American University of Ras Al Khaimah

School of Engineering

Chemical and Petroleum Engineering Department

Chemical Engineering Laboratory II

Manual

Prepared by:

Eng. Nour Alobaidi

Reviewed by:

Dr. Sara Tasfy

FALL 2018
Table of Content

General Safety Rules 3

Lab Report Writing Procedures 5

Part A: Reaction Engineering Experiments

Experiment #1 Batch Reactor 13

Experiment #2 Continuous Stirred Tank Reactor (CSTR) 28

Experiment #3 Continuous Stirred Tank Reactors in Series 42

Experiment #4 Tubular Flow Reactor 50

Part B: Unit Operations Experiment

Experiment #5 Gas Absorption 65

Experiment #6 Cooling Tower 81

Experiment #7 Fluidized Bed 142

Experiment #8 Liquid-Liquid Extraction 180

Experiment #9 Drying Characteristics in Try Dryer 197

2
 General Safety Rules
The basic purpose of laboratory safety is to protect students, researchers, technicians and teachers from
the many hazards encountered during the use of various materials and equipment’s, so safety in the
laboratory must be of vital concern to all those engaged in experimental work.

It is therefore the responsibility of everyone to adhere strictly to the basic safety precautions
provided and to avoid any acts of carelessness that can endanger his life and that of others around him. It
is equally important to always abide by all the instructions for conducting the experimental work during the
laboratory sessions. A set of information is presented here to safeguard you while in the laboratory.

 Smoking is not allowed in the laboratory; no food or beverages are allowed in the laboratory.

 Avoid long hair and long sleeved loose clothes and wear lab coat while conducting experiments
to minimize the risk of clothing getting caught in the machines.

 Use appropriate personal protective equipment PPE at all time, like Gloves, Safety glasses, skin
protection, hearing protection, and foot protection (don’t wear open sandals).

 No running, playing, bantering, and kidding in the laboratory.

 Know locations of first aid and all emergency equipment’s, such as fire Alarm, water hoses, fire
extinguishers, fire blankets, eyewash stations, and safety showers, know how to find and use
them.

 Use laboratory equipment for its designed purpose.

 Always follow instructions and use only machines and equipment that you are authorized and
qualified to operate. If you have any question, consult with your supervisor.

 Know and follow safety rules for specific experiments or tasks.

 Know potential hazards in your work and ways of working safely to prevent such hazards.

 Working alone should be avoided. Someone should always be within call when a laboratory
procedure is being performed.

 Avoid mouth contact with any laboratory equipment’s including pipettes. Use safety filler to fill
pipettes.

 Avoid exposure to gases, vapors, and particulates by using a properly functioning laboratory
fume hood.

 Use ground fault circuit interrupters where there is a risk of anoperator coming in contact with
water and electrical equipment simultaneously.
3
  Follow electrical safety rules and make sure your hands are dry before using electrical equipment,
grounding portable electrical tools. Make sure electrical wires are connected properly without
short circuit before operating. Wear protective clothing, well-insulated groves and boots, if
required.

 Only trained, qualified personnel may repair or modify electrical or any equipment.

 Properly support glass wares using stand, clamps, etc.

• Use proper rings to place round bottom flasks.

• Reduce fire hazard.

• Use shower for fire victims.

• While fire on clothing, do not run or fan flames.

• Smother flames by wrapping in fire blankets.

• Spills of flammable solvents can be a source of fire.

 Upon hearing fire alarm, you should evacuate the area and follow emergency procedure.

 Report all injuries including minor scratches, cuts, and burns for First Aid treatment. Corrective
actions should be taken to prevent future injuries.

 Report any damage to equipment or instrument and broken glassware to the laboratory instructor
as soon as such damage occurs.

 Wash hands upon completion of laboratory procedures and remove all protective equipment
including gloves and lab coats.

 Before you use the lab for any purpose other than Labs courses:

 1-Fill and sign from your supervisor, lab instructor and chair, a work permit form.

 2- Submit a Risk Assessment for the activity you need to do to the lab Instructor.

 Attend the safety workshop held at the second week of each semester and sign the attendance
sheet before you use the lab.

4
 Lab Report Writing Procedures
A good lab report should contain the following items:

1. Cover Page

The followings are included in a cover page:

 University name, school and department.

 Student name and number.

 Experiment name and number.

 Instructor name.

 Date.

2. Title

 Should tell the reader what report is about.

 Should be as short as possible.

3. Abstract

A single paragraph providing a succinct description of the work. Briefly describe the
purpose of the experiment, experimental methods, results, and conclusions. The abstract
must be self-contained and allow one to understand the essence of the entire report. Do not
refer to figures and tables located in other sections of the report. Avoid including symbols
or acronyms.

 Purpose of Abstract: briefly summarizes entire study

 Length: approximately 150-300 words - no more than 1 page

5
  Abstract includes: purpose, hypothesis, brief method (subjects, key apparatus),

brief procedure, results (general - no stats, just whether or not the experiment

"worked"), and concluding remarks.

 Hint: write last, after rest of report has been completed

4. Introduction

A review of relevant background information and a description of how this work

contributes to the field. Make sure to properly cite relevant references. Pick one of the
citation formats and stick with it throughout the report. E.g., you can refer to publications
by their number in the list of references, as in “additional details are provided in [1]”. An
example of the reference formatting is provided in the References section of this template.

5. Objectives of Performing the Experiment

 Objective1

 Objective2

6. Theory

Discussion of physical phenomena and relationships relevant to the experiment. Do not

include theoretical discussions or equations that are not relevant to the experiment. Do not
derive any equations that can be found in a textbook, a handbook, a journal publication, or
a lab manual posted online. Simply state the equation and include a reference to a reliable
source. E.g., “Henry’s law constant can be approximated as [2]”

1 1
𝐻 (𝑇 ) = 𝐻(𝑇 𝑟𝑒𝑓 ) exp [−𝐶 ( − 𝑟𝑒𝑓 )]. (1)
𝑇 𝑇

All equations should be centered on the page and numbered sequentially on the right. Insert
an equation by pressing the “Equation” button in the “Insert” menu tab. It is suggested to
create a three-column, one-row table for each equation, as illustrated by Eq. (1) above. The
equation should then be contained in the center column, the left column should be left blank

6
and the right column should contain the equation number. The cell borders of the table
should be invisible.

7. Method

Details about experimental methods, measurements, procedural s, materials, equipment,

and safety precautions. The presentation of this material may be aided by subsections, as
illustrated below.

7.1 Materials

Description of all materials used in the experiment. It may be useful to place all relevant
properties of the materials into a table.

7.2 Equipment

Describe all equipment needed to carry out the experiment. Consider including
photographs or schematics of the equipment or certain aspects of the measurements if these
make the equipment description or measurements more precise. Include information on
precision and range of measurement of all relevant data in the experiment.

7.3 Experimental procedures

Provide specific details on the sequence of steps involved in preparing initial conditions,
performing the experiment, and collecting the data.

7.4 Safety

Provide a summary of any safety issues and how these issues were mitigated.

8. Results

Include all figures, tables and relevant details that document your final results and analysis.
Introduce the reader to each figure and table with a brief paragraph indicating what
variables are plotted or tabulated. E.g., “Time dependence of the liquid temperatures at the
inlets and outlets of the heat exchanger is shown in Figure 1” or “Dependence of the heat
transfer coefficient on the liquid and gas flow rates is summarized in Each figure and table
must have a caption providing enough detail so that the figure/table is understandable

7
without reading the surrounding text. Use the “Insert Caption” option in the “Reference”
menu tab of MS Word to automatically number figures, tables, and equations. Use the
“Cross Reference” feature of the “References” tab to create a reference to a figure/table in
text, e.g. Figure 1 and Error! Not a valid bookmark self-reference..

Table 1” No figure or table should appear before its introductory paragraph. Unreferenced
figures and tables are not acceptable. Figures and tables should be numbered according
to the order in which they appear in the report.

FIGURE 1. TIME DEPENDENCE OF THE TEMPERATURES OF THE HOT AND COLD

WATER AT THE INLETS AND OUTLETS OF THE HEAT EXCHANGER .

Each figure and table must have a caption providing enough detail so that the figure/table
is understandable without reading the surrounding text. Use the “Insert Caption” option in
the “Reference” menu tab of MS Word to automatically number figures, tables, and
equations. Use the “Cross Reference” feature of the “References” tab to create a reference
to a figure/table in text, e.g. Figure 1 and Error! Not a valid bookmark self-reference..

TABLE 1. DEPENDENCE OF THE MASS TRANSFER COEFFICIENT KXA ON THE GAS AND
LIQUID FLOW RATES V AND L.

V L Kxa

(mol/s) (mol/s) (mol/s∙m)

… … …

… … …

8
In general, figures are preferable to tables, since experimental trends can be more clearly
seen in figures. Tables with raw data should be placed into the Appendix.

9. Analysis

This section shows how the outcomes were calculated briefly, what formulas and equations
were used in those calculations?

Error Analysis includes: listing errors types and sources and determining precision of the
experiment using two different errors associated with a directly measured quantity: the
standard deviation and the reading error.

10. Discussion

Interpretation of your experimental observations. Describe effects of control parameters on

outcomes of your experiments. Compare results of the experiments with predictions of the
theory discussed in the Theoretical Background section.

Provide plausible explanations if the experiments and the theory disagree. If you believe
that the experimental results are invalid, discuss what went wrong. Be specific. Do not use
vague statements such as “human error”.

Compare experimental data with the existing theories.

11. Conclusions and Recommendations

Conclusions are the series of numbered sentences which answer the questions posed at the
beginning of each experiments. Conclusions should also include main results (numerical
values) and the errors between the experimental and theoretical values. What you have
learned from the experiment should be mentioned as well, Conclusion is considered as a
brief statement of the primary contributions of the report. Unlike abstract, this section need
not to be a stand-alone summary of your report and may refer to other portions of the report
if necessary.

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, the

9
recommendations are usually listed by numbers, and each consists of only a sentence or
two.

12. Acknowledgements

Acknowledge anyone who played a specific and substantial role in the experimental work
but is not an author (e.g., other students, instructors, and staff).

13. References

Here, you should list the books, Journal’s articles, etc. used in writing your report and

analyzing the experiment. The reference should be completed (name of the book, author,

volume, date of publication, pages, etc.). References should be arranged alphabetically by

author’s names. 1. 1. 1. Author1, “Book title1”, publication date.

2. Author2, “Book title2”, publication date

Sample of References (APA (American Psychology style)

 Book: Geankoplis, CJ., (2003). Transport processes and separation process principles

(4th Ed.), simple distillation methods (pp. 700-720). Upper Saddle River, NJ: Prentice

Hall.

 Paper: Xara, S., Delgado, J., Almeida, M., Costa, C. (2009). Laboratory study on the

leaching potential of spent alkaline batteries.Waste Management, Vol. 29, pp. 21-26.

 Website: Wikipedia (2011). Flash evaporation. Retrieved October 25, 2011, from

http://en.wikipedia.org/wiki/Flash_evaporation.

14. 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.

15. Appendix
10
Raw data and other information that is relevant but is too lengthy to include in the body of
the report. If necessary, organize the Appendix in subsections, E.g. A1. , A2. , etc….. As
shown below. Each subsection must be self-contained and referred to in the body of the
report. An introductory paragraph should be used to inform the reader of the contents of
each subsection. All appendices and graphs should be attached at the end of the report.

A1. Raw Data:

It should contain the raw data (in the log sheet) collected during the experiment.

A2. Analysis of Data and Sample Calculations:

This shows how the collected experimental data are analyzed and transformed into
experimental results by using the appropriate equations. Also, how the theoretical results
are obtained using theoretical in terms of percentage error. Sample calculations should
contain each step, which is used to acquire certain results.

Note:

Organization and Neatness

The students must organize their reports in accordance with the format described earlier. It
is required/encouraged to use computer packages such as EXCEL, MATLAB or any other
suitable engineering software to draw graphs and fit the data. The following will determine
the neatness of a report:

Is the report prepared with the necessary editorial care? Note neatness, balanced page
layout, care of language, spelling errors, integrity with respect to numbering, grammatical
parallelism of headings and lists, sentence and paragraph construction, reference/citation
style and the correct application of conventions with regard to figure and table titles.

11
 PART A

REACTION ENGINEERING EXPERIMENTS

12
 EXPERIMENT #1
BATCH REACTOR

13
Objectives
This experiment aims to study the liquid-phase saponification reaction of ethyl acetate with

sodium hydroxide in an Isothermal batch reactor.

After conducting the experiment the students should be able to:

1. Determine the rate constant (k) of the saponification reaction.

2. Determine the activation energy (Ea) and frequency factor (A) for the

saponification reaction.

Safety Precautions
- This experiment uses both acids and bases. Use caution when handling these

reagents. Review the Material Safety Data Sheet (MSDS) of NaOH, CH3 COOC2 H5 ,

CH3 COONa and C 2 H5 OH before starting the experiment.

- Personal protective equipment (PPE): lab coat, safety glasses, mask and disposable

gloves should be worn when handling NaOH solutions.

- Mask should be used while using ethyl acetate since it is hazardous in case of

inhalation. In addition, ethyl acetate is highly flammable (flash point: -4.4o C) and

therefore, must be kept away from open flames, sparks, and heat

- A small amount of NaOH spilled on the outside of glassware can cause the glassware

and equipment to be extremely slippery when wet. Therefore, extreme care is

required while handling the glassware

- Collect all the waste of chemical solutions in the container labeled as waste solution.

14
 At the end of each lab period or the end of the experiment, add sufficient base

(NaOH) to yield a phenolphthalein end point (pink) that does not disappear

overnight. This indicates the reaction has gone to completion and the waste can be

disposed down the drain.

Introduction
A batch reactor has neither inflow nor outflow of reactant or products while the reaction is

being carried out. The reactants are simply charged to the reactor and allowed to react for

a fixed period of time after which the products are collected. A batch reactor is a closed

thermodynamic system and typically consists of a tank coupled with an agitator for

homogeneous mixing and an Integral heating or cooling system for controlling the reaction

temperature as shown in Figure 1.1.

FIGURE 1. 1: (A) AN IDEAL BATCH REACTO R WITH NO INFLO W O R O UTFLO W O F REACTANT AND
PRO DUCTS (B ) SIMPLE BATCH HO MO GENEO US REACTO R WITH INTEGRAL HEATING O R CO O LING
SYSTEM (FO GLER, 2005)

In an ideal batch reactor, both the concentration and the temperature are assumed to be

spatially uniform. This condition can be realized by vigorous agitation or stirring. In

15
addition, all the reaction elements spend the same amount of time in the reactor and,

therefore, have the same residence time.

Batch reactors are primarily used to determine rate law parameters for homogenous

reactions (Fogler, 2005). Typical characteristics of batch reactors are summarized in Table

1.1

TABLE 1. 1: APPLICATIONS , ADVANTAGES , AND DISADVANTAGES OF BATCH

REACTORS (FOGLER, 2005)

Type of Reaction Application Advantages Disadvantages

1. Gas phase 1. Determining rate law 1. High conversions 1. High labor costs per

reactions parameters batch

2. Easy to clean

2. Liquid phase 2. Small-scale operation 2. Variability of

3. Flexibility of
reactions products from batch
3. Testing new operation.
to batch
3. Liquid solid processes that have
4. The same reactor
reactions not been fully 3. Difficulty of large-
can produce one
developed scale production
product at one time

4. Manufacture of and another

expensive products different product at

another time.
5. Processes that are

difficult to convert to

continuous

operations

16
The saponification reaction of ethyl acetate with sodium hydroxide is expected to follow a

pseudo second order elementary irreversible reaction. The reaction will proceed according

to the reaction scheme shown below:

NaOH + CH3 COOC2 H5 → CH3 COONa + C2 H5 OH

This reaction may be either reversible or irreversible. If considered irreversible elementary

reaction, the kinetic expression or the rate law can be written as follows:

−𝑟𝐴 = 𝑘𝐶𝐴 𝐶𝐵 (1)

Where, 𝑟𝐴 is the rate of the reaction [mol/L.s], 𝑘 is the reaction rate constant [L/mol.s], and
𝐶𝐴 and 𝐶𝐵 are the concentrations [mol/L] of sodium hydroxide and ethyl acetate,
respectively.

The temperature dependence of the reaction rate constant (𝑘) could be correlated by
Arrhenius equation:
−𝐸𝑎
𝑘 = 𝐴𝑒 𝑅𝑇 (2)

𝐸𝑎
ln(𝑘) = ln(𝐴) − (3)
𝑅𝑇

Where, A is the pre-exponential factor or frequency factor [L/mol.s], 𝐸𝑎 is the activation

energy [J/mol], R is the gas constant [8.314 J/mol K], and T is the absolute temperature
[K] of the reaction medium.

In this experiment, conductivity measurements will be used to follow the progress of the
reaction. It is important to note that the conductivities of ethyl acetate and ethyl alcohol
can be neglected since the 𝑂𝐻 − ions are the most conductive species in the reaction
mixture. Therefore, the conversion of the reaction can be obtained by tracing the
conductivity of sodium hydroxide with time. The relationship between conversion and
sodium hydroxide conductivity is given by the following equation:

𝑘 − 𝑘𝑒𝑞
𝑋= (4)
𝑘𝑜 − 𝑘𝑒𝑞

17
Where, X is the conversion of sodium hydroxide at time t, 𝑘 is the measured specific
conductivity in the reactor at time t [mS/cm], 𝑘𝑜 is the initial specific conductivity of
sodium hydroxide solution [mS/cm], and 𝑘𝑒𝑞 is the specific conductivity in the reactor at
equilibrium, equilibrium means the conductivity remains constant. An assumption is made
that equilibrium is reached in 20 min. After 20 min a student can start the next run.

The mole balance equation on sodium hydroxide (species A) in a batch reactor gives the

following (recall the subject knowledge from CHEN-351):

𝑑 (𝑁𝐴⁄𝑉 ) 𝑑𝐶𝐴
= = 𝑟𝐴 (5)
𝑑𝑡 𝑑𝑡
Combinig Eq. (1) and Eq. (5), we get:

𝑑𝐶𝐴
= 𝑘𝐶𝐴 𝐶𝐵 (6)
𝑑𝑡

For constant volume reactions, the relationship between concentration and conversion is
given by the following equations:

𝐶𝐴 = 𝐶𝐴𝑂 (1 − 𝑋) (7)

𝐶𝐵 = 𝐶𝐴𝑂 (Ө𝐵 − 𝑋) (8)

In this experiment, the reaction will be carried out using equimolar initial concentrations
of Sodium Hydroxide and Ethyl Acetate (𝐶𝐴𝑂 = 𝐶𝐵𝑂 or Ө𝐵 = 1). Substituting Eq. (9) and
Eq. (8) in Eq. (6) we get:

𝑑𝑋
= 𝑘𝐶𝐴𝑜 (1 − 𝑥)2 (9)
𝑑𝑡

If the reactor is operated isothermally so that 𝑘 is a constant, Eq. (9) can be integrated as
follows:
𝑋 𝑡
𝑑𝑋
∫ 2
= 𝑘𝐶𝐴𝑜 ∫ 𝑡 (10)
0 (1 − 𝑋) 0

The complete integration yields the following equation:

𝑋
= 𝑘𝑡 (11)
𝐶𝐴𝑜 (1 − 𝑋)

18
Eq. (11) can be used to obtain the reaction rate constant (k).

The conversion (x), the rate constant (k), the activation energy (Ea) and the frequency factor
(A) calculation steps are as follows:

1. Operate the reactor isothermally at a specific temperature T1

2. Measure the conductivity κ inside the reactor with time and calculate the conversion X with

time using Eq. (4)

𝑋
3. Plot 𝐶 𝐴𝑜 (1−𝑋) vs. t (straight line through origin) to find the rate constant (𝑘1 ) at temperature

𝑇1 from the slope (Figure 1.2)

Repeat steps 1 to 3 at two different temperatures 𝑇2 and 𝑇3 to find the respective rate

constants 𝑘2 and 𝑘3

5. Use the Arrhenius Equation, Eq. (3), to obtain the activation energy (𝐸𝑎 ) and the frequency

factor (A) from the slope and intercept of ln(𝑘) vs. 1/T plot (Figure1.3)

Figure 1.2: Use Eq. (11) to find the rate constant 𝒌 at a specific temperature T

Note: the intercept is set to zero in Excel Fig 1.2

19
Figure 1.3: Finding the activation energy and frequency factor using Arrhenius Equation

Note: the intercept is not set to zero in Fig 1.3

Apparatus
The chemical reactors trainer (Model: CEB, MIK III, Armfield) will be used for this

experiment. The base is called reactors service unit is shown in Figure 4. This base can be

used to fit either the batch reactor or the CSTR. In this experiment, the base unit will be

fitted with the batch reactor. The base unit consists of a main switch to supply power to the

unit, heating Integral System.

