X-ray diffraction shared experimental facility




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CENTER FOR MATERIALS SCIENCE & ENGINEERING

at MIT


X-RAY DIFFRACTION SHARED EXPERIMENTAL FACILITY


Standard Operating Procedures


for the


Rigaku Cr-Source

RU300 Rotating Anode X-Ray Generator

185mm Radius Diffractometer


Scott A. Speakman


13-4009A

253-6887

speakman@mit.edu


http://prism.mit.edu/xray


Revision: 3 October 2011


These instructions describe the proper operation of the Rigaku RU300 Cr-source Rotating Anode X-ray generator and the MDI DataScan data collection software. The diffractometer attached to the generator is a Rigaku D/Max-b 185mm radius goniometer with diffracted-beam monochromator and scintillation point detector.


If there is any problem with the generator or diffractometer, you are required to report it to Scott Speakman immediately (13-4009A, x3-6887, speakman@mit.edu).

If the problem poses a safety hazard, turn off the generator (even if a scan is in progress) and post a note on the enclosure (so that no one else tries to use the instrument). Remember, you are not just responsible for your own safety; you are also responsible for the safety of those around you.


Operating Instructions: Abridged Checklist for Experienced Users.......................

Operating Instructions: Complete and Thorough Illustrated Instructions...............

I. Preliminary Checks..................................................................................

II. Setting up the Diffractometer................................................................

IV. Turning on the X-Ray Generator..........................................................

V. Using the Data Collection Software.......................................................

  • Creating a New Data Collection Program.......................................

  • Editing a Previous Data Collection Program..................................

  • If the Software Stops Communicating with the Diffractometer.....

VI. When Your Run is Finished..................................................................

Appendix A. Selecting Slits for your Experiment...................................................

Appendix B. Description of Scan Parameters and Data Collection Strategies.......

  • Scan Job Parameters....................................................................................

  • Additional Information about using the Task List in DataScan..................

  • Some Data Collection Strategies.................................................................

pg 3-4

pg 5-14

pg 6

pg 7

pg 8-9

pg 10-14

pg 11

pg 13

pg 14

pg 15

pg 16-18

pg 19-23

pg 19-21

pg 21-22

pg 22-23

ru300 overview copy

Operating Instructions: Abridged Checklist for Experienced Users

More detailed instructions start on page 5; if you are unsure about the proper way to do something, consult those instructions or ask SEF staff (Scott Speakman) for help


  1. Engage Coral to start Logging Time




  1. Assess the Instrument Status and Safety

    1. Is the Generator on?

    2. Is the Shutter open?

    3. If the generator is OFF, go to step 3.

    4. If the generator is ON and the shutter is closed, go to step 2.



REMEMBER:

  • The shutter has a pair of “Shutter Open” Warning Lights.




  • Never open the doors while the Generator is ON.



If the generator is ON, then turn it OFF

    1. Check that no scan is running and that the shutter is closed.

    2. Slowly turn down the current (mA)

    3. Slowly turn down the voltage (kV)

    4. Press the red OFF button on the generator control panel.




  1. Set up the Diffractometer

    1. Check the slits (DS, SS, RS, and RSM)

    2. Insert the sample and place the sample chamber cap above the sample holder.

    3. Close the Enclosure Doors




  1. Turn On the X-Ray Generator

  1. Press the white T-REV button.

  • The amber READY light on the generator control panel should light up brightly

  • If the READY light does not light up, or lights up only dimly, then check:

  • that all enclosure doors are properly closed.

  • that the voltage and current dials are turned fully counterclockwise to their minimum positions.

  • If correcting these does not cause the amber ready light to light up, contact Scott immediately.

  1. Press the white ON button.

  • If the CW light in the Alarm section illuminates, then:

  • Press the RESET button

  • Start over with step a

  • If any other alarm light is lit, do not attempt to operate the instrument- contact Scott

  1. Wait for the voltage (kV) meter to settle at 10kV and the current (mA) meter to settle at 20mA.

  2. Turn up the generator power.

    1. Use only the coarse adjust dials for kV and mA.

    2. First turn up the kV slowly to 50 kV, waiting for the gauge to settle between each detent.

    3. Then turn up the mA slowly to 200 mA, pausing between each detent (i.e. click).
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