Beamline Proposal & Experiment Guide

Hints for a Successful Beamline Proposal

The number of applications the Powder Diffraction beamline receives each round always exceeds the amount able to be accepted. For your proposal to be competitive, it is important to follow the guidelines below.

Additional information, including our proposal round deadlines, can be obtained on the general User Guide Melbourne website.

For further information, email us at: AS-PD@ansto.gov.au

General Hints

Understand what you want to measure and what you want to obtain from the data.
Prepare proposals early to allow enough time to complete it properly, and to also have time to make enquiries, and receive a response.
Students cannot be the principal investigator on a proposal.
Take care to describe the synchrotron-relevant aspects of your experiment and describe them in sufficient detail.
Consider the skills needed to successfully carry out the experiment. If you do not know how to process the data is there someone you could collaborate with?
Plan your experiment so you maximise your beamtime. We recommend preparing your samples before your arrival.

Technical Feasibility

Proposals will be initially assessed by the beamline staff for technical feasibility. It is highly recommended to confirm the feasibility of your proposal before submitting. Typical reasons why proposals are marked unfeasible include:

Safety procedures are not adequately described – All experiments need to be carried out in a safe manner at all times. It is extremely important that the researchers have considered strategies to minimise hazard exposure as well as not damage our equipment. For example, consider what will happen if there is a material spill?
Sample composition – Sometimes based on the composition of your sample, an energy that avoids absorption edges and minimises micro-absorption (from high Z elements) cannot be selected. The energy range of the PD beamline is 8-21 keV. Please talk to a Beamline Scientist to check.
Insufficient or confusing information – The experiment is not explained in enough detail, or is not explained clearly, therefore we are unsure what you want to do and what resources you need.
Researchers haven’t discussed the experiment with beamline staff prior to proposal submission –This is mandatory if you are bringing your own sample environment/equipment as we need to know that it will work on the beamline. Also, this is mandatory for all experiments using flammable gases or those needing a pressure higher than atmospheric.
Generation of toxic gases – The beamline currently does not have an extraction system in the hutch to remove toxic gases such as CO or H₂S. Proposals cannot be accepted if toxic gases will be generated.

Writing the Proposal

All proposals will be evaluated by external reviewers and members of the Proposal Advisory Committee (PAC). There are three evaluation categories to consider when preparing proposals with reference to the evaluation categories:

Scientific relevance and merit – Ensure that reviewers can easily determine the scientific value of the synchrotron experiment you are seeking to undertake and how it will contribute to the relevant field of research or application.
Track record of applicants, particularly publications resulting from prior Australian Synchrotron beamtime – It is now necessary to upload prior publication(s) resulting from use of ANSTO facilities to the online proposal system. This listing will be used to evaluate the likelihood of a publication arising from the proposed experiment, based on previous history. For new users, their publication history and laboratory experience will be evaluated.
Need for synchrotron radiation – This aspect is a valuable tool in gauging whether it is understood what a synchrotron experiment will contribute to the research. There are many reasons why a synchrotron experiment is sought and may include: the properties of the radiation, the time scale of the experiment, the resolution of the data, the experiment set-up that is achievable, etc.

Tips on Completing the Proposal Sections

National benefit and applications of the proposed research –It is extremely important to demonstrate why this research is important to Australia and what are potential long term outcomes for the nation. Does your research align with an Australian Government Science and Research Priority? The application of this work needs to be described and how it will contribute to advancing Australia’s scientific knowledge. One sentence is not enough for this section. Also, include where you plan to publish your synchrotron data?
Experience of participants, and outcome of previous Australian Synchrotron experiments – For all researchers, include their title, institution, research interests, their number of publications, powder diffraction workshops and conferences attended, and describe their powder diffraction expertise in the laboratory and at synchrotron facilities. Include what each participant will contribute to the experiment, and detail who has expertise in the materials used, and who has expertise in diffraction data analysis.
The need to use Synchrotron Radiation for this research– Application need to show proof of concept of why the experiment cannot be carried out in the laboratory. All proposals should contain laboratory powder diffraction data with areas of interest highlighted and easily visible. Also, if the beamtime proposal relates to ‘nano-sized’ crystallites, representative laboratory data MUST accompany the proposal to demonstrate the sample has sufficient long-range order. Data from other techniques can also be included if it will assist in assessing the feasibility of the experiment.

