) and a
sampling cock V9).
The level of the water/solvent interface in the column is determined by the operation of
the solenoid valve (6) (C3) in the solvent outlet pipeline. The operation of this valve is
controlled by water-sensing electrodes, one set fitted to the top plate (31) and another
set to the bottom plate (11). A switch (S2) on the system control panel (34) (see also
diagram of the panel) selects the electrodes in use and hence determines whether the
interface is at the top or bottom of the column. Each electrode set consists of three
stainless steel electrodes, a bare earth electrode to make continuous contact with the
water and two others of different lengths insulated to points 5mm from their ends.
These insulated electrodes are set to heights differing by 5mm which produces a liquid
level differential of 5mm. The purpose of this arrangement is to avoid frequent opening
and closing of the solenoid valve which would occur with a simple single-electrode
system. The electrical sensing system operates at a low AC voltage and the conduction
current through the water is small, the latter being translated into a solenoid-operating
voltage by a plug-in module behind the control panel.
The receiver vessel (36) (L3) may be connected to the solvent supply vessel via a
pipeline and a valve (38) (V4). Thus, liquid which has passed through the column once
may be treated again in a batch wise fashion or the valve (38) (V4) may be left open
5
during the extraction to provide a closed circuit, the solvent then being recirculated
continuously.
The distillation column boiler (20) (L6), mounted behind the extraction column, is
fitted at such a height that liquid may be drained into it from the upper of the three
solvent tanks and can be drained from it into the lowest tank. The valve (18) (V7)
controls the release of solvent into the boiler. Like pipe work, valves and fittings, the
boiler is constructed in tainless steel. Heating is by means of two 500W cartridge
elements inserted at the base of the boiler and boiler temperature is indicated on a
thermometer in the side. The boiler lid is perforated where the distillation column is
fitted (35) and three blind tapped holes around this area accept bolts fixing the column
flange to the boiler.
The column proper is made up of a glass section (22) containing four sieve plates. The
glass reflux divider (33) bolts to the column top and to the stainless steel condenser
above it with bolts and flanges and all the sections are sealed together with molded
PTFE gaskets.
The reflux divider is fitted with a thermometer (30) (T2) to indicate the vapors
temperature beneath the divider. The condensate outlet tube and the thermometer tube
on the divider are terminated with glass screw-thread connectors and screw caps to
form secure but demountable connections. The
condenser (29) is vented to atmosphere at the top and its jacket is water-cooled by a
supply via the copper pipes
(32) at the rear. The boiler, distillation column and condenser are all lagged to minimise
heat losses.
3. Condensate from the reflux divider flows under gravity into the middle solvent tank
(39 (L4) via the flow control valve (17) (C2) which thus determines the reflux ratio.
The contents of the middle tank (39) (L4) can be drained into the solvent supply tank
by opening the valve (41) (V5) between the two.
6
The three solvent tanks (36) (L3), (39) (L4), (3) (L5) are vented to atmosphere through
a vent pipe which is inserted into the top of the condenser. Solvent levels in the tanks
and boiler are indicated with glass sight tubes protected by clear polyethylene sleeves.
Control of the equipment is simplified with a system diagram panel (34) shown in
detail on page 12. The complete solvent/water flow system is shown with electrical
controls at the appropriate points on the diagram. These are mains on/off switch (S1),
water pump on/off switch (S3), solvent pump on/off switch (S4), boiler heater switch
(S5) and power regulator (R1), electrode changeover switch (S2), and solenoid valve
'open' indicator light. The four mains supply switches are self-illuminating in the 'on'
position. A mains transformer (42) is supplied when the electrical supply is 120V,
60Hz A.C.
7
2.4.GENERAL SAFETY RULES
1 Follow Relevant Instructions
Before attempting to install, commission or operate equipment, all relevant
suppliers/manufacturers instructions and local regulations should be understood and
implemented.
It is irresponsible and dangerous to misuse equipment or ignore instructions,
regulations or warnings.
Do not exceed specified maximum operating conditions (e.g. temperature, pressure,
speed etc.)
2 Installation
a. Use lifting tackle where possible to install heavy equipment. Where manual lifting
is necessary beware of strained backs and crushed toes. Get help from an assistant if
necessary.
Wear safety shoes where appropriate.

b. Extreme care should be exercised to avoid damage to the equipment during
handling and unpacking. When using slings to lift equipment ensure that the slings
are attached to structural framework and do not foul adjacent pipework, glassware
etc. When using fork lift trucks, position the forks beneath structural framework
ensuring that the forks do not foul adjacent pipework, glassware etc. Damage may
go unseen during commissioning creating a potential hazard to subsequent
operators.
c. Where special foundations are required follow the instructions provided and do not
improvise. Locate heavy equipment at low level.
d. Equipment involving inflammable or corrosive liquids should be sited in a
containment area or bund with a capacity 50% greater than the maximum
equipment contents.
e. Ensure that all services are compatible with the equipment and that independent
isolators are always provided and labelled. Use reliable connections in all instances,
do not improvise.
8
f. Ensure that all equipment is reliably earthed and connected to an electrical supply
at the correct voltage. The electrical supply must incorporate a Residual Current
Device (RCD) (alternatively called an Earth Leakage Circuit Breaker - ELCB) to
protect the operator from severe electric shock in the event of misuse or accident.
g. Potential hazards should always be the first consideration when deciding on a
suitable location for equipment. Leave sufficient space between equipment and
between walls and equipment.
3 Operation
g. Ensure that students are fully aware of the potential hazards when operating
equipment.
h. Students should be supervised by a competent member of staff at all times when in
the laboratory. No one should operate equipment alone. Do not leave equipment
running unattended.
i. Do not allow students to derive their own experimental procedures unless they are
competent to do so.
j. Serious injury can result from touching apparently stationary equipment when
using a stroboscope to `freeze´ rotary motion.
4 Maintenance
a. Badly maintained equipment is a potential hazard. Ensure that a competent
member of staff is responsible for organizing maintenance and repairs on a
planned basis.
b. Do not permit faulty equipment to be operated. Ensure that repairs are carried
out competently and checked before students are permitted to operate the
equipment.
5 Using Electricity
a. At least once each month, check that RCD's (ELCB's) are operating correctly
by pressing the TEST button. The circuit breaker must trip when the button is
pressed (failure to trip means that the operator is not protected and a repair must
be effected by a competent electrician before the equipment or electrical supply
is used).
9
b. Electricity is the commonest cause of accidents in the laboratory. Ensure that
all members of staff and students respect it.
c. Ensure that the electrical supply has been disconnected from the equipment
before attempting repairs or adjustments.
d. Water and electricity are not compatible and can cause serious injury if they
come into contact. Never operate portable electric appliances adjacent to
equipment involving water unless some form of constraint or barrier is
incorporated to prevent accidental contact.
e. Always disconnect equipment from the electrical supply when not in use.
6 Avoiding fires or explosion

a. Ensure that the laboratory is provided with adequate fire extinguishers
appropriate to the potential hazards.
b. Where inflammable liquids are used, smoking must be forbidden. Notices
should be displayed to enforce this.
c. Beware since fine powders or dust can spontaneously ignite under certain
conditions. Empty vessels having contained inflammable liquids can contain
vapour and explode if ignited.
d. Bulk quantities of inflammable liquids should be stored outside the laboratory
in accordance with local regulations.
e. Storage tanks on equipment should not be overfilled. All spillages should be
immediately cleaned up, carefully disposing of any contaminated cloths etc.
Beware of slippery floors.
f. When liquids giving off inflammable vapours are handled in the laboratory, the
area should be ventilated by an ex-proof extraction system. Vents on the
equipment should be connected to the extraction system.
g. Students should not be allowed to prepare mixtures for analysis or other
purpose without competent supervision.
8 Handling poisons, corrosive or toxic materials
a. Certain liquids essential to the operation of equipment, for example mercury,
are poisonous or can give off poisonous vapours. Wear appropriate protective
10
clothing when handling such substances. Clean up any spillage immediately and
ventilate areas thoroughly using extraction equipment. Beware of slippery
floors.
b. Do not allow food to be brought into or consumed in the laboratory. Never use
chemical beakers as drinking vessels.
c. Where poisonous vapours are involved, smoking must be forbidden. Notices
should be displayed to enforce this.
d. Poisons and very toxic materials must be kept in a locked cupboard or store and
checked regularly. Use of such substances should be supervised.
e. When diluting concentrated acids and alkalis, the acid or alkali should be added
slowly to water while stirring. The reverse should never be attempted.
9 Avoiding cuts and burns
a. Take care when handling sharp edged components. Do not exert undue force on
glass or fragile items.
b. Hot surfaces cannot in most cases be totally shielded and can produce severe
burns even when not `visibly hot´. Use common sense and think which parts of
the equipment are likely to be hot.
10 Eye protection
a. Goggles must be worn whenever there is a risk to the eyes. Risk may arise from
powders, liquid splashes, vapours or splinters. Beware of debris from fast
moving air streams. Alkaline solutions are particularly dangerous to the eyes.
b. Never look directly at a strong source of light such as a laser or Xenon arc
lamp. Ensure that equipment using such a source is positioned so that passersby
cannot accidentally view the source or reflected ray.
c. Facilities for eye irrigation should always be available.
11 Ear protection
a. Ear protectors must be worn when operating noisy equipment.
12 Clothing
11
a. Suitable clothing should be worn in the laboratory. Loose garments can cause
serious injury if caught in rotating machinery. Ties, rings on fingers etc. should
be removed in these situations.
b. Additional protective clothing should be available for all members of staff and
students as appropriate.
13 Guards and safety devices
a. Guards and safety devices are installed on equipment to protect the operator.
The equipment must not be operated with such devices removed.
b. Safety valves, cut-outs or other safety devices will have been set to protect the
equipment. Interference with these devices may create a potential hazard.
c. It is not possible to guard the operator against all contingencies. Use common
sense at all times when in the laboratory.
d. Before starting a rotating machine, make sure staff are aware how to stop it in
an emergency.
e. Ensure that speed control devices are always set at zero before starting
equipment.
14 First aid
a. If an accident does occur in the laboratory it is essential that first aid equipment
is available and that the supervisor knows how to use it.
b. A notice giving details of a proficient first-aider should be prominently
displayed.
c. A `short list´ of the antidotes for the chemicals used in a particular laboratory
should be prominently displayed.
SOLVENT/SOLUTE SYSTEMS FOR USE WITH UOP5
Two systems are recommended for use with UOP5:

