CEY Issue 3 Instruction Manual

PLUG FLOW REACTOR
Instruction Manual
CEY
ISSUE 3
December 2010
Table of Contents
Copyright and Trademarks ...................................................................................... 1
Use with CEX Service Unit.......................................................................................... 2
General Overview ....................................................................................................... 3
Equipment Diagrams................................................................................................... 5
Important Safety Information....................................................................................... 6
Introduction.............................................................................................................. 6
Electrical Safety....................................................................................................... 6
Wet Environment ..................................................................................................... 6
Heavy Equipment .................................................................................................... 6
Chemical Safety ...................................................................................................... 7
Water Borne Hazards .............................................................................................. 7
Description .................................................................................................................. 9
Overview.................................................................................................................. 9
Flow of Material ..................................................................................................... 10
Installation ................................................................................................................. 14
Advisory................................................................................................................. 14
Installation Process ............................................................................................... 14
Operation .................................................................................................................. 18
Operating the Software.......................................................................................... 18
Operating the Equipment....................................................................................... 29
Equipment Specifications.......................................................................................... 34
Overall Dimensions ............................................................................................... 34
Connection to Drain............................................................................................... 34
Ventilation.............................................................................................................. 34
Environmental Conditions...................................................................................... 34
Routine Maintenance ................................................................................................ 36
Responsibility ........................................................................................................ 36
General.................................................................................................................. 36
RCD Test............................................................................................................... 36
ii
Table of Contents
Temperature sensors Calibration .......................................................................... 36
Conductivity probe calibration ............................................................................... 37
Low conductivity Calibration (0-5 mS/cm) ............................................................. 37
Pipe work and connections.................................................................................... 38
Column packing..................................................................................................... 40
Static Premixer Packing ........................................................................................ 43
CEXC sensors fitting ............................................................................................. 44
Laboratory Teaching Exercises................................................................................. 46
Index to Exercises ................................................................................................. 46
Nomenclature ........................................................................................................ 46
Common Theory.................................................................................................... 47
Exercise A - Flow pattern characterisation - Step change ........................................ 49
Exercise B - Flow pattern characterisation - Pulse change....................................... 60
Exercise C - Conversion experiment......................................................................... 69
Contact Details for Further Information ..................................................................... 79
iii
Disclaimer
This document and all the information contained within it is proprietary to Armfield
Limited. This document must not be used for any purpose other than that for which it
is supplied and its contents must not be reproduced, modified, adapted, published,
translated or disclosed to any third party, in whole or in part, without the prior written
permission of Armfield Limited.
Should you have any queries or comments, please contact the Armfield Customer
Support helpdesk (Monday to Friday: 0800 1800 GMT). Contact details are as
follows:
United Kingdom
International
(0) 1425 478781

(calls charged at local rate)
+44 (0) 1425 478781

(international rates apply)
Email: support@armfield.co.uk
Fax: +44 (0) 1425 470916
Copyright and Trademarks

Copyright 2009 Armfield Limited. All rights reserved.
Any technical documentation made available by Armfield Limited is the copyright
work of Armfield Limited and wholly owned by Armfield Limited.
Brands and product names mentioned in this manual may be trademarks or
registered trademarks of their respective companies and are hereby acknowledged.
Use with CEX Service Unit

This instruction manual describes the use of the CEY Plug Flow Reactor in
conjunction with the CEXC Computer Controlled Service Unit.
An alternative instruction manual is available from Armfield that describes the use of
the CEY in conjunction with the CEX Service Unit. Please contact Armfield if a copy
of this instruction manual is required. Contact details are included later in this
document.
General Overview
This instruction manual should be used in conjunction with the manual supplied with
the CEXC Computer Controlled Chemical Reactor Service Unit.
This Manual provides the necessary information for operating the equipment in
conjunction with the CEXC Computer Controlled Chemical Reactor Service Unit, and
for performing a range of Teaching Exercises designed to demonstrate the basic
principles of Chemical Reactors theory and use.
Tubular reactors are often used when continuous operation is required but without
back-mixing of products and reactants. In a tubular reactor, the feed enters at one
end of a cylindrical tube and the product stream leaves at the other end. The long
tube and the lack of provision for stirring prevent complete mixing of the fluid in the
tube. Hence the properties of the flowing stream will vary from one point to another in
both radial and axial directions.
The Armfield CEY-Plug Flow Reactor is an example of an ideal tubular reactor
specially designed to allow detailed study of this important process. It is one of five
reactor types which are interchangeable on the Computer Controlled Reactor Service
Unit (CEXC), the others being CEM MkII - Continuous Stirred Tank Reactor, CET
MkII Tubular Reactor, the new CEB MkIII Transparent Batch Reactor and CEZ
Laminar flow reactor.
Reactions are monitored by conductivity probe as the conductivity of the solution
changes with conversion of the reactants to product. In addition, all the experiments
are followed visually by means of the reactor transparency and the use of colour
indicators in all the experiments.
Armfield Instruction Manual
CEY Plug Flow Reactor
Equipment Diagrams
Figure 1: Front View of Plug Flow Reactor Unit
Figure 2: Top View of Plug Flow Reactor Unit
Important Safety Information

Introduction
All practical work areas and laboratories should be covered by local safety
regulations which must be followed at all times.
It is the responsibility of the owner to ensure that all users are made aware of
relevant local regulations, and that the apparatus is operated in accordance with
those regulations. If requested then Armfield can supply a typical set of standard
laboratory safety rules, but these are guidelines only and should be modified as
required. Supervision of users should be provided whenever appropriate.
Your CEY Plug Flow Reactor Unit has been designed to be safe in use when
installed, operated and maintained in accordance with the instructions in this manual.
As with any piece of sophisticated equipment, dangers exist if the equipment is
misused, mishandled or badly maintained.
Electrical Safety
The equipment described in this Instruction Manual operates from a mains voltage
electrical supply. It must be connected to a supply of the same frequency and voltage
as marked on the equipment or the mains lead. If in doubt, consult a qualified
electrician or contact Armfield.
The equipment must not be operated with any of the panels removed.
To give increased operator protection, the unit incorporates a Residual Current
Device (RCD), alternatively called an Earth Leakage Circuit Breaker, as an integral
part of this equipment. If through misuse or accident the equipment becomes
electrically dangerous, the RCD will switch off the electrical supply and reduce the
severity of any electric shock received by an operator to a level which, under normal
circumstances, will not cause injury to that person.
At least once each month, check that the RCD is operating correctly by pressing the
TEST button. The circuit breaker MUST trip when the button is pressed. Failure to
trip means that the operator is not protected and the equipment must be checked and
repaired by a competent electrician before it is used.
Wet Environment
The equipment requires a header tank containing water. During use it is possible that
there will be some spillage and splashing.
All users should be made aware that they may be splashed while operating
the equipment, and should wear appropriate clothing and non-slip footwear.
Wet Floor warnings should be displayed where appropriate.
Electrical devices in the vicinity of the equipment must be suitable for use in
wet environments or be properly protected from wetting.
Heavy Equipment
This apparatus is heavy.
The apparatus should be placed in a location that is sufficiently strong to

support its weight, as described in the Installation section of the manual.
6
Important Safety Information
Use lifting tackle, where possible, to install the equipment <give specific
instructions>. Where manual lifting is necessary, two or more people may be
required for safety, and all should be made aware of safe lifting techniques to
avoid strained backs, crushed toes, and similar injuries.
Safety shoes and/or gloves should be worn when appropriate.
Chemical Safety
Details of the chemicals intended for use with this equipment are given in the
Operation section. Chemicals purchased by the user are normally supplied with a
COSHH data sheet which provides information on safe handling, health and safety
and other issues. It is important that these guidelines are adhered to.
It is the users responsibility to handle chemicals safely.
Prepare chemicals and operate the equipment in well ventilated areas.
Only use chemicals specified in the equipment manuals and in the

concentrations recommended.
Follow local regulations regarding chemical storage and disposal.
Specific Safety Guidelines:
Indigo Carmine is dangerous and so should be used with the necessary

safety procedures. When handling use of rubber gloves and protection
glasses are strongly recommended.
Ethyl acetate is highly inflammable. Be careful with possible ignition sources,

such as electric current, very hot surfaces or flames. Avoid breathing the ethyl
acetate vapours.
Extreme care should be taken whilst handling either acetic acid or acetic
anhydride. Both chemicals are highly corrosive and care should be taken to
avoid contact or inhalation of vapour.
Water Borne Hazards

