Contents

• Sample Stages
• Sample Types
• Sample Environments
• Preparation Facilities
• Transport & Safety
• Waste Disposal

Sample Stages

Click on a heading below for more information.

GAS PHASE EXPERIMENTS

60 cm Multipass Glass Cells

The IR beamline has two 60 cm multipass cells; one for exotic or reactive species (figure 1) and one for standard or non-reactive samples (figure 2). Light is passed through the sample multiple times in the cell, increasing the path length of the source and thus increasing the sensitivity of the system (Beer’s Law). Figure 3 shows the mirror in the base of the glass cell for non-reactive species. The number of spots (figure 4) indicates the number of times the beam is bounced through the cell.

The glass cell for exotic or reactive species can be coupled to a furnace (figures 5&6) capable of reaching temperatures <1100 °C. Please indicate to IR beamline staff if you wish to use the furnace.
 

Figure 1. 60 cm Multipass Glass Cell for reactive species. The cell has three inlet/outlet ports. The cell can be attached to a ventilation exhaust system. The cell is shown wrapped in heating-tape; the cell can be heated to temperatures of 80 °C.	Figure 2. 60 cm Multipass Glass Cell for non-reactive species.

Figure 3. The beam can be bounced through these cells multiple times; max. path length approx.  20 m.	Figure 4. The bottom mirror of the 60 cm cell for non-reactive species. The number of spots indicates the number of times the beam is bounced through the cell. Spots were visualised using a near-IR viewer.

Figure 5. The IR Furnace;  can reach temperatures of < 1100 °C. Please indicate to IR beamline staff if you wish to use this equipment.	Figure 6. Showing the furnace coupled to the multipass cell for reactive species. The sample gas is passed through the furnace and into the multipass cell for analysis.

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Enclosive Flow Cooling (EFC) Cell

This cell can reach liquid nitrogen or liquid helium temperatures and is used for the study of gases, particulates and/or cluster species. The cell can operate in two modes: flow-through or static mode. The cell is currently being commissioned but can be used in the static mode. Please ask IR beamline scientists with regards to flow-through experiments.

Figure 7. The Enclosive Flow Cooling (EFC) Cell; designed & built by S. Baurecker. Permanently on loan to the Australian Synchrotron from the Molecular Spectroscopy & Centre for Biospectroscopy group at Monash University, Clayton.

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CONDENSED PHASE EXPERIMENTS

Typical condensed phase experiments at the Australian Synchrotron Far IR & HR beamline utilise the wide spectral range and high intensity of the synchrotron source. Condensed phase samples can be supported/mounted for analysis in a number of different ways.

Single Disc Holder for Transmission

For the study of samples that can be pressed into disks or pellets 13 mm in diameter (see Sample Types). Note that a pellet press is available in the Chemistry Laboratory. Please inform IR Beamline staff if you require access to this instrument to press your samples.

Triple Sample Holder for Transmission (Vertical)

For discs 10 mm in diameter. Ideal for polarisation studies or ellipsometry (see figure 9).

Figure 8. Triple Sample Holder for Transmission Studies. Top view.	Figure 9. The sample clamp; for samples 10 mm in diameter. Can hold up to 3 samples at a time.

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 Cryogen-cooled Cryostat, Triple Sample Holder for Transmission (Vertical)

For discs 10 mm in diameter. Ideal for the study of phonon modes in cryogenically-cooled crystals.

• Liquid Nitrogen cooled Cryostat
• Sample rotation axis perpendicular to the IR beam axis 

Figure 10.The Cryostat (Janis Research); shown mounted to the sample compartment of the Brüker IFS 125HR FTIR spectrometer.	Figure 11. The sample clamp; for samples 10 mm in diameter. Can hold up to 3 samples at a time.	Figure 12. Robert Falconer, University of Queensland, shown cooling the Cryostat with liquid nitrogen.

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 Grazing Incidence Angle (GIA)

For the study of thin films or monolayers. Ideally samples should be uniformly deposited on a gold- or aluminium-coated microscope slides, 3“x1” in size, however sample masks are available for irregular sized samples (see figure 14). Contact IR Beamline staff for more information. The grazing angle of incidence can be varied between 30° and 80° in 1° increments. 