Trichloroethylene, Propionic acid and water
Leksol, Propionic acid and water
12
Leksol is a non-flammable solvent consisting mainly (approx 95%) of n-propyl
bromide. Leksol is obtainable from Conservation Resources International (Information
available from http://www.conservationresources.com/).
CALIBRATING THE SOLVENT METERING PUMP
Because of tolerances in manufacture and assembly of the solvent metering pump the
flow rate will vary slightly from pump to pump at a given setting of the stroke adjuster.
To allow experiments to be conducted at a known flow rate it is recommended that the
following procedure is adopted to obtain a calibration graph for the pump. The graph
obtained can be used in subsequent experiments without the need to repeat the
procedure.
Set valve V8 to the calibrate position and place a suitable container below the outlet on
valve V8. Start the solvent metering pump then set the stroke adjuster to maximum
flow rate (set F2 to10 on the dial). When the pump and pipe work have fully primed use
a measuring cylinder (not supplied) and stopwatch (not supplied) to determine the
actual flow rate in ml/min and record the flow rate obtained at a setting of 10 on the
dial. Change the setting to 9 on the dial. Repeat the procedure to measure and record
the actual flow rate. Repeat this procedure for settings of 8, 7, 6, 5, 4, 3, 2 & 1 on the
dial.
Plot a graph of flow rate in ml/min against setting of the stroke adjuster (1 -10).
Thereafter any required flow rate may be obtained by using the graph and setting the
stroke adjuster to the appropriate position.
13
2.5.INDEX TO EXPERIMENTS
EXPERIMENT A
Determination of Distribution Coefficient
EXPERIMENT B
Basic Operation of the Liquid/Liquid Extraction Column
EXPERIMENT C
Overall Mass Balance and Mass Transfer Coefficients with the
Aqueous Phase as the Continuous Medium
EXPERIMENT D
Overall Mass Balance and Mass Transfer with the Organic
Phase as the Continuous Medium
EXPERIMENT E
Demonstration of Solvent Recovery
14
2.5.1. EXPERIMENT A
2.5.1.1.OBJECT OF EXPERIMENT:
To determine the distribution coefficient for the system organic solvent-
Propionic Acid-Water and to show its dependence on concentration.
The following apparatus is required:
250ml Conical stoppered flask

250ml Measuring cylinder
250ml Separating funnel
Pipette with rubber bulb
Sodium Hydroxide Solution (0.1 M)
Phenolphthalein
Propionic acid
WARNING Ensure that diluted Sodium Hydroxide (NaOH) is used when performing
this experiment.
The solvent (water) and solution (organic solvent/propionic acid) are mixed together
and then allowed to separate into the extract phase and the raffinate phase. The extract
phase will be water and propionic acid and the raffinate, organic solvent with a trace of
propionic acid.
The distribution coefficient, K, is defined as the ratio
Concentration of solute in the extract phase, Y

Concentration of solute in the raffinate phase, X
15
It is assumed that equilibrium exists between the two phases.
At low concentrations, the distribution coefficient is dependent on the concentration
and thus Y = KX.
1. Make up in a conical flask a mixture of 50ml organic solvent and 50ml of
demineralized water.
2. Add 5ml of propionic acid. 5ml can be pipetted into the flask using a pipette with a
rubber bulb.
3. Place a stopper into the flask and shake for a minimum of 5 minutes.
4. Pour into a separating funnel, leave for 5 minutes and remove the lower aqueous
layer.
5. Take a 10ml sample of this layer and titrate against 0.1 M sodium hydroxide solution
using phenolphthalein as indicator.
6. Repeat the experiment for two further concentrations of propionic acid i.e. for initial
additions of 3ml and 1ml of propionic acid.
2.5.1.4.RESULTS:
Propionic Acid added (ml)
Titre of M/10 NaOH
Propionic Acid
Concentration in
Aqueous Layer, Y
Propionic Acid
Concentration in
Organic Layer, X
K=Y/X
16
2.5.2. EXPERIMENT B
To observe the hydraulics of counter current flow in a packed column.
The experiment will be carried out using the two immiscible liquids organic solvent
and water and the column will be operated in the following two modes:
(a) The aqueous phase as the continuous medium.
(b) The organic phase as the continuous medium.
It is normal to operate a column so that the continuous phase 'wets' the packing. If the
acking is 'wetted' by the dispersed phase then coalescence will be increased and the
mass ransfer/unit volume will be reduced. The rate of mass transfer of a solute from
one phase to another is normally increased with greater throughput of material, because
of increased turbulence giving better mixing. There is however, a limit to the maximum
amount of material that can be fed through the column. The limit is called the 'Flooding
Point' and occurs at specific flow rates of constituents resulting in one of the phases
being rejected from the column.
2.5.2.4.PROCEDURE:
(a) The Aqueous Phase as the Continuous Phase

1. Set the level control (electrode switch S2) to the central (OFF) position.
2. Fill the organic phase feed tank (bottom tank) with 10 litres of trichloroethylene.
17
3. Fill the water feed tank with 15 litres of clean de-mineralised water then start the
water feed pump (switch S3) and fill the column with water at a high flow rate.
4. As soon as the water is above the top of the packing, reduce the water flow rate to
200 ml/min. Start the organic phase metering pump (switch F4) and set a flow rate of
200 ml/min by adjusting the dial (F2) on the pump (refer to the calibration graph
obtained earlier to determine the required setting on the dial).
Drops of solvent will flow downwards through the packing and collect at the base of
the column.
5. Eventually water will overflow from the top of the column into the water collection
tank (L1). Gradually, the level of the solvent will increase at the base of the column.
When the interface between the solvent and the water is just above the middle height
level electrode, set the level control (electrode switch S2) to the BOTTOM position.
The solenoid valve (C3) will open (Red indicator illuminated on the control panel) and
solvent will flow from the base of the column to the top solvent collection tank (L3)
under gravity.
6. The solenoid valve will open and close at intervals to maintain the interface between
the lowest and middle level electrode.
7. Slowly increase both water and organic solvent flow rates in small steps and note
where flooding occurs in the packing.
(b) The Organic Phase as the Continuous Phase

8. Empty the column and return the organic solvent and water into their respective feed
tanks. This is achieved by allowing the weight of the water to push the organic solvent
to the solvent collection tank (top tank L3); this may mean adding more water with the
level control (electrode switch S2) set to the TOP position. Drain water from the
column and tank L1 via the drain valves. Refill water tank L2.
18
10. Start the metering pump (switch S4) and fill the column quickly with solvent at
high flowrate. When the solvent reaches the top of the packing reduce the flow to 200
m1/min by adjusting the dial (F2) on the pump (refer to the calibration graph obtained
earlier to determine the required setting on the dial).
11. Start the water pump (switch S3) and adjust the flow to 200 ml/min. Drops of water
will flow upwards through the packing and collect on top of the solvent.
12. Gradually, the level of the water will increase on top of the solvent and the interface
between the water and solvent will rise... Eventually water will overflow from the top
of the column into the water collection tank (L1).
13. When the interface between the solvent and the water is just above the middle
height level electrode, set the level control (electrode switch S2) to the TOP position.
solvent will flow from the base of the column to the top solvent collection tank (L3).
14. Slowly increase both flow rates in small steps until flooding occurs.
2.5.2.5.RESULTS:
Observe if there is any difference between operating with the aqueous phase as the
continuous medium compared with the organic phase as the continuous medium.
Is there any difference in droplet size?
Also observe what happens as the flow rates are increased.
Does flooding occur, if so at what flow rates?
19
2.5.3. EXPERIMENT C
To demonstrate how a mass balance is performed on the extraction column, and
to measure the mass transfer coefficient with the aqueous phase as the
continuous medium.
Let Vw = Water flow rate (l/s)

