WinXPOW 3.05

POW
WinX
Software Manual
Version 3.05
(c) STOE & Cie GmbH 2011
STOE & CIE GmbH, Hilpertstrae 10, D-64295 Darmstadt

Phone (+49) 6151 / 9887- 0 Fax (+49) 6151 / 988788
E-mail: stoe@stoe.com Homepage: www.stoe.com
Contents
1 General 1-1
1.1 Introduction 1-1
1.1.1 General Remarks 1-1
1.1.2 Input Elements 1-1
1.2 Installation 1-3
1.3 The Main Menu 1-6
1.4 User 1-7
2 Instrument Parameters 2-1

2.2 Configuration 2-2
2.3 PSD settings 2-6
2.4 Defaults 2-10
3 Diffractometer Control 3-1

3.2 File 3-2
3.2.1 New 3-2
3.2.2 Open 3-2
3.2.3 Save 3-2
3.2.4 Save As 3-2
3.2.5 Print 3-3
3.2.6 Print Preview 3-3
3.2.7 Print Setup 3-3
3.2.8 Most Recent File List 3-3
3.2.9 Exit 3-3
3.3 Setup 3-4
3.3.1 Detector 3-4
3.3.2 Generator 3-4
3.3.3 Sample Changer 3-5
3.3.4 Title / Comment 3-5
3.3.5 Options 3-5
3.4 Diffractometer 3-7
3.4.1 Open Shutter 3-7
3.4.2 Close Shutter 3-7
WinXPOW Software Manual 0-2

3.4.3 Drive Circles 3-7
3.4.4 Set Slit Width 3-8
3.4.5 Sample Changer (Next Sample) 3-9
3.4.6 Sample Position 3-10
3.4.7 Erase IP-PSD 3-11
3.5 Ranges 3-12
3.5.1 Scan Mode 3-12
3.5.2 Scan Range(s) 3-13
3.5.3 Scan Usage 3-15
3.6 Measure 3-19
3.6.1 Data Collection 3-19
3.6.2 Step Scan 3-20
3.6.3 Count 3-21
3.6.4 Beam Optimization 3-21
3.6.5 Sample Position Measurement 3-23
3.6.6 PSD Calibration 3-24
3.6.6.1 General 3-24
3.6.6.2 PSD Calibration File 3-24
3.6.6.3 PSD Calibration Measure 3-25
3.6.6.4 PSD Calibration Evaluation 3-27
4 High-Temperature Data Collection 4-1

4.2 Configuration 4-1
4.3 Creation of the Raw Data File 4-3
4.4 High Temperature Data Collection 4-4
4.4.1 File 4-4
4.4.2 HTC Parameter File Setup 4-5
4.4.3 Input of a Temperature Program 4-6
4.4.4 Preferencess 4-8
4.4.5 HTC Measurement, Run and Control 4-9
5 Graphics 5-1
5.2 Files 5-2
5.3 View 5-4
5.4 Options 5-6
5.5 Window 5-11
6 3D-Graphics 6-1
6.2 Files 6-2
6.3 View 6-3

6.4 Options 6-5
6.4.1 Colour 6-5
6.4.2 Font 6-6
6.4.3 Labels 6-6
6.4.4 Scaling 6-7
6.4.5 Title 6-7
7 Raw Data Handling 7-1

7.1.1 Menu-, Caption-, Status- and Toolbars 7-2
7.1..2 Layer Panel 7-2
7.1.3 History Panel 7-3
7.1.4 Range View Window 7-3
7.1.5 Report Panel 7-4
7.2 File 7-5

7.2.1 Different Working Modes 7-6
7.2..2 Export Files 7-7
7.2.3 Preferences 7-8
7.3 View 7-10
7.4 Parameter 7-10
7.5 Ranges 7-11
7.6 Operations 7-13
8 Pattern Fitting 8-1

8.2 File 8-1
8.3 Parameters 8-4
8.4 Operations 8-10
8.5 View 8-14
8.6 Options 8-16
9 Peak Calibration 9-1

9.2 Files 9-1
9.3 Match Peaks 9-2
9.4 Calculate 9-4
9.4.1 Calculate polynomials 9-4
9.4.2 Calculate spline 9-4
9.5 Calibrate peakfile 9-6
9.6 Auto calibrate 9-6
9.7 Write IP calibration 9-6

10 Index & Refine 10-1
10.2 File 10-2
10.3 View 10-3
10.4 Index 10-4
10.4.1 Indexing Parameters for Werners algorithm (TREOR) 10-4
10.4.2 Indexing Parameters for Vissers algorithm (ITO) 10-6
10.4.3 Indexing Parameters for Lours algorithm (DICVOL) 10-7
10.4.4 Output from the indexing routines 10-10
10.5 Refine 10-11
11 Theoretical Pattern 11-1

11.2 File 11-2
11.2.1 Example CIF file 11-3
11.2.2 TIN file format 11-5
11.3 Setup 11-7
11.3.1 Crystal Parameters 11-8
11.3.2 Atom List 11-10
11.3.3 Pattern Parameters 11-12
11.3.4 Load from ICDD 11-14
11.4 View 11-15
12 Crystallinity 12-1
12.2 File 12-3
13 Size / Strain 13-1

13.2 File 13-3
13.3 View 13-4
13.4 Options 13-4
13.5 Output 13-5
14 System-Evaluation 14-1
14.2 The menu- and tool-bar 14-2
14.3 The Caption-Bar 14-5

14.4 The Operation Bar 14-5
14.5 The Display Window 14-10
14.6 The Report Bar 14-12
14.7 Example for Processing Data 14-14
14.8 Preference Dialog 14-15

1. General
1.1 Introduction
1.1.1 General Remarks

The WinXPOW Program Package is a true 32 bit Windows application with all the benefits of the graphical user
interface of Microsoft Windows 2000, Windows XP and Windows 7. This manual cannot explain how to use Windows,
so the user should be familiar with its basic operations.
1.1.2 Input Elements

When the program is started, the main menu bar is presented to the user. The menus can be selected by a mouse
click on the menu text, or by pressing ALT followed by the underlined letter (hotkey) on the keyboard. In most cases a
drop-down menu with more selections will be opened. When a shortcut key exists for a menu item, this is indicated.
The menu items can behave in different ways :
Selections that can be turned on and off. When turned on, a check mark is displayed.
Items take effect as soon as selected.
Items requiring further information, which is usually obtained through dialog boxes. This is indicated by an ellipsis
( ... ) following the menu item text.
The WinXPOW programs use three different kinds of dialog boxes :
1. Common dialog boxes supplied by Windows ( Open File, Save File as ... ) which are used in almost all Windows
applications with the same design and input elements ( selection of drive, directory and file names ). Because they
are supplied by the users version of Windows, their input elements will be named in the language used by
Windows. WinXPOW uses only English names, so it is possible that two different languages are used in the same
dialog box ! For file operations, WinXPOW makes use of the convention that the default directory for output files is
the same as the directory of the corresponding input files.
2. Dialog boxes where parameters can be entered. Here the user is confronted with the full variety of input elements
available under Windows :
Edit fields Fields containing text or numerical values with full editing functionality
Radiobuttons Represent a single choice in a set of mutually exclusive choices
Checkboxes Options which can be turned on or off
List boxes Display choices or results
Pushbuttons Buttons which initiate an action
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WinX 3.05 Software Manual - General 1-1
Many of the list boxes allow selection of more than one entry. To select multiple entries, use the mouse together
with the SHIFT or CTRL keys, as for example in the Windows file manager.
The Enter key is used differently as compared with other Windows applications. When Enter is pressed after
modification of a parameter value, other fields depending on that parameter will be updated. Sometimes it is also
used to start an action. As will be seen later, this behaviour simplifies program handling.
These boxes provide two buttons for exit ( Okay and Cancel ), another possibility is the ESC key or Close from
the top right corner of the box; both are equivalent to Cancel.
Only when the Okay button is pressed, the new set of parameters will be stored, whereas the Cancel button
causes all changes to be ignored.
3. Dialog boxes which also provide diffractometer operations in addition to the previous type. Common to all is the
following set of buttons.
The Start button will start the operation ( Scan, Data collection ), all other buttons except Stop will then be
disabled until it is finished. With the Stop button the current operation will be stopped immediately. Finally Exit
closes the dialog box and returns to the previous menu or dialog box. When parameters related to the procedure
have been modified, they will be updated as soon as Start is selected.
For convenient viewing and printing of text files which have been created by WinXPOW, the utilitiy Textview is
supplied.
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1.2 Installation
The WinXPOW package comes with an installer application. The installer should be used to install the WinXPOW
package or perform an upgrade of an existing installation. You must have 'Administrator' privileges for running the
installer application. It is strongly recommended to close all other programs during the installation process. Especially
any running program from an older WinXPOW version must be closed, otherwise the upgrade may fail!
Start the installer application by double clicking on the WinXPOW_3.00_Setup.exe icon. The installer wil open and
shows a welcome screen. Press the Next > button to proceed.
The installer will present the software license. To proceed with the installation you must accept the license
agreement. Press the Next > button to proceed.
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On the next screen the installer will show you the location where the software will be installed. Usually you should
accept the default location and never change it. Press the Next > button to proceed.
Now the installer will copy all files onto the computer and perform all necessary setup steps.
If no error occurred during installation the installer will present a last page. By pressing the Finish button you leave
the installer.
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If you have installed WinXPOW for the first time on the computer the license file stadip.lic must be manually
copied to the WinXPOW setup folder ( as described on the last installer page ) before using the software.
When performing an update the installer will not change any existing setup- , instrument- and user files. Nevertheless
it will save all previous WinXPOW programs into a new folder called programs_before_x.xx ( with x.xx equal to the
installed version ).
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1.3 The Main Menu
The available items of the main menu are shortly described here. Each item consists of a group of related functions
and will be discussed in detail in the following chapters.
User is used to select the users parameter file.

