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Standard Operating Procedure for UVVis, FTIR and Fluorolog spectrometers

These guidelines have been prepared by Dr Michael Staniforth


These guidelines have been prepared by Dr Michael Staniforth
Before commencing work with the fluorolog 3, Bruker 70V FTIR, or Lambda 850 UVVis spectrometers, you must read this document, and have completed training with a member of WCUS staff to confirm that you have understood the content and that you agree to abide by the protocols contained herein.


Purpose and Structure of this document
The principal aim of this document is to outline the elements of good practice as they apply specifically to experiments currently being undertaken in the above laboratories. General aspects of laser safety are covered in sections of the manuals accompanying the lasers.
The document is structured as follows: at the top level (this sheet) an overall description is made of research activity in this laboratory. General precautions are then given followed by detailed schemes of work. Emergency procedures are outlined at the end.


Description of Activity:
MAS 2.11 contains a Brucker 70V IR spectrometer, emitting monochromated light between 360 nm and 670 microns, and a Fluorolog 3 fluorescence spectrometer, emitting monochromated light between 250 nm and 2 microns. P2.54 contains a Lambda 850 UVVis spectrometer emitting light between 175 nm and 800 nm.
Four types of situation have been identified which require separate safety protocols, where appropriate:
- Sample preparation
- Taking measurements
- Sample disposal
- Maintenance

Please see Risk Assessment included in this pack for further details.
Authorised users of the above systems are:
Supervisors: James Lloyd-Hughes, Vas Stavros
Facility Manager: Michael Staniforth
Students and others: Please see further documentation or go.warwick.ac.uk/wcus

General Precautions
1. (Not applicable to UVVis) The laser curtain must not be passed to enter the laser area of WCUS at any time. If a user’s eye line must go below the level of the curtain at any point – protective eyewear must be worn and care be taken not to look towards the laser setups. Alternatively, assistance can be requested from a Registered Laser User.
2. General safety specs must be warn at all times. Gloves and lab coats should be worn when handling chemical samples. Any extra precautions for particularly hazardous samples must be taken where appropriate.
3. All standard University health and safety protocols should be observed at all times.
4. Low irradiance or enclosed laser systems may be in use with these experiments. Interlocks on these systems should not be broken and no alignment should be attempted by any user other than service engineers.

Cryogens (Not applicable to UVVis)
1. Insulated gloves and safety specs must be worn at all times when handling cryogens. As much skin as possible should be covered – i.e. long trousers and shirts and lab coats should be worn – to minimise exposure.
2. Ensure that the area is well ventilated and oxygen sensors are installed before transferring liquid nitrogen, and only transfer between containers designated as for liquid N2.
3. While liquid N2 is being transferred, only trained users should be present in the laboratory space, even if working on a separate experiment.

Vacuum Systems (Not applicable to UVVis)
1. When changing oil or aluminium beads, lab coats, safety specs and gloves must be warn. When servicing the pump, time should be given after operation for the pump to cool and other users should be away from the area where the pump is being but may remain inside the lab. Servicing should only be attempted by trained users.
2. Always ensure the vacuum is off or valve is closed before breaking a seal.
3. Only vacuum rated materials should be used with the vacuum system.
4. A burn risk exist as the vacuum pump gets hot during operation; appropriate care should be taken.

Pressurised Gas (N2/Ar/Air)
1. Goggles must be worn at all times when working with pressurised gas.
2. All seals must be checked with regulators set at low pressure before increasing the flow rate.
3. All gas cylinders are kept outside of the laboratories.
4. Ensure regulator is closed before breaking a seal.
5. Ensure that the area is well ventilated and oxygen sensors are installed before flowing N2.