If the base unit is used in conjunction with the batch reactor, the reactants can be fed

directly into the reactor. The switch box also contains a switch and an adjuster to control

the stirrer (0 to 300 rpm). Behind the switch box, there is a water tank with a heater and a

centrifugal pump with which hot or cold water can be supplied to the stainless-steel heat

exchanger coils (Figure 1.5) within the batch reactor. The hot water is required in case if

the batch reactor is to be operated under isothermal conditions. The temperature in the hot

water tank is controlled by a controller fitted on the switch box. This controller switches

20
the heater ON or OFF based on the signal received from the temperature sensor fitted

within the water tank. The switch box also contains ON/OFF switches for both the heater

and the water pump. The water pump must be switch on for isothermal reactor operation.

Figure 1.4: Base unit for Chemical Reactors Trainer (Armfield, CEB MKII issue 3)

For adiabatic operation, the water pump must be switched off. In order to measure the

conductivity of the reaction mixture, the equipment is supplied with a combined

conductivity and temperature probe as shown in Figure 1.5. The conductivity and the

temperature inside the reactor are displayed as digital readings using armsoft data logger

unit.

21
 Figure 1.5.A: CEB MKII Transparent Batch Reactor, diagram and Layout

The batch reactor is shown in Figure 1.5. It is simply a transparent vessel with a capacity

of approximately 1-2 L. The reactor comes with a cover or lid and is fitted with an electric

motor-driven stirrer. The cover of the reactor is shown below and has an opening in order

to insert the combined conductivity and temperature probe. In addition, the reactor consists

of self-sealing quick-action couplings for the water inlet and outlet.

Figure 1.5.B: Reactor Led

22
 Figure 1.5.C: PID diagram

Procedures
Preparation of equimolar reactant feeds

1. Make up three 0.5 liter batches of 0.1 M sodium hydroxide and three 0.5 of 0.1M

ethyl acetate for each run use two equal batches from the prepared solutions.

IMPORTANT: It is essential when handling these chemicals to wear protective clothing,

gloves and safety spectacles.

2. Open Armfield Software and choose ‘Isothermal operation’

3. Set up the Hot Water Circulator as detailed in the Operation section in the operation

manual.

4. Adjust settings on the PID loop as detailed in Operation procedure for Isothermal

Operation and set point to 25°C, 30°C and 35°C for run1, run 2 and run 3

respectively.

5. Charge the batch reactor with 0.5 liters of the sodium hydroxide solution.

23
 6. Set the reactor agitator to '50%' and press ‘Power on’ to start the agitation. Then

press ‘Hot Water Circulator’ and water will start to recirculate through jacket

reactor and vessel.

7. As the experiment involves the collection and storage of conductivity data, the data

output port in the plinth must be connected to the computer with Armfield Interface

data logger. This will enable data logging of the conductivity, temperatures and

stirrer speed values at selected time intervals over a selected period.

8. Ensure the conductivity and temperature sensors have both been installed in

accordance with the Installation section.

9. Collection of data will be until a stable condition is reached in the reactor and this

takes approximately 30 minutes. It is advisable to set the data collection period to,

say, 45 minutes.

10. Switch on the Hot Water Circulator. The temperature of the sodium hydroxide in

the reactor vessel will begin to rise and will be automatically maintained at the

desired set-point (25o C in the first run) by the action of the HWC in the jacket.

11. Carefully add to the reactor 0.5 L of ethyl acetate solution and instigate the data

logger program.(Don’t Forget to start recording the data at this moment)

It has been determined that the degree of conversion of the reagents affects the conductivity
of the reactor contents. By recording the conductivity with respect to time, either manually
or using the Armfield Data Logger, the amount of conversion can be calculated.

12. Record conversion values every 30 seconds for 30 minutes

24
 13. The experiment should be repeated as above but with the temperature controller set

to 30°C or 35°C.

Data collected/entered
1- Initial concentrations, volumes of each reactant

2- Isothermal Temperature

3- Conductivity Vs time

4- Conversion of NAOH Vs time

Results Analysis
1. Plot conversion factor/initial concentration Versus time for each run

2. From the isothermal batch reactor data, calculate the reaction rate constant (𝑘) at 25 o C,

30o C, and 35o C by creating plots shown in Figure 1.2

What is the effect of the temperature on the specific rate constant?

3. From the calculated rate constants, determine the activation energy (𝐸𝑎 ) and the

frequency factor (𝐴) for the reaction (Figure1.3)

4. Compare the results with values reported in the literature

Activation Energy Ea from Literature

(J/mol) 48367

Calculated Ea (J/mol)

5. Compare and discuss the reaction medium temperature effect on the conversion values.

Errors

Random Error

25
Every measurement that was conducted in this experiment produced a percentage
uncertainty which ultimately led to the overall percentage uncertainty of the activation
energy this produces a near negligible percentage uncertainty contribution to the overall
percentage discrepancy. How-ever, due to the only two data points available, there is a low
condense in the reliability of this experiment. The total amount of random error in this
experiment could be reduced by increasing the amount of measured temperatures and trials
per temperature.

Systematic Error

The systematic error of this experiment is expected to have a near 100% contribution to
the overall percentage discrepancy and is main error that should be considered to improve
the experimental procedure. The systematic error differs from the random error such that
is it due to an experimental law that pushes the direction of the data points in one specific
direction.

A possible experimental law with this experiment is due to the inadequate calibration of
the conductivity probes that may possibly show a lower rates of reactions at higher
temperatures which may reflect on a less steep slope which ultimately leads to a lower
reported activation energy (if it was found to be lower for example or vice versa so reflect
it to your specific case) which corresponds to the data points obtained.

This experimental law could be overcome by calibrating the conductivity probes with
conductivity buffer solutions. This would allow the measure conductivity values to be
within the calibrated values.

26
 Data Sheet:

Experiment # 1– Kinetic Studies in a Batch Reactor

Running Mode:

Volume of NaOH and Ethyl Acetate:

Total Volume of reactor:

Initial concentration of NaOH or Ethyl Acetate:

Final concentration of NaOH or Ethyl Acetate:

Table 1.2: Collected data from the batch reactor

NO. Temperature, Conductivity Concentration of Conversion,

Time, 𝒕 (s)
NaOH (M)
T (o C) k(mS/cm) X(-)

27
 EXPERIMENT #2
CONTINUOUS STIRRED TANK REACTOR (CSTR)

28
Objectives
The aim of this experiment is to study the liquid-phase saponification reaction of ethyl acetate with sodium
hydroxide in a continuous-stirred tank reactor (CSTR). The main objectives of the experiment are to:

1. Operate and analyze a CSTR

2. Monitor and analyze the CSTR from start-up (unsteady state) to steady state

3. Study the effect of space time on the steady- state conversion in the CSTR

4. Compare the experimental conversion to the theoretical conversion values.

Safety Precautions
1. This experiment uses both acids and bases. Use caution when handling these reagents. Review the

Material Safety Data Sheet (MSDS) of NaOH, CH3 COOC2 H5 , CH3 COONa and C 2 H5 OH before

starting the experiment and Read the Risk Assessment for the performed experiment.

2. Personal protective equipment shall include safety glasses. Disposable gloves should be worn when

handling NaOH solutions

3. Mask should be used while using ethyl acetate since it is hazardous in case of inhalation. In addition,

ethyl acetate is highly flammable (flash point: -4.4o C) and therefore, must be kept away from open

flames, sparks, and heat

4. A small amount of NaOH spilled on the outside of glassware can cause the glassware and

equipment to be extremely slippery when wet. Therefore, extreme care is required while handling

the glassware

5. Collect all the waste chemical solutions in the container marked as waste solution. At the end of

each lab period or the end of the experiment, add sufficient base (NaOH) to yield a phenolphthalein

29
 end point (pink) that does not disappear overnight. This indicates the reaction has gone to

completion and the waste can be disposed down the drain.

Introduction
A continuous-stirred tank reactor (CSTR) is used very commonly in industrial processing and is simply a

stirred tank operated continuously (continuous flow of reactants and products) as shown in Figure 2.1

Figure 2.1: Continuous Stirred Tank Reactor CSTR (Fogler, 2005)

A CSTR may also be referred to as vat, or back-mix reactor, and is used primarily for liquid phase
reactions. Normally, a CSTR is operated under steady state conditions. The reactor is also well-mixed
which allows for modeling the CSTR with no spatial variations in temperature, concentration, or reaction
rate throughout the reactor. This means that every variable is the same at any point within the reactor.
Since the temperature and the concentration are identical everywhere inside the reactor, they are also the
same at the exit of the reactor. Thus, the temperature and concentration in the exit stream are modeled as
being the same as those inside the reactor. However, in systems where mixing is highly non-ideal, the
well-mixed model is inadequate and other modeling techniques such as residence time distribution are
required in order to obtain meaningful results. Typical characteristics of CSTRs are summarized in Table
2.1.

30
 Table 2.1: Applications, advantages, and disadvantages of batch reactors (Fogler, 2005)

Type of Reaction Advantages Disadvantages

1. Gas liquid reactions 1. Continuous operation 1. Low conversion per unit volume

2. Liquid phase reactions 2. Good temperature 2. By-passing and channeling

control possible with poor agitation

3. Liquid solid reactions

3. Robust control

4. Low labor cost

5. Easy cleanup

Theory
The saponification reaction of ethyl acetate with sodium hydroxide is expected to follow a pseudo second

order elementary irreversible reaction. The reaction will proceed according to the reaction scheme shown

below:

NaOH + CH3 COOC2 H5 → CH3 COONa + C2 H5 OH

This reaction may be either reversible or irreversible. If considered irreversible elementary reaction, the

kinetic expression or the rate law can be written as follows:

−𝑟𝐴 = 𝑘𝐶𝐴 𝐶𝐵 (1)

Where, 𝑟𝐴 is the rate of the reaction [mol/L.s], 𝑘 is the reaction rate constant [L/mol.s], and 𝐶𝐴 and 𝐶𝐵 are
the concentrations [mol/L] of the sodium hydroxide and ethyl acetate, respectively.

The temperature dependence of the reaction rate constant (𝑘) could be correlated by Arrhenius equation:
−𝐸𝑎
𝑘 = 𝐴𝑒 𝑅𝑇 (2)

−𝐸𝑎
ln(𝑘) = ln (𝐴) − (3)
𝑅𝑇

31
 Where, A is the pre-exponential factor or frequency factor [L/mol.s], 𝐸 is the activation energy [J/mol], R
is the gas constant [8.314 J/mol K], and T is the absolute temperature [K].

In this experiment, again conductivity measurements will be used to find out the steady state concentration

of sodium hydroxide and hence, the steady state conversion in the CSTR. Recall that the conductivities of

ethyl acetate and ethyl alcohol can be neglected since the OH- ions are the most conductive species in the

reaction mixture. Therefore, the steady state conversion of the reaction can be obtained by tracing the

steady state conductivity of sodium hydroxide. The calibration plot between the specific conductivity and

sodium hydroxide concentration is shown in Figure 2.2.

Figure 2.2: Example of Calibration curve between specific conductivity in the CSTR and sodium
hydroxide concentration

Equipment
 The base unit for this experiment is the same as in the batch reactor experiment. The chemical

reactors trainer (Model: CEM MKII, Armfield) will be used. The base of the unit is shown in

Figure 2.3 and will be used to fit the CSTR.

32
 FIGURE 2. 3: BASE UNIT FOR CHEMICAL REACTORS TRAINER (ARMFIELD , UK)

In this experiment, the base unit will be fitted with the CSTR. The base unit consists of a main switch to

supply power to the unit and two feed tanks for the reactants (sodium hydroxide and ethyl acetate). The

two reactants can be fed to the reactor from the tanks using two peristaltic pumps fitted in front of the base

unit. The pumps can be switched ON or OFF using the switches on the switch box. In addition, the pump

speed can be adjusted by tuning the potentiometers which act as pump speed regulators. The switch box

also contains a switch and an adjuster to control the stirrer. Behind the switch box, there is a water tank

with a heater and a centrifugal pump with which hot or cold water can be supplied to the stainless steel

heat exchanger coils (Figure 2.4) within the CSTR. The hot water is required in case if the CSTR is to be

operated under isothermal conditions. The temperature in the hot water tank is controlled by a controller

fitted on the switch box. This controller switches the heater ON or OFF based on the signal received from

the temperature sensor fitted within the water tank. The switch box also contains ON/OFF switches for

both the heater and the water pump. In order to measure the conductivity of the reaction mixture, the

33
 equipment is supplied with a combined conductivity and temperature probe. The conductivity and the

temperature inside the reactor are displayed as digital readings on the switch box of the base unit.

The CSTR is shown in Figure 2.4 and is simply a tank made of chemically resistant borosilicate glass.

The CSTR contains an adjustable overflow (a sliding pipe) that enables the experiment to be performed

with different volumes between 0.4 to 1.5 L. From the overflow, the products and unreacted feeds exit the

reactor. The CSTR is also equipped with an electrical motor driven stirrer (0 to 300 rpm). The top of the

reactor has an opening in order to insert the combined conductivity and temperature probe.

The piping & instrumentation diagram (P&ID) of the apparatus is shown below:

FIGURE 2.3: P&ID OF THE CSTR APPARATUS . 1) CSTR, 2) PERISTALTIC PUMP, 3) REACTANT A
TANK, 4) R EACTANT B TANK, 5) PRODUCT OUTLET, 6) WATER PUMP, 7) WATER HEATER, 8)
WATER TANK

Procedures
Preparation of equimolar reactant feeds

Prepare 5 L of 0.25 M sodium hydroxide solution and 5 L of 0.25 M ethyl acetate solutions at room

temperature

Fixing the reaction mixture volume

34
The experiment can be carried out at different volumes of reaction mixture by adjusting the height of the
overflow in the CSTR. In this experiment, the volume of the reaction mixture will be fixed at 1 L. In order
to adjust the reaction mixture volume, follow the sequence of steps given below:

1. Fix the CSTR on the base unit CEXC

2. Make sure the CSTR is empty

3. Make sure the feed pipes are connected to the reactor inlets

4. Adjust the height of the overflow to the sign at the middle of the reactor height

Determining the space time (τ)

1. Set the flow rate of each reactant (both are equal) calculate the total volumetric flow rate in to the

reactor.

2. Divide the reaction mixture volume (1 L) by the volumetric flow rate to determine the space time

Studying the effect of space time on conversion

1. Remove the caps of the reagent bottles and carefully fill with the reagents to a level approximately
50mm from the top using a funnel if necessary. Refit the caps.

2. Start the software using the option of the experiment with heater.

3. Click the ‘Power on’ button on the mimic diagram, click the ‘Hot Water Circulator’ button and
water will start to recirculate through the hot water circulator and coil in the reactor.

4. Adjust the set point of the PID controller to 30°C. Change the PID ‘mode of operation’ to
‘Automatic’

5. Collection of conductivity data should continue until a steady state condition is reached in the
reactor and this takes approximately 30 minutes. It is advisable to set the data collection period to,
say, 45 minutes.

6. Set the pump speed controls to 40ml/min flow rate in the software.

7. Fill the concentration of both solutions in their respective boxes in the software.

35
 8. Fill the volume of the reactor in the box on the software. Set the stirrer speed to 50% in the
software.

It has been determined that the degree of conversion of the reagents affects the conductivity of the reactor
contents so that recording the conductivity with respect to time using the Armfield data logger can be used
to calculate the amount of conversion.

1. Repeat steps 1-8 at 50 ml/min and 60 ml/min reactants flow rates

2. Observe the effect of space time (reactant flow rates) on the steady state conductivity inside the

CSTR

3. Drain the CSTR and rinse it with pure water

Results Analysis
1. Plot the conservation by time for each run

2. Compare and discuss the effect of space time on steady state conversion

3. Calculate the reaction rate constant at each run

4. Calculate theoretical Steady State Conversions for each run and compare with the experimental

values.

36
Example of Calculations
If the following data is given estimate the error in the conversion experimental values:

Volume of the reactor

1.2
(L)

Initial concentration of
NaOH to reactor inlet, 0.125
Cao (M)

Theoretical rate constant

at room temperature, k 0.1125*
(L/mol.s)

*reference. (pg. 1839)

https://www.uv.es/idiqlab/labquimicos/documentos/art%C3%ADculo%20con%20la%20energ%C3%ADa%20de
%20activaci%C3%B3n%20de%20la%20reacci%C3%B3n.pdf

Fill the following Table:

Flow (L/s) of each space time (s) Experimental Da number Theoretical % Error
reactant conversion X conversion X
using Da number

2.9804E-03 0.61
0.48
4.7509E-03
0.41
5.5383E-03

37
Solution:
Flow (L/s) of each space time (s) Experimental Da number Theoretical % Error
reactant conversion X conversion X
using Da number
201.32
2.9804E-03 0.61
126.29 0.48
4.7509E-03
108.34 0.41
5.5383E-03

1. Equations used to estimate the space time:

Equations used to estimate the experimental conversion:

𝑘 − 𝑘𝑒𝑞
𝑋=1−
𝑘𝑜 − 𝑘𝑒𝑞

X is conversion, k is steady state specific conductivity,

𝑊ℎ𝑒𝑟𝑒, 𝑘𝑒𝑞 𝑖𝑠 𝑡ℎ𝑒 𝑒𝑤𝑢𝑖𝑙𝑖𝑏𝑟𝑖𝑖𝑢𝑚 𝑓𝑖𝑛𝑎𝑙 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑐𝑜𝑛𝑑𝑢𝑐𝑡𝑖𝑣𝑖𝑡𝑦, 𝑘𝑜 𝑖𝑠 𝑡ℎ𝑒 𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 𝑐𝑜𝑛𝑑𝑢𝑐𝑡𝑖𝑣𝑖𝑡𝑦

Equations used to estimate the reaction rate constant:

Consider 2nd order reaction:

𝑉 𝐶 𝑋
𝜏= = 𝐴𝑜 𝐴
𝜈𝑜 −𝑟𝐴

−𝑟𝐴 = 𝐾𝐶𝐴 𝐶𝐵

𝐶𝐴 = 𝐶𝐴𝑜 (1 − 𝑋)

38
 𝐶𝐵 = 𝐶𝐵𝑜 (Ө𝐵 − 𝑋)

𝑏𝑢𝑡, 𝐶𝐵𝑜 = 𝐶𝐴𝑜 , Ө𝐵 = 1

So,
𝐶𝐵 = 𝐶𝐴𝑜 (1 − 𝑋)

−𝑟𝐴 = 𝐾𝐶𝐴 2

𝐶𝐴𝑜 𝑋𝐴 𝐶𝐴𝑜 𝑋𝐴 𝑋𝐴
𝜏= = =
−𝑟𝐴 𝐾𝐶𝐴 2 𝐾𝐶𝐴𝑜 (1 − 𝑋)2

𝑋𝐴
𝜏𝐾 =
𝐶𝐴𝑜 (1 − 𝑋)2

𝑋𝐴
𝐺𝑟𝑎𝑝ℎ𝑖𝑐𝑎𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛: 𝑖𝑓 𝑦𝑜𝑢 𝑝𝑙𝑜𝑡 𝑉𝑒𝑟𝑠𝑢𝑠 𝜏, 𝑡ℎ𝑒 𝑠𝑙𝑜𝑝𝑒 𝑚𝑢𝑠𝑡 𝑏𝑒 𝑡ℎ𝑒 𝐾 𝑣𝑎𝑙𝑢𝑒.
𝐶𝐴𝑜 (1 − 𝑋)2

𝑇𝑜 𝑑𝑜 𝑡ℎ𝑖𝑠 𝑦𝑜𝑢 𝑛𝑒𝑒𝑑 𝑐𝑜𝑛𝑣𝑒𝑟𝑠𝑖𝑜𝑛 𝑎𝑛𝑑 𝑠𝑝𝑎𝑐𝑒 𝑡𝑖𝑚𝑒 𝑣𝑎𝑙𝑢𝑒𝑠 𝑓𝑜𝑟 3 𝑟𝑢𝑛𝑠

2. Equations used to estimate the Damkohler number (Da no).:

−𝑟𝐴𝑜 𝑉 𝐾𝐶𝐴𝑜 2 𝑉 𝐾𝐶𝐴𝑜 𝑉

𝐷𝐴 = = = = 𝐾𝐶𝐴𝑜 𝜏
𝐹𝐴𝑜 𝐶𝐴𝑜 𝜈𝑜 𝜈𝑜

Theoretical value of K is given, space time 𝜏 𝑖𝑠 𝑐𝑎𝑙𝑐𝑢𝑙𝑎𝑡𝑒𝑑 𝑓𝑟𝑜𝑚 𝜏 =

𝑉
, 𝑤ℎ𝑒𝑟𝑒 𝑉 𝑖𝑠 𝑡ℎ𝑒 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑟𝑒𝑎𝑐𝑡𝑜𝑟, 𝜈𝑜 𝑖𝑠 𝑡ℎ𝑒 𝑡𝑜𝑡𝑎𝑙 𝑣𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤 𝑖𝑛 𝑡𝑜 𝑡ℎ𝑒 𝑟𝑒𝑎𝑐𝑡𝑜𝑟.
𝜈𝑜

3. Equations used to estimate the Theoretical conversion;

Consider 2nd order reaction:

39
 1 + 2𝐷𝐴 − √1 + 4𝐷𝐴
𝑋𝐴𝑡ℎ =
2𝐷𝐴

4. Equations used to estimate the % Error:

𝑋𝑡ℎ −𝑋𝑒𝑥𝑝
% 𝐸𝑟𝑟𝑜𝑟 = | | 𝑥100%
𝑋𝑡ℎ

40
Data Sheet
Reaction mixture volume = 1 L

Table 2. 1: Space time data

#Run Reactant total Volumetric Flow rate, Volumetric Reactor Space time
flow rate v0 (ml/min) Flow rate, v0 Volume (L)
𝜏(s)
(ml/min) (L/s)

1 25x2 50

2 30x2 60

3 40x2 80

Table 2. 2: Data for calculating the reaction rate constants

#Run Total Volumetric Steady state

flow rate conversion

(ml/min) T= 30o C

1 50

2 60

3 80

41
 EXPERIMENT #3
CONTINEOUS STIRRED TANK IN SERIES
Residence Time Distribution (RTD)

42
Objectives
The objective is to:

1. Calculate the residence time distribution (RTD) of three reactors in series followed by a tubular

reactor by introducing a pulse change in the input

2. Use the RTD curve to determine the fraction of material leaving the reactor in a certain time

interval

Safety Precautions:
 Ware your safety googles, gloves and lab coat.

