Beamline updates

 

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 not available.

  • 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 and 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 KBrPEand 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

  • Program proposals valid for up to 2 years will be accepted in addition to normal proposals

  • Please specify in your proposed experiment the total number of shifts anticipated to be required over the life of the program proposal and submit a separate beamtime request for the number of shifts required in round 2010/3

  • Energy range from 5.5 - 18 keV 

  • User changeable energy from 9.0 to 17.5 keV

  • Fluorescence scans for MAD and metal identification

  • MAD energies from 9 - 17.5 keV

  • Robotic loading and remote access is available

  • Rapid access is available.

MX2: Micro Crystallography beamline

  • Program proposals valid for up to 2 years will be accepted in addition to normal proposals

  • Please specify in your proposed experiment the total number of shifts anticipated to be required over the life of the program proposal and submit a separate beamtime request for the number of shifts required in round 2010/3

  • Microfocus beam with FWHM of 30x30 microns (HxV)

  • Extremely high flux with up to 3e12 ph/s/mm2 in the focussed beam

  • High resolution high framerate sample video for alignment of microcrystals

  • User changeable energy

  • Fluorescence scans for MAD and metal identification

  • MAD energies from 5.5 - 21 keV

  • User-changeable micro-collimator now available with 20, 10, 7.5 and 5 micron apertures

  • Robotic loading and remote access.

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POWDER DIFFRACTION

PROPOSAL PREPARATION
  • Users can find tips on proposal preparation under 'Beamtime on this beamline' on the powder diffraction beamline's 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.

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’ at http://www.synchrotron.org.au/index.php/aussyncbeamlines/powder-diffraction/samples/sample-types
  • 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 / 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 use in 2012 are:
    • Cryostream (80-450 K)
    • Hot-air blower (100-900 °C)
    • Furnace (25-2300°C)
    • Gas/vacuum flow cell for capillary samples
    • High-throughput stage

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SOFT X-RAY SPECTROSCOPY

  • The grating change mechanism has been repaired in January 2011 and both gratings are now available for use. Commissioning to ensure the correct alignment and hence the excellent photon energy resolution of this beamline is ongoing and will be complete by the end of March 2011.
  • The electronics for the Micro Channel Plate partial electron yield detector cannot be relied upon to operate in the partial electron yield mode. However the detector does operate extremely well as a total fluorescence (TFY) detector.   Extremely good data can be taken in TFY mode for light elements B, C and Nitrogen. 
  • The beamline prior to the grating mechanism repair was operating very well with all user systems working reasonably well. During the extended commissioning period maintenance activities on the user chamber are being carried out to ensure that this system stays at peak performance.
  • 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 we would be happy 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 SCATTERING

  • The operations of the SAXS/WAXS Beamline have been reviewed and revised. In order to sustain critical beamline developments and the high numbers of experiments scheduled, SAXS/WAXS staff will be on site only until 6pm. After hours phone and remote access support until 12 pm will be available via the control room. You must plan the details of your experiment so that all setups, changes in camera length, sample environment etc. are be completed before 6pm. For example this will require camera length changes (if needed) to commence no later than 5 pm.

  • Proposals are required to clearly state what q-range(s) are required. 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.

  • Protein solution Users:  New Users are encouraged to seek advice and assistance from experienced Users and/or from the PAC when formulating their 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 Biologic FPLC 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 capillaries, please note that you must bring sufficient capillaries for your experiment. The beamline strongly recommends the use of 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 cannot guarantee to provide capillaries.

  • The temperature inside the experiment hutch is typically 28 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 what equipment will be used in order to determine the technical feasibility of proposals. Make sure you clearly state whether you plan on using equipment from the Beamline or whether you are planning to bring your own equipment. The minimum cable length from the sample stage to the user area is 7m.

  • Users are reminded that SAXS/WAXS beamtime is highly oversubscribed, and that clearly demonstrating progress and outcomes from previous beamtime is a critical part of evaluating proposals. If you have any data from previous experiments please include an example, and more particularly outline your conclusions and any useful comments. Make sure you update all submitted and accepted publications on the facility publications database through the website. Be concise and include all the important detail on samples and the experimental plan. A clearly defined hypothesis can be very helpful. 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.

  • Your PAC members are working closely with beamline scientists to, amongst other things, (i) support beamline scientists, (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: Kevin Jack (University of Queensland, This e-mail address is being protected from spambots. You need JavaScript enabled to view it), Craig Buckley (Curtin University), Matthew Wilce (Monash University), John White (Australian National University), Tracey Hanley (ANSTO), Terry Mulhern (University of Melbourne).