Safety protocol: Sample Preparation – All Spectrometers
Definition
Sample preparation applies to the making of solutions or solid samples and preparing the appropriate vessels for the spectrometer.
Protocol/Scheme of Work
Planning:
• As much sample preparation should be done in another lab equipped with a fume hood as is possible. All sample preparation at the spectrometers should be kept to a minimum, preferably zero, as these spaces are not equipped for such activity
• All appropriate MSDSs and risk assessments must be carried out prior to the experiment beginning, and uploaded to the appropriate section of go.warwick.ac.uk/wcus
• Cleaning of sample vessels for the spectrometer should, where possible, take place in other labs in a fume hood, prior to use of the spectrometer.
• Provision of suitable PPE should be addressed at this stage.
Preparing a sample:
• In cases where sample preparation must occur at the spectrometer – for instance, where multiple samples must be measured with the same sample vessel and moving between distant labs is unfeasible – care must be taken to keep this to the absolute minimum.
• Sample preparation must be limited to cleaning sample vessels, transferring new samples to the vessel and diluting very small amounts of sample in solvents, exclusively. If any further sample preparation is necessary, the facility manager must be contacted to make arrangements, or it must be done off site.
• PPE must be worn at all times during sample preparation.
• A chemical resistant container must be used to carry samples and solvents into the lab and sample preparation must take place inside this container.
• Each experimental run on all spectrometers requires a maximum of 3ml of solution or 1 cm2 solid sample. No more than is necessary for the experimental runs should be brought into the labs. No more than 50 ml total of samples and solvents should be brought into the labs. If more is necessary, then the experiment must be split into two or more runs.
• Samples must be ensured to be sealed before moving from the preparation area into the spectrometer.

Safety protocol: Taking measurements – UVVis
Definition
Taking measurements applies to transferring samples to moving samples into the spectrometer and obtaining UVVis absorption spectra under air and N2.
Protocol/Scheme of Work
Planning:
• Before taking measurements, the instructions on running the UVVis spectrometer (placed by the spectrometer) should be read and understood.
• All protocols outlined in the preceding scheme of work must be followed.
Taking a measurement:
• When moving sample between the preparation area and the spectrometer, care must be taken to ensure the sample is sealed and the vessel exterior is clean.
• Only the sample area on the spectrometer need be accessed by the user at any time. If there are any problems with the equipment either the facility manger, Mick Staniforth, or the facility owners, Vas Stavros or James Lloyd-Hughes, should be contacted. On no account should users try to access any other part of the spectrometer.
• Only trained users, who have been approved by the facility manager should be taking measurements of the spectrometer unsupervised.
• The instructions for use of the spectrometer should be followed at all times.
• While all light produced at the sample area is eye safe, jewellery should not be worn and care should be taken against stray reflections from the sample area.
• When running under dry nitrogen environment – safety goggles should be worn at all times – seals should be checked with a low pressure on the regulator before flowing at higher pressures – the area should be well ventilated – this should only be performed by trained personnel and with permission of the facility manager.

Safety protocol: Taking measurements – Fluorolog
Definition
Taking measurements applies to transferring samples to moving samples into the spectrometer and obtaining fluorescence spectra in the UV/VIS and IR regions with room temperature and cooled detectors.
Protocol/Scheme of Work
Planning:
• Before taking measurements, the instructions on running the fluorescence spectrometer (placed by the spectrometer) should be read and understood.
• All protocols outlined in the preceding scheme of work must be followed.
Taking a measurement:
• When moving sample between the preparation area and the spectrometer, care must be taken to ensure the sample is sealed and the vessel exterior is clean.
• Only the sample area on the spectrometer or the excitation monochromator need be accessed by the user at any time. If there are any problems with the equipment either the facility manger, Mick Staniforth, or the facility owners, Vas Stavros or James Lloyd-Hughes, should be contacted. On no account should users try to access any other part of the spectrometer.
• To change the monochromator, instructions given by the spectrometer must be read and followed at all times – the monocromator should only be replaced by trained personnel approved by the facility manager
• Only trained users, who have been approved by the facility manager should be taking measurements of the spectrometer unsupervised.
• The instructions for use of the spectrometer should be followed at all times.
• While all light produced at the sample area is eye safe, jewellery should not be worn and care should be taken against stray reflections from the sample area.
• When running under dry nitrogen environment – safety goggles should be worn at all times – seals should be checked with a low pressure on the regulator before flowing at higher pressures – the area should be well ventilated – this should only be performed by trained personnel and with permission of the facility manager.
• When using an IR detector which must be liquid nitrogen cooled, the cryogen general precautions must be followed – insulated gloves and safety goggles should be worn at all times – the area should be well ventilated - this should only be performed by trained personnel and with permission of the facility manager – other users should be made aware of the procedure and should be absent from the area if possible.

