Module Guide

Principles of Separation &

Reaction
EAA_5_968
Laboratory Guide and Sheets
Staff
Mr Steve Jones
Ms Rim Saada

Session: 2013/2014
Faculty of Engineering, Science & the Built Environment

become what you want to be

A:

General

1
Laboratory studies constitute the main coursework element of the unit. The coursework is
equivalent to 30% of the unit assessment. Students must pass the laboratory studies in order to pass the
unit. It is therefore important that you attend all lab sessions and hand in all lab reports and deliver the
oral presentations for assessment.
2

Each student will undertake the following four investigations:

Ammonia Absorption

ii

The Wetted -Wall Column

iii

Liquid Phase Chemical Reactor

iv

Continuous Stirred Tank Reactors

3
Lab sessions are as indicated on the attached programme. No student will be allowed into a lab
session more than 15 minutes late. Please make sure you arrive for your lab sessions on time.

Safety

1
You would all have received copies of the lab safety document when you enrolled. Make sure
you are familiar with what the document says about lab safety.
2
Safety must be observed at all times. Please DO NOT do anything that may place your safety
and that of other users of the lab at risk.
3
Ask for assistance if you are not sure about how to use or operate an apparatus or equipment.
An experienced technician will be present at all lab sessions.
4
DO NOT attempt to repair any faults (mechanical, electrical etc). Bring any faults to the
attention of the lab technician.
5
Do make sure to wear appropriate safety clothing whilst in attendance at lab sessions. These
include lab coats and safety glasses where specified.

Assessment

Each student must submit TWO written reports and participate in preparation and delivery of TWO oral
presentations (see the enclosed timetables). Each report and oral presentation is accounted for 20% of
the total lab mark. Lob books are also accounted for 20% (see section D).
The following guidance give you details about each method of assessment.

C-1

Laboratory Reports

Refer to "Notes on Laboratory Reports" issued to all students at the start of the academic year. However,
note that assessment will be based on the following key points, which must therefore be covered in your
reports.

Summary: must include brief statements on the following:

i
ii
iii
iv
v
vi

Topic investigated and its significance in chemical engineering.

Objectives of the lab study.
Equipment used
Key results
Main conclusions
What you have learned from the lab study.

Introduction
i
Background, including theory and the importance of the topic investigated in
chemical engineering.
ii
Objectives of lab study (must be stated in introduction as well as summary)

Experimental Equipment
i
Drawing showing layout of equipment
ii
Brief description indicating any special features, capacities, range, make and type (Do
Not copy the lab sheet).

Experimental Procedure and Observations

i
Description of procedure, indicating measurements taken
ii
Observations made during investigation, making note of any problems encountered
which may have affected results.

Results and Calculations

i
Tabulate all results/measurements obtained during lab study.
ii
Tabulate all calculated results. Show sample calculations for each type calculated
result.

Discussion of Results
i
Discuss all results, making sure you sddress each objective in the light of your results.
ii
Discuss any discrepancies between your results and theory, indicating possible reasons.
iii
Use this section to demonstrate that you have understood the topic you investigated and
its significance in chemical engineering; explain what you have learned as a result of
carrying out the study.

Conclusions
Make clear conclusions on each of the objectives in the light of your results and discussions.

References

All reports will be submitted as detailed reports. Reports will be marked according to the following
scheme:

Summary
Introduction
Experimental Equipment
Procedure and Observations
Results and Calculations
Discussion
Conclusions
References

10%
10%
10%
10%
20%
20%
10%
10%

All reports must be handed in at the Faculty Office by 4 pm on the day before the next lab session. They
must be marked for the SUPERVISOR attention.
Faculty guidelines on late submissions will be applied.
Handwritten reports are NOT acceptable.

C-2 Oral Presentations

Oral presentation is a team activity. Students in each subgroup (eg, A1, B2, C3, etc.) will be divided
into two teams (2 or 3 students in each team) to prepare their presentation. All students in a team
must participate in the preparation and delivery of the presentation. You give your presentation to
your lab supervisor in his/her office approximately two weeks after the day of the experiment.
You may bring your presentation in a USB stick or, alternatively, use your own laptop for the
presentation.
Also bring in your log books which should contain your RAW DATA, and a SAMPLE OF
CALCULATIONS.
Be prepared to deliver a 15-minute presentation and 10-minute Q&A. At the end, your supervisor
will give you a verbal feedback. You will be assessed on individual basis as well as team effort and
quality of the PowerPoint slides. The individual marks will be published on the Blackboard soon after
the presentations.

