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The next step is to manually accept candidates that have a high score and that match the peaks and features of the measurement.
For that, select and drag the matching candidate patterns from the Candidates list to the Accepted Ref. Patterns list in the upper half of the Pattern List tab to accept it (Figure 13). When you select matching patterns, it is highlighted in gray and lines are displayed in the Main Graphics window and Additional Graphics panes (Figure XX13). Peaks will lose the "V" mark above the line. These peaks have been explained by the reference pattern. Peaks with a "V" have not been explained and/or matched (Figure XX13).
There are several views in the Additional Graphics pane to support the visual comparison between reference pattern sticks and the measurement. For instance:
- Select View > Additional Graphics > Compare Mode or
- Select View > Display Mode > Show Calculated Profile
Figure 1113. Move accepted peaks from the candidate window the accepted reference pattern. Candidates sub-panel the Accepted Ref. Patterns sub-panel
To check if the accepted patterns are indeed minerals and comply with the sample description, right-click a specific reference pattern in the Accepted Ref. Patterns list. Select Show Pattern to view the subfile information of that pattern (Figure XX14).
Figure 14. Information on an accepted reference pattern
If you wish to save the complete file (including the candidate list and the accepted reference patterns), click File > Save Document. HighScore Plus file format is .hpf.
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To complete a quantitative phase analysis you will use the Rietveld refinement in HighScore Plus software.
Starting Quantitative Phase Analysis
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- Determine the background
- Search peaks
- OPTIONAL: Strip the K-αα2 signal
- Peak Search and Match
Now you are ready to complete quantitative phase analysis using the Rietveld method. This method is a full pattern fit method. It is typically used for standardless, quantitative phase analysis.
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Select the desktop layout from Phase-ID to Rietveld Analysis on the Desktop toolbar (Figure 1215, arrow A).
Or View > Desktop > Desktop Name > Rietveld Analysis.
You can change the Desktop layout depending on the XRD analysis you perform in the HighScore Software.
Refinement ControlObject InspectorMain GraphicsAdditional Graphics.
In addition to the Main Graphics and Additional Graphics pane, available on the Phase-ID desktop as well, there are two other panes: Refinement Control and Object Inspector (Figure 15).
Figure 15. Figure 12: Rietveld Analysis Desktop Layout
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Start Analysis
Select Analysis > Fitting. Check that the option Fitting Mode is set to Automatic (Figure 15). Correct if necessary.
Select Analysis > Fitting > Start Fit> and then select <Phase fit> Default Rietveld to start the refinement with the default Rietveld parameters set (Figure 15, arrow B). Wait until it is finished, this may take a few minutes (Figure XX).
The peaks and the calculated profile are in the Main Graphics pane.
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In the 'Refinement Control' tab in the
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Refinement Control
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pane on the main display, double-click the Global Variables (Figure 16, arrow A) to open the 'Object Inspector' pane
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(Figure
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16). Select Global Settings>Agreement Indices to view the values of the Goodness of Fit and Weighted R profile (Figure
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16, arrow B).
Figure XX16. Refinement Control window pane displaying the Refinement Control, global variablesGlobal Variables. The Object Inspector can be used to look at the fit properties and agreement indices.
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Display the Phase Amounts
The phase amounts will automatically be displayed together with the phase legend in the 'Main Graphics' pane once the Rietveld analysis is completed (Figure XXA17A). Alternatively, you can open the 'Quantification' tab in the 'Refinement Control' pane and view a pie chart of the quantification (Figure XXB17B).
Figure XX17. A. Phase amounts as a percentage are displayed on the main graphics window. B. Pie chart of the phase amounts for the quantification of the phase.phases
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Export and Save a File
To export a file or save the file as a working file, click File>Save As.
Save the document as a .HPFhpf file (this is the HighScore working file format).
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