|
Experimental: Sample and Experimental Details |
Course Material Index
Section Index
Previous Page
Next Page
Experimental: Sample and Experimental Details
Listed below are points which should be included in the descriptions of
the material the data is collected on, its preparation for data
collection and the data collection itself. Some of the information may be given
in tabular form; various common options are
outlined for guidance.
- Sample Details
- the material itself - whether synthesised in the laboratory, purchased from a company or extracted from the earth;
- preparation of the powder - how it was ground; if it was sieved or mixed with a
support material to reduce preferred orientation.
- sample holder and collection geometry - flat plate for reflection, capillary tube for transmission.
- sample details - dimensions of specimen; if the sample was open to the
atmosphere during collection or not.
- sample environment - whether the sample was studied at non-ambient
temperature (cryostat, furnace) or pressure (diamond anvil).
- Diffractometer and Data Collection Details
- radiation source - options include sealed X-ray tube (specifying target metal),
a synchrotron for X rays, or a neutron reactor or spallation source for
neutrons.
- radiation - the wavelength (with an error on the value if it was calibrated)
if it was monochromatic, or whether a white beam was used.
- diffractometer - the type of instrument; the geometry (Bragg-Brentano,
Debye-Scherrer) in which it was operated.
- pre-sample devices - monochromator (give the material
and diffraction plane used) or filters.
- pre-detector devices - monochromator or Soller slits.
- detector - type (scintillation, position sensitive detector, image plate)
and specific details.
- scan details - including the type of scan (step or continuous); 2q range;
step size; detector counting time at each step.
- the software used to operate the diffractometer.
Interpretation
When reading these sections in an article you should be looking for the points
described above in the text or tables. If the information is presented well you
should be able to visualize the type of experiment that was performed, and this
should start you thinking about problems that may have arisen. You should
remember to look for discussion of such problems later in the article. For
example, if the sample is prepared so as to avoid preferred orientation, you
should look to see if this preparation overcame the problem or whether
corrections were applied in the refinement procedure, if values of related
parameters occur in any of the tables or if there are any traces of preferred
orientation in the final plots.
Course Material Index
Section Index
Previous Page
Next Page