Vo = Organic solvent flow rate (l/s)
X = Propionic Acid concentration in the organic phase (kg/l)
Y = Propionic Acid concentration in the aqueous phase (kg/l)
Subscripts: 1 = Top of column
2 = Bottom of column
1. Mass Balance
Propionic Acid extracted from the organic phase (raffinate) = Vo (X1-X2)
Propionic Acid extracted by the aqueous phase (extract) = Vw(Y1-0)
Therefore Vo(X1-X2) = Vw(Y1-0)
2. Extraction Efficiency
Mass transfer coefficient (based on the raffinate phase) Rate of Acid Transfer
/Volume of Packing x Mean Driving Force
Log mean driving force = x1 x2) /1n( x1/ x 2)
where _X1 = Driving force at the top of the column = (X2-0)

_X2 = Driving force at the bottom of the column = (X1-X1*) where X1* is the
concentration in the organic phase which would be in equilibrium with concentration
20
Y1 in the aqueous phase. The equilibrium values can be found using the distribution
coefficient found in the first experiment.
2.5.3.3.PROCEDURE:
1. Add 100ml of propionic acid to 10 litres of the organic phase. Mix well to ensure an
even concentration then fill the organic phase feed tank (bottom tank) with the
mixture.
3. Fill the water feed tank with 15 litres of clean de-mineralised water, start the water
feed pump (switch S3) and fill the column with water at a high flow rate.
4. As soon as the water is above the top of the packing, reduce the flow rate to 200
ml/min. Start the organic phase metering pump (switch F4) and set a flow rate of 200
l/min by adjusting the dial (F2) on the pump (refer to the calibration graph obtained
earlier to determine the required setting on the dial).
Drops of solvent will flow downwards through the packing and collect at the base of
the column.
5. Eventually water will overflow from the top of the column into the water collection
tank (L1). Gradually, the level of the solvent will increase at the base of the column.
When the interface between the solvent and the water is just above the middle height
level electrode, set the level control (electrode switch S2) to the BOTTOM position.
solvent will flow from the base of the column to the top solvent collection tank (L3).
6. The solenoid valve will open and close at intervals to maintain the interface between
the lowest and middle level electrode.
21
7. Run for approximately 40 minutes until steady conditions are achieved, monitor flow
rates during this period to ensure that they remain constant.
7. Take 15ml samples from the feed, raffinate and extract streams. DO NOT use the
calibration valve V8 for taking feed samples.
8. Titrate 10ml of each sample against 0.1 M NaOH using phenolphthalein as the
indicator. (To titrate the feed and raffinate they may need continuous stirring using a
magnetic stirrer. Alternatively: 0.025 M NaOH may be used which will lead to phase
inversion of the raffinate and feed streams so that the aqueous phase is the continuous
phase).
this experiment.
2.5.3.4.RESULTS:
Flow rate of Aqueous Phase
Flow rate of Organic Phase
Titre of M/10 NaOH
Concentration of Propionic Acid kg/l
Feed
Raffinate
Extract
Propionic acid extracted from the organic phase
Propionic acid extracted from the aqueous phase
Mass Transfer Coefficient
22
2.5.4. EXPERIMENT D
To demonstrate how a mass balance is performed on the extraction column, and
to measure the mass transfer coefficient with the organic phase as the
continuous medium.
Let Vw = Water flow rate (l/s)
Vo = Organic phase flow rate (l/s)
X = Propionic Acid concentration in the organic phase (kg/l)
Y = Propionic Acid concentration in the aqueous phase (kg/l)
Subscripts: 1 = Top of column
2 = Bottom of column
1. Mass Balance
Propionic Acid extracted from the organic phase (raffinate) = Vo (X1-X2)
Propionic Acid extracted by the aqueous phase (extract) = Vw(Y1-0)
Therefore Vo(X1-X2) = Vw(Y1-0)
2. Extraction Efficiency
Mass transfer coefficient (based on the raffinate phase) Rate of Acid Transfer
/Volume of Packing x Mean Driving Force
Log mean driving force = Δx1- Δx2/ 1n Δx1/Δx 2
where _X1 = Driving force at the top of the column = (X2-0)

_X2 = Driving force at the bottom of the column = (X1-X1*) where X1* is the
concentration in the organic phase which would be in equilibrium with concentration
Y1 in the aqueous phase. The equilibrium values can be found using the distribution
coefficient found in the first experiment.
23
this experiment.
2.5.4.3.PROCEDURE:
1. Add 100ml of propionic acid to 10 litres of the organic solvent. Mix well to ensure
an even concentration then fill the organic phase feed tank (bottom tank) with the
mixture.
3. Fill the water feed tank with 15 litres of clean de-mineralised water.
4. Start the metering pump (switch S4) and fill the column quickly with solvent at high
lowrate. When the solvent reaches the top of the packing reduce the flow to 200 ml/min
by adjusting the dial (F2) on the pump (refer to the calibration graph obtained earlier to
determine the required setting on the dial).
5. Start the water pump (switch S3) and adjust the flow to 200 ml/min. Drops of water
will flow upwards through the packing and collect on top of the solvent.
6. Gradually, the level of the water will increase on top of the solvent and the interface
between the water and solvent will rise. Eventually water will overflow from the top of
the column into the water collection tank (L1).
24
Exp# 3
Distillation
25
3.1.INTRODUCTION
3.1.1. DISTILLATION PRINCIPLES
Separation of components from a liquid mixture via distillation depends on the

differences in boiling points of the individual components. Also, depending on the
concentrations of the components present, the liquid mixture will have different boiling
point characteristics. Therefore, distillation processes depends on the vapour pressure
characteristics of liquid mixtures.
3.1.2. VAPOUR PRESSURE AND BOILING
The vapour pressure of a liquid at a particular temperature is the equilibrium

pressure exerted by molecules leaving and entering the liquid surface the vapour
pressure and hence the boiling point of a liquid mixture depends on the relative
amounts of the components in the mixture distillation occurs because of the differences
in the volatility of the components in the liquid mixture
3.1.2.1. The Boiling Point Diagram

The boiling point diagram shows how the
equilibrium compositions of the
components in a liquid mixture vary with
temperature at a fixed pressure. Consider
an example of a liquid mixture
containing 2 components (A and B) - a
binary mixture. This has the following
boiling point diagram. The boiling point
of A is that at which the mole fraction of
A is 1. The boiling point of B is that at
which the mole fraction of A is 0. In this
example, A is the more volatile component and therefore has a lower boiling point than
B. The upper curve in the diagram is called the dew-point curve while the lower one is
called the bubble-point curve.
26
The dew-point is the temperature at which the saturated vapour starts to condense.
The bubble-point is the temperature at which the liquid starts to boil.
The region above the dew-point curve shows the equilibrium composition of the
superheated vapour while the region below the bubble-point curve shows the
equilibrium composition of the subcooled liquid. This difference between liquid and
vapour compositions is the basis for distillation operations.
3.1.2.2. Relative Volatility
Relative volatility is a measure of the differences in volatility between 2

components, and hence their boiling points. It indicates how easy or difficult a
particular separation will be. The relative volatility of component ‘i’ with respect to
component ‘j’ is defined as
y
x 
 ij =  i  (1.2)
 yj 
 
 x j 
yi = mole fraction of component ‘i’ in the vapour

xi = mole fraction of component ‘i’ in the liquid
Thus if the relative volatility between 2 components is very close to one, it is an

indication that they have very similar vapour pressure characteristics. This means that
they have very similar boiling points and therefore, it will be difficult to separate the
two components via distillation.
3.1.3. TYPES OF DISTILLATION COLUMNS
There are many types of distillation columns, each designed to perform specific types
of separations, and one way of classifying distillation column type is to look at how
they are operated. Thus we have:
• batch and
27
• Continuous columns:
Continuous columns can be further classified according to:
The nature of the feed that they are processing,
binary column - feed contains only two component
multi-component column - feed contains more than two components
The number of product streams they have

