Rapid Access Mail-In

The Powder Diffraction beamline offers a rapid access mail-in service for powder samples in capillaries at ambient conditions. This service should not be used as a replacement for merit access that is available 3 times per year.

Commercial users cannot use the mail-in service and need to contact the beamline staff directly at: as-pd@ansto.gov.au

When does the proposal round open & close? Find out in the PD Rapid Access Mail-in section here

When does the proposal round open & close? Find out in the PD Rapid Access Mail-in section here

Notes

  1. Groups can only submit 1 proposal per round.

  2. There is a maximum of 20 samples or a 3 hour shift (whichever is smaller), per group per round. Users requiring more samples or beamtime can submit a merit round proposal. The experiment may be cut short if it exceeds the permitted 3 h.

The PD team aim to run samples before the end of the merit round however this cannot be guaranteed as beamtime availability may be affected by unplanned beamline or machine problems.

Please see our Frequently Asked Questions

 

Please see the following standard operating procedure (SOP) to assist in accessing the PD rapid access mail-in program.

Standard operating procedure (SOP)

 

Standard operating procedure (SOP)

 

Submitting a proposal

Users need to submit a short proposal in the Australian Synchrotron User Portal. Proposals can be submitted in the ~6 rapid access rounds offered per year, and are reviewed by our PAC. This proposal will require:

  • A title

  • A brief summary of the research to be undertaken and it's importance, including a description of why this work requires synchrotron radiation

  • A brief summary of the national benefit & applications of the proposed research,

  • How many samples will be measured

  • How much time is required for data collection from each sample

  • Energy required - The available energies are 21 or 16 keV. Details on how to choose an energy for you samples can be found here in the “Avoiding Fluorescence/ Absorption edges” section.

  • Address to send sample box kit if proposal is successful

  • Elemental composition and safety information

  • Sample & robot spreadsheet

  • Any lab XRD data you have - Submitting this data with your proposal is highly recommended

The PD team are not responsible for delays in running samples due to the postal address being incorrectly provided by the user. 

Sample Box Kit

When your proposal is approved we will send you a sample box and pins to mount your samples. The sample box will be sent to the address nominated during proposal submission. Staff will confirm this address before shipping the box and will include a return address label.

Some users with a small number if samples may be asked to send us the samples directly and will not receive a box.

The kit that will be mailed to you will contain:

  • Sample box

  • Pins - The number of pins sent will be the number of samples listed on the proposal. All must be returned to the AS when you return the sample box.

  • Wax

  • Protractor template

  • Return mailing address label

  • QR code with link to this web page (Confluence Cloud) - Here you can find information on how to prepare your samples and send them to the AS.

Users are required to supply their own capillaries as the PD beamline cannot supply them.

Please do not submit a proposal unless you have capillaries in time to prepare and send them back to us.

Users are required to supply their own capillaries as the PD beamline cannot supply them.

Please do not submit a proposal unless you have capillaries in time to prepare and send them back to us.

Experiment Authorisation

An Experiment Authorisation (EA) will need to be completed and approved before you return your sample box kit. There may be delays in measuring your samples if the box is returned before your EA is approved. The Australian Synchrotron cannot accept samples that are not associated with an approved EA.

A sample robot template needs to completed during proposal and EA submission. This requires the following to be input: sample box position, sample name, sample base/pin ID (printed on the base of the pin, i.e. PD201), number of positions (2), detector position 1 and 2 (difference of 0.5° 2θ), collection time (use the same for each detector position) and data file name. The data file name cannot have spaces, or special characters.

Robot Spreadsheet

 

Robot Spreadsheet

 

Safety

The PD beamline will only accept low risk materials for mail-in. All hazards of your samples need to be disclosed in the EA form otherwise the experiment will be cancelled. We cannot accept any samples that are:

  • Radioactive

  • Explosives or unstable materials

  • Fatal if swallowed

  • Fatal in contact with skin

  • Causes severe skin burns and eye damage

  • Causes serious eye damage; and

  • Fatal if inhaled

Sample Preparation & Mounting

Capillaries need to be 0.2-0.7 mm ID, and between 30 - 40 mm in length, as measured from the end of the pin. Larger ID capillaries cannot be sent as they are too fragile. The beam will be centered on the capillary 11 mm from the pin. Capillaries can be purchased from Charles Supper or Hilgenberg.

How to fill and mount a capillary

  1. Fill the capillary so that 45 mm of material is in the capillary.

  2. Break off the funnel, ensuring the capillary is ~45 mm in length.

  3. Insert the broken end of the capillary all the way into the sample pin.

  4. Melt a small amount of wax onto the capillary to fix it into position. Wax can be easily melted using a solder iron, or gas stove lighter. Check that the capillary is 30-40 mm, as measured from the end of the pin. The robot will break capillaries longer than 40 mm.

  5. Use the cardboard protractor to align the capillary in the pin, and ensure the difference between the sample pin base and capillary is <5°. Capillaries will not align on the diffractometer and be run if the angle is >5°.

How to fill and mount a capillary

  1. Fill the capillary so that 45 mm of material is in the capillary.

  2. Break off the funnel, ensuring the capillary is ~45 mm in length.

  3. Insert the broken end of the capillary all the way into the sample pin.

  4. Melt a small amount of wax onto the capillary to fix it into position. Wax can be easily melted using a solder iron, or gas stove lighter. Check that the capillary is 30-40 mm, as measured from the end of the pin. The robot will break capillaries longer than 40 mm.

  5. Use the cardboard protractor to align the capillary in the pin, and ensure the difference between the sample pin base and capillary is <5°. Capillaries will not align on the diffractometer and be run if the angle is >5°.

The PD team can provide information and tips on sample preparation and mounting. We are not responsible for samples that cannot be run due to incorrect mounting, poorly filled capillaries or not enough sample in the capillary.

Sending Samples to the Australian Synchrotron

Please follow the instructions on how to send samples to the Australian Synchrotron. All packages need to be addressed to the PD beamline and have the EA number clearly visible as without these there may be a delay in sample receival. There is a return shipping address included in the sample preparation kit. All samples need to be sent according to Australian and international transportation regulations.

Only send samples when your EA has been approved otherwise they may be sent back to you

Only send samples when your EA has been approved otherwise they may be sent back to you

Only send samples when your EA has been approved

All samples must arrive at least 7 days prior to the date of scheduled beamtime otherwise they will be run during the following scheduled beamtime.

PD will check all sample pins have been returned, and all samples are labelled correctly when the sample box is received. The samples will not be run unless all pins are returned.

The PD team have to right to delay running samples if all samples pins are not returned to the AS.

Address to send samples:

STORES

Attention: PD Beamline

Experiment Proposal Number (EPN): → Don’t forget to fill this in

ANSTO - Australian Synchrotron

800 Blackburn Rd

Clayton VIC 3168

Australia

The PD team are not responsible for any capillaries that are received broken or capillaries that break during analysis.

The PD team are not responsible for incorrectly labelled samples, or information incorrectly entered by the user into the robot spreadsheet.

Data Collection

Parameters for data collection need to be specified in the robot spreadsheet at the time the EA is submitted. These parameters cannot be changed once the EA is submitted.

All samples will be run using our robot at the next available beamtime.

After your Experiment

Beamline staff will email you with details on how the data was collected and how to access your data. Please remember to acknowledge the beamline in all publications!

Sample Disposal

All samples will be disposed of at the Australian Synchrotron.