PANalytical X-Ray Diffractometer Standard Operating Procedure

Version 21 (May 2012)


Training Rules:

First time: watch trainer and take notes

Second time: do by yourself with supervision following your notes

Third time: do by yourself with supervision without help (Dr. Bykov must approve the authorization for independent use)

After the third time, you are completely independent and responsible for the instrument.

Operating Rules:

1. Only authorized people can use XRD.

2. You must sign up for time on the XRD using the online system through Forum:

http://134.74.50.69/ccnycores/main.php

3. All samples must be recorded in XRD logbook including the date, time, user, powder, sample name, program name, and filename.

4. Please DO NOT troubleshoot by yourself.

Call: Alexey Bykov

212-650-5548 (Laboratory) or 646-725-0270 (cell phone)

Outline:

1. To turn on the instrument

2. Tube breeding

3. To make a new program

4. Typical Operation with fixed holder

5. Typical Operation with spinner holder

6. To export data

7. To turn off the instrument

Appendix

1.  Slit selection

2.  PDF4+ database

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1.  Turn on the Instrument:

1.1  Press power switch on the water recirculator to turn on cooling water. (Make sure pump selection switch is switched to right side.) Cooling water valves on the wall must be always on.

1.2  Double click on X’Pert Data Collector icon on the desktop.

If the program is already ON, but the generator status is OFF (Tension = 0 kV and Current = 0 mA) skip steps 1.2-1.5 and go to step 1.6. If the program is ON and the generator status is also ON (Tension > 20 kV, Current > 5 mA) go to step 2.3.

1.3  Type user name: User-1 and password: galaxy in Login dialogue box.

1.4  Go to Instrument menu and click Connect.

1.5  Select Stage Flat Sample for regular measurements or Sample Spinner if you need to rotate your sample during scanning procedure. (To switch sample holders go to Tools menu à Exchange Sample Stage with following connection procedure (Instrument menu and Connect ).

1.6 
Double click on X-ray . Check the Generator on box at the Instrument Setting press Apply , and wait until energy goes up to 30 kV and 10 mA .

2.  Tube Breeding

If X-rays have been turned off for an extended period of time, tube breeding is necessary. Check the log book first to see when last time the instrument used was. Breed at normal speed if the instrument was left idle for 100 hours or more (breed takes about 30 minutes). Breed at fast speed if the instrument was used recently (within the last 100 hours). In this case, tube breeding takes about 6 min.

2.1  Click Breed . Choose fast or normal in Tube Breeding box OK

2.2  Tension during breeding procedure goes up to 60 kV then down to 40 kV. After breeding the parameters of the generator will be 40 kV and 10 mA

2.3  On the Instrument Settings window set measurement parameters (usually 40 kV and 40 mA). Click Apply, click OK.

3.  To Make a New Program:

3.1

Go to File menu and click New program. The New Program window will appear.

Click OK for Absolute scan program type.

If you have already saved program in previous sessions use Open Program in File menu and edit your program for current measurements.

3.2 Choose your scanning parameters on the Prepare absolute scan window.

-  In configuration, select stage flat samples (for fixed holder) or sample spinner Reflection-Transmission (for spinner holder).

-  In Scan Axis, select the type you want, a typical scan for powders is Gonio.

-  Click Scan properties tab to edit the scanning parameters: Continuous scan is typical for regular powder diffraction measurements, set your angle range, step size, time per step (or scan speed).

-  Click on Repetition, select then Single scan or other scan type.

-  Go to main menu, select File, click save as, use your first name (Ex: ChunMin) and then click OK .

For previous saved program with XRD already on you may start here

If you use spinner sample holder, skip 4 “Typical Operation with fixed holder” then go to “5 “Typical Operation with spinner holder”

4.  Typical Operation with Fixed Holder

4.1.  Load XRD sample slides on the fixed sample holder.

4.2.  Go to main menu, click File, choose Open program and check if the program settings are appropriate.

4.3.  Go to main menu, Select Measure and click on Program, click OK after you choose your program.

4.4.  Click the folder icon on the right (If you are a new user please create a folder under your group folder)

4.5.  Type in the file name for example: ChunMin5_

4.6. 

Click OK on the Start window. Absolute scan window will appear with scanning curve.




5.  Typical Operation with Spinner Holder

5.1. To switch sample holders you should first disconnect XRD Instrument – Disconnect, then go to Tools menu à Exchange Sample Stage , choose Reflection Transmission Spinner at Change Sample Stage window, press Apply. Follow the instructions of the X’Pert Wizard.

The Fixed Stage is mounted to the base by four screws. Unscrew all of them and carefully remove the stage. Take the Spinner Holder and attach to the base. Mount the holder using three screws only.




Then connect the instrument (Instrument menu and Connect ). Sample stage Reflection Transmission appears in the instrument setting window

The instrument is ready for measurements.

5.2. To load your sample you should bring the holder in lower position. Click Sample Stage tab Uncheck Lift Up and click Apply





Load the sample as shown below.


After loading the sample check Lift Up and click OK . The sample will move up to the measurement position.


5.3. Go to the File menu then choose Open program. The program settings are appropriate to sample spinner Reflection-Transmission mode ( Configuration – Sample Spinner Reflection.., Scan Axis – Gonio. Set spinning parameters (Revolution time (sec)) in the Setting window. Click Apply. Start scanning.


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5  To export data:

1.  On the desktop, double click on X’pert High Score Plus , click OK.

2.  Go to File menu then Open select the file from your folder.

3.  In the List Panel, select Anchor Scan Data tab, move mouse to the excel chart and right click. To get XY data, select Save list as , and name your file. Make sure saving the data as a .txt format file.

4.  To export data in different format, go to File menu and select Save As and select the desired data format, such as: RD, UDF, DAT…etc.

Data saved in C:\X’Pert Data\ automatically after running instrument

6  To Turn off the Instrument:

1.  To shut off instrument, double click Tension in

Sample Spinners Stage Reflection-Transmission window on left side change energy back to 30 kV and 10 mA in Instrument Settings box. Click Apply then wait for ~1 min.

2.  Uncheck the Generator box on box then click OK. Do not turn off the key.

3.  Turn off the cooling water switch on chiller (recirculator).

Do not close the software program

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Appendix.

1. Slit selection

For general scanning:

Incident beam (left) Detector (right)

Fixed Divergence slit (FDS) / Beam mask / Anti-scattering slit (A-S slit) / Filter / Receiving slit
1/2° / 10 mm / 1/2° / Ni / 1/4°

For low angle scanning:

1/4° / 10 mm / 1/4° / Ni / 1/32°

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1.  PDF4+ (ICDD DD view software) XRD database

2.  Double click PDF4+ 2008 icon on desktop

3.  Click Periodic Table tab in the Search window

4.  Select the corresponding elements in the table (Ex: Zn and O)

5.  Check Only box and press Add

6.  Click Search