IMAGING AND MEDICAL

IN 2014/1 IMBL AIMS TO OFFER THE FOLLOWING 3 OPERATING MODES:

  • 2-Dimensional imaging of live animals, and 3-Dimensional imaging of materials in hutch 3B
  • Fast computed tomography (CT) of small objects in hutch 2B
  • Micro-beam radiation therapy (MRT) in hutch 1B

PREPARING FOR BEAMTIME APPLICATIONS

For information on how to prepare your application and more detail on the available options refer to the Beamtime on this beamline (IMBL) information page.

ANIMAL ETHICS

For experiments using live animals first read the guidance provided.
Animal ethics procedures must be addressed well in advance of submission of the beamtime proposal.

INFRARED

IR MICROSCOPE

  • The ATR objective is currently available for use. Please indicate in your proposal if this is required.
  • The Grazing Angle Objective is currently available. Contact beamline staff for more details if this is required.
  • The Focal Plane Array FTIR microscope is currently available for booking with beamtime proposals. Contact beamline staff if this is required.
  • A Linkham heated sample stage is available for use. Contact beamline staff for more details if this is required.
  • Class II containment facilities are now available within the Biochemistry support laboratory. Users requiring access to this facility should contact IR beamline staff prior to submitting a proposal.

Beamline Contact: irm@synchrotron.org.au

FAR-IR & HIGH RESOLUTION

THE FOLLOWING INSTRUMENTS ARE UNDER COMMISSIONING BUT ARE AVAILABLE TO EXPERT USERS:

Gas-phase

An Enclosive Flow Cooling (EFC) cell with multipass optics that will enable the study of gases at cryogenic temperatures & clusters. The EFC cell is equipped with KBr, PEand TPX windows, and thus, can cover a wide spectral range from 10 cm-1 to energies greater than 4000 cm-1; it can achieve path lengths less than 20 m. Presently operating at temperatures ranging from100-300 K, the EFC cell is also designed to run at liquid helium temperature. The cell has been adapted to operate in the far-IR spectral region.

Condensed-phase

A vacuum-proof cell for qualitative and quantitative analysis of liquid samples; the cell is equipped with polyethylene, AgCl or AgBr window materials, and spacers ranging from 6-250 microns.

THE FOLLOWING INSTRUMENTS ARE AVAILABLE TO ALL USERS:

Gas-phase

  • A multipass gas-cell 300-380 K that can offer path lengths up to 20 m
  • A furnace to generate short-lived species by pyrolysis; it can only be coupled to the 300-380 K gas cell
  • A room temperature multipass glass gas-cell that can offer path lengths up to 40 m

Condensed-phase

  • A cryostat to study solid homogeneous samples down to liquid nitrogen or (helium) temperature.
  • A Grazing Incidence Angle accessory that is ideal for the study of thin samples at grazing angles.

Please contact the Far-IR and High Resolution beamline staff if you wish to use any of these instruments.

Beamline Contact: farir@synchrotron.org.au

MACROMOLECULAR CRYSTALLOGRAPHY

MX1: MACROMOLECULAR CRYSTALLOGRAPHY BEAMLINE

  • Energy range from 5.5 - 18 keV
  • User changeable energy from 8.5 to 17.5 keV
  • Fluorescence scans for MAD and metal identification
  • Robotic loading and remote access is available
  • Rapid access is available

MX2: MICRO CRYSTALLOGRAPHY BEAMLINE

  • Energy range from 5.5 - 18.0 keV
  • User changeable energy from 8.5 to 15.5 keV
  • Microfocus beam with FWHM of 30x15 microns (HxV) - VFM mirror upgraded (July 2012)
  • High flux with up to 3e12 ph/s/mm2 in the focussed beam
  • High resolution high framerate sample video for alignment of microcrystals
  • Fluorescence scans for MAD and metal identification
  • User-changeable micro-collimator now available with 20, 10, and 7.5 micron apertures
  • Robotic loading and remote access
  • Rapid access is available

More info on technical updates page.