Diffract1 and Diffract2 comprise routines for setting up an instrument parameter file, collecting raw data,
controlling a diffractometer, and calibrating PSDs for up to two separate diffractometers controlled from one
computer.
Raw Data is used for handling and displaying of raw data, format conversion, peak picking, profile fitting and
evaluation of internal standards.
Cell contains a collection of routines that index powder patterns, refine lattice constants, or generate patterns
from user input.
Phase Analysis comprises the (optional) phase identification routine, which is also conveniently used for
browsing through the ICDD data base, and a module to calculate crystallinity indices of partly crystalline samples.
'Extras' contains a viewing tool for ASCII files, a particle-size analysis routine and an (optional) reflectometry
evaluation program.
Help provides information about the program and on-line help texts.
Exit is not a menu item on its own, but is available through the User menu item, as in most Windows applications. A
shortcut keystroke for exit is ALT + F4. The third possibility to exit is to select the Close command from the Control
Menu ( in the top left corner of the window ).
The Change Directory button is used to change the default directory for file input/output operations.
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1.4 User
The user parameter files can be handled in the option User. It is good practice to assign every user working on a
given computer his own user file where default values, file names etc. are continuously updated. The user files may,
alternatively, also be associated with certain projects or sample types.
Select User opens a dialog box with the names of all user files in the system. The eight most recently used user
files can also be selected from the recent file list.
New User is used to create new user file entries.
Login, Logout, User Management are functions used by the WinXPOW GMP-package and are described in a
separate manual.
Exit terminates the WinXPOW program package. This is possible after all WinXPOW programes had been closed.
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2 Instrument Parameters
2.1 Introduction
Instrument Parameters defines the diffractometer system in terms of available options, hardware settings, serial
line and USB definitions and all other relevant information. The type of diffractometer used is displayed in the title bar.
File contains the options New ( which is only enabled if no existing instrument parameter file has been found ) and
Exit.
Configuration is used to input parameter settings via six property sheets, Configuration, Hardware, ,Ranges,
Generator, SPC (sample position control), and HTC (high temperature control).
PSD settings change the parameters of position sensitive detectors (PSDs) and their counting electronics via the
property sheets Interface, Linear PSD, Curved PSD, in case of an image plate detector ,IP-PSD and in case of the
Mythen 1k detector Mythen 1k.
Defaults allows the user to define default data collection parameters.
WinXPOW 3.05 Software Manual Instrument Parameters 2-1

2.2 Configuration
The Configuration property sheet offers combo boxes and check boxes to define all available parts of the
diffractometer system.
The syntax of all serial port definitions must be COMx : baudrate, data bits, parity.
The baudrate should always be left at 9600 as all STOE interfaces have this baud rate set ex factory. Data bits
are 8 for all generator and diffractometer types and 7 for the high-temperature and sample position
controllers. Parity is N for all generators and diffractometers, E for the high temperature controller and O for
all types of sample position -, slit system - or monochromator angle - controllers.
The property sheet defines the basic setup of the diffractometer (e.g. radiation type used) as well as available options
like high-temperature stage or sample changer which might be mounted on the system. As far as detectors are
concerned, the principal availability of PSDs or scintillation counter is input here, not the current setup. Temperature
attachments, sample position control and sample changer exclude each other from being used. These options have
therefore to be input according to the current diffractometer setup.

In the Hardware property sheet the installation parameters of the respective hardware setup of the system are
defined. Only fields referring to options defined
as part of the system in the Configuration
property sheet are enabled.
Dead time of Sci.Counter refers to the dead

time correction of the Scintillation Counter. If a
non zero value is provide the measured
intensities will be corrected as : I = I / ( 1 I * c).
( with I = estimated intensity, I = measured
intensity, c = correction factor ).
Sample changer position defines the position
of the sample holder, and therefore the position
of the omega circle, when changing a sample
with the transmission sample changer.
The distance values describes the geometry of
the diffractometers beam path.

The Ranges property sheet offers edit fields to define the maximum permissible angular positions, the positions of
the reference marks and the check box for the
reflection mode. Again only fields referring to
options defined as part of the system in the
Configuration property sheet are enabled.
The Generator property sheet is used to define the tube ratings and if a PC-controlled generator like the Seifert ID
3003 is available the serial line definition. In the
example below, the COM settings are not
accessible as a generator with manual control
has been selected in the Configuration sheet.
The maximum tubes values should be carefully
edited according to the installed x-ray tube and
generator. Improper values will destroy the x-ray
tube and/or the generator! For appropriate values
please refer to operation manuals of the tube and
generator!

The SPC property sheet defines the resolution, moving speed and serial line definition of sample holders with
additional PC-driven translational, rotational or
tilting movement. Usually, no changing of the
stepping resolution or stepping speed will be
necessary as the default values correspond to
the hardware settings of the various attachments.
Incorrect setting of the Steps parameter will lead
to wildly incorrect positioning of the motors while
incorrect Speed settings will result in loss of
reproducibility.
The HTC property sheet defines the controller type, serial line definition, PID parameters, thermocouple type, and the
maximum permissible temperature and ramp rate
of a high temperature attachment. Care should
be taken when changing any of these parameters
because an incorrect setting will invalidate all
software precautions against inappropriate user
input and might result in damage to the high
temperature chamber.
In case of nonlinear characteristics of the

temperature the run of the temperature curve can
be corrected by a Calibration file (see chapter
4.2. HTC Configuration). In the example below,
the PID values are good standard values for the
thermocouple S. If a thermocouple K (NiCr/Ni) is
installed, 300 / 8 / 1 for Proportional band /
Integral Time / Derivative Time are a better
choice.

2.3 PSD settings
The PSD settings comprise the definition of the interface type between controlling computer and counting electronics
and the parameters for the PSDs defined as part of the system in the Configuration sheet.
If a wire PSD (curved or linear) is installed, the Interface sheet is used to define the type of connection between PSD
counting electronics and computer.
The interface type PDT-ISA has to be selected for all compact PSD supply units delivered after November 1994
bearing the STOE logo on its front panel, which are connected to the controlling computer by a thick black cable
conduit containing two small cables with green and orange plugs and a ribbon cable. Compact PSD supply units
delivered after April 2004 normally contain additional USB inserts which establish the connection between the PSD
electronics and the computer by an USB cable. Compact ETH supply units delivered after July 2010 are connected
via Ethernet cable.
The (hexadecimal) base address for the parallel board and the (decimal) USB Identifier must correspond to the dip
switch settings in the hardware, respectively (see the PSD hardware manual for the dip switch coding). Default values
for PDT-ISA interfaces are 0x310. In case of USB interfaces the respective identifier number of the insert in the PSD
electronics has to be chosen. In case of the ETH interfaces the switch settings (Switch 1 and 2) must be chosen to
match the position of the switches 1 and 2 in the interface. Using these switches the user can choose between 4
different IP addresses for the interface: 10.0.2.128 (switch 1 and 2 are both off, standard case), 10.0.2.129 (switch 1
is on, switch 2 is off), 192.168.2.128 (switch 1 is off, switch 2 is on), 192.168.2.129 (switch 1 and 2 are both on).

