tube change for panalytical x-pert...

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

http://www.biophysics.fsu.edu/soma

mailto:[email protected]

X-Ray Tube Change Procedure for PANalytical X-Pert Pro | 2

;© 2013-16 Thayumanasamy Somasundaram

CONTENTS

Summary 3

Molybdenum to Copper tube change for PANalytical X-Pert Pro Powder 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

http://www.sb.fsu.edu/soma

http://www.sb.fsu.edu/soma



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

• 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.



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



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.



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.

• 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)

• 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



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.

XPert Pro in position for tube change Instrument Settings Window

• 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



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}



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 View of tube housing from the back side



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)



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



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

• 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



Tube and housing and Line Focus

• 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



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 2-theta 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.



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.



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

mailto:[email protected]

http://www.biophysics.fsu.edu/soma

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