Multi-product column - column has more than two product streams
Extractive distillation - where the extra feed appears in the bottom product stream
Azeotropic distillation - where the extra feed appears at the top product stream
3.1.4. MAIN COMPONENTS OF DISTILLATION COLUMNS
Distillation columns are made up of several components, each of which is used either to
transfer heat energy or enhance material transfer. A typical distillation contains several
major components:
• A vertical shell where the separation of liquid components is carried out.
• Column internals such as trays/plates and/or packing which are used to enhance
component separations.
• A reboiler to provide the necessary vaporisation for the distillation process.
• A condenser to cool and condense the vapour leaving the top of the column.
• Refluxes drum to hold the condensed vapour from the top of the column so that
liquid (reflux) can be recycled back to the column.
The vertical shell houses the column internals and together with the condenser and
reboiler, constitutes a distillation column. A schematic of a typical distillation unit with
a single feed and two product streams is shown below
28
Figure 1.1 shows schematic of a typical distillation unit with a single feed and two product
streams
3.1.5. LIQUID AND VAPOUR FLOWS IN A TRAY COLUMN
Figures (1.2 & 1.3) show the direction of vapour and liquid flow across a tray, and
across a column.
Figure 1.2 Figure1.3
Each tray has 2 conduits, one on each side, called ‘downcomers’. Liquid falls through
the downcomers by gravity from one tray to the one below it. A weir on the tray
29
ensures that there is always some liquid (holdup) on the tray and is designed such that
the the holdup is at a suitable height.
Being lighter, vapour flows up the column and is forced to pass through the liquid, via
the openings on each tray. The area allowed for the passage of vapour on each tray is
called the active tray area.
3.1.6. FACTORS AFFECTING DISTILLATION COLUMN
OPERATION
The performance of a distillation column is determined by many factors, for example:
• Feed conditions
• State of feed
• Composition of feed
• Trace elements that can severely affect the VLE of liquid mixture
• Internal liquid and fluid flow conditions
• State of trays (packings)
• Weather conditions
Some of these will be discussed below to give an idea of the complexity of the
distillation process.
3.1.6.1. Feed Conditions
The state of the feed mixture and feed composition affects the operating lines and hence
the number of stages required for separation. It also affects the location of feed tray.
3.1.6.2. Reflux Conditions
As the reflux ratio is increased, the gradient of operating line for the rectification
section moves towards a maximum value of 1. Physically, what this means is that more
and more liquid that is rich in the more volatile components are being recycled back
into the column. Separation then becomes better and thus fewer trays are needed to
30
achieve the same degree of separation. Minimum trays are required under total reflux
conditions, i.e. there is no withdrawal of distillate.
On the other hand, as reflux is decreased, the operating line for the rectification section
moves towards the equilibrium line. The ‘pinch’ between operating and equilibrium
lines becomes more pronounced and more and more trays are required. This is easy to
verify using the McCabe-Thiele method.
The limiting condition occurs at minimum reflux ration, when an infinite number of
trays will be required to effect separation. Most columns are designed to operate
between 1.2 to 1.5 times the minimum reflux ratios because this is approximately the
region of minimum operating costs (more reflux means higher reboiler duty).
3.1.6.3. Vapour Flow Conditions

Adverse vapour flow conditions can cause
• Foaming.
• Entrainment.
• Weeping/dumping.
• Flooding.
3.1.6.4. Column Diameter

Vapour flow velocity is dependent on column diameter. Weeping determines the
minimum vapour flow required while flooding determines the maximum vapour flow
allowed, hence column capacity. Thus, if the column diameter is not sized properly, the
column will not perform well. Not only will operational problems occur, the desired
separation duties may not be achieved.
3.1.6.5. State of Trays and Packings

The actual number of trays required for a particular separation duty is determined by
the efficiency of the plate, and the packings if packings are used. Thus, any factors that
cause a decrease in tray efficiency will also change the performance of the column.
31
Tray efficiencies are affected by fouling, wear and tear and corrosion, and the rates at
which these occur depends on the properties of the liquids being processed. Thus
appropriate materials should be specified for tray construction.
3.1.6.6. Weather Conditions
Most distillation columns are open to the atmosphere. Although many of the columns
are insulated, changing weather conditions can still affect column operation.
3.2. DESCRIPTION
All numerical referees relate to the figures (2.1, 2.2 2.3)
The equipment comprises a 50 mm diameter sieve plate column made up of two glass
sections (3) and (4) each containing four sieve plates. The columns are separated by a
central feed section and arranged vertically for counter-current vapor/liquid flow. Also
installed within the framework are:
Reboiler (13)
Two 5 litre feed tanks (5), (6)
Peristaltic type feed pump (7)
Condenser (8)
Bottom (9) and top (10) product tanks
Decanter (11)
Reflux valve (12)
Azeotropic dosing vessel (24)
Vacuum pump (20)
The Reboiler (13) situated at the base of the column is manufactured from 316 stainless
steel and incorporators a flameproof immersion type heating element. Either each batch
or continuous distillation can be carried out using this reboiler.
32
In continous operation, valve (V1) is open and bottom product flows from the reboiler
through the bottom product cooler (15) to the bottom product tank (9). It is possible to
preheat the feed to the column by directing the feed through a spiral coil in the bottom
product cooler where heat is transferred from product leaving the reboiler at the boiling
point.
For batch operation, valve (V1) remains closed so that the reboiler can be filled with
initial charge (10 to 12 litres) of binary mixture.
A level sensor (17) inside the reboiler protects the heating element from overheating
due to low operating level and a sign glass 18 allows the level in the reboiler to be
observed.
Feed mixture from either of the feed tanks is pumped by pump (7) to the base, centre or
top of the distillation column at connections (A), (B) or (C).
The glass column incorporates a total of eight sieve plates in two sections (3) and (4)
each containing four plates. Each plate (D) is located by a central support rod (E) and
incorporates a weir (F) and downcomer (G) to create a liquid seal between successive
stages.
Vapor from the top of the column passes to a water-cooled, coil –in-shell condenser (8).
The shell of the condenser incorporated a pressure relief valve (PRV1) to protect the
system in the event of a blocked vent and cooling water failure.
Condensate is collected in a glass decanter (11) (phase separator) which is by-passed
for normal distillation experiments by opening valve (V10).
With valve (V10) open, condensate from the condenser outlet passes directly through
the decanter to the inlet of the reflux ratio control valve (12) which is a 3-way solenoid
operated valve. Depending on the reflux timers, condensate is directed by the reflux
valve either back to the top of the column or to the top product collecting vessel (10).
Temperatures within the system are monitored by fourteen thermocouple sensors (T1 to
T14). The total pressure drop across the column is indicated on a U-tube manometer
(P1) via appropriate tappings in the column fitted with isolating valves (V6) and (V7).
33
Figure 2.1
34
Figure 2.2
35
Figure 2.3
36
3.3. OPERATIONAL PROCEDURES
3.3.1. Control console
37
3.3.2. Reflux Ratio Control
The reflux ratio timer on the control console is used to set the quantity and frequency of
condensate returning to the distillation column. With the timer switched off, all of the
condensate will be directed to the column (total reflux).
Pressure drop in column
The overall pressure drop over the column can be measured using the manometer ∆P1.
Always open V6 before V7, take the pressure reading then immediately close both
valves. This will reduce the risk of contamination of the manometer water by the
hydrocarbons.
Reboiler
Heating of the liquid in the reboiler is achieved by an electrical heating element. The
maximum power of the element is 2.0 kW and this is adjustable at the control console.
3.3.3. EXPERIMENT A BATCH DISTILLATION
3.3.3.1. Objective
To determine the pressure drop over the distillation column for various boil-up rates
3.3.3.2. Equipment set-up:
38
3.3.3.3. Theory
The total pressure drop across each tray is the sum of that caused by the
restriction of the holes in the sieve tray, and that caused by passing through the liquid
(foam) on the top of the tray.
As the velocity of the vapors passing up the column increases then so does the overall
pressure drop. The velocity is controlled by varying the boil-up rate which is done by
varying the power input to the broiler. Under conditions with no liquid present, the
sieve trays will behave like an orifice in that the pressure drop will be proportional to
the square of the velocity. Due to the fact that there is a liquid head however, this
square relationship does not become apparent until the head of liquid has been
overcome and foaming is taking place.
39
3.3.3.4. Procedure
1. Before starting, make sure all valves on the equipment are closed
2. Open valve V10 on the reflux pipe.
3. Fill the boiler with 10 liters of mixture (methanol & water) to be distilled.
4. Turn on the power to the control panel and set the temperature selector switch to
T9 (the temperature in the reboiler).
5. Open valve V5 admitting the cooling water to the condenser at the flow rate on
F11 of approximately 3 liters/min.
6. On the control panel turn the power controller for the reboiler heating element
anti clockwise until a reading of approximately 0.5 kW is obtained on the digital
wattmeter.
7. When the equilibrium condition is reached the boil up rate can be measured by
operating valve V3 so that all the condensate is diverted into a measuring
8. Take reading of pressure drops over both the rectifying (top) and the stripping
(bottom) sections by opening the valves V6 & V7 on the manometer. (When
opening the valves, make sure always to open valve V6 then V7 to prevent
vapor from the column to entering the manometer).close the valves in the same
order, when finished the pressure drop reading.
9. Set up the boil-up rate in 250 Watt increments up to maximum 1.5 kW by

adjusting the boiler heater power controller.
40
3.3.3.5. Raw Data and Results Tables
Record your reading as follows:
Table 4.1 Raw Data for Experiment A
Boil-up Rate Pressure Drop (cm H2O) Degree of Foaming

