Sample Stages

CONDENSED PHASE EXPERIMENTS

Typical condensed phase experiments at the Australian Synchrotron FIR & 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. Note that a pellet press is available at the Australian Synchrotron in the chemistry laboratory. Please inform IR Beamline staff if you require access to this instrument to press your samples.

Sample holder for pressed discs.

The pellet press available at the AS in the chemistry laboratory. Please inform IR Beamline staff if you require access to the pellet press.

Triple Sample Holder for Transmission (Vertical)
For discs 10 mm in diameter. Ideal for polarisation studies or ellipsometry.

Triple Sample Holder for Transmission. Can rotate samples perpendicular to the IR beam axis and/or to the plane perpendicular to the IR beam while the sample is under vacuum. The sample holder itself is also shown.

Triple Sample Holder for Transmission (Vertical), Cryostat
For discs 10 mm in diameter. Ideal for the study of phonon modes in cryogenically-cooled crystals.

• LN2 Cryostat
• Sample rotation axis perpendicular to the IR beam axis.

Robert Falconer, University of Queensland, cooling the Cryostat with LN2. The Cryostat is shown mounted to the sample compartment of the Brüker IFS 125/HR FTIR spectrometer.

The Cryostat sample holder can hold up to three sample discs at a time.

Grazing Incidence Angle (GIA)
For the study of thin films or monolayers. Samples should be uniformly deposited on a gold-coated microscope slide, 3“x1” in size. Contact IR Beamline staff for more information. The grazing angle of incidence can be varied between 30° and 80° in 1° increments, allowing you to optimise the angle of analysis.

The Grazing Angle Incidence (GIA) cell. A gold-coated plate coated in your sample is placed face down in the sample holder. The whole cell is then placed into the sample compartment of the Brüker spectrometer and placed under vacuum.

Sample holders for the Grazing Angle Incidence (GIA) cell. Gold-coated reference and sample slides are shown, as are reference and sample holders.

GAS PHASE EXPERIMENTS

60 cm Multipass Glass Cell

The IR beamline has two 60 cm multipass cells; one for standard or non-reactive samples and one for exotic or reactive species. The latter can be coupled to a furnace capable of reaching temperatures ? 1100 °C. Please indicate to IR beamline staff if you wish to use the furnace.

Light passes through the sample in the glass cell multiple times, increasing the path length of the source. The photo shows the mirror in the base of the glass cell. The number of spots indicates the number of times the beam is bounced through the cell.

A. 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 can also be wrapped in heating-tape (see inset) and heated to temperatures of 80 °C.
B. 60 cm Multipass Glass Cell for non-reactive species.

The Furnace. The sample passes through the furnace and into the multipass cell. This furnace can reach temperatures of ? 1100 °C. Please indicate to IR beamline staff if you wish to use this equipment.

Standard Fittings for the 60cm Mutlipass Cells:

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

Enclosive Flow Cooling (EFC) Cell
This cell can reach LN2 or LHe 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.

The Enclosive Flow Cooling (EFC) Cell & schematic.

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. You must supply your own gas regulator. Fittings must be ¼” Swagelock. Please provide IR Beamline staff with details of cylinder volume.

Condensed Phase Sample Types

Optical Sample Support Material

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

Crystals/Particulates

• Press pellets
• Disk diameter: 13mm
• Materials including KBr powder and polyethylene powder (not supplied by the AS)
• A pellet press is available for use at the AS. Please indicate if you require use of this instrument.

The Pellet Press. Available at the AS in the Chemistry Laboratory. Please inform IR Beamline staff if you require access to the Pellet Press.

Grazing Incidence Angle

• For thin films
• Gold coated microscope slide, 3“x1” size

Sample holders for the Grazing Angle Incidence (GIA) cell. Gold-coated reference and sample slides are shown, as are reference and sample holders.

Self-supported Sample

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

Environments

Condensed phase experiments are typically conducted under vacuum conditions. When using the Cryostat, sample temperatures can be reduced to LN2 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 LN2 or LHe.

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 pages).

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.

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.