Processing of diffraction data with the HIGH SCORE PLUS program

1. Introduction
XPert High Score is the next generation software identification program supplied by
Malvern/PANalytical. It is designed especially for easy evaluation of complex phase mixtures. The
program contains a number of supporting functions, such as simulation of diffraction, modification of
diffraction data, semi-quantitative phase analysis, etc. Generates its own type of report. It also supports
the "Clipboard" feature, so you can create your own reports using Microsoft Word. A quick guide to
using the High Score program is demonstrated on the file Mixture3. RD, an artificial mixture of 3
minerals. To evaluate the phase composition, it is possible to use both the small demonstration database
from the ExampleDb directory and the converted ICDD PDF2 database. The most important commands
required to perform each action or sequence of successive steps are shown in bold italic.

2. Retrieving and displaying data

To load data into High Score, the standard File – Open procedure will be used (after the HighScore
program has been started). Then you need to choose from the correct directory with the file we want to
process. The program is set up in such a way that the data directory shows files with all allowed suffix
types, ie. XRDML and other older types of Philips extensions (RD, SD, UDF, etc.), files measured on
the difractometers from Bruker, Stoe, Seifert with their extensions and files processed by various
crystallographic programs. When you select and double-click the Mixture3. RD file, the High Score
desktop is divided into several table windows ("Panes"). In the largest-left upper part is a window with
a graphic record of the scan.

If we know that some of the compounds are certainly present in the sample, we can put their reference
codes directly into the window of accepted phases (the window in the upper right section titled "Lists
Pane, Pattern List – „accepted"). In the demonstration example, this is the calcite compound and the
procedure is as follows: Reference Pattern – Retrieve Pattern by – Reference Code. In the displayed

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window we have to write the card PDF number(Reference codes) 05-0586 (Calcite)(we must know the
code from our previous work).

We can enter cards from database using their PDF number, phase name or by their chemical formula.
After clicking the load button, the "Peak List" window appears in the upper left part and the "05-0586"
tab window below it with line intensities. The switch between this card and the diffraction record is
achieved using the Analyze and Pattern buttons in the bar below this window. If we toggle the
corresponding button on the scan, we see vertical gray stripes under some peaks, which show which
parts of the scane are explained by the calcite compound (comparing the first 20 reflections from the
card with the measured scan).

In the "Lists Pane" window, the "Accepted" section has lines with the specified phases (in this case,
only the Calcite phase). Data such as reference codes, compound name, chemical formula, scale factor,

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etc. are listed. In the last 2 columns the Relative Intensity Ratio (usually called „corund number“ if
available on the card) and semi-quantitative estimate based on RIR value is shown here – 100, since we
have accepted only one phase.
If a phase search is specified by name or chemical formula, the number of phases that contain that
specified string appears in the „accepted“ window. The incorrect or unlikely phases should then be
erased by the illumination of these phases and using the DEL button.
If we place the cursor on this line and click on the right mouse button, a submenu will appear where the
line "Analyze Patterns Lines" is first. When you click on it, you will see Reference pattern 05-0586
including Intensities, d-spacings, 2Th values, which indicates which reference intensities have been
successfully used for identification (in the column "Matched" values, ).

3. Processing of Diffractogram(powder patterns)

At this stage, data are prepared for phase identification. The most important steps are to specify the
background and to find all peaks. For demonstration of both steps, we will use the file Mixture3. RD
again. We load it in the same way as in the previous chapter.

To determine the background, you need to click Treatment – Determine Background. Then a small
window "Determine Background" appears, and the graphic record of the scan renders with a different
color of the background design (preprogrammed color is green).

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In the "Determine Background" window it is possible to choose from several pre-programmed
parameter sets for the processing of diffractogram. Click the More button and the arrow (the parameter
sets will appear in the list). When you click the selected file, the background is automatically
interleaves. Another option is to perform background fitting with our own parameters. There are 3
buttons at the top of the Determine Background window. If we click on Automatic, the background will
be fitted and the Bending factor can be used to adjust the background. For detailed control, you can use
zoom at any point of the scan. If we want to insert the background manually, we click the Manual
button. After that, we have the ability to add more, move, or delete suggested background points.
Button By Peak Search usually does not give useful background.