The equipment described in this instruction manual involves the use of water, which
under certain conditions can create a health hazard due to infection by harmful
micro-organisms.
For example, the microscopic bacterium called Legionella pneumophila will feed on
any scale, rust, algae or sludge in water and will breed rapidly if the temperature of
water is between 20 and 45C. Any water containing this bacterium which is sprayed
or splashed creating air-borne droplets can produce a form of pneumonia called
Legionnaires Disease which is potentially fatal.
Legionella is not the only harmful micro-organism which can infect water, but it
serves as a useful example of the need for cleanliness.
Under the COSHH regulations, the following precautions must be observed:
Any water contained within the product must not be allowed to stagnate, ie.
the water must be changed regularly.
Any rust, sludge, scale or algae on which micro-organisms can feed must be
removed regularly, i.e. the equipment must be cleaned regularly.
Where practicable the water should be maintained at a temperature below

20C. If this is not practicable then the water should be disinfected if it is safe
and appropriate to do so. Note that other hazards may exist in the handling of
biocides used to disinfect the water.
A scheme should be prepared for preventing or controlling the risk

incorporating all of the actions listed above.
Further details on preventing infection are contained in the publication The Control
of Legionellosis including Legionnaires Disease - Health and Safety Series booklet
HS (G) 70.
Description
Where necessary, refer to the drawings in the Equipment Diagrams section.
Overview
The reactor column is mounted on a stand to allow careful vertical alignment of the
reactor. The CEY should be located close to the CEXC unit to allow connection to the
instrumentation.
The plug flow reactor is an acrylic column with a total volume of 1 L. It is packed with
3 mm glass beads to give plug flow with axial dispersion and improve flow
distribution.
At the bottom of the reactor a static premixer with a total volume of 1.6 ml is located.
It is packed with glass beads of 1.2 mm in diameter to thoroughly mix the reactants
before they enter the reactor.
To avoid movement of the glass beads there are four meshes, which are located at
the ends of the reactor column and the static premixer.
The temperature of materials exiting the column is measured by temperature sensor
(T1) which is fitted into the sensor block and is located at the top of the stand. The
temperature value is displayed on the mimic screen of the CEXC software.
An additional temperature sensor T2 is supplied with the CEXC and can be
monitored. It is not necessary to use the Hot Water Circulator.
The conductivity probe supplied with the CEXC unit is also fitted into this sensor
block allowing the conductivity to be monitored at the exit of the reactor.
The reactor is supplied with a Feed assembly, which is made up of a 6 port injection
valve, PTFE pipe, silicone pipe with smaller diameter and two barbed connectors.
The 6 port valve allows injection of a determined volume of liquid for tracer
experiments.
Sockets on the rear of the service unit provide connections for the conductivity probe
and thermocouple plugs.
Figure 1: CEY reactor
Flow of Material
Reactants are pumped from the reagent bottles to the reactor passing through the 6
port injection valve. See Figure 2.
At the exit of the reactor the stream enters the sensor block where conductivity and
temperature values are monitored and then drained. See Figure 3.
10
Description
Figure 2: Flow of material circuit
It is recommended to place the Plug flow reactor close to CEXC plinth in order to
simplify the sensor connections and shorten the reactants path.
11
Figure 3: Flow Exit Reactor
Injection valve operation

The injection valve has 6 ports and two positions. In one position adjacent ports are
linked together inside the valve so that there are 3 pairs of linked ports. Changing the
position of the valve links the alternate port pair together (Figure 4.2). The function of
the valve is to inject the tracer solution (colourful solution) in a defined volume ratio.
This is achieved by using a tracer solution loop of defined lengths (230 cm for a
volume of 10 ml).
When the injection valve is in the load position (Figure 4.1) the tracer solution loop is
filled. Tracer solution passes out of the injection valve and it is recirculated. Carrier
liquid (water) is directed to the reactor.
When the injection valve is switched to the injection position (Figure 4.2) the carrier
liquid (water) picks up the volume of the tracer solution (dye) contained in the loop
and passes it to the reactor.
12
Description
Figure 4.1 and 4.2: Injection valve positions
Figure 5: Injection Flow Assembly (FIA)
13
Installation
Advisory
Before operating the equipment, it must be unpacked, assembled and installed as
described in the steps that follow. Safe use of the equipment depends on following
the correct installation procedure.
Installation Process
Locate the CEXC unit in the desired location, on a steady workbench.
Mount the 6 port injection valve assembly on to the CEXC using the two locating
studs and the black thumbnuts. Position the valve on the left hand side of the base.
Position the reagent bottles in the channel through the unit.
Locate the CEY reactor unit close to the CEXC unit.
Change the silicone tubing on both sides of the CEXC peristaltic pumps for the new
Silicone tubing (smaller diameter).
Tubing on the left side of each feed pump is fitted into the bottles as shown. Tubing
on the right side is connected to the corresponding ports of the valve through the
barbed connector supplied.
If connections to the 6 port valve are necessary see below:
14
Installation
Note: Changing the length of the Loop changes the volume of tracer injected into the
column.
Check that the two solutions follow two different circuits:
Circuit 1(for water): Bottle 1- enter valve- exit valve- reactor.
Circuit 2(Tracer): Bottle 2-enter valve enter Loop (exit valve) Exit Loop
(enter valve) Exit valve.
Fit the CEXC conductivity sensor into the gland in the sensor block of the reactor unit
(bottom channel of the sensor block).
Fit the CEXC temperature sensor into the other gland on the sensor block (top
channel of the sensor).
Sensors should be inserted as described in CEXC sensors fitting.
15
Connect the conductivity probe and temperature sensor (T1) plugs to the sockets at
the rear of the service unit.
Check that the voltage specified on the equipment matches the supply voltage.
Note: this unit must be earthed.
Connect the power socket at the rear of the plinth to a suitable mains electricity
supply.
Ensure that the circuit breakers and RCD are switched to ON (up).
The on/off switch for the apparatus is located on the orange panel on the front of the
plinth.
Switch on the apparatus.
Connect CEXC to a PC using the USB cable supplied.
Insert the CEY software CD-ROM into the CD-R drive of a suitable PC. The
installation program should auto run. If it does not, select Run... from your Start
menu, type run d:\setup where d is the letter of your CD-ROM drive.
16
Installation
Follow the instructions on screen.

Run the software.
The basic operation of the CEY has been confirmed. Refer to the Operation section
for further information.
17
Operation
Where necessary, refer to the drawings in the Equipment Diagrams section.
The apparatus must be set up in accordance with the Installation section.
Additionally, ensure that you have read the Important Safety Information at the
beginning of this manual.
Operating the Software

Note: The diagrams in this section are included as typical examples and may not
relate specifically to the individual product described in this instruction manual.
The Armfield Software is a powerful Educational and Data Logging tool with a wide
range of features. Some of the major features are highlighted below, to assist users,
but full details on the software and how to use it are provided in the presentations
and Help text incorporated in the Software. Help on Using the Software or Using the
Equipment is available by clicking the appropriate topic in the Help drop-down menu
from the upper toolbar when operating the software as shown:
Before operating the software ensure that the equipment has been connected to the
IFD5 Interface (where IFD5 is separate from the equipment) and the IFD5 has been
connected to a suitable PC using a USB lead. For further information on these
actions refer to the Operation manual.
Load the software. If multiple experiments are available then a menu will be
displayed listing the options. Wait for the presentation screen to open fully as shown:
Before proceeding to operate the software ensure that IFD: OK is displayed at the
bottom of the screen. If IFD:ERROR is displayed check the USB connection between
18
Operation
the IFD5 and the PC and confirm that the red and green LEDs are both illuminated.
If the problem persists then check that the driver is installed correctly (refer to the
Operation manual).
Presentation Screen - Basics and Navigation

As stated above, the software starts with the Presentation Screen displayed. The
user is met by a simple presentation which gives them an overview of the capabilities
of the equipment and software and explains in simple terms how to navigate around
the software and summarizes the major facilities complete with direct links to detailed
context sensitive help texts.
To view the presentations click Next or click the required topic in the left hand pane
as appropriate. Click More while displaying any of the topics to display a Help index
related to that topic.
To return to the Presentation screen at any time click the View Presentation icon
from the main tool bar or click Presentation from the dropdown menu as
shown:
For more detailed information about the presentations refer to the Help available via
the upper toolbar when operating the software.
Toolbar
A toolbar is displayed at the top of the screen at all times, so users can jump
immediately to the facility they require, as shown:
The upper menu expands as a dropdown menu when the cursor is placed over a
name.
The lower row of icons (standard for all Armfield Software) allows a particular
function to be selected. To aid recognition, pop-up text names appear when the
cursor is placed over the icon.
Mimic Diagram
The Mimic Diagram is the most commonly used screen and gives a pictorial
representation of the equipment, with continuously updated display boxes for all the
various sensor readings, calculated variables etc. directly in engineering units.
19
To view the Mimic Diagram click the View Diagram icon

from the main tool bar
or click Diagram from the View drop-down menu as shown:
A Mimic diagram is displayed, similar to the diagram as shown:
20
Operation
The details in the diagram will vary depending on the equipment chosen if multiple
experiments are available.
21

