Panalytical XPert Powder X-Ray Diffraction SOP

Table of Contents

1.0 Safety

2.0 Training

3.0 Sample Preparation

4.0 Pre-Operation

5.0 Sample Loading

6.0 Running a Measurement

7.0 To Stop a Scan in Progress

8.0 Sample Unloading

9.0 Post-Operation

10.0 Converting Data

1.0 Safety

1.1 High Voltage This machine uses high voltages, especially to generate

the X-ray beam. Do not touch any parts of the machine aside from those

specifically mentioned in this SOP.

1.2 X-rays X-rays are a very harmful form of radiation and care should be

taken to minimize exposure. The radiation material MUST be reviewed

prior to training or use of this machine. Additionally, all users MUST have

obtained their X-ray badge prior to use or training on this machine. Your

X-ray badge MUST be worn at all times during operation and only those

wearing X-ray badges should be permitted in the room.

1.3 Moving Components This machine has heavy moving parts. Although

these parts only move inside the machine while the X-ray is on (and thus

ould be taken to ensure you do

not get in the way of a moving part.

CAUTION

CAUTION The detector can burn out if a measurement sweeps across a single

crystal peak. If your measurement burns out the detector, your

PI/advisor will be charged for the repair

CAUTION

CAUTION

Some signal may come from this dummy sample, so

ensure that it is not single crystal as well.

2.0 Training

2.1 Training for this machine is scheduled on demand. Please use the RSC

website to request training if you would like to use the machine.

2.2 Prior to training, users MUST review safety information about X-rays and

obtain an X-ray dosimetry badge. The training slides are available when

you sign up for training and the dosimetry (X-ray) badge application is

available in the Docs section of the RSC website.

3.0 Sample Preparation

3.1 This tool can only measure polycrystalline materials

3.2 Samples should be loaded on a glass (not quartz) slide

3.2.1 The glass slide will not introduce too much additional signal

3.3 If measuring a powder, use double-sided tape to create a thin layer of

powder in the middle of your glass slide

3.4 If measuring a sample, the sample can sit directly on the glass slide (no

need for tape as it will not move)

3.5 We have aluminum holders you may also use, these are to remain in the lab, and should be cleaned after each use. Please ask for assistance if you need to use the aluminum holders.

3.6 The sample needs to be height-matched when loaded so that the top of

the sample is at the focal point of the X-ray beam

3.6.1 For powder samples, a section of single-sided tape on the loading

end is sufficient

3.6.2 For larger samples, an additional dummy sample of similar height

will need to be loaded into the clip.

4.0 Pre-Operation

4.1 Ensure you have a reservation or that no one will have a reservation

during your time.

4.2 Ensure that the angles displayed on the front of the machine are the

proper

Angle displays on the front of the machine.

4.3 Ensure that the system is at standby power by checking the voltage and

current on the front of the tool

Standby Power Full Power

Voltage 45kV 45kV

Current 20mA 40mA

4.3.1 X-ray source voltage should be 45kV

4.3.1.1 If the voltage is not 45kV, do not use the tool. Please

send an email to rscinfo@mail.ufl.edu

4.3.2 X-ray source current should be 20mA (standby current)

4.3.2.1 If the current is higher than 40mA or lower than

20mA, do not use the tool. Please send an email to

rscinfo@mail.ufl.edu

4.3.2.2 If the current is between 20mA and 40mA, the

machine can still be used, but please send an email to

rscinfo@mail.ufl.edu with the time, date, and details

4.3.3 If you are using the machine IMMEDIATELY after another user,

they may leave the system at full power for you. Otherwise, the

machine must be brought to standby power after measurements

are finished.

Indicator on the front of the machine showing the source voltage and current at standby power.

4.4 Log in to the TUMI system at the laptop computer

4.5 The Data Collector software should be left running. If it is not, follow

these steps to get it running

4.5.1

Data Collector and Viewer programs in the Windows bar.

4.5.2 Login with the username and password posted on the PC

4.5.2.1 Username: class

4.5.2.2 Password: class1

4.5.3 Select Instrument -> Connect

4.5.4

4.5.5 Same config

4.5.6

4.6 Once the software is running, raise the system power to full (40mA)

4.6.1 Double click the current in the left window

4.6.2 Increase the Current by 5mA and select “Apply”

4.6.3 Double check on the front of the machine that

the current was raised

4.6.4 Let the Machine saturate at this level for 30-45 seconds.

4.6.5 Repeat until you reach 40mA (full power) Select “OK” to close Instrument settings window.

4.6.6 Double check on the front of the machine that the current was

raised to 40mA

Raise the current to 40mA in 5mA intervals

The machine should now read full power.

5.0 Sample Loading

5.1 Before opening the door, ensure that the X-ray is blocked

5.1.1 The doors should be locked if the X-ray is not blocked, but use the

indicator on the front of the tool to be sure

The shutter is closed

The X-ray is blocked

Safe to open

The shutter is open

The X-ray is NOT blocked

NOT safe to open

5.1.2 Open the doors by sliding each outward

5.1.2.1 The doors are heavy, so do this slowly and carefully

5.1.3 Insert your sample into the spring-loaded clip

Picture of a loaded sample Diagram of loading a larger sample

5.1.4 Close the doors slowly and ensure they are completely closed

CAUTION CAUTION

Start angles smaller than 5 degrees will cause the X-ray beam

to shine directly into the detector and burn it out

CAUTION CAUTION

End angles larger than 140 degrees can cause the source

and the detector to collide during the measurement

6.0 Running a Measurement

6.1 To edit your scan parameters, select File -> Open Program

6.2 Select the program you wish to use:

Powder Th-2Th Basic Scan- This is the basic scan type

(previously “use this program”) It works best for infinitely thick

samples, or phase ID scans of any thickness.