Click Accept to confirm the suggested background.

Click „Anchor Scan Data“ button in the "Lists Pane" window and columns will display with
background values.

4.(Search Peaks)
To find the peaks, click Treatment – Search Peaks.

After the action is executed, the window with the parameters of the signification and peak width
described above is opened. These parameters are connected with the search procedure using method
Minimum 2nd derivative. There is still a method of searching by the vertex of the smoothed peaks.
Once again you may click the More button, you can select from one of the pre-programmed search
parameter files.

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When you click the Search Peaks button, the graphic record of the scan shows the suggested peaks both
inside the graph and above the window. The full line marks the peaks belonging to Kα1 and Kα mixed
peaks, dashed line marks Kα2 peaks. Peaks that are not yet assigned at this stage are marked with a
small "v" at the lines above the window with the scan. The quality of the proposed peak detection can
be checked again in detail using zoom. Click Accept, if the suggested peaks are correctly chosen,. Then
the Peak List appears on the right side of the screen in the "Lists Pane" window with positions, heights,
halfwidths and other parameters of the peaks found. Kα2 peaks are listed on a grey background. To
clear a peak from the list, you can highlight the corresponding row and click the DEL button, add a
peak using the Treatment – Insert Peak and move the large cross to the appropriate position by clicking
the left mouse button. To exit the insertion, it is necessary to perform the Treatment – Insert Peak
again.
The obtained results can be saved(recommended) using File – Save Document to a file that is
automatically assigned the HPF suffix.

5. Search-Match
The phase identification (Search-Match procedure) can be done after a diffraction record has been
processed, i.e. the background determination and search peaks. You can also use previously processed
files and open their version with the HPF extension. The Search-Match procedure only works with Kα1
peaks. The stripping of the Kα2 contribution shall be made automatically without external visibility. In
order to see which data the search procedure uses "de facto", the user must do Kα1/α2 splitting, or Kα2
Stripping (see the corresponding line in the Treatment menu).

For demonstration purposes, we will open the file Mixture2. HPF using File – Open. We run the
Search-Match procedure with the sequence of Analysis-Search-Match commands.

The "Search-Match" window will be opened on the screen. At the top of this window there are 3 tabs:
Restriction – On this tab you can select a filter for the phase database. No restrictions are considered in
the None selection. When you select the Restriction set, you can choose one of the pre-programmed
filters (Common for general phases, Default without limits at max. Number of 105 phases, Inorganic
limited to inorganic phases, Low sets with Excluding the phases calculated from the structural
information – ICDD Set 70 and above, Minerals with restricted to mineralogical phases, NoNonsence
excluding rare and inert elements and cards marked by users for deletion, Organic restricted to organic
phase and Star restricted To phases where quality factor in the database is marked as *(Star). Each of

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these filters can still be edited using the Edit Restriction Sets button. You can also create your own
restrictions and load them after checking the Subset option and selecting the restriction name.
Parameters – use this tab to select other Search-Match parameters. The "Data Source" parameter
specifies if only peak intensity, peak profiles, or peaks & profiles are used for the search. The parameter
"Scoring scheme" can be chosen to distinguish between samples having one-phase or more phases. In
single phase option, all reference phases are penalised, which do not explain all the peaks and profiles
of the measured scan.