Structure of the presentation

Context - 1 slide
Objectives of the experiment - 1 slide
Diagram of the apparatus - 1 slide
Results - maximum 10 slides
[Discussion - verbally through the results]
Conclusions - 1 slide
References 1 slide

Context, Objectives of the lab, Conclusions: Use bullet points to highlight different items.
Diagram : Must not be hand drawn. Describe the full operation of the apparatus.
Results: Present the raw data in tabular form and the calculated results in figures.
Number and label all tables and figures.
Label axes correctly and ensure that all units are included.
Discussion: Do not add written comments. Go through your results, analyse and discuss them,
explain any anomalies and source of possible errors, and finally suggest ways to improve the
experiment.
Conclusions: Mind how you prepare this slide as it could be the most crucial of all!
State your findings using bullet points. Remember to relate them to the objectives.
References: Use Harvard referencing system.

Font
Arial 18, or times New Roman 20 (except for tables and figures which you may use smaller font
size).
Do not put too much text in a slide. Use bullet points wherever possible.

Organise yourselves!
Prepare! Decide who is going to do what. Make sure that all of you participate in the presentation
and Q&A. For example, for a group of 3, one can go through the Context, Objectives and Diagram,
one through the Results (including sample of calculations and explanation of tables/figures), and one
through the analysis and discussion of results and conclusions. All of you are expected to participate
in answering the questions.

You will be given individual marks based on your participation in the presentation.
Introduce yourself before starting your part!
Rehearse! Make sure that you keep to the time.

Assessment and feedback

Your supervisor will assess individual participation in the presentation as well as team effort. You
will be given a verbal feedback right after your presentation. You will be aware of your marks
through the Blackboard soon after the presentation.
Marking scheme guidance:
Theory/Introduction
20%
Results/Conclusions
40%
Question handling
20%
Oral presentation skills 20%

Presentations timetable
The presentations are carried out in a suitable date and time approximately two weeks after the day of
the experiment. A timetable for the oral presentations will be published nearer the time.

Do not miss your allocated date and time!

If a team miss the allocated time for the presentation, without a very good and convincing reason,
they will NOT be given an alternative time and will be given zero mark for that experiment. Note that
arranging a suitable date and time for both you and your supervisor could be very difficult, so make
every effort to deliver your presentation according to the timetable.
If an individual misses the presentation, WITH or WITHOUT a good reason, his/her mark will be
calculated as HALF of the average mark for the team mates who have given the presentation,
providing that he/she has participated in preparation of the presentation. If it appears that he/she has
not participated in preparation of the presentation, a zero mark will be given for that experiment.

Log Books

All students must keep a personal log book which must be brought to lab classes. The log book will be
marked (equivalent to one lab report) and must be handed in together with the last report that you
submit. The following must be recorded in your log book for each lab session and will form the basis for
marking your log book:
(i)
(ii)
(iii)
(iv)
(v)

Date on which lab study was undertaken

Objectives of lab study (with a brief explanation of each objective)
Experimental observations
Experimental results as obtained during lab session (if not written in the tables provided in the
lab sheet.)
Sample calculations

Log books must be signed by the academic supervisor at the end of each lab session.

AMMONIA ABSORPTION
Effect of Flowrate on Mass Transfer Coefficient

Objective:
To determine the overall mass-transfer coefficient (Kga), in
a small packed column for the air/ammonia/water system
at several different air flow rates.

Division of Chemical and

Petroleum Engineering

Make up 25 mls of 0.01 N sulphuric Acid and add some

phenolthalein indicator. Split the 25 mls between the 2
absorption bottles in the absorption train say 5 mls to
the first bottle after the column and 20 mls to the second
bottle. Make up to a greater depth with 50 mls distilled
water to ensure adequate bubbling. (The additional water
makes no difference and is ignored in subsequent
calculations.)
Turn on the air at 4 L/min to bubble through the ammonia
supply bottle and up through the column exiting through
the safety bottle of dilute sulphuric acid.
Start the clock and turn the three-way valve at the same
time to shut off the dilute sulphuric acid bottle and direct
the air through the absorption train. When the acid in the
first bubbler bottle has been exhausted the indicator will
change colour and the test should be stopped.
Remix the contents of both bottles of both bottles and
back-titrate against 0.01 N NaOH to calculate the excess of
H2So4 used in the absorption bottles and thereby calculate
the quantity of NH3 absorbed. Repeat this dummy runs if
necessary using different solution concentrations until you
get a test time of about 10 minutes. Actual tests will be
longer but should not exceed 30 minutes.

