SlideShare a Scribd company logo
1 of 49
Download to read offline
Transparent Batch Reactor
Instruction Manual
CEB-MkIII
ISSUE 2
December 2011
Table of Contents
Copyright and Trademarks...................................................................................... 1
General Overview ....................................................................................................... 2
Equipment Diagrams................................................................................................... 3
Important Safety Information....................................................................................... 4
Introduction.............................................................................................................. 4
Water Borne Hazards.............................................................................................. 4
Electrical Safety....................................................................................................... 4
Hot Surfaces and Liquids ........................................................................................ 5
Chemical Safety ...................................................................................................... 5
Description .................................................................................................................. 6
The Reactor Vessel................................................................................................. 6
Installation................................................................................................................... 9
Advisory................................................................................................................... 9
Installation Process ................................................................................................. 9
Operation .................................................................................................................. 12
Operating the Software.......................................................................................... 12
Operating the Equipment....................................................................................... 22
Equipment Specifications.......................................................................................... 28
Environmental Conditions...................................................................................... 28
Routine Maintenance ................................................................................................ 29
Responsibility ........................................................................................................ 29
General.................................................................................................................. 29
RCD Test............................................................................................................... 29
Temperature sensors calibration........................................................................... 29
Calibration of the conductivity sensor.................................................................... 29
Laboratory Teaching Exercises................................................................................. 32
Index to Exercises ................................................................................................. 32
Nomenclature ........................................................................................................ 32
Common Theory.................................................................................................... 33
ii
Table of Contents
iii
Exercise A - Isothermal Operation ............................................................................ 35
Exercise B - Reactant Concentration........................................................................ 41
Exercise C - Adiabatic Operation.............................................................................. 42
Contact Details for Further Information..................................................................... 45
1
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 Thursday: 0830 – 1730 and Friday 0830 - 1300 UK
time). 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 © 2011 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.
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.
Batch reactors are used widely in industry at all scales. Batch reactors are tanks,
commonly provided with agitation and a method of heat transfer (usually by coils or
external jacket). This type of reactor is primarily employed for relatively slow
reactions of several hours duration, since the downtime for filling and emptying large
equipment can be significant. Agitation is used to maintain homogeneity and to
improve heat transfer.
The Armfield CEB MkIII Transparent Batch Reactor is specially designed to allow
detailed study of this important process. It is one of five reactors 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, CEY Plug Flow 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 and visually due to the use of
indicators.
CEXC fitted with CEB MkIII Transparent batch reactor
Note: If CEB-MKIII is to be used with a CEX rather than CEXC, then optional
temperature sensor ST54 will be required if it is required to measure reactor
temperature (the temperature sensor supplied with CEX is used to control the hot
water temperature in isothermal operation).
2
Equipment Diagrams
Figure 1: CEB MkIII Transparent batch reactor
3
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 CEB MkIII Transparent Batch Reactor 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.
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 45°C. 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
20°C. 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.
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
4
Important Safety Information
5
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.
Hot Surfaces and Liquids
The unit incorporates a pumped electric water heater, and is capable of producing
temperatures that could cause skin burns.
Before disconnecting any of the pipes or tubing:
 Stop all the pumps.
 Leave time for the water to cool
 Check that the temperature is at a safe level
Do not touch any surfaces close to ‘Hot Surfaces’ warning labels, or any of the
interconnecting tubing, whilst the equipment is in use.
Chemical Safety
Details of the chemicals intended for use with this equipment are given in the
Operational Procedures 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 user’s 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.
Description
Where necessary, refer to the drawings in the Equipment Diagrams section.
The Reactor Vessel
The reactor vessel is a double skinned glass vessel with one litre and a half of
internal working volume. It is set on a baseplate which is designed to be located on
the four studs of the CEXC service unit and then secured by thumbnuts. The reactor
is supported by three pillars; position the reactor on the CEXC service unit such that
a single pillar is to the front.
CEB MKII Transparent Batch Reactor
Hot water from the CEXC or cold water from CW17 can be recirculated to the jacket
for temperature control purposes. Either the hot water circulator or the CW-17 chiller
is connected to the ‘Heater/Cooler attachments’. Note: the water inlet is at the
bottom of the reactor jacket and the water outlet is at the top of the reactor jacket.
A turbine agitator works to provide efficient mixing and heat transfer. The agitator is
driven by an electric motor mounted on the lid of the reactor. The speed of the motor
can be controlled by using Amrfield software interface. The socket for the electrical
motor plug is sited at the rear of the service unit.
6
Description
Reactor Lid
Glands in the reactor lid house the conductivity and temperature sensor provided
with the CEXC service unit. The larger of the two glands is for the conductivity probe.
The glands are unscrewed by hand, the sensors inserted completely into the reactor
until they rest a few cm from the bottom and then the glands re-tightened by hand.
Sockets at the rear of the service unit are provided to connect each sensor. The
conductivity probe is connected to the 3 pin socket marked ‘HIGH COND’. The
temperature sensor is connected to the k-thermocouple socket marked ‘T1’. Both
temperature values and conductivity values are data logged using a PC in
conjunction with the Armfield software interface.
An additional temperature sensor ‘T2’ is supplied with CEXC that allows the Hot
Water Circulator temperature to be also monitored. Therefore T2 temperature sensor
must be immersed in the Hot Water Circulator vessel through the hole in the lid.
There is an extra temperature ‘T3’ and ‘Low conductivity’ plug at the rear of the
service unit with outputs on the software for extra connections made by the user. If
solutions with low conductance are used, connect the conductivity probe to the
socket marked as ‘LOW COND’ and conductivity values will be data logging more
accurately in a low range.
7
Armfield Instruction Manual
8
CEB MkIII Transparent Batch Reactor
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
1. Mounting the CEB MKIII onto the CEXC
 The reactor vessel is set on a baseplate which is itself located on four studs
on the service unit and secured by thumbnuts. The feed bottles provided with
CEXC are not required with the batch reactor configuration.
 Plug the temperature sensor and conductivity sensor supplied with CEXC into
the appropriate sockets at the rear of the service unit then insert the sensors
through the appropriate glands in the lid of the reactor. Check that the
sensors are fully immersed then tighten the glands.
 Connect the stirrer plug to the socket located on the rear of the CEXC.
2. Connecting the HWC to CEB MKIII
9
Armfield Instruction Manual
 Connect return pipe of the HWC (1) to the connection at the top of the reactor
vessel.
 Connect the supply pipe of the HWC (2) to the connection at the bottom of the
reactor vessel.
3. Connection to electricity supply
 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 circuit breakers and RCD are 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.
4. Connection to data logger
 Connect CEXC to a PC using the USB cable supplied.
 Insert the CEB MkIII 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.
 Follow the instructions on screen
10
Installation
11
 Run the software
5. Priming the hot water circulator (HWC)
 Fill HWC vessel with water up to the low level tip (30 cm from top).
 Switch on the Hot Water Circulator and Power On. Level of water in the
vessel will decrease as reactor jacket is filled. Keep filling the HWC vessel
until the level in the vessel is stable and over the Low level tip.
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
12
Operation
the IFD5 and the PC and confirm that the red and green LED’s 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.
13
Armfield Instruction Manual
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:
The details in the diagram will vary depending on the equipment chosen if multiple
experiments are available.
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.
14
Operation
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%,
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.
15