The 4 parameter boxes listed under Scoring scheme part may be used to determine options for the
Search-Match procedure :
Auto-Residue: If ON, then the Score parameter is recalculated for other candidates when the phase is
accepted.
Match intensity: If it is ON, the Score parameter also reflects the intensity match, not just the presence
of the peak and its position
Demote unmatched strong: If ON, then the phases with more than one misssing strong line (> 50%) are
excluded regardless of their Score parameter. Normally this is a fairly good way suppressing unwanted
candidates. When phases with very low concentrations or strong textured are present in the samples, the
choice of this parameter may lead to incorrect results
Allow pattern shift: When searching for phases, the 2Th line „card positions“ are changed (varried) to
fit better the measured data. The maximum offset is 4 x FWHM. If this parameter is ON, it must match
a position of at least 2 lines, otherwise the phases are marked as "No matching lines".(this feature is
useful)

Automatic – This tab describes the conditions for automatic phase identification – box Identify fmust be
checked and parameters set . Candidates fulfilling these conditions are automatically accepted. The
Auto-residue parameter is always enabled for automatic identification, is ON.
Maximum no. of accepted patterns: specifies the max. number of accepted (i.e. identified) phases
Minimum candidate score: the minimum value of the Score parameter to consider the phases for
automatic identification
Search depth: limits the number of candidates to be included for the automatic identification
Matched lines/total lines: specifies the minimum percentage of matching lines for candidates to be
accepted

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Minimum new lines: prescribes the minimum number of new matching lines for each candidate
Minimum scale factor: prescribes the minimum value of the Scale factor parameter. Candidates with
lower Scale factor are excluded from automatic identification.

As with the "Search Peak" window, you can use the „More“ button in the "Search-Match" window and
choose from a pre-programmed set of search-match parameters even for identification. These batch files
are marked as "User Batches" in the High Score program, and some of them are also available as
buttons in a row below the "Additional graphics" window.
All these batch files perform the following sequential steps before the phase search-match – background
determination, peak search and scan conversion from automatic divergence slit mode (ADS) to fixed
divergence slit mode (FDS)(cards in PDF database have relative intensities measured in FDS mode,
score performed on intensities is significantly less important than score on d-spacings so i tis
recommended not to perform conversion from ADS to FDS mode).
Overview of "User Batches" and their parameters:
Default – No restriction, Peak & Profile Data, Multi phase, Auto residue, Match Intensity, Demote
unmatched strong, No automatic Identify (i.e a list of possible phases will be created, so-called
candidates, using the above parameters, but none will be accepted)
IdeAll - No restriction, Peak & Profile Data, Multi phase, Match Intensity, Demote unmatched strong,
Automatic Identify s paramery: Max patterns 5, Minimum Score 27, Search depth 6, Mached lines 60
%, Min. new lines 3, Min. Scale factor 0.06
IdeCom – Restriction on Common Phases, than same as IdeAll only Matched lines 40 %
IdeMin - Restriction on subfile Minerals, than same as IdeAll only Matched lines 40 %
Minor Commons – Restriction on Common phases, Peak & Profile Data, Multi phase, Auto residue,
Match Intensity, No automatic Identify
Minor Minerals – Restriction on subfile Minerals, Peak & Profile Data, Multi phase, Auto residue,
Match Intensity, No automatic Identify
Minors – No restriction, Peak & Profile Data, Multi phase, Auto residue, Match Intensity, No automatic
identify
PrintIdeAll – like IdeAll, only Matched lines 40 %
Untitled – Restriction on phases with quality „*-Star“, Peak & Profile Data, Multi phase, Auto residue,
Match Intensity, Demote unmatched strong, No automatic Identify.

For demonstration purposes, using the „More“ button, we select "Default" and click on Search. After a
while which is necessary for search-match the PDF database, a list of candidates appears on the right
side of the desktop in the "Lists Pane" window. Strips with the line positions of the illuminated(chosen)
candidate and ow it the line positions found by the "Peak Search" procedure will appear below the
measured scan in the "Additional graphics" window. A residual colour is shown in green in this strip,
i.e. unexplained peaks (either total peak intensites or parts of their intensities). For further work, press
the OK button in the "Search-Match" window to confirm the list of found phases-candidates.