Power (kW)
(litres/hr) Top Bottom Overall on Trays
The comment “ Degree of Foaming on Trays” should be filled in using descriptive

words e.g. None, gentle Localised, Violent Localised, Foaming Gently Over Whole
Tray, Foaming Violently Over Whole Tray, Liquid Flooding in Column.
3.3.3.6. Report Requirement
1. From the results, plot the curve relating pressure drop as a function of boil-up
rate on log/log graph paper.
2. Discuss the results and effect of Foaming, Flooding and weeping.
41
The final results should be reported in the following format
Table 4.2 Processed Data for Experiment A
Boil-up Rate Pressur Drop (cm H2O) Degree of

Power (kW)
(litres/hr) Top Bottom Overall Foaming on Trays
42
3.3.4. EXPERIMENT B BATCH DISTILLATION
3.3.4.1. Objective
Use the refractometer for determining mixture composition
3.3.4.2. Theory
It is essential to have a convenient quick method of determining the

composition of the binary mixture taken from the various sample points on the
distillation column. Such a method involves the use of a refractometer since the
refractive index of these mixtures varies with composition.
For the system Methanol/Water, mixtures of known concentration can be made
up and their refractive indexes measured. The refractometer measured the critical angle
of the liquid under test and each concentration will show a different critical angle.
3.3.4.3. The refractive index
The ratio of the velocity of light in vacuum to the velocity of light in a medium
is referred to as the medium's refractive index, denoted by the letter n.
Figure 4.1. Light incident on a glass plate. The reflected part of the ray is shown along with the
light path for the refracted component.
43
3.3.4.4. Procedure
1. Measure the refractive index (R.I) of pure methanol and pure water.
2. Make up small quantities of 25 mol percent, 50 mol percent, 75 mol percent
methanol and measure their R.I.
3. calculate the volume of constituents to use as follows:
For 25 mol percent methanol, ie. 75 mol percent water
Molecular weight of methanol = 32

Molecular weight of water = 18
Density of methanol = 0.791 g/ml

Density of water = 1 g/ml
Vol methanol X Methanol 100

M .WMethanol
25 = (4.1)
Vol Methanol  Methanol VolWater Water
+
M .WMethanol M .WWater
Thus
100
25 =
VolWater M .WMethanol 
1+   Water
Vol Methanol M .WWater  Methanol
Vol Water M.Wwater ρ

= 3Χ Χ Methanol
Vol Methanol M.WMethanol ρ Water
VolWater 18 0.791
= 3Χ Χ
VolMethanol 32 1
1 Vol Water = 1.3348 Vol Methanol
44
Table 4.3 Raw Data for Experiment B
Concentration of Methanol R.I.
100%
75%
50%
25%
0%
1. From the results, plot graph of refractive index versus mol percent methanol in
methanol/water mixture.
2. Discuss the results.
45
3.3.5. EXPERIMENT C BATCH DISTILLATION
3.3.5.1. Objective
To determine the overall column efficiency at varying boil-up rates
3.3.5.2. Equipment Set up
The equipment will be set up to operate at total reflux so that the charge of feed mixture
can be loaded directly into the reboiler.
3.3.5.3. Equipment
1. Distillation Column
2. Refractometer
3. 250 ml measuring cylinder graduated in mls.
4. stop watch
3.3.5.4.Chemicals/materials
1. Methanol
2. Deionized Water
46
3.3.5.5. Theory
To calculate the number of theoretical plates for a given separation at total; reflux
fenske developed the following formula:
 x   x  
log A  . B  
 x B  d  x A  b 
n +1 = (4.2)
log( AB )av
Where n = number of theoretical plates

xA = mole fraction of more volatile component
xB = mole fraction of more volatile component
av = average relative volatility
Subscripts d , b indicate distillate and bottom respectively
 av =  d . b (4.3)
The efficiency is given by,
Number of theoritical plates

E= Χ 100% (4.4)
Number of actual plates
Knowing the composition of distillate and bottom and the corresponding volatilities,
the column efficiency can be determined.
47
3.3.5.6. Procedure
anti clockwise until a reading of approximately 0.75 kW is obtained on the
digital wattmeter.
8. Take a sample of the overheads through valve V3. When doing that, be careful
never to drain the condensate return line.
9. Record the refractive index for the taken overhead sample.
10. Take a sample of the bottom through valve V2.
11. Record the refractive index for the taken bottom sample.
12. Repeat this procedure for several different boil-up rates to cover the operating
range of the column.
13. Determine the concentrations of the components in the taken samples by using
calibration graph (see experiment B).
48
Table 4.4 Raw Data for Experiment C
Boil-up Rate
Rectifying Stripping
(l/hr)
Temperature (ºC) Temperature (ºC)
T1 T5
T2 T6
T3 T7
T4 T8
Average
T1 T5
T2 T6
T3 T7
T4 T8
Average
1. Calculate the number of theoretical plates using eq. (4.2).

2. Calculate the efficiency using eq.(4.4).
49
Table 4.5 Processed Data for Experiment C
Boil-up
Rate Rectifying Stripping
(l/hr)
Temperature Temperature
R.I. (XA)d R.I. (XA)b
(ºC) (ºC)
T1 T5
T2 T6
T3 T7
T4 T8
Average Average
T1 T5
T2 T6
T3 T7
T4 T8
Average Average
50
3.4.4. EXPERIMENT D BATCH DISTILLATION
3.4.4.1. Objective
To carry out a distillation at constant reflux ratio-varying top and bottom compositions
with time.
3.4.4.3.Equipment
2. Refractometer
4. stop watch
1. Methanol
2. Deionized Water
51
3.4.4.5.Theory
Since there is no feed, no bottom product, the liquid flow in the column is equal to the
vapor flow in the column.
V =L (4.5)
A material balance over the M.V.C. (most volatile component) gives:
V y n = L x n +1 (4.6)
Since V = L this gives
yn = xn+1 (4.7)
3.4.4.6. Procedure
digital wattmeter.
7. Set the reflux controller to the desired value i.e start with 5:1, meaning 5 sec
back to column and 1 sec to top product receiver.
52
13. Record the temperatures T8 - T1 to calculate the average column temperature.
14. Repeat this procedure for different reflux ratio.
15. Repeat the whole procedure for several different boil-up rates to cover the
operating range of the column.
Table 4.6 Raw Data for Experiment D
Boil-up Rate
(l/hr)
Reflux Ratio =
T1 T5
T2 T6
T3 T7
T4 T8
Average Average
T Column average (ºC) =
Reflux Ratio =
T1 T5
T2 T6
53
T3 T7
T4 T8
Average Average
3.4.4.8.Report Requirement

2. Calculate the number of theoretical plates using tray-by-tray calculations.

3. Calculate the efficiency using.
Table 4.7 Processed Data for Experiment D
Boil-up Rectifying Stripping

Rate
(l/hr)
Reflux Ratio =
R.I. (XA)d Temperature R.I. (XA)b Temperature (ºC)
(ºC)
T1 T5
T2 T6
T3 T7
T4 T8
54
Average Average
Reflux Ratio =
R.I. (XA)d Temperature R.I. (XA)b Temperature (ºC)

(ºC)
T1 T5
T2 T6
T3 T7
T4 T8
Average Average
3.4.5. EXPERIMENT E CONTINUOUS DISTILLATION
3.4.5.1. Objective
Steady state distillation of a binary mixture under continuous operation.
55
3.4.5.3. Requirements
2. Refractometer
4. stop watch
5. Calibration curve for the feed pump.
6. Calibration graph for refractometer.
7. Equilibrium data for methanol/water at atmospheric pressure.
1. Methanol
2. Deionized Water
3.4.5.5.Theory
Calculation of number of plates using the LEWIS-SOREL method
56
Material Balance of top of column
Vn = Ln +1 + D
(4.8)
With respect to M.V.C. this becomes
ynVn = Ln +1 xn +1 + Dxd
Ln +1 D (4.9)
yn = xn +1 + xd
V Vn
Since the liquid overflow is constant Ln = Ln+1
Ln +1 D
yn = xn +1 + xd (4.10)
Vn Vn
Material Balance of bottom of column.
Vm = Lm +1 − W (4.11)
ymVm = Lm +1 xm +1 − Wxw
(4.12)
57
Lm +1 W
ym = xm +1 − xw (4.13)
Vm Vm
Since the liquid overflow is constant Lm = Lm+1
Lm +1 W
ym = xm +1 − xw (4.14)
Vm Vm
Equations (4.10) and (4.14) combined with the equilibrium curve can be used to
calculate the composition on the various plates working from the condenser down to
the still. The plate which has a composition nearest to that of the feed should be used as
the feed plate.
Consequently the number of theoretical plates and position of entry for the feed can be
calculated.
3.4.5.6. Procedure
1. the feed to the column must be admitted at the mid point (onto try 5)
digital wattmeter.
5. Start the experiment with total reflux.
6. Before switching on the reflux switch, Set the reflux ratio to 5:1, meaning 5 sec
7. When the column has stabilized at total reflux, the flow of feed and the reflux
can be started at the same time.
8. It is advisable to set a feed flow 2 litres/hr.
58
9. After feeding approximately 3 litres take a sample of the overheads through
valve V3. When doing that, be careful never to drain the condensate return line
ie . partially open V3 to leave a small amount of liquid in the line all the time.
15. repeat the sample taking a further three times during the experiment (before
feed runs out)
Table 4.8 Raw Data for Experiment E
No. Power (kW) Feed Position Feed Flow Reflux Ratio