Armfield Instruction Manual
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 icon from the
main toolbar. One set of data will be recorded each time the icon is clicked.
Automatic logging is selected when transients need to be recorded so that they can
be plotted against time. Click the icon from the toolbar to start recording, click
the icon from the toolbar to stop recording.
The type of logging can be configured by clicking Configure in the Sample drop-
down 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:
16
Operation
Tabular Display
To view the Table screen click the View Table icon from the main tool bar or
click Table from the View dropdown menu as shown:
The data is displayed in a tabular format, similar to the screen as shown:
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.
17
Armfield Instruction Manual
Graphical Display
When several samples have been recorded, they can be viewed in graphical format.
To view the data in Graphical format click the View graph icon from the main
tool bar or click Graph from the View drop-down menu as shown:
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.
18
Operation
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:
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:
19
Armfield Instruction Manual
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
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:
20
Operation
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.
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:
21
Armfield Instruction Manual
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.
22
Operation
Operation Hot Water Circulator
The hot water circulator vessel should be filled with water before use, and drained
after use if the equipment is not going to be used for some time. When use fill the
vessel by pouring clean (preferably demineralised) water until the level is
approximately 20 mm from the top.
Top up the level of this vessel as necessary to maintain the level above the tip of the
level electrode (typically 20 mm from the top of the vessel).
Heater is controlled from a PC via the CEB software. A PID controller within the
software maintains the heater setting based on the temperature measured by the
chosen temperature sensor. The Set Point temperature, proportional Band and the
Integral and Derivative times may be adjusted by the user. Alternatively the heater
power setting may be entered manually as a percentage value, using the same
controller window as for the PID settings.
Operation of Data Logger and Software
The Armfield CEB MkIII reactor is controlled using the CEB MkIII software supplied,
which allows real-time monitoring and data logging of all sensor outputs and control
of the heater unit. 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 >
CEB). 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 includes controls for the stirrer and the Hot
water Circulator. The stirrer is controlled from the software using the up/down buttons
or typing in directly a value between 0 and 100 %.
Concentration and volume values must be filled in the boxes on each experiment so
that software will carry out the convenient calculations.
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.
23
Armfield Instruction Manual
Controlling the HWC
The heater is controlled by a controller in the software. Click on the appropriate
CONTROL symbol to open the controller window.
24
Operation
Control can be either closed loop (Automatic) which uses the temperature sensor
immediately following the heater as the process variable in a PID loop, or open loop
(Manual) where the user defines the percentage time the heaters are ‘ON’ for, and
hence the output power.
When performing a reaction it is best to use Automatic control as this produces
stable temperatures most rapidly, and maintains these conditions by varying the
heater power.
Operating the CEB MkIII
There are two modes of operation with the CEB batch reactor: Isothermal and
Adiabatic operation. The temperature and conductivity sensors must be situated well
below the liquid surface inside the reactor.
Isothermal Operation
When operating isothermally the temperature sensor T2 supplied with CEXC should
be set as the temperature sensor to be controlled in the PID loop box on the
software. This sensor must be immersed in the vessel of the Hot Water Circulator.
On the other hand the other temperature sensor T1 is used to monitor the reaction
temperature during the experiments.
PID settings need to be adjusted to suit the experiment conditions. When using the
Chiller CW-17 PID settings are not required. See the installation guide for appropriate
controller settings when using the CW-17.
In the case of Isothermal Operation the PID settings recommended are:
25
Armfield Instruction Manual
Note these values are suitable when the controlling sensor is T2 which is fitted in the
HWC vessel.
The setpoint can be varied as required to suit the experiment.
Adiabatic Operation
When operating the batch reactor adiabatically, temperature control is not required
so either Chiller or HWC are not required.
The contents of the reactor are stirred by an agitator which is driven by an electrical
motor/gearbox combination mounted on the lid. The motor is connected to the
electrical supply by a jack plug which is plugged into a socket at the rear of the CEXC
service unit. The agitator speed is adjusted using the Armfield software interface
supplied with the reactor. See mimic Adiabatic Operation Diagram below.
26
Operation
27
Ensure that protective gloves are worn when handling any of the substances used in
the reactor. Once the experiment is finished wash the reactor with distilled water.
Equipment Specifications
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;
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 (over-
voltage) 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
28
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 re-
calibration. However should calibration become necessary follow the below
procedure. This should only be done once the unit has fully warmed up.
The temperature 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).
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.
If a thermocouple calibrator is available:
Connect Thermocouple calibrator simulator to T1 input socket. Set to 25ºC and
adjust VR1 (T1 ZERO) and VR2 (T1 SPAN) on the PCB to give 25ºC displayed on
PC. Check accuracy at 15º and 40ºC.
Repeat the same procedure for T2 by adjusting VR3 (T2 ZERO) and VR4 (T2 SPAN)
on the PCB to give 25ºC displayed on PC, and VR5 (T3 ZERO) and VR6 (T3 SPAN)
for T3.
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 0ºC, then sensors should be dipped into boiling water and
then adjust the SPANS to 100ºC.
Calibration of the conductivity sensor
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
29
Armfield Instruction Manual
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.
High conductivity Calibration
Fill a small beaker with a Conductivity standard solution (e.g. 0.1M KCI giving a
conductivity of 12.88 mS at 25°C) 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
Fill a small beaker with a Conductivity standard solution (e.g. 0.01M KCI giving a
conductivity of 1.41mS at 25°C) 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.
12.88 mS/cm at 25ºC 0.1 M KCl
ºC mS/cm ºC mS/cm
5 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
30
Routine Maintenance
31
18 11.19 25 12.88
19 11.43 26 13.13
1.413 mS/cm at 25ºC 0.01 M KCl
ºC mS/cm ºC mS/cm
5 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
Laboratory Teaching Exercises
Index to Exercises
Exercise A - Isothermal Operation
Exercise B - Reactant Concentration
Exercise C - Adiabatic Operation
Nomenclature
Symbol Name Unit
ao initial sodium hydroxide conc. (mol/dm3
)
a1 sodium hydroxide conc. in reactor at time t (mol/dm3
)
sodium hydroxide conc. in reactor after
time
(mol/dm3
)
b ethyl acetate conc. (mol/dm3
)
(same subscripts as above for a)
c sodium acetate conc. (mol/dm3
)
(same subscripts as above for a)
C acetic anhydrite conc. at time t (mol/dm3
)
C0 acetic anhydrite conc. at t = 0
k specific rate constant
r reaction rate (s)
tr reaction time (s)
t elapsed time (s)
T reactor temperature (K)
V volume of reactor (dm3
)
Xa
conversion of sodium hydroxide =
Xc
conversion to sodium acetate =
32
Laboratory Teaching Exercises
conductivity (Siemens/cm)
initial conductivity
conductivity at time t
conductivity after time
sodium hydroxide conductivity
sodium acetate conductivity
k0 Arrhenius frequency factor
E Activation energy (J/mol)
R gas constant (J/mol K)
ρ density (kg/dm3
)
H molar enthalpy (J/mol)
mean heat capacity (J/kg K)
Common Theory
The Armfield batch reactor is designed to demonstrate the mechanism of a chemical
reaction in a reactor, as well as the effects of varying process conditions such as
reaction temperature, reagent concentrations etc.
The reaction chosen for the isothermal demonstration is the saponification of ethyl
acetate by sodium hydroxide, as it can be carried out under safe conditions of
temperature and pressure and is well documented. The use of indicators allows to
follow the reaction by changing the colour as the reaction takes place.
The reaction chosen for the adiabatic demonstration is the hydrolysis of acetic
anhydride. This involves the use of glacial acetic acid and sulphuric acid as well as
acetic anhydride.
Although it may be possible to carry out demonstrations using other chemicals, it is
not advisable as the materials of construction of the reactor may not be compatible.
Before carrying out reactions involving any other reagents please refer to Armfield
Ltd. for advice.
Dilution of Ethyl Acetate for use with CEB MKII Batch Reactor
Armfield recommends the use of a 0.1M solution of Ethyl Acetate in the CEB MkII
reactor. This should be made by diluting concentrated Ethyl Acetate as follows:
33
Armfield Instruction Manual
34
Therefore add 4.895 ml of concentrated Ethyl Acetate to 400 ml of deionised or
distilled water.
Shake the mixture vigorously until the two liquids have mixed. Add further water to
make up the final volume to 500 ml.
Note: The practice of making a strong solution (e.g. 1M) then further diluting this to
the required concentration (e.g. 0.1M) cannot be applied when using Ethyl Acetate.
The required dilution should be made directly as stated above.
To get the colourful solution add 0.00394 gr of Crystal Violet to the 500 ml of Ethyl
Acetate to make up a final solution of 1·10-5Mol/l of CV when both reagents are
mixed.
Dilution of Sodium Hydroxide for use with CEB MKII Batch Reactor
Armfield recommends the use of a 0.1M solution of Sodium Hydroxide in the CEB
MkIII reactor. This may be made by adding 50ml of NaOH 1M to 450 ml of distilled
water then making up the solution to 500ml.
Exercise A - Isothermal Operation
Objective
To find the reaction rate constant in a stirred batch reactor.
Theory
The reaction:
NaOH + CH3COOC2H5 → CH3COONa + C2H5OH
Sodium Hydroxide + Ethyl Acetate → Sodium Acetate + Ethyl Alcohol
Assuming that the initial concentrations are equal and that the amount of reagent
used up after time t is X then the concentrations at time t are:
NaOH + CH3COOC2H5 → CH3COONa + C2H5OH
a-X + a-X → X + X
From the kinetic analysis of a general second order reaction it can be shown that:
(1)
where k is the reaction rate constant and t is the time of reaction. Using notation from
