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Info for XRD1 Users

Sample Holders

In order to speed up measures, bring your samples already mounted on specific holders. Hereafter we list some of the common holders adopted according to the sample size and nature. Special attention has to be taken to the chemical nature of the sample support in case of fluorescence (link) analysis. In case of doubts, do not hesitate to contact the beamline staff.

  • Single crystals – for structure determination (small molecules, MOF, proteins, ..): we strongly suggest to use SPINE standardized holders and exploit the sample changer for sample manipulation in cryogenic conditions. Pin type and relative holders are described in detail hereafter. We can send you some holders and relative containers if needed. (contact the  beamline staff).
  • Powder samples in capillary: use borosilicate, kapton or quartz capillaries according to your needs. It is possible to use the classical pin support (fig.1) – mounting manually each sample – or a standardized SPINE base and use the sample changer for automatic sample manipulation and alignment to the photon beam.  In this case we recommand to keep the capillary length from 20 to 30 mm in order to allow the use of plastic vial caps (see "Single Crystal" samples section)  
  • Grazing incidence diffraction experiments: TBD
  • Bulky samples: voluminous or heavy (up to 500 grams) can be fixed directly on the goniometer head using the interface described in figure 3. In designing the sample support, goniometer linear and angular ranges as well as distances to X-ray nozzle, detector surface, and beam stopper have to be taken into account.

 

Sample Changer

The sample changer has a capacity of 50 samples mounted on SPINE standard bases. The sample changer can work in cryogenic conditions (e.g. single crystals for structure determination) as well as at room temperature (e.g. loose powders in capillaries). The sample changer uses ESRF SPINE style pucks and can accommodate 5 pucks at the time. We recommend that you use the pucks barcode to identify them and enable us to quickly locate your samples.

  • Cryogenic samples are expected to arrive at Elettra in dedicated dewars. In these cases (small molecules, MOF, proteins, etc.) we suggest to use SPINE bases with datamatrix 2D barcode printed on white background (they don't rust, last longer and are easier to read – see figures).  The sample-supporting pin should be 22 mm in length from the base to the start of the loop (this is default for the beamline: contact the beamline staff for different dimensions!). Samples on the relative bases have to be closed in the relative SPINE plastic vial (avoid screw-able and old-style vials!). Samples can be transferred to the relative containers (pucks, see figures below ) at the beamline if necessary.
  • Room temperature samples (like lose powders in capillaries or other small samples) are expected to be mounted on SPINE bases (we suggest to use bases with datamatrix 2D barcode printed on white background as are easier to read – see figures). Samples (in particular capillaries) must extend between 20 and 30 mm and have to allow the use of the SPINE plastic vial to encapsulate the sample. Please note that to be used for capillaries larger than 500 microns in diameter, the SPINE base have to be adapted, expanding opening to an appropriate size. Capillaries need to be glued at the base.
If needed, appropriate supports (bases, caps and pucks) are available at the beamline and can be borrowed. Supports can also be sent to your home institution to be prepared and sent back for remote or deputed data collection. Ask the beamline staff for availabilities.

 










Last Updated on Monday, 20 July 2020 15:19