XPert HighScore Plus Introduction

A brief introduction to Search/Match, Rietveld-, Cluster-, and Crystallographic Analyses

Contents
Search/Match
Configure reference database Perform automatic search/match/identify Step by Step instructions

Rietveld analysis example

Perform a standardless quantitative analysis on a mixture of three minerals

Cluster analysis example

Analyze a set of 18 scans simultaneously to look for similarities

Search unit cell example

Determine the cell type for a material, index the reflections, and refine the cell parameters

Search/Match configure reference database

1. Load ICDD reference database CD (PDF2 or PDF4) in your CD-ROM drive (newest versions must be installed first on your PC according to ICDD instructions and run at least once) Menu Customize, select Program Settings Click on tab Reference Patterns Under Database conversion section, press Browse button to find the PDF2 folder on your CD with the reference data file (e.g.pdf2.dat) and click OK Press Start Conversion of ICDD Database button this could take 20 or more minutes depending on your computer speed

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Search/Match example
1. Select the Phase-ID desktop from the lower toolbar Open the example file c:/Program Files /PANalytical /Xpert HighScore Plus /Tutorial/mixture3.xrdml Click on Batch Button IdeAll on lower toolbar this will start a sequence of analysis steps in which the background is determined, peaks are searched, then the peaks and profile are compared to the entire reference database to identify the phases present.

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Search Match Step by Step

1. 2. Open another example file, such as PCHIPS. Under menu Treatment, perform a background determination and accept the result. Next select Peak Search. And again accept the result. It is not necessary to strip Kalpha2, smooth, or profile fit the pattern for the purposes of search/Match. Kalpha2 peaks are determined and marked in the Peak List

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Search Match Step by Step

1. Under Menu Analysis, Search Match, Execute Search Match, you can set restrictions based on reference database subfile, chemistry or reference card quality. For chemistry, click an element until it turns blue to indicate it may be present, or red to exclude it from the search. Grey elements will be allowed. Green restricts phases to the exact chemistry with all green elements.

Search Match Step by Step

1. Once restrictions are set, press Parameters tab to change the scoring scheme or allow pattern shift Press Automatic tab to set up filter to accept phases that match Press Search, then OK. The Pattern List tab will have two components: an Accepted Patterns list, and a Candidates list. You can drag and drop phases from one pane to the other, and the candidate list will automatically rescore based on the unaccounted peaks. See Chapter 10 in the Quick Start Guide under Help in the software for Phase Identification Strategy & Troubleshooting

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Rietveld Example
1. 2. Select the Structures desktop from the lower toolbar. Open file Mixture3, located at c:/Program Files / PANalytical /Xpert HighScore Plus /Tutorial/mixture3.xrdml. Insert the structures by going to Menu File, Insert, and browse for the example structure set at c:/Program Files / PANalytical /Xpert HighScore Plus / Structures/example. Check off the phase present: Eskolaite, Fluorite, and Calcite. On the Lists Pane, you will see under the Refinement Control tab the three phases appear. Clicking on any one will show the parameters that may be part of the Rietveld refinement.

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Rietveld Example

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To start a Refinement, go to menu Analysis, Rietveld, Start Rietveld Refinement press the arrow to the right to see the choices select default for this example. This will execute an automatic refinement using the parameters that can be found under the menu item Edit Automatic Rietveld Steps. As the refinement progresses, you can dynamically see how the least squares refinement converges (R-values window), and you can see how the weight fractions change as the scale factors are refined (Quant chart on pattern select Show Quantification Chart from upper toolbar). To display a single phase profile, press show selected phase profile button on upper left tool bar, then click on any phase in refinement control window. Right click in the Additional Graphics pane to select Difference Plot for viewing For manual refinement control, see the Quick Start Guide chapter 9 under Help in the software.

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Cluster Example
1. 2. Open the file c:/Program files /PANalytical Xpert HighScore Plus/Tutorial/Cluster Go to menu Analysis, Cluster Analysis. This will automatically produce tabulated results with a correlation matrix, dendrogram, PCA and clusters. The cutoff for the clusters is automatically determined by the KGS test.

Cluster Example

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Click on PCA tab. Click, hold, and move mouse to rotate plot. Scan 18 appears visually as more of an outlier, so to remove it from the cluster, go back to the Dendrogram tab. In the Cluster parameterswindow to left, next to cut off method select Manual, then using the mouse click and hold the cut off line and drag it to the left to redefine the clusters.

Cluster Example

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Now the PCA and Cluster tabs are updated. Each individual cluster tab shows all scans in the cluster overlaid, with the most representative pattern marked with *** in the legend. This pattern can then be further processed, e.g. search/match performed, to understand the composition of the cluster scans. The outlier pattern is on its own tab to the right in the Cluster Analysis Window under Not Clustered.

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Cell Search/Cell Refinement Example

1. Open file c:/Program File/ PANalytical/XPert HighScore Plus/ Tutorial/ TaSSe.rfl Click on Scan list, double click on the file TaSSe, then in object inspector scroll down and doubleclick on Instrument settings, then check the first box for incident monochromator (this particular file was collected with alpha1 only) Menu Treatment/ Determine Background fit and accept a background. Menu Treatment/Search Peaks, perform and accept a Peak Search. Go to Menu Analysis/ Crystallography / Search Unit Cell. Execute a Cell Search, press OK. You can try an additional Indexing Method for this example, such as DICVOL. The results will add to the list of Cell Candidates. Click on the candidate with the highest figure of merit (FOM), then press the Refine button 2.

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Cell Search/Cell Refinement Example

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Press Start Refinement to refine the unit cell. Press on the Calculated and Observed Peaks to see the hkls assigned, and see how well the calculated and observed peaks agree. Press the Space Group Test tab if you wish to have all space groups in the symmetry class identified tested against your data. Press the button Start Space Group Test to initiate this test. The candidate list it produces can be resorted by FOM by clicking on the header FOM. Highest FOM values all indicate a BCC cell.

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Further Guidance
1. Online Help XPert HighScore Plus contains an extensive online HTML based help. At any time, if you press F1, it will take you to the help section associated with the particular window you are in. Please read Chapter 3 Basic Ideas for an overview of the software and user interface. It is also possible to print dedicated chapters or the entire help guide by selecting a help contents item first. Quick Start Guide Under Help there is a Quick Start Guide intended to introduce you to these same basic steps, with more depth Practical Also under Help in Chapter 8 is an extensive Practical that walks you through analysis of the example files provided with the software in the Tutorial folder. A Literature List is available under Help, for further reading on the various topics. Website still need help? Specific questions can be submitted in writing on our website www.PANalytical.com and press Contact in the upper right hand corner. Application support may also be available by phone. Contact your regional PANalytical office for further assistance. Courses are also offered regionally.

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