Beamline Contact: mx@synchrotron.org.au

POWDER DIFFRACTION

PROPOSAL PREPARATION

  • Users can find tips on proposal preparation under Beamtime on this beamline on the powder diffraction beamlines' webpage.
  • Proposers interested in performing total scattering experiments should consult the Total Scattering Analysis page and prepare their proposal accordingly.
  • All proposals must be accompanied by evidence of previous diffraction measurements; i.e. a laboratory or synchrotron powder diffraction pattern that is indicative of the data obtained from the sample(s) of interest.
  • Experiments at high pressure are complex and users new to the technique should contact beamline staff before submitting their proposals

DETECTORS

The detectors which are currently available are:

  • Mythen microstrip
  • Photonic Sciences VHR CCD
  • MAR165 CCD

ANCILLARIES

  • Details of the ancillaries available at the beamline can be found under Sample stages and Environments.
  • Users should, as much as possible, select all of the appropriate ancillaries for their proposed experiment using the list of options within the portal
  • Note that users seeking to use their own sample stage and/or ancillaries should discuss this in advance with the powder diffraction beamline staff AND provide drawings of the equipment to show how it is anticipated that this equipment will fit at the end station
  • Available for experiments are:
    • Cryostream (80 - 450 K)
    • Hot-air blower (100 - 900 °C)
    • Anton Paar strip furnace (25 - 2300 °C)
    • STOE capillary furnace (25 - 1100 °C)
    • Gas/vacuum flow cell for capillary samples
    • High-throughput stage
    • Cryostat for samples in transmission geometry (10 - 300 K)
    • Diamond Anvil Cell (DAC) at ambient temperature only

BEAMLINE CONSUMABLES

The typical consumables required for most experiments on the Powder Difrraction beamline are listed below. A significant reduction in the beamline consumables budget has necessitated a number of new policies to come into effect that will affect those experiments requiring the use of the Anton Paar furnace and the DAC specifically.

Capillary experiments

  • Quartz and borosilicate capillaries can be purchased from hilgenberg remember to allow plenty of time to order your capillaries as the beamline does not provide them.
  • For experiments requiring pressures: 5 - 10 bar, quartz capillaries with a wall thickness of 0.02 mm are required.
  • For experiments requiring pressures: 10 – 20 bar, quartz capillaries with a wall thickness of 0.05 mm are required.
  • Sapphire capillaries are required for experiments using the capillary furnace for temperatures >1100°C and those experiments requiring pressures greater than 2 MPa (20 bar).
  • For experiments using the Norby or capillary flow cell, graphite Supelco M2-A ferrules are also required and can be obtained from here.

Anton Paar furnace experiments

  • Anton Paar furnace experiments requiring either platinum or tungsten heating strips must be supplied by Users.
  • The heating strips can be purchased from Anton Paar, see here for more details.
  • For experiments requiring temperatures 900°C or less, inconel heating strips may be used and are available for Users.

High pressure Diamond Anvil Cell (DAC) experiments

For experiments at pressures >10 GPa users will need to provide their own diamonds and seats. They can be purchased from: https://www.diamondanvils.com/ or http://www.almax-industries.com/ . Users must consult beamline staff for more information before purchasing.

HIGH PRESSURE AND TEMPERATURE CONDITIONS AVAILABLE AT THE POWDER DIFFRACTION BEAMLINE

Capillary Flow Cell Experiments

The maximum pressure at the beamline in a capillary is 2 MPa (thick-walled capillaries required as above) unless prior agreement is reached with beamline staff.
For experiments which use > 5% Hydrogen gas, the maximum temperature which can be used is 500°C.

Capillary Furnace Experiments

The maximum operating temperature is 1100°C for quartz capillaries
The maximum operating temperature is 1350°C for sapphire capillaries.