 Read the MSDS of NaOH before performing the experiment.

 Prepare NaOH and operate the equipment in well ventilated areas.

 A small amount of NaOH spilled on the outside of glassware can cause the glassware to be

extremely slippery when wet. Be careful.

Introduction
The residence time distribution (RTD) is probability distribution function that describes the amount of
time spent by a fluid element inside a reactor. RTD studies on reactors are performed in order to study the
mixing and flow characteristics and compare the performance of real reactors with the ideal ones. In any
given reactor, the amount of time spent inside the reactor (residence time) is different for each element
present. This implies that the reaction time for each element and hence, the product distribution within the
reactor will vary.

The RTD is typically determined experimentally by injecting an inert chemical called tracer into the
reactor at some reference time t = 0 followed by measurement of the tracer concentration at the outlet. The
properties of an ideal tracer are the following:

1. The tracer must be inert to the reaction mixture (non-reactive)

2. It must be easily detectable using simple measurement devices (such as conductivity, color, etc.)

43
 3. It must possess physical properties similar to those of the reaction mixture

4. It should not adsorb on the walls or other surfaces in the reactor

In this experiment, RTD will be determined by introducing a pulse change at the reactor input. At time t
= 0, the tracer (0.1 M NaCl) will be introduced for a certain time interval. The NaCl concentration at the
reactor outlet C(t) will be measured with time. The RTD distribution function E(t) can then be determined
as follows (Fogler, 1999):

Eq (3.1)

In case of pulse input change, the expected response in the outlet tracer concentration is shown in Figure
3.1.

Figure 3.1: Response to pulse change in the reactor inl

44
Apparatus
Figure 3.2 shows the Armfield CEP MKII equipment used to demonstrate the concept of RTD as the liquid
moves through three CSTRs in series and one tubular reactor (PFR). The RTD is generated by making a
pulse change in NaCl concentration in the inlet stream to the first reactor and measure the change in
conductivity in the subsequent reactors.

The apparatus consists of two feed tanks (1) containing either deionized water or a 0.1 M sodium chloride
solution. The feed is pumped through the liquid feed lines (2) using peristaltic pumps (3 and 4). The pump
speed can be regulated on the potentiometers (5). From the peristaltic pumps, the feed is pumped into
reactor 1 at (6). The reactor content is mixed by the stirrer (7), which is driven by an electromotor (8). The
stirrer speed is controlled by the potentiometer (9). The sodium chloride concentration in reactor 1 is
measured by a conductivity cell (10). A similar arrangement of conductivity cells, stirrers, motors and
control units are used for reactors 2 and 3. From reactor 1, the liquid flows through an underflow into
reactor 2 and from reactor 2 through an overflow (11) into reactor 3. From this reactor, the liquid flows
into a tubular reactor (12), and from there to a final measurement cell (13). The height of the last
conductivity cell should be adjusted so it is in level with the overflow in the reactors. The conductivity
measured by the conductivity cells can be read on the display (14). The cell value to be displayed is chosen
by turning the selector knob (15). The conductivity reading, stirrer speed, and liquid flow can be
transmitted from the data output sockets (16) to a PC. The pumps can be turned off by switching the switch
(17) from manual to remote and on by switching back to manual. The main switch for the CEP MK II is
on the front at (18).

45
 Figure 3.2: CEP MKII apparatus from Armfield for measuring RTD in series of reactors

Procedure

46
 1. Make sure the main switch on the apparatus is turned off

2. Switch both peristaltic pumps on remote mode

3. Switch all stirrers on remote mode

4. Prepare 0.1 M NaCl solution by dissolving 29 gram NaCl in five liters of deionized water

5. Fill the salt solution tank with the 0.1 M salt solution

6. Fill the deionized water tank with 5 liters of deionized water

7. Fill the three CSTRs with deionized water. Do not use the peristaltic pump since it will fill the

tank very slowly

8. Switch on the main switch of the apparatus

9. Turn the stirrer switches to manual mode and set their speed setting to 8.0 on the speed adjust

dial.This will switch on the stirrers

10. Turn the deionized water pump to manual and adjust the volumetric flow rate to the desired

value ( set to 6.0 on the speed adjust dial)

11. Start the water feed pump and set to 6.0 on the speed adjust dial. Note: When using the data

logger, the pump and stirrer speeds should be set using the appropriate10 turn

potentiometer with the switch set to ‘On’. The set speed will then be recorded by the data

logger.

12. While the flow settles, setup the data logger on the PC take samples of conductivities every 10

seconds over a 45 minute period.

13. Make sure all measuring points are delivering data to the PC and that the readings for feed flow

and stirrer speed is correct

14. Start recording the data

47
 15. Switch on the salt-solution pump, with the speed set to 6.0 on the speed adjust dial for 20

seconds, to introduce a pulse change at the input

16. Switch of the salt-solution pump

17. Follow the change in conductivity in the four reactors on the PC

18. Switch off the pumps once the conductivity values become constant

19. Save the data in an Excel file

20. Turn off stirrers and main switch

After the end of the experiment

1. Undo all the connections to the reaction vessels and remove the measuring sensors

2. Rinse the measuring sensors with water

3. Drain the reaction vessels and rinse it out with water

4. Drain both tanks and rinse it out

5. Operate NaOH pump with water to clean it

6. Correctly dispose of the product of the reaction collected in the collecting tray

7. Switch off unit at master switch

48
Calculations
1. Plot the concentration in reactor 1 versus time

2. Determine E(t) using Eq. (3.1)

3. Plot E(t) versus time

4. Compare the response to the expected response shown in Figure 3.1

5. Interpret the RTD curve

49
 EXPERIMENT #4
TUBULAR FLOW REACTOR

50
Objectives
The object of this experiment is to study the behaviour of a plug-flow reactor by performing a series of
experiments on the saponification of ethyl acetate.

1- Estimate the Order of the reaction and the rate constant using the Numerical Differential method

https://www.youtube.com/watch?v=9LFwcgJ0Q28

1- Estimate the Order of the reaction and the rate constant using the Graphical Integral method

https://www.youtube.com/watch?v=7dWjyjcYrm8

https://www.youtube.com/watch?v=plXbgRYW7B8

Introduction
Tubular reactors are often used when continuous operation is required but without back mixing of

products and reactants. The Armfield CET MkII Tubular Reactor is specially designed to allow detailed

study of this important process. It is one of three reactor types which are interchangeable on the Reactor

Service Unit (CEX MkII), the others being CEM MkII Continuous Stirred Tank Reactor and CEB MkII

- Batch Reactor.

Reactions are monitored by conductivity probe as the conductivity of the solution changes with

conversion of the reactants to product. This means that the inaccurate and inconvenient process of

titration, which was formally used to monitor the reaction progress, is no longer necessary.

Equipment
The Reactor Vessel

51
FIGURE 4. 1 TUBULAR REACTOR VESSEL (ARMFIELD, 2016)
As shown in Figure 4.1, the reactor vessel (1) is set on a baseplate (14) which is designed to be located
on the four studs of the CEX service unit and then secured by thumbnuts (15). The positioning of the
reactor on the service unit is illustrated. The reactor is positioned on the service unit with the non-return
valve sited on the left and towards the rear. The tubular reactor in which the chemical reaction takes place
is a flexible coil (4) wound around an acrylic former. Total volume of the reactor coil is 0.4 L. In order
to maintain a constant temperature throughout the reactor coil, the coil bundle is submerged in circulating
water which is automatically maintained at a pre-selected temperature by the temperature controller (TIC)
in the console. The actual temperature of the circulating water and therefore the reactants is relayed to the
controller by a sensing probe (TS) which is held in gland (8) in the lid. Water enters from the circulator
at the non-return valve (11) - this prevents water draining back through the priming vessel of the circulator
when the pump is stopped. Water leaves the reactor at overflow (12) and returns to the circulator.

FIGURE 4. 2 TOP OF THE TUBULAR R EACTOR VESSEL

52
A filling plug (17) is provided on the top of the reactor vessel to allow the vessel to be filled with clean

water. This plug (with sealing washer) must be fitted when the hot water circulator on the CEX service

unit is in operation. Sockets in the side of the console pod of the service unit are provided to connect the

conductivity probe and temperature sensor to the instrumentation in the console. These are of a different

size so that the probes cannot be wrongly connected. When not in use, the reactor can be drained using

valve (13) in the base.

Flow of materials

Reactants are pumped from the two feed tanks by the peristaltic pumps and enter the reactor through

connectors (6) and (7) in the lid of the vessel. Each reactant is preheated by heat transfer coils (2) and (3)

before being blended together in “T” fitting (5). The reactants pass up through the reactor coil and leave

the reactor vessel through the conductivity probe housing (16). This housing allows the conductivity

probe (CP) to be held in the stream of reactants emerging from the reactor. Flexible tubing from the hose

nozzle (10) is used to guide the reactants to drain.

53
FIGURE 4. 3 TUBULAR REACTOR LAYOUT

Temperature in the reactor is controlled by circulating heating or cooling liquid through the interior of

the reactor (13). The volumetric ratio in which the reactants are mixed is defined by the relative flow rates

of the two pumps. If the pumps are operated at the same flow rate then the reactants are mixed in equal

volumes. The residence time in the reactor is defined by the total flow rates of the two feed pumps. The

total volume of the reactor coil is approximately 400 mL. Dividing this volume by the combined flow

rates of the feed pumps in mL/s will yield the residence time in seconds. The extent of conversion of the

reactants is determined from the conductivity, which is measured by the conductivity probe sited in the

housing (16) where the liquid stream exits the reactor. It is important that the probe is inserted into the

housing with the electrode access holes in the glass surround in line with the flow.

54
 FIGURE 4. 4 TUBULAR REACTOR VESSEL TUBES AND VALVES
The Armfield Continuous Tubular Flow Reactor is designed to demonstrate the mechanism of a chemical

reaction in such a reactor as well as the effects of varying the process conditions such as reaction

temperature, reactant concentration, feed rate etc

The reaction chosen is the saponification of ethyl acetate by sodium hydroxide as it can be carried out

under safe conditions of temperature and pressure and is well documented although it may be possible to

carry out demonstrations using other chemicals it is not advisable as the materials of construction of the

reactor may not be compatible. Before carrying out reactions involving any other reagents please refer to

Armfield Ltd. for advice.

Procedures

DILUTION OF ETHYL ACETATE FOR USE WITH CET MKII REACTOR

55
Armfield recommends the use of a 0.1M solution of Ethyl Acetate in the CET MkII reactor. This should

be made by diluting concentrated Ethyl Acetate as follows:

Therefore add 9.79 ml of concentrated Ethyl Acetate to 900 ml of deionised or distilled water. Shake the

mixture vigorously until the two liquids have mixed. Add further water to make up the final volume to

1000 ml.

Note: The practice of making a strong solution (e.g. 1M) then further diluting this to the required

concentration (e.g. 0.1M) cannot be applied when using Ethyl Acetate. The required dilution should be

made directly as stated above.

DILUTION OF SODIUM HYDROXIDE FOR USE WITH CET MKII REACTOR

Armfield recommends the use of a 0.1M solution of Sodium Hydroxide in the CET MKII reactor. This

may be made by adding 4.0g of NaOH to 960ml of deionised water then making up the solution to 1000ml.

56
IMPORTANT: It is essential when handling these chemicals to wear protective clothing, gloves and
safety spectacles.

1. Remove the lids of the reagent vessels and carefully fill with the reagents to a level approximately

50mm from the top. Refit the lids.

2. Adjust the set point of the temperature controller to 25°C.

3. As the experiment involves the collection and storage of conductivity data, the data output port in

the console must be connected to the Armfield IFD data logger and the computer as detailed in

the instruction leaflet supplied with the interface. This will enable data logging of the conductivity

at selected time intervals over a selected period. If a computer is not available then the conductivity

can be recorded manually at half minute intervals, by reading the value directly from the

conductivity meter in the console.

4. Ensure the conductivity probe and temperature sensor have been installed in accordance with the

section CONNECTION TO SERVICES.

5. Collection of data will be until a steady state condition is reached in the reactor and this takes

approximately 30 minutes. It is advisable to set the data collection period to, say, 45 minutes.

6. Set the pump speed controls to give 40 ml/min, 50 ml/min and 60 ml/min flow rate for each

reactant in the first second and third run respectively.

7. Prior to priming the hot water circulating pump, fill the reactor with cold water. To fill the vessel,

it is necessary to pinch together the walls of the tubing connecting the overflow to the hot water

circulator, either manually by bending and holding the tube or using a suitable clip (ensuring that

any clip used will not cause damage to the tubing).

8. Fill the vessel to a level above the overflow (return to the circulator), just below the reactor lid,

using a suitable hose from a domestic supply through the temperature sensor gland (8) in the lid.

57
 A non-return valve (11) prevents water flowing out of the reactor via the inlet. Ensure the

temperature sensor is re-fitted and the gland tightened securely by hand before releasing the outlet

tubing.

9. Prime the pump as detailed in the OPERATIONAL PROCEDURES section of the CEX manual.

10. Switch on the hot water circulator. The temperature of the water in the reactor vessel will begin

to rise and will be automatically maintained at the desired set-point (25o C in this instance).

11. Switch on both feed pumps and instigate the data logger program (or begin taking readings if no

computer is being used).

12. Reactants will flow from both feed vessels and enter the reactor through the connections in the

lid. Each reactant passes through pre-heat coils submerged in the water in which they are

individually brought up to the reaction temperature. At the base of the tubular reactor coil, the

reactants are mixed together in a "T" connection and begin to pass through the coil. The reacting

solution will emerge from the coil through connector (16) in the lid where a probe senses

continuously the conductivity which is related to degree of conversion.

It has been determined that the degree of conversion of the reagents affects the conductivity of the reactor

contents so that recording the conductivity with respect to time using the Armfield Data Logger can be

used to calculate the amount of conversion.

Results Analysis

1. The conductivity measurements must now be translated into degree of conversion of the constituents.

2. Both sodium hydroxide and sodium acetate contribute conductance to the reaction solution whilst

ethyl acetate and ethyl alcohol do not. The conductivity of a sodium hydroxide solution at a given

concentration and temperature however, is not the same as that of a sodium acetate solution at the

same molarity and temperature and a relationship has been established allowing conversion to be

inferred from conductivity

58
 3. The calculations are best carried out using a spreadsheet such as EXCEL so that the results can be

displayed in tabular and graphical form.

4. On conclusion of the experiment using the Armfield data logger, a set of readings of conductivity

with time will be stored in the computer.

5. At this point, this data can be transferred onto the spreadsheet.

6. Start the spreadsheet program.

7. Now enter the following known constants from the experiment using the Nomenclature list on the

end of the experiment manual. Ensure use of correct units.

59
For the values of each of the above, the spreadsheet can be used to calculate values of sodium hydroxide

concentration (a1 ) and sodium acetate concentration (c1 ) and the degree of conversion (Xa ) and (Xc) for

each of the samples of conductivity taken over the period of the experiment.

These can be calculated and listed in columns (use spreadsheet COPY facility) alongside the readings of

conductivity using the following equations

To calculate the specific rate constant, k:-

The overall mass balance at steady-state condition may be written as:-

Input – Output ± Reaction = 0 i.e. for a reactant a in a reactor of volume V

For the continuous reactor operating at steady state the volume may be assumed constant and

The steady state concentration of NaOH in the reactor a1 may be used to calculate the specific rate constant
k. Comment upon the results obtained.

Notes:

1. It is recommended that this experiment should be repeated at various other temperatures to investigate

the relationship between the specific rate constant (k) and the temperature of reaction.

60
2. It is further recommended that the experiment be repeated using dissimilar flowrates for the caustic soda

and ethyl acetate solutions to investigate the effect that this will have upon the saponification process.

3. Rinse the feed tanks with demineralised water and pump the water through the reactor to rinse out the

chemicals. The reactor can be left with water in the coil ready for the next experiment.

4. When removing the CET reactor from the service unit always drain using the drain valve under the

baseplate first.

61
Results Analysis

1. Plot the concentration in reactor 1 versus time

2. Use integral method to find the order of the reaction

3. Use the differential method to find the order of the reaction

4. Interpret the RTD curve

Technical data:

Reactor dimensions:

Pre-heat coils (each):

Total length: 1.2m

Internal diam: 4.9mm

Total vol of coil: 0.02L

Reactor coil:

Total length: 20.9m

Internal diam: 5.0mm

62
 Experiment#4 Tubular Reactor

Data Sheet

Flow Rate of each reactant (ml/min):

Temperature (oC): Initial concentration of NaOH M= Volume of reactor (L)=

Time (s) Conductivity k (mS/cm) Conversion of NaOH x

63
PART B

UNIT OPERATIONS LAB EXPERIMENTS

64
 EXPERIMENT #5
Packed Bed Absorption Column

65
Objective
The objectives of this experiment are to:

1- Determination of Overall Mass Transfer Coefficient (K og) of carbon dioxide into caustic soda in

Gas Absorption unit

2- Test the effect of changing gas flow rate on the Overall Mass Transfer Coefficient (Kog)

Safety Precaution
1. The following safety considerations need to be taken into account during the experiment:

2. Personal Protective Equipment (PPE): lab coat, googles, safety hats, safety boots and heat protective

gloves.

