Panalytical Aeris Research XRD Tutorial

Overview:

Use our Panalytical Aeris Research XRD (X-ray diffractometer) to analyze properties such as phase composition, crystal structure, and orientation of solid samples, with precise results in less than five minutes.

Index:

Standard operating protocol - (startup, operation, shutdown)
Materials and sample prep
Detailed operating instructions
Data processing and analysis
Using HighScore Plus
Common failure modes
Manufacturer manuals
Links
Exercises

Standard operating protocol:

Instrument startup:

Make sure at least one position in the sample changer is free (no sample holder in place)
Turn the mains power switch at the rear of the instrument
Make sure that the cover is closed
Press the power button to switch on the instrument
Turn the HT keyswitch to switch on the HT generator

Operation:

Prepare your sample externally at the sample prep table
Put the sample holder in a loading position on the sample changer
Select a measurement program from the drop-down list
Put in a descriptive sample name
Start the measurement
Export results to networked workstation or USB drive
Fill out your information in the X-ray safety log book
Repeat as needed - additional samples can be loaded and added to the queue while current sample is being measured

Instrument shut down:

Press the Power button to switch off the instrument
Turn the HT Keyswitch counter-clockwise to switch off the HT generator
If the instrument will be switched off for a long period of time, you can also switch off the mains power supply

Compatible materials and sample prep:

The Aeris has a Cu Kα x-ray generator with penetration on the order of 100 µm. For powder samples, grain size should be on the order of 5-10 µm to ensure sufficient grains of various compounds contribute to the reflection of the beam. This source will cause fluorescence in samples with iron and manganese, and may not provide suitable results for samples with those elements. Panalytical provides an excellent sample preparation guide, available in paper form in the lab and here in pdf form, please refer to it for instructions on use of the different types of sample holders and associated sample prep techniques. Page 1.4 lists all the various types of sample holders that can be obtained. Of those, we have:

PW1811/00 and PW1811/27 for back or front loading of powders
PW1812/00 for odd shapes (fixed with plasticine or wax)
PW1813/26 for metal plates, membrane filters, pressed pellets, etc. XRD sample holders, mounting clay, and other small materials are stored in the black cabinet next to the sample prep table. Perform all sample loading steps at the table and transfer sample holders to the instrument on the tray once complete.

Detailed operating instructions:

Sample loading:

Remove plastic sample case cover
Place a prepared sample in any of the six positions on the sample changer
Replace plastic sample changer cover

Running a measurement program:

Choose measurement program
Enter sample ID
Edit file name as necessary
Click Add to Queue

Exporting data:

Data can be saved on a USB drive, or exported to a shared network drive on the XRD workstation to the right of the instrument. The workstation can be accessed using a common login. The username is xrd and the password is xrd-password. Data can be found in the folder C:\XRD\XRD data

export directory image — Recommended export location in Windows explorer

New measurement programs:

New measurement programs can be created using the software XRDMP Creator on the workstation that supports the XRD, though programs stored on the instrument should cover most basic analysis needs. Documentation on the use of XRDMP Creator is available in the XRDMP Creator Help menu. If you need to create new programs and need assistance, please contact Breakerspace staff.

Advanced mode:

Advanced mode is used to change optical components, manage data (including importing programs, and deleting programs and results), and other advanced configuration tools. Lab users typically will not need to access advanced mode, and instruction of its use is beyond the scope of this tutorial.

Data processing and analysis:

Data from the Aeris can be processed using HighScore Plus 5.0

Using High Score Plus:

Determine background:

Treatment > Determine Background
Automatic usually does the job.
Granularity changes the distance between points of inflection on the background curve.
Bending factor determines how bendy the background is (as the name suggests).
Click Accept.

Determine peaks:

Treatment > Search Peaks
Play with the significance until the peaks reflect what you think are peaks.
Under Peak List, go through the peaks detected to make sure the software didn’t make any mistakes. Delete peaks by Right Click > Delete Peak. Insert peaks by
- Option 1: Treatment > Insert Peak (Ctrl+R). Click on the tip of each peak you want to add.
- Option 2: In Peak Lists > Right Click > Add Peak… and manually enter the data.

Determine a mystery compound:

After determining the background and peaks,Right Click > Search Match > (Optional) change the search settings > Search > Ok.
Options for improving your outcomes:
- Under the Restrictions tab > Restrictions set > Select Restriction set, you can pick your type of material from a drop down menu. For example, if you material is organic, select “Organic”
- Under the Restrictions tab > Edit… will give you a pop up for many ways to restrict your search. For example, under Chemistry, one can input the elements that are or are not present in the sample. Ther
- Clicking Execute Fitting > Default often improves the confidence and precision of the results.
Interpreting the Matches:
- Score shows the confidence of the program in the pattern match between your samples and the candidate. To check if the program was correct, click on the candidate you are interested in. Thin blue lines will show up on the graph. Check that each blue line matches up with the height and location of a peak of your sample.
- Once you are confident with your match, left click and pull it to the Pattern List panel. This “accepts” it. On the graph, if any peak is not matched by the accepted candidate’s pattern, it will retain a blue downward facing arrow on it. The candidates list reorganizes to find a compound that fits the unfitted peak.
- Continue this process until all peaks have been matched and all compounds in your sample have been found.

Common failure modes:

Booting the instrument with all sample changer positions occupied will result in an error. Remove one of the sample holders, so that there is a free spot.

Manufacturer’s manuals:

Exercises:

Beginner: Identify the mystery powder
Intermediate: Distinguish amorphous and crystalline polymers
Intermediate: Distinguish mineral forms of calcium carbonate, i.e. calcite and aragonite
Advanced: Identify mystery powder and label each peak with the crystal plane it results from