Beamline Contact: powder.diffraction@synchrotron.org.au

SOFT X-RAY SPECTROSCOPY

    • Kane O’Donnell has joined the beamline as a postdoctoral researcher. His forte is computation using a variety of codes to calculate the band structure of materials. Kane is interested in collaborating on suitable user projects but he is also available to advise users on theoretical calculation issues associated with Nexafs.
    • The beamline continues to operate well, and recent tests with the undulator mean we can now offer the potential of rotating the linear polarisation of the x-ray beam. For small samples this offers an easier method of making a polarisation analysis than by rotating the sample.
    • The beamline has new thermal evaporation sources. One source is optimised for organic evaporants in the temperature range from 50 to 300°C. The other is optimised for 200-800°C, but can operate to 1100°C with a suitable crucible. The beamline would prefer to offer these systems to users who wish to thermally evaporate material. A higher temperature evaporator, to 1400°C, may also be available. Further information on source specifications can be found in the beamline technical pages. We have a supply of crucibles available which we will exchange for each new evaporant. We are happy to support users who wish to use the full in situ surface science capabilities of the beamline. We are also happy to discuss how we can extend our capabilities, but we cannot guarantee that we will be able to do this in every case.
    • A new 4 point probe for measuring the surface conductivity of samples in UHV has been installed and tested in the preparation chamber. This is a specialist device that can be useful for a limited range of experiments. As an experimenter you will probably have knowledge of the information that can be obtained using such a device. If this would be useful as an adjunct to your experiment please contact us to discuss its use during your experiment. We are not offering this device as a general part of the user environment.
    • The beamline scientists of the soft x-ray beamline are very happy to hear directly from potential users and we would urge you if you would like to perform an experiment on this beamline to email or telephone us directly. For information, the beamline contact address below sends your email to all three beamline scientists.

Beamline Contact: softxray@synchrotron.org.au 

SMALL AND WIDE ANGLE X-RAY SCATTERING

Tips for SAXS users:

  • New 18/8/14: A replicate of the sample stage in the hutch has been set up outside in the beamline cabin, saving valuable beamtime by allowing Users to configure setups offline rather than in the hutch. Increased efficiency not only helps your own experiments but also maximises the number of experiments that can be scheduled.  This stage, known as Sampson (Sample Setup Station), replicates the full geometry around the sample position (including the WAXS goniometer when used) as in the hutch, and the same breadboard-based sample mounting design, XYZ motorised translation and on-axis sample camera function. Tools, fasteners, consumables and sample mounting hardware are also available in the cabin. Sampson allows you to assemble complete experimental setups outside in the cabin, and simply carry them into the hutch basically ready to go. This is particularly useful for complex setups, or if you have multiple setups to swap over during your beamtime. Setups can be done in advance (use the afternoon before your beamtime to get ready) or during the course of experiment (have one person doing the next sample setup whilst a colleague is running the beamline).
  • New 18/8/14: A significant change in beamline operations is now in action: Users will be required to take a much greater role and responsibility for setting up experimental equipment than has typically been the case in previous rounds. Unlike previous rounds where much of the setup work was done by beamline staff, Users will be required to lead setup work with only minimal assistance and oversight from beamline staff, who will focus mostly on setting up the optics and detectors. For User provided equipment, you need to take full responsibility for equipment and setup, including doing all plumbing, electrical and mechanical setup including installing it on the beamline yourself. Make sure you bring all the equipment, fittings, plumbing, connectors etc. you need because the beamline will typically not provide this support. Make sure you have fully bench-tested equipment before you arrive so it can be setup efficiently and operate reliably. You will also be responsible for mounting your samples and your equipment– make sure systems are fully compatible with our standard beamline mounting systems in advance. We do not plan to support last minute modifications or make adapter parts. It may well be worth contacting beamline staff in advance for advice or assistance when planning the details of your experiment. Sampson (Sample Setup Station) in the cabin allows you to setup experiments ahead of time, so consider coming to the beamline the afternoon before your beamtime and get yourself setup early. More information and advice on sample mounting and matching your setups to the beamline will be provided on the beamline website in the near future.
  • New 24/4/14: Very detailed guidance, recommendations and advice on preparing high quality proposals for SAXS/WAXS is now available here This material covers each of the major sections in the proposal system, gives some perspective on technical and safety feasibility assessment, and in particular provides specific guidance for each of the major disciplines currently running on the beamline including
    • Protein solution scattering
    • Time resolved analysis
    • In-situ measurements
    • Weakly scattering samples
    • Anomalous scattering
    • Grazing incidence scattering
    The material is designed to assist all proposals, primarily by describing the sorts of things reviewers often expect, and the quality of successful proposals. It is not intended to be prescriptive, but to outline ways to improve proposals based consistent patterns throughout many rounds of operations on the beamline. The material should be of benefit to most Users, particularly to those who may have missed out on beamtime and are looking to make their proposals more competitive. We will periodically update the information over coming cycles. Any feedback or suggestions are welcome: please send to the beamline’s email address.
  • New 24/4/14: From June 2014, Users will be required to take a much greater role and responsibility for setting up experimental equipment than has typically been the case in previous rounds. We are constructing a replicate of the sample stage and the space around the sample you use in the hutch with x-rays, outside in the cabin so that many setups can be put together and tested offline and then transferred quickly on the beamline. Details will be posted on the beamline website as soon as available. Unlike previous rounds where much of the setup work was done by beamline staff, Users will be required to lead setup work with only minimal assistance and oversight from beamline staff, who will focus mostly on setting up the optics and detectors. For User provided equipment, you need to take full responsibility for equipment and setup, including doing all plumbing, electrical and mechanical setup yourself. Make sure you bring all the equipment, fittings, plumbing, connectors etc. you need because the beamline will typically not provide this support. Make sure you have fully bench-tested equipment before you arrive so it can be setup efficiently and operate reliably. You will also be responsible for mounting your samples and your equipment– make sure systems are fully compatible with our standard beamline mounting systems in advance. We do not plan to support last minute modifications or make adapter parts. It may well be worth contacting beamline staff in advance for advice or assistance when planning the details of your experiment.
  • When planning the content of your experiment, be aware that SAXS/WAXS staff will be on site only until 6pm. Plan the scope of your experiment so that setups, changes in camera length, sample environment etc. are complete before 6pm. For example this will require camera length changes (if needed) to commence by 5 pm or that you will be able to perform your own setup or camera changes. After hours phone and remote support will be available via the control room until 11 pm. The beamline is operating on limited staffing which affects the amount of time available for experiment support.
  • Good proposals clearly state what q-range(s) are required. Poor proposals often don’t. We advise you to use the online q-range calculator available on the beamline website in order to plan your experiment and minimise delays from changing setup. Staff are happy to help in this aspect if you need any guidance or are unsure.
  • Protein solution Users: New Users are encouraged to seek advice and assistance from experienced Users, staff and/or from the PAC when formulating proposals and conducting their experiments. As a working guide, for medium sized proteins we recommend at the upper concentration end of dilution series around 50 µL of 1-5 mg/mL for static samples. Make sure you have buffer blanks available (e.g. by dialysis), and that you have checked samples are monodisperse in advance. We can offer an in-line size exclusion chromatography system on the Beamline for samples that require it. Users are advised to bring their own columns to ensure reliable performance – for details please contact Beamline staff. Please note that due to the dilution that occurs in the FPLC we recommend that samples are at least 5 mg/mL and 50 µL in volume. Proteins are normally run over the range of 0.01 to 0.3 Å-1 unless small (less than ~5 kD) or large (>~200kDa).
  • If you are intending to analyse samples in free capillaries, please note that you must bring sufficient capillaries for your experiment. The beamline strongly recommends using quartz capillaries (due to significantly improved data quality for weak scatterers over glass or Kapton) and also 1.5mm diameter due to the geometry of the beam and absorption lengths for water-based samples. We would not normally provide free-mounted capillaries.
  • The temperature inside the experiment hutch is typically 26 ºC. If you require temperature control, including if you are bringing you own sample environment equipment, please contact the beamline staff at least a week ahead so that we can properly assist you.
  • We must know from the proposal what equipment will be used during the experiment, in order to determine the technical feasibility of proposals. This is particularly the case if User provided equipment is needed, and such proposals must include sufficient detail to support its technical feasibility assessment. The minimum recommended cable length from the sample stage to the user area is 7m should you need o cable directly to your external control system.
  • Users are reminded that access to SAXS/WAXS beamtime is highly competitive, and that clearly demonstrating progress and outcomes from previous beamtime is a core part of evaluating proposals. If you have data from previous experiments it is in your interest to include key data supporting a new related proposal, and more particularly to convey the status of data analysis and interpretation, and outline conclusions if available. Make sure you update all accepted publications on the facility publications database through the website. Be concise but include all the important detail on samples in the experimental plan, in particular the details of any sample setups you wish to bring. Good proposals provide clear, detailed explanations of the estimated amount of beamtime required. Simply saving time on a lab-based instrument is unfortunately not a compelling reason even for outstanding science. It is often very helpful if lab-based SAXS data is included especially in areas where the technique has not been used before. A clearly defined scientific hypothesis can be very helpful in supporting the scientific case for a proposal.
  • Your Program Advisory Committee (PAC) members are working closely with beamline scientists to, amongst other things, (i) support beamline activities, (ii) represent your interests, and (iii) continue to develop an outstanding scientific program. The PAC is regularly briefed by beamline scientists and AS Management. Please contact PAC members if you have any questions or comments about AS operations and/or your scientific projects (future plans, clarification of proposal assessment, guidance etc) and please complete the AS feedback form as often as possible.
  • The SAXS PAC members are: Bridget Ingham (Callaghan Innovation NZ, bridget.ingham@callaghaninnovation.govt.nz), Patrick Kluth (Australian National University), James Murphy (Walter and Eliza Hall Institute), Robert Knott (ANSTO), Charlotte Conn (CSIRO), Suzanne Norwood (University of Quensland).
  • For successful proposals, one week before your beamtime the User Office process will require you to submit a form providing a detailed outline of your experimental requirements including changes expected during the beamtime. The beamline staff may ask for clarification or provide feedback on an experiment design, particularly if problems of technical feasibility or support/timing issues are identified. Staff are happy to advise and assist with any aspects of experiment planning.