6. Phase identification
The identification consists in selecting the correct phases from the list of candidates and moving them to
the "Accepted Ref. Pattern" window (the top of the "Lists Pane" window). The "Additional Graphics"
window is used as supporting information for this selection – when we right click on this window, the
"Show Graphic" menu appears and we can select different options for additional graphic information:
Difference plot, FWHM Statistics, Separate Patterns, All in One, Compare Mode, Zoom Overview a
Pattern Overview. The most commonly used modes are All in One and Compare Mode. Additional
support information can be obtained by right-clicking on the candidate-phase line. A submenu appears
and we may select Analyze Patterns Lines (see chap. 2). This will display the phase list of peaks, their
intensities, d-spacings(interplanar distances), positions 2θ and the indication whether the peak matches

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the line in the measured scan. Based on this information, we can try to move the
iluminated(highlighted) phase to the "accepted" section. For the demonstration file, select e.g. Escolaite
– Cr2O3 and drag it to the accepted section.

If you have the All in One mode selected in the „Additional Graphics“ window, we can see the lines of
the accepted phases at the bottom strip, in the middle strip are peaks found by the Peak Search
procedure and the residuum (green), then in the upper strip are the lines of the first phase from the
„Candidates“ window.

When the first selected phase (candidate) is accepted, the remaining candidates are reorganised
according to their new Score factors (we can see that the number of Calcite phases are moved in the
first places). After accepting the most appropriate calcite phase (dragging it to the „Accepted..
„ section), the list of candidates is reorganised again (as the Auto Residue function was switched on).
The first places, according to the highest Score factor, were now given to Fluorite phases. Please note
at the same time, that a large number of „v“ symbols dissepeared over explained lines in the peak
marking above the measured scan.

The gray stripes inside and under the peaks of the scan indicate the area of peaks explained by
acceptance of the selected phases. The acceptance of Fluorite manages to explain all the measured lines.

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The final step of phase identification is to save the results using the File – Save Document or File –
Save As... sequence. . Saved files have a .HPF extension.

7. Changing the "Score" parameter

The "Score" parameter is a rather complex expression, the calculation of which depends on the settings
of the search parameters (see the Parameters tab in the Search-Match window). The higher the score is,
the better the consensus between the lines of the candidate phase and the lines of the measured
diffractogram (powder pattern). The Score parameter can also change after performing a search-match
operation. In the case of a mixture of 3 minerals, three phases Cr2O3, CaCO3 and CaF2 were identified,
which were moved from the candidate list to the "accepted Ref. Pattern" window.
By dragging Flourite back to the candidates, the Score parameter of all candidates are automatically
recalculated. Further changes of the Score value parameter (possibly the order of phases) can be
achieved by changing the search parameters

Click on the Search-Match icon and run Search-Match repeatedly selecting Profile Data, Peak data and
then Peak & Profile Data. You can also turn off the "Match intensity" parameter and follow the change
of Score parameter again by clicking Search. It is also possible to observe the change of Score in the
Single phase and Multi phase selection or when the "Allow Pattern Shift" parameter is turned ON and
OFF.

8. Phase identification strategy

In general, there is no universal phase identification guide. You can still build an overview of
recommended steps and procedures that can help identify or overcome problems with finding the right
phases:
Start
Load the correct data file into the High Score program. It is recommended to check the wavelength
used. If the λ information is not included in the measured file, it is supplemented by a preset (default)
value set in the High Score program. It is also recommended to check the assignment of the correct
database of reference phases before starting the analysis.
Pattern Treatment