3. Follow the procedures carefully to avoid pump damage or Colum overflow.

4. Record the data on your data sheet to avoid missing the data.

Introduction

Packed bed absorption columns are extensively used in the chemical and petrochemical industry for
absorption of gases in liquids whether the gas is a useful product or harmful off-gas that has to be removed
from the exhaust gas (Treybal, 1987). To operate an absorption column successfully it is important to know
the hydraulic properties of the column. The removal of one or more selected components from a mixture
of gases by absorption into a suitable liquid is the second major operation of chemical engineering that is
based on inter- phase mass transfer controlled largely by rates of diffusion. Thus, acetone can be recovered
from an acetone-air mixture by passing the gas stream into water in which the acetone dissolves while the
air passes out. Similarly, ammonia may be removed from an ammonia-air mixture by absorption in water.
In each of these examples the process of absorption of the gas in the liquid can be treated as a physical
process, the chemical reaction having no appreciable effect. However, when oxides of nitrogen are absorbed
in water to give nitric acid, or when carbon dioxide is absorbed in a solution of sodium carbonate, a chemical
reaction occurs, the nature of which influences the actual rate of absorption. Absorption processes are
therefore conveniently divided into two groups, those in which the process is solely physical and those
where a chemical reaction is occurring. In absorption, the feed is a gas and is introduced at the bottom of
the column, and the solvent is fed to the top, as a liquid; the absorbed gas and solvent leave at the bottom,
and the unabsorbed components leave as gas from the top.

66
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:

Where,

N= Rate of absorption (g.moles/second)

Kog = Mass transfer coefficient (g.mol/atm.m2 .s)

a= specific area of packing /unit volume of tower (m2 /m3 )

AH= volume of column (m3 )

△Pm = log mean driving force (atm, mm Hg)

The log mean driving force is expressed as:

Where,

pi is pressure at the column inlet and p o is the pressure at column outlet.

67
Data Required

1. Liquid flow rate

2. Air flow rate

3. CO2% in the inlet and outlet

Procedure

A- To measure the absorption of carbon dioxide into caustic soda solutions flowing down the tower

using the gas analysis equipment provided.

1. Ensure that the water outlet from the column is fitted to the pipe that returns

water to the tank.

2. 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.

3. With gas flow control valves C2 and C3 closed, start the liquid pump and adjust the flow of caustic
soda through the column to approximately 3 litres/min on flowmeter F1 by adjusting control valve
C1.

4. Start the compressor and adjust control valve C2 to give an airflow of approximately 30
litres/minute in flowmeter F2.

68
 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.

5. Carefully open the pressure regulating valve on the carbon dioxide 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.

Analysis using Liquid stream:

6. After 15 minutes of steady operation, take samples at 20 minute intervals simultaneously from S4

and S5. It is recommended that a 250ml sample is taken so analysis can be done in duplicates. Note the

time the samples were taken in each case. Analyse both samples according to the procedure detailed

overleaf.

Analysis of Carbon Dioxide Dissolved in Caustic Soda/Sodium Carbonate Solutions Theory:

Under the conditions chosen for the absorption exercises, the amount of CO2 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.

69
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.

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. Accurately measure 100ml into two separate conical flasks for each

sample.

b. Flask 1 - Add a drop of phenolphthalein solution 1) to the contents and titrate until the pink colour just

disappears with the standard hydrochloric acid 3) Note the volume of acid added - T1, which is that

needed to neutralise 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 neutralisation 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 – T3, 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.

It is advisable to repeat all of the above to check reproducibility.

Calculations of Sample Composition

a. Concentration of NaOH in original sample:

b. Concentration of Na2CO3 in original sample:

70
 c. Amount of CO2 removed from air mixture:
During a time interval, or between the top and bottom of the column,
CN will increase as CO2 is absorbed in equi-molar proportions, while Cc should decrease in twice-
molar proportions.

Readings:

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:

Similarly, over a time period Ө seconds after a first sample is taken from the sump S 5:

CO2 absorbed = Volume of liquid in whole system x [(C N )t=Ө - (CN )t=o]

71
b- Analysis of Gas stream:

That gas samples at the inlet and outlet are to be taken using the following procedures:

Equipment Required

1. Carbon dioxide cylinder with integral pressure regulator, connected to regulator R on gas inlet on the
apparatus.

2. Approximately 300ml of 1.0M caustic soda solution with safety gloves and goggles. Small funnel and
tubing for filling analysis equipment.

Steps 1-5 are the same in part a

Step no. 6:

After 5 minutes or so of steady operation, take readings of CO2 % in the inlet and outlet gas streams.

Results:

A. CO2 content of gas samples:

Calculation of amount of CO 2 absorbed in column from analysis of samples at inlet and outlet.

If Fa is litres/second of CO 2 absorbed between top and bottom, then:

Where,

Yi: carbon dioxide mass fraction in the inlet stream

Yo: carbon dioxide mass fraction in the outlet stream

72
F2: flow rate of air in L/s

F3: flow rate of carbon dioxide in L/s

Fa CO 2 absorbed between top and bottom in L/s

Note: Litres/second can be converted to g.moles/second as follows:

G can be calculated from the fact that one gram-mole occupies 22.4 litres at

273k and 760mm Hg pressure.

G can be calculated from the fact that one gram mole occupies 22.42 litres at 273K and 760mm Hg
pressure:

Mass Balance:

At steady state, the transfer of absorbing gas from the gas stream should equal that transferred to the
liquid.

73
Let: L1 and Lo be the volume flow of liquid entering and leaving the column respectively.

Let: Gi and Go be the total gas molal flow entering and leaving the column respectively.

Let: Yi and Yo be the mole fractions of CO2 entering and leaving the column in the gas stream.

Amount of CO2 removed from the gas stream:

Gi - Go (gm.moles/sec) …... (1)

as no air dissolved in the solution.

But from Exercise B, the amount of CO 2 removed from the liquid stream equals the

amount of carbonate ions produced:

Lo.CNo - Li.CNi (gm.moles/sec) ….. (2)

The object is to check that (1) equals (2). Note that, while the liquid flows in and out are the same in this
exercise (Lo = Li), the gas flows are not equal because of the removal of CO2, and also because of the
pressure drop across the column.

Go can be calculated from a molar balance on the air stream, none of which is absorbed:

Go (1 - Yo) = Gi (1 - Yi)

G can be calculated from the fact that one gram mole occupies 22.42 litres at 273K and 760mm Hg
pressure:

G is the total molar flow with respect to temperature and pressure drop in the column Yi and Yo values
are taken from the apparatus.

Results and Calculations

1. N is calculated as explained before.

2. a is specific area of packing/unit volume of tower, which for 9mm Raschig rings is 440 m 2/m 3.

3. A.H. is volume of the column.

= volume of tower

74
4. Partial pressures (of CO 2):

Partial pressure = mole fraction x total pressure

Partial pressure = volume fraction x total pressure

Mass transfer coefficient:

75
Data Sheet:

EXP. 5. Gas Absorption

76
77
78
79
The results of both (2) and (3) show the mass balance and agree well with (1).

80
 Experiment #6
Cooling Tower

81
Objective:
- Perform mass and energy balance across the cooling Tower

- Test the cooling tower performance using different operating conditions

Safety Precautions
- Avoid contact between water and electricity.

- Wear your PPE’s

- Don’t run the pump if the water level below the minimum.

- Check the level of the tank to add makeup water every 10-15 minutes

- Use demineralized water in this experiment.

Introduction:
Bench Top Cooling Towers Study Unit enables the students to gain understanding of the operating

principles of cooling towers, where hot water is cooled by means of a large stream of air by

exploiting the water’s latent vaporization heat; it also makes it possible to compare the effects of different

filling packages. The training set is self-sufficient and can be easily moved within the laboratory.

The set reproduces on a small scale the operation of a forced circulation cooling tower, i.e., the type of

system widely used at present, though it should be noted that natural circulation towers are also used

commonly. With the aid of a forced air tower, the process is enhanced in clear and highly significant

manner. The self-sufficient unit allows to perform experiments on water cooling by using 3

interchangeable cooling towers having packing’s with different heat exchange surface.

82
Theory:

Cooling Tower Terminology

Forced Draft – This is the system utilised on UOP6-MKII whereby a fan (or fans) at the base
the cooling tower promotes a forced upward flow of air through the packing. Alternative
arrangements used in full sized systems are Induced Draft whereby fans located at the top of
the tower pull air through the packing or Natural Draft where the height and hyperboloid
shape help to induce a natural draft.

Packing or Filling - The material over which the water flows as it falls through the tower, so
that a thin film of water is spread over a large surface area in contact with the air stream.

The type of packing supplied is referred to as ‘Film Fill’ type whereby water flows over the
surface of the packing creating a thin film that is spread over a large area. An alternative type
of packing (not supplied) is ‘Splash’ type packing whereby the packing interrupts the flow of
water and causes splashing to increase contact with the air.

Range (Cooling Range) – This is the overall change in water temperature as it passes through
the packing I.e. the reduction in water temperature between the top and the bottom of the
packing.

Range = Twin – Twout °C

Cooling Load - The rate at which heat is removed from the water. This is expressed in kW
(Btu/h or kCal/h in alternative units). At steady state this equates to the power supplied to the
heater in the sump tank ignoring minor effects such as radiation to the tower, heat input from
water pump etc.

Cooling Load = Pwr kW (Calculated from Heater voltage and PID controller output in the
software)

83
 Approach – This is the difference between the water temperature leaving the base of the
packing and the wet-bulb air temperature entering the base of the packing Sometimes referred
to as ‘Approach to wet-bulb’. This is an important parameter that is used to assess the
performance of a cooling tower. The wet-bulb air temperature can be obtained from the
measured air temperature (dry-bulb) and the measured Relative Humidity of the air using an
appropriate Psychrometric App or the Relative Humidity table below.

Approach = Twout – Tairin (wet) °C

Ideal Range – This is the theoretical maximum range that could be achieved with the given
conditions.

Ideal Range = Twin – Tairin (wet) °C

Effectiveness – This is the ratio of the Range to the Ideal Range expressed as a percentage,
higher values indicating the cooling tower is more effective.

Effectiveness = 100 * Range / Ideal Range

= 100 * (Twin - Twout) / (Twin – Tairin(wet)) °C

Evaporation Loss – This is the quantity of water evaporated from the tower in creating the cooling duty.
Under steady state conditions the evaporation loss will equal the loss of water from the sump tank,
indicated via level sensor Lw.

The cross sectional area of the tank is:

Plan dimensions of tank 0.285 m by 0.22 m

Plan area of tank = 0.285 * 0.22 = 0.0627 m2

Liquid / Gas Ratio (L/G) – This is the ratio between the water mass flow rate (L) and the air mass flow
rate (G).
84
 Thermodynamic rules dictate that the heat loss from the water must equal the heat gained by
the air. Therefore the following will apply:

L* - a * (h2 – h1 )

Where h1 is the enthalpy of the air entering the tower and h2 is the enthalpy of the air leaving
the tower.

Make-up - The quantity of fresh water which must be supplied to the water circuit to make
good the losses due to evaporation and other causes. Under steady state conditions a level
sensor indicates the rate of fall in water level in the sump tank indicating how much make up
would be required if the tower was operated continuously at the particular operating conditions.

Drift or Carry Over - Droplets of water which are entrained in the air stream leaving the top of
the tower.

Drain Down - Water deliberately removed from the water system in a full sized system to prevent the
excessive concentration of dissolved solids (due to evaporation) and sludge (due to impurities from
the atmosphere).

Basic Principles of the Evaporative Cooling Tower

Many applications such as air conditioning in buildings, manufacturing processes in industry

or power generation require heated water to be cooled to a lower temperature. To this end,
cooling towers are used to reduce the temperature of a stream of water by evaporating some of
the water into the atmosphere resulting in a significant reduction in the water temperature.
Water flows down the tower against air flowing upwards through the tower resulting in
evaporation of a small proportion of the water. The change in latent heat when the water
evaporates results in significant heat loss as the humidified air escapes atmosphere resulting in
cooling of the remaining water.

85
 Packing is usually installed inside the cooling tower to increase the surface area of the water in
contact with the air to optimise the evaporation process and therefore increase the rate of
cooling.

The use of evaporation to produce the cooling means that a cooling tower can reduce the temperature of
water much more energy efficiently than an air cooled heat exchanger or similar device that relies on the
temperature of the air only to reject heat.

S chematic diagram of a typical forced draft cooling

tower

86
 Evaporative cooling inside the packing

Assuming that the water is hotter than the air, it will be cooled by:

Radiation – Likely to be very small under normal conditions, and may be neglected.

Conduction and convection – Usually small but depends on the temperature difference, the
surface area, air velocity, etc.

Evaporation – This is by far the most significant effect. Cooling takes place as molecules of water diffuse
from the surface into the surrounding air. These molecules are then replaced by others from the liquid
(evaporation) and the energy required for this is taken from the remaining liquid resulting in cooling of
the water.

87
Evaporation from a wet surface

The rate of evaporation from a wet surface into the surrounding air is determined by the
difference between the vapour pressure at the liquid surface, i.e. the saturation pressure
corresponding with the surface temperature, and the vapour pressure in the surrounding air.
The latter is determined by the total pressure of the air and its absolute humidity.

In an enclosed space, evaporation can continue until the two vapour pressures are equal,

i.e. until the air is saturated and at the same temperature as the surface. However, if unsaturated
air is constantly circulated, the wet surface will reach an equilibrium temperature at which the
cooling effect due to the evaporation is equal to the heat transfer to the liquid by conduction
and convection from the air, which under these conditions will be at a higher temperature.

The equilibrium temperature reached by the surface under adiabatic conditions (i.e. in the
absence of external heat gains or losses), is the “wet-bulb temperature”, which is well known
in connection with hygrometry.

In a cooling tower of infinite size and with an adequate air flow, the water leaving will be at
the wet-bulb temperature of the incoming air. For this reason, the difference between the
temperature of the water leaving a cooling tower and the local wet-bulb temperature is an
indication of the effectiveness of the cooling tower. The ‘Approach‘ is one of the important
parameters in the testing, specification, design and selection of the cooling tower.

Theoretical analysis from first principles

The Merkel Equation, developed in 1925, is accepted as the appropriate method to analyse the
performance of a cooling tower from first principles. This analysis considers the sensible heat
transfer due to temperature changes in the air and water combined with the latent heat transfer
due to evaporation of the water by considering the changes in enthalpy in the process. However,
this analysis is complex and beyond the scope of this simple introduction to a Cooling Tower.

88
With water and air flowing countercurrent through the packing, the process can be represented on an
Enthalpy / Temperature diagram as follows:

Water entering the top of the packing at temperature Twin is surrounded by a boundary film of
air that is in intimate contact with the water and the air. This film is assumed to be saturated
with water vapour at the bulk water temperature. This is point A on the saturation curve. As
the water is cooled to Twout the film enthalpy follows the saturation curve to point B.

Air entering the base of the packing at wet-bulb temperature Tairin (wet) has an enthalpy
corresponding to point C’ on the saturation curve. The driving force is represented by the
vertical distance BC.

Heat removed for the water is added to the air so its enthalpy increases along the line CD and
terminates at a point D below point A. The slope of the straight line CD is equal to the ratio
L/G where L is the Liquid (water) mass flow rate and G is the Gas (air) mass flow rate.

Cooling Tower Performance

Conditions within a cooling tower packing are complex due to the changing air temperature,
humidity and water temperature as the two fluids pass through the tower- usually in a contra
flow fashion. There are five parameters that in combination dictate and define the performance
of a particular cooling tower:

89
 Temperature of the heated water entering the tower

Temperature of the cooled water leaving the tower

The Temperature and Relative Humidity (RH) of the air entering the tower
(particularly the corresponding wet-bulb temperature)

Flowrate of the air

Flowrate of the water

In addition the following design features are relevant to the performance of the tower:

The surface area and volume of the packing used

The height of the tower / packing

The type of packing used

Unless the Cooling Tower is operated in a room fitted with climate control it will not be
possible to vary the Temperature or the Relative Humidity of the ambient air entering the
Cooling Tower. However, the UOP6-MKII Basic Water Cooling Tower enables all of the other
factors to be varied so that an overall appreciation of cooling tower characteristics can be
obtained.

Use of a Psychrometric App

Although the results obtained from the UOP6-MKII Cooling Tower can be analysed by plotting
them on a Psychrometric chart, it is more convenient to use a Psychrometric App that can be
downloaded to a Smartphone or a suitable PC. These Apps are readily available and can be
used to determine the unknown Psychrometric parameters from the measured values. For
example, by entering the air temperature (dry-bulb) measured at the inlet (Tain ) or at the outlet
(Taout) and the corresponding Relative Humidity value RHin or RHout, the App will calculate
the following parameters:

90
 Wet-Bulb Temperature

Humidity Ratio

Dew Point

Specific Volume

Specific Enthalpy

Relative Humidity Table

If access to a Psychrometric chart or Psychrometric App is not available then the following
lookup table can be used to obtain an approximate value for the wet-Bulb air temperatures.

To use the table locate the measured air temperature (dry-bulb) on the left hand column, locate
the corresponding measured Relative Humidity within the array then read off the corresponding
wet-bulb depression along the top row.

91
Example:

Dry Bulb = 13°C

Relative Humidity =

51%

Difference between Wet and Dry bulb readings = 5°C (from chart)

Wet-Bulb Temperature = Dry-bulb temperature – Wet-Bulb Depression

Therefore:

Wet Bulb Temperature = 13°C - 5°C = 8°C

92
 Note: The Teaching Exercises include in this instruction manual assume the use of a
Psychrometric App or the Relative Humidity Table to obtain the performance data quickly. A
Psychrometric Chart can be used if it is preferred to use the traditional approach.

93
Exercise A - Observation of the processes occurring within a forced
draught cooling tower

Objective
The UOP6-MKII Basic Water Cooling Tower is a miniaturised forced draft cooling tower. The
objective of the exercise is to introduce the construction, the operation and the characteristics
of a typical forced draft cooling tower with film packing installed

Method
Water in the sump tank will be heated to a constant temperature before it is pumped to the top
of the tower and allowed to flow downwards in a thin film over the surface of the packing
inside the tower. Ambient air will be drawn in to the equipment by a centrifugal fan and blown
upwards through the packing contacting the film of water in the process. The resultant changes
in the water temperature, the air temperature, the Relative Humidity of the air and the water
volume will be monitored to demonstrate the principle of the cooling tower using evaporation
of the water to effect the cooling.

Equipment Required
UOP6-MKII Basic Water Cooling Tower fitted with the standard density packing (packing

A) PC with UOP6-MKII software installed

Optional Equipment
None

Theory
No mathematical analysis is required for this demonstration where the aim is for the operator
to observe and understand the basic processes occurring in the air and water streams of the
cooling tower. However, two important calculated variables are used in the analysis of the
cooling tower performance. These are:

Range (Cooling range) = Twin – Twout °C

Approach (Approach to wet-bulb) = Twout – Tain(wet) °C

94
 Load (Cooling load) = Power to the heater PWR under steady state conditions (calculated in
the software from heater voltage and controller output)

The Range and Approach are shown diagrammatically below for information:

95
 In later exercises the changes in these calculated variables will be used to monitor changes in
performance of the tower under different operating conditions.

Equipment Setup
Standard density packing fitted (Packing A with 27 mm spacing between flutes).

Fill the sump tank to maximum water level on the indicator using demineralised water.
Replace the cap at the filling point when the sump is full.

Ensure that the room is well ventilated to minimise any changes in the temperature and
especially the RH of the air entering the cooling tower.

Procedure
Ensure that the UOP6-MKII software is running on the PC. View the Process screen, check
that the software is communicating with the equipment (IFD:vCOM(x)m in bottom right corner
of screen) then click the Power on button to enable the hardware.

96
 Check that values displayed on the Process screen are sensible. E.g. temperatures are approximately
ambient.

Add a note in the software that Packing A is fitted.

Adjust the pump speed to give a water flowrate of 1.0 l/min. so that water is sprayed onto the
top of the packing.

Adjust the fan speed to give an air flow of 40 l/s.

Set the PID controller Mode to Auto, adjust the controller setpoint (SP) to 40°C water
temperature T1 (Twin ) then click Apply.

Allow the equipment to stabilise, indicated by a constant water temperature at T1.

Click the zero button alongside the water level indication Lw so that any change in water
level can be monitored from a fixed datum.