the nomenclature:
substituting for X in equation (1) above gives:
Hence a plot of against t gives a straight line of gradient k.
Method
Make up 0.5 litre batches of 0.1M sodium hydroxide and 0.5 of 0.1M ethyl acetate
(containing 1·10-5
Mol/l Crystal Violet)
IMPORTANT: It is essential when handling these chemicals to wear protective
clothing, gloves and safety spectacles.
Open Armfield Software and choose ‘Isothermal operation’
Set up the Hot Water Circulator as detailed in the Operation section.
Adjust settings on the PID loop as detailed in Operation procedure for Isothermal
Operation and set point to 25°C.
35
Armfield Instruction Manual
Charge the batch reactor with 0.5 litres of the sodium hydroxide solution. Set the
reactor agitator to '50%' and press ‘Power on’ to start the agitation. Then press ‘Hot
Water Circulator’ and water will start to recirculate through jacket reactor and vessel.
As the experiment involves the collection and storage of conductivity data, the data
output port in the plinth must be connected to the computer with Armfield Interface
data logger. This will enable data logging of the conductivity, temperatures and stirrer
speed values at selected time intervals over a selected period.
Ensure the conductivity and temperature sensors have both been installed in
accordance with the Installation section.
Collection of data will be until a stable condition is reached in the reactor and this
takes approximately 30 minutes. It is advisable to set the data collection period to,
say, 45 minutes.
Switch on the Hot Water Circulator. The temperature of the sodium hydroxide in the
reactor vessel will begin to rise and will be automatically maintained at the desired
set-point (25o
C in this instance) by the action of the HWC in the jacket.
Carefully add to the reactor 0.5 litres of the ethyl acetate solution and instigate the
data logger program (or begin taking readings if no computer is being used).
It has been determined that the degree of conversion of the reagents affects the
conductivity of the reactor contents. By recording the conductivity with respect to
time, either manually or using the Armfield Data Logger, the amount of conversion
can be calculated.
If time permits the experiment should be repeated as above but with the temperature
controller set to 35°C, or at other temperatures below room temperature like 15ºC. It
is also recommended to repeat the experiment at another stirrer speed to study the
effect of the mixing on conversion.
When temperature is below room temperature, the use of a Chiller is required.
Connect the Chiller system as detailed in the OPERATIONAL PROCEDURES
section of the CEXC manual.
It is recommended to fit the CEXC temperature probe T2 into the HWC vessel hole
for better PID control, as described in Isothermal operation section, and the use of
the T1 temperature sensor also supplied to follow the temperature in the reactor.
Interpretation of results
Armfield Interface data logger performs all the calculations while the experiment
takes place. However if better understanding of the experiment is needed, follow
below procedure to calculate the specific rate constant and effect of the temperature
on the specific rate constant.
Having recorded the conductivity of the contents of the reactor over the period of the
reaction, the conductivity measurements must now be translated into degree of
conversion of the constituents.
Both sodium hydroxide and sodium acetate contribute conductance to the reaction
solution whilst ethyl acetate and ethyl alcohol do not. The conductivity of a sodium
hydroxide solution at a given concentration and temperature however, is not the
same as that of a sodium acetate solution at the same molarity and temperature and
36
Exercise A
a relationship has been established allowing conversion to be inferred from
conductivity:
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, the set of readings of conductivity with time will
need to be transferred to the computer as two columns of data.
Now enter the following known constants from the experiment using the
Nomenclature. Ensure use of correct units.
a = (Sodium Hydroxide conc. in feed bottle)
a0 = (Sodium Hydroxide conc. in mixed feed) =
b = (Ethyl acetate conc. in feed bottle)
b0 = (Ethyl acetate conc. in mixed feed) =
c =
T = (Reactor temperature, T1)
V = (Total volume in the reactor vessel)
Using the spreadsheet, calculate the values of
from the following formulae:
For the values of each of the above, the spreadsheet can be used to calculate values
of sodium hydroxide concentration (a1) and sodium acetate concentration (c1) and
37
Armfield Instruction Manual
the degree of conversion (Xa) and (Xc) for each of the samples of conductivity taken
over the period of the experiment.
These can be calculated and listed in columns (use spreadsheet COPY facility)
alongside the readings of conductivity using the following equations:
The concentration of NaOH can be plotted against time:
To calculate the specific rate constant, k:
38
Exercise A
It is recommended that this experiment be repeated at various other reactor
temperatures to investigate the relationship between the specific rate constant k and
the temperature of reaction.
The effect of temperature on the reaction rate constant is determined by the
activation energy of such a reaction, through the Arrhenius law:
k = k0 e-E/RT
where k0 is the frequency factor, E is the activation energy, R is the ideal gases
constant and T is the absolute temperature.
Once the kinetic constant at three different temperatures is known, for instance 15ºC,
20ºC and 25ºC, is straightforward to apply the Arrhenius law and calculate the
frequency factor and the activation energy values for:
39
Armfield Instruction Manual
40
Obtaining the reaction rate constant in function of the temperature:
High activation energy implies a significant sensibility of the reaction kinetics to the
temperature.
Exercise B - Reactant Concentration
Objective
To determine the effect of reactant concentration on the reaction rate.
Theory
In homogenous reaction systems, reaction rates depend on the concentration of the
reactants. Collision theory indicates a rate increase if the concentration of one or
both of the reactants is increased. 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 is:
where: r = reaction rate
k = rate constant
[A]n
, [B]m
= molar concentrations of reactants
n, m = appropriate powers (based on experimental data)
Method
Use the same procedure as for Exercise A. Run the experiment using different initial
concentrations of the reagents, for example, 0.1M, 0.08M and 0.02M. 0.5 litre of each
solution will be required for each mixture tested.
Using the Armfield Data Logger in each experiment, graphs can be plotted relating
reaction rate to concentration level for each of the reactants tested.
A logarithmic plot of reaction rate to concentration level will give a straight line of
slope equal to the power of the relationship.
Hence the rate law for sodium hydroxide and ethyl acetate can be written in the form
41
Exercise C - Adiabatic Operation
WARNING: 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.
DO NOT add acetic anhydride directly to sulphuric acid, as the reaction is
violent and will cause the chemicals to be sprayed into the air.
The reaction described in this experiment should be carried out in a fume
cupboard. On completion, the reaction products should be discarded
according to local regulations (for example into a copious flow of cold water to
a suitable drain), taking care to avoid inhalation of vapour.
Objective
To determine the rate equation for the hydrolysis of acetic anhydride to acetic acid in
an adiabatic reactor.
Theory
The hydrolysis of acetic anhydride in water, in the presence of a catalyst of sulphuric
acid is described by:
This reaction can be assumed to have simple power law kinetics of the form
, if the reaction is zero order in water. The concentration of the protonic
acid remains constant for the duration of the run and thus k is a catalytic rate
constant that includes this concentration, also in power law form. For any system of
this particular type the instantaneous value of the acetic anhydride concentration can
be eliminated between the material and thermal balance equations to give a linear
equation (which can therefore be subjected to a statistical test). Use of this equation
requires that values of the gradient of temperature with respect to time be found.
If the concentration of acetic anhydride at any time t is C, then the rate of the reaction
is given by:
(1)
with C = C0 at t = 0. The heat generation rate is:
(2)
with T = T0 at t = 0. Substituting equation (1) in equation (2), integrating with
respect to time and using the boundary conditions, we obtain:
(3)
For the n-th order case, the rate may be expressed in Arrhenius form:
42
Exercise C
(4)
Using and rearranging, equation (3) becomes:
Using equations (4) and (2), we obtain:
(5)
Using when the reaction is complete gives:
Substituting for  in equation (5) and rearranging, we have:
Taking logarithms of both sides of this equation gives:
(6)
and so a plot of ln(LHS) vs. 1/T should be linear with an intercept of ln(A) and a
gradient of .
Method
Ensure the reactor has been set up with the special temperature sensor and
computer interface for the adiabatic reaction as described in the Installation section.
If possible the reactants should be at approximately 30°C before mixing. If they are
cooler than this, the reaction will take much longer to complete.
Charge the reactor with 100ml of acetic anhydride and 250ml of demineralised water.
Start the reactor agitator and adjust the variable speed drive to position '5.0'.
Add 150ml of glacial acetic acid (since the water and acetic anhydride are mutually
insoluble, but are both soluble in acetic acid, this ensures that the reaction mixture is
homogeneous - the acetic acid does not form part of the reaction).
43
Armfield Instruction Manual
44
Start the data logger program choosing 15 seconds as the interval between samples
and 1500 seconds as the total running time of the experiment (a longer duration will
be required if the temperature of the reactants is less than 30°C). It is essential to log
data until the temperature in the reactor begins to fall again.
Immediately add 25ml of 0.5M sulphuric acid as the catalyst. The reaction will
commence.
Switch off the agitator.
When the reaction has completed, the temperature data can be viewed within the
software, either in tabular or graphical format. The data should be saved as an excel
file. It is then possible to carry out the second part of the analysis described above,
by calculating the terms of equation (6), and plotting the graph.
In order to find dT/dt, it will be necessary to extract the linear region of data from a
graph of temperature vs. time for the experiment. This will entail discarding the first
few points, and also any points after the temperature reaches the peak value. See
figure below
Several runs similar to that described above should be performed, using differing
quantities of sulphuric acid catalyst (e.g. 15ml to 40ml in 5ml increments).
It will then be necessary to find the best value for n in equation (6) by trial and error,
refining the value until the best straight line fit is obtained.
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
45