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1.specify the background correctly - determine background (if not done, the background is determined
automatically when searching for peaks). When the background is too low, the number of phases that
can explain the measured scan increases (sometimes disproportionately)
2.choose a higher "Significance" value for Peak Search (if the profile data is used to identify phases,
there is no need to localize all small peaks)
3.convert intensities from automatic divergence slit to fixed divergence slit – Correction + Convert
Divergence Slit (not strictly necessary, but after conversion the measured data matches with the
reference better)
Search-Match getting list of „candidate“ phases.
To solve phase identification problems, it is recommended to change some of the Search-Match
parameters to
create a more acceptable list of candidates by changing the Score parameter. The procedure is described
in the previous Chapter 7. It is possible that the missing phase is not included in the candidate phase list
because the restrictions or some search parameters are set too "tight" or too "loosely". You can also try
using the Track Graph function – after enlarging the area of angles with unexplained peaks, the Track
Graph function is clicked (the last icon on the right side of the bottom bar). The search procedure
focuses only on the enlarged area. If it fails, it is possible to try to limit the scan to this area ( use the
Clip Achor Scan Range) and perform a Search Match on this "new" scan.

9. To display multiple diffraction patterns in one image

Before loading more diffraction patterns into one image, consider which diffraction pattern use as the
first one which will serve as so-called anchor scan. The standard File – Open procedure is used to
retrieve it. Another simultaneous retrieval of the diffraction pattern (i.e. insertion) into the HighScore
program is done using the File-Insert command (CTRL I abbreviated notation). After inserting a new
diffraction pattern, the two diffraction records are shown separately in the main window below each
other, see the following example:

To view both records in a single coordinate system, simply click the compare tab in the bar below the
diffractograms (see next figure). Both records will be overlapped or shifted (see example on the

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following figure):

The Edit Scan Parameters window (in the Treatment menu) is used to move the Anchor scan. When it is
opened, the "Add" check box is selected and the vertical displacement value is entered in the adjacent
box. In the following figure is an example of an offset entry of 100 cts.

Edit Scan Parameters window can be used well for shifting other diffraction records. Clicking the Scan
List in the List Pane window will display a list of inserted diffraction records in rows. Clicking the

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right mouse button on the corresponding line will open a menu to manipulate the scan. The first line of
this menu is Edit Scan Parameters. The subsequent displacement is done in the same manner as
described in the paragraph above.

Another option to move the inserted diffraction record (the position of the original Anchor scan remains
unchanged) is to click on Treatment at the top of the main bar and in the expanded menu to the next-last
item from the bottom of the ADJUST to Anchor.... A window will then open to allow you to
manipulate the selected inserted record:

The diffractogram with which we want to manipulate is displayed in the "Adjust" line. When you insert
multiple diffractograms, you need to select the one you want to manipulate.
In the next step, you can choose the way of manipulation. The inserted record can be fitted or shifted
horizontally and vertically. To shift by a certain value, you need to select "User Defined" in the
"Method" window:

The example below shows the offset of the inserted record "Kotlik8. Rd" from the above example about
100 pulses in the vertical direction:

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After using sequence "Adjust", "Accept" and "Compare", the selected record is shifted in one window –
see the following figure:

10. Peaks labeling

The diffractogram, which is displayed in the main window, can be labeled in 2 ways. You can either use
simultaneous description of all the peaks displayed in the main window (depending on the zoom used),
or you can describe individual peaks separately.
Simultaneous description
The mouse cursor should be placed in the main window with diffractogram. Then the right mouse
button is clicked. The menu will then be clicked on Label Peaks. This will open a window where you
can select the information that will be listed for each peak (see the "Labels" column). If the text option
is selected, you can type it in the Text window. When you click the Font button, you can select the font
type that contains the information:

Since the selected information can be placed in a horizontal, vertical or rotated position, it is
recommended to choose the font type TT or O, which allows the shooting of descriptions. To shoot the
descriptions you need to click on the arrow in the "Align Labels" section and the Angle option is
selected here.

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Labeling individual peaks
To start labeling peaks separately one must click the Switch to Write Text Mode in the left vertical bar.