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X-RAY ABSORPTION SPECTROSCOPY

 

  • A strategic plan to implement improvements at the XAS beamline is now in progress. Please click here for details.
  • A proposal guidelines document (click here) has been prepared jointly by the Proposal Advisory Committee and beamline staff. The document identifies the questions that need to be addressed in the proposal. Failure to address all of these points is likely to render the proposal uncompetitive. New users to the XAS beamline are strongly urged to contact beamline staff well in advance of the proposal deadline to assess the feasibility of their proposed experiments.
  • Standard XAS experiments (i.e. samples mounted onto XAS standard sample environments – room temperature sample stick or He cryostat) are available in the first hutch (B) which contains 3 ion chambers, 100 element Ge fluroescence detector, 12 - 300K cryostat and room temperature sample stick.  This end station is fixed and cannot be modified.
  • The available energy range is 5.5 - 42 keV via the following operation modes:
o    Mode 1: 4 - 10 keV focussed ~ 0.25 x 2 mm Si(111) 1010 - 1012 ph/s
o    Mode 2: 8 - 18 keV focussed ~ 0.25 x 2 mm Si(111) 1010 - 1012 ph/s 
o    Mode 3: 15 - 22 keV focussed ~ 0.25 x 2 mm Si(111) 1010 - 1012 ph/s
o    Mode 4: 15 - 35 keV focussed ~ 0.25 x 2 mm Si(311) 109 - 1011 ph/s
o    Mode 5: 10 - 42 keV unfocussed < 3 x 15 mm Si(311) (no mirrors, thus no harmonic rejection)
 
  • Proposals will necessarily be grouped together based on their energy range / operation 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.
  • Cooling issues with the first mirror are expected to be rectified in Jan 2012.
  • Hutch C, for non-standard experiments, will not be available.
  • Fast shutter and filters / soller slits in front of the 100 element detector are available.  
  • Vibration of the sample in the cryostat is a significant issue for data quality for transmission samples that cannot be prepared as a uniform thin film.
  • The 100 element detector will be operating in step-settle-read-step mode with a non-negligible overhead..
  • For fluorescence measurements some estimate of the absorber concentration is needed to assess feasibility. Normal fluro scan times should be: XANES 20 mins, EXAFS ~ 60 mins. As a guide users should expect to perform 1/2 the number of fluorescence scans compared to ANBF for similar data quality.

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X-RAY FLUORESCENCE MICROSCOPY

  • Beamline
  • Microprobes
    • KB mirror microprobe with 2 by 1 micron focal spot (H by V). Stage range 100 mm * 100 mm. Compatible with Vortex and Maia detectors.
    • Zone plate nanoprobe with 80 nm focal spot (<7 keV) or 150 nm focal spot (>8 keV). Compatible with Vortex detector only (at present).
  • 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. Presently compatible only with the KB mirror microprobe.

      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. 
    • 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 absorption 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.
    • 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 (<~500 micron diameter) at ~2-5 micron resolution using the KB mirror microprobe with the Maia384 detector.
      High-resolution tomography (500 mn likely) is possible on the ZP nanoprobe, but presently untested.
      Potential tomography users should contact Martin de Jonge to discuss their proposed study.
    • High monochromaticity XANES (311 crystal) is available.
      Potential users should contact David Paterson 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) operates with the support of ARC LIEF funding channelled through the Australian Synchrotron until the end of 2012. Access to the ANBF is subject to availability.

    This mature facility complements the XAS capabilities available at the Australian Synchrotron XAS beamline.

  • While both fluorescence and transmission measurements are possible at both beamlines, the bending-magnet-based ANBF is best suited to experiments requiring low-medium energy and/or low-medium photon flux. The wiggler-based Australian Synchrotron beamline is more appropriate for medium-high energy and/or high photon flux experiments. Applicants seeking beamtime at either the ANBF or AS are encouraged to indicate and justify their preferred choice of beamline or contact the beamline scientists for advice.

  • Experiments requiring powder diffraction capabilities are no longer feasible at the ANBF.

    As a condition of the LIEF grant, funding for travel and accommodation at the ANBF is only available to Australian-based university researchers, including those with honorary positions, and applications should be lodged with the relevant university research office.

    Further information is available on the external beamlines page.

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