X-Ray Tube Change Procedure for PANalytical X-Pert Pro
How to change x-ray tube for PANalytical X-Pert Pro in CSL 1011 @ Florida State
University
2014-16 Dr Thayumanasamy Somasundaram, Senior Research Associate
Florida State University— 91 Chieftan Way, Tallahassee, FL 32306-4380
T: 1-850-644-6448 | E: [email protected]
Updated: February 03, 2016
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 2
CONTENTS
Summary
Molybdenum to Copper tube change for PANalytical X-Pert Pro Powder
3
3
Materials needed before starting the procedure
3
At the computer
3
Incident Beam and Diffracted Beam PreFIX
4
PreFIX Removal
5
Tube movement
6
At the back of the instrument
8
At the back panel of the instrument
9
At the Tube Housing
10
Putting it back together
12
Testing with Silicon
14
Version: 20160203 | Copyright © 2012-16 Thayumanasamy Somasundaram
Version: 20160203; Original version: 20151201
Author: Thayumanasamy Somasundaram
Institute of Molecular Biophysics | Florida State University | Tallahassee, FL 32306-4380
Copyright © 2012-16 Thayumanasamy Somasundaram
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 3
Summary
This procedure is for changing the fixed-anode molybdenum tube in line-focus mode to fixed-anode copper
tube in line-focus mode. This procedure is usually done when one wants to use different monochromatic
wavelength for the powder diffaction work. Molybdenum (Mo) has a shorter Kalpha wavelength of 0.722 Å
(0.0722 nm; 17.15 keV) compared to Copper (Cu) which is 1.549 Å (0.0722 nm; 8.005 keV).
Molybdenum to Copper tube change for PANalytical X-Pert Pro Powder
Materials needed before starting the procedure
 SHALLOW PANE TO CATCH WATER (1-2 INCHES DEEP AND ABOUT ~9”X12” OR EQUIVALENT)
 PAPER TOWELS TO REMOVE WATER
 T27 SCREW DRIVER
 T25 SCREW DRIVER
 T20 SCREW DRIVER
 SMALL AND MEDIUM SIZE ADJUSTABLE SPANNERS
 SPANNERS
 BIG PHILIPS SCREW DRIVER
 CAN OF DRY AIR
At the computer
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Username: ZZZZZZZZ
Password: xxxxxxxxx
Before we switch the anode, it is preferable to remove the PreFIXes both on the Incident Beam and
Diffracted Beam sides.
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 4
Incident Beam and Diffracted Beam PreFIX
Incident Beam Optics PreFIX attached
Diffracted Beam Optics PreFIX attached
Both Incident Beam Optics and Diffracted Beam Optics PreFIXes attached
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 5
PreFIX Removal
Incident Beam Optics PreFIX removed
Diffracted Beam Optics PreFIX removed
Both Incident Beam Optics and Diffracted Beam Optics PreFIXes removed
Now that we have removed the PreFIXes we can proceed with removing the anode.
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 6
Tube movement
During the normal operation of the instrument the position of the X-Ray tube is very low, for example
the could be close to ω=5° or 10°. However, in order to remove the copper anode the X-Ray tube
needs to move beyond ω=90°. The following section will show how to achieve that position.
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Start Data Collector (by default it should be running) program [If not, Start >All
Programs>PANanalytical Data Collector > Data Collector]
PANalytical Data Collector Program Graphical User Interface (GUI)
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In Data Collector GUI, Go to Instrument Setting tab
o Under X-ray sub-tab click on X-ray tube: Empyrean Mo LFF HR DK378018
o A new window “Instrument Settings” will open
o In that window go to Position sub-tab
o Enter 90.0° in the 2-theta box (originally it will read 40.957°)
o Set Omega off-set to 45.0°
o This will automatically set Omega to 90°
o Enter 0.0° for Phi
o Hit apply
o Wait for the instrument to get this position
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 7
Original setting
After setting 2-Theta and Omega offset
Position sub-sub-tab on Instrument Settings sub-tab on X-Ray tab
Once 2-Theta=90° and Omega=90° is achieved the X-Ray Tube will look like the following image.
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XPert Pro in position for tube change
X-Ray Tube Copper Empyrean System
o Open Drop-down menu and select “Copper”
o Hit Apply
o This will bring the “Tube Change Wizard
Follow the wizard
;© 2013-16 Thayumanasamy Somasundaram
Instrument Settings Window
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 8
Selecting to change to Copper anode
Tube Change Wizard Starts
• Follow the wizard:
o The dialog box reminds you to remove all the PreFIX components [this is dependent on
what PreFIX modules are installed; we have X-Caliber]
o It will remind you to close the door
o The wizard moved the 2theta to 110° and theta to 110.0° automatically
o The wizard brought the voltage back to zero and zero
o The wizard will remind you to switch the HT key to off position
o We switched off the HT key to off position
At the back of the instrument
•
We walked to the back of the instrument
o We turned the water circulation off [at the back right hand side Haskris back panel;
Haskris was running but we closed the supply and return valves by hand]
o We turned th HT breaker switch at the back of the instrument off [back of the
instrument; mounted on the back wall; pull the handle down to off position] {may be
not needed}
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 9
Haskris Chiller Supply & Return Valves
Panalytical PXRD Main Power
At the back panel of the instrument
o Open the back-door after removing the screw w/ T27 screw driver (supplied with the
instrument; back door has a safety micro switch)
o Now you have better access to the tube housing
Undoing the screw to open back door
;© 2013-16 Thayumanasamy Somasundaram
View of tube housing from the back side
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 10
At the Tube Housing
Tube Housing and tube back side
o At the back of the tube housing there are four screws. Loosen them slightly using T25
screw driver (supplied with the instrument)
o Gently wiggle the collar (Bayonet Connector Ring, if the figure above) and remove it
o Remove the white string, High tension safety plug (unplug it)
o Remove the silver plug, Tube identification plug (unplug it)
Tube Housing
Collar (Bayonet Connector Ring removed)
o Slowly pull the tube out by pulling the HT cable assembly from the tube housing
o As you pull out notice that the POINT FOCUS will be facing you and LINE FOCUS will be
facing the floor. Make a note of it.