Equipment:
A 5 cm diameter absorption column packed with a 1 cm
Raschig rings to a height of about 12 cms.
Water enters the top of the column via a flowmeter,
passes down through the packing, and leaves through a Utrap at the bottom of the column.
Air passing from a rotameter bubbles through a
concentrated solution of ammonia to pick up ammonia
gas.
It then enters the bottom of the column where most, but
not all, of the ammonia is absorbed. The exit air leaving
the top of the column is passed through the two-bottle
ammonia absorption train to measure the ammonia
concentration in the air.
Whilst waiting for a test to stabilise, the exit air leaving the
top of the column must be bubbled through a safety
bottle containing dilute sulphuric acid to remove any
unabsorbed ammonia.
Symbols:
T = duration of test
seconds
-1
N = rate of mass transfer
molNH3s
-1
FA = Flow rate of the air
Ls
-1
FW = Flow rate of water
Ls
-1
yi = conc of ammonia in inlet air molNH3L of air
-1
yo = conc of ammonia in outlet air molNH3L of air
*
y = conc of ammonia in air in equilibrium with the
solution of ammonia
xi = conc of ammonia in inlet water = zero
-1
xo = conc of ammonia in water out molNH3L of water
-1
-1
kga = mass transfer coefficient,
mols bar

Test 1:
Set the water flow to 1.0 L/min and allow to run for about
10 minutes to ensure that the packing is thoroughly
wetted.
Make up the absorption train with 25 mls of 0.01 N of acid
as before.
Turn on the air at 4 L/min to pass up the column. Adjust
the height of the U-trap to maintain a liquid level in the
bottom of the column to prevent air and ammonia
escaping from the bottom of the column.
When conditions have stabilised, start the clock and turn
the three-way valve as before.
Collect all the water containing the absorbed NH3 leaving
the bottom of the column (over the same period) and
titrate it with 0.01 N H2SO4 to calculate the quantity of
NH3 absorbed by the water. If there is too much effluent
water, analyse a sample only, e.g. or 1/10 of the total
and multiply up. The NH3 entering the column in the air
can be calculated by mass balance.

Procedure:
This is suitable for the average flow rates experienced in
this test but if a test is too short or too long the solution
strengths used should be changed to suit the new
conditions.
Dummy run:
Do a dummy run with NO water passing down the column
to ensure that you are completely familiar with the
analytical procedure and calculations when ammonia is
absorbed. It will also help to establish the correct solution
concentrations and the most suitable time for the test. It
does not matter if you have wet the column by mistake.

Test 3:
Repeat the test to get reproducible results.
Test 4:
Repeat at four other air flow rates using the same water
rate.

Theory:
The process may be represented by the following diagram:

Absorption Graph: (concentration of ammonia in water)

gas
entering
yi

safety bottle

absorption train

xi
FW

fraction of
ammonia in air

water
operating line
yo
yo*

ammonia
absorption
column

ammonia bubbler
FA
yi

equilibrium line
yi*
xi water
entering

xo water
leaving

Report:
For each test, calculate the mass balance to obtain the
amount of ammonia in each stream and the amount of
ammonia absorbed. Plot the equilibrium curve y =
0.0012x, and the operating line as shown in the diagram
above. Note: the operating line is obtained by joining the
points. (xi , yo) and (xo , yi) by a straight line.
From the graph determine y and y, and hence calculate
kga using equation (2).
The correct values of kga obtained in the tests should be
plotted against air flow rate, FA, on log-log graph paper.
The slope "n" of the best straight line so obtained should
be measured and compared with literature value of 0.83.
0.83
i.e. kga = B * FA

adjustable
U-trap
drain

By mass balance on the ammonia,

N = FA * (yi yo)
= FW * (xo xi) = FW * xo ; since xi = 0
FA * yi FA * yo = FW * xo
yi = ( FW * xo + FA * yo ) / FA
i.e.
We can calculate the inlet ammonia concentration, yi,
from the other readings.

