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Inform your local contact of any packages that you are sending and provide them with information such as tracking numbers and estimated delivery dates. See Shipping Goods to Diamond for more information.
Know Your Samples
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It is important to characterise the samples for a PDF experiment as comprahensively as possible before the 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 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 in either g cm-3 or atoms Å-3.
- Packing fraction - This is a value between 0-1 and is often estimated to be ca. 0.6.
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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. |
There are additional factors that should be considered regarding the samples, such as;
- Are there any peaks at low Q? This may require the beamstop 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 and given a friendly reminder at the start of your beamtime. Q is defined as;
- 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?
- Have you packed as many capillaries as you can at your home institution? We will post empty capillaries to you where necessary. Please refer to the "Know Your Setup" section and discuss with your local contact.
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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) |
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If you are bringing your own cell this should be brought to the attention of the local contact and discussed in detail. This should be done well in advance of the beamtime to address any issues that may become evident. |
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It's time for you to return to your home institution with high quality PDF data in hand.
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The following section is designed to walk you through the beamline checkout process.
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- All of your samples are packed to be taken off site with you when you leave.
- All of your equipment and chemicals are boxed up ready for collection by courier at a later date.
- You have disposed of any gloves, bench protectors and waste through the appropriate route.
- All equipment is clean and returned to the appropriate storage location, including pestle and mortars, spatulas etc.
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