Then a pencil tip symbol appears under the cross cursor. The cursor must be moved to the desired
location near the peak where the description should be placed. When you click the mouse, a window
will open to create a peak description

After writing the desired text (you can choose the size, type of font and horizontal or vertical placement
in the diffractogram), you need to click the OK button. For the Greek alphabet, you need to select
Symbol as the Font. This is what you need to do with all the peaks where the label is required. From the
text mode, click the Switch to Write Text Mode icon again to jump. An example of labeling part of the
diffraction record is in the following figure:

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 Counts
Mixture3.RD
Calcite

10000

Fluorite

Green cinnabar

2500

Fluorite

Calcite

0
28 30 32 34

Position [°2Theta]

11. Graphics
You can change the graphics of the diffractogram (s) through the Document Settings window. To
invoke it, you have to click either the Customize item in the main top bar, Document Settings line, or
click the right mouse button in the diffractogram window, and the left click confirms the selection of
the last line of Document Settings. In a pop-up window, you can change the graphics of the
diffractogram through Graphics Display and Graphics Colours. In the Graphics Display, you can
change scales of the axes, the thickness of the scan lines, the frame, the divisions on axes, the bar
marking of peaks and phases. An example is shown in next Fig.:

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On the Graphics Colours, you can change the colors of the calculated lines and their style (solid line,
dashed..).
On the Legends & Grids, you can set an auto heading for the diffractogram. To do this, click the Scan
View Legend... button. And check the box here. If the "Scan Name" check box is selected, the title and
extension (e.g. Rd or XRDML) are entered in the heading. If we want to give the name without
extension, the last lower field "Sample Identification" will be checked. If a description other than the
name of the measurement file is to be automatically entered in the title, you need to remember this
when filling in the "Identification" field when running the measurement in the Data Collector program.
If necessary, the "Sample Identification" can still be edited via the Edit Scan Parameters window (in the
Treatment menu). Here is the "Sample identification" check box in the Middle Special Data tab, in
which the change can be made. The modified text is then automatically transferred to the diffractogram
name (its location is in the upper left corner of the diffractogram).
Another option is to include a title by switching to text mode. The procedure is the same as mentioned
in the previous chapter for the description of individual peaks (see Switch to Write Text Mode).
12. Copying images into the text editor
To transfer the measured or processed diffraction record into a text editor (e.g. Word) can be done in
multiple ways.
The HighScore Program can create reports. To create them you need to click on Reports in the upper
main bar and in the expanded menu you can select either Create RTF Report or Create Word Report.
Both formats can use predefined versions of reports or users may create their own versions of reports,
which can also be incorporated into predefined versions of reports.
You can also use the Copy to Clipboard feature to transfer a record to a text editor. To do this, click the
mouse to the main window in the diffractogram area, and then use the File – Copy sequence or the
shortcut CTRL + C. Depending on what options are checked in the HighScore graphics settings, the
image is copied to the Clipboard either the main window with a diffractogram or a window with
additional graphics (located at the bottom left of the screen below the main window) or both Windows.
In the graphical settings, you can also select the order of colors that will be automatically assigned to
the loaded or inserted diffraction records — see the following illustration:

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The third option is to transfer the screen using the ALT + PrintScreen buttons to the Windows Paint
program (Start – Programs – Accessories – Paint commands). Copy the entire screen to the Clipboard
by using ALT + PrintScreen, the entire image is pasted into the window in paint by using CTRL + V.
Next, the left vertical bar is clicked on the selection icon (dotted rectangle), and when the left mouse
button is pressed, it is selected The area to be transferred to a text editor — see the following
illustration:
The selected viewport is copied back to the clipboard using CTRL + C and when you switch to the text
editor it will be pasted to the position of the cursor using CTRL + V, see example in the following
illustration :

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Counts

Fluorite, syn
Mixture3_Defect.CAF

10000

Calcite

Eskolaite, syn

Eskolaite, syn
Eskolaite, syn

2500

Calcite
Calcite

Fluorite, syn
0 Calcite
20 25 30 35
Position [°2Theta]

13. To insert a new card int the database

The PDF database must be writable - (Customize-Manage Databases-click writable). Creating a new
card assumes either that the diffractogram of the new compound is available, or the file with 2Th
positions and intensities (2theta and I) in the ASCII form is available. If we do not have a diffractogram
but 2theta and I from the article, so I need to first create an ASCII file *. Dbi. We load this file into the
HS and then click on the Reference Pattern, ADD user pattern to database.