Rate (l/hr)
59
2. Calculate the number of theoretical plates using the LEWIS-SOREL

method.
Table 4.9 Processed Data for Experiment E
Power (kW) =
Feed Position =
Feed Flow Rate (l/hr) =
Reflux Ratio =
Trial # 1
60
Trial # 2
Trial # 3
Trial # 4
Trial # 5
3.4.6. EXPERIMENT F CONTINUOUS DISTILLATION
3.4.6.1. Objective
Effect of varying the feed position under continuous operation.
3.4.6.2.Equipment Set up
61
3.4.6.3.Requirements
2. Refractometer
4. stop watch
5. Calibration curve for the feed pump.
6. Calibration graph for refractometer.
7. Equilibrium data for methanol/water at atmospheric pressure.
1. Methanol
2. Deionized Water
62
3.4.6.5. Theory
Calculation of number of plates using the LEWIS-SOREL method

Material Balance of top of column
Vn = Ln +1 + D − F
(4.15)

ynVn = Ln +1 xn +1 + Dxd − FxF
Ln +1 xn +1 D Fx (4.16)
yn = + xd − F
Vn Vn Vn
Since the liquid overflow is constant Ln = Ln+1
Ln +1 xn +1 Dxd FxF
yn = + − (4.17)
Vn Vn Vn
Material Balance of bottom of column.
Vm = Lm +1 − W (4.18)
63
ymVm = Lm +1 xm +1 − Wxw
(4.19)
Lm +1 W
ym = xm +1 − xw (4.20)
Vm Vm
Since the liquid overflow is constant Lm = Lm+1
Lm +1 W
ym = xm +1 − xw (4.21)
Vm Vm
As the feed is introduced in the top of the column Lm = Ln and also Vm = Vn
3.4.6.6. Procedure
1. The feed to the column must be admitted above the top plate.
digital wattmeter.
5. Start the experiment with total reflux.
6. Before switching on the reflux switch, Set the reflux ratio to 5:1, meaning 5 sec
7. When the column has stabilized at total reflux, the flow of feed and the reflux
can be started at the same time.
8. It is advisable to set a feed flow 2 litres/hr.
9. After feeding approximately 3 litres take a sample of the overheads through

valve V3. When doing that, be careful never to drain the condensate return line
ie . partially open V3 to leave a small amount of liquid in the line all the time.
64
15. repeat the sample taking a further three times during the experiment (before
feed runs out)
Table 4.10 Raw Data for Experiment F
No. Power (kW) Feed Position Feed Flow Reflux Ratio

Rate (l/hr)

2. Calculate the number of theoretical plates using the LEWIS-SOREL

method.
65
Table 4.11 Processed Data for Experiment E
Power (kW) =
Feed Position =
Feed Flow Rate (l/hr) =
Reflux Ratio =
Trial # 1
Trial # 2
Trial # 3
Trial # 4
Trial # 5
66
Exp# 4
Single Stage
Evaporator
67
4.1. The falling film evaporator
4.1.1. Introduction
The falling film evaporators are used industrially to concentrate solutions,
especially solutions with heat sensitive components.
Over the past 40 years the falling film evaporator has practically replaced the
force recirculation evaporator. This type of evaporator is desirable, from a
product point of view, as it can be operate with very low temperature
differences between the heating media and the boiling liquid, short holding
time (typically just few seconds) and a good control of the temperature of the
product to be concentrated.
The falling film evaporator has a very small hold up of liquid. This is
advantageous during operations (quick start up high response to changing of
operative conditions), avoiding browning of sensitive product and during
cleaning requiring a minimum of cleaning liquid. Further the amount of
product in the evaporator is reduced and the surface from which the
evaporation takes place is increased.
Falling film evaporators are highly responsive to alterations of parameters such
as energy supply, vacuum, feed rate, concentrations, etc. When well controlled,
they can produce a very consistent concentrated product.
These characteristics make the falling film evaporator particularly suitable for
heat-sensitive products, and it is today the most frequently used type of
evaporator.
The evaporator consists of a number of tubes built together side by side. At
each end the tubes are fixed to tube plates, and finally the tube bundle is
enclosed by a jacket.
The liquid to be evaporated is evenly distributed on the inner surface of a tube
and will flow downwards forming a thin film, from which the
68
boiling/evaporation will take place because of the heat applied by the steam.
This gravity-induced downward movement is increasingly augmented by the
counter-current vapor flow.
The steam will condense and flow downwards on the outer surface of the tube.
The steam is introduced through the jacket. The space between the tubes is thus
forming the heating section. The inner side of the tubes is called the boiling
section. Together they form the so-called calandria. The concentrated liquid
leaves the calandria at the bottom part and the vapor leaves at the top. The
heating steam, which condenses on the outer surface of the tubes, is collected
as condensate at the bottom part of the heating section, from where it is
discharged by means of a steam trap.
The pressure in the tubes maybe lower than atmospheric pressure, in order to depress
the solution’s boiling point.
69
Falling film evaporators are common in the manufacture of concentrated orange juice
and condensed milk. They are attractive as a concentration process because of their
energy efficiency and thermal gentleness.
4.1.2. Description
The system is installed within a stainless steel framework and the main
components are stainless steel falling film evaporator (E1) with a stainless steel
condenser (E2).
The solution to be concentrated is contained in a glass tank (D1) and it is
pumped at the top of the evaporator using a metering pump (G1).
The concentrated product is cooled in an exchanger (E3) and stored in a glass
tank (D2).
The vapor leaves the evaporator from the top and it is condensed in the
condense (E2) and collected in a glass tank (D3).
The system can operate under vacuum via a liquid ring vacuum pump connected
with the condenser (E2).
The steam flow rate is measured at the inlet of the evaporator jacket, using a
calibrated orifice connected with a differential pressure transmitter (FT1).
70
The steam flow rate, and indirectly the steam pressure in the evaporator jacket,
can be adjusted using a pneumatic valve (FV1).
In the low part of the jacket of the evaporator, there is a steam trap connected
with a graduated tank (D4) to measure the condensate flow rate.
A safety valve (PSV1) protects the evaporator jacket from excessive pressures
due to wrong operations.
A CIP pump (G2) allows to clean the piping, the evaporator and the tanks with
cleaning solution.
4.1.3. Technical Characteristics
• Metering pump in stainless steel AISI 316, range 0+24 l/h, equipped
with pneumatic actuator driving with 0.2+1 bar signal, code G1
• CIP pump in stainless steel AISI 316, 30 1/min @ 2bar, code G2.
• Liquid ring vacuum pump, code G3.
• Air-water separator for vacuum pump, stainless steel AISI 304
execution, code D5
• Feed tank in borosilicate glass, capacity of 25 1, code D1
• Collection tank for the concentrated product in borosilicate glass,
capacity of 10 1, code D2
• Collection tank for the condensed solvent in borosilicate glass, capacity
of 10 1, code D3
• Graduated borosilicate glass collection tank for the condensed steam,
capacity of 1 1, code D4
• Steam trap in stainless steel AISI 304, code SC
• Falling-film evaporator, stainless steel AISI 316 execution on the tube
side and stainless steel AISI 304 on the shell side, exchange surface of
0.27 m2, code E1
• Safety valve for steam 2 bar, code PSV1
• Shell-and-tube condenser, stainless steel AISI 316 execution on the tube
side and stainless steel AISI 304 on the shell side, exchange surface of
1.1 m2, code E2
71
• Tube-tube heat exchanger in stainless steel AISI 304, code E3
• Bourdon pressure gages, range 0÷4 bar, code PI1
• Bourdon pressure gage, range of 0÷1.6 bar, code PI2
• Bourdon vacuum gage, range of 0÷-1 bar, code PI3
• Flow rate steam transmitter pressure type, stainless steel AISI 316
execution, range 0 to 1000 mm H2O , output signal of 4 to 20 mA
proportional to 0+15 kg/h of steam at 4 bar, code FT1
• Calibrated orifice for steam flow rate measure in stainless steel AISI 304
• Steam flow rate pneumatic control valve, stainless steel AISI 316
execution, Cv = 0.32, code FV1
• Variable area flow meter for condenser cooling water, code FI2
• 6 RTD’s Pt 100, with sheath of stainless steel AISI 316, code TI1, TI2,
TI3, TI4, TI5 and TI6
• 6 electronic temperature indicators, range 0÷200 0C
• Absolute pressure transmitter, stainless steel AISI 316 execution, range
0÷1000 mbar, code PI3
• Vacuum pump solenoid valve, code EV1
• Electric switchboard, protection level IP 55, with synoptic of the plant,
E.L.C.B and interface modules for the connection of the plant with a P.C. via
serial cable
Data logging software for Windows
Connecting lines and valves of stainless steel AISI 304 and 316
Adjust the steam flow rate using valve FV1
• The system is in the stationary condition only when the condensate
solvent starts to fail in tank D3; drain the solution collected until this moment
in tank D2 (see below the drain instruction)
• If the temperature of the condensate is too high, increase the flow rate
of water to the cooling exchanger (E3) opening the valve V11
• To increase the concentration of the product, increase the steam flow
rate to the primary evaporator or decrease the feeding flow rate or increase
72
the vacuum; adjust the vacuum very slowly (using valve V22) to avoid
dragging of solvent in the tank D3
To drain the tank D2, operate as follows:
− Close the valves V12 and V14
− Open the valve V13
• To enable the tank D2 again, operate as follows:
− Close the valve V16
− Open the valves V14 slowly and when the pressure is stabilized,
open the valve V12
• To drain the tank D3, operate as follows:
− Close the valves V18 and V19
• To enable the tank D3 again, operate as follows:
− Open the valves V18 slowly and when the pressure is stabilized,
open the valve V19
4.2. Operating instruction