More Related Content

What's hot

MASS TRANSFER OPERATION-DISTILLATION
MASS TRANSFER OPERATION-DISTILLATIONMASS TRANSFER OPERATION-DISTILLATION
MASS TRANSFER OPERATION-DISTILLATIONHoneyAgrawal16
 
Gas Absorption Laboratory Experiment
Gas Absorption Laboratory ExperimentGas Absorption Laboratory Experiment
Gas Absorption Laboratory Experimentdp93
 
Scale up of agitated vessels and static mixer
Scale up of agitated vessels and static mixerScale up of agitated vessels and static mixer
Scale up of agitated vessels and static mixerVivek5103
 
Reporte practica 6 Separación Mecánica
Reporte practica 6 Separación Mecánica  Reporte practica 6 Separación Mecánica
Reporte practica 6 Separación Mecánica Beyda Rolon
 
Armfield Gas Absorption Column Experiment
Armfield Gas Absorption Column ExperimentArmfield Gas Absorption Column Experiment
Armfield Gas Absorption Column ExperimentHadeer Khalid
 
Curso inciación a COCO Simulator y ChemSep - Simulación de procesos químicos ...
Curso inciación a COCO Simulator y ChemSep - Simulación de procesos químicos ...Curso inciación a COCO Simulator y ChemSep - Simulación de procesos químicos ...
Curso inciación a COCO Simulator y ChemSep - Simulación de procesos químicos ...CAChemE
 
Estimacion de costes y rentabilidad
Estimacion de costes y rentabilidadEstimacion de costes y rentabilidad
Estimacion de costes y rentabilidadLUIS MONREAL
 
Boiler control system engineering
Boiler control system engineeringBoiler control system engineering
Boiler control system engineeringHernan Coba
 
Design of thermosyphon reboiler
Design of thermosyphon reboilerDesign of thermosyphon reboiler
Design of thermosyphon reboilerHarshad Vaghela
 
Sizing of relief valves for supercritical fluids
Sizing of relief valves for supercritical fluidsSizing of relief valves for supercritical fluids
Sizing of relief valves for supercritical fluidsAlexis Torreele
 
Steam ejector working principle
Steam ejector working principleSteam ejector working principle
Steam ejector working principleKarnav Rana
 
Mass transfer 192
Mass transfer  192Mass transfer  192
Mass transfer 192Mehtab Rai
 
Types and design of the towers trays
Types and design of the towers traysTypes and design of the towers trays
Types and design of the towers traysFertiglobe
 

What's hot (20)

Ejercicio acetona agua
Ejercicio acetona aguaEjercicio acetona agua
Ejercicio acetona agua
 
MASS TRANSFER OPERATION-DISTILLATION
MASS TRANSFER OPERATION-DISTILLATIONMASS TRANSFER OPERATION-DISTILLATION
MASS TRANSFER OPERATION-DISTILLATION
 
Gas Absorption Laboratory Experiment
Gas Absorption Laboratory ExperimentGas Absorption Laboratory Experiment
Gas Absorption Laboratory Experiment
 
Scale up of agitated vessels and static mixer
Scale up of agitated vessels and static mixerScale up of agitated vessels and static mixer
Scale up of agitated vessels and static mixer
 
Reporte practica 6 Separación Mecánica
Reporte practica 6 Separación Mecánica  Reporte practica 6 Separación Mecánica
Reporte practica 6 Separación Mecánica
 
Armfield Gas Absorption Column Experiment
Armfield Gas Absorption Column ExperimentArmfield Gas Absorption Column Experiment
Armfield Gas Absorption Column Experiment
 
Simulación y optimización
Simulación y optimización Simulación y optimización
Simulación y optimización
 
Chapter 6
Chapter 6Chapter 6
Chapter 6
 
Curso inciación a COCO Simulator y ChemSep - Simulación de procesos químicos ...
Curso inciación a COCO Simulator y ChemSep - Simulación de procesos químicos ...Curso inciación a COCO Simulator y ChemSep - Simulación de procesos químicos ...
Curso inciación a COCO Simulator y ChemSep - Simulación de procesos químicos ...
 
Estimacion de costes y rentabilidad
Estimacion de costes y rentabilidadEstimacion de costes y rentabilidad
Estimacion de costes y rentabilidad
 
VÁVULAS DE SEGURANÇA E ALÍVIO
VÁVULAS DE SEGURANÇA E ALÍVIOVÁVULAS DE SEGURANÇA E ALÍVIO
VÁVULAS DE SEGURANÇA E ALÍVIO
 
Boiler control system engineering
Boiler control system engineeringBoiler control system engineering
Boiler control system engineering
 
Design of thermosyphon reboiler
Design of thermosyphon reboilerDesign of thermosyphon reboiler
Design of thermosyphon reboiler
 
Sizing of relief valves for supercritical fluids
Sizing of relief valves for supercritical fluidsSizing of relief valves for supercritical fluids
Sizing of relief valves for supercritical fluids
 
Absorption process
Absorption processAbsorption process
Absorption process
 
Steam ejector working principle
Steam ejector working principleSteam ejector working principle
Steam ejector working principle
 
Mass transfer 192
Mass transfer  192Mass transfer  192
Mass transfer 192
 
Tiempo de-escurrimiento-pdf
Tiempo de-escurrimiento-pdfTiempo de-escurrimiento-pdf
Tiempo de-escurrimiento-pdf
 
Homogeneous Reactors
Homogeneous ReactorsHomogeneous Reactors
Homogeneous Reactors
 
Types and design of the towers trays
Types and design of the towers traysTypes and design of the towers trays
Types and design of the towers trays
 

Similar to Transparent Batch Reactor - Instruction Manual

Copy of jimma university institute of engineering and technology
Copy of jimma university institute of engineering and technologyCopy of jimma university institute of engineering and technology
Copy of jimma university institute of engineering and technologyDeginet Yossef
 
Hướng dẫn sử dụng testo 550
Hướng dẫn sử dụng testo 550Hướng dẫn sử dụng testo 550
Hướng dẫn sử dụng testo 550Tenmars Việt Nam
 
Robur calorio manual_en
Robur calorio manual_enRobur calorio manual_en
Robur calorio manual_encelo1964
 
Atlas-Copco-QAS-100. intruction manual.pdf
Atlas-Copco-QAS-100. intruction manual.pdfAtlas-Copco-QAS-100. intruction manual.pdf
Atlas-Copco-QAS-100. intruction manual.pdfLuis64166
 
Instruction Manual EOTECH CNVD-T3 | Optics Trade
Instruction Manual EOTECH CNVD-T3 | Optics TradeInstruction Manual EOTECH CNVD-T3 | Optics Trade
Instruction Manual EOTECH CNVD-T3 | Optics TradeOptics-Trade
 
iTime - Time and Attendance Manual
iTime - Time and Attendance ManualiTime - Time and Attendance Manual
iTime - Time and Attendance Manualamanodirect
 
Seminar report on foot step power generation
Seminar report on foot step power generationSeminar report on foot step power generation
Seminar report on foot step power generationJitendra Rajput
 
Haier l26 f6 l32f6 l42f6 sm oficial (1)
Haier l26 f6 l32f6 l42f6 sm oficial (1)Haier l26 f6 l32f6 l42f6 sm oficial (1)
Haier l26 f6 l32f6 l42f6 sm oficial (1)flillud
 
Aermec-HYDRONIC-SYSTEMS-en-AERMEC-0-catda665a68.pdf
Aermec-HYDRONIC-SYSTEMS-en-AERMEC-0-catda665a68.pdfAermec-HYDRONIC-SYSTEMS-en-AERMEC-0-catda665a68.pdf
Aermec-HYDRONIC-SYSTEMS-en-AERMEC-0-catda665a68.pdfReneJaqiRuna
 
2015-2016 MechanicalCivil Undergraduate Senior DesignWa.docx
2015-2016 MechanicalCivil Undergraduate Senior DesignWa.docx2015-2016 MechanicalCivil Undergraduate Senior DesignWa.docx
2015-2016 MechanicalCivil Undergraduate Senior DesignWa.docxeugeniadean34240
 
Kawasaki fh721 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh721 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh721 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh721 d 4 stroke air-cooled v-twin gasoline engine service repair ma...fujsjfjskekemmem
 
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...ufjjjsejfjksekm
 
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...ufujjdfjjskekemm
 
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...ufuusjjfjkskekmem
 
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...ufjdjfjkskefmme
 
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...fujsjefjkskeksmem
 
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...ufjjdfjkskemfmme
 

Similar to Transparent Batch Reactor - Instruction Manual (20)

Copy of jimma university institute of engineering and technology
Copy of jimma university institute of engineering and technologyCopy of jimma university institute of engineering and technology
Copy of jimma university institute of engineering and technology
 
[IJET V2I2P19] Authors: Pandey Anand, Baraiya Bhavesh, Pal Ranjit, Dubey Ashi...
[IJET V2I2P19] Authors: Pandey Anand, Baraiya Bhavesh, Pal Ranjit, Dubey Ashi...[IJET V2I2P19] Authors: Pandey Anand, Baraiya Bhavesh, Pal Ranjit, Dubey Ashi...
[IJET V2I2P19] Authors: Pandey Anand, Baraiya Bhavesh, Pal Ranjit, Dubey Ashi...
 