14. Create report – Information about the sample evaluation in the form of Word document *.
doc
It is not available yet.

15. Comparison of 2 diffractograms with different wavelengths

*.xrdml, *. raw or *. rd files contain wavelength information. If we want to compare 2 diffraction
records with different wavelengths, we load the first diffractogram, which will be an anchor scan and its
wavelength may differ from the „default“ wavelength of the document. We insert 2nd diffractogram.
This is converted to the wavelength of the first diffractogram. It is possible to insert additional
diffraction, all of which will be recalculated to the wavelength of the first diffractogram.
I may want to recalculate a diffraction record measured with a wavelength Cu to another wavelength
e.g. Co. I have to open any diffractogram (raw) measured on the Co lamp, insert diffractogram
measured on the Cu lamp, the conversion to Co lamp is performed and then I save as *. XRDML.

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It is possible to insert additional diffraction records, all of them will be recalculated to the wavelength
of the first (anchor) diffractogram.
16. How to generate a diffraction record for the structure retrieved from CSD, from the *. cif
a. Insert file *.cif and change desktop setting to the Desktop Structures. To generate a diffraction record
with the *. xrdml or *.asc extensions is not possible (no measurement information). The way to
generate the diffractogram is as follows. We go to Peak List, click a right mouse, Copy Peaks to New
document. A new document is created, and then data can be exported to *. ASC.
b. Insert file *.cif and go to Desktop Structures.To generate a diffraction record – Analysis-Rietveld-
Start Pattern Simulation, click the right mouse in the scan sheet, Convert calc profile to Scan, take the
new scan as anchor and export it as *.xrdml.
The minimum step is currently 0.001 °, setting simulation. Changes in FWHM did not affect on the
width of reflexions. The width of the reflexions could be changed in the Refinement control, Caglioti
width, W. It was pretty unstable, even W = 0.00001 could be used. It is also possible to generate a
diffractogram with only Ka1.

17. Create a new desktop

To create a new window layout, open one from the pre-programmed desktop layouts, save it with a new
proper name. Then edit a new layout and save it.

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18. LeBail fit
Find peak positions. Analysis-Rietveld-Enter New Structure, enter space group, lattice parameters. Go
to Lists Pane, Refinement Control, click New Phase and change the Structural fit to the LeBail fit.
Then perform refinement of the lattice parameters and get reflectio indexing.

18.Phase analysis – intermediate examples

Pl.rd – click Ideall, remove accepted phases, choose teflon. Peak at 37° is clearly asymetric, which
supports phase Teflon.
Quatrz.rd – click Ideall, SiO2 is OK, some peaks not explained. Some other information is necessary,
e.g. minerals. It is still problem to get kaolinite which is caused by measurement from rather larger 2Th
angle.
CSAND.rd – click Ideall, remove accepted phases. Choose Aragonite. The other phase is not clear, fill
in some other small peaks and Calcite can be clearly seen.
Niore.rd – click Ideall, remove accepted phases. Fill in all peaks, watch changing phases order.
TB3.rd – click Ideall, remove accepted phases. Fill in all peaks, watch changing phases order. LaB6,
LaB5, BaCl2x2H2O.
Akku6b.rd – click Ideall, remove accepted phases. Fill in all peaks, watch changing phases order. 5 Pb
phases
Demo16.rfl – click Ideall, remove accepted phases. Fill in all peaks, watch changing phases
order.Zeolit.
Pure2.rd – click Ideall, remove accepted phases. Fill in all peaks, watch changing phases
order.Olanzapin.

