You’ve written an amazing proposal and the panel has awarded you time, congratulations! Now you need to prepare for your experiment to make sure you get the best use of your time. On this page, you’ll find some general information which is applicable to most experimental sessions that run on I15-1. There are also some more specific instructions for particular experiment types on the following pages:
General Information About Preparing for a Session
Some considerations that apply in some way to most experiments on I15-1.
Fed IDs
Everything at Diamond is accessed using your federal identification, or fed id. If you haven’t committed it to memory, you should ensure you have access to it when you arrive at Diamond.
User Office Arrangements
Once your experiment has been scheduled, you will be required to complete the user office arrangements section on the UAS. You will need to complete this section even if you have been awarded remote or easy access time, as it is here where you select who has access to the data.
Experimental Risk Assessment
Whichever access route you have taken, it is essential that you fill in the experimental risk assessment on the UAS.
The Experimental Risk Assessment (ERA) is the place to record and address any hazards that may arise from your experiment. It is critical to complete the ERA for all experiment types at Diamond.
Samples
One of the most common hazards for an experiment at Diamond is the samples themselves. Every sample that you bring to Diamond must be covered by one of the sample entries in the ERA. Your experiment might be to look at 10 samples of very similar composition with the same associated risks: in this case you need only submit one sample to the ERA.
The sample acronym is going to be important for identifying your samples later on. Make sure all your samples have unique and relevant acronyms.
Equipment
If you’re bringing your own equipment to I15-1 (i.e. your own in situ environment) then you need to risk assess it here.
Experimental Methods
Here you should specify all of the processes which are going to occur on the beamline during your experiment. For even the simplest experiment, you will still be mounting and unmounting samples from the beamline so you should describe here how that is going to be done, and any precautions you need to take.
Lab Access
If your experiment involves you coming to Diamond (i.e. it’s not an easy access experiment); you should request lab access. This is required for you work in our side labs, irrespective of how non-hazardous your samples are.
Even if you are planning on loading your capillaries before you come to Diamond, you may need some lab space to reload capillaries in the event that one of them gets broken.
Sample Information
In order to get a PDF from your sample, we need to know a few things about it, including the composition, density, and packing fraction.
It is important to characterise the samples for a PDF experiment as comprehensively as possible before your beamtime. The three key properties that are required are;
Sample composition - Quantitative analysis should be performed to identify the most accurate composition possible for the samples. This is the full composition for the sample, including any water, binder or support materials that may be present, not just the composition of the material of interest.
Density - The density of the sample should be known, preferably in g cm-3
Packing fraction - This is a value between 0-1 and is often estimated to be ca. 0.6.
The sample composition, density and packing fraction are essential parameters that should be known as accurately as possible in order to perform the data reduction step and generate the PDFs.
A range of suitable analysis methods should be performed such as XRF, TGA/DSC-MS etc. to characterise the sample in advance of the beamtime.
Additional information such as amorphous content, concentration of impurity phases etc. will also be useful during analysis.
Additional Factors
There are additional factors that should be considered regarding the samples, such as:
Are there any peaks at low Q? This may require the beam stop to be moved further from the sample. If you have a peak at Q ≤ 1 Å-1 then your local contact should be made aware before the experiment. Q is defined as 4 π sin(θ) / λ.
Have you simulated the pdf and the scattering data for comparison?
Do you have .cif files that you can bring with you?
Which of your samples are likely to be the most strongly scattering? This can be effected by the concentration of highly scattering elements, the crystallinity of the sample and the presence of large crystallites in your powder.
Is your sample a "good" powder? Are there likely to be larger crystallites that need further grinding to give a good powder average?
All samples should be labelled with the visit number, date, name of the investigator/group and a suitable description of the material (i.e. the full composition including any support materials/binders).
Laboratory Information Management System
We use a LIMS called ispyb to track sample and data collection information.
You can read full instructions on uploading your sample information here.
Consumables
We supply capillaries for experiments that require them.
If you require particular chemicals or reagants for your experiment, you are encouraged to bring your own wherever possible. It is also good practice to inform you local contact of any requirement so that they can ensure that you are booked into an appropriate lab in advance of your arrival.
We currently do not have gas mixing capabilities on the beamline and so any special gas mixes must be ordered at least 8 weeks in advance. It is essential that you local contact is informed even if only common gases are required (e.g. CO2) so that stocks can be maintained and delivery can be arranged from the EHCs.