97
Results (Observations)
While the cooling tower becomes stabilised the following features should be observed:

Water System

i. The warm water enters the top of the tower and is sprayed onto the top of the packing.

ii. The packing has an easily wetted surface and the water spreads over this to expose a large
surface to the air stream. Examination of the packing will reveal that the structure is cross fluted
to provide a large surface area in a relatively small volume.

iii. The water, cooled within the packing, falls from the bottom of the packing into the basin where
its temperature is measured. It then drains back into the sump tank for recycling. In an industrial
system warm water from a process would be cooled in the tower before it is returned to the
process.

iv. Small droplets of water (resulting from splashing etc.) may become entrained in the air stream
and then lost from the system as the air exits the top of the tower. This loss does not contribute
to the cooling, but results in loss of water from the sump tank (indicated by level sensor Lw).
In a commercial system this must be made good by “make-up”.

To minimise this loss, a “droplet arrestor” or “eliminator” is fitted at the tower outlet.
This component causes droplets to coalesce, forming drops that are too large to be
entrained, and these large droplets fall back into the packing.

Air System

v. Under the action of the fan, air is forced upwards through the wetted packing. It will be seen
that the change of air temperature (the dry bulb temperature) is small but the change in Relative
Humidity (RH) is large and the air leaving is close to saturated I.e. the RH is close to 100%.
Note that the air may become fully saturated at the outlet if the RH of the ambient air entering
the tower is high. This increase in the moisture content of the air is due to the conversion of
water into water vapour and the “latent heat” change associated with this is responsible for most
of the cooling effect.

If the wet-bulb air temperature is determined from the measured air outlet temperature
and the RH readings (from Taout and RHout using a Psychrometric App or the look-up
table supplied) then it will be seen that at the air outlet there is little or no difference
98
 between the wet-bulb temperature and the dry bulb temperature confirming that air
leaving is fully saturated or very close to fully saturated.

Turn off the cooling load by switching off the PID controller or set the Power output to
zero so that the water heater is turned off and allow the tower to re-stabilise.

The water temperature will continue to fall and may fall below the measured incoming
air temperature (dry bulb) due to the continuing cooling effect in the tower. However,
in theory, the temperature of the water leaving the packing cannot be cooled below the
wet-bulb temperature of the air entering the packing. In practice the water temperature
will remain slightly above the wet-bulb air temperature because of

99
 residual heat, the small heat input from the circulating pump, thermal radiation to the
tower etc.

Determine the wet-bulb temperature Tain (wet) of the air entering the packing (from
Tain and RHin using a Psychrometric App or the look-up table supplied). Compare this
with the water temperature Twout and confirm that Twout remains slightly above
Tain (wet).

Results (Measurements / Calculations)

When the tower has fully stabilised obtain the following values from the measurements
recorded on the PC:

T1 Twin °C Temperature of water entering top of packing T2

Twout °C Temperature of water leaving bottom of packing

T3 Tain °C Temperature of air entering bottom of packing (Dry bulb)

T4 Taout °C Temperature of air leaving top of packing (Dry bulb) RH1

% RH of air entering bottom of packing

RH2 % RH of air leaving top of packing

PWR kWatts Cooling load (Power to heat the water)

Using a Psychrometric App or Psychrometric table as appropriate obtain the Wet-bulb

temperature of the air entering and leaving the tower from the measured dry bulb temperature
and the Relative Humidity.

Tairin (wet) °C

Tairout (wet) °C

Calculate the Cooling Range Twin – Twout °C

100
 Calculate the change in air temperature Ta in – Taout

°C

Calculate the Approach value Twout – Tain (wet) °C

Calculate the Effectiveness = 100 * Cooling Range / (Range + Approach) %

Comment on the calculated values in relation to the observations listed above.

Conclusions
The basic operation of a Forced Draught Cooling Tower should have been clearly
demonstrated.

The difference between value Twout – Tain (wet) is called the Approach (Approach to wet- bulb)
and is an important parameter in determining the performance of a cooling tower. An inefficient
tower will have a large Approach value compared with a more efficient tower. As the calculated
Approach value nears zero the tower is effectively producing the maximum amount of cooling
that is possible given the current configuration and operating conditions.

101
Exercise B - Effect of water inlet temperature on the performance of a
cooling tower

Objective
To show how changes in the water temperature entering the cooling tower affect the
performance of the tower and the corresponding values for Range, Approach and Cooling
Load.

Method
The cooling tower will be operated with the standard packing (Packing A) installed with
constant water flowrate and with constant air flow. The temperature of the water entering the
top of the packing will be varied by changing the setpoint on the PID controller and the
corresponding changes in performance will be observed and compared.

Equipment Required
UOP6-MKII Basic Water Cooling Tower fitted with the standard density packing (packing

A) PC with UOP6-MKII software installed

Optional Equipment
None

Theory
If the temperature of the water entering the cooling tower is increased then the difference
between the water and the air inlet wet-bulb temperature will also increase allowing more
evaporation to occur and therefore more cooling to occur.

The associated changes in the tower are complex and the effect of changes in Water Inlet Temperature
can best be shown by plotting appropriate graphs such as:

Range against Water inlet temperature Cooling

Load against Water inlet temperature

102
 Approach against Water inlet temperature

Effectiveness against Water inlet temperature

Approach against Cooling Load when the Water inlet temperature is changed

103
 The graph above shows a typical change in Approach against Cooling Load as the Inlet Water
Temperature is varied. Note that the actual values and the shape of the graph will vary with
changes in the other parameters such as Air Flow rate or Water Flow rate.

Equipment Set Up
Standard density packing fitted (Packing A with 27 mm spacing between flutes).

Fill the sump tank to maximum water level on the indicator using demineralised water.
Replace the cap at the filling point when the sump is full.

Ensure that the room is well ventilated to minimise any changes in the temperature and
especially the RH of the air entering the cooling tower.

Procedure
Ensure that the UOP6-MKII software is running on the PC. View the Process screen, check
that the software is communicating with the equipment (IFD:vCOM(x)m in bottom right corner
of screen) then click the Power on button to enable the hardware.

Check that values displayed on the Process screen are sensible. E.g. temperatures are approximately
ambient.
104
 Add a note in the software that packing A is fitted.

Adjust the pump speed to give a water flowrate of 1.0 l/min. so that water is sprayed into the
top of the tower.

Set the PID controller mode to Auto, adjust the controller setpoint (SP) T1 (Twin ) to be approximately
10°C above the ambient air temperature then click Apply.

Allow the equipment to stabilise, indicated by a constant temperature at T1 (Twin ).

Adjust the fan speed to give an air flow of 40 l/s.

Click the zero button alongside the water level indication Lw so that any change in water
level can be monitored.

Allow the system to stabilise then view the readings obtained for information.

105
 Click the Power On button in the software to momentarily stop the heater, the fan and the pump.
Refill the sump tank to the Max level, replace the cap on the filling tube then click the Power
On button.

Increase the setpoint in the PID controller by 5°C, allow the system to stabilise then view the
readings as before.

Repeat the procedure with the water temperature increasing in steps of 5°C until the maximum
of 45°C is reached.

When all runs are complete stop logging, switch off the PID controller, switch off the pump
but leave the fan running at 100% speed for as long as practicable to dry the tower unless an
additional exercise is to be carried out.

Results
For each run, with a different water inlet temperature, use a Psychrometric App or
Psychrometric table as appropriate obtain the wet-bulb temperature of the air entering and
leaving the tower from the measured dry-bulb temperature and the corresponding Relative
Humidity.

Tairin (wet) °C

Tairout (wet) °C

Calculate the Cooling Range Twin – Twout °C

Calculate the change in air temperature Tain – Taout

°C

Calculate the Approach value Twout – Tain (wet) °C

106
 Calculate the Effectiveness = 100 * Cooling Range / (Range + Approach) %

Comment on the calculated values in relation to the observations listed above.

Analyse the results and compare the performance for each water temperature as follows:

Water temperature in °C 30°C 35°C 40°C 45°C

Approach value °C

Range °C

Cooling Load kW

Effectiveness %

Plot the graphs listed in the above Theory to observe the changes in performance with
change in Inlet Water Temperature.

Conclusion
Comment on the variation in the above parameters when the Water Inlet Temperature is
varied.

107
Exercise C - Effect of air flow rate on the performance of a cooling tower

Objective
To show how changes in the air flow and therefore the air velocity upwards through the packing
inside the cooling tower affect the performance of the tower and the corresponding values for
Range, Approach and Cooling Load.

Method
The cooling tower will be operated with the standard packing (Packing A) installed with
constant water flowrate and with constant water inlet temperature. The flow of air through the
packing will be varied by changing the speed of the centrifugal fan and the corresponding
changes in performance will be observed and compared.

Equipment Required
UOP6-MKII Basic Water Cooling Tower fitted with the standard density packing (packing

A). PC with UOP6-MKII software installed.

Optional Equipment
None

Theory
If the flow of air through the packing is increased then the water will evaporate more quickly
resulting in more cooling and corresponding changes in the Range, Approach, Cooling Load
etc.

The changes in the tower are complex and the effect of change in air flow can be shown
graphically by plotting appropriate graphs such as:

Range against Air flow rate

Cooling Load against Air flow rate

Approach against Air flow rate

Effectiveness against Air flow rate

108
 Approach against Cooling Load when the Air flow rate is changed

109
 The graph above graph shows a typical relationship between Approach value and Air flow rate.
Note that the Approach values and the shape of the graph will vary with changes in the other
parameters such as Water Inlet Temperature and Flow rate.

Equipment Set Up
Standard density packing fitted (Packing A with 27 mm spacing between flutes).

Fill the sump tank to maximum water level on the indicator using demineralised water.
Replace the cap at the filling point when the sump is full.

Ensure that the room is well ventilated to minimise any changes in the temperature and
especially the RH of the air entering the cooling tower.

Procedure
Ensure that the UOP6-MKII software is running on the PC. View the Process screen, check
that the software is communicating with the equipment (IFD:vCOM(x)m in bottom right corner
of screen) then click the Power on button to enable the hardware.

110
 Check that values displayed on the Process screen are sensible. E.g. temperatures are approximately
ambient.

Add a note in the software that packing A is fitted.

Adjust the pump speed to give a water flowrate of 1.0 l/min. so that water is sprayed into the
top of the tower.

Set the PID controller mode to Auto, adjust the controller setpoint (SP) to 40°C then click
Apply.

Allow the equipment to stabilise, indicated by a constant temperature at T1 (Twin ).

Adjust the fan speed to give an air flow of 15 l/sec.

111
 Click the zero button alongside the water level indication Lw so that any change in water level
can be monitored.

Allow the system to stabilise then view the readings obtained for information.

Click the Power On button in the software to stop the heater, the fan and the pump, Refill the
sump tank to the Max level, replace the cap on the filling tube then click the Power On button.

Increase the air flow to 30 l/sec, allow the system to stabilise then view the readings as before.

Repeat the procedure with the air flow at 45 then 60 l/sec.

When all runs are complete stop logging, switch off the PID controller, switch off the pump
but leave the fan running at 100% speed for as long as practicable to dry the tower unless an
additional exercise is to be carried out.

Results
For each run, with a different air flow, use a Psychrometric App or Psychrometric table as
appropriate obtain the wet-bulb temperature of the air entering and leaving the tower from the
measured dry-bulb temperature and the corresponding Relative Humidity.

Tairin (wet) °C

Tairout (wet) °C

Calculate the Cooling Range Twin – Twout °C

112
 Calculate the change in air temperature Tain – Taout

°C

Calculate the Approach value Twout – Tain (wet) °C

Calculate the Effectiveness = 100 * Cooling Range / (Range + Approach) %

Comment on the calculated values in relation to the observations listed above.

Analyse the results and compare the performance for each water temperature as follows:

Air flow l/sec 15 30 45 60

Approach value °C

Range °C

Cooling Load kW

Effectiveness %

Plot the graphs listed in the above Theory to observe the changes in performance with
change in Air flow rate

Conclusion
Comment on the variation in the above parameters when the Air flow rate is varied.

113
Exercise D - Effect of water flow rate on the performance of a cooling
tower

Objective
To show how changes in the water flowrate downwards through the packing inside the cooling
tower affect the performance of the tower and the corresponding values for Range, Approach
and Cooling Load.

Method
The cooling tower will be operated with the standard packing (Packing A) installed with
constant air flow and with constant water inlet temperature. The flow of water through the
packing will be varied by changing the speed of the centrifugal pump and the corresponding
changes in performance will be observed and compared.

Equipment Required
UOP6-MKII Basic Water Cooling Tower fitted with the standard density packing (packing

A). PC with UOP6-MKII software installed.

Optional Equipment
None

Theory
If the flow of water through the packing is increased then there will be corresponding
changes in the Water outlet temperature, Range, Approach, Cooling Load etc.

The changes in the tower are complex and the effect of change in water flowrate can be
shown graphically by plotting appropriate graphs such as:

Range against Water flow rate

Cooling Load against Water flow rate

114
 Approach against Water flow rate

Effectiveness against Water flow rate

Approach against Cooling Load when the Water flow rate is changed

Equipment Set Up
Standard density packing fitted (Packing A with 27 mm spacing between flutes).
Fill the sump tank to maximum water level on the indicator using demineralised water.
Replace the cap at the filling point when the sump is full.

Ensure that the room is well ventilated to minimise any changes in the temperature and
especially the RH of the air entering the cooling tower.

Procedure
Ensure that the UOP6-MKII software is running on the PC. View the Process screen, check
that the software is communicating with the equipment (IFD:vCOM(x)m in bottom right corner
of screen) then click the Power on button to enable the hardware.

115
 Check that values displayed on the Process screen are sensible. E.g. temperatures are
approximately ambient.

Add a note in the software that packing A is fitted.

Adjust the pump speed to give a water flowrate of 1.0 l/min. so that water is sprayed into the
top of the tower.

Set the PID controller mode to Auto, adjust the controller setpoint (SP) to 40°C then click
Apply.

Allow the equipment to stabilise, indicated by a constant temperature at T1 (Twin ).

Adjust the fan speed to give an air flow of 40 l/sec.

Click the zero button alongside the water level indication Lw so that any change in water level
can be monitored.

Allow the system to stabilise then view the readings obtained for information.

Click the Power On button in the software to stop the heater, the fan and the pump, Refill the
sump tank to the Max level, replace the cap on the filling tube then click the Power On button.

Increase the water flowrate to 1.5 l/min, allow the system to stabilise then view the readings.

Repeat the procedure with the water flowrate at 2.0 then 2.5 l/min.

When all runs are complete stop logging, switch off the PID controller, switch off the pump
but leave the fan running at 100% speed for as long as practicable to dry the tower unless an
additional exercise is to be carried out.

116
Results
For each run, with a different water flowrate, use a Psychrometric App or Psychrometric table
as appropriate obtain the wet-bulb temperature of the air entering and leaving the tower from
the measured dry-bulb temperature and the corresponding Relative Humidity.

Tairin (wet) °C

Tairout (wet) °C

Calculate the Cooling Range Twin – Twout °C

Calculate the change in air temperature Ta in – Taout

°C

Calculate the Approach value Twout – Tain (wet) °C

Calculate the Effectiveness = 100 * Cooling Range / (Range + Approach) %

Comment on the calculated values in relation to the observations listed above.

117
 Analyse the results and compare the performance for each water temperature as follows:

Water flowrate l/min 1.0 1.5 2.0 2.5

Approach value °C

Range °C

Cooling Load kW

Effectiveness %

Plot the graphs listed in the above Theory to observe the changes in performance with
change in Water flow rate.

Conclusion
Comment on the variation in the above parameters when the Water Flowrate is varied.

118
Exercise E - Effect of packing density on the performance of a cooling
tower

Objective
To show how changes in the density / surface area of the packing inside a cooling tower affect
the performance of the tower and the corresponding values for Range, Approach and Cooling
Load.

Method
The cooling tower will be operated initially with no packing installed (a spray tower only) then
with the two different sizes of packing fitted with all other parameters remaining constant. The
corresponding changes in performance will be observed and compared.

Equipment Required
UOP6-MKII Basic Water Cooling Tower fitted with the following packing:

No packing

Packing A with 27 mm spacing between flutes (125 m2 /m3 )

Packing B with 19 mm spacing between flutes (70 m2 /m3 )

PC with UOP6-MKII software installed

Optional Equipment
None

Theory
If the density of the packing is increased (I.e. the surface area to volume ratio is increased) the
film of water exposed to the air will also increase resulting in better and longer contact between
the air and the water. This will produce more evaporation and therefore increase the cooling of
the water. However, as pointed out in exercise A, a limit will be reached when the Approach
value nears zero.

119
 Note: The design of the packing and the water loading (the amount of water held in the packing
at a given flowrate) may limit the performance of the tower if the packing is not wet over the
whole of its surface area. A dense packing may not therefore perform any better than a packing
with smaller surface area unless the conditions are optimised.

Typically, the Approach value will vary with the packing density as shown below:

120
Equipment Set Up
Remove any packing fitted inside the tower then refit the front panel (The tower will be
initially operated as a spray tower).

Fill the sump tank to maximum water level on the indicator using demineralised water.
Replace the cap at the filling point when the sump is full.

Ensure that the room is well ventilated to minimise any changes in the temperature and
especially the RH of the air entering the cooling tower.

Procedure
Ensure that the UOP6-MKII software is running on the PC. View the Process screen, check
that the software is communicating with the equipment (IFD:vCOM(x)m in bottom right corner
of screen) then click the Power on button to enable the hardware.

Check that values displayed on the Process screen are sensible. E.g. temperatures are approximately
ambient.

121
 Add a note in the software that no packing is fitted (Spray tower).

Adjust the pump speed to give a water flowrate of 1.0 l/min. so that water is sprayed into the
top of the tower.

Set the PID controller mode to Auto, adjust the controller setpoint (SP) to 40°C water
temperature then click Apply.

Allow the equipment to stabilise, indicated by a constant temperature at T1 (Twin ).

Adjust the fan speed to give an air flow of 40 l/s.

Click the zero button alongside the water level indication Lw so that any change in water
level can be monitored.

Allow the system to stabilise then view the readings obtained for information.

122
 Click the Power On button in the software to stop the heater, the fan and the pump. Install
packing A (27 mm between flutes) inside the tower by removing the front panel. Refill the
sump tank to the Max level, replace the cap on the filling tube then click the Power On button
and repeat the above procedure. Add a note in the software that Packing A is fitted.

Repeat the procedure with Packing B installed. At the start of the run add note that Packing B
is fitted.

When all runs are complete stop logging, switch off the PID controller, switch off the pump
but leave the fan running at 100% speed for as long as practicable to dry the tower unless an
additional exercise is to be carried out.

Results
For each run, with different packing installed, use a Psychrometric App or Psychrometric table
as appropriate obtain the wet-bulb temperature of the air entering and leaving the tower from
the measured dry-bulb temperature and the corresponding Relative Humidity.

Tairin (wet)

°C

Tairout (wet)

°C

Calculate the Cooling Range Twin – Twout °C

Calculate the change in air temperature Tain – Taout

°C

Calculate the Approach value Twout - Tain(wet) °C

Calculate the Effectiveness = 100 * Cooling Range / (Range + Approach) %

Comment on the calculated values in relation to the observations listed above.

123
 Analyse the results and compare the performance for each packing as follows:

Packing Density m-1 Spray 70 125 150

Approach value °C

Range °C

Cooling Load W

Effectiveness %

Draw a graph of Approach v Packing Density to compare the performances.

Conclusion
Comment on the variation in the above parameters when the Density / Surface area of the
packing is varied. Comment on the performance when operated as a spray tower.

124
Exercise F - Effect of packing height on the performance of a cooling
tower

Objective
To show how the height of the packing inside a cooling tower affects the performance of the
tower and the corresponding values Cooling Load, Cooling Range and Approach.

Method
By operating the cooling tower with 1/3 height packing, 2/3 height packing and full height
packing installed the changes in performance can be observed and compared.

Equipment Required
UOP6-MKII Basic Water Cooling Tower fitted with the following

packing: Packing C1/3 height

Packing D 2/3 height

Packing AFull height

PC with UOP6-MKII software installed.

Optional Equipment
None

Theory
If the height of the packing is increased then the surface area is increased and the film of water
exposed to the air also increases resulting in better and longer contact between the air and the
water. This produces more evaporation and therefore increased cooling of the water.