The PSD sheet contains the Calibration settings which show the date of the last PSD calibration evaluated and
written to the instrument parameter file. The calibration file name of the currently active calibration is also given. The
radio buttons beneath are used to switch off and on the use of the calibration curve during data collection and should
always be set to Yes and Address, respectively. Changing these settings should only be done for good reasons as
correct peak positions and intensities can only be obtained when both corrections are active. The View button
opens a diagram showing the calibration curves stored in the instrument parameter file.
First Channel and Last Channel define the actual address range which is used when collecting data with the PSD
and, therefore, the active angular range of the PSD. The PSD Stepsize is the increment in 2 between two adjacent
channels (defaults : 0.005 for the linear PSD and 0.015 for the curved PSD).
Angular range ( 2 ) = ( Last Channel First Channel ) * PSD stepsize ( 2 / channel )
Running the PSD calibration routine and updating the instrument parameter file will update the values for the first and
last channel used according to the values selected in the PSD calibration routine (see chapter PSD Calibration).
TAC, Delay, TDC Resol., and HV refer to electronic settings of the PDT counting electronics. These values are a
characteristic of every PSD / counting electronics pair and should not be changed from their factory settings without a
very good reason. In any case, a PSD calibration has to be performed when any of these values has been changed.
The default values for the PSD high voltage ( = HV ) is for an linear PSD 4800, respectively 5200 for PSDs delivered
after Nov. 2009, and 4300 for a curved PSD. The TAC range is usually between 3200 and 3800 for the linear PSD,
and between 2300 and 2700 for the curved PSD. When using a ETH counting electronic the TAC must be set to 173.
The delay value is in the range 110-150 for the linear PSD and 150-200 for the curved PSD. The setting TDC Resol.
is only relevant for an ETH counting electronic. When operating a linear PSD with a ETH counting electronic the TAC
value is 173 and it should not be changed or used to calibrate the PSD. Instead the TDC Resolution value has to be
adjusted. Normal values are 10300 to 10900 for 230 mm sample-detector distances, or 7400 to 7700 for 330 mm.
When operating an ETH interface and beginning with version 3.04 of WinXPOW, the user must also provide the
Firmware Version and the Module number of the ETH interface.

If an image plate PSD is installed, the IP-PSD sheet contains the Calibration settings, some electrical hardware
settings, and the type of the IP-PSD.
For a 140 IP-PSD IP-PSD large has to be chosen, (ver. 1) refers to detectors with tooth belt ( manufacted before
March 2004 ), while (ver. 2) refers to newer detectors with flat belt. When operating an 80 IP-PSD IP-PSD small
has to be chosen.
The activation of the Inverse Scan option is only necessary when operating certain STADI-MP setups.
If a calibration has been performed the Calibration settings show the date of the last calibration evaluated and
written to the instrument parameter file. The calibration file name of the currently active calibration is also given. The
check box 2Theta correction is used to switch off and on the use of the calibration during data collection and should
always be marked when an up-to-date calibration file is given.
Samplingrate, Triggerposition, and Scanrange refer to electronic settings of the IP-PSD. These values are a
characteristic of every IP-PSD / counting electronics pair and should not be changed from their factory settings
without a very good reason. When a IP-PSD calibration is used, it has to be performed in any case when any of these
values has been changed. The default values for the Samplingrate are between 970 and 990. The value for the
Triggerposition is usually between 30 and 40 for the small IP-PSD, and between 60 and 70 for the large IP-PSD
(given in degrees 2theta).
Samplingrate and Triggerposition are normally valid for every 2theta position of the detector. In contrast, when
measuring on different positions, a separate calibration file should be recorded for every position of the IP-PSD thus
avoiding small deviations in 2theta.
The Scanrange is the maximum angular range ( detector internal 2 ) which is simultaneously detected by the IP-
PSD.
If a Mythen detector is installed, the Mythen 1k property tab contains the Calibration settings, options and hardware
settings for this detector. The Calibration settings are identical to those already described for wire linear PSD: the
user should read the corresponding documentation. It should only be mentioned here, that by pressing the View
button a diagram appears showing the calibration curves stored in the instrument parameter file and the MIP of the

Mythen detector used to measure the calibrations. If the MIP shown are all zero (uninitialized), the calibrations were
measured with a version of WinXPOW earlier than 3.04.
First Channel and Last Channel define the actual address range which is used when collecting data with the
Mythen 1K detector and, therefore, the active angular range of the detector. The PSD Stepsize is the increment in
2theta between two adjacent channels (defaults : 0.01).
Angular range ( 2 ) = ( Last Channel First Channel ) * PSD stepsize ( 2 / channel )
Performing a Mythen 1K calibration and updating the instrument parameter file will update the values for the first and
last channel used according to the values selected during the calibration (see chapter PSD Calibration).
The Address setting tells the measuring programs PSDCal and PowDat at which address should the Mythen
detector be contacted: this is normally set to Address 0 unless Mythen has been predefined with Address 1.
The activation of the Inverse Scan option is only necessary when operating certain STADI-MP setups.
The Use default keV threshold option is normally activated and corresponds to threshold value about half of the
energy of the anode radiation (the exact value depends on the internal calibration of the detector): photons having
energies less than this threshold are not counted. To suppress fluorescence, the user might deactivate this options
and specify a new value for the threshold in keV up to a maximum of 65.5 keV accordingly to his special needs.
Starting with version 3.04 of WinXPOW, the user must also provide Firmware Version and Module number of the
specific Mythen system he wants to connect to using the button Change Mythen1K Identification Parameters. If the
Mythen system has Firmware Version lower than M2.0.0 (like M1.3.0) also the DCS-MAC Address of the Detector
Controlling System must be given. Values for DCS-MAC and Module number must be taken from the System
Information Sheet which is delivered with all Mythen systems: the DCS-MAC is highlighted in red and the Module
number in blue. During start-up PSDCal and PowDat check that the Mythen Identification Parameters given in input
by the user correspond to those queried from the Mythen Hardware and refuse to activate the detector if they differ.
Changes of the Mythen Identification Parameters or Mythen Settings cause entries to be written in GMP Log file.

2.4 Defaults
This dialog box is intended for the setup of a standard data collection procedure which will be used for the creation of
the raw data file if no raw data file is opened by the user after starting the Diffractometer Control module.
The edit and list boxes contain a short version of the Scan Mode and Edit Ranges parameter input tools of the
Diffractometer Control program. Please refer to the Diffractometer Control manual, chapter Edit Ranges for a
detailed description of these input windows.

3 Diffractometer Control /
PSD Calibration
3.1 Introduction
The Diffractometer Control module is used for all diffractometer operations like data collection, PSD calibration,
alignment etc. with the exception of high-temperature data collection which is a separate program. The PSD
calibration program is an individual program started directly from the MainMenu.
The WinXPOW MainMenu allows communication with two different diffractometer systems from one computer at the
same time. If more than one diffractometer is active in the menu bar, select the one you wish to use Diffract.1 or
Diffract.2 and start Diffractometer Control.
The program then checks the necessary communication lines to the diffractometer and detectors and displays an
error message if communication could not be established. In this case, the user should check whether the appropriate
system components are switched on and if the communication cables are connected properly to the computer and
system interfaces.
WinXPOW 3.05 Software Manual Diffractometer Control 3-1

When the initial check has been completed, the program displays the current instrument parameters in the lower
splitter window. A raw data file should always be created if data collection is to be performed, otherwise collected
data may be lost if all warnings are ignored by the user. For low-level-diffractometer commands like driving the circles
or doing a step scan, a raw data file name need not to be given.
3.2 File
3.2.1 New
To create a new raw data file the option New is used. This file will be created in the folder determined by the user
directory and receive default scan mode and range settings. The user may then alter the file settings according to his
wishes, and rename it after that by the option Save As....
3.2.2 Open
To load an existing raw data file, option Open is used. This is indicated when data collection parameters for a new
measurement shall be copied from an existing raw data file. For that purpose, this existing raw data file should be
opened and then written to the new file name using the option Save as.... Raw data subsequently collected will then
be stored in the new file. When an existing raw data file actually contains measured data a warning will be displayed
in case the user tries to overwrite these data by initializing data collection again.
After the raw data file has been created with the option New or loaded with the option Open, the main window
displays the fundamental settings of this file like diffractometer type, radiation and detector used. If the file has been
created on quite another instrument, with another wavelength, or with other fundamental parameters differing from
the current setup, the error message This file cannot be used with the current instrument configuration is displayed
and a new raw data file should be created or the system configuration changed accordingly.
3.2.3 Save
During data collection, data are saved automatically to the raw data file. However, if some scan ranges have been
changed in a file and no data collection started yet, it may be useful to store the changes done so far to the raw data
file. This can be done using the option Save.
3.2.4 Save As
The Save As option is useful for copying all relevant file information including scan range parameters to another
file, either new or old. Data collection settings can thus be used for several files without the need of typing them in
every time a new file is created. If the currently loaded file contains collected data, these data are not copied to the
new file.