In addition to measured variables such as Temperature, Pressure and Flowrate (from
a direct reading flowmeter), calculated data such as Motor Torque, Motor Speed and
Discharge / Volume flowrate (from pressure drop across an orifice plate) are
continuously displayed in data boxes with a white background. These are
automatically updated and cannot be changed by the user.
Manual data input boxes with a coloured background allow constants such as Orifice
Cd and Atmospheric Pressure to be changed by over-typing the default value, if
required.
The data boxes associated with some pressure sensors include a Zero button
alongside. This button is used to compensate for any drift in the zero value, which is
an inherent characteristic of pressure sensors. Pressing the Zero button just before
starting a set of readings resets the zero measurement and allows accurate pressure
measurements to be taken referenced to atmospheric pressure. This action must be
carried out before the motor is switched on otherwise the pressure readings will be
offset.
The mimic diagram associated with some products includes the facility to select
different experiments or different accessories, usually on the left hand side of the
screen, as shown:
Clicking on the appropriate accessory or exercise will change the associated mimic
diagram, table, graphs etc to suit the exercise being performed.
Control Facilities in the Mimic Diagram

A Power On button allows the motor to be switched off or on as required. The button
always defaults to off at startup. Clicking this button switches the power on (1) and off
(0) alternately.
A box marked Motor Setting allows the speed of the motor to be varied from 0 to
100% either stepwise, by typing in values, or using the up / down arrows as
appropriate. It is usual to operate the equipment with the motor initially set to 100%,
22
Operation
then reduce the setting as required to investigate the effect of reduced speed on
performance of the equipment.
When the software and hardware are functioning correctly together, the green LED
marked Watchdog Enabled will alternate On and Off. If the Watchdog stops
alternating then this indicates a loss of communication between the hardware and
software that must be investigated.
Details on the operation of any automatic PID Control loops in the software are
included later in this section.
Data Logging Facilities in the Mimic Diagram

There are two types of sampling available in the software, namely Automatic or
Manual. In Automatic logging, samples are taken regularly at a preset but variable
interval. In Manual logging, a single set of samples is taken only when requested by
the operator (useful when conditions have to be changed and the equipment allowed
to stabilize at a new condition before taking a set of readings).
The type of logging will default to manual or automatic logging as appropriate to the
type of product being operated.
Manual logging is selected when obtaining performance data from a machine where
conditions need to stabilize after changing appropriate settings. To record a set of set
of data values from each of the measurement sensors click the
main toolbar. One set of data will be recorded each time the
icon from the

icon is clicked.
Automatic logging is selected when transients need to be recorded so that they can
be plotted against time. Click the
the
icon from the toolbar to start recording, click
icon from the toolbar to stop recording.
The type of logging can be configured by clicking Configure in the Sample dropdown menu from the upper toolbar as shown:
In addition to the choice of Manual or Automatic sampling, the parameters for

Automatic sampling can also be set. Namely, the time interval between samples can
be set to the required number of minutes or seconds. Continuous sampling can be
selected, with no time limit or sampling for a fixed duration can be set to the required
number of hours, minutes or seconds as shown:
23
Tabular Display
To view the Table screen click the View Table icon
click Table from the View dropdown menu as shown:
from the main tool bar or
The data is displayed in a tabular format, similar to the screen as shown:
24
Operation
As the data is sampled, it is stored in spreadsheet format, updated each time the
data is sampled. The table also contains columns for the calculated values.
New sheets can be added to the spreadsheet for different data runs by clicking the
icon from the main toolbar. Sheets can be renamed by double clicking on the
sheet name at the bottom left corner of the screen (initially Run 1, Run 2 etc) then
entering the required name.
For more detailed information about Data Logging and changing the settings within
the software refer to the Help available via the upper toolbar when operating the
software.
Graphical Display
When several samples have been recorded, they can be viewed in graphical format.
from the main
To view the data in Graphical format click the View graph icon
tool bar or click Graph from the View drop-down menu as shown:
25

The results are displayed in a graphical format as shown:
(The actual graph displayed will depend on the product selected and the exercise
that is being conducted, the data that has been logged and the parameter(s) that has
been selected).
Powerful and flexible graph plotting tools are available in the software, allowing the
user full choice over what is displayed, including dual y axes, points or lines,
displaying data from different runs, etc. Formatting and scaling is done automatically
by default, but can be changed manually if required.
To change the data displayed on the Graph click Graph Data from the Format
dropdown menu as shown:
The available parameters (Series of data) are displayed in the left hand pane as
shown:
26
Operation
Two axes are available for plotting, allowing series with different scaling to be
presented on the same x axis.
To select a series for plotting, click the appropriate series in the left pane so that it is
highlighted then click the appropriate right-facing arrow to move the series into one of
the windows in the right hand pane. Multiple series with the same scaling can be
plotted simultaneously by moving them all into the same window in the right pane.
To remove a series from the graph, click the appropriate series in the right pane so
that it is highlighted then click the appropriate left-facing arrow to move the series into
the left pane.
The X-Axis Content is chosen by default to suit the exercise. The content can be
changed if appropriate by opening the drop down menu at the top of the window.
The format of the graphs, scaling of the axes etc. can be changed if required by
clicking Graph in the Format drop-down menu as shown:
For more detailed information about changing these settings refer to the Help
available via the upper toolbar when operating the software.
PID Control
Where appropriate, the software associated with some products will include a single
or multiple PID control loops whereby a function on the product can be manually or
27

automatically controlled using the PC by measuring an appropriate variable and
varying a function such as a heater power or pump speed.
The PID loop can be accessed by clicking the box labelled PID or Control depending
on the particular software:
A PID screen is then displayed as shown:
The Mode of operation always defaults to Manual control and 0% output when the
software is loaded to ensure safe operation of the equipment. If appropriate, the
operator can retain manual operation and simply vary the value from 0 to 100% in the
Manual Output box, then clicking Apply.
Alternatively, the PID loop can be changed to Automatic operation by clicking the
Automatic button. If any of the PID settings need to be changed from the default
values then these should be adjusted individually before clicking the Apply button.
28
Operation
The controller can be restored to manual operation at any time by clicking the
Manual button. The value in the Manual Output box can be changed as required
before clicking the Apply button.
Settings associated with Automatic Operation such as the Setpoint, Proportional
Band, Integral Time, Derivative Time and Cycle Time (if appropriate) can be
changed by the operator as required before clicking the Apply button.
Clicking Calculations displays the calculations associated with the PID loop to aid
understanding and optimization of the loop when changing settings as shown:
Clicking Settings returns the screen to the PID settings.

Clicking OK closes the PID screen but leaves the loop running in the background.
In some instances the Process Variable, Control variable and Control Action can
be varied to suit different exercises, however, in most instances these boxes are
locked to suit a particular exercise. Where the variables can be changed the options
available can be selected via a drop-down menu.
Advanced Features
The software incorporates advanced features such as the facility to recalibrate the
sensor inputs from within the software without resorting to electrical adjustments of
the hardware. For more detailed information about these advanced functions within
the software refer to the Help available via the upper toolbar when operating the
software.
Operating the Equipment

Switching on the Unit
The unit is switched on using the switch on the front of the unit. The circuit breakers
and RCD device located at the rear of the unit should be turned on beforehand. Both
the temperature controller and conductivity display should illuminate.
29
Filling the feed bottles

Lift the feed bottle lids and pour solutions in from above.
Operation of Data Logger and Software

The Tubular Reactor is controlled using the CEY software supplied, which allows
real-time monitoring and data logging of all sensor outputs and control of the heater
unit and pumps. Recorded results can be displayed in tabular and graph format. The
software runs on a WindowsTM PC which connects to the CEXC using a USB
interface.
Installation of the software is described in the Installation Guide, and the software
must be installed before connecting the PC to the CEXC. The software may then be
run from the Start menu (Start > Programs > Armfield Chemical Reactor Software >
CEY).
Operation of the software is described in a walkthrough presentation within the
software, and also in the online Help Text accessible via the software Help menu.
Operation and setting of specific controls is also provided within the experiments
described in this manual.
Mimic Diagram and software

The equipment is usually controlled from the Mimic Diagram screen in the software.
This shows all the sensor outputs, and controls for the pumps. There is an extra
temperature sensor T3 and Low conductivity plugs with outputs on the software for
extra connections made by the user.
30
Operation
31
Feed pump speeds are controlled using up/down arrows or typing the flow rate in a
value between 0 and the maximum ml/min. Click on the appropriate POWER ON
symbol to start up the pumps.
Concentration values must be typed in on each experiment so that the software will
carry out the subsequent calculations.
Conductivity and temperature values will be monitored on the screen and the data
logged when GO is clicked.
The software also automatically generates a series of Watchdog pulses, required by
the plc, ensuring that the hardware shuts down safely in case of a software or
communications failure.
Operating Plug Flow Reactor