Hướng dẫn sử dụng testo 550
Hướng dẫn sử dụng testo 550Hướng dẫn sử dụng testo 550
Hướng dẫn sử dụng testo 550
 
434 15
434 15434 15
434 15
 
YCAJ_IOM
YCAJ_IOMYCAJ_IOM
YCAJ_IOM
 
Robur calorio manual_en
Robur calorio manual_enRobur calorio manual_en
Robur calorio manual_en
 
Atlas-Copco-QAS-100. intruction manual.pdf
Atlas-Copco-QAS-100. intruction manual.pdfAtlas-Copco-QAS-100. intruction manual.pdf
Atlas-Copco-QAS-100. intruction manual.pdf
 
Instruction Manual EOTECH CNVD-T3 | Optics Trade
Instruction Manual EOTECH CNVD-T3 | Optics TradeInstruction Manual EOTECH CNVD-T3 | Optics Trade
Instruction Manual EOTECH CNVD-T3 | Optics Trade
 
iTime - Time and Attendance Manual
iTime - Time and Attendance ManualiTime - Time and Attendance Manual
iTime - Time and Attendance Manual
 
Seminar report on foot step power generation
Seminar report on foot step power generationSeminar report on foot step power generation
Seminar report on foot step power generation
 
Haier l26 f6 l32f6 l42f6 sm oficial (1)
Haier l26 f6 l32f6 l42f6 sm oficial (1)Haier l26 f6 l32f6 l42f6 sm oficial (1)
Haier l26 f6 l32f6 l42f6 sm oficial (1)
 
Aermec-HYDRONIC-SYSTEMS-en-AERMEC-0-catda665a68.pdf
Aermec-HYDRONIC-SYSTEMS-en-AERMEC-0-catda665a68.pdfAermec-HYDRONIC-SYSTEMS-en-AERMEC-0-catda665a68.pdf
Aermec-HYDRONIC-SYSTEMS-en-AERMEC-0-catda665a68.pdf
 
2015-2016 MechanicalCivil Undergraduate Senior DesignWa.docx
2015-2016 MechanicalCivil Undergraduate Senior DesignWa.docx2015-2016 MechanicalCivil Undergraduate Senior DesignWa.docx
2015-2016 MechanicalCivil Undergraduate Senior DesignWa.docx
 
Kawasaki fh721 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh721 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh721 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh721 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
 
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
 
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
 
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh680 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
 
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh601 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
 
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
 
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
Kawasaki fh641 d 4 stroke air-cooled v-twin gasoline engine service repair ma...
 

Recently uploaded

(MEERA) Dapodi Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Escorts
(MEERA) Dapodi Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Escorts(MEERA) Dapodi Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Escorts
(MEERA) Dapodi Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Escortsranjana rawat
 
Top Rated Pune Call Girls Budhwar Peth ⟟ 6297143586 ⟟ Call Me For Genuine Se...
Top Rated  Pune Call Girls Budhwar Peth ⟟ 6297143586 ⟟ Call Me For Genuine Se...Top Rated  Pune Call Girls Budhwar Peth ⟟ 6297143586 ⟟ Call Me For Genuine Se...
Top Rated Pune Call Girls Budhwar Peth ⟟ 6297143586 ⟟ Call Me For Genuine Se...Call Girls in Nagpur High Profile
 
Sheet Pile Wall Design and Construction: A Practical Guide for Civil Engineer...
Sheet Pile Wall Design and Construction: A Practical Guide for Civil Engineer...Sheet Pile Wall Design and Construction: A Practical Guide for Civil Engineer...
Sheet Pile Wall Design and Construction: A Practical Guide for Civil Engineer...Dr.Costas Sachpazis
 
Introduction to Multiple Access Protocol.pptx
Introduction to Multiple Access Protocol.pptxIntroduction to Multiple Access Protocol.pptx
Introduction to Multiple Access Protocol.pptxupamatechverse
 
Coefficient of Thermal Expansion and their Importance.pptx
Coefficient of Thermal Expansion and their Importance.pptxCoefficient of Thermal Expansion and their Importance.pptx
Coefficient of Thermal Expansion and their Importance.pptxAsutosh Ranjan
 
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...ranjana rawat
 
Decoding Kotlin - Your guide to solving the mysterious in Kotlin.pptx
Decoding Kotlin - Your guide to solving the mysterious in Kotlin.pptxDecoding Kotlin - Your guide to solving the mysterious in Kotlin.pptx
Decoding Kotlin - Your guide to solving the mysterious in Kotlin.pptxJoão Esperancinha
 
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...Dr.Costas Sachpazis
 
Call Girls Service Nashik Vaishnavi 7001305949 Independent Escort Service Nashik
Call Girls Service Nashik Vaishnavi 7001305949 Independent Escort Service NashikCall Girls Service Nashik Vaishnavi 7001305949 Independent Escort Service Nashik
Call Girls Service Nashik Vaishnavi 7001305949 Independent Escort Service NashikCall Girls in Nagpur High Profile
 
College Call Girls Nashik Nehal 7001305949 Independent Escort Service Nashik
College Call Girls Nashik Nehal 7001305949 Independent Escort Service NashikCollege Call Girls Nashik Nehal 7001305949 Independent Escort Service Nashik
College Call Girls Nashik Nehal 7001305949 Independent Escort Service NashikCall Girls in Nagpur High Profile
 
Processing & Properties of Floor and Wall Tiles.pptx
Processing & Properties of Floor and Wall Tiles.pptxProcessing & Properties of Floor and Wall Tiles.pptx
Processing & Properties of Floor and Wall Tiles.pptxpranjaldaimarysona
 
Extrusion Processes and Their Limitations
Extrusion Processes and Their LimitationsExtrusion Processes and Their Limitations
Extrusion Processes and Their Limitations120cr0395
 
VIP Call Girls Service Hitech City Hyderabad Call +91-8250192130
VIP Call Girls Service Hitech City Hyderabad Call +91-8250192130VIP Call Girls Service Hitech City Hyderabad Call +91-8250192130
VIP Call Girls Service Hitech City Hyderabad Call +91-8250192130Suhani Kapoor
 
Microscopic Analysis of Ceramic Materials.pptx
Microscopic Analysis of Ceramic Materials.pptxMicroscopic Analysis of Ceramic Materials.pptx
Microscopic Analysis of Ceramic Materials.pptxpurnimasatapathy1234
 
UNIT-V FMM.HYDRAULIC TURBINE - Construction and working
UNIT-V FMM.HYDRAULIC TURBINE - Construction and workingUNIT-V FMM.HYDRAULIC TURBINE - Construction and working
UNIT-V FMM.HYDRAULIC TURBINE - Construction and workingrknatarajan
 
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur Escorts
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur EscortsCall Girls in Nagpur Suman Call 7001035870 Meet With Nagpur Escorts
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur EscortsCall Girls in Nagpur High Profile
 

Recently uploaded (20)

(MEERA) Dapodi Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Escorts
(MEERA) Dapodi Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Escorts(MEERA) Dapodi Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Escorts
(MEERA) Dapodi Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Escorts
 
Top Rated Pune Call Girls Budhwar Peth ⟟ 6297143586 ⟟ Call Me For Genuine Se...
Top Rated  Pune Call Girls Budhwar Peth ⟟ 6297143586 ⟟ Call Me For Genuine Se...Top Rated  Pune Call Girls Budhwar Peth ⟟ 6297143586 ⟟ Call Me For Genuine Se...
Top Rated Pune Call Girls Budhwar Peth ⟟ 6297143586 ⟟ Call Me For Genuine Se...
 
Roadmap to Membership of RICS - Pathways and Routes
Roadmap to Membership of RICS - Pathways and RoutesRoadmap to Membership of RICS - Pathways and Routes
Roadmap to Membership of RICS - Pathways and Routes
 
Sheet Pile Wall Design and Construction: A Practical Guide for Civil Engineer...
Sheet Pile Wall Design and Construction: A Practical Guide for Civil Engineer...Sheet Pile Wall Design and Construction: A Practical Guide for Civil Engineer...
Sheet Pile Wall Design and Construction: A Practical Guide for Civil Engineer...
 
Introduction to Multiple Access Protocol.pptx
Introduction to Multiple Access Protocol.pptxIntroduction to Multiple Access Protocol.pptx
Introduction to Multiple Access Protocol.pptx
 
Coefficient of Thermal Expansion and their Importance.pptx
Coefficient of Thermal Expansion and their Importance.pptxCoefficient of Thermal Expansion and their Importance.pptx
Coefficient of Thermal Expansion and their Importance.pptx
 
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...
 
Decoding Kotlin - Your guide to solving the mysterious in Kotlin.pptx
Decoding Kotlin - Your guide to solving the mysterious in Kotlin.pptxDecoding Kotlin - Your guide to solving the mysterious in Kotlin.pptx
Decoding Kotlin - Your guide to solving the mysterious in Kotlin.pptx
 
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...
 
Call Us -/9953056974- Call Girls In Vikaspuri-/- Delhi NCR
Call Us -/9953056974- Call Girls In Vikaspuri-/- Delhi NCRCall Us -/9953056974- Call Girls In Vikaspuri-/- Delhi NCR
Call Us -/9953056974- Call Girls In Vikaspuri-/- Delhi NCR
 
DJARUM4D - SLOT GACOR ONLINE | SLOT DEMO ONLINE
DJARUM4D - SLOT GACOR ONLINE | SLOT DEMO ONLINEDJARUM4D - SLOT GACOR ONLINE | SLOT DEMO ONLINE
DJARUM4D - SLOT GACOR ONLINE | SLOT DEMO ONLINE
 
Call Girls Service Nashik Vaishnavi 7001305949 Independent Escort Service Nashik
Call Girls Service Nashik Vaishnavi 7001305949 Independent Escort Service NashikCall Girls Service Nashik Vaishnavi 7001305949 Independent Escort Service Nashik
Call Girls Service Nashik Vaishnavi 7001305949 Independent Escort Service Nashik
 
College Call Girls Nashik Nehal 7001305949 Independent Escort Service Nashik
College Call Girls Nashik Nehal 7001305949 Independent Escort Service NashikCollege Call Girls Nashik Nehal 7001305949 Independent Escort Service Nashik
College Call Girls Nashik Nehal 7001305949 Independent Escort Service Nashik
 