4.2.1. Commissioning
1. Close the valves V2, V3, V4, V5, V6, V7, V8, V9, V13, V15, V16, V17,
V20 and V21
2. Open the valves V1, V12, V14, V18 and V19
3. Open partially the valves V10, V11, V22 and V23
4. Connect the plant to the electrical supply: three-phase + N +G, P=3 kW
73
5. Connect the plant to the tap water and to a water drain (see plant
synoptic and labels on the pipe) using the rubber pipe and the metal hose
clamps supplied
6. Connect the pressure reducers under the switchboard to the compressed
air line (6bar) using the pipe supplied and set the pressure following the
labels
7. Open the main air supply
8. Close the pneumatic valve FV1 using the related knop (Ga1 flow
control) positioned on the switchboard (rotating clockwise = increase the
valve opening, anti clockwise = decrease the valve opening); the
pressure on the related manometer is proportional to the degree of
opening of the valve: 0.5 bar = valve completely close, 1 bar = valve
fully open
9. Connect valve V6 with the steam line using the flexible pipe for steam
supplied: the steam pressure must be at maximum 4.5 bar (max.
consumption about 20 kg/h)
10. Open the main feed steam valve (V1 on steam generator)
11. Open the main water flow line
12. Set the cooling water flow rate to the condenser E2 at 150 l/h about
using valve V10
13. Insert the E.L.C.B (‫)االمان‬
14. Pull the emergency knob out
15. Press the pushbutton “ START”
16. Fill the feeding tank D1 with the solution to be concentrated
17. Open partially valve V22
18. Start the pump G3 (switch to 1)
19. Control the residual preesure, at -0.7 bar (=300 mbar) for example, with
the valve V22: closing the valve the vacuum increase
• ‫ حيث‬3‫ ومن ثم طفي مضخة‬22 ‫ للتاكد من ان المضخة سليمة بدون تنفيس يمكن اغالق صممام‬:‫مالحظة‬
‫عندها يجب‬PI3‫ان التزيد قراءة‬
20. Open the valve V6
74
21. Open valves V7 and V8
22. Open the valve FV1 (steam flow control) at 50% ( detemined by needle
position on the red FV1) using the related knop on the switchboard
4.2.2. Shut Down
▪ Close the valve V6

▪ Close the vale FV1
▪ Stop the pump G1 turning the switch to 0
▪ Stop the vacuum pump G3 running the switch to 0
▪ Open the valve V22
▪ Drain the tank D1
▪ Drain the piping using the drain valves
▪ Clean the plant at the end of each working cycle
following the operating instruction of previous
chapter
▪ Disconnect the power supply
▪ Close the main valve of the tap water
▪ Close the main valve of the compressed air
4.2.3. Emergency Stop
▪ press the emergency button
4.2.4. Cleaning Uperations
IMPORTANT: During the washing operations, use safety gloves and eye ware.
If the product treated is milk, the plant must be washed. AT THE END OF
EACH WORKING CYCLE, as follows:
▪ Fill tank D1 with clean tap water
▪ Open valves V13 and V20
▪ Open partially valves V5, V15, V17
75
▪ Close valve V11
▪ Start the pump G2 and adjust the flow rate of cleaning solution using:
− valve V5 to clean the evaporator E1
− valve V15 to clean the tank D2
− valve V17 to clean the tank D3
▪ When the tank D1 is almost empty, stop the pump G2
▪ Drain the tanks D2 and D3
▪ Fill tank D1 with NaOH/H2O (1-2% wt) solution
▪ Close valve V17
▪ Start the pump G2 and adjust the flow rate of cleaning solution using
valves V5, V15 and V17
▪ Close the valve V12 and fill the evaporator E1 up to sight glass
▪ Stop pump G2
▪ Open the valve FV1 and heat at 70 0C(TI2) for 20 minutes
▪ Drain the evaporator E1
▪ Start pump G2 and wash the evaporator
▪ When the tank D1 is almost empty, stop the pump G1
▪ Repeat a cleaning cycle using tap water
▪ Repeat the cleaning operation using a HNO3/H2O (0.8%) solution at 700C
▪ Repeat the cleaning operation using water till to the PH of water collected
in the tank D2 is about 7
▪ Discharge the tanks and the piping
If the product treated is citrus juice, water sugar solution etc. (that is solution easy to
wash), the plant must be washed, AT THE END OF EACH WORKING CYCLE, with
a cleaning cycle with water at 70 0C
Note: for the cleaning operation, it is possible to use commercial detergent for food
machinery but the above parameters (concentration and composition) must always be
fulfilled.
This product must be compatible with stainless steel.
76
4.3. Data acquisition software
The software, Window based, supplied on CD-ROM, allowing real time data
acquisition via serial port, mimic diagram of process with real time parameters
and real or historical graphs of variables.
The data are exportable in Excel.
• Install on P.C., from windows. The supervision software (PROGRAMM
INSTALLATION and PLANT INSTALLATION) using the auto play of
the CD.
• Connect the plant to the PC via serial cable using COM1 serial port (or
COM2)
• Run the supervision software Pilot for Windows
77
• Select COM2 using COM2 serial port
• Open the file UMEC doe the supervision of the plant
For further information on the software, consult the help on line.

Some examples of possible screens are shown in the following pages
78
79
4.4. Experiments
4.4.1. Concentration of a sugar solution
1) Concentration of a sugar solution

• Prepare 10 liters of a 5% (g/100 ml) distilled water and sugar solution
(sucrose, C12H22O11)
• Trace, using s refractometer, a calibration curve for water/sugar solution
with concentration between 0 and 50% (wt/wt)
g/100ml 0 5 10 15 20 30 40 50
nD 1.331 1.3385 1.33450 1.3520 1.3590 1.3735 1.3850 1.4000
nD=1.33133+ 0.00137 C%
Where:
nD = refraction index
C% = concentration of sugar (g/100ml)
• Start the plant and in the stationary conditions(generally after 10-min), calculate
the energy balance, mass balance and the overall heat transfer coefficient
• The operative conditions could be the following:
80
Feeding flow rate, Fi 10 l/h(45%)
Feeding concentration 5%
Steam flow rate, FI1 6 kg/h (42%)
Steam pressure, PI1 3 barg
Working pressure, PI3 500 mbar
Cooling water flow rate, FI2 250 l/h
Determination of steam consumption using a chronometer and the graduated tank D4:
Volume = 380 ml, time = 3 min and 45 sec equal to a flow rate = 4.8 kg/h
The same procedure can be adopted to measure the steam flow rate corresponding to
FI1 = 100%
Energy balance on evaporator
Total heat
𝑄𝑇 = 𝐹𝐼1 × ∆𝐻𝑐 (𝑃𝐼3) = 4.8 × 540 = 2592 𝑘𝑐𝑎𝑙 ⁄ℎ
Sensible heat
𝑄𝑠 = 𝐹𝑖 × 𝐶𝑝 × (𝑇12 − 𝑇11)
Cp(5%) = 0.97 kcal/kg
Cp(10%) = 0.94 kcal/kg
Heat for evaporation = QT - Qs
Efficiency = (QT –Qs)/QT
Heat balance on condenser
Total heat
𝑄 = 𝐹𝐼2 × 𝐶𝑝(𝐻2𝑂) × (𝑇16 − 𝑇15)
Evaporation rate E = Q/∆𝐻𝑐 (𝑃𝐼3)
Mass balance
Inlet concentration Cin = 5%
Outlet concentration Cout (to be calculated via refraction index)
𝐶𝑖𝑛 × 𝐹𝑖 = 𝐶𝑜𝑢𝑡 (𝐹𝑖 − 𝐸)
81
4.4.2. Concentration of water/glycol ethylenic solution
2) Concentration of water/glycol ethylenic solution