There are two modes of operation with the CEY Plug flow reactor: tracer experiment
and conversion experiment operation. The type of experiment performed defines the
operational layout. When tracer experiments take place, one solution is injected into
the reactor after another. However, when conversion experiment takes place two
solutions are injected into the reactor at the same time so that a T- connector is
necessary.
When performing experiments follow the experimental layouts described in each
exercise.
32
Operation
Operational Layout for tracer experiments
Overall Process
Having reviewed the components of the CEY it is worthwhile considering the process
as a whole.
The feed pump delivers the feed to the injection valve assembly. All the connections
should be set so that each solution passes through the correct port of the injection
valve and is delivered to the reactor or back to the vessel.
In the teaching exercises section each experiment fully describes the required
connections.
Air bubbles in the reactor column

Bubbles should not be allowed to enter the reactor column since this will have a
negative effect on performance. Care should be taken not to pump any bubbles into
the column.
If any bubbles enter the column before the tracer solution is injected, continue flowing
water into the reactor until all bubbles are gone. However, if a bubble enters the
reactor when the tracer solution has been injected, the experiment has to be
restarted since flow distribution will be affected and so will conductivity values.
33
Equipment Specifications
Overall Dimensions
Reactor Unit:
Height:
1381 cm
Width:
859 cm
Depth:
330 cm
Reactor dimensions:
Reactor column:
Total length:
1044 mm
Internal diameter:
34 mm
External diameter:
40 mm
Total volume column: 0.919 dm3

Pre mixer cylinder:
Length
42 mm
Diameter internal
8.65 mm
Diameter external
20 mm
Connection to Drain
Water exiting the equipment should be directed to a suitable drain capable of
accepting volumes of up to 90 ml/min at temperatures not greater than room
temperature.
The chemical solutions used in each experiment at the required concentration should
be directed to a suitable drain capable of accepting volumes of up to 90 ml/min at
room temperature.
Ventilation
For optimum results it is advisable to operate the reactor column in a ventilated
environment at a room temperature up to 25C.
Environmental Conditions
This equipment has been designed for operation in the following environmental
conditions. Operation outside of these conditions may result reduced performance,
damage to the equipment or hazard to the operator.
a. Indoor use;
b. Altitude up to 2000 m;
c. Temperature 5 C to 40 C;
34
Equipment Specifications
d. Maximum relative humidity 80 % for temperatures up to 31 C, decreasing
linearly to 50 % relative humidity at 40 C;
e. Mains supply voltage fluctuations up to 10 % of the nominal voltage;
f.
Transient over-voltages typically present on the MAINS supply;

NOTE: The normal level of transient over-voltages is impulse withstand (overvoltage) category II of IEC 60364-4-443;
g. Pollution degree 2.
Normally only nonconductive pollution occurs.
Temporary conductivity caused by condensation is to be expected.
Typical of an office or laboratory environment
35
Routine Maintenance
Responsibility
To preserve the life and efficient operation of the equipment it is important that the
equipment is properly maintained. Regular maintenance of the equipment is the
responsibility of the end user and must be performed by qualified personnel who
understand the operation of the equipment.
General
The equipment should be disconnected from the electrical supply when not in use.
After use the feed bottles, reactor vessel, sump tray and pipework should be washed
through with water to remove chemical residues, and then drained.
RCD Test
Test the RCD by pressing the TEST button at least once a month. If the RCD button
does not trip when the Test button is pressed then the equipment must not be used
and should be checked by a competent electrician.
Temperature sensors Calibration

The temperature sensors are calibrated before delivery and should not require recalibration. However, should calibration become necessary use the following
procedure. This should only be done once the unit has fully warmed up.
Connect CEXC service unit to a PC and start up the Armfield software. Open mimic
diagram screen where T1, T2 and T3 windows are displayed.
The temperature conditioning circuit (which provides the reading from the
thermocouples supplied with the CEXC service unit) is located on a printed circuit
board (PCB) inside the plinth on the right-hand side. However, should re-calibration
become necessary the appropriate calibration potentiometers can be located using
the diagram given in the CEXC manual (Routine Maintenance).
Ensure the equipment has been connected to the electrical supply and switched on
for at least 20 minutes. Start up the Armfield software for the specific reactor. To
access the PCB remove the panel on the right hand side of the plinth by removing
the four fixing screws.
If a thermocouple calibrator is available:
Connect Thermocouple calibrator simulator to T1 input socket, located at the rear of
the plinth. Set to 25C and adjust VR1 (T1 ZERO) and VR2 (T1 SPAN) on the PCB
to give 25C displayed on PC. Check accuracy at 15 and 40C.
Repeat the same procedure for T2 by adjusting VR3 (T2 ZERO) and VR4 (T2 SPAN)
on the PCB to give 25C displayed on PC, and VR5 (T3 ZERO) and VR6 (T3 SPAN)
for T3 (if an extra thermocouple is used).
If a thermocouple calibrator is not available:
Temperature sensor T1, T2 and T3 should be dipped into crushed ice, and then
adjust the ZEROS to give 0C, then sensors should be dipped into boiling water and
then adjust the SPANS to 100C.
36
Routine Maintenance
When the conditioning circuit has been re-calibrated, replace the front panel of the
electrical console and re-install the sensors in the appropriate place on the CEXC
service unit.
Conductivity probe calibration

The conductivity conditioning circuit (which provides the reading from the conductivity
probe supplied with the CEXC service unit) is located on a printed circuit board inside
the plinth on the right-hand side. This circuit is calibrated before despatch and should
not require re-calibration. However, should re-calibration become necessary the
appropriate calibration potentiometers can be located using the diagram given in the
CEXC manual (Routine Maintenance).
Ensure the equipment has been connected to the electrical supply and switched on
for at least 20 minutes. Start up the Armfield software for the specific reactor. To
access the PCB remove the panel on the right hand side of the plinth by removing
the four fixing screws.
Disconnect the conductivity probe from the socket at the back of the plinth. Connect
an AC Voltmeter (Range AC mV) to pins 1 and 2 of the vacant socket and adjust
potentiometer VR10 on the PCB to give a reading of 50 mV (RMS) on the Voltmeter
(probe excitation voltage).
Disconnect the Voltmeter then reconnect the probe to the socket having removed the
probe from the appropriate reactor fitted to the CEXC.
Note that there are two, High Cond and Low Cond sockets. Connect the probe to
the one which is going to be calibrated and read the conductivity value in the right
window on the software.
High conductivity Calibration (0-20 mS/cm)

Fill a small beaker with a Conductivity standard solution (e.g. 0.1M KCI giving a
conductivity of 12.88 mS at 25C) and measure the temperature of the standard
solution using a suitable thermometer. From the table supplied determine the actual
conductivity of the solution at the measured temperature.
Immerse the probe into the Conductivity standard solution in the beaker then adjust
potentiometer VR7 to give a reading of the standard solution in the High conductivity
box on the software to match the conductivity.
Low conductivity Calibration (0-5 mS/cm)

Fill a small beaker with a Conductivity standard solution (e.g. 0.01M KCI giving a
conductivity of 1.41mS at 25C) and measure the temperature of the standard
solution using a suitable thermometer. From the table supplied determine the actual
conductivity of the solution at the measured temperature.
Immerse the probe into the Conductivity standard solution in the beaker then adjust
potentiometer VR8 to give a reading of the Standard solution in the Low conductivity
box on the software.
When the conditioning circuit has been re-calibrated replace the panel and re-install
the probe in the appropriate reactor on the CEXC service unit.
37
12.88 mS/cm at 25C 0.1 M KCl

C
mS/cm
mS/cm
8.22
20
11.67
10
9.33
21
11.91
15
10.48
22
12.15
16
10.72
23
12.39
17
10.95
24
12.64
18
11.19
25
12.88
19
11.43
26
13.13
1.413 mS/cm at 25C 0.01 M KCl

C
mS/cm
mS/cm
0.896
20
1.278
10
1.02
21
1.305
15
1.147
22
1.332
16
1.173
23
1.359
17
1.199
24
1.386
18
1.225
25
1.413
19
1.251
26
1.441
Pipe work and connections

The CEY pipework is mainly hard walled Teflon tubing (4 mm o.d., 2.5 mm i.d.).
However for peristaltic pumps soft walled tubing is used. Two basic types of
connectors are used: reducing connectors for soft walled tubing connected to hard
walled tubing (see below) and silicone pipe to connect barbed connector from 6-port
injection valve to Teflon pipe. This allows simple connection and disconnection as
required.
38
Routine Maintenance
Connecting hard walled to soft walled tubing
The CEY is supplied with all pipework and connections in place, however there may
be an instance when the user wishes to alter the arrangement.
The barbed adaptors used on the 6-port injection valve remain connected. The only
connection that maybe required is Teflon pipe with the injection valve, and this must
be done using a piece of silicone pipe (see below).
Pipework connections with Injection valve
Any extra connection between hard walled Teflon tubing can be done using a piece
of silicone tube with the same inner diameter as that provided with the equipment.
Connection to reactor fittings

