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    XRD

    Uploaded by

    Hardik Chauhan

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    © All Rights Reserved
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    XRD

    Uploaded by

    Hardik Chauhan
    2 views2 pages

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    © © All Rights Reserved

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    © All Rights Reserved
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    2 views2 pages

    XRD

    Uploaded by

    Hardik Chauhan

    Copyright:

    © All Rights Reserved
    Download as DOCX, PDF, TXT or read online from Scribd
    Download as docx, pdf, or txt
    of 2

    Procedure

    1. Collecting Single Crystal XRD Data

    1. Grow suitable crystals for XRD. For more information, please see videos "Growing
    Crystals for X-ray Diffraction Analysis" in the Essentials of Organic Chemistry series
    and "Preparation and Characterization of a Quadruply Metal-Metal Bonded
    Compound" in the Inorganic Chemistry series.
    2. Add a drop of paratone oil to a glass slide. Using a spatula and a small amount of
    paratone oil, scoop some crystals from the vial used to grow the crystals and add them
    to the drop of oil on the slide.
    3. Under a microscope, select a crystal that has uniform, well-defined edges.
    4. Pick up the selected crystal using a suitable mount (here we use a Kapton loop). Make
    sure that there that any oil stuck to the crystal is minimal once it is mounted.
    5. Open the instrument doors.
    6. Attach the mount to the goniometer head on the instrument.
    7. Center the crystal with respect to the location of the X-ray beam.
    8. Close the instrument doors.
    9. Open the APEX3 software suite, a graphical user interface (GUI) for X-ray
    crystallography.
    10. Run a short data collection sequence and determine the unit cell.
    11. Based on the unit cell data, pick a data collection strategy and run a full data
    collection.
    12. Workup the data using a suitable program. Here we use SHELX in the APEX 3 suite.
    13. Refine the structure in a suitable GUI. Here we use SHELX in OLEX2.

    2. Loading a Powder Sample onto the Sample Holder for Powder

    XRD

    NOTE: Here we will use a Si crystal zero background holder. There are a

    variety of alternate sample holders that can accommodate different

    amounts of material. The Si crystal zero background holder produces no

    background noise from 20-120 ° (2 θ, using Cu radiation).

    1. Place a fine mesh sieve above the Si crystal.


    2. Pour approximately 20 mg of the sample onto the sieve, making sure that most of the
    sample is directly above the Si crystal on the mount.
    3. Tap the sieve on the bench top until a monolayer of sample covers the Si crystal
    surface.
    4. Unscrew the sample holder and place the crystal in the holder.
    3. Collecting a Powder XRD Pattern

    1. Open the instrument doors.


    2. Mount the sample holder in the instrument.
    3. Open the Commander software suite (a program used to collect powder XRD
    patterns).
    4. In the "Wizard" tab, load a standard data collection scan.
    5. Select the amount of time to run the scan (20 min). Running a longer scan over the
    same angle range will generate a better resolved powder XRD pattern.
    6. Select the angle range (2 θ) that will be scanned (5-70 °). The angle range selected
    depends on the material. The wavelength range given here is appropriate for
    molecular inorganic materials.
    7. Hit the "start" button to start data collection.
    Results

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