Sample Calculation:
The accuracy of this calculation is not guaranteed!
The units and concentrations in this example may be
entirely different from those used in your experiment.
However, the general principles are the same. Duration of
test, T = 1200 seconds:
If air flow rate = 4 L/min.
FA = 4/60 = 0.0667 L/s
Volume of 0.01 N H2SO4 used in absorption train =25 ml.
Volume of back titration using 0.001 N NaOH = 7.3 ml.
i.e. Volume of 0.01 N H2SO4 neutralised by NH3
= 25 7.3 = 17.7 ml.
(Note: If the test is too short, the back titration will be
large and will not give accurate results.)
A 0.1 N solution contains 1 mol of NH3 per litre of solution.
-3
17.7 ml of 0.01 N solution contain (17.7*10 *0.01)
-5
mol = 17.7*10 mol
-5
i.e. Moles of NH3 absorbed = (17.7*10 ) / 1200 mol/s
-7
=1.475 * 10 mol/s
i.e. Concentration of NH3 in air leaving column is given by:
-7
-6
yo = 1.475 * 10 / 0.0667 = 2.21* 10 mol/L
Suppose total absorption water used in test = 73 ml. The
NH3 absorbed by the water can be measured by titration
of a sample with 0.001 N H2SO4 and multiplying up in
proportion.
i.e. If a 10 gm sample of absorption water is titrated
against 1.2 ml of 0.01 N H2SO4; moles of NH3 in 10 gm
-3
-5
sample (volume of water) = (1.2*10 )*0.01 = 1.2*10 mol
Concentration of NH3 in water out
-5
-3
-3
Xo = (1.2*10 ) mol / (10*10 ) L = 1.2*10 mol/L

In the air-ammonia-water system, the gas film controls the

rate of mass transfer according to the equation:
N = kg * a * (y y*) - - - - - - - - - - - (1)
Where (y y*) is the difference between the ammonia
concentration in the bulk gas flow and the ammonia
concentration at the water/gas interface,
i.e.
y* is the equilibrium value for the ammonia concentration
in the liquid phase, x.
The equation for the equilibrium curve is:
y = 0.0012x
Where:
y = concentration of ammonia in air in moles per litre
x = concentration of ammonia in water in moles per litre
The average value of the rate of mass transfer is given by:
N = kg * a * (y)mean - - - - - - - - - - (2)
Use the arithmetic mean difference. Do not use the "log
mean" as it can exaggerate errors.
(y)mean = * (ytop + ybottom)
ytop = (yo y*i) = yoi since y*I = 0 ; when xi = 0
ybottom = (yi yo)
Using equation (2) and the experimental data obtained in
the test, kga, the overall mass transfer coefficient, can be
determined.

Table of Test Results:

Experimental results

Calculated results

Duration
of
test

water
flow

air
flow

H2SO4 conc
used in
absorption

initial
H2SO4
vol used

back
titre

Volume of
water used
in absorption

NH3
in air
absorption

NH3
in air
leaving

NH3
in water
leaving

mass
transfer
coefficient

FW

FA

ml

ml

ml

yi

yo

xo

kga

Revised: Dr F Jahanzad / Dr S Larkai

January 2011

CONTINUOUS STIRRED TANK REACTORS

Division of Chemical and
Petroleum Engineering

Effect of Residence Time on Conversion

Objectives:
1. To simulate the conversion of reactant in a
cascade of three continuous stirred tanks.
2. To determine the effect of flowrate (i.e.
residence time) on the conversion of reactant in one tank
in a cascade of continuous stirred tanks.

Symbols:
Q = volumetric flowrate
V = volume of tank
C = solution conductivity
C0 = initial salt concentration in tank 1
C1 = conductivity in tank 1 at time t
C2 = conductivity in tank 2 at time t
C3 = conductivity in tank 3 at time t
t = the time after start up
= mean residence time in each tank

Introduction:
Many processes in the chemical industry involve the
addition of reactants to a cascade of several continuous
reactors in series, i.e. CSTR. The liquid feed enters the first
tank and overflows to each of the subsequent tanks in the
cascade. The rate of reaction in each tank is affected by
the concentration of the reactants at any specific time.
Liquid phase reactions are carried out on small to medium
scale, for the manufacture of organic chemicals and
pharmaceutical products. For example, ethanol is
produced by a reaction between sodium hydroxide and
ethyl acetate.