3.2.5 Print
This option prints the most recently collected powder diagram displayed in the upper splitter window, after the user
has defined the print options in the standard Windows Print box.
3.2.6 Print Preview
opens a Windows standard WYSIWYG window of the printout.
3.2.7 Print Setup
opens a Windows standard printer setup window.
3.2.8 Most Recent File List
contains the names of the eight most recently used file names.
3.2.9 Exit
returns to the WinXPOW main menu. If parameters have been edited by the user, but not stored yet, the user is
prompted whether he wants to update the current file or not.

3.3 Setup
3.3.1 Detector
If more than one kind of detector is defined in the instrument parameter file, the user may switch from one detector to
the other using this option after replacing the detector on the diffractometers 2Theta arm. Only those detectors are
accessible for selection which have been defined in the Instrument Parameters Configuration sheet. If two kinds of
PSD are connected to a PDT type of PSD interface, all changes relating to electronic and HV settings are executed
automatically. When the user attempts to switch to a Mythen 1K detector, the Mythen Identification Parameters (MIP)
given in Instpar with the Change Mythen1K Identification Parameters button are compared with the values queried
directly from the Mythen hardware and the detector switch is going to fail if they differ (the detector is therefore not
available for usage). After a successful detector initialization, the program also compares the MIP in the calibration
(see PSD Calibration) with the MIP queried from the Mythen Hardware. Under GMP, the Mythen detector is made
available for usage only if the two MIP sets are identical (therefore the calibration was measured with the same
system presently connected). In non-GMP environments other situations are also allowed: the program warns the
user that a mismatch between MIP was detected and expects the user to explicitly allow or forbid the activation of the
detector.
3.3.2 Generator
The dialog box which is opened after selecting this option serves a twofold purpose : The first is to document the
generator settings in the raw data file for comparison reasons. The second requires a generator with an interface to
the computer so that the generator settings entered can be transferred to the generator and set accordingly.
The edit boxes kV and mA and the Exit button are always accessible, even if a manual type of generator is part of
the system.
In case of a computer-controlled generator, additional buttons and an additional check box are activated :
Set kV, mA sets the generator to the ratings given in the kV and mA boxes.
Shutdown switches the high voltage to 20 kV and the current to 5 mA as the lower power limit for tube idling.
If the Shutdown at the end of data collection box is checked, the generator is automatically set to minimum power
(20 kV, 5 mA) every time a data collection has been completed. This feature is useful for runs overnight or over
weekends, if data collection stops sometime in the middle of the night and there is no need to run the tube at full
power until its settings are decreased by the user.

3.3.3 Sample Changer
This option is only activated when a sample changer has been defined as part of the system in the Instrument
Parameters Configuration sheet. When Enabled is selected, all requests for a new sample issued by the program
will be sent to the sample changer. This is the normal operation mode. For testing purposes the sample changer may
be Disabled and the user will be prompted to insert a new sample manually every time the program requires one.
3.3.4 Title / Comment
This option opens an input window for the definition of a file title and additional comments. This information may also
be input just before the data collection is started (see chapter 3.6.1)
3.3.5 Options
A dialog is opened with several property sheets where some several aspects of the program could be edited.
The Common property sheet contains two options : if the

network option is enabled and the file that will contain the
measured data is located on a network drive, the measured
data will be stored first on a local drive and copied after the
successfully completed measurement to the designated file
location. This option could be used to prevent a break of the
data collection resulting from instable or slow networks.
local path holds the path on the local computer where the
measured data should be stored temporarily.
The option erasing IP-PSD could be used when

accomplishing HTC measurements using very long time
spans for temperature stabilisation or tempering steps. The
long time spans between two measurements, and therefore
erasure cycles, may result in an increase of the detectors
background. When editing a non zero value the IP-PSD
detector will be erased before a new measurement if it wasnt
erased before in the given time span.

The After Measurement sheet contains actions to be done after a measurement was successfully finished. If the
option print diagram after measurement is activated the
measured data will be print out on the local default printer.
The execute script option allows executing an external
script (i.e. batch file, Visual Basic script) or external program
after each measured file.
Script parameters holds, if needed, the parameters for the
script. The user can either provide literal parameters as well
as certain macros. While the literal parameters will be left
unchanged when calling the script, the macros will be
substitute with the current values from the running
measurement.
The macros $FILEPATH and $FILENAME will be substitute
with the file path and file name of the currently measured
data file, while $USERNAME will be substitute with the
name of the current user.
For example, if the path of the currently measured file is
D:\Data\D356.raw, the parameter line /U $FILEPATH
will be translated to /U D:\Data\D356.raw. Analogous
/U $FILENAME will result in /U D356.raw
By activating the option wait for script termination the
next measurement will not be executed until the script has terminated. It should be avoided that the script asks for
user input, since this will block further measurements if the whole measurement is running unattended.
The Tasklist Setup sheet is described in in chapter 3.5.3 Scan Usage.
The Printing Setup sheet is used to define some aspect of printing. When choosing output file header info the
diagram will be printed together with all data collection
parameters at the bottom. With frame Pen Width the user
can control the thickness of the frame surrounding the data
and header info. With Date format and Time format the
user can control the output of the current date and time
which will be printed if not suppressed by choosing no
output - in the upper right area of the surrounding frame. By
clicking the Defaults button the options will be reset to
default values.

3.4 Diffractometer
3.4.1 Open Shutter
While the shutter is always automatically opened when data are collected, this option is used to open the shutter for
alignment purposes. The shutter status window in the programs lower splitter window is changed accordingly.
Note : There is no feedback from the diffractometers safety circuit to the computer. It may well be that the shutter is
shown as open on the monitor while the safety circuit has closed the shutter due to open panels or the like.
3.4.2 Close Shutter
Selecting this option closes the shutter. When a data collection run has been finished or when the users exits the
program, the shutter is closed automatically.
3.4.3 Drive Circles
All commands relating to circle movement (without data collection) are accessible from the dialog box which is
opened when this option is selected.
Drive Mode defines the relation between 2Theta and Omega positions : When Coupled is selected, only one
value for 2Theta needs to be entered in the Move to edit box, Omega will be set to half this
value. When Independent is selected, values for 2Theta and Omega need to be entered; if only
one value is given, Omega will remain at its current position.

Requested Pos. is displayed in the edit box where the angular positions for 2Theta and Omega may be entered.
Current Position is displayed below the requested position and shows the current positions of both circles.
Synchronize is an important procedure when the diffractometer interface has been switched off. After switching
on again, position information is lost and all circles are reset to 0. The Synchronize command
drives both the 2Theta and Omega circles to mechanical reference marks defined by micro
switches and encoder marks and assigns values stored in the instrument parameter file
(Instrument Parameters : Ranges sheet : 2Th, Omg (Ref) ) to these positions.
Note : The program requests the user to drive both circles manually to positions physically above
the reference marks as both circles begin to move in negative direction until the appropriate
microswitch is depressed; if one of the circles is positioned below this position, the circle will move
into the low-angle limit switch and the program will stall.
Check Positions performs movement similar to the Synchronize command but also compares the expected
(=stored) reference position to the actual position. If they are not identical, the stored reference
position is assigned to the current position and a warning message appears.
Define as allows the user to correct zero position errors induced by small changes of the primary beam. The
positions entered in the Requested Position edit box will be assigned to the current positions
thus changing the zero position of the circles.
Usually a standard peak of known position is scanned at regular intervals (e.g. every week using
the Step Scan option) and the peak maximum determined in this way is then re-defined to its
theoretical value. The program also automatically updates the current detectors reference marks
so that the next Synchronize command executed will locate the correct circle positions.
Move to executes the command to move 2Theta and Omega to the positions defined in the Move to edit
box. The same effect can be achieved when the enter key is hit in the Requested Position edit
box.
Viewing Position drives the 2Theta arm to a position which allows the user to mount the microscope and to have
easy access to the sample stage for aligning purposes. The viewing position depends on the kind
of detector currently in use.
Stop interrupts the movement of circles at once. The button is only active while circles are moving.
Exit closes the dialog box.
3.4.4 Set Slit Width
opens a dialog box with edit boxes for the width of the automated divergence and receiving slits. If no automated slit
system is defined in the instrument parameter file, this option is disabled.
Receiving Slit is the width of the slit in front of the detector in mm. The edit box is used to input the requested
setting, the greyed box labelled Current shows the current opening.
Divergence Slit is the width of the slit between tube and sample in mm. The edit box is used to input the
requested setting, the greyed box labelled Current shows the current opening. The permissible
range for both slits is 0 to 2 mm. There is a mutual influence between the setting of this
parameter and the next three parameters. Every time any of these four parameters is changed
and the enter key pressed, the other edit boxes are updated accordingly.
Divergence Angle allows the input of a certain opening angle from which the width in mm is calculated by the
program.
Sample Area is the width of the primary beam intercepting the sample in mm and thus the irradiated width of
the sample. For a given slit width (and divergence angle) it depends on the angle between
sample surface and primary beam, Omega.