Quick connectors are found in every connection between Teflon pipe and reactor
unit. These connections are located at the inlet and outlet of the column reactor, and
at the inlet and outlet of the sensor block.
39
Column quick connectors
These connectors are made up of two parts; the body, which is screwed into the
reactor, and cap which is connected to the Teflon pipe.
Two steps comprise the connection;
1. Push cap against body until it clicks
2. Screw cap connector until sealed
Connections with quick connectors
Column packing
CEY column should be provided already packed. However, if packing or unpacking
should be necessary follow the below procedure.
40
Routine Maintenance
Plug flow reactor assembly
Unpacking
1. Disconnect CEXC unit from the electrical supply
2. Disconnect pipe and sensors from CEXC unit which are connected to the reactor
unit (PTFE tubing, T1 and Conductivity plugs) so that the reactor unit can be moved
3. Disconnect pipe which goes from the reactor exit to sensor block
4. Unscrew the head screw so that the top bracket will come loose from the stand
and also the top of the reactor. Do not unscrew the 6 screws from the top reactor
5. Unscrew the six screws from the bottom and do not take the lid off from the
column until required
6. Keeping the lid on to avoid dropping glass beads, turn the reactor around so that
the bottom becomes the top of the reactor and vice versa
7. Remove the lid, the mesh and the O-ring and keep them safe. See below.
8. Empty the reactor
41
Packing column
Initial procedure if column is not packed

1. Follow the same procedure as described above until point 4
2. Unscrew the six bottom screws and remove the lid
3. Turn the reactor around so that the bottom becomes the top and vice versa. See
Packing Column above.
Packing:
4. Once initial procedure has been done, fill the reactor with water blocking the other
end so that it does not drain. The glass beads will gently settle.
5. Once column is filled with water, start filling in with the 3 mm glass beads.
Then, start the reassembly:
6. Unblock lower part of the reactor emptying the water
7. Replace the mesh and o-ring
8. Replace the lid and hold it close to the reactor so as not to spill glass beads
9. Turn the reactor down to its normal position
42
Routine Maintenance
10. Place it over the bottom bracket matching the holes of the reactor column and lid
11. Tighten the six bottom screws so that the bottom part of the reactor is fixed
12. Tighten the head screw so that the top part of the reactor is fixed
Static Premixer Packing
Static Premixer
Packing/unpacking
1. Disconnect pipe connected to the premixer from the reactor column
2. Remove the premixer the reactor
3. Remove the o-ring
4. Unscrew the fitting which connects the reactor column with the premixer
5. Remove the mesh
6. Make sure that at the bottom of the premixer there is a small mesh
7. Fill up the premixer with water keeping the other side blocked so that it does not
drain
8. Fill the premixer with 1.3 mm diameter glass beads and leave sufficient room to fit
the quick connector
9. Replace the mesh and refit the quick connector
43

10. Replace the o-ring and refit the premixer into the bottom of the reactor column
CEXC sensors fitting
Sensor block parts and fitting
It is recommended to place the CEY reactor close to CEXC plinth in order to simplify
the sensor connections and shorten the reactants path.
Note that CEXC is supplied with two temperature sensors. T1 is usually fitted in each
reactor, and T2 is fitted in the Hot water Circulator (HWC). However the HWC is not
required for the experiments with this reactor.
Temperature sensor (T1) connection

The procedure for fitting the sensor is as follows:
Unscrew gland T1
Handling carefully the temperature sensor, pass it through the gland and fit it
into its corresponding hole.
Push the sensor down to the end of the channel so that the detecting part is
in the flow path.
Then pull the probe back a few mm to allow the flow to pass through the path.
Re-tighten the gland in order to seal.
Conductivity sensor (CS) connection

Be careful handling the conductivity probe since the glass part is very fragile.
When fitting sensor use following procedure:
44
Unscrew cable gland CS
Handling the conductivity sensor carefully, pass it through the cable gland
and fit it into its corresponding channel so that the two holes at the end of the
Routine Maintenance
probe are positioned inline with entrance and exit of the sensor block and not
towards the walls.
For experiments described in this manual, high conductivity values are monitored (020mS/cm). However if other solutions are used with lower conductivity values (0-5
mS/cm), connect the conductivity probe to Low cond. socket and monitor the
reading on the Low cond window.
It is IMPORTANT to fit the probe into the sensor block as described above so that the
two holes of the conductivity probe will be open to the flow. Otherwise the flow will be
blocked by the conductivity probe and the conductivity values will not be accurate.
Once the conductivity sensor is correctly positioned then retighten the gland in order
to seal.
45
Laboratory Teaching Exercises

Index to Exercises
Exercise A - Flow pattern characterisation - Step change
Exercise B - Flow pattern characterisation - Pulse change
Exercise C - Conversion experiment
Nomenclature
Symbol
Name
Unit
C NaOH0
sodium hydroxide initial conc. in

(mol/dm3)
mixed feed
C NaOH (t)
sodium hydroxide conc. in

reactor at time t
(mol/dm3)
sodium hydroxide conc. in

reactor after
time
(mol/dm3)
C0
Tracer concentration
specific rate constant
overall length of tubular reactor (cm)
cross sectional area of tubular

reactor
reaction rate
tR
residence time
(s)
elapsed time
(s)
reactor temperature
(K)
volume of reactor
(dm3)
Pe
Peclet number
Tau, space time
X NaOH
conversion of sodium hydroxide

conductivity at time t
(cm2)
(s)
(Siemens/cm)
initial conductivity
46
Laboratory Teaching Exercises
conductivity at
time
sodium hydroxide conductivity
Arrhenius frequency factor
Ea
activation energy
(J/mol)
gas constant
(J/mol K)
E(t)
residence time distribution

function
Initial mixing proportion =

C B0 /C A0
D ax
Axial dispersion
Common Theory
The Armfield CEY Plug flow reactor is designed to demonstrate the mechanism of
chemical reactions in continuous flowing systems and also to obtain the flow pattern
by using tracer experiments. A tubular reactor packed with glass beads has a
Residence Time Distribution that is very similar to that of a plug flow reactor, but with
some axial dispersion.
Two experiments demonstrate the flow pattern by means of tracer techniques and
the calculation of the RTD. Another experiment demonstrates the steady state
conversion of a second order reaction in a tubular reactor packed with glass beads.
Although it may be possible to carry out demonstrations using other chemicals it is
not advisable without first contacting Armfield as the materials of construction of the
reactor may not be compatible.
DILUTION OF POTASSIUM CHLORIDE AND INDIGO CARMINE FOR USE

WITH TRACER TECHNIQUES
0.1M solution of Potassium Chloride containing 0.01% w/w of Indigo carmine
This should be made by dissolving potassium chloride as follows:
Mass of Indigo Carmine =
47

Then, weight 7.459 g. of KCl and 0.1 g of IC and dissolve it in distilled water up to 1
litre
Follow the same procedure for 1 M solution:
If the necessary volume is 150 cm3,
For Indigo Carmine solution at determined % (w/w) respect to the potassium chloride
solution, make up as follows:
Then, weight 11.18gr of KCl and 0.15 gr of IC and dissolve it in distilled water up to
150 cm3
DILUTION OF ETHYL ACETATE AND SODIUM HYDROXIDE FOR USE

WITH REACTION EXPERIMENT
0.25 M solution of Ethyl Acetate containing 0.01% w/w of IC
This should be made by diluting concentrated Ethyl Acetate as follows:
As explained before, the indigo carmine at determined concentration C% (w/w)

respect to the concentrate should be diluted as follows:
1 L of 0.2 M solution of 1 M Sodium Hydroxide
Then, in order to obtain a solution 0.2 M from a 1M NaOH solution, measure 0.2 litres
of 1M NaOH and add distilled water until 1 litre.
48
Exercise A - Flow pattern characterisation - Step change

