Tube Change for PANalytical X-Pert Pro How to change x-ray tube for PANalytical X-Pert Pro in CSL 1011 @ Florida State

University

Dr Thayumanasamy Somasundaram, Senior Research Associate

Florida State University— 91 Chieftan Way, Tallahassee, FL 32306-4380

T: 1-850-644-6448 | E: tsomasundaram@fsu.edu

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Summary This procedure is for changing the fixed-anode copper tube (either in line-or point-focus) to molybdenum (line- of point-focus). This procedure is usually done when one wants to use different monochromatic wavelength for the powder diffaction work. Molybdenum (Mo)has a shorter Kalpha wavelenght 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)

CONTENTS

Summary 2

Lab notes for Copper to Molybdenum tube change for PANalytical X-Pert Pro Powder 3

Materials needed before starting the procedure 3

At the computer 3

At the back of the instrument 4

At the back panel of the instrument 5

At the tube 5

Putting it back together 7

Testing with Silicon 8

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

[Trainer: Katherine Macchiarola, PANalytical, Raw notes are at end of this document [Raw notes1 and RawNotes2]

Materials needed before starting the procedure

SHALLOW PANE TO CATCH WATER (1-2 INCHES DEEP AND ABOUT ~9”X12” OR EQUIVALENT) PAPER TOWELS T27 SCREW DRIVER T25 SCREW DRIVER T20 SCREW DRIVER SMALL AND MEDIUM SIZE ADJUSTABLE SPANNERS SPANNERS PHILIPS SCREW DRIVER BIG

At the computer

• Username: User-1 {note the “U” in User-1 is capital letter} • Password: xxxxxxxxx • Start Data Collector (by default it should be running) program [Start >All

Programs>PANanalytical Data Collector > Data Collector]

PANalytical Data Collector Program Graphical User Interface (GUI)

• In Data Collector Go to Instrument Setting tab o Under X-ray sub tab look for X-ray tube: Empyrean Cu LFF HR (9430 033 7310x) and

click it o A new window “Instrument Settings” will open o In that window go to X-ray sub tab

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Set 2-theta to 90.0° Set Omega off-set to 45.0° This will automatically set Omega to 90° Hit apply Wait for the instrument to get this position

XPert Pro in position for tube change Instrument Settings Window

• X-Ray Tube Copper Empyrean System o Open Drop-down menu and select “Molybdenum” o Hit Apply o This will bring the “Tube Change Wizard

• Follow the wizard o We ignored the dialog box about Remove all the PreFIX components [this is dependent

on what PreFIX modules are installed; we have X-Caliber] 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 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]

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At the back panel of the instrument

o Open the back-door which has a micro switch using T27 screw driver (supplied with the instrument)

At the tube

Tube Housing and tube back side

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o At the back of the tube there are four screws. Loosen them slightly using T25 screw driver (supplied with the instrument)

o Gently wiggle the collar (ring with knurled pattern) 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 Collar (knurled ring)

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 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

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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

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• 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

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Standard Silicon disc run

SummaryLab notes for Copper to Molybdenum tube change for PANalytical X-Pert Pro PowderMaterials needed before starting the procedureAt the computerAt the back of the instrumentAt the back panel of the instrumentAt the tubePutting it back togetherTesting with Silicon