at Omega is the incidence angle for which the sample area is calculated from the slit setting (or vice
versa).
Set Slit starts the movement of both slit systems to their respective requested positions.
Home finds the reference marks of both slit systems and is useful to restart the slit controller if slit limit
switches have been activated.
Define as allows the user to re-define the current slit widths as the requested widths. This will also change the
values of the slits home positions accordingly.
Stop interrupts slit movement immediately.
3.4.5 Sample Changer (Next Sample)
This option opens a dialog with commands for operating the sample changer. If no sample changer is defined in the
instrument parameter file, this option is disabled.

next sample will remove the currently loaded sample from the measuring position and insert the next sample.
Reset will reset the internal counter to the first sample.
Goto is disabled for a transmission sample holder as it is shown in the example above. For other sample
changers, this button is used to move a definite sample directly to its measuring position.
Calibrate opens a dialog box where the user is allowed to re-define the positions of the sample changer. This
is an option a transmission sample holder cannot execute and is therefore also disabled in the
example above.
When calibrating a High Throughput sample stage, the user is allowed to change its position either
using relative values for the moving distances, or absolute values defining the absolute position (the
corresponding box has to be checked for that purpose). All buttons are the same as described in
the following chapter 3.4.6.
Stop interrupts sample changer movement.
Done closes the dialog box.
3.4.6 Sample Position
This option opens a dialog box with edit boxes for the positions of an automated sample holder. If no sample position
control is defined in the instrument parameter file, this option is disabled.
The layout of the dialog box depends on the type of the automated sample holder defined in the Instrument
Parameters. The example below is for a High Throughput sample stage with two independent movements,
translation x and translation y.
The edit boxes are used to input the requested positions of both motors, the greyed boxes beneath show their
respective current values.
Move to starts the movement of the sample stage to the requested position in x and y.
(search) Home is used to find the reference marks which locate a defined position even after switching off the
controller of the High Throughput sample stage.
Spin is an option the High Throughput sample stage cannot execute. For other sample holders, it is
used to start continuous rotation about a movable axis.
Define As allows the user to re-define the current positions as the requested ones. This will also change the
values of the home positions of the translational movements accordingly.

Stop interrupts motor movement immediately.
Exit (Done) closes the dialog box.
3.4.7 Erase IP-PSD
Selecting this option erases the IP-PSD when installed. This is normally not necessary to execute manually because
after a data collection run recorded with an IP-PSD has been finished the detector is erased automatically.

3.5 Ranges
3.5.1 Scan Mode
The number of accessible input elements in the Scan Mode dialog box is strongly influenced by the diffractometer
and detector type in use. Seen below is an example for a transmission diffractometer with linear PSD.
Scan Mode relates to the type of sample holder which is used. It influences the movement of the circles
during measurement in the following way :
Transmission and Reflection mode usually keep a constant 2:1 ratio between 2Theta and
Omega position (the exact relation is however defined with the Scan Type edit box described
below); Debye-Scherrer keeps Omega constant at 0 for every 2Theta. If the Reflection mode
is set on a transmission diffractometer, a constant offset of 90 is added to Omega to account
for the different orientations of sample surface relative to the primary beam in transmission and
reflection geometry.
Note : The 90 offset for Reflection scans is taken into account for all commands in
the Measure pull-down menu, but not for the Drive commands which refer to
the true physical circle positions. Likewise, the angle display in the status
window always shows the physical position of the circles !
With Bragg-Brentano- and Theta-Theta-diffractometers, the only possible scan mode is
Reflection.
Scan Type This list box is only activated if Scan Mode is not set to Debye-Scherrer. Its setting overrides
the default scan modes for Transmission and Reflection explained above.
2Theta defines a scan with moving counter, but Omega kept constant at a user-defined value.
Omega is a scan with fixed detector position and moving Omega ( rocking curve ) which may
only be selected if a scintillation counter is used. Oscillating the well plate of a High Throughput
sample stage during the measurement can be performed by checking the box Oscillate Wells.

2Theta : Omega invokes the normal 2:1 coupling between 2Theta and Omega positions during
the scan.
Independent lets the user define 2Theta and Omega movements independently from each
other; e.g. a certain Omega-offset and/or a 1:1 ratio between 2Theta and Omega step width
may be entered in the Edit Ranges dialog box.
PSD Mode can only be changed between Stationary and Moving if a linear PSD is the current detector.
Stationary are all scans which require less than four PSD positions to scan the selected 2Theta
range. Moving is the usual PSD mode for the linear PSD if a complete powder diagram is to be
collected.
Omega Mode is only activated if a PSD is selected as current detector. Fixed means that for every PSD
position Omega will be driven to 2Theta divided by 2 and will remain there for all the measuring
time of this PSD step. Moving Omega means that the Omega circle is continuously moved
during data collection which usually requires longer step times and thus should only be used if
additional particle randomization is required. Gandolfi is only used when the corresponding
sample holder is mounted and Debye-Scherrer is chosen for the Scan Mode.
Oscillate Wells can only be activated when a High Throughput sample stage is mounted and a continuously
movement of the well plate during the measurement is requested. By checking this box, the well
plate performs a moving in the Omega range between 5 and+5 (Omega Mode has to be
switched to Moving).
Points to be added is only activated for a PSD as current detector. This option is useful to gain intensity at the
expense of data resolution. When two addresses of the PSD ADC (analog-digital-converter) are
summed up to one data point in the raw data file, the nominal step width of data points is
doubled and the intensity per data point is approximately doubled, too. For very badly diffracting
samples this value may be increased up to a point where the nominal data step width is about a
third of the expected peak halfwidths.
Corrections displays the kind of raw data correction which will be applied to the scan. For information on
how to change the kind of raw data correction please refer to the chapter Instrument
Parameters.
If a scintillation counter is the current detector, the only possible correction is Dead time which
will only affect intensities, not positions. If Dead time in the Instrument Parameters Hardware
sheet is set to 0, no correction at all will be applied.
For PSDs, position and intensity corrections may be applied. For details, see the PSD
calibration part and the chapter Peak Calibration of this manual.
3.5.2 Scan Range(s)
This option is used to define scan ranges after the fundamental scan properties have been defined in Scan Mode.
The upper part of the dialog box which is opened after selection of the Scan Range(s) option shows the detailed
scan mode and detector as setup in the Scan Mode dialog box.
The list box shows the scan ranges currently defined. Every raw data file may contain a maximum of 8 scan ranges,
regardless whether they are identical or differ in certain parameters and regardless of the order in which they are to
be measured. Note that the fundamental parameters defined in Scan Mode are identical for all ranges.
With a range highlighted, one of the three first buttons below the list box may be pressed :
+ will copy the currently highlighted scan range after the last scan range. The user may then
alter the settings of the new scan range according to his wishes. When no range is present
at the beginning, a new scan range is created receiving default scan range settings.

- deletes the highlighted scan range from the list.
OK stores the changes before leaving the dialog box.
Cancel discards all changes and leaves the settings as they were before opening the dialog box.
By double clicking an range entry a dialog box will open allowing to edit the range parameters. The layout of the Edit
dialog box depends on the system configuration and the Scan Mode settings. Below is an example for a
transmission diffractometer with linear PSD in Moving PSD- and 2Theta:Omega scan mode.
For systems without automated slits or with a PSD, the edit boxes in the last row are disabled and the user may only
input the 2Theta range, stepwidth and dwell time per step. If a scintillation counter is used for data collection, a dwell
time of 0 may be input. In this case, a continuous scan with hardware-fixed speed will be performed.