Objective
The aim of this practical exercise is to study the flow pattern characterisation of a
tubular reactor packed with glass beads. This characterisation will be performed
using a model considering a plug-flow reactor with axial dispersion and by
determination of the Residence Time Distribution, RTD.
Method
The study of the flow pattern in a reactor is usually done by using tracer techniques
which consist of injecting several perturbations in the inlet reactor and waiting for its
response. The commonly used perturbations in a plug flow reactor are a Pulse
change and Step change. Coloured tracer solution is used in order to make the
propagation of the concentration wave visible.
In this exercise the Step change as a perturbation is studied.
Equipment Required
Armfield service unit CEXC
Armfield Plug Flow reactor unit CEY
Compatible PC with Armfield software
Chemicals
Distilled water
Potassium Chloride
Indigo carmine
Theory
The flow characterisation of a reactor is done by the determination of the RTD, which
is obtained using tracer techniques. The RTD curve allows us to obtain the
permanence of each fraction of volume of fluid inside the reactor and also to
demonstrate its behaviour, ideal or not ideal.
Tracer techniques use several perturbations in the inlet of the reactor and wait for the
reactor response. The most common perturbations used in a plug flow reactor are
the named Step change and Pulse change. The perturbations use tracer solutions
containing a detectable solution which can be detected and therefore followed. This
allows the full comprehension of the reactor behaviour.
In this experiment the tracer solution is made up of a salt, therefore detectable by
conductivity measurement, and a dye, which allows it to be followed visually.
Step change
Step input or step change consists of an instant change in concentration of the tracer
from one concentration to another.
49
The response of the reactor is mathematically represented by the following function:

C(t) = C 0 [1-H(t-0)]
(1)
(H) = Heaviside function

The RTD equation for plug flow with axial dispersion, considering a semi infinite
reactor;
(2)
Integration of these equations gives the curve named Danckwerts curve P(t), reactor
response to a Step change of C(t) = C 0 [1-H(t-0)] at the inlet concentration:
(3)
for a plug flow reactor,
(4)
C: concentration at the reactor outlet
C 0 : the initial concentration (tracer concentration)
Pe: Peclet number
: Dirac delta function
Then, by this change in concentration, experimentally, one has access to the P curve
which allows the determination of the RTD:
50
Exercise A
(5)
For an ideal reactor in general, closed to the diffusion and in steady state conditions,
and for an axially-dispersed plug flow reactor in particular, the mean residence time,
, is equal to the space-time, , i.e., the ratio between the useful reactor volume V
and the feed flow rate
follows:
. Therefore, equation (2) can be written as
(6)
The axially-dispersed plug flow model has two parameters in the E(t) curve: , Pe.
Peclet number is a parameter used to measure the behaviour of a chemical reactor.
It is used as a correlation parameter which takes into account the axial dispersion
model. When Pe = axial dispersion does not exit and the reactor behaves as an
ideal plug flow reactor. When Pe number decreases some axial dispersion appears.
When the tendency is Pe = 0 the residence time distribution (RTD) is wider and the
reactor behaves as stirred tank reactor.
Those two parameters are obtained by minimising the square of the residuals relative
to the experimental curve. This is explained in detail in the results treatment section
The normalisation of the concentration C/C 0 is obtained experimentally by recording
the conductivity values during experiment, since conductivity of a solution varies
linearly with the concentration.
Experiment set up
Re-arrange the experimental assembly in accordance with the following:
51
Layout Step experiment
Verify the directional process of the six port injection valve by following the labels.
Ensure there is enough volume of solutions made to the correct concentrations and
they are well mixed.
Ensure pumps are calibrated and they give the right flow rate
The T connector supplied with the reactor unit is used in this case. Connect it to the
entrance of the reactor. The PTFE pipe, which comes with the T connector, has to be
connected to the right port of the injection valve. See Installation section for valve
connections.
Temperature and conductivity sensors have to be correctly fitted in accordance with
CEXC sensors fitting section and plugged in the right socket at the rear of the CEXC
service Unit.
As the experiment involves the collection and storage sensors data, the USB port
located on the right hand side of the plinth must be connected to the Armfield IFD
data logger. This will enable data logging of conductivity, flow rates and temperature
at selected time intervals over a selected period.
Procedure
Make up 1 litre of 0.1 M Potassium Chloride containing 0.01% of Indigo Carmine.
The procedure on how to make the solutions is given in the introduction of this
section.
IMPORTANT: It is essential when handling these chemicals to wear protective
clothing, gloves and safety spectacles.
Remove the lids of the reagent bottles and carefully fill bottle 1 with the tracer
solution, and bottle 2 with 2 litres of water. Refit the lids.
Arrange the experimental assembly in accordance with Experiment set up above.
52
Exercise A
Set data collection of conductivity at 3 seconds on the software.
Collection of data should continue until steady state conditions are reached in the
reactor. This takes approximately 30 minutes.
Take the feed pipe from the reagent bottle 2 and introduce it into reagent bottle 1, so
that both pumps pump the same solution into the reactor.
Type the flow rate in the software 50 ml/min in each window for each pump so that
the total flow rate of the solution entering the reactor will be 100 ml/min.
Switch on the pumps by pressing POWER ON and instigate the data logger program
(or begin taking readings if computer is being used) by pressing GO.
Take note of the time the solution takes to reach the reactor (column) and the time
taken from the exit of the reactor solution takes until detector. The recorded times will
allow estimation of the reactor space time and the space time in the connection
tubes.
Check whether the solution conductivity corresponds to its concentration and start
the conductivity data acquisition, otherwise try to identify and solve the problem.
Start the conductivity data acquisition in the computer.
Turn off the peristaltic pump and change the tubes from vessel 1 to vessel 2 with
water and turn on the pump again, taking note of the time at which this change has
been done.
Take note of the temperature at the exit stream at the beginning, in the middle, and
the end of the experiment.
Solution is pumped from reagent bottles to injection valve and hence to the reactor.
At the exit the solution is directed to the sensor block where conductivity probe is
fitted and conductivity values are continuously registered.
When the conductivity logged is 0.00 mS/cm2, stop the experiment and the pump.
Flow more distilled water to clean the reactor.
Empty the reactor by means of inverting the pump tubes and connected the pumps
will suck the water out from the reactor.
Notes:
1. Check if the peristaltic pumps tubes have the flexibility and position required to a
keep a constant flow rate. It is recommended to check the flow rate sometimes by
measuring it at the exit of the conductivity probe.
2. Rinse the feed bottles with distilled 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.
Results treatment
Make up a table with the values of your experiment as follows:
53

Useful volume reactor (ml)
372
Flowrate (ml/s)
1.76
Residence time (s)

Pe
tau (V/Fr) (s)
210.00
Tubes time (s)
16.63
SQD
Flowrate and reactor volume are parameters of the experiment. The tubes time as
explained on the experimental procedure is the time taken by the solution travelling
through the connection tubes before and after reactor column until it reaches the
conductivity cell. This time must be calculated before or during the experiment at the
flow rate of the experiment.
The calculations are best carried out using a spreadsheet such as EXCEL so that the
results can be displayed in tabular and graphical form.
Using the Armfield data logger, a set of readings of conductivity against time are
stored in the computer.
At this point, this data can be transferred onto the spreadsheet.
Start the spreadsheet program.
Plot the dimensionless concentration curve C/C 2 along time with the
experimental data
Dimensionless concentration curve (column C)
54
Eliminate from column C those values relating to the connection tubes

(column D)
Exercise A
Plot a column with equation (2), although the t r and Pe are unknown and
without taking into account the integration:
Pe and t r numbers will be found through the model equation using the solver function.
In order to obtain the integral of the equation (4), perform as follows:
Plot the mean point column of E column:
(Column F)
55
Plot the accumulative sum of the last one, using the following excel
function:
SUM(F i ,F i + 1 ,)
(Called column G)
Then plot the final model equation (equation 4): 1-G i (called column H)
In order to use the solver function, set in the SQD cell of your table the function
SUMXMY2 selecting column D and H, which means will sum the squares of the
differences between these two columns; experimental and model curves.
56
Exercise A
Then, go to the Solver function and in set target cell select SDQ cell; in
Equal to select Min with value 0, which means will minimize this value. In
by changing cells select the cells of residence time and Pe number on the
table built.
Note: The smaller value of SDQ the better match between curves and therefore
between residence time distribution and space time.
Press Solve bottom, Pe and residence time numbers will be found, as well as
the unknown columns.
57
Plot Experimental and Model columns, columns D and H, and compare them.
Normalised potassium chloride concentration at the reactor outlet along time.
Repeat the experiment changing some variables, like flow rate and tracer
concentration, to understand how significantly these parameters affect the residence
time distribution.
Study the different Pe numbers and the curves obtained.
Repeat the same experiment without static premixer and compare the difference.
58
Exercise A
Reactor responses for the plug flow reactor with axial dispersion model
Conclusion
One of the possible causes of the difference between model and experimental curve
can be the error on the reading of the conductivity because of dead or stagnant
volumes.
Compare the reactor space time,
obtained from tracer experiment.
, with the mean residence time,
A significant difference between both values, beyond the experimental errors, may
indicate the presence of dead volumes or stagnant regions when
presence of short circuits when
, or the
, or even other anomalies.
As experimental errors are common, make a sensible analysis to determine where

the experimental errors affect the results more significantly. For example: does 1 sec
error in the reading of the time required to fill graduated cylinder, used in the flow rate
measurement, significantly affect the space time calculation?
59
Exercise B - Flow pattern characterisation - Pulse change

