I need you to write about the safety in this lab report. please include all important safety point in the attachment. i need complete sentences (paragraphs). don’t copy them exactly! but paraphrase with out changing the meaning of sentences (ur own words.Also, i need a method analysis section, see figure attached for more about how to write this section.CEM file is where u get the safety and other info. u dont need outside refernces. ASK IF U HAVE A QUESTION.
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cem_mkii_issue_20_instruction_manual.pdf
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Continuous Stirred Tank Reactor
Instruction Manual
CEM-MKII
ISSUE 20
September 2013
Table of Contents
Copyright and Trademarks ………………………………………………………………………….. 1
Use with CEX Service Unit……………………………………………………………………………… 2
General Overview …………………………………………………………………………………………. 3
Equipment Diagrams……………………………………………………………………………………… 4
Important Safety Information…………………………………………………………………………… 5
Introduction……………………………………………………………………………………………….. 5
Water Borne Hazards …………………………………………………………………………………. 5
Electrical Safety…………………………………………………………………………………………. 6
Hot Surfaces and Liquids ……………………………………………………………………………. 6
Chemical Safety ………………………………………………………………………………………… 6
Description …………………………………………………………………………………………………… 7
Overview…………………………………………………………………………………………………… 7
Flow of materials ……………………………………………………………………………………….. 7
Installation ……………………………………………………………………………………………………. 9
Advisory……………………………………………………………………………………………………. 9
Installing the PC Software …………………………………………………………………………… 9
Installing the Equipment ……………………………………………………………………………… 9
Operation …………………………………………………………………………………………………… 12
Operating the PC Software………………………………………………………………………… 12
Operating the Equipment…………………………………………………………………………… 12
Equipment Specifications……………………………………………………………………………… 17
Overall Dimensions ………………………………………………………………………………….. 17
Environmental Conditions………………………………………………………………………….. 17
Routine Maintenance …………………………………………………………………………………… 18
Responsibility ………………………………………………………………………………………….. 18
General…………………………………………………………………………………………………… 18
RCD Test………………………………………………………………………………………………… 18
Temperature sensor calibration………………………………………………………………….. 18
Calibration of the conductivity sensor………………………………………………………….. 18
ii
Table of Contents
Laboratory Teaching Exercises……………………………………………………………………… 21
Index to Exercises ……………………………………………………………………………………. 21
Nomenclature ………………………………………………………………………………………….. 21
Common Theory………………………………………………………………………………………. 22
Exercise A – To find the reaction rate constant in a Continuous Stirred Tank Reactor
…………………………………………………………………………………………………………………. 24
Exercise B – To determine the effect of inadequate mixing on the reaction rate……. 29
Exercise C – Determination of the Residence Time using tracer techniques ………… 30
Contact Details for Further Information …………………………………………………………… 33
iii
Disclaimer
This document and all the information contained within it is proprietary to Armfield
Limited. This document must not be used for any purpose other than that for which it
is supplied and its contents must not be reproduced, modified, adapted, published,
translated or disclosed to any third party, in whole or in part, without the prior written
permission of Armfield Limited.
Should you have any queries or comments, please contact the Armfield Customer
Support helpdesk (Monday to 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: [email protected]
Fax: +44 (0) 1425 470916
Copyright and Trademarks
Copyright © 2013 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.
1
Use with CEX Service Unit
This instruction manual describes the use of the CEM-MKII Reactor in conjunction
with the CEXC Computer Controlled Service Unit.
An alternative instruction manual is available from Armfield that describes the use of
the CEM-MKII in conjunction with the CEX Service Unit. Please contact Armfield if a
copy of this instruction manual is required. Contact details are included later in this
document.
2
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.
The continuous stirred tank reactor in the form of either a single tank or (more often)
tanks in series, is used widely and is particularly suitable for liquid phase reactions. It
is particularly used in the organic chemicals industry. Advantages include consistent
product quality, straightforward automatic control and low manpower requirements.
The Armfield CEM MkII Continuous Stirred Tank Reactor is specially designed to
allow detailed study of this important process. It is one of five reactor types which are
interchangeable on the Reactor Service Unit (CEXC), the others being CET MkII Tubular Reactor, CEB MkIII – Transparent Batch 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 by temperature.
CEXC fitted with CEM MkII Continuous Stirred Tank Reactor
3
Equipment Diagrams
Figure 1: Reactor Unit
4
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 CEM-MKII Continuous Stirred Tank 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.
5
Armfield Instruction Manual
Electrical Safety
The equipment described in this Instruction Manual operates from a mains voltage
electrical supply. It must be connected to a supply of the same frequency and voltage
as marked on the equipment or the mains lead. If in doubt, consult a qualified
electrician or contact Armfield.
The equipment must not be operated with any of the panels removed.
To give increased operator protection, the unit incorporates a Residual Current
Device (RCD), alternatively called an Earth Leakage Circuit Breaker, as an integral
part of this equipment. If through misuse or accident the equipment becomes
electrically dangerous, the RCD will switch off the electrical supply and reduce the
severity of any electric shock received by an operator to a level which, under normal
circumstances, will not cause injury to that person.
At least once each month, check that the RCD is operating correctly by pressing the
TEST button. The circuit breaker MUST trip when the button is pressed. Failure to
trip means that the operator is not protected and the equipment must be checked and
repaired by a competent electrician before it is used.
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
Operation section. Chemicals purchased by the user are normally supplied with a
COSHH data sheet which provides information on safe handling, health and safety
and other issues. It is important that these guidelines are adhered to.
6
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.