• Repeat the experiment no1 using a 5% water/glycol ethylenic solution
4.4.3. Concentration of milk
• 15 liters of whole milk are treated in the following conditions:
Feeding flow rate, Fi 12l/h (50%)
Steam flow rate, FI1 4.5 kg/h (30%)
Steam pressure, PI1 3.5 barg
Working pressure, PI3 270 mbar
Cooling water flow rate, FI2 150 l/h
• In stationary conditions, we measure 5 liters of concentrated product in D1

and 1 liter of water in tank D3
• The concentration then is increased of 17%
4.5. Safety
• Any maintenance operation must be carried out by authorized and skilled

operator
• Disconnect the voltage before any maintenance operation
• Keep attention to the hot surfaces (evaporator E1, steam pipe etc.)
• During the washing operations, use safety gloves and eye wear.
6. Maintenance
• Grease the metering pump G1 every year, the grease nipple is available on
the pump body.
82
83
84
85
86
Exp# 5
Steam Distillation
87
Steam Distillation of an Essential Oil
5.1. Introduction
In this laboratory exercise we will employ Steam Distillation to isolate an Essential Oil
from either Mint leaves/ Rose Mary leaves or Orange peel. This will involve distilling a
mix of the plant material with Water vapor to obtain the Oil, extracting the Oil from the
Water, and then isolating the Oil from the extraction solvent. In the end, we will analyze
the Oil’s composition by measuring its refractive index.
Essential Oils are a mix of fragrant compounds common to a number of plants such as
Mint, Lavender, Rosemary, thyme, sage, etc. which are isolated via steam distillation.
Because these Oils were once considered to be the essence of the plant, they were initially
sought as possible pharmaceuticals and are a part of early medicine's contribution to
modern chemistry. Today they are used as flavorings, perfumes and deodorants.
Essential Oils are mixtures of organic compounds that are dominated by the Terpenes and
the Terpenoids, oxygen containing derivatives of the terpenes. Terpenes themselves are a
class of compounds built on the five carbon skeletal fragment of Isoprene.
For example, Limonene, the major constituent of the Oil of Orange has the formula C 10H16.
Menthol
Attempting to distill these Essential Oils directly from the plant material is generally not
feasible. In general, most of the Oils' constituents are high boiling and will decompose
under the high heat needed to bring them to a boil. Steam distillation is a much gentler
method of achieving the same end. In steam distillation, the distilling pot is infused with
88
steam, which carries the Oil’s vapor into the distilling head and then into the condenser,
where the Oil and Water co-condense. As an alternative, steam is generated in situ in the
distilling pot.
5.2. Theory
In our case the steam generator is connected directly to the a steam distillation unit as
shown below:
Steam distillation works because the Water and the Oil are immiscible. Hence, they boil
independent of each other.
So, boiling occurs when the sum of the pure vapor pressures equals the atmospheric
pressure:
Patm= PWato+ POilo (Eq. 1)
Thus, a mixture of two immiscible liquids boils at a temperature lower than the Normal
Boiling Point or either component of the mixture. Because PWato>>POilo, the mixture will
boil at a temperature slightly less than the normal boiling point of Water. This means the
Oil will vaporize under very mild conditions.
However, this methodology leaves us with one complication; the distillate is a mixture of
Oil and Water. The relative numbers of moles (n) of each component of the distillate will
be given by:
nOil/ nWat= POilo/ PWato (Eq. 2)
89
If we know the average molecular weigth (M) of the Oil, then we can estimate the mass (m)
of Oil that will be obtained in a given amount of Water:
mOil/ mWat= (POiloMOil) / (PWatoMWat) (Eq. 3)
Different cases may be faced, oil is very slightly dissolve in water, or some polar organic
constituents dissolve in water. In this case we need to Extract the Essential Oil from the co-
distilled Water. We will take advantage of the fact that the Oil is soluble in non-polar
solvents like Diethyl Ether (CH3CH2OCH2CH3). Ether is added to the Oil-Water mixture
in a Separatory Funnel. This funnel allows the two solvents to layer and subsequently we
can drain one solvent layer away from the other.
After a few moments of shaking, the Oil will Partition into the Ether layer. Draining the
Water layer from the Ether removes the Oil from the Water. The partitioning is almost
never complete, so an Extraction is usually carried-out multiple times. The resulting Ether
layers are collected and combined. (Caution must be observed when shaking the system.
First, the system must be vented continuously because of vapor build-up that occurs within
the flask. Second, the shaking cannot be too vigorous or else the system will emulsify. If
emulsification occurs, separation of the two layers will become very difficult.)
It may seem as though we have traded one problem for another; we now have a mixture of
Oil and Ether that must be separated. However, this is not a major problem. The Ether will
boil at a low enough temperature that it can simply be boiled off from the Essential Oil.
After the Ether is stripped off, our isolation of the Essential Oil is complete.
5.3. Procedure
This steam generator is able to supply steam to the systems needing it. Its potentiality
enables to supply steam to two systems at the same time.
5.3.1. Installation
• Connect the softener to tap water end to a drain
• Connect the valve V8 of steam generator to a drain
• Open valves V4, V5, V6, V7
• Close valve V1, V2, V3, V8
• Connect the softener to the electrical supply
• Connect the steam generator to the electrical supply
90
• Drain the generator opening valve V8 and V9 until to the level of the
water is at the medium of the sight glass of the level gauge LG1
• Close valve V8 and V9
5.3.2. Start up
• Connect the steam distillation to steam generator
• Press the pushbutton" RESET"
• Switch the selector of pump G1 in position "AUT"
• Switch on the heaters
• Wait that the pressure on manometer increase up to 1 bar
• Discharge the air opening partially valve V9
• Repeat the operation till to steam exits through the valve V9
• Close valve V9
• When the pressure on manometer PI1 is about 4 bar, open the valve V1
5.3.3. Shut down

• Close valve V1
• Switch off pump G1 position "0"
• Switch off the heaters
• For emergency shut down, push the red emergency pushbutton
91

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An-Najah National University

Chemical Engineering Department

Dr. Abed Al-Raheem Abu Safa

Evaluation Criteria Grade

a. An introductory statement about the subject matter

8. Conclusion and Recommendation

12. Organization and Neatness

2. Confine long hair and loose clothing when in the laboratory.

‫قواعد السالمة المهنية في مختبر التحكم بالعمليات‬

6. Never leave unattended an experiment that is in progress.

‫قواعد السالمة المهنية في مختبر وحدات صناعية‬

1.1- THEORITICAL BACKGROUND:

Co(t) : excess hydrogen ion concentration in the effluent stream (mol/L)

1.2- TECHNICAL CHARACTERISTICS

Figure 1.3 pH control system

1.3- OPERATING PRINCIBLE

• During the experiments, take care in wearing the necessary protections:

• Shut off valves V1, V2, V4 and V6.

• Shut off valve V1

3.2- TECHNICAL CHARACTERISTICS

3.3- OPERATING PRINCIBLE

The operating principle of the equipment can be described as follows.

The phenomenon is described by the following equation:

• Shut off the valves V1, V2, V3, V4, V6 and V7

3.5- STOP THE SYSTEM

• Shut off the valve V3

Process fluid: Water

Process fluid: Air

• AISI 304 stainless steel framework

4.5- Stop of the system

5.1- THEORITICAL BACKGROUND:

Substituting the flow-head relation, q3 = h/R, and introducing deviation variables

Thus, we obtain the transfer functions

5.2- TECHNICAL CHARACTERISTICS

• AISI 304 stainless steel framework

5.3- OPERATING PRINCIBLE

• Close valves V1,V2, V3 and V4

6.1.1 Design of Columns

As an example, for an ethanol-water mixture, there is an azeotrope at x1 = 0.8943 (for pressure of

6.1.2 Pressure drop over the distillation column:

6.1.3 The boil-up rate:

6.1.4 Equilibrium condition

6.1.6 PROPERTIES OF METHANOL AND WATER

Equilibrium Data For The Methanol- Water @ Atmospheric Pressure

Depend on % mole of Methanol

Liquid Vapor Temperature C

Equation for Equilibrium

6.1.7 CALCULATION OF REFLUX

The minimum reflux can be calculated using the following equation:

Then R required = 1.5Rmin

6.1.9 DEW POINT AND BUBBLE POINT CALCULATION

6.1.9.1 Bubble point calculation

4. If yI is too large try lower temperature.

6.1.9.2 Dew point calculation

Component Pi⁄ at Tguess Ki yi xI=yi/Ki

4. If xI is too large try a higher temperature.

Input Variables Output Variables

USING A PID CONTROLLER WITH UOP3CC

The object of the experiment can be:

6.2.1 REBOILER POWER CONTROL:

Reboiler power control from the tray temperature T7.

6.2.1.2 Open Loop System

• Plot T7 versus Time