Beamline updates

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 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.

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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.

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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.

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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 0.05 mm are required.
    • For experiments requiring pressures: 10 – 20 bar, quartz capillaries with a wall thickness of 0.1 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
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.
 
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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.
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SMALL AND WIDE ANGLE X-RAY SCATTERING

  • 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, This e-mail address is being protected from spambots. You need JavaScript enabled to view it), 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.

 

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X-RAY ABSORPTION SPECTROSCOPY

OVERVIEW

  • The available energy range is 5 - 35 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 - 35 keV using Si(311)
  • Standard XAS experiments (i.e. where samples are mounted using standard sample holders and analysed at room temperature or in the He cryostat) are available in the first experimental station (Hutch B). Hutch B has 3 ion chambers and a 100 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 scientists. These guidelines aim not only at improving proposal quality further, but also to encourage more user / beamline scientist interaction prior to proposal submission. Please follow these guidelines diligently. Failure to follow these guidelines makes it difficult for the PAC and beamline scientists to assess the viability of an experiment, thus likely to render your proposal uncompetitive.
  • Proposals will necessarily be grouped together based on their energy range / operational mode and proposals will only be allocated time for a SINGLE mode.   Proposals needing more than one mode of operation MUST be duplicated for each mode.
  • For fluorescence measurements an estimate of the absorber concentration is needed to assess feasibility. Normal scan times are (minimum): XANES 20 mins, EXAFS 45 mins.

LATEST NEWS

  • Hutch C, for non-standard experiments, is available for transmission type experiments, e.g. for in-situ heater work. The This e-mail address is being protected from spambots. You need JavaScript enabled to view it must to be contacted prior to submitting a proposal that seeks access to Hutch C.
  • Fast shutter and filters / soller slits in front of the 100 element detector are available.
  • A new cryostat has been installed in Hutch B. The cryostat significantly reduces sample vibration and thus enhances data quality. However, and as a matter of good XAS practice, samples always need to be prepared as homogenously as possible in order to promote good spectral results. Do note that we no longer pre-cool the cryostat sample rod in liquid nitrogen prior to insertion into the cryostat. Please contact the This e-mail address is being protected from spambots. You need JavaScript enabled to view it if you have any questions.
  • The 100 element detector readout time (overhead) is about 1 s.
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X-RAY FLUORESCENCE MICROSCOPY

  • BEAMLINE
  • Incident energy range:               4.2 to 25 keV
  • Incident energy resolution:     DeltaE/E = 10-4
  • MICROPROBES
  • KB mirror microprobe: 2 micron focal spot (H by V). Stage range 100 mm * 100 mm. Can be used with Vortex and Maia detectors
  • Zone plate nanoprobe with 80 nm focal spot (<7 keV) or 150 nm focal spot (>8 keV). Can be used with Vortex detector (by default) or Maia detector (by special arrangement and subject to availability).
  • DETECTORS
  • Vortex: silicon drift diode detector. Detector orientation: 90-degree. Energy sensitivity 1.5 to 25 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.
  • DPC: segmented photodiode detector for differential phase contrast in transmission. Can be used with either the ZP Nanoprobe or the KB microprobe.   NOT PRESENTLY AVAILABLE
  • Transmission: Ion chambers and photodiodes
  • On axis, in-line optical microscope with ~5 um resolution, 700 um field-of-view.  Backside viewing only.
  • MODES OF OPERATION
  • SFXM Scanning Fluorescence X-ray Microscopy
  • 2D elemental mapping of fluorescence emission in the range 1.5 to 25 keV (Vortex detector) or 3.3 to 19.5 keV (Maia detector).
  • Micro-XANES - spatially resolved x-ray fluorescence near edge spectroscopy
  • Single point XANES from 4.2 to 25 keV (Sc to Ag, and L-edges falling within this energy range) using the Vortex detector.
  • Stack XANES / imaging XANES from 4.2 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 to 25 keV
  • Fluorescence tomography
  • Single-slice (2-D) or volumetric (3-D), on small specimens (typically <500 micron diameter) at ~2-5 micron resolution using the KB mirror microprobe with the Maia384 detector.
  • High-resolution tomography (500 nm likely) is possible on the ZP nanoprobe, but presently untested.
  • Potential tomography users should contact Martin de Jonge to discuss their proposed study.
  • Large area mapping (600 mm X 300 mm) with 20 – 200 micron resolution is in commissioning.  Potential users should contact Daryl Howard to discuss the status of this capability.
  • An FAQ is available to assist you with your application: Click here.
  • 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.
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  • 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.