Equipment Set Up
Install the 1/3 height section of packing (packing C) then refit the front panel.

125
 Install the spray nozzles directly above the packing by interchanging the blanking plate and
the nozzle assembly.

Fill the sump tank to maximum water level on the indicator using demineralised water.
Replace the cap at the filling point when the sump is full.

Ensure that the room is well ventilated to minimise any changes in the temperature and
especially the RH of the air entering the cooling tower.

Procedure
Ensure that the UOP6-MKII software is running on the PC. View the Process screen, check
that the software is communicating with the equipment (IFD:vCOM(x)m in bottom right corner
of screen) then click the Power on button to enable the hardware.

Check that values displayed on the Process screen are sensible. E.g. temperatures are approximately
ambient.

Add a note in the software that 1/3 height packing is fitted.

Adjust the pump speed to give a water flowrate of 1.0 l/min. so that water is sprayed onto the top
of the packing.

126
 Set the PID controller mode to Auto, adjust the controller setpoint (SP) to 40°C water
temperature T1 (Twin ) then click Apply.

Allow the equipment to stabilise, indicated by a constant temperature at T1 (Twin).

Adjust the fan speed to give an air flow of 40 l/s.

Click the zero button alongside the water level indication Lw so that any change in water level
can be monitored.

Allow the system to stabilise then view the readings obtained for information.

Click the Power On button in the software to stop the heater, the fan and pump. Remove the
1/3 height packing (packing C). Install the spray nozzle assembly at 2/3 height then install the
2/3 height packing (packing D). Refill the sump tank to the Max level, replace the cap on the
filling tube then click the Power On button and repeat the above procedure. Add note that 2/3
height packing is fitted.

Repeat the procedure with both sections of packing installed (packing C above packing D with
the spray nozzle assembly at the top of the tower).

Add a note in the software that full height packing is fitted

When all runs are complete stop logging, switch off the PID controller, switch off the pump
but leave the fan running at 100% speed for as long as practicable to dry the tower unless an
additional exercise is to be carried out.

127
Results
For each run with different packing installed use a Psychrometric App or Psychrometric table
as appropriate obtain the wet-bulb temperature of the air entering and leaving the tower from
the measured dry bulb temperature and the corresponding Relative Humidity.

Tairin (wet) °C

Tairout (wet) °C

Calculate the Cooling Range Twin – Twout °C

Calculate the change in air temperature Ta in – Taout

°C

Calculate the Approach value Twout – Tain (wet) °C

Calculate the Effectiveness = 100 * Cooling Range / (Range + Approach) %

Comment on the calculated values in relation to the observations listed above.

128
 Analyse the results and compare the performance for each packing as follows:

Packing Height 1/3 Height 2/3 Height Full Height

Approach value °C

Cooling Range °C

Cooling Load W

Effectiveness %

Draw a graph of Approach v Packing Height to compare the performances.

Conclusion
Comment on the variation in the above parameters when the Height of the packing is varied.

129
Exercise G - Performing a mass balance and a heat balance across
the tower

Objective
To perform a mass balance and a heat balance on the system.

Method
To compare the mass of water lost from the sump tank with the mass of water lost through evaporation.

To compare the heat gained by the air exiting the tower with the heat input to the system via
the water heater.

Equipment Required
None

Previous results obtained using UOP6-MKII will be used to perform the exercise.

Optional Equipment
None

130
Theory

UOP6-MKII S ystem for analysis

Mass Balance
The mass of water lost from the sump tank in a given time t (secs) can be determined from
the change in water level using the readings from the level sensor Lw (mm).

131
 The corresponding volume of water can be calculated using the cross sectional area of the sump
tank:

Plan dimensions of tank 0.285 m by 0.22 m

Plan area of tank = 0.285 * 0.22 = 0.0627 m2

Therefore volume of water lost in time t = Lw * 0.0627 *1000 (m3 )

Rate of water loss by volume = (Lw * 0.0627 *1000) / t (m3 /sec)

Rate of water loss by mass (Make- water * Lw * 0.0627 *1000) / t (kg/s)

The mass of water gained by the air can be determined from the change in Specific Humidity
(Humidity Ratio) of the air:

Considering a fixed parcel of air, the Specific Humidity SH is the ratio of the mass of water
vapour (mv ) in the parcel to the total mass of air (ma + mv ) where ma is the mass of dry air
present. In practice the Specific Humidity is approximately equal to the ratio of the mass of
water vapour (mv ) in the parcel to the mass of dry air (md).

Therefore by using a Psychrometric App or Psychrometric chart to determine the Specific

Humidity the change in the mass of water vapour between the inlet and outlet of the tower can
be determined.

Mass flow of air ma at inlet and outlet can be calculated from = Q a a

From the measurements of Dry bulb Temperature and Relative Humidity at inlet and outlet the
increase in the mass of water vapour at the outlet can be calculated:

Increase in mass of water vapour = mv (Outlet) - mv (Inlet) =

= (ma * SH) at Outlet - (ma * SH) at Inlet

132
 In practice a small amount of water may be lost from the system via the orifice at the top of the
tower in the form of small droplets. For this reason the loss of water from the sump tank will
usually be larger than the calculated loss due to the increase in humidity of the air.

Heat Balance
Heat input to the system consists of electrical power supplied to the water heater (PWR) and
work done by the water pump (P). However, the small size of the DC motor driving the water
pump on UOP6-MKII means that heat input to the water via the pump is negligible and can be
ignored. In a larger system heat input via the pump might be significant and should be included.

In the system low humidity air enters at the base of the tower and high humidity air leaves at
the top resulting in a change in enthalpy.

The Liquid to Gas ratio L/G of a cooling tower is the ratio between the water and the air mass
flow rates.

Thermodynamics dictate that the heat removed from the water must be equal to the heat
absorbed by the surrounding air.

Therefore L * Cpwater * (Twin –Twout ) = G * Cpair * (hout – hin )

133
 Where L is the Mass flow of Liquid (Water) kg / sec

G is the mass flow rate of Gas (Air) kg / sec

Cpwater is the Specific heat of water kJ / kg / k

Cpair is the Specific heat of air kJ / kg / k

Twin (T1) is the Inlet Water Temperature (top of packing) °C

Twout (T2) is the Outlet Water Temperature (bottom of packing) °C

hout is the Enthalpy of the air at the outlet (top of packing) kJ/kg

hin is the Enthalpy of the air at the entry (bottom of packing) kJ/kg

Analysis of the results requires mass flowrates rather than volume flowrates that are
measured using the PC. To convert to mass flowrates:

L = Qw * water

G = Qa air

In practice a small amount of heat will be transferred from the tower, sump tank etc. to the
surroundings.

For this reason power supplied to the heater PWR may be slightly larger than the heat
transferred in the system.

Conclusion
Comment on any mass balances and heat balances carried out and account for any variation.

134
Project 1 - Investigation of locally designed and manufactured
packing

The design of the cooling tower with a removable front panel allows alternative packing
supplied by or constructed by the user to be evaluated.

Removal of Packing
Remove the thumb nuts that secure the front panel to the tower.

Carefully remove the front panel then remove the current packing, if fitted.

Install the required alternative packing ensuring that it is supported by the side lugs at the
base of the tower.

Replace the front panel and tighten the thumb nuts.

If the packing is significantly shorter than the original packing supplied then the spray assembly
can be reinstalled in one of the lower apertures by removing the thumb nuts securing the
appropriate blanking plate then installing the spray assembly in its place. The blanking plate
must be fitted in the original aperture occupied by the spray assembly to ensure that all air
leaving the tower passes through the orifice plate for measurement.

Design of alternative Packing

An ideal packing for a cooling tower will:

a. Expose a large and uniform water surface to the air stream,

b. Offer a small and uniform resistance to the passage of air,

c. Be inexpensive,

d. Be robust, easily formed and easily handled

135
 e. Be durable under the prevailing conditions*

f. Not be combustible.

*e.g. it must withstand conditions ranging from dry and well ventilated during shutdown, to
continuous soaking in warm water which is possibly contaminated with airborne pollution,
biological growth and excessive dissolved solids.

1. When designing and installing locally manufactured packing, the following points should be
considered:

a. The fan installed limits the resistance of the packing to about 10mm H2 O at a normal air
velocity through the tower of 2 ms-1 .

b. “Splash” packing offers a smaller resistance than “Film” packing, but the formation of
small airborne droplets of water may be troublesome.

c. If a loose filling is used it must be supported on a grid (e.g. a wire mesh screen) at the
lower end of the tower.

136
 d. Packing materials should not break up or decompose during use (the pump will withstand
a small amount of suspended matter, but the filter and water flow meter are likely to become
blocked).

e. The water must be uniformly applied to the top layer of the packing.

137
Project 2 - Demonstration of cooling a process using a Cooling Tower

Many industrial and commercial refrigeration and other plants reject heat to the atmosphere via
a cooling tower.

The combination of a cooling tower and refrigeration plant condenser (or cooling tower and
any other process requiring cooling water) and its characteristics can be demonstrated as shown
in the diagram below.

All connections should be made with 10mm (3/8”) bore plastic tubing and the length of these
tubes should be kept to the minimum.

The pump selected must be capable of producing a head of 1.5m + the resistance in the cooling
water circuit, at a maximum flow rate of 50 cm3 s-1 .

The following restrictions apply:

Maximum cooling load 2 kW

Maximum water temperature (at tower inlet) 50ºC

Maximum wet-bulb temperature 23ºC

Maximum water flow rate 2.5 l/min

Minimum water flow rate 1 l/min

The water heater in the Basic Water Cooling Tower must be switched off.

The water circuit should, if possible, be filled with demineralised or distilled water.

138
 It will be necessary to top up the sump tank at regular intervals if it is required to operate the
setup for a prolonged demonstration.

Any of the previous exercises can be performed while the cooling tower is connected to the
external process. However, the heater in the sump tank will not be used during this
demonstration so measurement of heater power using the software will not be relevant. If the
external system has independent instrumentation then this can be used to confirm the heat
transferred from the process to atmosphere using the cooling tower.

Temperature sensor T1 (Twin ) will indicate the temperature of the water leaving the external
process and entering the cooling tower.

Temperature sensor T2 (Twout ) will indicate the temperature of the water leaving the cooling
tower and returning to the external process.

139
 Connections between Armfield Basic Water Cooling Tower and an external process requiring cooled water

140
Project 3 - Effect of inlet air temperature or inlet RH on tower
performance

If a climate controlled room is available then an exercise or exercises can be carried out to
investigate the effect of a change in air inlet temperature (dry bulb) and / or a change in
the Relative Humidity of the incoming air (change in wet-bulb air temperature) on the
performance of the tower.

If results are obtained using the standard packing A together the following settings used
in the previous exercises then the results obtained can be directly compared with previous
results.

Inlet water temperature

40°
C Water Flowrate 1.0
l/min

Air flow 40 l/se

141
 Experiment # 7
Fixed and Fluidised Packed bed

Figure 1: CEL-MKII Fixed and Fluidised Bed Apparatus

142
Objectives
- The study of the fluid- mechanical behavior of fixed and fluidized packed beds, focusing on the

incipient fluidization velocity and the dependence of bed expansion on the superficial velocity.

Safety Precautions
- Avoid contact between water and electricity.

- Wear your PPE’s

- Don’t run the pump if the water level below the minimum.

- Check the level of the tank to add makeup water every 10-15 minutes

- Use demineralized water in this experiment.

INTRODUCTION

Packed and fluidized beds play a major role in many chemical engineering processes. Packed-
bed situations include such diverse processes as filtration, wastewater treatment, and the flow of crude oil
in a petroleum reservoir. In these cases, the interest centers on the pressure drop through the bed as a
function the volumetric flow rate or superficial velocity.

If the particles in the bed are loose and there is sufficient volume in the device containing the
particles, the particles may fluidize at high flow rates. Fluidized beds are used extensively in the chemical
process industries, particularly for the cracking of high-molecular-weight petroleum fractions. Such beds
inherently possess excellent heat transfer and mixing characteristics. In the study of the fluid- mechanical
behavior of these beds, the focus here is on the incipient fluidization velocity and the dependence of bed
expansion on the superficial velocity.

THEORY

The theory for this experiment is covered in Chapter 7 of McCabe, Smith, and Harriott
(M,S&H). The following material is a condensation of that chapter as it relates to the experiment at hand.
As an aid to you, some specific equations in M,S,&H are referred to. There are three areas of interest
to us: (1) Relationship between the pressure drop and the flow rate; (2) Minimum fluidization velocity,
and; (3) Behavior of the expanded bed.

(1) Relationship between pressure drop and flow rate

The flow of a fluid, either liquid or gas, through a static packed bed can be described in a
143
quantitative manner by defining a bed friction factor, fp , and a particle Reynolds number, NRe,p , as
follows:

Note that this equation cannot be derived directly by extrapolating the case of flow through a circular
conduit since friction factor defined in both cases is different (see McCabe and Smith 4th edition, pg.
137)

Vo Dp 
N Re, p  (2)


where 

P = pressure drop across the bed

L = bed depth or length
gc = conversion constant (= unity if SI units are used)
Dp = particle diameter
 = fluid density
 = bed porosity or void fraction
Vo = superficial fluid velocity
 = fluid viscosity
s = sphericity

144
 The friction factor and the Reynolds number are dimensionless. Some typical sphericity factors are
given in McCabe, Smith and Harriott (p. 928, Table 28.1).

 
For laminar flow, where only viscous drag forces come into play, N Re, p 20 , experimental
data may be correlated by means of the Kozeny-Carman equation:

Note: According to Yates ("Fundamentals of Fluidized-bed Chemical Processes," by J. G. Yates,

Published by Butterworths, 1983, p. 7-8) the factor of 150 was originally given by Carman as 180 for
the case of laminar flow. Ergun later suggested a better value was 150 when the particles are greater
than about 150 𝛍m in diameter.


While both equations (3) and (4) have a sound theoretical basis, Ergun empirically found that
the friction factor could be described for all values of the Reynolds number by simply adding the right-
hand sides of equations (3) and (4). Thus:

(2) Minimum fluidization velocity

At a sufficiently high flow rate, the total drag force on the solid particles constituting the bed becomes equal
to the net gravitational force and the bed becomes fluidized. For this situation a force balance yields:

pA  LA 1   M  p  g / gc  Mp   

 g / gc p (6)
where
M = void fraction at the minimum fluidization velocity
A = cross-sectional area of the bed
p = particle density
g = gravitational constant

145
 M = total mass of packing

This is Eq. 7.48, 7.49 MS&H . The superficial fluid velocity at which the fluidization of the bed
commences is called the incipient or minimum fluidization velocity, V 0M . The incipient fluidization
velocity may be determined by combining equations (1), (3), and (6) with the following result [Eq.
(7.52) MS&H] for the case of small particles and consequent, NRe<1:



This equation is the basis for some empirical equations found in the literature. The terms can be
grouped as follows:

The first factor contains the sphericity of the particles and the bed porosity at the point of incipient
fluidization. Neither of these factors is usually known with a high degree of accuracy. If spheres are
assumed  s 1 and a reasonable value of voidage, say  M  0.4 , then the first factor is 0.00071. The
factor is quite sensitive to  M . For example, if  M  0.413, then the factor is 0.0008.

One investigator, [D. Geldhart, "Types of Fluidization," Powder Technology, 7 (1973), 285-
292; Geldhart and Abrahamsen, Powder Technology, 19 (1978), 133-136] simply determined the first
factor from his data and actually found 0.0008 to be the best value; that is, he reported the following
correlation:

146
Behavior of the expanded bed

The expansion of fluidized beds is discussed in the text on Pages 170-173. The treatment to be
used here is slightly different. For fluid velocities exceeding the incipient fluidization velocity, the bed
expands. The porosity, , of an expanded bed may be related to the superficial fluid velocity, V o , by
means of an empirical relation suggested by Richardson and Zaki (1,2):

where ut is the terminal velocity of a spherical particle in a fluidizing medium (3). The exponent, n,
depends on the flow conditions -- that is, on the Reynolds number. Thus:

N Re, p  0.2 n  4.65 (11)

0.2  N Re, p 1.0 n  4.35N Re,

0 .03
p
(12)

1 N Re, p  500 n 4.45 NRe,0.1p (13)

N Re, p  500 n 2.39 (14)

147
Because the terminal velocity, ut , is a constant for a given particle, it can be seen that Equation
(10) above is essentially the same as the empirical equation in the text; namely Eq. (7.59) MS&H.

The void fraction of the expanded bed, , is related to that at incipient fluidization by the
following equation:

For this square both sides of Eq. (15) and utilize the definition of NRe,p (Eq. (2)) to obtain:

All parameters on the right are known. This suggests that a plot of C D N 2Re, p versus N Re, p can be
constructed and used to avoid the trial-and-error procedure.

The plot is prepared in the following way. Pick a series of point coordinates off the plot shown
above. Some examples for spheres are:

2
N Re, p CD CD N Re, p

.001 22,000 22
.01 2,200 22
.1 220 22

148
 1,000 0.48 480

Pick off a dozen similar pairs. Then plot CD N Re, p as the ordinate against corresponding N Re, p as the
2
abscissa. For each bed, calculate C D N Re, p from Eq. (16). From your plot read the corresponding

N Re, p . Then use Eq. (2) to calculate ut .

149
EQUIPMENT AND PROCEDURE

In this experiment the friction factor will be measured as a function of Reynolds number for the
flow of air through a bed of solid particles. Experimental results will be compared with theoretical
predictions for the appropriate flow regimes. A flow sheet of the experimental set-up is depicted
schematically in Figure 1 below. The equipment includes three transparent beds, air and water
flowmeters, manometers, a source of low pressure air, water basin, water pump and appropriate valves
and fittings.

Figure 2: Layout of the CEL-MKII

150
 Figure 3: Section through H2O (Water) Column on CEL-MKII

151
 Figure 4: Section through Air Columns on CEL-MKII

Granular material (glass beads)

The glass beads supplied with the equipment specifications are as follows:

H2O Column and Air Column 1:

Ballotini Grade 4502 (Catalogue no. 136-014) Range 0.50 to 0.75mm

(625 micron nominal).

Air Column 2:

Ballotini Grade 5216 (Catalogue no. 136-001) Range 0.20 to 0.30mm

(250 micron nominal).

Measure the bed height after tapping the bed gently until no further change is observed. Adjust
152
the valves to Control the flow of air through the system by manipulating the required valve.

Increase the flow rate of air in small steps noting the rotameter and manometer readings until the
bed is fluidized and the pressure drop does not change appreciably. Also, record the corresponding bed
height at each flow rate. Continue the measurements until the bed is appreciably fluidized and obtain at
least fifteen readings in the packed-bed region and ten readings in the fluidized-bed region.
Decrease the flow rate noting the flow rate and pressure drop values.

The region where fluidization just begins -- namely, at the "minimum fluidization velocity" -- is of
special interest. In Figure 2, it occurs at Point B. [This plot is based upon one in "Design for Fluidization,

Part 1," by J. F. Frantz, Chemical Engineering, September 17, 1962, pp. 161-178.] At this point, where
the pressure drop through the fixed bed becomes equal to the weight of the bed per unit area, a slight
rearrangement of particles occurs and the particles shift position so as to present maximum flow area to
the gas. Quoting from the article above, "This causes a slight decrease in pressure drop, and channeling
occurs. Only at a higher gas velocity does the entire bed become fully supported by the gas stream. Leva,
Shirai and Wen realized this phenomenon took place, and thus the defined minimum fluidization velocity
as a gas velocity 10% greater than the point at which, with increasing velocity, the pressure drop through
the fixed bed first equals the weight of the bed per unit area."

In view of this, repeat the run to check for reproducibility, making sure that you get sufficient
data in the somewhat ill-defined region between Points B and D.

The theory of this experiment is built around the assumption that at "steady state," the particles
are uniformly distributed in the bed. As you increase the flow rate of air, take some notes concerning
what the bed looks like at various stages. This may help to explain some discrepancies between measured
and theoretical values.

Repeat the measurements on the other bed by reconnecting the appropriate lines.

Repeat the experiment at least twice (preferably thrice) with each bed to ensure that you are
sufficiently sure about the quantity of the data.