3 -1

m s
3
m
-1
Siemens m
-1
Siemens m
-1
Siemens m
-1
Siemens m
-1
Siemens m
s
s

Theory:
In this experiment it is assumed that:
a) salt concentration is proportional to solution
-1
conductivity (units: Siemensm ) for dilute solution and
does not vary very much with temperature
b) complete mixing takes place in each tank
instantaneously
c) zero concentration corresponds to the
concentration of the raw water supply, about 800
-1
microSiemenscm

In this experiment, no chemical reaction takes place. The

residence time behaviour of a dissolved salt through a
cascade of three continuous stirred tanks is examined at
different flowrates for a constant starting concentration
of salt. The experimentally determined variation of slat
concentration with time in each tank is compared with
results predicted from theoretical equations, allowing
deviations from ideal behaviour to be observed.
Conversion of reactant is then estimated by graphical
integration for both the experimental results and
theoretical data. The general effects of the transient
concentration of reactants are similar to those induced in
a chemical reactor, subject to variation in throughput.

Tank 1:
Water enters a tank flowrate, Q and a salt concentration
of zero. The salt concentration in the tank is C0 at zero time
and decreases with time as it is diluted by influent water.
Taking an incremental mass balance for the slat when the
concentration changes by dC in time dt:

i.e.

0=Q.C.dt V .dC

(i)

Rearranging we get:

Equipment:
1. Three equal sized Perspex tanks with provision
for overflow from tank 1 to tank 2 then to tank 3, and for
the overflow from drain. Each tank measures 152mm by
254mm deep with the overflow weirs being placed
228mm from the base. The tanks are stirred by propellers
driven by the same drive motor. A rotameter controls the
feed to tank 1.
2. A portable conductivity meter is available to
measure the conductivity of the solution in each tank. It
has four scales, which can be adjusted to give a reading in
the desired range. For dilute solutions, conductivity is
approximately proportional to salt concentration. The
units on the meter must be checked.

C.Q
dt (ii)
V
C
dC= dt (iii)
dC=

Or:

Where

= mean residence time = V/Q

Rearranging (iii) gives:

dC
1
= dt
C

(iv)

Integrating for time between 0 and t; and concentration

between C0 and C1 gives:

5. Deducting the conductivity of tap water (e.g. 800

-1
mScm ) from this value gives the standardised value of
-1
the initial concentration: C0=(2000-800)=1200 mScm
Experiment 2
Repeat the procedure in experiment 1 at water flowrates
of 0.5 L/min and 2 L/min respectively, but measure the
time dependent conductivity in tank 1 only.

( )

( )
Rearrange to give:
(

( )

Results:
Experiment 1
1. Plot graphs of standardised conductivity vs. time
for each tank on the same graph and compare the shapes
of the graphs.
2. Calculate theoretical values of conductivity for
each tank using the relevant theoretical equations and the
measured standardised value of C0. For each tank, plot
theoretical and experimental conductivities on the same
graph and compare the shapes of the graphs. Comment on
the reasons for any differences in your discussion.
3. For both the experimental and theoretical curves
calculate the area under the graph for each tank up to t=5
(you may use any numerical integration method, such as
Simpsons rule). The area represents reactant conversion
and should be approximately the same for all tanks.
Comment on the reasons for any differences in your
discussion.

i.e.
C1 decreases with time.
Tank 2:
By similar differential mass balance and integration, we
get:
( )

( )

Tank 3:
Similarly, the time dependent concentration in tank 3 is
given by:
( )

i.e.
C3 increases initially with time then decreases.
Procedure:
Experiment 1
1. Fill the tanks with cold water directly from the
tap initially, and then through the rotameter unit all tanks
are full and flowing freely down the cascade. Stop the
water flow and remove half of the water from the first
tank. Place 50g of sodium chloride in a 500ml beaker, add
some cold water and stir with a glass rod to dissolve the
salt. Pour the solution into the first tank and start the
stirrers to mix completely.
2. Start the water flow at 1.0 litre per min into the
first tank using the rotameter (range 0.2 to 3.4 L/min).
The water levels in each tank will automatically adjust
until the flow in and out of each tank is the same.
3. The test starts when the water starts to overflow
from tank 1 to tank 2. Start the clock at this point and
take conductivity readings in each tank at various time
intervals, e.g. every 1 or 2 minutes, so that graphs of
conductivity in each tank can be drawn as a function of
time. The solution conductivity is measured by dipping
the probe into the tank and allowing a few seconds
before taking a reading. It is not necessary to wash the
probe between readings. Also it is not necessary to
sample all tanks at exactly the same time provided that
the correct time is recorded for each reading.
4. Take a sample of tap water in a clean beaker and
measure the conductivity. (Typically the conductivity of
-1
the tap water about 700 to 800 microSiemens cm ).
Obtain standardised values of the conductivity in each
tank by deducting the conductivity of tap water from the
values measured in step 3. For example, when the salt
solution is added to tank 1 in step 1 and the tank is filled
with water to the weir from the rotameter, the
-1
conductivity should be about 2000 microSiemens cm .