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Vp.rd – click Ideall, remove accepted phases. Fill in all peaks, watch changing phases order. Na,P
compounds.

19. How to insert or edit RIR value(„corundum number“)

Click with the right mouse selected card in Pattern List („Accepted“), User Reference Patterns-Edit
Pattern(or Reference Patterns-Edit Pattern) and insert or edit the RIR number. Database must be
writable.
20. Peak and scan intensity statistics

Sum of net Intensity (cts) is equal to sum of all pulses Area (cts**2Th) of all peaks in the Peak List
including Ka2 without background.
Sum of backgr. Intensity (cts) is equal to sum of all pulses below background line.
Sum of Observed Intensity (cts) is equal to sum of all pulses in diffraction record.
To get net intensity for only one peak, choose the proper peak range, Clip range and Sum of net
Intensity (cts) equals the sum of all the pulses for that peak

21. Semiquant
Semiquant calculates the mass concentration using all available reflections in measured range . The
concentration can change if we change the range used. It may be useful in the case of existing texture to
avoid textured reflection by decreasing range used with Clip range.

22. Data *.asc

You may download data form Web, open it in Notepad. Edit them and save them as text format in file
with .asc sufix.

23. Change data *.xye from synchrotron to *.asc.

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Open *. xye in Wordpad , Save As „text document“ in file with the extension *. asc.

24. Changing the wavelength

To change the wavelength, load the data and change the wavelength via Edit scan parameters.
Remarks
1. Spectral lines – CuKb,WL, CuKa1, CuKa12,Ka2
2. Spectral lines – WL, CoKb,, CoKa1, CoKa12,Ka2

2. Inserting peaks and editing in Peak list – Edit Peak Parameters.

25. Pictures

To make a black and white picture, you have to change each scan to a black color first. You can have 5
different ways of hatching. To make a thicker line use Customise Document setting Graphics Display
Line width.

25. Fixing line code.

Use Customize, save to normal matrix.

26. Editing peak positions.

Switch to "Select mode" and then move peak to the correct position.e.

27. 3D picture.
View Cursor mode, 3D Adjust Depth Mode a 3D Adjust Angle Mode gives possibility to set the
correct view towards diffractograms.

28. How to load x,y,z coordinations from cards with reference code 01, 04 into refinement
control.
Highlight the card line ina Pattern list, click right mouse, Convert Pattern to Phase.

29.Asymetric fit of peak profile

Cange to desktop "Profile Fitting". To fit the peak (or the part of diffraction record), select the proper
2Th range in the main window and select "Refinement Control" in the "Lists Pane", click „Global
Variables“. In the "Object Inspector", under "Profile fitting" set the asymmetrical fit. In "Assymetry
Type" choose "Split Width and Shape", which divides the left and right parts of the peaks in both width
and shape (you can select as well only division in width or the shape – " Split Width "," Split Shape ").
The fit will start by selecting the Treatment – Profile Fit.
30. Merging scans
Diffraction records have to overlap. The problem was to perform an Extend Anchor with Scan... When
the scans were in the *. xrdml format. The connection occurred, but the portion of the corresponding

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anchor scan had a significantly lower intensity. I exported the scans as *. ASC and then it was possible
to perform an Extend Anchor with Scan... No problem.

31.Adjust scan
Difraktogramy by se měly překrývat. Byl problém provést Extend Anchor with Scan…, když byly
scany ve formátu *.xrdml. Vyexpotortoval jsem scany jako *.asc a pak šlo provést Extend Anchor with
Scan… bez problému.

32.Powder pattern simulation

Customize-Program setting-Simulation –step 0.001 FWHM 0.05

33.Amoprphous content calculation - autoscale

Phase concentration can be calculated if for all phases present in the sample 100% standards are
available. Load the mixture and take it as a ANCHOR SCAN. Load standards and perform: Analysis-
Start Autoscale-Default. We click on the scan of standard and at autoscale we find the content of the
standard.

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