Rigaku MiniFlex 600 X-ray Diffractometer

Standard Operating Procedures (SOP)

Version: 07/21/2016
By: Mike Manno

Figure 1 (a) External and (b) internal component overview of the Rigaku MiniFlex 600
X-ray Diffractometer.
Safety Note

This instrument is designed to create high energy x-rays which will scatter off a desired sample
for diffraction analysis. These x-rays can be hazardous to your health if exposed to them. It is
important to recognize all the safety features that the instrument has as well as the safety
protocols that must be followed. This will ensure the safe operation of the equipment.

Instrument Safety Features

 Fully enclosed goniometer system which is surrounded by a steel casing.

 Automatic x-ray source shutter system tied to safety circuit. The shutter light will turn red
when the shutter is open. However the enclosure hides this light.
 The shutter system has switch-based sensors to recognize when the shutter is open and
closed. If the shutter gets stuck the generator will turn itself off.
 X-ray generation light at top of instrument. This light comes on when x-rays are being
generated in the source. This does not imply that x-rays are interacting with the sample.
 Door locking system that is tied to the safety circuit. The x-ray shutter will only open
when the door is locked and the door button is pressed. Pressing the door button when the
shutter is open will close the shutter and then unlock the door.

Safety Protocols

 User loading a sample must wear a safety ring. DO NOT TAKE THE RING OUT OF
THE ROOM.
 Lead the safety badge next to the diffractometer. DO NOT TAKE THE BADGE OUT
OF THE ROOM.
Instrument Start-up

1) Log onto the computer using the local user account labeled on the front of the computer.
2) Start the program MiniFlex Guidance, which can be found on the desktop of the computer.
a) Login name: Administrator
b) Password:
i) Do not type anything!
3) Wait until the start-up procedure finishes.

Initializing the Goniometer

1) Select the Control tab, Initialize Individual Axis. A pop-up window will appear.
2) Select Theta / 2-Theta and press the Execute button.
3) Press OK on the confirmation pop-up window.
4) Wait until the Hardware Control pop-up disappears.
5) Then hit the Close Button on the Initialize Individual Axis pop-up window.

Powering up the X-ray Generator

1) Select the Control tab, XG Control

2) A pop-up window will appear. Set the Voltage field to 40 kV and set the Current field
to 15 mA.
3) Press the Set button.
4) Wait until the Hardware Control pop-up window disappears.
5) Press the Close button on the XG Control pop-up window.

Checking Instrument Status Before Measurement

1) In the lower left region of the main screen make sure that these settings are kept:
a) Water flow: Between 4.0 – 5.0 L/min
b) Tube voltage: 40 kV
c) Tube current: 15 mA
2) If any of these values are not correct, make sure to contact the TA.
Sample Measurement

Note: This section assumes that you know how to properly prepare a sample in an appropriate
holder. Contact the TA or instructor if you have any questions about this before continuing.

1) Press the Door Lock button on the front of the diffractometer.

2) The Door Lock button light will turn on until the door is successfully unlocked, then it will
start to flash and an audible alarm will start to sound.
3) Open the door.
4) Load the sample straight into the center clip point. The thin end of the holder will slip into
place. Try to keep the sample centered into the holder and onto the mount.
5) Close the door.
6) Press the Door Lock button again. The button will stop blinking, the audible alarm will turn
off, and the door will lock again.
7) Go to the upper left window of the instrument software and left click on General
Measurement.
8) A yellow field with the text 1 General Measurement will appear in the window below (See
Figure 2). Make sure the pop-up window has the following information entered:
a) For row No. 1, make sure a check mark is entered in the Exec. Field.
b) Click on the “…” button (between file name and sample name) to select a folder location
and file name for the measurement results. Data should be saved in the folder:
C:\Windmax\Data\.
c) Enter a sample name in the Sample name field. This is additional information that is not
required, but helps keep track of the runs.
9) Click on the Set Meas. Conditions… button. A new pop-up window will appear
(See Figure 3).
10) Make sure that the fields in Slit condition and Optical devices match the current
configuration of the instrument. The instrument is typically set to the following conditions
listed in Table I, but confirm this prior to your measurement:

Table I Typical Configuration of X-ray Diffractometer

Soller(inc): 5o Soller(rec.): 5o
IHS: 10 mm RS: 0.3 mm
DS: 0.625o Monochromation: Monochromator
Variable & Fixed
SS: 1.250o Slit Condition
slit
11) Under Measurement condition enter the following values:
a) Scan axis Theta / 2-Theta
b) Mode: Step
c) Start (deg): Enter your starting angle
d) Stop (deg): Enter your stopping angle
e) Step (deg): Enter your step size
f) Duration(sec): Enter your dwell time here
g) Voltage (kV): 40
h) Current (mA): 15
12) After everything has been selected press the OK button to get back to the General
Measurement pop-up window (i.e., Figure 2).
13) To run a measurement, press the Run button at the lower left corner of the pop-up window. A
new pop-up window will appear, and the measured data will appear in the main window of
the program.
14) The data will be saved in folder path provided previously. The raw data will be saved in two
file formats, a .ras format (a Rigaku proprietary format) and a .raw format. You need to use
JADE to convert the .raw format to a .xy file if you wish to use another program to plot the
data.

Instrument Shutdown

1) Remove the sample in a similar method to loading a sample.

2) Now power down the X-ray tube to standby power
a) Select the Control tab, XG Control
b) A pop-up window will appear. Set the Voltage field to 20 kV and set the
Current field to 2 mA.
c) Press the Set button.
d) Wait until the Hardware Control pop-up window disappears.
e) Press the Close button on the XG Control pop-up window.
3) Close down the collection software and log off the computer.
Figure 2 General Measurement pop-up window

Figure 3 Measurement Condition popup window