Experiment 2
1. For each flowrate (including the flowrate used in
experiment 1), plot graphs of standardised conductivity vs.
time for tank 1 only, on the same graph and compare the
shapes of the graphs.
2. For the experimental curves only, calculate the
area under the graph for tank 1 up to t=5. Comment on
the changes in values of area under curves with flowrate in
your discussion.
Reference:
1. F.A.Holland and F.S.Chapman "Liquid Mixing and
Processing in Stirred Tanks", p.109 (Chapman & Hall,
1996).
2. J.JCarberry. "Chemical & Catalytic Reaction
Engineering", p.92 (McGraw-Hill, 1976).
Conductivity in a stirred tank cascade.

Conductivity

C3
C2

C1
Time

Revised: Dr S Larkai/Dr F Jahanzad (January 2011)

Results
Experiment 1
Flowrate = 1.0 L/min
Measured C0 =

Time
(s)

Tap water conductivity =

Tank 1
Measured
conductivity
(microSiemens/cm)

Tank 2
Measured
conductivity
(microSiemens/cm)

Tank 3
Measured
conductivity
(microSiemens/cm)

Standardised C0 =

Tank 1
Standardised
conductivity
(microSiemens/cm)

Tank 2
Standardised
conductivity
(microSiemens/cm)

Tank 3
Standardised
conductivity
(microSiemens/cm)

Experiment 2
Measured C0 =

Time
(s)

Tap water conductivity =

Flowrate = 0.5
L/min
Measured
conductivity
(microSiemens/cm)

Flowrate = 1.0
L/min
Measured
conductivity
(microSiemens/cm)

Flowrate = 2.0
L/min
Measured
conductivity
(microSiemens/cm)

Standardised C0 =

Flowrate = 0.5
L/min
Standardised
conductivity
(microSiemens/cm)

Flowrate = 1.0
L/min
Standardised
conductivity
(microSiemens/cm)

Flowrate = 2.0
L/min
Standardised
conductivity
(microSiemens/cm)

LIQUID PHASE CHEMICAL REACTORS

Division of Chemical and
Petroleum Engineering

Effect of Temperature on Reaction Rate Constant

BATCH CHEMICAL REACTOR

Objective:
To find the reaction rate constant in a batch stirred tank reactor for the saponification of ethyl acetate with dilute
sodium hydroxide.
Summary of Theory:
The overall mass balance for the stirred tank reactor may
be written as:

The rate of this reaction can be expected to depend on

the concentrations of both A (NaOH) and B (ethyl
acetate). The reaction is known to be first order in both
components.
Thus, from Equations (1) and (2), we have:

dC A
=kCA C B
dt

And, for batch operation, this can be rearranged to:

Further, if we make the two concentrations equal from

the start, we have:

i.e. for a material (A)

dC A
=rA
dt

dC A
=kCA2
dt

(1)

Where:
CA0 is input concentration of A in the input stream
CA is exit concentration of A in the exit stream
rA is the rate of reaction of A

Integrating this gives:

kt=

In homogeneous reaction systems, reaction rates depend

on the concentration of the reactants.

-rA kC C

m
B

Experimental Procedure:
"Safety goggles must be worn whilst carrying out these
experiments. You are also advised to wear the protective
gloves provided"
You are provided with stock solutions of 0.1M sodium
hydroxide and 0.1M ethyl acetate.
1.

(2)

2.

Where:
k
= rate constant
n, m = appropriate powers (based on experimental data)

3.

The reaction to be studied is:

NaOH CH 3 COOC2 H 5 CH 3 COONa C 2 H 5 OH

4.

(3)

Thus the batch stirred tank reactor allows us to measure

rates of reaction by observing the change of reactant
concentration within the reactor with time. We can also
easily change and control the temperature of the system.
The experiments will be used to find values of the rate
constant and the Arrhenius parameters.