o NO NEED to take out fully NOW
o Put the plastic pane (for catching water) on the instrument base panel (inside the
instrument and directly below the tube)
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 11
o Hold couple of paper towels in one hand and using an adjustable spanner (or spanner
provided with the instrument) start undoing the water line using the other hand. When
you start seeing water escape [Note that even though we stopped the flow of water
earlier it will still spill] wipe it with paper towel and pull out the tube and place it the
plastic pane
o Now undo the water line completely and remove one of the hoses (can be in IN or OUT)
o Wipe it clean
o Now put the tube back again inside the housing and undo the other water hose (if you
took out IN first now it will be OUT). Again if you see water wipe it and quickly bring the
tube to the plastic pane and pull the water hose out
o One can completely remove water hoses out of the Collar (knurled ring; but remember
to put it through the collar during the installation back again)
o Place couple dry paper towels on the instrument base panel
o Now you will see four screws (2 are short and 2 are tall). I have written ”T” next to tall
ones
o Using the T20 screw driver undo the 2 short ones
o After a while you can undo the 2 tall ones
o Take all four screws are completely out
o Now wiggle the HT cable out of the tube assembly and keep it on a dry paper towels
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 12
High
tension
cable
o If the off-white part (rubber tip) of the HT cable looks dry put some P4 Silicone grease
Putting it back together
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Gently put the HT cable back inside noting that the HT cable will go one way only
(see the photo)
The brass cut-out that is holding the HT cable and has four holes for the 2-short and
2-tall screws are made in a special way
The brass cut-out will sit correctly in one way only while the screw holes are aligned
Start with 2-tall screws and once they are tight enough the HT cable will be getting
secured firmly
Now add the 2-short screws and start tightening them all
Follow the scheme North South East West
The 2-tall ones will stop tightening first
The 2-short ones will stop tightening later
Make sure the water hoses are threaded through inside of the collar (knurled ring)
and IN hose is paired with SUPPLY on the tube and OUT is paired with OUT
Tighten the screws using adjustable spanner
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 13
Tube and housing and
Line Focus
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Put the tube back inside the tube housing making sure that POINT FOCUS is facing
you and the LINE FOCUS is facing the sample (down toward the base panel)
Push on the collar (knurled ring) and click it
Now tighten the four screws using T25 gently and hand-tighten. The loosen them
1/8 turn
Put the Silver plug back in
Put the black plug with white string back in
Open the water SUPPLY and INLET and ensure no water is leaking
Close the back door
Put the screw back on the back door
Switch on HT breaker on the back wall
Follow the wizard
Run a standard sample Silicon
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 14
Testing with Silicon
Now we have to confirm whether the alignment (tube height) is good. Generally, it doesn’t
change but it is always good to check it. So run the Si standard sample from 10-100° for 12
minutes (here I have confirmed that there are 10 steps for FWHM). Then I compared the 2theta values of my (observed) values against those [reported] NIST Standard. There was a
small error: 28.527° -28.443° (84/1000th of a degree).
Standard Silicon disc with no adjustment to the tube height
So I removed the Silicon standard and put the alignment disc. I moved the 2-theta and
omega to 90.0 values as shown in the figure below.
Alignment disc in 15 sample magazine
2-Theta and Omega setting for measurement
Using the “Load from magazine position 1” mode of the Sample Changer tab, I loaded the
alignment disc and using “Shutter Open” button of the X-ray tab, I opened the x-ray shutter.
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 15
An image of the x-rays can be seen on the alignment disc once the ambient light and cabinet
lights are off.
Alignment disc in 15 sample magazine
2-Theta and Omega setting for measurement
In my case the x-ray image was between Position 1 and Position 2 indicating the tube height
was lower than ideal. So on the X-Ray Tube I rotated the top knob counter clockwise about
90° and the bottom knob clockwise about 90°. This would raise the tube.
X-rays (yellow color) between Position 1 and 2
Rotating top knob counter clock-wise
I measured the Silicon sample again and compared it with reported value. I repeated the
process until the match was less than 3/1000th of a degree. This meant, I rotated the top
knob about 2 full turns anti-clockwise and the bottom knob 2 full turns clockwise. The final
results are shown below.
;© 2013-16 Thayumanasamy Somasundaram
X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 16
Final alignment of x-rays (yellow color) falling
exactly on top of position 1
Rotating bottom knob clock-wise
Now, again I ran the Si standard sample from 10-100° for 12 minutes. Then I compared the
2-theta values of my (observed) values against those [reported] NIST Standard. There was a
very small error: 28.446° -28.443° (3/1000th of a degree).
Standard Silicon disc with no adjustment to the tube height
This completes the molybdenum to copper anode switch.
© 2013-16 Thayumanasamy Somasundaram | Kasha Laboratory
Version: 21060203
Institute of Molecular Biophysics | Florida State University, Tallahassee, FL 32306-4380
[email protected] | www.biophysics.fsu.edu/soma | 1-850-644-6448
;© 2013-16 Thayumanasamy Somasundaram