Processing & Properties of Floor and Wall Tiles.pptx
Processing & Properties of Floor and Wall Tiles.pptxProcessing & Properties of Floor and Wall Tiles.pptx
Processing & Properties of Floor and Wall Tiles.pptx
 
9953056974 Call Girls In South Ex, Escorts (Delhi) NCR.pdf
9953056974 Call Girls In South Ex, Escorts (Delhi) NCR.pdf9953056974 Call Girls In South Ex, Escorts (Delhi) NCR.pdf
9953056974 Call Girls In South Ex, Escorts (Delhi) NCR.pdf
 
Extrusion Processes and Their Limitations
Extrusion Processes and Their LimitationsExtrusion Processes and Their Limitations
Extrusion Processes and Their Limitations
 
VIP Call Girls Service Hitech City Hyderabad Call +91-8250192130
VIP Call Girls Service Hitech City Hyderabad Call +91-8250192130VIP Call Girls Service Hitech City Hyderabad Call +91-8250192130
VIP Call Girls Service Hitech City Hyderabad Call +91-8250192130
 
Microscopic Analysis of Ceramic Materials.pptx
Microscopic Analysis of Ceramic Materials.pptxMicroscopic Analysis of Ceramic Materials.pptx
Microscopic Analysis of Ceramic Materials.pptx
 
UNIT-V FMM.HYDRAULIC TURBINE - Construction and working
UNIT-V FMM.HYDRAULIC TURBINE - Construction and workingUNIT-V FMM.HYDRAULIC TURBINE - Construction and working
UNIT-V FMM.HYDRAULIC TURBINE - Construction and working
 
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur Escorts
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur EscortsCall Girls in Nagpur Suman Call 7001035870 Meet With Nagpur Escorts
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur Escorts
 