Collision theory indicates a rate increase if the

concentration of one or both of the reactants is increased.
Conversely, lowering the concentration should have the
opposite effect. However, the specific effect of
concentration changes in a reaction system has to be
determined by experimental methods. Increasing the
concentration of substance A in reaction with substance B
could increase the reaction rate, decrease it or have no
effect on it depending on the particular reaction. It is
important to recognise that the balanced equation for the
net reaction does not indicate how the reaction rate is
affected by a change in concentration of reactants.
The general form of the rate law for a bimolecular reaction
is:
n
A

1
1

C A C A0

Set up the conductivity meter and place the

Set the reaction temperature (initially 25C) on

the thermostatic bath.
Fill to the mark the two 1 litre flasks with,
respectively, sodium hydroxide solution and ethyl
acetate solution and place them in bath.
Set the reaction temperature on the reactor
control panel.

probe end in the bath to come reaction

temperature.
5. Allow the flasks to reach reaction temperature.
6. Add the 1 litre of sodium hydroxide solution to
reactor.
7. Add the 1 litre of ethyl acetate solution to reactor
and start the clock when ca. 50% added.
8. Wait about 30 seconds, withdraw ca. 200ml
sample, and as soon as possible measure its
conductivity, noting time; then return sample to
reactor and the probe to the bath.
9. Repeat every 0.5 to 1 minute for about 10
minutes.
10. Allow to run for a further 20 minutes taking
readings every 3 or 4 minutes.
11. Repeat experiment at about 30C and 40C.
Results and Calculations:
Concentration of the hydroxide, CA can be shown to be the
following function of conductivity:

C A=C A0

k k
k0 k

Where:
k0 = is the initial conductivity at time t=0
k = is the final conductivity when the reaction is
complete.
1.

Plot the graph of measured k vs t

2.

Extrapolate to t=0 to find k0.

3.

Extrapolate to large t to find k.

4.

Hence calculate the hydroxide concentration

using the expression above and use this with the
rate expression to find the rate constant for the
reaction by drawing a suitable graph and finding
the gradient.

5.

Use the rate constant at different temperatures

to find the Arrhenius parameters.

Revised: Dr R Best/Dr F Jahanzad (January 2011)

WETTED WALL COLUMN

Effect of Reynolds Number on Mass Transfer Coefficient

Objectives:
1. To establish the variation of mass transfer
coefficients for humidification of air with air
flowrate.
2. To determine the correlation between mass
transfer coefficient and Reynolds number for (i)
laminar flow (ii) turbulent flow.

kg
a
d

Re

-1

=
=
=
=
=
=

-2

mass transfer coefficient, kg s m

2
wetted surface area of column, m
diameter of column, m
-3
density of air, kg m
viscosity of air, Pa s
Reynolds number, calculated as:
4 Q
Re =
d
Note: H3 and H4 represent the humidities of the layer air
immediately in contact with the liquid film at the air inlet
and air outlet respectively.

Introduction:
Wetted wall columns are used mainly for the theoretical
studies of mass transfer. In some cases however these are
used industrially for mass transfer applications where high
rates of heat transfer are required. A wetted wall column
is a simple vertical tube, with gas flowing either countercurrent or co-current to a 'volatile' liquid. The liquid flows
down the surface of the tube in a thin film. The interfacial
area between the gas phase and the thin film of liquid is
measurable and is kept constant. The mass transfer
coefficient for the gas phase (i.e. transfer of liquid from
the film to the gas) is calculated from the evaporation rate
of liquid into the gas stream. The rate of evaporation, i.e.
rate of mass transfer, depends on the conditions at the
interface between the liquid film and the gas stream.
Usually the flow of the liquid film is laminar, but the flow
of the gas stream could be laminar (no ripples at the
interface) or turbulent (ripples at the interface). Thus the
rate of mass transfer, and hence mass transfer coefficient
will depend on whether the gas phase flow is laminar or
turbulent.

Theory:
A mass balance of the water (vapour) transferred from
liquid film to air along the entire height of the column is
given by:

Q( H 2 H 1 )=k g aH M

(i)

Re-arranging equation (i) gives:

kg

Q( H 2 H 1 )
aH M

(ii)

A mathematical correlation, similar to the one predicted

by Gilliland and Sherwood, may be used to describe the
relationship between mass transfer coefficient and
Reynolds number. For constant temperature applications
or where temperature variations are negligible, the
correlation is of the general form:
k g d B Re N

Equipment:
1. Three vertical glass tubes measuring:
i. 4.1 cm internal diameter, 74 cm high
ii. 2.1 cm internal diameter, 64.5 cm high
iii. 1.4 cm internal diameter, 64 cm high
2. Rotameters for air flow
3. Wet and dry bulb thermometers

(iii)

Where B and N are constants which are determined

experimentally. For turbulent flow, N is approximately
equal to 0.83 (according to the Gilliland and Sherwood
correlation).
A plot of log(kgd) versus log(Re) should give a straight line
with a slope equal to N.