Objective
The aim of this practical exercise is to study the flow pattern characterisation in a
tubular reactor packed with glass beads. This characterisation will be performed
using a model considering a plug-flow reactor with axial dispersion and by
determination of the RTD.
Method
The study of the flow pattern in a reactor is usually done using tracer techniques
which consist of introducing several perturbations at the inlet of the reactor and
monitoring the effect in the reactor. The commonly used perturbations in a plug flow
reactor are a Pulse change and Step change. A coloured tracer solution is used to
make the propagation of the concentration wave visible.
In this exercise the pulse change perturbation will be studied.
Equipment Required
Armfield Plug Flow Reactor CEY
Feed assembly
Optional Equipment
Chemicals
Distilled water
Potassium Chloride
Indigo Carmine
Theory
The flow characterisation of a reactor is done by the determination of the RTD, which
is obtained using tracer techniques. This curve enables the permanence of each
fraction of volume of fluid inside the reactor to be determined and also to show if its
behaviour is ideal or non ideal and how it differs.
Tracer techniques use several perturbations at the inlet of the reactor and wait for the
reactor answer. The most common perturbations used in a plug flow reactor are a
Pulse input and Step input.
60
Exercise B
Pulse input
Pulse input consists of an instantaneous injection of a small quantity of tracer

solution and it is mathematically represented by the following function:
C(t) = C 0 [H(t-0)-H(t-t)]
(1)
H: Heaviside function
t:duration of the perturbation
And the response of the reactor is:
(2)
Taking into account that for a plug-flow reactor the RTD is:
(3)
(t) : Dirac delta function
: space time
t r : Residence time
The response of a plug flow reactor with axial dispersion to a pulse input in the inlet
concentration is:
(4)
For a sufficiently small pulse,
:
61
(5)
Then, equation (4), for plug flow with axial dispersion, is simplified:
(6)
For infinitesimal pulses, Equation 5 predicts that the maximum concentration appears
at t = . For finite pulses, the maximum concentration comes out at t = + t/2. Thus,
in these circumstances, equation 5 is given by:
(7)
Experimental set up
Re-arrange the experimental assembly in accordance with the following:
.
Layout Pulse experiment
Verify the directional position of the six port injection valve so that water is pumped
into the reactor and coloured solution (tracer) is being recirculated. The loop will
contain the coloured solution. See Injection valve operation.
Ensure there is sufficient volume of solutions and that they are well mixed.
Ensure pumps are calibrated and they give the right flow rate
62
Exercise B
T connector supplied with the unit is not necessary in this case since just one
solution is injected into the reactor at a time.
Connect the single PTFE tube to the reactor through the quick connector.
CEXC sensors fitting section and plugged in the correct sockets at the rear of the
unit.
As the experiment involves the collection and the storage of sensors data, the data
USB port on the right hand side of the service unit 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, flow rates and
temperature values at selected time intervals over a selected period.
Procedure
Make up the tracer solution with 250 cm3 of 1 M Potassium Chloride solution
containing 0.1% of Indigo Carmine.
Rearrange the experimental assembly in accordance with Experimental set up
above.
Pour about 250cm3 of tracer solution in bottle 1, and about 1 litre of distilled water in
bottle 2.
Start the software using option Pulse Experiment.
Ensure that the injection valve is in the loading position (L position).
When switching the injection valve from one position to another, turn the handle of
the valve until it clicks so it is sure that connections between ports have been done
properly. Otherwise, ports will be blocked, pressure will increase and pipe will split
splashing with the solution contained. Once the loop has been loaded with tracer it is
RECOMMENDED to stop the pump, so if blockage occurs during switch pressure will
not increase on the tracer channel.
Type flow rates in the software for each solution and press POWER ON to start up
the pumps. Note that the flow rate of the tracer solution is not important as it will be
recirculated all the time.
Take note of the time required for the water to reach the reactor entrance (after static
premixer), the time spent in the reactor column, and the time spent between the exit
reactor and the detector. The total time will help to obtain the space time spent in the
connection tubes and to predict the reactor space time.
To make sure air does not get inside the conductivity cell, take out conductivity
sensor and as the water is exiting the reactor and overflows through the cell, fit the
sensor back into the cell and screw until sealing.
Then, start data acquisition by pressing GO. At the same time switch the injection
valve position to injection position (I), and take note of the time at which this has
been done. The solution inside the loop (tracer) will be injected into the reactor.
63

Once the tracer is injected, change the valve position to loading position (L).
Finish the experiment when the conductivity is approximately 0.01 mS/cm.
Click again POWER ON to finish the experiment. Stop data logging.
At the end, empty and wash the reactor column with distilled water. Flow distilled
water through the continuous flow electrode to remove any potassium chloride
residues.
CEY in the Pulse injection experiment
Results
The calculations are best carried out using a spreadsheet such as Microsoft EXCEL
so that the results can be displayed in tabular and graphical form.
On conclusion of the experiment using the Armfield data logger, a set of readings of
conductivity with time will be stored in the computer.
At this point, this data can be transferred onto the spreadsheet.
Start the spreadsheet program.
64
Exercise B
Make up a table as follows:

1.76
Flowrate (ml/s)
Residence time (s)
Pe
tau (V/Fr) (s)
210.00
Tubes time (s)
16.63
SQD
With the values of time and conductivity obtained from the experiment plot the
dimensionless concentration curve along time: C/C 0 against time,
Dimensionless concentration curve

Eliminate from C(t) curve, those values relating to the connection tubes. (See
Column C)
The following step is to determine the Peclet number and Residence time. It will be
necessary to use the solver function.
Plot a column with the following equation:
(Column D)
as t r and Pe are unknown, it is likely that nonsensical values will appear.
Then plot the final model curve ,
(Column E)
65
In order to use the solver function, set in the SQD cell the function SUMXMY2
selecting column C and E. This will sum the squares of the differences between
these two columns, to minimise the difference.
66
Then, go to solver and in set target cell select SDQ cell, in Equal to select
Min with value 0, which will minimize this value. And in by changing cells
select the cells of residence time and Pe number on the table.
Press Solve button Pe and residence time numbers will be found, and also
the two columns (model and equation).
Exercise B
Then plot C (t) column (C) and model equation column (H), and compare
them
Normalised potassium chloride concentration at the reactor outlet, along time.
Repeat the experiment changing some variables; flow rate, tracer concentration or
amount tracer injected. Study Peclet number and compare the different curves
obtained. This will help to understand the concepts explained on this section.
67
Conclusions
As experimental errors are common, make a sensible analysis to determine which
experimental errors affect the results most significantly. For example: does a sec
error in the reading of the time that water takes to reach entrance reactor significantly
affect the space time calculation?
One of the possible causes of the difference between the model and the
experimental curve can be the error on the reading of the conductivity because of
stagnant volumes.
Comparing the reactor space time, , and the mean residence time, t r , a significant
difference between both values, may indicate the presence of dead volumes or
stagnant regions. When t r < , this is a sign of stagnant regions and when t r > , this
can be a sign of short circuits.
68
Exercise C - Conversion experiment