Completing the Section 'Proposed Experiment'

Details of a typical experiment need to be described. Sufficient detail needs to be included for the proposal to be accurately assessed. When submitting proposals, users should take care to address the following experimental and technical aspects:

How many samples are to be analysed? – Clearly indicate the number and identity of the samples that are the subject of the synchrotron proposal.
Sample mounting –Determine how the sample(s) will be mounted: this may be either in a capillary or a flat plate or on an alternate sample mount that is to be user-supplied. If the sample stage or mount is supplied by the user, please contact beamline staff prior to submitting the proposal to discuss the requirements. Note that small capillaries reduce absorption (and improve resolution when using the Mythen detector) but reduce the amount of scattering material.
Sample environment ancillaries – Indicate whether a sample environment, such as a temperature ancillary or gas flow equipment, is required (whether user-supplied or provided by the Australian Synchrotron). Describe the temperature range and regime to be used, if relevant. Experiments at high pressure are complex and users are encouraged to contact beamline staff before submitting their proposals. The maximum pressure allowed on the beamline is 20 bar. It is mandatory to contact the beamline for all experiments needing pressures greater than atmospheric.
Time requested – The amount of beamtime requested for the experiment must be justified by taking into account such details as the following: set-up time, number of samples, temperature regime, etc. Contact staff to determine how much time will be required for your setup. Please note, time will be allocated in units of days, however, the portal requires the total number of shifts to be entered; there are 3 shifts per day. It is strongly advised to convey this information using a table.
Please explain how you intend to analyse the data you collect – It is important to describe in detail how you will analyse the data and what information do you hope to gain from the experiment. Discuss what you will be determining, as it is not sufficient to just list the software packages you will use.
Describe in detail any hazards selected above and any safety procedures used to control the associated risks – Outline all safety procedures for all steps of the experiment, as it needs to be made clear that the researchers are aware of the hazards associated with their experiment and have thought about how to mitigate the risks. Information on why a particular pH, gas or temperature program needs to be included. If a hazardous material will be produced from a reaction carried out at the beamline, a calculation should be provided to estimate the quantity of this material produced.

Before your Experiment

Primary Investigators (PIs) are responsible for organising their experiments. Please be aware of the following:

Experiments should be adequately staffed at all times. It is recommended that at least two people be present at or near the beamline during experiments at all times.
Ensure that ALL your samples and their hazards are listed on the Experiment Authorisation (EA) form more than one week before the schedule experiment date. Please include any risk assessments and highlight any OHS concerns. Any samples that are not listed on the EA form will not be allowed at the beamline. If samples that are not on the EA form are run on the beamline, the experiment will be cancelled.
Ensure you bring all required equipment onsite as the beamline has limited resources. The beamline cannot supply ferrules and many capillaries. Consider bringing gas fittings, lines, and regulators the day before your experiment as this will also minimise setup time. Please note all of our Swagelock fittings are in metric sizes and we don't have adapters to imperial fittings.

The Day of your Experiment

Following successful completion of the facility safety induction, users need to participate in the beamline-specific safety induction, prior to beginning their experiment. All experiment participants are requested to make themselves available for this induction at the beginning of the experiment as ONE group.
Researchers should arrive at the time said to them by the Beamline Scientist. Arriving before this time will not speed up the setup.
It is unacceptable for individual researchers to attend an experiment for more than 12 h straight without going home or back to their accommodation to rest. Operating the beamline in these situations is unsafe, and the experiment will be cancelled.
Experiments involving hazardous procedures (flammable gas at any pressure or inert gases at pressures >10 bar), requires the presence of 2 people at the beamline at all times. One person needs to be vigilantly watching the experiment at all times from the camera in the cabin in case there is an issue. This means the researcher watching the experiment is also not on their telephone or computer while watching.