Safety protocol: Taking measurements – FTIR
Definition
Taking measurements applies to transferring samples to moving samples into the spectrometer and obtaining FTIR absorption spectra under air, vacuum and with room temperature and cooled detectors.
Protocol/Scheme of Work
Planning:
• Before taking measurements, the instructions on running the FTIR spectrometer (placed by the spectrometer) should be read and understood.
• All protocols outlined in the preceding scheme of work must be followed.
Taking a measurement:
• When moving sample between the preparation area and the spectrometer, care must be taken to ensure the sample is sealed and the vessel exterior is clean.
• Only the sample area on the spectrometer need be accessed by the user generally. Detectors and beamsplitters may need to be changed or cooled. If there are any problems with the equipment either the facility manger, Mick Staniforth, or the facility owners, Vas Stavros or James Lloyd-Hughes, should be contacted. On no account should users try to access any other part of the spectrometer.
• Only trained users, who have been approved by the facility manager should be taking measurements of the spectrometer unsupervised.
• The instructions for use of the spectrometer should be followed at all times.
• While all light produced at the sample area is eye safe, jewellery should not be worn and care should be taken against stray reflections from the sample area.
• When running under vacuum, safety goggles should be worn at all times. The user will have no need to access the vacuum itself. If there are any problems, the facility manager or owners should be notified.
• No attempt should be made to open the spectrometer while under vacuum.
• When using an IR detector which must be liquid nitrogen cooled, the cryogen general precautions must be followed – insulated gloves and safety goggles should be worn at all times – the area should be well ventilated - this should only be performed by trained personnel and with permission of the facility manager – other users should be made aware of the procedure and should be absent from the area if possible.

Safety protocol: Sample Disposal – All spectrometers
Definition
Sample disposal applies to disposing of waste solvents, solutions and solid samples and cleaning of the sample vessels after use
Protocol/Scheme of Work
Planning:
• All protocols outlined in the preceding schemes of work must be followed.
Disposing of samples/waste and cleaning:
• Safety specs and gloves should be worn at all times.
• Any waste solvents or sample produced in sample preparation should be stored in a sealable glass container and transferred to the waste solvent bottle in the solvent cabinet in MAS2.11 once the experiment is complete. This container must be large enough to feasibly contain any waste that will be produced during the experiment. However, as outlined above, sample sizes should be kept to a minimum.
• Waste should be disposed of in appropriate waste containers (e.g. solid/flammable/halogenated etc..).
• Waste containers should not be bought into P5.24 except those outlined above and should never be left there.
• Once an experiment in completed, all samples, solvents, and waste, and any other equipment associated with that individual experiment, should be removed from the laboratory in an appropriate carrier, and all waste disposed of as outlined here. The spectrometer must be ensured to be clean and uncontaminated.

Safety protocol: Maintenance – All spectrometers
Definition
Sample disposal applies to routine or extraordinary maintenance of the spectrometers by trained maintenance engineers.
Protocol/Scheme of Work
Planning:
• All potential users of the space/lab where the engineer will be working should be notified in advance
• Health and safety officers should be notified of the visit and all documentation for the engineer checked prior to work commencing.
• If possible, the engineer should be the only person working in the space/lab while maintenance is ongoing.
Maintenance:
• Should user need to be in the lab at the same time as the engineer, all users must be kept informed of the ongoing activities of the engineer.
• The spectrometer should be isolated from the surrounding lab as much as possible, particularly where light sources are exposed.
• All interlocks and other safety mechanisms must be in place before the spectrometer is handed back to the facility manager.
• Full briefing and documentation on the updated specifications of the spectrometer should be made available to all users after work has been completed.