When automated slits are used on a Theta-Theta-diffractometer, the user may input the (fixed) receiving slit width in
mm in the edit box Rec. Slit.
The width of the divergence slit may be input in either of two ways :
When the divergence slit width is input in the Div.Slit edit box, the width remains constant during the scan.
Due to the variation of the angle between sample surface and primary beam the sample area irradiated by a beam of
fixed width decreases with increasing Omega. On the other hand, the penetration depth of the beam increases with
increasing Omega thus leading to a constant volume irradiation of the sample over the whole scan range (at least as
long as the projected beam size does not exceed the sample area).
When the divergence slit width is input in the Sample Area edit box, the slit width is automatically varied
over the scan range in such a way (~sin) that the irradiated sample area remains constant throughout the scan. The
input in the Sample Area is not the area itself, but the required width of the sample irradiation area (in mm). The
irradiated area is of course also influenced by the height of the beam which is defined by the choice of vertical
divergence slits and does not change with Omega.
3.5.3 Scan Usage
For all standard tasks Scan Usage is set to Single Sample and need not be changed.
If any other scan usage is selected, data will not be written to the master file filename.raw, but to a set of files named
filename.001, filename.002 etc. The extension of the first file may be selected by entering it in the First File number
edit box. The master file should however be kept after data collection has been completed as it provides a fast way of
accessing the whole set of adhering files in the 3DGraphics - routine.
One feature which is useful for monitoring changes in samples with time is the possibility to select Repetition as scan
usage. The program will then repeat all scan ranges defined in Edit Ranges as many times as input with a user-
defined waiting time between repetitions. When appropriate accessories for the diffractometer are defined as part of
the system in the instrument parameter file, scan usage may also be set to High-temp., Sample-pos. or the like. In
the case of Multi-sample runs using an automated sample changer, the box Individual Parameters may be checked
by the user which enables the Ranges, Files, ... button.
By pressing the Ranges, Files, ... button an input window is opened which allows the change of the default file titles,
comments, file names and scan ranges that the different samples will receive.

Sample may be any valid sample number ( 1, 2, 3 or A1, G5, H12 when using the high-throughput
samplechanger).
Range is only activated if more than 1 scan range has been created in the Edit Ranges window as described in
chapter 3.5.2. It provides the possibility to have different samples measured with different scan
parameters, i. e. in different scan ranges and with different scan times. The total number of possible
different scans is limited to the usual maximum number of ranges in a file, eight. In this case, setting up
requested scan ranges in the Edit Ranges box does not necessarily mean that all samples will be
collected in all these scan ranges. By selecting one of these ranges for an individual sample the
assignment of the scan range to be measured to the sample is achieved. If all ranges defined shall be
measured for a sample, a range number of 0 must be entered.
File may be any valid filename ( the extension .raw will be added by the program ). A double-check for already
existing files with the filenames input (which would be overwritten) will be done when pressing the OK
button.
Title By default, every file will receive the title given for the master file plus the identification sample x (x is the
sample number). This standard title may be changed by the user. If & is the first character in the title
given, the input string will be appended to the title defined for the master file (if necessary, suitably
truncated).
Comment The edited text will be insert into the comment field of the measured file. If & is the first character in the
comment given, the input string will be appended to the comment defined for the master file (if necessary,
suitably truncated).
Reset will assign the programs default values to all samples.
Reassign will change the sample number of every entry, so that the sample numbers starting with 1 and are
consecutive. This command may be usefull after editing a sample list for the transmission- or reflection
samplechanger, which could not change sample randomly.
OK will exit from the window after checking the current directory for existing files with filenames as changed by
the user.
Cancel will discard all changes and return to the Scan Usage window.
All values may be changed by double-clicking on the corresponding entry and confirming with the <Enter> key.
Additionally, measurements of single samples may be deleted by highlighting the corresponding line and pressing the
minus-button.

Another way to edit the data is to import them from a spreadsheet program with the Drag&Drop mechanism. The user
prepares a spreadsheet having as many rows as with Number of Samples specified and at least 4 columns
containing the samples index number, the range, the name of the RAW file and its title. The columns can be
arranged in any order and they can also be non-sequentially arranged.
To inform the program which column of the spreadsheet contains which information, the Setup / Options / Tasklist
setup property sheet is used.
By default the dialog box searches the sample index number in column A, the range in column B, the file name in
column C and the title in column D. But the user can also use a spreadsheet containing more columns and then
change the letters in the dialog box correspondingly.
The user can specify up to 4 columns as title by entering in the Tasklist setup / Title more than one character
labelling each column and separating them with commas (,) so that the entire title of the measurement is obtained by
joining the individual contents of the specified columns.
The following table for example contains an extra column (column C) that the program must ignore because it
contains only a comment and no data relevant for the measurement:
A B C D E
1 1 Comment1 File.001 Title1

This table can be processed using the following settings in the Tasklist setup dialog box:
Sample number A
Range B
Filename D
Title E, C
When the table is ready, the user simply selects all rows and columns of interest in the spreadsheet, copies them and
then right-clicks on the white area of the Individual Ranges / Files / Titles dialog box: a context menu appears
containing the command Paste that can be executed.
The content of the spreadsheet table will be transferred into the dialog box.

3.6 Measure
3.6.1 Data Collection
starts data collection after scan mode and scan ranges have been defined using the appropriate options in the
Ranges menu items pull-down menu. In the dialog box a title and a longer user text describing details of the sample
or the data collection may be entered.
By checking the Print data when finished box an automatic printout of the diagram on the standard system printer
may be invoked.
By pressing the OK button data collection is started which displays the ongoing measurement in the main window. If
the raw data file already contains measured data, the user will be prompted whether he really wants to overwrite
these.
Measuring with a linear PSD, the raw data file is automatically updated with counts after a certain time has elapsed.
Data which have already been saved to the file are displayed in blue, unsaved data in red. The Stop button of the
small info window may be used to interrupt data collection at any time. Red datapoints will in this case be lost, blue
datapoints will be kept in the raw data file.
When a IP-PSD is used for the measurement, data are shown at the end of the data collection due to the different
PSD technique using an image plate which is only read out completely after exposition.

3.6.2 Step Scan
This option is used for the alignment of the diffractometer and a quick check of peak positions. The collected data are
not stored in a raw data file, but only displayed on the screen.
The Scan Centre edit box is used to define the middle of the step scan to be undertaken. The first value corresponds
to 2Theta, the second to Omega. When Drive Mode in the Drive Circles dialog box is set to Coupled, Omega need
not be given; it is automatically set to 2Theta / 2.
Time defines the measuring time per detector step. For the scintillation counter, the total count time is therefore the
product of Time and Nsteps, for a PSD (which remains stationary during the scan) the total count time is equal to
the count time per step.
Depending on the detector in use, the Step Size edit box is either disabled (for PSDs) or enabled (for a scintillation
counter).
The NSteps edit box is used to define the number of steps the scintillation counter takes around the requested peak
position or to define the number of data points that are shown on the screen for a PSD.
After completion of the scan, the peaks centre of gravity, integral intensity and integral breadth are displayed and the
detector is moved to the position of the detected centre of gravity. If the scanned peak was a standard peak of known
position, the 2Theta angle may now be corrected using the Define as button.
The Start button starts the step scan after the scan parameters have been defined in the edit boxes.
Stop immediately interrupts the scan and is only activated while the scan is in progress.

3.6.3 Count
This option is only enabled when a scintillation counter is selected as detector. When clicking on this option, the
shutter is opened with both circles at their current positions and the monitored count rate is displayed numerically and
graphically on the screen. Data are not stored to the raw data file.
3.6.4 Beam Optimization
This option is enabled if a motorized primary monochromator has been defined as part of the system in the
Instrument Parameters routine. It performs the same measurement as the Step Scan option but moves the
monochromator in small steps during the beam optimization repeating the step scan with the monochromator angle
slightly changed. Thus, monitoring the peak intensity (proportional to the primary beam intensity with all other
parameters constant) changing with the monochromator position lets the program drive the monochromator to the
optimum angle leading to a maximum of beam intensity. Depending on the step time selected, this procedure may
take between 2 and 10 minutes.
The input boxes are the same as for the Step Scan option described in chapter 3.6.2 with the addition of the Check
Alpha1 checkbox. If this is checked, the program will not only look for the local intensity maximum, but will scan a
larger range of the monochromator angle with a coarser resolution making sure that the beam is K1 radiation and
not the closely spaced K2. When the K1 maximum has been identified by the program, the variation of peak
intensity with monochromator angle is displayed.

After that it automatically performs the optimization of the monochromator setting at this monochromator position with
the smaller normal monochromator step width.
The check box deactivate monochromator may be used to switch off the holding current which fixes the step motor
of the monochromator. When this box is checked, optimization of the monochromator can be done by hand as well.