Objective
The specific goal of this practical work is the determination of the steady state
conversion, for a second order reaction between sodium hydroxide and ethyl acetate,
in a tubular reactor packed with glass beads.
Method
The steady state conversion of the packed flow reactor is usually done by a reaction
in a steady state condition. In this case, it will be a study of a second order reaction
at 25C considering that the model of this reactor is Plug flow axially dispersed since
this was demonstrated in the previous experiment.
Equipment Required
Armfield Plug Flow Reactor CEY
Feed assembly
Optional Equipment
Chemicals
Sodium hydroxide
Ethyl Acetate
Indigo Carmine
Distilled water
Theory
In the previous experiments the flow pattern in the tubular reactor packed with glass
beads was characterised. In the present work we intend to determine the steady
state conversion in the same tubular reactor, at room temperature. If we assume that
the flow pattern in the reactor is described by the plug axially dispersed model, the
steady state conversion for a second order reaction should be obtained from the
reactor steady state mass balance:
The steady state conversion for a second order reaction should be obtained from the
reactor steady state mass balance:
(1)
where u es the superficial velocity, x A is the conversion of the limiting reactant A, z is
the axial coordinate, k is the reaction kinetic constant, C A0 is the concentration of
species A at the reactor inlet, M = C B0 /C A0 1, B being the second reactant, and D ax
is the axial dispersion.
Previous expression can be written in dimensionless form:
69
(2)
where z* = zL and L is the length of the reactor. Introducing now the dimensionless
Peclet number, Pe = uL/D ax , and the space time = L/u:
(3)
Once the residence time distribution is known, the steady state conversion can be
determined by;
(4)
replacing the C NaOH (t)/C NaOH0 for a second order reaction, yields:
(5)
Finally,
(6)
For an ideal plug flow reactor
state conversion:
, an analytical solution exists for the steady
(7)
for M >1, and for M=1:
(8)
The kinetic constant and activation energy are data which can be obtained with a
batch reactor at different temperatures. Once k 0 and Ea are known obtain the kinetic
constant at the temperature of the experiment through:
70
Exercise C
If this information can not be obtained, use Figure C2 data as necessary:
Figure C1: Conversion of the NaOH at different temperatures
Figure C2: Linearization of NaOH conversion
71
being
Ea (kJ/mol) = 29.4
(11)
k 0 (m3/mol s) = 12.5
m = slope
M = C B0 /C A0
For example, for a C A0 = 0.1, C B0 = 0.125 and at these different temperatures:
K (17C) = 6.40E-05 m3mol-1s-1
K (22C) = 8.00E-05 m3mol-1s-1
K (27C) = 9.60E-05 m3mol-1s-1
Experiment set up
Re-arrange the experimental assembly in accordance with Figure C3.
Verify the directional process of the six port injection valve so that solutions, sodium
hydroxide and ethyl acetate with indigo carmine, are injected into the reactor. See
Injection valve operation as necessary.
Fit the T-connector into the reactor inlet. Then connect PTFE tubing to the injection
valve as detailed in the Installation section.
CEXC sensors fitting section and plugged into the correct socket of the control
console.
As the experiment involves the collection and the storage of the conductivity data, the
data output port on the right hand side of the service unit must be connected to
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, flow
rates and temperature at selected time intervals over a selected period.
72
Exercise C
Figure C3: Layout Conversion experiment
Procedure
Make up 1 L of sodium hydroxide of approximately 0.2 M but of rigorous titre and 1 L
of ethyl acetate 0.25 M with Indigo Carmine at 0.01% w/w.
Fill one bottle with 0.2M NaOH and the other one with the other solution; 0.25M ethyl
acetate (with 0.01% w/w indigo carmine), and connect the corresponding tubes in
each vessel.
Bottles should be closed to protect from air.
Set same flow rates as used in the pattern characterisation experiment (Exercise A
and B), by filling the right value in the software.
Set data collection at 3 seconds on the software.
Start the data acquisition by pressing GO, and wait until the continuous flow reactor
reaches the steady state. This should take about 5 minutes.
It is recommended to check flow rate and temperature at the beginning, in the middle
and at the end of the experiment.
Pay attention to the colour change between reactor inlet and outlet, and try to relate it
with the pH of the medium and with the sodium hydroxide conversion. The reactor
inlet should be yellowish, whereas the outlet nearly dark blue.
When solutions are almost finished, stop data logging and turn off the peristaltic
pumps, drain the remainder into a flask and fill reagent vessels with distilled water.
Empty the reactor by disconnecting tubes from the bottom and put a flask underneath
to collect the solution inside.
73

Then, reconnect the tubes and start pumping distilled water into the reactor and
sensor block to eliminate the residues of the experiment.
Check that the conductivity values have reached the values corresponding to distilled
water.
Results
The calculations are best carried out using a spreadsheet such as Microsoft EXCEL
so that the results can be displayed in tabular and graphical form.
Make up a table as follows:
ml
Pe
[NaOH]
0.2
Tau
[EtAC]
0.25
K0
mS/cm2
K final
mS/cm2
1.76
1.25
[NaOH] 0
0.1
ml/sec
Peclet number and space time should be obtained from the last experiment.
Therefore, the flow rate should be the same in both experiments.
Kinetic constant, k, depends on the temperature, therefore obtain that value at the
temperature of the experiment. See kinetics data above as necessary.
IMPORTANT: It is necessary to take into account the following considerations:
C NaOH0 : Concentration of NaOH in the mixture (in this case 0.2/2 = 0.1)
K0: conductivity of NaOH
K: Final conductivity
Obtention of K 0 , K:
Pour 100 cm3ml of the sodium hydroxide prepared into a flask and add 100 ml of
distilled water mix it and take note of the conductivity value which corresponds to the
sodium hydroxide 0.1 M (K 0 ).
Measure again 100 cm3 ml of the prepared sodium hydroxide solution and pour it into
a flask or glass reactor. Add 100 cm3 of the prepared 0.25 M ethyl acetate solution
(with 0.01% w/w IC) and start the magnetic stirrer. Colour changes go from dark
green to light and later on to blue at the end of the reaction. Take note of the
conductivity when reaction is complete, K.
74
Exercise C
If those values can not be obtained by experimental method, apply the following
equations:
K 0 = 0.195[1+0.0184(T-294)] C NaOH 0
T ( K )
C NaOH 0 ( mol/cm3)
K = 0.070[1+0.0284(T-294)] C NaOH 0
T ( K )
C NaOH 0 ( mol/cm3)
For C
NaOH 0
< C EtAc 0
since NaOH is limiting reagent
Once parameters are obtained, continue as follows:
Plot the following equation (column D) to obtain C NaOH :
(12)
Plot conversion column (column E)
(13)
Plot same columns for Ethyl acetate (column F and G):

(14)
(15)
The following experimental results do not intend to be real, they are a demonstration
of the data required and mathematical treatment must be done.
The operating conditions are presented in the following table:
75
Figure C4: Steady state conversions along time. Operation temperature = 20 C
Now, obtain the steady state conversion from the model equation and compare with
the experimental value.
76
Plot equation (6) without apply the integration, using Pe, Tau numbers from
tracer experiment. (Column H)
Then, plot the mean point of this column :
Exercise C
Finally, plot the SUM of the last column so that the integration is complete.
Perform the steady state conversion experiment at different flow rate, different
temperature, and different Ethyl acetate concentrations. Compare and analyse what
happens and why.
77

Perform the experiment without pre mixer and it will observe a segregation
phenomenon.
78
Contact Details for Further Information

Main Office:
Armfield Limited
Bridge House
West Street
Ringwood
Hampshire
England BH24 1DY
Tel: +44 (0)1425 478781
Fax: +44 (0)1425 470916
Email: sales@armfield.co.uk
support@armfield.co.uk
Web: http://www.armfield.co.uk
US Office:
Armfield Inc.
436 West Commodore Blvd (#2)
Jackson, NJ 08527
Tel: (732) 928 3332
Fax: (732) 928 3542
Email: info@armfieldinc.com
79

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Use with CEX Service Unit

Armfield Instruction Manual

CEY Plug Flow Reactor

Figure 1: Front View of Plug Flow Reactor Unit

Figure 2: Top View of Plug Flow Reactor Unit

Important Safety Information

Wet Floor warnings should be displayed where appropriate.

The apparatus should be placed in a location that is sufficiently strong to

Important Safety Information

Safety shoes and/or gloves should be worn when appropriate.

It is the users responsibility to handle chemicals safely.

Prepare chemicals and operate the equipment in well ventilated areas.

Only use chemicals specified in the equipment manuals and in the

Follow local regulations regarding chemical storage and disposal.

Specific Safety Guidelines:

Indigo Carmine is dangerous and so should be used with the necessary

Ethyl acetate is highly inflammable. Be careful with possible ignition sources,

Water Borne Hazards

Armfield Instruction Manual

Where practicable the water should be maintained at a temperature below

A scheme should be prepared for preventing or controlling the risk

Armfield Instruction Manual

Figure 1: CEY reactor

Figure 2: Flow of material circuit

Armfield Instruction Manual

Figure 3: Flow Exit Reactor

Injection valve operation

Figure 4.1 and 4.2: Injection valve positions

Figure 5: Injection Flow Assembly (FIA)

Armfield Instruction Manual

Follow the instructions on screen.

Operating the Software

Presentation Screen - Basics and Navigation

Armfield Instruction Manual

To view the Mimic Diagram click the View Diagram icon

A Mimic diagram is displayed, similar to the diagram as shown:

Armfield Instruction Manual

Control Facilities in the Mimic Diagram

Data Logging Facilities in the Mimic Diagram

icon from the

icon from the toolbar to start recording, click

icon from the toolbar to stop recording.

In addition to the choice of Manual or Automatic sampling, the parameters for

Armfield Instruction Manual

from the main tool bar or

The data is displayed in a tabular format, similar to the screen as shown:

Armfield Instruction Manual

Armfield Instruction Manual

A PID screen is then displayed as shown:

Clicking Settings returns the screen to the PID settings.

Operating the Equipment

Armfield Instruction Manual

Filling the feed bottles

Operation of Data Logger and Software

Mimic Diagram and software

Armfield Instruction Manual

Operating Plug Flow Reactor

Operational Layout for tracer experiments

Air bubbles in the reactor column

Total volume column: 0.919 dm3