Transparent Batch Reactor - Instruction Manual

  • 1. Transparent Batch Reactor Instruction Manual CEB-MkIII ISSUE 2 December 2011
  • 2. Table of Contents Copyright and Trademarks...................................................................................... 1 General Overview ....................................................................................................... 2 Equipment Diagrams................................................................................................... 3 Important Safety Information....................................................................................... 4 Introduction.............................................................................................................. 4 Water Borne Hazards.............................................................................................. 4 Electrical Safety....................................................................................................... 4 Hot Surfaces and Liquids ........................................................................................ 5 Chemical Safety ...................................................................................................... 5 Description .................................................................................................................. 6 The Reactor Vessel................................................................................................. 6 Installation................................................................................................................... 9 Advisory................................................................................................................... 9 Installation Process ................................................................................................. 9 Operation .................................................................................................................. 12 Operating the Software.......................................................................................... 12 Operating the Equipment....................................................................................... 22 Equipment Specifications.......................................................................................... 28 Environmental Conditions...................................................................................... 28 Routine Maintenance ................................................................................................ 29 Responsibility ........................................................................................................ 29 General.................................................................................................................. 29 RCD Test............................................................................................................... 29 Temperature sensors calibration........................................................................... 29 Calibration of the conductivity sensor.................................................................... 29 Laboratory Teaching Exercises................................................................................. 32 Index to Exercises ................................................................................................. 32 Nomenclature ........................................................................................................ 32 Common Theory.................................................................................................... 33 ii
  • 3. Table of Contents iii Exercise A - Isothermal Operation ............................................................................ 35 Exercise B - Reactant Concentration........................................................................ 41 Exercise C - Adiabatic Operation.............................................................................. 42 Contact Details for Further Information..................................................................... 45
  • 4.
  • 5. 1 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 Thursday: 0830 – 1730 and Friday 0830 - 1300 UK time). 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 © 2011 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.
  • 6. 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. Batch reactors are used widely in industry at all scales. Batch reactors are tanks, commonly provided with agitation and a method of heat transfer (usually by coils or external jacket). This type of reactor is primarily employed for relatively slow reactions of several hours duration, since the downtime for filling and emptying large equipment can be significant. Agitation is used to maintain homogeneity and to improve heat transfer. The Armfield CEB MkIII Transparent Batch Reactor is specially designed to allow detailed study of this important process. It is one of five reactors 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, CEY Plug Flow 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 and visually due to the use of indicators. CEXC fitted with CEB MkIII Transparent batch reactor Note: If CEB-MKIII is to be used with a CEX rather than CEXC, then optional temperature sensor ST54 will be required if it is required to measure reactor temperature (the temperature sensor supplied with CEX is used to control the hot water temperature in isothermal operation). 2
  • 7. Equipment Diagrams Figure 1: CEB MkIII Transparent batch reactor 3
  • 8. 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 CEB MkIII Transparent Batch Reactor 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. 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 45°C. 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 20°C. 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. 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 4
  • 9. Important Safety Information 5 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. Hot Surfaces and Liquids The unit incorporates a pumped electric water heater, and is capable of producing temperatures that could cause skin burns. Before disconnecting any of the pipes or tubing:  Stop all the pumps.  Leave time for the water to cool  Check that the temperature is at a safe level Do not touch any surfaces close to ‘Hot Surfaces’ warning labels, or any of the interconnecting tubing, whilst the equipment is in use. Chemical Safety Details of the chemicals intended for use with this equipment are given in the Operational Procedures 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 user’s 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.
  • 10. Description Where necessary, refer to the drawings in the Equipment Diagrams section. The Reactor Vessel The reactor vessel is a double skinned glass vessel with one litre and a half of internal working volume. It is set on a baseplate which is designed to be located on the four studs of the CEXC service unit and then secured by thumbnuts. The reactor is supported by three pillars; position the reactor on the CEXC service unit such that a single pillar is to the front. CEB MKII Transparent Batch Reactor Hot water from the CEXC or cold water from CW17 can be recirculated to the jacket for temperature control purposes. Either the hot water circulator or the CW-17 chiller is connected to the ‘Heater/Cooler attachments’. Note: the water inlet is at the bottom of the reactor jacket and the water outlet is at the top of the reactor jacket. A turbine agitator works to provide efficient mixing and heat transfer. The agitator is driven by an electric motor mounted on the lid of the reactor. The speed of the motor can be controlled by using Amrfield software interface. The socket for the electrical motor plug is sited at the rear of the service unit. 6
  • 11. Description Reactor Lid Glands in the reactor lid house the conductivity and temperature sensor provided with the CEXC service unit. The larger of the two glands is for the conductivity probe. The glands are unscrewed by hand, the sensors inserted completely into the reactor until they rest a few cm from the bottom and then the glands re-tightened by hand. Sockets at the rear of the service unit are provided to connect each sensor. The conductivity probe is connected to the 3 pin socket marked ‘HIGH COND’. The temperature sensor is connected to the k-thermocouple socket marked ‘T1’. Both temperature values and conductivity values are data logged using a PC in conjunction with the Armfield software interface. An additional temperature sensor ‘T2’ is supplied with CEXC that allows the Hot Water Circulator temperature to be also monitored. Therefore T2 temperature sensor must be immersed in the Hot Water Circulator vessel through the hole in the lid. There is an extra temperature ‘T3’ and ‘Low conductivity’ plug at the rear of the service unit with outputs on the software for extra connections made by the user. If solutions with low conductance are used, connect the conductivity probe to the socket marked as ‘LOW COND’ and conductivity values will be data logging more accurately in a low range. 7
  • 12. Armfield Instruction Manual 8 CEB MkIII Transparent Batch Reactor
  • 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 1. Mounting the CEB MKIII onto the CEXC  The reactor vessel is set on a baseplate which is itself located on four studs on the service unit and secured by thumbnuts. The feed bottles provided with CEXC are not required with the batch reactor configuration.  Plug the temperature sensor and conductivity sensor supplied with CEXC into the appropriate sockets at the rear of the service unit then insert the sensors through the appropriate glands in the lid of the reactor. Check that the sensors are fully immersed then tighten the glands.  Connect the stirrer plug to the socket located on the rear of the CEXC. 2. Connecting the HWC to CEB MKIII 9
  • 14. Armfield Instruction Manual  Connect return pipe of the HWC (1) to the connection at the top of the reactor vessel.  Connect the supply pipe of the HWC (2) to the connection at the bottom of the reactor vessel. 3. Connection to electricity supply  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 circuit breakers and RCD are 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. 4. Connection to data logger  Connect CEXC to a PC using the USB cable supplied.  Insert the CEB MkIII 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.  Follow the instructions on screen 10
  • 15. Installation 11  Run the software 5. Priming the hot water circulator (HWC)  Fill HWC vessel with water up to the low level tip (30 cm from top).  Switch on the Hot Water Circulator and Power On. Level of water in the vessel will decrease as reactor jacket is filled. Keep filling the HWC vessel until the level in the vessel is stable and over the Low level tip.
  • 16. 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 12
  • 17. Operation the IFD5 and the PC and confirm that the red and green LED’s 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. 13
  • 18. Armfield Instruction Manual 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: The details in the diagram will vary depending on the equipment chosen if multiple experiments are available. 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. 14
  • 19. Operation 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%, 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. 15
  • 20. Armfield Instruction Manual 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 icon from the main toolbar. One set of data will be recorded each time the icon is clicked. Automatic logging is selected when transients need to be recorded so that they can be plotted against time. Click the icon from the toolbar to start recording, click the icon from the toolbar to stop recording. The type of logging can be configured by clicking Configure in the Sample drop- down 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: 16
  • 21. Operation Tabular Display To view the Table screen click the View Table icon from the main tool bar or click Table from the View dropdown menu as shown: The data is displayed in a tabular format, similar to the screen as shown: 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. 17
  • 22. Armfield Instruction Manual Graphical Display When several samples have been recorded, they can be viewed in graphical format. To view the data in Graphical format click the View graph icon from the main tool bar or click Graph from the View drop-down menu as shown: 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. 18
  • 23. Operation 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: 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: 19
  • 24. Armfield Instruction Manual 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 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: 20
  • 25. Operation 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. 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: 21
  • 26. Armfield Instruction Manual 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. 22
  • 27. Operation Operation Hot Water Circulator The hot water circulator vessel should be filled with water before use, and drained after use if the equipment is not going to be used for some time. When use fill the vessel by pouring clean (preferably demineralised) water until the level is approximately 20 mm from the top. Top up the level of this vessel as necessary to maintain the level above the tip of the level electrode (typically 20 mm from the top of the vessel). Heater is controlled from a PC via the CEB software. A PID controller within the software maintains the heater setting based on the temperature measured by the chosen temperature sensor. The Set Point temperature, proportional Band and the Integral and Derivative times may be adjusted by the user. Alternatively the heater power setting may be entered manually as a percentage value, using the same controller window as for the PID settings. Operation of Data Logger and Software The Armfield CEB MkIII reactor is controlled using the CEB MkIII software supplied, which allows real-time monitoring and data logging of all sensor outputs and control of the heater unit. 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 > CEB). 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 includes controls for the stirrer and the Hot water Circulator. The stirrer is controlled from the software using the up/down buttons or typing in directly a value between 0 and 100 %. Concentration and volume values must be filled in the boxes on each experiment so that software will carry out the convenient calculations. 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. 23
  • 28. Armfield Instruction Manual Controlling the HWC The heater is controlled by a controller in the software. Click on the appropriate CONTROL symbol to open the controller window. 24
  • 29. Operation Control can be either closed loop (Automatic) which uses the temperature sensor immediately following the heater as the process variable in a PID loop, or open loop (Manual) where the user defines the percentage time the heaters are ‘ON’ for, and hence the output power. When performing a reaction it is best to use Automatic control as this produces stable temperatures most rapidly, and maintains these conditions by varying the heater power. Operating the CEB MkIII There are two modes of operation with the CEB batch reactor: Isothermal and Adiabatic operation. The temperature and conductivity sensors must be situated well below the liquid surface inside the reactor. Isothermal Operation When operating isothermally the temperature sensor T2 supplied with CEXC should be set as the temperature sensor to be controlled in the PID loop box on the software. This sensor must be immersed in the vessel of the Hot Water Circulator. On the other hand the other temperature sensor T1 is used to monitor the reaction temperature during the experiments. PID settings need to be adjusted to suit the experiment conditions. When using the Chiller CW-17 PID settings are not required. See the installation guide for appropriate controller settings when using the CW-17. In the case of Isothermal Operation the PID settings recommended are: 25
  • 30. Armfield Instruction Manual Note these values are suitable when the controlling sensor is T2 which is fitted in the HWC vessel. The setpoint can be varied as required to suit the experiment. Adiabatic Operation When operating the batch reactor adiabatically, temperature control is not required so either Chiller or HWC are not required. The contents of the reactor are stirred by an agitator which is driven by an electrical motor/gearbox combination mounted on the lid. The motor is connected to the electrical supply by a jack plug which is plugged into a socket at the rear of the CEXC service unit. The agitator speed is adjusted using the Armfield software interface supplied with the reactor. See mimic Adiabatic Operation Diagram below. 26
  • 31. Operation 27 Ensure that protective gloves are worn when handling any of the substances used in the reactor. Once the experiment is finished wash the reactor with distilled water.