3.6.5 Sample Position Measurement
The option Sample Position Measurement is a special scan mode for texture and crystal orientation problems. It only
works with a computer-controlled sample positioning device in combination with a scintillation counter, which is
moved to a user-defined 2theta position and remains at this position counting intensities while the sample is moved
through the primary beam. The Omega position is also kept at a fixed angle (independent of 2Theta) during the scan.
If several degrees of freedom are available from the sample stage used, the sequence of their movement is selected
from the 'Sequence' list box. The uppermost movement is executed in the innermost loop and is taken as the x-axis
for the on-line display during data collection.
The range for sample movement is given in mm for translations and in degrees for rotations. The 'Scan Mode' used
for the measurement is taken as entered in the appropriate dialog box (see 3.5.1).
The output file is an ASCII file with default extension *.spm containing a header describing important parameters of
the experiment and a table of the count rates at different sample positions :
! STOE SPM File : C:\winxpow\DATA\sijustiertx.spm

! created at 30-Oct-98 07:53 by WinXPOW
Wavelength : 1.54060 Cu
2Theta,Omega : 28.440 14.220
Time/Step : 1.0
Sample Pos.1 : -10.00 10.00 0.10 201 Translation X
Sample Pos.2 : 0.00 0.00 0.00 1 Translation Y
Sample Pos.3 : 0.00 0.00 0.00 1 Rotation (Phi)
DataPoints : 3 201
-10.00 0.00 0.00 4.0
-9.90 0.00 0.00 5.0
-9.80 0.00 0.00 3.0
-9.70 0.00 0.00 43.0
-9.60 0.00 0.00 188.0
-9.50 0.00 0.00 384.1
-9.40 0.00 0.00 460.2
-9.30 0.00 0.00 668.4
-9.20 0.00 0.00 954.9
-9.10 0.00 0.00 988.0 etc.

3.6.6 PSD Calibration
3.6.6.1 General
This option is not intended for data collection, but starts a necessary calibration procedure for wire PSDs and the
Mythen 1K detector. This procedure needs to be performed every few months and should only be done by qualified
personnel. To account for even the smallest deviations of the electronic address scale from the true 2Theta scale and
to determine the response function of each individual PSD, two standard samples NBS silicon and amorphous
metal foil of high iron content - are provided with every PSD which are used in this procedure.
PSD calibration comprises two procedures :
Calibration Curve : A sample of known lattice constants is placed in the sample holder and one of the peaks
(with precisely known peak position) is measured at different PSD positions so that the peak maximum is
measured at different electronic addresses. The difference between theoretical and observed peak position
is tabulated (together with the peaks integral intensity and halfwidth) for every address at which the peak
maximum was detected.
Address-Check : A sample giving no Bragg peaks but only high uniform background ( for Cu radiation,
amorphous iron foil) is measured with the PSD at a fixed 2Theta position. When the counting statistics are
good enough ( > 10000 counts in every address), the measured intensities in the usable address range
should all be equal within 1% statistical error. Deviations from the mean intensity value are thus due to
electronic bias or PSD-specific sensitivity differences over the length of the counting wire. Dividing the mean
intensity by each individual intensity thus provides an efficient address-wise intensity calibration by
multiplying every measured intensity in this address by this address-specific factor.
When selecting the option PSD Calibration, a program window opens up which offers several options in pull-down
menus. Many of them are well known from the diffractometer control window (see chapters 3.1 3.5).

3.6.6.2 PSD Calibration File
Parameters and results of the PSD calibration are stored in two files, one binary with the extension .cal for
calculations, and one in ASCII format of the same name but with the extension .lcl for later inspection and
documentation. It is good practise to give a new name to each calibration run and not to overwrite old files so that the
history of the PSD can be documented if necessary.
To create a new calibration file, option New is used. The default file name is noname.cal which is supplied by the
program. If a Mythen detector is selected as current detector, the Mythen Identification Parameters (MIP) described
under Instrument Parameters are copied also in the .cal file and printed in the lcl file. They are also displayed on
the main window of the program as Firmware version, mod (Module number both in decimal and hexadecimal
number format) and DCS-MAC.
Open opens an existing calibration file. If the opened .cal file was generated with a Mythen 1K detector system, the
program shows on the main window the Mythen Identification Parameters of the system used to measure the .cal
file. If the .cal file was generated with a version of WinXPOW earlier than 3.04, the MIP are zero, that is, uninitialized. If
a Mythen 1K detector is connected, the MIP contained in the .cal file are compared with those of the presently
connected Mythen 1K detector and, if they differ, the program might prevent the user from performing operations like
changing or adding calibrations (see 3.6.6.3) or writing the calibration to the IPR file for later use in PowDat (see
3.6.6.4).
Save can be used to store the calibration parameters and calibration curves. These are, however, also stored
automatically after calibration data have been measured.
Save As lets the user rename the calibration file. This should be done after a new calibration file is created and
before any changes to the parameters etc. are made or a calibration measurement is started.
Graphics Export is only activated when a calibration curve or an address check diagram has been evaluated. With
this option the user is allowed to save the displayed data in a graphic format.
Exit is intended to exit the PSD calibration routine.

3.6.6.3 PSD Calibration Measure
When both types of wire PSDs are installed, the user may select the one to calibrate with the option Detector.
Parameters opens a dialog box which allows the user to define the parameters for the calibration measurements:
Calibration Peak is the theoretical 2Theta value of the standard peak which shall be used for position calibration
( e. g. 28.443 for the Si(111) reflection using CuK1 radiation).
First PSD Address and
Last PSD Address define the (electronic) address range which shall be scanned during calibration. These values
can easily be obtained using the Measure - Address Check and Evaluate - Address Check
commands ( see chapters 6.4.4 and 6.4.5 ).
Measuring Time is the dwell time of the PSD at each position.
2Theta Interval is the step width by which the PSD is moved over the standard reflection. 0.1 is usually a
good choice for the linear PSD, 0.5 for the curved PSD.
Addr.Check Position is the position at which the PSD will collect data stationary (either using the amorphous
sample for intensity calibration or any sample for determining the first and last address for the
calibration measurement). For the linear PSD, every value between approx. 15 and 45 is
acceptable, the curved PSD should be positioned at 30 as the fluorescence background of
the iron sample is slightly angular dependent and is only constant in the aforementioned
2Theta range.
Omega Position is the fixed position of the sample during data collection (either using the amorphous sample
for intensity calibration or the sample for the calibration measurement). Using e. g.the Si(111)
reflection with CuK1 radiation, the value should be 14.221.
The options Calibration Curve and Address Check in the menu PSD Calibration Measure allow the user to
start the corresponding routine for the calibration of the PSD. If a Mythen 1K is selected as current detector, the user
can replace, measure again or add missing calibrations to a .cal file only if the MIP in .cal file exactly match the MIP
of the Mythen 1K system presently connected.

When Calibration Curve is chosen, a dialog box is opened, and the user is prompted to press the Start button.
After doing so, the program starts the calibration run displaying one measured peak after the other and listing the
observed peak positions, addresses of the peak centre, deviations from the expected position, intensities and
halfwidths. All these data are also automatically written to the calibration files (*.cal and *.lcl). By clicking on a list box
item, the profile of this particular measurement can be recalled to the screen. With the Stop (Measurement) button,
the run of the measurements may be terminated. Exit brings the user back to the PSD calibration menu (disabled
during measurement).
When Address Check is selected from the menu, the program will display the accumulated count rates in the main
window and continue collecting data until the user clicks on the Stop button.

3.6.6.4 PSD Calibration Evaluation
From this menu item either the Calibration Curve routine or the Address Check procedure can be evaluated.
Calibration curve will display the outcome of the calibration curve routine in two diagrams : the upper one showing
the variation of position offset with PSD address number, the lower one showing the variation of the standard peaks
integrated intensity. The user may select the useable address range either by clicking on one of the two red lines and
moving them to the desired position or by entering an address in one of the edit boxes of the Calibration dialog box.
The useable address range thus defined should show no spikes or drop-outs in either of the diagrams, but only a
smoothly varying curve. A smoothed cubic spline is fitted to the data points in the selected address range; the degree
of smoothing is again set by the user by moving the sliders to a position where the interpolated curve fits the
observed data well enough without showing too many sharp turns. In general, the smoothing for the position data in
the upper diagram will be smaller than for the intensity data which may be effected by poor counting statistics. No
point of the spline should be further than 0.005 (for the linear PSD) away from a data point.
Only the smoothed splines will be written to the instrument parameter file (see 6.4.6) and will thus be available for all
consecutive data collections, so the choice of address range and smoothing should be made with care.
Address Check will display the accumulated counts over the PSD addresses which have been collected with the
Measure - Address Check option. Again the user may select the useable address range either by moving the red
cursor lines or by entering the first and last address in the appropriate edit boxes.

