Frequently Asked Questions

Q: Can I run 20 samples each at 30 min?

No, as the total time for the analysis will be ~10 h and there is a maximum of 3 h for an experiment

 

Q: Can I run 40 samples each at 4 min?

No, although the total time for the analysis is ~160 min and less than 3 h, there is a maximum of 20 samples for an experiment

 

Can I come onsite for the experiment?

No, the rapid access round is for mail-in samples only. Sample kits are also able to be picked up and the samples then dropped off to the Australian Synchrotron, by prior arrangement only.

What acquisition time should I put for my samples in the robot spreadsheet?

Estimate how much time is needed based on the chemistry, degree of crystallinity and what information you want to obtain from the data. Generally 150 seconds a position is a good place to start.

 

Where is the robot spreadsheet?

The robot spreadsheet needs to be submitted for the proposal and EA. It is an additional tab at the bottom of the sample spreadsheet.

The pin numbers can be left blank when submitting your proposal but they need to be filled in when submitting your EA.

 

What capillaries should I buy?

These can be purchased from Charles Supper or Hilgenberg. They are typically made from glass, boron rich glass or quartz and the choice of which one to buy depends on (1) if you samples will react with any of the materials and (2) if the capillary will be heated.

The quartz capillaries are more resistant to heat and chemical corrosion but can be more fragile compared to glass capillaries. We have received samples in both glass and quartz capillaries that haven't broken during transit. As the mail-in experiments are only carried out at room temperature it might be unnecessary to have quartz if your samples don't react with glass. The boron capillaries are considered to have the lowest absorption.

Thin walled capillaries (0.01 mm) x 80 mm capillaries are generally sufficient for the mail-in program but need to be 0.2 - 0.7 mm in diameter.

 

What is the difference between the experiment setup at PD and my laboratory XRD?

Powder diffraction data is collected differently at the synchrotron compared to the laboratory.

In a common laboratory XRD, the X-ray tube and detector move and go through the angles step-wise (Bragg-Brentano geometry – usually point detector). The start and finish angle need to be specified.

At PD we measure the intensity of all diffracted X-rays at the same time (Debye-Scherrer geometry – 1D detector) so don’t specify an angular range. We need to specify the starting angle (i.e. position - 3 degrees) and our angular range is determined by the number of modules in our detector. Our detector has 16 Si modules, each covering 5 degrees, so can collect 80 degrees 2theta. The two positions - 3 degrees and 3.5  degrees is because our detector has gaps between the modules, so we collect data at 3 degrees, then move the detector to 3.5 degrees, and collect again. The data is spliced and normalised together so the gaps are removed. Our users ccan do this using PDViPeR.

 

When will my data become available?

We aim to have the data available within 2 weeks of the scheduled beamtime. However, there may be delays due to unplanned beamline or machine problems. Beamline staff will contact you when the data is available.