Symbols:
3
Q = air flowrate, m (dry air)/s
H1 = humidity of air entering column, kg water/kg dry air
H2 = humidity of air leaving column, kg water/kg dry air
H3 = saturation air humidity at inlet water temperature,
kg water/kg dry air
H4 = saturation air humidity at outlet water temperature,
kg water/kg dry air
HM = arithmetic mean humidity difference, calculated as:
HM

Division of Chemical and

Petroleum Engineering

Procedure:
1. Select a column and circulate water through it in
a thin film, ensuring that the complete surface is
wetted. A drop of Teepol may be used to assist
wetting, and the tube can be cleaned with a long
brush if necessary. Note that the water inlet
temperature and the water outlet temperature
for each test. The water rotameter is for
guidance only.
2. Ensure that the inlet and outlet air hygrometers

(H 4 H1 ) (H 3 H 2 )
2

are wet at all times.

3.

4.

For each column, select a low air flowrate on the

air rotameter. Allow the temperatures to reach a
steady-state (about 15 min) and take readings of
wet and dry bulb temperatures for both the inlet
air and the outlet air. Use the psychometric chart
to convert these readings to air humidity at inlet
and outlet.
Repeat at four higher flowrates of air.

Results:
1. Calculate the Reynolds number corresponding to
each flowrate.
2. Combine the data from all three columns and sort
into laminar flow and turbulent flow.
Laminar flow: Re<2000
Turbulent flow: Re>2000
3. For each type of flow, i.e. laminar and turbulent,
plot a graph of kgd versus Re using log scales.
4. For each graph calculate the slope of the best
straight line so obtained, which is equal to the
exponent N in the general correlation.
5.

6.
7.

In your discussion explain how air flowrate affects

the mass transfer coefficient, indicating whether
or not this agrees with known theory.
In your discussion explain how Reynolds number
affects the mass transfer coefficient.
Indicate the differences between the
experimentally exponents in the correlation and
those indicated in the text. For turbulent flow
Gilliland and Sherwood indicate that N=0.83.
Explain possible reasons why the value of the
exponent may be different for laminar flow and
turbulent flow.

References:
1. Chemical Engineering Vol. 1, Chapter 10, J M
Coulson & J F Richardson
2. Principles of Unit Operations, Foust et al
3. Absorption, Distillation and Cooling Towers, W S
Norman
4. Ind. Eng. Chem. 26(516), 1934 E R Gilliland & TK
Sherwood

Revised: Dr S Larkai/Dr F Jahanzad (January 2011)

MEASUREMENT OF HUMIDITY

Experimental Results:

Column 3: 4.1 cm internal diameter, 74 cm high

Air Flowrate
(rotameter)
(L/min)

Water inlet
temperature
(C)

Water outlet
temperature
(C)

Air inlet dry

bulb
temperature
(C)

Air inlet wet

bulb
temperature
(C)

Air outlet dry

bulb
temperature
(C)

Air outlet wet

bulb
temperature
(C)

Air inlet dry

bulb
temperature
(C)

Air inlet wet

bulb
temperature
(C)

Air outlet dry

bulb
temperature
(C)

Air outlet wet

bulb
temperature
(C)

Air inlet dry

bulb
temperature
(C)

Air inlet wet

bulb
temperature
(C)

Air outlet dry

bulb
temperature
(C)

Air outlet wet

bulb
temperature
(C)

Column 2: 2.1 cm internal diameter, 64.5 cm high

Air Flowrate
(rotameter)
(L/min)

Water inlet
temperature
(C)

Water outlet
temperature
(C)

Column 1: 1.4 cm internal diameter, 74 cm high

Air Flowrate
(rotameter)
(L/min)

Water inlet
temperature
(C)

Water outlet
temperature
(C)

A. Laminar Flow (Re<2000)

Column
diameter,
d (m)

Air
Flowrate
3 -1
(m s )

Reynolds
Number
Re

H1

H2

H3

H4

HM

Mass
transfer
coeff., kg

kgd

H1

H2

H3

H4

HM

Mass
transfer
coeff., kg

kgd

B. Turbulent Flow (Re>2000)

Column
diameter.
d (m)

Air
Flowrate
3 -1
(m s )

Reynolds
Number
Re