Highscore Analysis

Susie Speller

A Basic Introduction to Highscore XRD Analysis Software

Displaying Scans Open raw data (.RD) file in Highscore. Inserting scans into an existing Highscore (.HPF) project. Displaying and changing scan properties in the object inspector pane. Different ways to display multiple scans in the main graphics pane. Zooming in on areas of interest. Document settings.

Phase Indentification Various pattern treatments need to be carried out before phase ID can be performed. These can be fully automated and performed as a batch program, but it is usually necessary to customize this program for your particular samples to obtain the correct results. In a batch program (such as IdeAll) all the pattern treatments are carried out unseen so you cant influence them. I suggest each stage described below is carried out separately to begin with, and only write a batch program if you have many scans on similar samples to analyze. Pattern Treatments Prior to Identification 1. Determine background. The auto function is usually acceptable, and the bending factor and granularity can be varied to get the best fit for the background. (This step can be done unseen when peak search is performed, but the algorithm used is different and there is no user input.} 2. Peak search to find peaks with high significance. The accepted peak data is given in the peak list tab of the lists pane. 3. Strip K2 peaks. (This is done unseen when search match is performed, which is often preferred because the graphics will then show the original data.) Search and Match and Phase Identification Search matching is used to find candidate phases from the reference database to explain the peak features in the measured scan. Advisable to set-up restrictions so that only a sensible subset of the full database is searched. The way in which the candidates are scored can be adjusted with various parameters either before search match is carried out, or afterwards (buttons on the bottom taskbar). Candidate phases can be shown in the main graphics pane with the scan data. When a phase is accepted (either by dragging from candidate list to accepted list, or by right-click and accept pattern), the scores of the remaining candidate phases change accordingly.

Highscore Analysis

Susie Speller

Unmatched peaks are indicated in analyze view by a v marker at the top of the scan. The residual unmatched peaks can be viewed in the additional graphics pane. This process can be automated by checking the identify box in the automatic tab of the search and match window, but need to have a good restrictions set and must check result is sensible! Peaks can be labeled using Tools / Label Peaks.

Example 1: Identifying Phases present in scan Mixture3.xrdml

Profile Fitting The Peak Search algorithm is good at finding significant peaks, but it does not accurately fit the shape of each peak. In order to carry out accurate peak-broadening calculations to estimate crystallite size and/or lattice strain (by Scherrer method), it is necessary to fit each peak required independently the profile fitting algorithm. This method will also give more accurate peak positions and intensity information for phase ID or quantitative analysis respectively. Note: For the best results, it is important to zoom in on the peak to be fitted so that no other peaks are in the frame before profile fitting is carried out. Example 2: Fitting peaks using the profile fitting algorithm using scan MB2470024.RD

Cluster Analysis It is possible to run cluster analysis on a series of scans to group them with other similar scans. There are a lot of parameters that can be adjusted to optimize this function, but it can be a very powerful technique. Basically each scan is compared with each other scan in the set and given a correlation score (according to the parameters chosen). This is displayed in a correlation matrix. The scans are linked together using an algorithm of your choice and visualized using a dendrogram. A cut-off value is selected and the clusters can be viewed in the pca tab (principle component analysis). Scans from each cluster can be viewed separately and phase ID can be carried out on a typical scan from each cluster if desired. Example 3: Basic demonstration of Cluster Analysis using MgB2 data (alldata.HPF).

Highscore Analysis Some Other Functions

Susie Speller

Degree of Crystallinity need a reference sample with known crystallinity. Full Pattern Autoscale quantitative / semi-quantitative analysis of an unknown sample using standards preferably with internal calibration. Scherrer Calculator estimates either crystallite size or lattice strain from a single peak using standard sample with large crystallites and no strain to measure instrumental broadening.

Reporting / Extracting the Data The software will create Word or RTF format reports which can be fully customized in Report / Edit Report Definition. Select items required on the left hand panel and drag into the right hand panel. To modify the default items in the left hand panel, click the item to view the parameters. When you have modified the parameters, click the <<More button to view the save icon. Save the new parameter set with a new name. Limitations of the Highscore Software The Highscore software does not have the capability to carry out full Rietveld Analysis, although if required this can be performed using XPert Plus on the old analysis PC. The Highscore software does not have the capability to create different users. The only way to achieve this is to set-up each user with an individual windows login. Since there are so many users of this system, this is not feasible. The Highscore software is very customizable. By all means create your own parameter sets, but it is very important to give them your name as well as an identifier because they will be available for everyone.

NB: Please be considerate of other users: if you do customize the window, return it to its original state before finishing. The default view can be reset using view / panes default setting. NB: Never enable any scan treatments to occur unseen when the scan is opened. These may not be acceptable for other users. More Help ? If you need more help to analyze your data, please do not hesitate to contact me. The Help section is very good for this software and gives practical examples, explains the functions and gives details of the algorithms used and references.