1. Completed by: A/Prof. Naresh Kumar
Staff/Student number:
The Writing Safe Work Procedures Guideline (OHS027) should be consulted to assist in the completion of this form
Faculty/Division:
Faculty of Science
Document number
F10-SWP-373a
Initial Issue date
28.10.2011
Current version
V1
School/Unit:
School of Chemistry
Current Version
Issue date
28 October 2011
2.Safe work procedure title and basic description of activity
Title: Atmospheric Pressure Hydrogenation reaction (in the Hydrogenation room 232 only!)
Next review date
28 October 2013
Description of activity:-
Reduction of an organic compound with hydrogen gas and a catalyst
3.List Hazards and risk controls as per risk assessment
Associated risk assessment number and location:
F10-RA-373a
(School and
Faculty database)
Hazards:
Hydrogen gas: and Fire asphyxiation
Palladium on
Carbon, Platinum oxide, and Raney
Nickel: Fire
Fire explosion and
Spillage contamination and from chemicals
Physical injury due to glassware
Controls:
Highly flammable gas, consult MSDS. Hydrogen is much lighter than air and therefore will collect in roof spaces. Air/hydrogen mixture ignites very rapidly.
Proper training: Ensure all work with hydrogen gas is carried out in the fume hood in the hydrogenation room and that there are no ignition sources in the vicinity. Personnel must be inducted into the lab and be aware of the nearest appropriate fire extinguisher/blanket. Do not change cylinders unless trained to do so. Ensure to close hydrogen source off immediately after use and all adapters are tightly fitted to flasks. Room should be well-ventilated and contain a functioning gas detection system.
In general hydrogenation catalysts are pyrophoric (ignite spontaneously in air). Proper training: consult the relevant MSDS and understand the hazards involved. Ensure all work with the catalyst is carried out in the fume cupboard located in the hydrogenation room and always wear the appropriate PPE.
Avoid prolonged exposure of pyrophoric solids to air.
When handling any flammable solvents/liquids, ensure the work is carried out in a fume hood and bottles are returned to flammable cabinets when not in use. Avoid the use of ethereal solvents because of their high flammability
(Class 3, Packing Group 1) if at all possible.
Consult MSDS for all chemicals used and fill in the corresponding School of Chemistry Risk assessment form . Appropriate training. First aid on site.
Wear proper PPE, especially chemically compatible gloves and protective eyewear. Dilute corrosive substances if possible. Avoid ignition sources.
When possible, carry out all work in a fume hood.
Clean up spillages immediately.
Proper training: inspect all glassware for cracks before use and replace if faulty.
4.List resources required including personal protective clothing, chemicals and equipment needed
Materials and Equipment

Hot-plate stirrer and stirrer bar

Quick-fit round bottom flask
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Quick-fit adaptor and stoppers to seal round bottom flask

Bunding container capable of containing entire contents of round bottom flask

Tubing for hydrogen flow

Grease

Hydrogen gas

Inert gas (argon or nitrogen)

Vacuum

Catalyst (as above)

Solvent (typically ethanol, methanol, ethyl acetate or acetic acid)

Compound to be reacted

Small quantities of organic or inorganic acid or base may be added to neutral solvents to affect the course of some hydrogenation reactions.
Personal Protective Clothing and Equipment

Laboratory coat

Protective safety glasses

Enclosed shoes
Gloves (select according to chemical compatibility
5.List step by step instructions or order for undertaking the task
All of the following activities should be conducted in a fume hood!
This procedure is written for performing this procedure in the hydrogenation room (232) on Level 2, the Chemical
Science Building. It is not valid for other locations.
Sample Preparation

Weigh compound to be hydrogenated into a quick-fit round bottom flask.

Stopper the flask and dissolve or disperse the sample in desired amount of solvent by swirling the flask in a fume cupboard.

Purge the reaction vessel three times with an inert gas and stopper the flask. The reaction flask must be purged with argon or nitrogen gas before the addition of the catalyst to remove any possibility of producing a spark .

Weigh the desired amount of the catalyst, carefully to avoid any inhalation of the catalyst dust. Transfer the catalyst to the reaction flask in a fume cupboard and stopper the flask after the addition of the catalyst. The catalyst must be added to the flask in a fume cupboard immediately before proceeding to the hydrogenation room.