Overview
The reactor vessel 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.
A stainless steel coil inside the reactor provides the heat transfer surface for either
heating or cooling the chemical reactants. The coil is connected either to the hot
water circulator (for exercises above ambient temperature) or the optional CW-17
chiller. The coil inlet is at the front of the reactor and the coil return is at the rear of
the reactor (for exercises below ambient temperature).
A stirrer (turbine agitator) works in conjunction with a baffle arrangement to provide
efficient mixing and heat transfer. The stirrer is driven by an electric motor mounted
in the lid of the reactor. The motor is controlled by the software supplied with the
Service Unit. The electrical socket for the motor is located at the rear of the service
unit.
Glands in the reactor lid house the conductivity and temperature sensors provided
with the service unit. The larger of the two glands is for the conductivity probe. The
glands are unscrewed by hand, the probes inserted completely into the reactor until
they rest on the reactor base and then the glands re-tightened by hand. Electrical
sockets at the rear of the service unit are provided to connect each probe. These are
of different size so that the probes cannot be wrongly connected. The conductivity
probe can be connected to low or high conductivity channels to suit the range of
measurements expected. For normal use the probe should be connected to the high
conductivity channel.
Flow of materials
The two feed pumps on the service unit pump the chemical reagents from the two
feed bottles into the reactor separately through connectors in the base of the reactor.
As reagents are pumped into the reactor, the level increases until it finally overflows
the stand pipe and flows to drain. The stand pipe may be adjusted in height by
loosening the hexagonal gland nut. A mark is etched onto the stand pipe. For
maximum operating volume of the reactor, this mark should be aligned with the gland
nut. A stop prevents the stand pipe from being completely removed, and this also
defines the minimum working volume which is half of the maximum volume.
When the reactor is not being used, it can be drained using the valve sited on the
underside of the reactor.
7
Armfield Instruction Manual
CEM MKII Continuous Stirred Tank Reactor
8
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.
Installing the PC Software
Before operating CEM-MKII it will be necessary to install the software from the CDROM supplied with CEXC onto an appropriate PC (PC not supplied).
For instructions on how to install and run the software insert the CD-ROM into the
optical drive on the PC (PC not supplied) then choose ‘Help’ from the menu.
After installing and running the software on the PC, instructions on how to operate
the software can be obtained by choosing the ‘Help’ tab in the top right hand corner
of the screen as shown below:
Note that when operating the software for the first time it will be necessary to enable
the USB virtual COM port by choosing the Red telephone icon (Start COM session).
Full instructions about enabling the port are included in the Help menus.
Installing the Equipment
Mounting the CEM MKII onto the CEXC
Fit the CEM-MKII assembly to the CEXC using the 4 locating studs and black
thumbnuts. The reactor is supported by 3 pillars; position the reactor on the
CEXC so that a single pillar support is at the front.
Connect the two flexible pipes from the feed pumps to the connectors on the
base of the reactor as shown.
Connect the electrical plugs from the conductivity probe, temperature sensors
T1 & T2 and the stirrer to the sockets located on the rear of the CEXC. For
normal use the conductivity probe should be connected to the socket marked
9
Armfield Instruction Manual
‘High Conductivity’. If measured values will not exceed 5 mS/cm then the Low
Conductivity input can be used to improve accuracy.
Fit the conductivity probe and temperature sensor to the appropriate gland on
the lid of the CEM-MKII reactor ensuring that they reach the bottom of the
reactor. The gland nut should be loosened prior to fitting the probe / sensor
then tightened to secure them.
CEXC fitted with CEM MkII Continuous Stirred Tank Reactor
Connection to the Hot Water Circulator
Connect return pipe of the HWC (1) to the connection for the top of the coil
(rear).
Connect the supply pipe of the HWC (2) to the connection for the bottom of
the coil (front)
Connection to Electricity Supply
Check the voltage specified on the equipment matches the supply voltage.
Note: this unit must be earthed.
10
Installation
Connect the power socket at the rear of the plinth to a suitable mains
electricity supply.
Ensure the circuit breakers and RCD are switched to ON (up position).
The on/off switch for the apparatus is located on the orange panel on the front
of the plinth.
Connection to a PC for Control and Data Logging
Ensure that the software has been installed as described in the section ‘Installing the
PC software’.
Switch on the PC and connect the USB lead from the CEXC to the PC.
Load the CEM software then choose the appropriate experiment from the menu. For
detailed information about operating the software refer to the section Operating the
PC Software.
Display the mimic diagram by choosing View then Diagram or via the mimic diagram
icon from the top toolbar:
If operating the software for the first time enable the virtual COM port using the red
telephone icon in the top toolbar:
Refer to the section Operating the PC Software if necessary.
Connect the mains supply to the CEXC then switch on the CEXC. Click the ‘Power
On’ button on the mimic diagram:
Confirm that the appropriate measured variables are displayed on the mimic
diagram.
The software and equipment are ready for use.
11
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 PC Software
Details about operating the software can be obtained by choosing the ‘Help’ tab in
the top right hand corner of the screen as shown below:
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 before hand. Both
the temperature controller and conductivity display should illuminate.
Filling the feed bottles
Unscrew the feed bottle caps and pour appropriate reagent solutions in using a
suitable funnel if necessary.
Operating the Hot Water Circulator
The hot water circulator vessel should be filled with clean water before use, and
drained after use if the equipment is not going to be used for some time. When in use
fill the vessel by pouring clean (preferably demineralised) water into the vessel until
the level is approximately 30mm from the top. Click the ‘Hot Water Circu …
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