Beamline Contact: saxswaxs@synchrotron.org.au

X-RAY ABSORPTION SPECTROSCOPY

 

OVERVIEW

  • The available energy range is 5 - 31 keV via the following operational modes:

Mode 1: 5 - 9 keV using Si(111)

Mode 2: 8.5 - 18.5 keV using Si(111)

Mode 3: 15 - 31 keV using Si(311)

  • Standard XAS experiments, that is where samples are mounted using standard sample holders and analysed at room temperature or in the He cryostat at 10K, are available in the first experimental station (Hutch B). Hutch B has 3 ion chambers and, currently, a 36 element Ge fluorescence detector. The setup in this end station is fixed and cannot be modified. Non-standard experiments are run in the second experimental station (Hutch C).

 

PROPOSAL GUIDELINES

  • A proposal guidelines document has been prepared by the Proposal Advisory Committee (PAC) and the beamline team. Please read these guideliens carefully and follow them diligently as they give important information on how to write a sound proposal for access to the XAS beamline. Failure to follow the guidelines makes it difficult for the PAC and beamline scientists to assess the viability of an experiment, thus likely rendering a proposal less competitive.
  • Proposals will necessarily be grouped together based on their energy range / operational mode and each proposal will only be allocated time for a SINGLE mode. If you need access to more than one beamline mode, please submit TWO separate proposals, one for each mode, and indicate that they are linked.
  • For fluorescence measurements an estimate of the absorber concentration is needed to assess feasibility. Typical scan times are: XANES 20 mins, EXAFS 45 mins.

 

EXPERIMENTAL ENVIRONMENTS

  • Hutch C, for non-standard experiments, is available for transmission type experiments, e.g. for in-situ heater work. Please contact the beamline team BEFORE you submit a proposal that seeks access to Hutch C.
  • Fast shutter, filters, and soller slits for fluorescence experiments are available.
  • A sample cryostat is available for use in Hutch B. Although the cryostat is vibration-less, as a matter of good XAS practice, samples always need to be prepared as homogeneously as possible in order to promote good spectral results.
  • The fluorescence detector readout time (overhead) is about 1 s per point.
  • We also have a PIPS fluorescence detector, which can be useful for certain experiments. This type of detector is not energy resolving and can be used for non-complex samples where the concentration of the element of interest is around a few 1000s ppm.

 

CONTACT

  • We strongly encourage you to contact us before you submit any non-standard proposal or if you have not used the XAS beamline before. Please contact us via xas@synchrotron.org.au

X-RAY FLUORESCENCE MICROSCOPY

BEAMLINE

Incident energy range: 4.2 to ~22 keV
Incident energy resolution: DeltaE/E = 10-4

MICROPROBES

KB mirror microprobe: ~1 μm focal spot. Stage range 100 mm * 100 mm.  Can be used with Vortex or Maia detector

Cryostream in commissioning 2014r3, should be ready for use in 2015. Contact Martin de Jonge to discuss if interested.

