OHS026
1. Completed by: Justin Nash/Toby
Jackson
Safe work procedure
The Writing Safe Work Procedures Guideline (OHS027) should be consulted to assist in the completion of this form
Faculty/Division:
Science
Document number
F10-SWP-139
School/Unit:
Chemistry
Initial Issue date
29th November 2011
Current version
V1.1.
Current Version
Issue date: 29th November 2011
Next review date:
29th November 2013
2.Safe work procedure title and basic description of activity
Title: The use of CEM Microwave Reactor
Description of activity:Microwave assisted organic synthesis using a CEM Explorer Microwave
instrument.
Reaction mixtures are loaded to dedicated microwave tubes (not more than 5 mL per tube). These tubes are placed in a
carrousel and a unique heating profile can then be programmed for each experiment using the CEM Synergy Software.
The tubes are sequentially loaded into the reactor via a robotic arm. The reactor cools each tube on completion of a run
using compressed air and returns it to it’s original position in the carousel. The tubes can then be collected and the
reaction worked up by the user.
3.List Hazards and risk controls as per risk assessment
Associated risk
assessment
number and
location:
F10-RA-139
See School of
Chemistry Safety
Page and Faculty
of Science
Database
Hazards
Controls
Hazards from
handling chemicals,
Spills/chemical
exposure to
Corrosive, Toxic
Flammable,
Oxidising and
Chemicals with
unknown properties.
Consult MSDS for all chemicals used and fill in the corresponding School
of Chemistry Risk assessment form. Appropriate training. First aid on site.
Appropriate PPE (safety glasses/goggles, lab coat, gloves).
Carry out procedure in a fume cupboard/ventilated laboratory.
Keep chemical quantities to the minimum required.
Isolate sources of ignition and ensure fire equipment is available and
operational.
Ensure all lab systems are operational.
Ensure a spill kit is available
Physical injury due to
glassware, sharp
edges, cracks, broken
glass
Appropriate training. Inspect all glassware before handling. Correct use of
glassware. Use gloves preferably leather and other appropriate PPE such as
protective safety glasses and a laboratory coat.
Fire or electrocution
from electricity
Ensure the equipment has been tested (every 12 months – check tag). Visually
check condition of power lead. Use an RCD socket.
Pressure/
Explosion
Only use the dedicated vials sealed with caps. Check before use.
Don’t overfill vials,. Inbuilt pressure venting ( IntelliVentT Pressure System).
Carefully remove caps in a fume cupboard. PPE: Safety glasses, labcoat, gloves
Inline pressure regulator.
Heat
Cooling cycle on reaction run.
Microwave Radiation
Contained microwave source with automatic cut out safety features preventing
direct exposure
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OHS026 safe work procedure
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4.List resources required including personal protective clothing, chemicals and equipment needed
PPE: Safety glasses/goggles (as per MSDS), Lab Coat, Compatible Gloves.
Microwave tube & cap – Available individually from the Chemistry Stores
5.List step by step instructions or order for undertaking the task
Sample Preparation:
NOTES:
 The microwave uses a sealed tube (as indicated above), in which reactions on the scale of 200 μL up to a
maximum of 5 mL can be performed.
The tubes can be purchased from the Chemistry Store.
IMPORTANT: Do NOT fill the tubes more than 50 % capacity as explosion of contents is likely to occur!!

The easy-to-use caps allow any excess pressure in the reaction vessel to be released prior to user
intervention, ensuring the safest possible mode of operation before, during, and after the reaction.
PREPARATION:
Must be performed in a fume cupboard and contents sealed in the microwave tube before moving to the
microwave reactor
1. A risk assessment (OHS17) of the reaction must be performed before carrying out any reaction and
included in the risk assessment folder located with the microwave.
2. Charge microwave tube with contents for reaction
3. Clip the cap onto the top of the tube
Ensure this is done correctly to make a firm seal!
If not a pressure error will occur during the run and the sample will not be run!
4. Insert the sample into the automation deck and note its position
These are identified by a Letter and Number
e.g. A1 – This number must also appear on your risk assessment to identify its location
Start-up:
1. Fill out your details (Name, date, experiment code, rack position, risk assessment number) in the CEM
Microwave Log Book located along side instrument. Ensure your tube is labelled. Insert a copy of your
experiment risk assessment into the CEM Microwave Risk Assessment Folder.