Figure 13. The Grazing Angle Incidence (GIA) cell (PIKE Technologies). The whole cell is placed into the sample compartment of the  spectrometer and your sample slide is placed face down on top of the accessory.	Figure 14. A series of masks to hold GIA samples. Mask dimensions: a, 1.25x3"; b, 1x3", c, 0.615" aperture; d, 0.372" aperture. Gold-coated reference (e, 1.25x3") and sample (f, 1x3") slides are shown (Thermo Scientific).

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Sample Types

Gas Phase Sample Types

Transport and use of gas phase samples at the Australian Synchrotron is at the discretion of OHSE approval (see your Experiment Authorisation form: submit appropriate Risk Assessments and MSDSs). Small gas cylinders may be brought onsite by the user but they must be OHSE approved by your place of work for use and transport (appropriate date stamps must be present). You must supply your own gas regulator. Fittings must be 6 mm or ¼” Swagelock. Please provide IR Beamline staff with details of the sample including cylinder volume.

Standard Fittings for the 60cm Multipass Cells:

• ¼” and 6 mm Swagelock fittings
• Compression and UltraTorr fittings for ¼” and 6 mm O.D. tubes
• KF16, 25 & 40 flanges
• Please ensure your sample vials/cylinders conform to these standard attachments
   

Condensed Phase Sample Types

Optical Sample Support Material

• Potassium bromide (KBr) < 400 cm^-1
• Polyethylene (PE) < 400 cm^-1
• TDX < 200 cm^-1
• Quartz < 200 cm^-1

Crystals/Particulates

• Press sample into pellets
• Disk diameter: 10 - 13 mm
• Materials including KBr powder and polyethylene powder (not supplied by the AS); make sure you bring blank discs or discs made of your supporting material only (no sample) to use as references/backgrounds
• A pellet press is available for use at the AS; please indicate if you require use of this instrument

Grazing Incidence Angle Cell

• For thin films
• Typically samples are coated on gold- or aluminium-coated microscope slides, 3“x1” size, however smaller sized samples can be accomodated (see figure 14)

Self-supported Samples

• The sample must be suitable to mount to an appropriate accessory

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Sample Environments

Condensed phase experiments are typically conducted under vacuum conditions. When using the Cryostat, sample temperatures can be reduced to liquid nitrogen or intermediate temperatures.

Gas phase experiments are typically conducted at room temperature in one of the two glass cells. The 60cm Multipass Glass Cell for reactive species can be operated at warmer temperatures (up to 80°C). A furnace is available to heat reactive species; the furnace can reach temperatures of < 1100 °C. If cryogenic temperatures are required, the Enclosive Flow Cooling (EFC) cell can be used with liquid nitrogen or liquid helium.

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Preparation Facilities

Limited space is available in and outside of the IR Hutch for sample preparation. The Synchrotron has both a chemistry and a biochemistry laboratory onsite. These laboratories are equipped with fume cupboards, fridges, freezers, stereo microscope with camera, UV-Vis spectrometer and balances. Please consult IR Beamline staff if you require specific equipment for sample preparation (you may have to supply your own equipment).

A Class II biological containment laboratory is available for use during your beamtime if required. This contains a Class II safety cabinet, CO₂ incubator, inverted microscope, centrifuges, fridge, freezer and water bath. Users requiring access to this facility should contact the IR beamline staff when submitting a proposal which involves the handling of live biological material (see IR Microspectroscopy).

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Transport and Safety

Please see Sample Transport & Safety for more specific information.

Please consult your OHSE if unsure how to best transport your samples. If you have air or moisture sensitive materials, it is recommended you transport samples in a sealed box supplied with desiccant. An electric desiccator (10% humidity) is available in the IR Hutch to store your samples if necessary.

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Waste Disposal

Please see Waste Disposal for more specific information.

You must remove all waste from the beamline for disposal at your own facility. Some waste disposal facilities are available in the Chemistry and Biochemistry Laboratories. Please consult IR Beamline staff for more information.

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