153
 In a separate experiment, the porosity of a container of solid particles was measured using the
method of water displacement. This involves first weighting a measured volume of dry particles. Water
is then slowly added to the particles until the upper surface is wet. The weight of the water added can
then be used to calculate the porosity of the bed. This porosity corresponds to the value,  M , inEquation
(6). These values of bed porosity and particle spherocity are provided with the experimental system.

Calculations

1. For each bed, plot the measured pressure drop (in cm of H2O) versus the volumetric flow rate in
liters/min. Note that the manometer is at an angle of 19° and therefore, to get pressure drop, the
difference in manometer levels must be multiplied by sin(19°). There will likely be a "hysteresis
effect," in that the pressure drop curve for increasing flow rate will differ from that for decreasing
flow rate. Therefore, use different symbols for increasing and decreasing flow rates. Explain the
likely cause of this effect.

2. For each bed, calculate the friction factor and corresponding Reynolds number for each data
point using Equations (1) and (2). Then prepare a single plot of fp versus N Re,p which combines
the results for the two beds. Use a different symbol for each bed and show symbols only (no
lines). On this plot, also show the predicted values from Equations (3), (4), and (5). Show
these as solid or dashed lines, and do not show the points used for determining these plots.

3. From your plots in Part 1 above, determine the pressure drop at the point where fluidization
begins in cm H2O. Using Equation (6), calculate the predicted value of the pressure drop at this
point in cm H2O. Note that you have to know  M. Leva [Max Leva, "Chemical Engineering,
November, 1957, pp. 266-270] gives a correlation that can be used. Alternatively, you could
assume  M   as provided to you by the TA for the packed bed before fluidization
commences. Comment on your findings.

4. As noted earlier, the minimum fluidization velocity, V 0M , is of considerable interest. From your
results in Part 1, calculate experimental V0M in m/s and ft/s for each of your runs and beds.
Using the theoretical Equation (7), to also predict theoretical V0M in m/s and ft/s. Compare and
contrast the results.

Several empirical equations are available in literature based on experimental data. Three of these
will be used here for comparison with your experimental results.

(a) Leva et al.

Leva gives the following equation for the mass velocity at the point at which fluidization begins:

154
where:
Dp = particle diameter, inches
 = fluid density, lbm/ft3
s = particle density, lbm/fm3
 = fluid viscosity, centipoises
G mf V0M = mass velocity, lbm/ft2 , hr

The value of 688 was chosen by Leva as best based on 223 experimental points. Frantz noted
that the standard deviation was 33% and the average deviation was 22%. The equation is valid
for Reynolds numbers, Gmf Dp /, less than 5. Above 5, the value of Gmf must be multiplied by
the correction factor, Fg, given in the following plot (??).

155
 (b) Perry's Chemical Engineering Handbook, 6th Edition, p. 20-59.

Baeyens and Geldhart ["Fluidization and Its Applications," Proc. Int. Symp. Toulouse, 253
(1973)] gives "one of the better correlations:"

Where:
V 0M = minimum fluidization velocity, m/s
s = particle density, kg/m3
 = fluid density, kg/m3
g = 9.81 m/s2
DP = particle diameter, m
 = viscosity, kg/m,s

(c) Equation of Geldhart in "Powder Technology."

Using Equation (9).

For each bed, calculate V 0M from the equations of Leva, Perry's and Geldhart in m/s and ft/s.
Compare the results with your experimental values.

5. Finally investigate the behavior of your beds when they are expanded. At each data point in the
expanded regime, you can calculate  from Equation (7-58). For  M, assume that it has the
value given to you by the TA for the packed bed. Then tabulate corresponding values of V 0 on
the abscissa. Note that taking the logarithm of both sides of Equation (7) gives:
log V0  log ut n log  

6. Discuss your results critically.

156
 Exercise A – Determining the Voidage of granular material
Objective
a. To determine the Bed Voidage of the 625 microns / 0.625 mm glass beads
supplied with CEL-M KII

b. To determine the Bed Voidage of the 250 microns / 0.250 mm glass beads
supplied with CEL-M KII

Equipment Set-Up
CEL-MKII is not required to complete this exercise but dry samples of the
two sizes of glass beads supplied will be required.

Other essential equipment (Not supplied)

Weigh balance (typical range 1 Kg or 2.2 g)
Dry measuring cylinder (typical volume 0.5 litres)

Theory
To predict the performance of a fluidised bed in the later exercises it will be necessary
to know the Voidage of the granules used in the beds I.e. the ratio of the voids (spaces)
between the granules to the total volume.

The Voidage for glass beads is typically 0.4 but it is a useful exercise to determine the
actual value for the samples supplied. It will be necessary to determine the actual
Voidage of the materials used when carrying out Project 2.

The bed Voidage  can be determined using the following equation:

Where the Particle Density for the glass beads (Ballotini) supplied is 2500 kg/m3 .

Readings to be taken
Weigh the dry, empty measuring cylinder and record the weight or Tare the balance to read
0 Kg.

Fill the measuring cylinder with a dry sample of the larger granular material (0.625 mm
diameter glass beads) and record the volume from the scale on the measuring cylinder. The
actual volume chosen does not matter but the larger the sample the more accurate the result
will be, provided it is within the measuring range of the balance.

Measure the combined weight of the cylinder and granular material to determine the mass
of granules that corresponds with the volume recorded.

Repeat the procedure for a sample of the smaller granular material (0.250 mm diameter glass
beads)
157
 This technique can be used to determine the Voidage if using alternative materials in the
Project work exercises. The solid density of the material will be needed to calculate the
Voidage. If this is not known then it will be necessary to determine this value using a
Specific Gravity bottle (not supplied with CEL-MKII) or other technique.

Results
Calculate the Bed Voidage of the two samples using the above equation then record the
results for future reference.

Conclusions
The Voidage of the material used in the beds can be determined from measurements of the
Mass and Volume of the granules provided that the Particle Density i.e. the Solid Density
of the particle material is known.

158
 Exercise B - Flow through fixed and fluidised beds using water as the fluidising
medium
Objective
To investigate the characteristics associated with water flowing vertically
upwards through a bed of granular material as follows:
a. To determine the pressure drop (head loss) across the bed

b. To verify the Carman-Ko zeny equation

c. To observe the onset of fluidisation and differentiate between the

characteristics of a fixed bed and a fluidised bed

d. To compare the predicted onset of fluidisation with the measured pressure drop

Equipment Set-Up
CEL-MKII with the standard set-up (Left hand H2 O column filled to 300
mm height with coarse Ballotini i.e. glass beads with a nominal diameter of
625 microns / 0.625 mm).

27

159
Theory
To determine the pressure drop through a fixed bed we can show that the
Carman- Kozeny equation can be expressed in the form:

where

Dp = Size of granules (m) = 0.625 x 10 -

3 m L = Original height of bed (m) =

0.3 m

w= Viscosity of water (10-3 Nsm-2 ) (From Data sheet 1)

w= Kinematic viscosity of water (10 -6 m2 s-1 ) (From Data sheet 1)

w= Density of water (kgm-3 ) (From Data sheet 1)

 = Granule density (kgm-3 ) = 2500 kgm-3 (using glass beads)

 = Bed voidage (Use value from exercise A (Typically 0.4 for Ballotini)

Re = Average Reynolds' number based on Superficial velocity

(Dp .Vsm .w/w) which is dimensionless.

160
 If the flow rate Q is measured in litres/second, and Vsm is the average
superficial velocity in ms-1 , then

where

A = Bed cross-sectional area (Bed diameter = 0.05 m)

As the pressure drop (h) across the bed is measured in mm H2 O, then

where g = 9.81
Nm-2 Then our original equation
becomes:

The pressure drop at fluidisation can be predicted by using the equation:

The values of w, w and  w can be obtained from Data Sheet 1 or

alternative sources.

Readings to be taken
Ensure that the equipment is set up as described above.

Set the flow regulator in front of the column to minimum flow (fully
anticlockwise) then switch on the water pump via the switch on the console.

Adjust the water flow rate in increments of 0.05 l/min by slowly turning the
flow regulator clockwise and observing the flow reading on the display.
Continue increasing the flow until the bed is fully fluidised and the pressure
drop across the bed remains constant for several readings. At each setting
allow the conditions to stabilise then record the flowrate and the differential
pressure reading from the display. Also record the height of the bed, measured
using the scale on the column, and observe and record the state of bed i.e. any
movement of the granules.

161
Results
Measured Calculated Calculated
Measured Measured Bed Observed
Pressure Superficial Head Loss
Flow Rate Height Bed State
Drop Velcocity across bed
(l/min) (mm)
(mBar) (ms -1 ) (mBar)

For each set of measure me nts:

Calculate the Superficial Velocity

Calculated the predicted Head Loss across the fixed bed

Calculate the Predicted pressure drop at fluidisation

Draw the graph of measured pressure drop across the bed against water flow rate
from the experimental values obtained.

Draw the graph of predicted pressure drop across the bed against water flowrate and
compare this with the graph using experimental values

29

162
 Compare the predicted fluidisation point with the actual fluidisation point
obtained from the first graph

Give reasons for any discrepancies between the experimental and predicted results.

Conclusion
The head loss across a bed of granules will increase proportionally with increasing
flow of water until the drag on the granules caused by the water matches the weight of
the granules and the granules become fluidised.

From that point onwards, increasing flow of water will increase the height of the bed
but the head loss across the bed will remain almost constant (friction in the duct will
cause small increases in the losses but not the fluidised bed itself).

The flow of water through a bed of granules causes ‘Particulate Fluidisation’ whereby
the bed expands uniformly with no voids. The different characteristics of ‘Aggregative
Fluidisation’ will be demonstrated using air in exercise C.

163
Exercise C - Flow through fixed and fluidised beds using air as the fluidising medium
Objective
To investigate the characteristics associated with air flowing vertically
upwards through a bed of granular material as follows:
a. To determine the pressure drop (head loss) across the bed

b. To verify the Carman-Ko zeny equation

c. To observe the onset of fluidisation and differentiate between the

characteristics of a fixed bed and fluidised bed

d. To compare the predicted onset of fluidisation with the measured pressure drop

Equipment Set-Up
CEL-MKII with the standard set-up (Middle Air 1 column filled to 300 mm
height with coarse Ballotini i.e. glass beads with a nominal diameter of 625
microns / 0.625 mm).

164
Theory
To determine the pressure drop through a fixed bed we can show that:

where

Dp = Size of granules in (m) = 0.650

mm L = Original height of bed

(m) = 0.3 m

a = Viscosity of air (10-5 Nsm-2 ) (From Data sheet 2)

a = Kinematic viscosity of air (10-6 m2 s-1 ) (From Data sheet 2)

a = Density of air (kgm-3 ) (From Data sheet 2)

 = Granule density (kgm-3 ) = 2500 Kgm-3 (Glass beads)

 = Bed voidage Use value from exercise A (Typically 0.4 for Ballotini)

Re = Average Reynolds' number based on Superficial velocity

(Dp .Vsm . /) which is dimensionless.

If the flow rate Q is measured in litres/second, and Vsm is the average

superficial velocity in ms-1 , then

where A = Bed cross-sectional area (Bed diameter = 0.05 m)

As the pressure drop (h) across the bed is measured in mm H2 O, then

where g = 9.81 Nm-2

Then our original equation becomes

165
 which gives us

The pressure drop at fluidisation can be predicted by using the equation:

The values of a,  a and a can be obtained from Data Sheet 2 or alternative sources.

Readings to be taken
Close the flow regulator in front of air columns Air 1 and Air 2 (turn knob fully
anticlockwise).

Connect a compressed air supply to the inlet at the rear of the filter regulator.

Adjust the air flow rate in increments of 5 l/min by slowly turning the flow
regulator clockwise and observing the flow reading on the display. Continue
increasing the flow until the bed is fully fluidised and the pressure drop across
the bed remains constant for several readings. At each setting allow the
conditions to stabilise then record the flowrate and the differential pressure
reading from the display. Also record the height of the bed, measured using
the scale on the column, and observe and record the state of bed i.e. any
movement of the granules.

166
Results
Measured Calculated Calculated
Measured Measured Bed Observed
Pressure Superficial Head Loss
Flow Rate Height Bed State
Drop Velcocity across bed
(l/min) (mm)
(mBar) (ms -1 ) (mBar)

For each set of measure me nts:

Calculate the Superficial Velocity

Calculated the predicted Head Loss across the fixed bed

Calculate the Predicted pressure drop at fluidization

Draw the graph of measured pressure drop across the bed against air flow rate
from the experimental values obtained.

Draw the graph of predicted pressure drop across the bed against air flowrate
and compare this with the graph using experimental values

Compare the predicted fluidisation point with the actual fluidisation point
obtained from the first graph

Give reasons for any discrepancies between the experimental and predicted results.

167
Conclusion
The head loss across a bed of granules will increase proportionally with
increasing flow of air until the drag on the granules caused by the air matches
the weight of the granules and the granules become fluidised.

From that point onwards, increasing flow of air will increase the height of the
bed but the head loss across the bed will remain almost constant (friction in
the duct will cause small increases in the losses but not the fluidised bed itself).

The flow of air through a bed of granules causes ‘Aggregative Fluidisation’

whereby the bed expands erratically with large voids moving upwards through
the bed. This behaviour is quite different to ‘Particulate Fluidisation’
demonstrated using water in exercise A.

168
Exercise D – Effect of granule size using air as the fluidising medium

Objective
To investigate the difference between different sizes granular material on
fluidisation characteristics, using air as the fluidising medium.
a. To determine the pressure drop (head loss) across the beds with different particle
sizes

b. To observe the onset of fluidisation and differentiate between the

characteristics of a fixed bed and a fluidised bed for both particle sizes.

c. To compare the onset of fluidisation between the two particle sizes

Equipment Set-Up
CEL-MKII with the standard set-up (Right hand Air 2 column filled to 300
mm height with fine Ballotini i.e. glass beads with a nominal diameter of
250 microns / 0.250 mm)

169
Theory
The theory for this exercise is the same as Exercise C. Results from Exercise
C will be compared with the results from this exercise to show the effect of a
change in granule size.

Readings to be taken
As exercise C but adjust the air flow rate in steps of 0.5 l/m because the
smaller, lighter glass beads will fluidise at a much lower air velocity.

Results
As exercise C but using p D = Size of granules in (m) = 0.250 x 10 -3 m

Compare the graphs obtained with those from exercise C using larger

granules.

Conclusion
The size and weight of the particles will affect the head loss through the
fixed bed and the air velocity required to fluidise the particles.

170
Exercise E – Demonstration of Liquefaction of solids (Quicksand and similar
phenomena)
Objective
To demonstrate the phenomena of liquefaction of solids.

Equipment Set-Up
CEL-MKII with the standard set-up (H2 0 column filled to 300 mm height
with coarse Ballotini i.e. glass beads with a nominal diameter of 625
microns / 0.625 mm).

Other essential equipment

Rod supplied with CEL-MKII

Theory
As seen in previous exercises a solid bed of granules will become fluidised
when fluid flows upwards through it with sufficient velocity. At the onset of
fluidisation the bed of granules becomes liquefied reducing the ability of the
bed to support a solid object resting on the surface. When an object has sunk
into a liquefied bed it may become trapped when the upward flow of fluid
reduces and the bed becomes solid again.

171
Readings to be taken
Place the rod inside the H2 O column with the ball end resting on the surface of the bed.
The weight of the rod is supported by the compacted bed of granules.

Gradually increase the flow of water and observe that the rod sinks through the bed
of granules as the bed becomes fluidised. Gradually reduce the flow of water until the
flow stops then observe how the compacted bed of granules effectively trap the rod
requiring increased force to pull it through the bed.

Gradually increase the flow of water again and observe that the rod remains trapped
until the bed becomes fluidised again.

Repeat the exercise with the plain end of the rod resting on the bed. Observe that the
rod becomes trapped as before but the force required to remove it is less than before
because of the small cross section and parallel sides of the rod.

Note that in a real situation a large body sinking into a liquefied solid such as a sandy
beach would require significant force to remove it if the liquefaction ceases.

The exercise can be repeated using air to fluidise the bed of granules by removing the
172
 cap from the appropriate column by unscrewing the retaining screw then pulling the
cap upwards. The above exercise can then be repeated using air.

Note that when the cap is removed from an air column it is very easy to eject the
granules from the top of the column, creating a potential hazard. Extreme care must
be taken to prevent this by limiting the airflow. Ensure that the flow regulator is turned
fully anticlockwise before connecting the compressed air supply. With the cap
removed it will not be possible to measure the airflow but this is not necessary for this
simple demonstration.

Conclusion
A solid bed of granules will support a solid object resting on the surface even with
liquid flowing upwards through the bed, provided that the velocity of the fluid is not
sufficient to fluidise the bed.

When the upward velocity of the fluid is sufficient to fluidise the granules the object
on the surface will sink into the bed because the solid bed of granules has become
liquefied I.e. it behaves like a liquid. The object can be moved easily within the bed
while it is liquefied.

When the upward flow of fluid reduces and the bed of granules stops fluidising, the
object is surrounded by the solid bed and becomes trapped.

173
 Project Work 1
Objective
To investigate the characteristics associated with water flowing vertically
upwards through beds of different granular material

Equipment Set-Up
CEL-MKII with the left hand H2 O column filled to a height of 300 mm with
alternative granular material as required by the user.

It will be necessary to empty the standard filling from the water column and
refill it with the alternative material as follows:

Unscrew the two thumb screws that secure the water column to the base.

Carefully lift the column clear of the equipment then tip the existing filling
into a suitable container. If the material is damp from previous use then it
may be necessary to flush the column with water to remove all of the
material. Take care when handling the loose material because this could
create a hazard if spilt onto the floor or work surface.

Replace the column on the base and secure it using the two thumb screws.

Fill the column to a height of 300 mm with the required granular material
taking care not to spill any.

Other essential equipment

Granular material of different size, different shape or different density will be
required. This material is not supplied by Armfield.

To complete the second part of the project work exercise small solid objects
of different density will be required. Each object will require a lightweight
cord to be attached to allow the sample to be lowered into the fluidised bed
but retrieved using the cord. The objects should be close to density of water,
one slightly less dense and a few slightly denser than water. The correct
densities can be achieved using the same body that is slightly less dense than
water (E.g. Plastic such as Polyethylene that just floats in water) then drilling
a hole in the body and adding weight to achieve a body that just sinks in
water and a body that sinks rapidly in water. These solid objects are not
supplied by Armfield.

Theory
As Exercise A except that the characteristics of the material will differ when
calculating the theoretical behaviour.

Readings to be taken
Before filling the column use the weigh balance and measuring cylinder to
174
 determine the voidage of the required material as described in Exercise A.

Fill the water test column to a height of 300 mm with the required granular

material. Obtain readings as described in Exercise B but using the required

granular material. Repeat using alternative granular materials as required.

Results
As Exercise B.

Compare the results obtained with those using glass beads in Exercise B.

Conclusion
The head loss due to flow of water upwards through a bed of granular
material will depend on the size, shape and density of the granules.

The water velocity required to fluidise the granular material will depend on
the size, shape and density of the granules.

175
Project Work 2
Objective
To investigate the behaviour of solid bodies with different densities when
immersed in a fluidised bed.

Equipment Set-Up
CEL-MKII with the standard set-up (Left hand H2 O column filled to 300
mm height with coarse Ballotini i.e. glass beads with a nominal diameter of
625 microns / 0.625 mm).

Other essential equipment

Small solid objects of different density will be required. Each object will
require a lightweight cord to be attached to allow the sample to be lowered
into the fluidised bed but retrieved using the cord. The objects should be close
to density of water, one slightly less dense and a few progressively denser than
water. The correct densities can be achieved using the same body that is
slightly less dense than water (E.g.
Plastic such as Polyethylene that just floats in water) then drilling a hole in the
body and adding weight to achieve a body that just sinks in water and a body
that sinks rapidly in water. These solid objects are not supplied by Armfield.

Theory
As Exercise D except that objects with different densities will be lowered onto
the bed using the attached cord.

When the bed becomes fluidised the bodies will behave differently according
their specific gravities / densities.

176
 41
Armfield Instruction Manual

Readings to be taken
Set the flow regulator to minimum flow (fully anticlockwise) then switch on the water
pump via the switch on the console. Adjust the water flow rate in small increments
until the bed is fully fluidised. At each setting allow the conditions to stabilise then
observe the behaviour of the solid objects lowered into the column.