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OHS026 safe work procedure
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2.
3.
4.
5.
6.
7.
Turn power on to the microwave reactor (switch located on the left side toward the rear)
Turn power on to the explorer arm (switch located on the left side of arm)
Open supply air tap a single turn
Set air pressure by adjusting the inline pressure valve (pressure should be ?need to check this)
Start-up the computer
Run the Synergy Software.
Synergy Software:
1. Select your user name (setup by the system administrator – Toby Jackson)
2. Enter your password
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OHS026 safe work procedure
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Method Creation:
1. From the main screen a new method can be created by selecting the New icon or File > New
2. The method editor is then displayed in a new screen.
3. There are five different types of methods available to choose from
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Standard Method:
This is the simplest method. For this method all that is required is the temperature and the reaction time.
1. Enter a Method Name (e.g. Sample 1)
2. Set the temperature by entering the value in the field or sliding the bar
3. Set the reaction time by adjusting the hold time (hh:mm:ss)
4. Click OK.
The new method appears in the method folder for the current user.
The current user is shown in bold in the user tree on the left.
User Tree
Automation
Deck
5. Once the method is created and appears is in the user tree:
a. It can be moved into a spot on the automation deck by dragging and dropping the method name
into the appropriate location
b. OR by highlighting the desired method name and double clicking the appropriate location on the
automation deck.
The cell turns bright green indicating that it has been queued and displays a number indicating the order
that it will be processed (as shown in the sequence editor)
6. With active samples in the queue the play button at the top of the screen can be selected and the cell being
processed turns yellow.
NOTE: A calibration procedure of the instrument occurs automatically if it is the first reaction for the day
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7. When the experiment is in progress the reaction details are shown on the right of the screen.
Hot Keys
Stop
The blue hot keys allow for reaction parameters to be changed at any stage during the reaction.
The reaction can also be stop prematurely by pressing the red Stop button
8. When the reaction is complete, a data file appears in the data folder for the current user located in the user
tree.
9. The data can be view by using the data, graph and report options located at the top right
For example a report can be generated :
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Shut down instructions:
1. Remove appropriated microwave tube from Automation Deck and check for any leakage of contents
IF CONTENTS HAVE LEAKED please contact Toby Jackson immediately for best course of action for clean
up!
2. Close Synergy software and shut down computer.
3. Turn of Explorer arm
4. Turn of Microwave reactor
5. Close air supply (At Wall)
Sign off log book to indicate you are finished
6.List emergency shutdown procedures
Follow CEM Explorer shutdown procedures, select the STOP (red square icon) hot key on the main control bar (software
main screen) to prematurely halt a reaction.
7.List Emergency procedures for how to deal with fires, spills or exposure to hazardous substances
Contain the fire or spillage if safety of all personnel is not compromised, otherwise shutdown the power using the emergency cut-off
switch (red button) for the laboratory
and call the security for emergency (x56666).
8.List Clean up and waste disposal requirements
All chemical waste should be disposed of in the appropriate waste container.
9.List legislation used in the development of this SWP NSW OHS Act 2000, NSW OHS Regulation 2001, Code of Practice
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OHS026 safe work procedure
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for the Labelling of Workplace Substances
AS/ NSW OHS Act 2000,
NSW OHS Regulation 2001,
Code of Practice for the Labelling of Workplace Substances
AS/NZS 2243.2:2006. Safety in laboratories. Part 2: Chemical aspects
AS/NZS 2243.6-1990. Safety in laboratories. Part 6: Mechanical Aspects.
AS/NZS 2243.3:2006 Safety in Laboratories Part 7 Electrical aspects
AS/NZS 2161.1:2000 Occupational Protective Gloves – Selection, Use and Maintenance
10a.List competency required – qualifications, certificates, licensing, training - e.g. course or instruction:
This instrument is not to be operated without prior training and approval by the laboratory technical staff or nominated experienced
users.
10b. List competency of Assessor
11.Supervisory approval, And review
Supervisor:
Signature:
Responsibility for SWP review:
T. Jackson
Date of review:
12.SWP Sign off sheet
F10-SWP-139, CEM Microwave Reactor, Version 1:
In signing this section the assessor/ authorisor agrees that the following persons are competent in following this
SWP
Name
Signature
Date
Competent
Name of Assessor/Authoriser
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Assessor/Authoriser
signature
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