While the flask is in the fume cupboard take care to wash down all traces of the catalyst which might be adhering to the sides of the flask by swirling the suspension gently so that all the catalyst is covered by the solution. This is done to remove any risk of the catalyst sparking and igniting the solvent.

Remove the stopper and attach a well greased quickfit adaptor with a stopcock to the reaction flask and carry it in a container or basket (to rule out any possibility of spillage) safely to the hydrogenation room.
Hydrogenation

Connect the tubing from the control box to the reaction flask via a quickfit adaptor with a stopcock.

While the reaction mixture is being stirred evacuate the reaction flask by turning the three way control knob to vacuum

Wait for a few minutes (you may see some bubbling in the reaction mixture)

Close the vacuum by turning the three way tap

Add hydrogen gas slowly by turning the three way control knob to hydrogen.

Repeat this process three times to ensure that the reaction is carried out under an hydrogen atmosphere.
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Depending on the reaction it may take from 2 to 24 hours for the reaction to complete.
 For overnight reactions also place the “After Hours Reaction” sign next to the reaction apparatus.
Reaction Workup

When hydrogenation is complete stop the stirrer, close the three way control knob. (Caution: if air enters the flask there is risk of a fire).

Purge the flask two times with nitrogen using the three way control knob

Detach the hydrogenation flask from the hydrogenation apparatus and admit air slowly by opening the stopcock carefully

As soon as the flask is removed from the stirrer ensure that all traces of catalyst adhering to the sides of the flask are washed down below the surface of the solution. Do this by swirling the flask manually and then use a glass pipette or plastic wash bottle (where suitable) containing the solvent you have been using. (Caution: if residual catalyst is adhering to the wall of the flask it may ignite setting fire to the solvent).

Make sure that the reaction flask stopcock is secure and take the reaction flask back to the laboratory in a container or basket to prevent spillage.
Clean-up Procedure and Waste Disposal

In the fume cupboard filter off the spent catalyst on a Hirsch funnel using a small pad of Celite (filter aid)

Wash with a little of the solvent. Avoid using a filter paper and make sur e it doesn’t go dry,

Keep the catalyst wet because the dried catalyst can catch fire.

The damp used catalyst should be transferred immediately to a residue solid-waste container.
Be prepared for a possible fire. Fires are much more likely to occur using ethereal solvents. Finely divided catalyst adhering to the wall of the flask may be invisible to the naked eye but can cause a fire.
6.List emergency shutdown procedures
Close the three way control knob and turn off hot-plate stirrer
7.List Emergency procedures for how to deal with fires, spills or exposure to hazardous substances
Call security in the event of a serious emergency (x56666)
Fire: Cover the fire with a fire blanket if it can be fully contained underneath the blanket otherwise use a fire extinguisher.
Carbon dioxide or dry powder is suitable. Be prepared for re ignition: do not leave the scene unless the safety of personnel is compromised.
Spill: S pills should be cleaned up in accordance with the relevant SWP (e.g. SWP411 Spill cleanup for Flammable liquids) and if the safety of personnel is not compromised.
Exposure: remove contaminated protective clothing and examine your clothes for contamination which may have soaked through. If day clothing is contaminated, remove, and wash skin under running water immediately for 15 minutes or until medical attention arrives.
8.List Clean up and waste disposal requirements

Catalysts must be kept wet at all times and must be disposed into the appropriately labeled solid-waste container

All other chemicals and solvents should be disposed into the appropriate water containers (non-halogenated waste or halogenated waste) after consultation with the relevant MSDS
9.List legislation used in the development of this SWP
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 2161.1:2000 Occupational Protective Gloves – Selection, Use and Maintenance
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10a.List competency required – qualifications, certificates, licensing, training - e.g. course or instruction:
All personnel operating this equipment must have completed the general Laboratory Safety Awareness Course and, in addition, specific training and instructions on the safe use of the equipment and they must be assessed as competent.
10b. List competency of Assessor
11.Supervisory approval, And review
Note: Local supervisor must determine appropriate authorisation and final sign off when this document is
downloaded.
Supervisor: Signature:
Responsibility for SWP review: Date of review:
12.SWP Sign off sheet
SWP name and version:
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 Assessor/Authoriser signature
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