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X-Ray Fluorescence (XRF)
Standard Operating Procedure
INSTRUMENT:
Shimadzu EDX-720 X-Ray Fluorescence
----------------------------------------------------------------------------------------------------------------------------- This procedure assumes the instrument is off and the software is closed. If this is not
the case, see the alternate start-up procedures on page 6
------------------------------------------------------------------------------------------------------------------------------FILL THE XRF WITH LIQUID NITROGEN:
A. Fill the large white 10L dewar located in the gas storage room
1. Put on the gloves found in the gas storage room
2. Take off the cap to the white 10 L dewar
3. Take the rubber hose attached to the liquid nitrogen tank and place the hose into the
dewar approximately 2 inches
4. Holding the hose, open the liquid nitrogen valve half way until white gas starts
pouring out
5. When the rubber hose hardens, you can stop holding the hose
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6. Open the valve the rest of the way until you see liquid pouring into the dewar
7. Shut off the valve when the dewar is full
8. Place the cap back on the 10 L dewar (DO NOT FORCE THE CAP DOWN YOU WILL
BREAK THE CAP!)
9. Transfer the liquid nitrogen from the 10 L dewar into a 1 L dewar
Pour from the 5 L or 10 L Dewar
into a 1L or 500 mL Dewar
10. Log the approximate amount of liquid nitrogen used – the sheet is located on the
liquid nitrogen tank in the gas storage room
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B. Fill the detector with liquid nitrogen
1. The dewar is located under the hinged door at the back
of the instrument. The door is held on by only the two
hinges, so take care not to put weight on it when open.
2. Pull out the inner dewar cover, keeping the plastic collar
in place, add liquid nitrogen until filled.
3. It will take 15-20 minutes for the detector to reach its
operating temperature. Safety interlocks should
prevent high voltage from being applied to the detector
if it is not at the correct temperature.
C. Turn on the instrument
1. The on/off switch is located on the right side of the instrument
2. The instrument should be turned on first and the computer second, if it is also off.
3. After the instrument is on, please allow 5-15 minutes for the XRF to stabilize before
starting the software and initializing the instrument.
D. Open the software and initialize the instrument
1. Open the software from the PCEDX icon located on the desktop. The main toolbar
and Analysis windows will open
2. A pop-up window will appear indicating the instrument needs to be initialized. Click
OK.
3. After a short self-test, another pop-up window will appear requesting the X-Ray
power be turned on. Click OK. This will power up the X-Ray tube while the shutter
remains closed.
4. After the tube has been turned on, wait 30 minutes before using the instrument.
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CALLIBRATE THE DETECTOR:
A. Close the Analysis window
B. Click on the Maintenance icon from the main tool bar
C. Click on Instrument Calibration…
D. Locate the A750 Standard located in Drawer 63
E. Place the A750 Standard over the hole in the back of the instrument’s
stage. If the door is closed, press and hold Open until the door opens
all the way. Place the standard right side up with the A750 label
facing outward. It was recommended that the standard be placed in
the instrument the same way each time a calibration is done.
F. In the now open calibration window, select Yes for the Energy/FWHM Calibration and
then click Start. The door should close automatically after which the calibration starts.
The progress of the calibration will be indicated by the status bar at the bottom of the
Instrument Calibration window.
G. The calibration took 5-7 minutes to complete when done once every week. This time
will increase if there is a longer times between calibrations. If the instrument cannot
complete the calibration, Shimadzu should be contacted.
H. When the process is complete, the door opens. Close the Instrument Calibration
window and the Maintenance window.
------------------------------------------------------------------------------------------------------------------------------ANALYZE THE STANDARD TO CHECK THE CALIBRATION:
A. Click the Analysis icon. In this window, click Analytical Group
B. In the Select Analytical Group window, select System Group and the Owner of
Analytical Group
C. Select the Group Name easy and click OK
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D. In the Analysis window click Start. If the door does not close itself, press and hold the
Close button on the front of the instrument until it seals completely.
E. The analysis should take 3-5 minutes to complete. When complete, a Result Display
window will appear. The qualitative and quantitative results and the spectrum can be
printed and compared to the last analysis of the standard.
1. Please note that the line assigned to the Cu Ka transition should be at an energy of
8.04 +/- 0.04 KeV. This can be checked under the Peak List given in the Qualitative
Result portion of the display.
F. The standard can now be removed from the instrument.
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RUNNING AN EXPERIMENT:
A. Make sure you load the sample properly.
1. Solids need no sample preparation
2. Powders and liquids must be placed in a sample cup. Instructions can be found in
the XRF’s operator manual
B. Select the Group Name easy and click OK
C. In the Analysis window click Start. If the door does not close itself, press and hold the
Close button on the front of the instrument until it seals completely.
D. The analysis should take 3-5 minutes to complete. When complete, a Result Display
window will appear.
------------------------------------------------------------------------------------------------------------------------------INSTRUMENT SHUT-DOWN:
A. Turn off the X-Ray Tube
1. Close the Analysis window
2. Open the Maintenance window
3. Click Instrument Setup…
4. Under Shutdown, select X-Ray Power Off and click Execute Shutdown. This turns
the X-Ray tube off, but leaves the power to the detector on.
B. Wait 30 minutes after turning off the X-Ray tube before turning the instrument off.
This allows time for the fans to run and cool the X-Ray tube.
C. Close the software
------------------------------------------------------------------------------------------------------------------------------ALTERNATIVE START-UP PROCEDURE:
A. Check to make sure the detector is filled with liquid nitrogen.
1. If the instrument is not at the correct operating temperature, an error message will
appear on the screen.
2. Follow the procedure starting on page 1
B. If the instrument is on, but the software is closed:
1. Click on the PCEDX icon
2. The Start Up Status pop-up window will appear prompting you to Please Turn On XRay Power. Click OK.
3. Wait 30 minutes to the X-Ray tube to warm up before using the instrument
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C. If the instrument is on and the software is open, but the X-Ray tube is off:
1. Make sure the Analysis Window is closed
2. Click the Maintenance icon
3. Click Instrument Setup…
4. Click Execute Startup at the bottom of the window
5. Wait 30 minutes for the X-Ray tube to warm up before using the instrument.
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