Fast stages and tomography in commissioning also; should be available in 2015. Contact Martin de Jonge to discuss

Zone plate nanoprobe achieves focal spot down to 80 nm (8 keV).  Energy range 7 keV - 11 keV typical.  Sensitivity and spot size (resolution) can be traded off against one-another - resolution is 200 nm for typical geological concentrations, 300 nm for typical environmental concentrations, and 500 nm for biological concentrations.  Can be used with Vortex detector (by default) or Maia detector (by special arrangement and subject to availability).

Recent studies in sources of elemental background and spectral noise have improved sensitivity to (eg) Zn by a factor of 5; however, sub-Ar metals are still poorly imaged due to the absence of a He atmosphere. This will be investigated in the next developmental step, due by ~mid 2015.

'Milliprobe' / large area scanner is under commissioning 2014r3 / 2015r1. Beam is defined by the exit silt, and so typical resolution is 200-μm. Capable of scanning objects of order 600-mm by 1200-mm, principally artworks. With some effort (and call for need) could be used for mapping western-blots simultaneously with the use of the microprobes. Contact Daryl Howard to discuss if interested.

DETECTORS

Vortex: silicon drift diode detector. Detector orientation: 90-degree. Energy sensitivity above 1.6 keV; energy resolution ~140 eV. Typical dwell 0.2-2 sec/pixel. Can be used with either the ZP Nanoprobe or the KB microprobe.

Maia: 384-element silicon array detector for on-the-fly acquisition in 180 degree ‘backscatter’ geometry. Energy sensitivity 3.3 to 19.5 keV; energy resolution 300-400 eV. Typical dwell 0.5-50 msec/pixel. Default operation is on KB mirror microprobe; ZP nanoprobe by arrangement and subject to availability. While this detector is extremely reliable, it is a research detector and so we do not carry a complete spare. As such, it is available on a best-effort basis: every experiment should anticipate using the Vortex detector as a back up if required.

UPDATE: Maia Rev B should be available by early 2015. Rev B has improved low energy sensitivity, and so should be able to map S (~2.2 keV), and possibly P (~2 keV). He environment is not planned for 2015r1; this may follow an assessment of operations with the new detector and stages, depending on demand.

DPC: segmented photodiode detector for differential phase contrast in transmission. Can be used with either the ZP Nanoprobe or the KB microprobe.
*** DPC RECENTLY RECOMMISSIONED ***

Transmission: Ion chambers and photodiodes
On axis, in-line optical microscope with ~1-2 μm resolution, 700 μm field-of-view. Backside viewing only.

MODES OF OPERATION

SFXM Scanning Fluorescence X-ray Microscopy

2D elemental mapping of fluorescence emission in the range 1.6 keV to ~22 keV (Vortex detector) or 3.3 keV to 19.5 keV (Maia detector).

Micro-XANES - spatially resolved x-ray fluorescence near edge spectroscopy

Single point XANES from 4.2 keV to ~22 keV (Sc to Ru, and L-edges falling within this energy range) using the Vortex detector. Stack XANES / imaging XANES from 4.2 keV to 19.5 keV covering modest areas using the Maia detector.
High monochromaticity XANES (311 crystal) is available - potential users should contact David Paterson to discuss their proposed study.

STXM Scanning Transmission X-ray Microscopy

Fast transmission maps (absorption and differential phase contrast) with incident energy range from 4.2 keV to ~22 keV

Fluorescence tomography

Single-slice (2-D) or volumetric (3-D) tomography on the KB microprobe is well established - ultimate resolution around 2-5 μm.  Specimen diameter must be small enough to avoid self-absorption (for a discussion of self absorption, see de Jonge & Vogt, Current Opinion in Structural Biology 20 (2010)).  Typical specimen size is 150 μm diameter, up to 1-mm long.

High-resolution tomography (500 nm resolution likely) is possible on the ZP nanoprobe for highly concentrated elements.

Potential tomography users should contact Martin de Jonge to discuss their proposed study.

If your experiment requires other capabilities, please contact the beamline scientists prior to submitting your proposal.
Proposals that do not fit within these capabilities may still be considered for beamtime at the discretion of the PAC.
Please contact beamline scientists to discuss your particular sample mounting requirements.
Beamline Contact: xfm@synchrotron.org.au

AUSTRALIAN NATIONAL BEAMLINE FACILITY (ANBF)

The ANBF (Photon Factory, Tsukuba, Japan) has been decommissioned and is no longer available. Additional information can be found on the external beamlines page. 

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