Results
Record the behaviour of the solid objects:

When the bed in fixed

When the bed becomes fluidised

When the flow is increased and the bed expands

Conclusion
Bodies less dense than water will float on the water surface and rise from the
surface of the bed as the column fills with water.

Bodies slightly denser than water will sink through the water and may remain

177
 at the surface of the bed when fluidised or sink into bed then float to the
surface of the bed when the upward flow of water increases. The actual
behaviour will depend on the density and shape of the object and the upward
velocity of the water.

Bodies significantly denser than water will sink through the bed when the bed
becomes fluidised.

REFERENCES

1. J.F. Richardson and W.N. Zaki, Trans. Inst. Chem. Engrs., 32, 35 (1954).
2. J.M. Coulson and J.F. Richardson, "Chemical Engineering," Vol. II, p. 510-527, Pergamon
Press, Oxford (1960).
3. R.B. Bird, W.E. Stewart, and E.N. Lightfoot, "Transport Phenomena," p. 190-194, John Wiley
and Sons, New York (1960).
4. S. Ergun, Chem. Eng. Prog., 48, 89 (1952).
5. W.L. McCabe and J.C. Smith, "Unit Operations of Chemical Engineering," 3rd Edition, p. 146-
150, 159-160, McGraw-Hill, New York (1976).
6. A.S. Foust, L.A. Wenzel, C.W. Clump, L. Maus, and L.B. Anderson, "Principles of Unit
Operations," 2nd edition, p. 637-547, 699-714, John Wiley and Sons, New York (1980).

178
Appendix

Data Sheet 1: Properties of Water

Property Units Symbol 0°C 10°C 20°C 30°C 40°C 50°C

Density Kg m-3 ρw 999.84 999.7 998.2 995.7 992.2 988.1

Dynamic  w(x10 -3 )
N s m-2 1.787 1.307 1.002 0.798 0.653 0.547
Viscosity

Kinematic m2 s -1  (x10 -6 ) 1.787 1.307 1.004 0.801 0.658 0.553

w
Viscosity

Data Sheet 2: Properties of Air (At Atmospheric Pressure)

Property Units Symbol 0°C 10°C 20°C 30°C 40°C 50°C

Density Kg m-3 ρa 1.293 1.247 1.204 1.165 1.127 1.109

-6
Dynamic Viscosity N s m-2  a (x10 ) 17.23 17.72 18.21 18.68 19.15 19.61
-6
Kinematic Viscosity m2 s -1  a (x10 ) 13.32 14.21 15.11 16.04 16.98 17.95

179
 Experiment #8
Liquid-Liquid Extraction

180
Objectives
EXPERIMENT A: Determination of Distribution Coefficient

1. To determine the distribution coefficient for the system organic solvent-

Propionic Acid-Water and to show its dependence on concentration.

EXPERIMENT C

2. To perform mass balance across extraction column,

3. To estimate the mass transfer coefficient with the aqueous phase as the

continuous medium.

Safety Precautions
The unit UOP5 MKII is strictly to be used only for teaching purposes and must be operated

by competent laboratory personnel. Following safety considerations need to be taken into

account:

1. Read The MSDS of the chemicals used in the experiment

2. Ware lab coat, safety googles, protective mask and gloves

3. Use Fume Hood or adequate ventilation when you handle the chemicals in the

experiment.

4. The extraction column is sensitive and made of glass. When filling the

extraction column, open valve V30 for ventilation (see P&ID, Figure 6.2)

5. Electrical connections are exposed when the control cabinet is open. Therefore,

disconnect the plug from the power supply before opening the switch cabinet.

Also, protect the switch cabinet from humidity

181
 6. Contact with ethanol irritates the eyes and skin. Read the MSDS of ethanol

before operation. Wear protective gloves and protective goggles. In case of

contact with the skin, wash with plenty of water. In case of contact with the

eyes, rinse immediately with plenty of water. Do not inhale ethanol vapors

7. Keep ethanol away from all ignition sources owing to its very low flash point

Caution! : Water and electricity are not compatible and can cause serious injury if they

come into contact.

Introduction
Liquid-liquid extraction (LLE) simply involves transfer of a transition component (or
solute) from one liquid mixture into another immiscible liquid solvent. This separation
method is based on the difference in relative solubility of the solute in the two immiscible
liquids. The simplest form of liquid-liquid extraction involves only three liquids:

1. Transition component

2. Carrier liquid, and

3. Solvent

The liquid mixture containing the transition component and carrier liquid is called the feed.
The liquid used to extract the transition component from the feed is called the solvent. It is
important to note that the transition component must be soluble in both the carrier liquid
and the solvent. However, it is better that the transition component has a higher solubility
in the solvent. Ideally, the carrier liquid and the solvent should be immiscible (example, oil
and water).

After contacting the feed and the solvent, the two phases obtained at the end of liquid-
liquid extraction are called the extract and the raffinate. The extract is essentially a solution
of the transition component in the original solvent. The raffinate is essentially the original
182
feed with a decreased amount of transition component. Before going in details of the LLE
apparatus, Figure 6.1 provides an idea about the basics of extraction process.

Figure 8.1: Basics of liquid-liquid extraction, C: carrier liquid, S: solvent, T: transition

component

In Figure 8.1, the solvent is specifically heavier than the carrier liquid. The same case is

applicable to the experiment in this lab. Sunflower oil will be the carrier and water (heavier)

will be the solvent (ethanol will be the transition component). As mentioned earlier, a

condition for extraction is that the transition component is soluble in the solvent. This is

true for the liquid systems used in this lab since ethanol is more soluble in water compared

to oil.

The next step in Figure 6.1 shows is the mixing of the two liquid phases. Upon mixing,

droplets are formed, the specific surface area increases and the three liquids (carrier,

solvent, and transition phase) are brought into intensive contact. In doing so, the transition

component transfers from the carrier liquid into the solvent.

After mixing, two separate liquid phases are formed. The heavier solvent settles down

while the solvent (with the transition component) floats at the top. Finally, the two liquid

phases are transferred into separate beakers. In this lab, the extract will contain ethanol and
183
water. On the other hand, the raffinate will be sunflower oil (with small amount of un-

extracted ethanol). In order to know how much ethanol has been extracted, the extract

mixture density can be used using a pycnometer. The extract (water and ethanol) can be

finally separated using distillation.

LLE units can be of different types, most notable are the following:

1. Mixer settlers

2. Extraction columns

3. Centrifugal columns

In this lab, an extraction column will be used. Students are expected to explain different

types of LLE equipment in their lab reports.

Some applications of LLE in industries are the following:

1. Removal of high-boiling organics from wastewater

2. Recovery and purification of biofuels and chemicals generated by biological

processes such as fermentation and algae

3. Purification of heat sensitive materials, such as pharmaceuticals, flavors,

fragrances and food products

4. Recovery of products from chemical reactions

184
Piping & Instrumentation Diagram (P&ID):

The process diagram for the UOP5 MKII liquid-liquid extraction unit (supplied by

Armfield, UK) that will be used in this experiment is shown below:

Figure 8.1: Equipment P&ID for the LLE experiment

185
Equipment

Figure 8.3: Overview of the CE 620 liquid- liquid extraction system (GUNT, 2013)

In reference to Figure 8.3, the description of the labeled items is as follows:

1. Distillate tank (B2)

2. Control cabinet

3. Regulating valve for solvent inflow (V1)

4. Regulating valve for feed inflow (V2)

5. Extract tank (B3)

6. Regulating valve for feed return (V4)

186
 7. Distillation bridge (W1)

8. Distillation column (K2)

9. Extraction column (K1)

10. Round-bottomed flask (D1)

11. Heating mantle (H1)

12. Regulating valve for solvent return (V3)

13. Solvent tank (B1)

14. Feed tank (B5)

15. Raffinate tank (B4)

16. Feed pump (P2)

17. Solvent pump (P1)

The process starts from the solvent tank B1 (13) where the solvent (water) is placed and the feed tank

B5 (14) where the feed (oil with ethanol) is placed. Once both the positive displacement pumps:

solvent pump P1 (17) and feed pump P2 (16) are switched on from the control cabinet (2), the feed

starts flowing from the bottom of the extraction column K1 (9) while the solvent starts flowing from

the top of the column.

Extraction takes place inside the column where ethanol moves from the feed oil to the solvent (water).

Also, water, being heavier, occupies the lower portion of the extraction column while the oil occupies

the top portion. Therefore, the extract comes from the bottom of the column while the raffinate moves

out from the top.

187
 The CE 620 trainer can be operated either continuously or in batch mode depending on the position

of the 3-way ball valves V7 and V8 (see P&ID in Figure 8.2). For continuous mode, the raffinate

will move out from the top of the column and it will be collected in the raffinate tank B4 (15). On

the other hand, the extract will move from the bottom of the column to the extract tank B3 (5). Thus,

in continuous mode, the feed and solvent tanks will be emptied with time.

In batch mode, valves V7 and V8 are positioned such that raffinate will move out from the top of the
column and it will be collected in the feed tank B5 (14). On the other hand, the extract will move
from the bottom of the column to the solvent tank B1 (13). In other words, the solvent (water) will
flow into the column, it will extract ethanol from the oil and at the end return to the same solvent
tank B1 (13).

Once the extraction is done, the extract (ethanol and water) can be distilled in the distillation column
K2 (8) provided with heating mantle H1 (11). Ethanol, after distillation, will be collected in the
distillate tank B2 (1) and the water can be obtained from the bottom of the distillation column. Note:
ethanol recovery by distillation will not be performed in this experiment.

EXPERIMENT A:
OBJECT OF EXPERIMENT:

1. To determine the distribution coefficient for the system organic solvent-Propionic

Acid-Water and to show its dependence on concentration.

EQUIPMENT SET-UP:

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)

188
Phenolphthalein

Propionic acid

WARNING Ensure that diluted Sodium Hydroxide (NaOH) is used when performing this
experiment.

SUMMARY OF THEORY:

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

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.

READINGS TO BE TAKEN:

1. Make up in a conical flask a mixture of 50ml organic solvent and 50ml of de-mineralized 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.

189
Data Sheet

Experiment#8 L-L Extraction ( A)

190
EXPERIMENT C
OBJECT OF EXPERIMENT:

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.

EQUIPMENT SET-UP:

FIGURE 8.4 LIQUID -LIQUID EXTRACTION AQUEOUS PHASE AS CONTINUOUS MEDIUM

The solvent metering pump is calibrated in percentage of maximum flow which varies slightly from

pump to pump. The pump should be calibrated initially by setting F2 to 100%, setting valve V8 to

the calibrate position and measuring the flow from the pump, using a measuring cylinder and

stopwatch. Calculate the flow rate produced settings of 5% intervals (ml per minute), then plot a

graph of ml per minute against percentage of metering pump stroke. Thereafter any selected flow

may be obtained by using the graph.

SUMMARY OF THEORY:

Let:

191
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

192
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.

PROCEDURE:
1. Add 100ml of proprionic 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.

2. Switch the level control (electrode switch S2) to the OFF (central) position.

3. Fill the water feed tank with 15 litres of clean de-mineralised water, start the water feed pump 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 0.2 l/min (using the
calibration graph obtained as described above).

5. Set electrode switch S2 to the bottom position. Start the metering pump and set at a flow rate of
0.2 l/min.

6. Run for 15-20 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).

WARNING Ensure that diluted Sodium Hydroxide (NaOH) is used when performing this
experiment.

193
Data Sheet

Experiment#8 Liquid-Liquid Extraction (B)

Shut-down procedure

1. After 180min of extraction time, stop pumps P1 and P2

2. Close regulating valves V1-V4

3. Open valve V30

4. By opening the regulating valve V3, the solvent from the extraction column can flow back

into solvent tank B1 by gravity

5. Close V3 as soon as the phase boundary reaches the base of the extraction column

6. By opening valve V28, pour oil feed from the extraction column into a beaker

7. Drain measuring beaker into the feed tank B5

194
Appendix
Table A1: For the ethanol/water mixture: Density in kg/m³ as a function of mass fraction of ethanol
wE and temperature T

195
196
 EXPERIMENT #9
DRYING CHARACTERISTICS IN A TRAY DRYER

197
Objectives
The objectives of this experiment are:

1. To become familiar with the drying process and the operation of a tray dryer

2. To determine the psychrometric properties of air during drying process

3. To determine the moisture content, drying rate, and drying rate constant

4. To estimate the convective heat transfer coefficient

5. To produce drying rate curves

Safety Precautions
-Ware your heat protective gloves, lab coat and safety googles.

Introduction
Drying is one of the main processes in many industries such as pulp and paper, pharmaceutical,

ceramics and food industries. Drying combines both heat and mass transfer to reduce the moisture

content of a wet feedstock to meet the product specifications. The process can be operated in batch

or continuous. There are various types of drying units in industries such as drum dryers, tunnel

dryers, fluidized bed dryers, spray dryers, rotary dryers, and tray dryers. The operation of the latter

type, tray dryer, will be investigated in this experiment.

In tray dryers, the material being dried is placed uniformly in thin layers on the surface of trays

where drying takes place while heat is supplied by blowing hot air over the trays so that the product

will have a uniform moisture content at the e

198
nd of drying. To increase the efficiency of drying, tray dryers can also operate under vacuum and

they are usually suitable for small scale production of newly developed products. The operation of

tray dryer depends on providing a constant temperature and a uniform air velocity over the material

to be dried. Also, usually circulation of air is desired at velocities ranging from 1 to 10 m/s to the

enhance heat transfer coefficient and to eliminate stagnant air pockets. Trays can be of any shape,

but rectangular trays are often used with a surface area of 0.5-1 m2 and with a clearance of no less

than 4 cm between them. Figure 9.1 below shows a lab scale tray dryer.

FIGURE
IGURE7.1:
9. 1: SCHEMATICS OF LAB-SCALE TRAY DRYER (ARMFIELD, 1998)

The drying process involves some important definitions like moisture content X, moisture ratio

MR, gas humidity Hg and saturation humidity (humidity at the interface) Hs and drying rate

𝑑𝑊/𝑑𝑡 . The moisture content 𝑋 is defined as the ratio between the mass of moisture 𝑚 𝑤 to the

mass of solids on dry basis 𝑚 db, which is given by:

Moisture content =

𝑚𝑤
𝑋= (1)
𝑚db

199
And MR is defined as:
𝑋 −𝑋𝑒
𝑀𝑅 = (2)
𝑋0 −𝑋𝑒

Where, 𝑋 and 𝑋 𝑜 are the equilibrium and initial moisture contents. The water content in air 𝐻𝑔

(kg water/kg dry air) can be estimated from psychrometric charts using wet and dry bulb

temperature readings. The saturation humidity 𝐻𝑠 (kg water/kg dry air) can be found by the

following equation:

𝑀𝑤 𝑃∗
𝐻𝑠 = (3)
𝑀𝑎 (𝑃−𝑃∗ )

Where, 𝑀𝑤 and 𝑀𝑎 are the molecular weight of water and air, respectively, 𝑃 is atmospheric
pressure, and 𝑃 ∗is the vapor pressure of water evaluated at wet bulb temperature using Antoine
equation. The drying rate 𝑑𝑊/𝑑𝑡 (kg water/s) is evaluated as a change in the moisture content 𝑑𝑊
on a time interval 𝑑𝑡 for a material with a total surface area 𝐴 (𝑚2 ) which is given by:

𝑑𝑊
= −𝐴𝐾𝐻 (𝐻𝑠 − 𝐻𝑔 ) (4)
𝑑𝑡
1 𝑑𝑊
Where 𝐾𝐻 is the drying rate constant (kg/m2 .s). A plot of versus (𝐻𝑠 − 𝐻𝑔 ) gives a
𝐴 𝑑𝑡

straight line with a slope equal to the drying rate constant 𝐾𝐻 . The total heat transfer coefficient
ℎ (𝑊/m2 .o C), which is essentially convective, in the constant-rate period is evaluated by:

𝐾𝐻 (𝐻𝑠 −𝐻𝑔 )𝐿
ℎ= (5)
𝑇𝑔 −𝑇𝑠

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FIGURE 9. 2: DRYING RATE VERSUS MOISTURE CONTENT (CAENEPEEL, 2006)

here Tg (o C) is the dry bulb temperature of air, Ts (o C) is the wet bulb temperature (the surface

temperature), and L (J/kg) is enthalpy of vaporization for water at the interface temperature. The

drying curve behavior contains three main regions (Figure 2): warming up, constant rate and falling

rate periods. The drying rate of wet solids in air changes throughout the entire drying period due

to different controlling factors in each region of the drying rate curve. However, wet solids exhibit

a constant drying rate region where the drying rate can be correlated to the heat transfer coefficient

as in Eq. (5). Additionally, the surface temperature Ts (liquid/gas interface) at steady state is equal

to the wet bulb temperature of drying air.

The drying kinetics can be modeled using the following models:

Newton’s model:

𝑀𝑅 = exp(−𝑘𝑡) 𝐸𝑞. (6)

Two-term exponential:

201
 𝑀𝑅 = 𝑎 exp(−𝑘𝑡) + (1 − 𝑎) exp(−𝑘𝑎𝑡) 𝐸𝑞. (7)

Logarithmic:
𝑀𝑅 = 𝑎𝑒𝑥𝑝(−𝑘𝑡) = 𝑐 𝐸𝑞. (8)

Where, 𝑎, c, and k are model fitting parameters to be evaluated.

Equipment
The tray dryer apparatus (Armfield, 1998) is composed of an air duct equipped with a fan impeller

and an electrical heater to blow hot air through the duct, a vane anemometer to measure the velocity

of air at the outlet of the duct, a digital balance to measure the change in mass of the material being

dried, an aspirating psychrometer to measure wet and dry bulb temperatures, and shelves to keep

trays.

FIGURE 9. 2: LAB-SCALE TRAY DRYER (ARMFIELD , 1998)

Access point for the psychrometer are provided before and after the trays and are covered with
flaps when not in use. Additionally, the settings for air temperature and velocity can be adjusted
via control knobs in the control panel with a maximum of 1.5 m/s air velocity and up to 80 oC hot
air at low velocities.

Material Preparation
1. Mix 250 g of sand with 55 ml of water

202
 1. Experimental Procedure

2. Measure the mass of the empty tray

3. Record the tray dimensions

4. Cover the tray with approximately 100 g of wet sand (make sure to cover the entire surface

of the tray with sand)

5. Measure the initial mass of both the tray and wet sand

6. Switch on the unit, and set the air velocity control to 5 and the temperature control to 6

7. Leave the unit 5 minutes to warm up and stabilize

8. Measure the temperature of air at the inlet of the tray dryer using a digital psychrometer and

the velocity using an anemometer

9. Place the tray on shelves inside the dryer duct and start the timer.

10. Record the mass of the material being dried every 5 minutes and measure wet and dry bulb

temperatures at the outlet of the tray dryer using the psychrometer and record the sand surface

temperature using a mercury thermometer (Note: the psychrometer is inserted 3 minutes prior

to measurement time to obtain stable readings)

11. Terminate the experiment when no change in mass is observed.

12. Perform the experiment with same amount of wet sand at an elevated temperature

(temperature control = 9)

Analysis of Results

203
2 Calculate the moisture content, moisture ratio, and drying rate at each time interval

3 Plot both the moisture content and the drying rate versus time. Additionally, plot the drying curve

(i.e., drying rate versus moisture content) and discuss the behavior of graphs.

4 Determine the drying rate constant by plotting the drying rate versus the driving force (Hs-Hg)

5 Evaluate the heat transfer coefficient during the constant-rate period in the drying curve

6 Compare moisture content vs. time and drying rate vs. moisture content plots for both temperature

settings

7 Fit the experimental data to drying models proposed in Eq. (6) to Eq. (8)

204
Data Sheet

EXPERIMENT#9 Drying Characteristics for Tray Dryer

Tray dimensions:

Tray weight:

Initial weight of tray + wet sand:

Temperature control settings:

Fan speed control settings:

Mass of Dry Bulb Wet Bulb Surface

Time (min) Material+ Tray Temperature (o Temperature Temperature (o
(g) C) (o C) C)

10

15

20

25

30

35

40

45

50

205
206