  • 32. Equipment Specifications 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; 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 (over- voltage) 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 28
  • 33. 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 re- calibration. However should calibration become necessary follow the below procedure. This should only be done once the unit has fully warmed up. The temperature 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). 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. If a thermocouple calibrator is available: Connect Thermocouple calibrator simulator to T1 input socket. Set to 25ºC and adjust VR1 (T1 ZERO) and VR2 (T1 SPAN) on the PCB to give 25ºC displayed on PC. Check accuracy at 15º and 40ºC. Repeat the same procedure for T2 by adjusting VR3 (T2 ZERO) and VR4 (T2 SPAN) on the PCB to give 25ºC displayed on PC, and VR5 (T3 ZERO) and VR6 (T3 SPAN) for T3. 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 0ºC, then sensors should be dipped into boiling water and then adjust the SPANS to 100ºC. Calibration of the conductivity sensor 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 29
  • 34. Armfield Instruction Manual 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. High conductivity Calibration Fill a small beaker with a Conductivity standard solution (e.g. 0.1M KCI giving a conductivity of 12.88 mS at 25°C) 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 Fill a small beaker with a Conductivity standard solution (e.g. 0.01M KCI giving a conductivity of 1.41mS at 25°C) 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. 12.88 mS/cm at 25ºC 0.1 M KCl ºC mS/cm ºC mS/cm 5 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 30
  • 35. Routine Maintenance 31 18 11.19 25 12.88 19 11.43 26 13.13 1.413 mS/cm at 25ºC 0.01 M KCl ºC mS/cm ºC mS/cm 5 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
  • 36. Laboratory Teaching Exercises Index to Exercises Exercise A - Isothermal Operation Exercise B - Reactant Concentration Exercise C - Adiabatic Operation Nomenclature Symbol Name Unit ao initial sodium hydroxide conc. (mol/dm3 ) a1 sodium hydroxide conc. in reactor at time t (mol/dm3 ) sodium hydroxide conc. in reactor after time (mol/dm3 ) b ethyl acetate conc. (mol/dm3 ) (same subscripts as above for a) c sodium acetate conc. (mol/dm3 ) (same subscripts as above for a) C acetic anhydrite conc. at time t (mol/dm3 ) C0 acetic anhydrite conc. at t = 0 k specific rate constant r reaction rate (s) tr reaction time (s) t elapsed time (s) T reactor temperature (K) V volume of reactor (dm3 ) Xa conversion of sodium hydroxide = Xc conversion to sodium acetate = 32
  • 37. Laboratory Teaching Exercises conductivity (Siemens/cm) initial conductivity conductivity at time t conductivity after time sodium hydroxide conductivity sodium acetate conductivity k0 Arrhenius frequency factor E Activation energy (J/mol) R gas constant (J/mol K) ρ density (kg/dm3 ) H molar enthalpy (J/mol) mean heat capacity (J/kg K) Common Theory The Armfield batch reactor is designed to demonstrate the mechanism of a chemical reaction in a reactor, as well as the effects of varying process conditions such as reaction temperature, reagent concentrations etc. The reaction chosen for the isothermal demonstration is the saponification of ethyl acetate by sodium hydroxide, as it can be carried out under safe conditions of temperature and pressure and is well documented. The use of indicators allows to follow the reaction by changing the colour as the reaction takes place. The reaction chosen for the adiabatic demonstration is the hydrolysis of acetic anhydride. This involves the use of glacial acetic acid and sulphuric acid as well as acetic anhydride. Although it may be possible to carry out demonstrations using other chemicals, it is not advisable as the materials of construction of the reactor may not be compatible. Before carrying out reactions involving any other reagents please refer to Armfield Ltd. for advice. Dilution of Ethyl Acetate for use with CEB MKII Batch Reactor Armfield recommends the use of a 0.1M solution of Ethyl Acetate in the CEB MkII reactor. This should be made by diluting concentrated Ethyl Acetate as follows: 33
  • 38. Armfield Instruction Manual 34 Therefore add 4.895 ml of concentrated Ethyl Acetate to 400 ml of deionised or distilled water. Shake the mixture vigorously until the two liquids have mixed. Add further water to make up the final volume to 500 ml. Note: The practice of making a strong solution (e.g. 1M) then further diluting this to the required concentration (e.g. 0.1M) cannot be applied when using Ethyl Acetate. The required dilution should be made directly as stated above. To get the colourful solution add 0.00394 gr of Crystal Violet to the 500 ml of Ethyl Acetate to make up a final solution of 1·10-5Mol/l of CV when both reagents are mixed. Dilution of Sodium Hydroxide for use with CEB MKII Batch Reactor Armfield recommends the use of a 0.1M solution of Sodium Hydroxide in the CEB MkIII reactor. This may be made by adding 50ml of NaOH 1M to 450 ml of distilled water then making up the solution to 500ml.
  • 39. Exercise A - Isothermal Operation Objective To find the reaction rate constant in a stirred batch reactor. Theory The reaction: NaOH + CH3COOC2H5 → CH3COONa + C2H5OH Sodium Hydroxide + Ethyl Acetate → Sodium Acetate + Ethyl Alcohol Assuming that the initial concentrations are equal and that the amount of reagent used up after time t is X then the concentrations at time t are: NaOH + CH3COOC2H5 → CH3COONa + C2H5OH a-X + a-X → X + X From the kinetic analysis of a general second order reaction it can be shown that: (1) where k is the reaction rate constant and t is the time of reaction. Using notation from the nomenclature: substituting for X in equation (1) above gives: Hence a plot of against t gives a straight line of gradient k. Method Make up 0.5 litre batches of 0.1M sodium hydroxide and 0.5 of 0.1M ethyl acetate (containing 1·10-5 Mol/l Crystal Violet) IMPORTANT: It is essential when handling these chemicals to wear protective clothing, gloves and safety spectacles. Open Armfield Software and choose ‘Isothermal operation’ Set up the Hot Water Circulator as detailed in the Operation section. Adjust settings on the PID loop as detailed in Operation procedure for Isothermal Operation and set point to 25°C. 35
  • 40. Armfield Instruction Manual Charge the batch reactor with 0.5 litres of the sodium hydroxide solution. Set the reactor agitator to '50%' and press ‘Power on’ to start the agitation. Then press ‘Hot Water Circulator’ and water will start to recirculate through jacket reactor and vessel. As the experiment involves the collection and storage of conductivity data, the data output port in the plinth must be connected to the computer with Armfield Interface data logger. This will enable data logging of the conductivity, temperatures and stirrer speed values at selected time intervals over a selected period. Ensure the conductivity and temperature sensors have both been installed in accordance with the Installation section. Collection of data will be until a stable condition is reached in the reactor and this takes approximately 30 minutes. It is advisable to set the data collection period to, say, 45 minutes. Switch on the Hot Water Circulator. The temperature of the sodium hydroxide in the reactor vessel will begin to rise and will be automatically maintained at the desired set-point (25o C in this instance) by the action of the HWC in the jacket. Carefully add to the reactor 0.5 litres of the ethyl acetate solution and instigate the data logger program (or begin taking readings if no computer is being used). It has been determined that the degree of conversion of the reagents affects the conductivity of the reactor contents. By recording the conductivity with respect to time, either manually or using the Armfield Data Logger, the amount of conversion can be calculated. If time permits the experiment should be repeated as above but with the temperature controller set to 35°C, or at other temperatures below room temperature like 15ºC. It is also recommended to repeat the experiment at another stirrer speed to study the effect of the mixing on conversion. When temperature is below room temperature, the use of a Chiller is required. Connect the Chiller system as detailed in the OPERATIONAL PROCEDURES section of the CEXC manual. It is recommended to fit the CEXC temperature probe T2 into the HWC vessel hole for better PID control, as described in Isothermal operation section, and the use of the T1 temperature sensor also supplied to follow the temperature in the reactor. Interpretation of results Armfield Interface data logger performs all the calculations while the experiment takes place. However if better understanding of the experiment is needed, follow below procedure to calculate the specific rate constant and effect of the temperature on the specific rate constant. Having recorded the conductivity of the contents of the reactor over the period of the reaction, the conductivity measurements must now be translated into degree of conversion of the constituents. Both sodium hydroxide and sodium acetate contribute conductance to the reaction solution whilst ethyl acetate and ethyl alcohol do not. The conductivity of a sodium hydroxide solution at a given concentration and temperature however, is not the same as that of a sodium acetate solution at the same molarity and temperature and 36
  • 41. Exercise A a relationship has been established allowing conversion to be inferred from conductivity: 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, the set of readings of conductivity with time will need to be transferred to the computer as two columns of data. Now enter the following known constants from the experiment using the Nomenclature. Ensure use of correct units. a = (Sodium Hydroxide conc. in feed bottle) a0 = (Sodium Hydroxide conc. in mixed feed) = b = (Ethyl acetate conc. in feed bottle) b0 = (Ethyl acetate conc. in mixed feed) = c = T = (Reactor temperature, T1) V = (Total volume in the reactor vessel) Using the spreadsheet, calculate the values of from the following formulae: For the values of each of the above, the spreadsheet can be used to calculate values of sodium hydroxide concentration (a1) and sodium acetate concentration (c1) and 37
  • 42. Armfield Instruction Manual the degree of conversion (Xa) and (Xc) for each of the samples of conductivity taken over the period of the experiment. These can be calculated and listed in columns (use spreadsheet COPY facility) alongside the readings of conductivity using the following equations: The concentration of NaOH can be plotted against time: To calculate the specific rate constant, k: 38
  • 43. Exercise A It is recommended that this experiment be repeated at various other reactor temperatures to investigate the relationship between the specific rate constant k and the temperature of reaction. The effect of temperature on the reaction rate constant is determined by the activation energy of such a reaction, through the Arrhenius law: k = k0 e-E/RT where k0 is the frequency factor, E is the activation energy, R is the ideal gases constant and T is the absolute temperature. Once the kinetic constant at three different temperatures is known, for instance 15ºC, 20ºC and 25ºC, is straightforward to apply the Arrhenius law and calculate the frequency factor and the activation energy values for: 39
  • 44. Armfield Instruction Manual 40 Obtaining the reaction rate constant in function of the temperature: High activation energy implies a significant sensibility of the reaction kinetics to the temperature.
  • 45. Exercise B - Reactant Concentration Objective To determine the effect of reactant concentration on the reaction rate. Theory In homogenous reaction systems, reaction rates depend on the concentration of the reactants. Collision theory indicates a rate increase if the concentration of one or both of the reactants is increased. 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 is: where: r = reaction rate k = rate constant [A]n , [B]m = molar concentrations of reactants n, m = appropriate powers (based on experimental data) Method Use the same procedure as for Exercise A. Run the experiment using different initial concentrations of the reagents, for example, 0.1M, 0.08M and 0.02M. 0.5 litre of each solution will be required for each mixture tested. Using the Armfield Data Logger in each experiment, graphs can be plotted relating reaction rate to concentration level for each of the reactants tested. A logarithmic plot of reaction rate to concentration level will give a straight line of slope equal to the power of the relationship. Hence the rate law for sodium hydroxide and ethyl acetate can be written in the form 41
  • 46. Exercise C - Adiabatic Operation WARNING: 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. DO NOT add acetic anhydride directly to sulphuric acid, as the reaction is violent and will cause the chemicals to be sprayed into the air. The reaction described in this experiment should be carried out in a fume cupboard. On completion, the reaction products should be discarded according to local regulations (for example into a copious flow of cold water to a suitable drain), taking care to avoid inhalation of vapour. Objective To determine the rate equation for the hydrolysis of acetic anhydride to acetic acid in an adiabatic reactor. Theory The hydrolysis of acetic anhydride in water, in the presence of a catalyst of sulphuric acid is described by: This reaction can be assumed to have simple power law kinetics of the form , if the reaction is zero order in water. The concentration of the protonic acid remains constant for the duration of the run and thus k is a catalytic rate constant that includes this concentration, also in power law form. For any system of this particular type the instantaneous value of the acetic anhydride concentration can be eliminated between the material and thermal balance equations to give a linear equation (which can therefore be subjected to a statistical test). Use of this equation requires that values of the gradient of temperature with respect to time be found. If the concentration of acetic anhydride at any time t is C, then the rate of the reaction is given by: (1) with C = C0 at t = 0. The heat generation rate is: (2) with T = T0 at t = 0. Substituting equation (1) in equation (2), integrating with respect to time and using the boundary conditions, we obtain: (3) For the n-th order case, the rate may be expressed in Arrhenius form: 42
  • 47. Exercise C (4) Using and rearranging, equation (3) becomes: Using equations (4) and (2), we obtain: (5) Using when the reaction is complete gives: Substituting for  in equation (5) and rearranging, we have: Taking logarithms of both sides of this equation gives: (6) and so a plot of ln(LHS) vs. 1/T should be linear with an intercept of ln(A) and a gradient of . Method Ensure the reactor has been set up with the special temperature sensor and computer interface for the adiabatic reaction as described in the Installation section. If possible the reactants should be at approximately 30°C before mixing. If they are cooler than this, the reaction will take much longer to complete. Charge the reactor with 100ml of acetic anhydride and 250ml of demineralised water. Start the reactor agitator and adjust the variable speed drive to position '5.0'. Add 150ml of glacial acetic acid (since the water and acetic anhydride are mutually insoluble, but are both soluble in acetic acid, this ensures that the reaction mixture is homogeneous - the acetic acid does not form part of the reaction). 43
  • 48. Armfield Instruction Manual 44 Start the data logger program choosing 15 seconds as the interval between samples and 1500 seconds as the total running time of the experiment (a longer duration will be required if the temperature of the reactants is less than 30°C). It is essential to log data until the temperature in the reactor begins to fall again. Immediately add 25ml of 0.5M sulphuric acid as the catalyst. The reaction will commence. Switch off the agitator. When the reaction has completed, the temperature data can be viewed within the software, either in tabular or graphical format. The data should be saved as an excel file. It is then possible to carry out the second part of the analysis described above, by calculating the terms of equation (6), and plotting the graph. In order to find dT/dt, it will be necessary to extract the linear region of data from a graph of temperature vs. time for the experiment. This will entail discarding the first few points, and also any points after the temperature reaches the peak value. See figure below Several runs similar to that described above should be performed, using differing quantities of sulphuric acid catalyst (e.g. 15ml to 40ml in 5ml increments). It will then be necessary to find the best value for n in equation (6) by trial and error, refining the value until the best straight line fit is obtained.
  • 49. 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 45