Powder Th-2Th fixed -10mm- This scan is a basic powder scan

utilizing the programmable slits to maintain a 10mm irradiated

length on your sample. This can correct for the constant volume

assumption and allow refinements to be used. (Quantitative)

Powder Th-2Th fixed- 5mm- Same as 10mm program, just

shorter irradiated length on sample.

Thin Film 2Th-omega scan- This program runs a 2Theta-omega

scan (powder scan) with an omega offset, and a constant

irradiated length of 6mm on your sample. This can help scan

polycrystalline thin films on a single crystal substrate.

6.2.1.1 Select Open to open the window to edit the program parameters. For the Powder scans edit the 4 white boxes:

• Start angle, end angle, step size, and time per step.

6.3 Select the Repetition tab and ensure that the repetition is set to single

6.3.1 Ensure the scan is set to Continuous

6.3.2 The start angle MUST be larger than 5 degrees

6.3.3 The max angle MUST be less than 140 degrees

6.3.4 The step size will determine the resolution of your scan. Higher

resolution will increase the scan quality but take longer to run. The

following step sizes are offered as suggestions

6.3.4.1 0.033 will run a quick scan (searching for peaks)

6.3.4.2 0.016 will run a regular scan (general comparison)

6.3.4.3 0.008 will run a high resolution scan (publication quality)

6.3.4.4 0.002 is our max resolution with the X’Pert Powder

6.3.5 The time per step will determine how long the software integrates at

each step. Larger values will reduce noise but will take longer to

scan.

6.3.5.1 increase as needed

6.3.5.2 Your main peak should be in the:

• 1000s of counts for peak ID

• 10,000s of counts for quantification

• 100,000s of counts for structure determination

6.3.6 Leave all other parameters the same

Editing the scan parameters.

6.4 Click the close button (red X in the top right of the window) and select

save changes

6.5 To run the program, select Measure -> Program

6.5.1 Select the same program you just saved

6.5.2 This will open the measurement window

6.6 Select the large folder icon to choose where to save your scan data

6.6.1 Data should be stored in the XRD User Data library in a folder with

your name

You should only need to adjust these 4 boxes before saving the program

Your approximate scan time is shown here

6.6.2 The folders and subfolders in your named directory can be

whatever you like

Measurement window.

Store all measurements in your folder in the XRD User Data library.

6.7 Before beginning the run, ensure the machine doors are completely

closed

6.8 Select OK to begin the scan

6.8.1 The tool will lock the doors. DO NOT attempt to open the doors.

6.8.2 The scan will run autonomously at this point. A graph will pop up

and plot data as it comes in. There is no alert when the scan

finishes. When all data is compiled, the machine will return the X-

ray source back to the start angle and unlock the doors.

6.8.3 Once the doors are unlocked, you may proceed

7.0 To stop a scan in progress

7.1 You can pause or stop a scan during data collection:

7.2 Right-click within the scan display window

• Select Hold or Stop

7.3 Or you can go to the top menu bar and click on the or icons..

7.4 The diffractometer will stop at its current position and give you an Options

dialogue.

7.5 The shutter will remain open until you choose an option

7.6 You can choose to

• Abort the scan

• Data will be saved up to the point where you

aborted the scan

• The diffractometer will move to its ‘park’ position

and the shutter will close

• Continue the scan

• The scan will resume from the point where you

paused it

• The system will wait as long as you want it to until

you choose to continue

8.0 Sample Unloading

8.0 Once the doors are unlocked (there will be a loud click), you should be

safe to open the door. However, ensure the X-ray is blocked with the

indicator on the front of the machine.

8.1 If the X-ray is blocked (shutter is closed), open the doors slowly to retrieve

your sample.

8.2 If you are running additional samples, you may load them at this point,

close the doors, and run more measurements

8.3 If you are finished with all your scans, remove all samples and

loading/buffer slides from the machine and close the machine doors

9.0 Post-Operation

9.1 When finished with the machine, you will need to return it to standby

power

8.1.1 If someone is going to use the machine immediately after you and

power

9.2 Double click the current in the left window

9.3

9.4 Repeat until you reach 20mA (standby power)

9.5 Close all open windows in the Data Collector program, BUT DO NOT

CLOSE THE DATA COLLECTOR PROGRAM ITSELF

10.0 Converting Data

10.1 The tool stores data in its own proprietary format, which will include the

scan parameters, which can be directly imported to the JCPDS computer.

If you want an XY text file of data, use the following steps

10.2

Data Collector and Viewer programs in the Windows bar.

10.3 In the window that opens, select File -> Open

10.4 Navigate to Libraries -> XRD User Data -> [your name] and select all

)

.4.1 Each scan will open its own window and an additional window will

open with all scans plotted on top of each other

10.5 Select File -> Convert All

.5.1 This process is quick, and the program does not acknowledge

when it is finished

.5.2 Your XY files will be in the same folder as the original scans

Data Collector and Viewer programs in the Windows bar.

10.6 Close the data viewer program

10.7 Transfer your data files to a flash drive, you may leave data on this machine, but it is periodically cleaned, and we are not responsible for lost data.

10.8 You may transfer data to the JCPDS machine (will need a USB) to use HighScore Plus and the ICDD database to process your collected data.

10.9 At this point, you can log off at the TUMI computer