At the end of the calibration procedure it is important to activate the stored files so that the corrections will be applied
to every measurement. This is done by selecting Write IPR file. Thus, the instrument parameter file will be updated
with the evaluated PSD calibration. If a calibration for the currently active PSD is already stored in the instrument
parameter file, a warning is given. Under GMP if one has chosen Mythen as current detector (Measure / Detector /
Mythen 1K is checked) and has opened an old .cal file also created by a Mythen system, the Write IPR file is
allowed only if the two systems have identical MIP (therefore they are the same system). In non-GMP environment
the program warns the user that a mismatch was detected and expects the user to decide whether the Write IPR file
operation should be completed or not.

4 High-Temperature Data
Collection
4.1 Introduction
The HTC Data Collection module is a separate program and controls the low- and high-temperature data collection.
It provides the set-up of the temperature program and data collection parameters and calls the normal data collection
module when executed. The module is, among others, capable of controlling STOEs high temperature 0.65 ovens
and Oxford Cryosystems Cryostream coolers.
The application is accessible from the Diffract.1 respectively Diffract. 2 pull-down menu of the WinXPOW main menu.
4.2 Configuration
The HTC Data Collection module is only active under the WinXPOW main menu when a high- / low-temperature
device is chosen in the Instrument Parameter menu. To activate one of the optional devices open Instrument
Parameter from the WinXPOW main menu and select the mounted high- / low-temperature device from the Config
sheet.
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WinX 3.05 Software Manual High-Temperature Data Collection 4-1
For the configuration of the temperature device set-up select the HTC sheet from this Instrument Configuration
page.
Choose the actual Controller Type and Thermocouple. The Maximum Temperature is automatically selected
dependent on the thermocouple and corresponds to the maximum temperature pre-set in the HTC controller. The
COM Settings, as there are baud rate, data bits and parity should not be changed, only the COM port number
should be changed according to the hardware setting of the PC. The input of the Maximum Ramprate is shown on
the left side of the COM setting and is 100/ min by default and should not be above this rate. The PID Parameters
are used to control the temperature handling, the given default values are very well tested with respect to the
controller type and should not be changed.
To achieve the minimum possible error in the temperature reading, a correction curve for the thermocouple reading
may be set up by defining a temperature calibration file and activating the Use calibration button. Such a correction
curve must be defined in an ASCII file with the following format :
! TEMPERATURE CALIBRATION FILE 1.01

# Soll Ist
10 10
125 130
573 593
1064 1112
The first line must contain the file ID exactly as shown above; lines starting with # character will be treated as
comments and ignored. The first value in every line refers to the true sample temperature (in C), the second to the
thermocouple reading (in C). A linear interpolation will be done for temperatures between given calibration pairs; for
temperatures outside the lowest or highest temperature in the calibration file, the offset for the last entry will be used
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without extrapolation. (E.g., for the file given above a requested temperature of 300 will correspond to a
thermocouple reading of 310.9 and a requested temperature of 1200 will equal 1248 thermocouple reading.)
Using the temperature calibration will result in a systematic discrepancy between the temperature shown on the
controller display and the PC monitor, the size of the offset being equal to the temperature difference calculated from
the calibration curve.
The temperature calibration file is read in every time the HTC module is started; it must therefore not be deleted while
in use. Changing the contents of the temperature calibration file will affect every HTC run after (re-)starting HTC data
collection from the main menu.
By leaving the Instrument Parameter menu, the instrument parameter file will be updated automatically.
4.3 Creation of the Raw Data File

Before starting the HTC data collection module a raw data file must have neem created file which contains the
required measuring parameters as Detector Scan Mode Angle Ranges etc. (see Chapter 3 for additional
information), but does not contain any measured data.
In addition to the usual raw data file creation, in HTC data collection one has to select the option Scan Usage in the
Ranges pull-down menu and select the option Temperature in the Scan Usage window.
The option First File Number will be the extension of the first raw data file in a series of HTC measurements, e.g.
*.001. Therefore it is possible to continue a previous HTC measurement under the same raw data file name at a
specified temperature and completing the data collection by the insertion of a consecutive file number.
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4.4 High Temperature Data Collection
Select HTC Data Collection from the main menu. If more than one diffractometer is active in the menu bar, select
the one where the high- /low-temperature device is mounted, either Diffract.1 or Diffract.2 and start HTC Data
Collection.
The program first calls the data collection module which checks the necessary communication lines to the
diffractometer and detector and displays an error message if communication could not be established. After these
checks the HTC data collection main menu is called automatically.
4.4.1 File
Before a measurement can be performed a HTC parameter file must be loaded or created newly.
With the option New a new, empty file is created, while with File / Open a previously created file could be loaded
into the application.
With Save an edited file could be stored on disk. Before a measurement is performed the HTC parameter file must
be stored on disk.
With Save as a loaded file could be stored under a different name.
Print, Print Preview and Print Setup are commands to print out the contents of the application main window and
select and configure the used printer.
Graphic export provide an opportunity to create files in different formats for importing the display into other
applications. The user can choose the desired format with the combo box Save as type. The available formats are
Enhanced Metafile ( which will be the most adequate format when importing the display into other applications ),
TIFF- and Windows Bitmap file. With deactivated option only Diagram the output will be identical to the printed
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version, otherwise only the diagram itself will be exported. The default behaviour is to rescale the display to a DIN-A4
page, regardless of the current aspect ratio of the
display. To maintain the current aspect ratio the
keep aspect ratio option should be activated.
Exit will terminate the application, this is only possible if no measurement is running.
4.4.2 Parameter File Setup

To change parameters or to check the default values, select Parameters from the Setup pull-down menu. In the
displayed dialog two sheets are present : Raw Data File to select a raw data file to be used for measurement (see
above or Chapter 4.3) and Default Parameters for editing the pre-set default parameter values. Temperature
Step etc. are shown.
Temperature Step is the default temperature step for each ramp to execute. Ramp Rate and Ramp Time is the
rate a ramp should be performed respectively the time span a ramp should last. In the later case the resulting rate
should not exceed the controllers limits. Hold time is the time span the application will wait before performing a
measurement. Only if Measuring During Hold is marked, the data collection module will be activated and data will
be collected according to the chosen raw data file.
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Also, like in the normal data collection, a raw data file name has to be given, otherwise an error message is displayed
while executing the HTC data collection.
The selected values in the Set-up Parameters menu will be used as defaults in the Temperature Program.
4.4.3 Input of a Temperature Program
To set up a temperature program select option Temperature Program from the Setup menu. The figure below
shows the beginning of a temperature program input using the defaults described above.
The easiest way to set up a temperature program is to define proper defaults and to add the desired steps.
Add Ramp and Add Hold will insert a ramp respectively hold step with the corresponding default values at the
marked position in the list.
Add Step will insert a single temperature step consisting of a ramp and hold step, as well with the corresponding
default values. Add Steps will add an arbitrary amount of temperature steps, only limited by the allowed temperature
range of the controller. New steps will be insert at the marked list position.
Delete will delete the marked steps from the list
Parameters gives the user a quick access to the Setup Parameter dialog to change the default values.
Load List gives the possibility to load directly an already edited list from another HTC parameter file, the loaded list
will replace a potentially edited list. This could also be done by just dragn drop a HTC parameter file onto the
temperature list. This is a very versatile method to work with template curves.
However a temperature list was created it is possible to
change every step by just double-clicking on the desired
step. A dialog will open giving the opportunity to change
every step parameter. When editing a ramp, the editable
parameters are the temperature and the ramp rate
respectively the duration of the ramp. When changing the
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temperature the application will adjust the temperatures of the subsequent steps accordingly.
When editing a hold the user can change the hold time ( see above ), can switch on or off the data collection module
and if this is activated which range(s) of the raw data file should be measured. A range could be selected by typing
the range number. If more than one range should be measured the numbers must be separated by commas ( i.e 1,3
will select range 1 and 3). Consecutive ranges could be selected by typing the first and the last number separated by
a hyphen ( i.e. 1 3 will select range 1, 2 and 3).
The next two figures illustrate the investigation of the quartz transformation at 573 C which is often used for
temperature calibration purposes. The first window displays the input of the ramp/hold interval, temperature,
measurement stages, the approximate duration of the experiment etc.
After leaving this menu by pressing OK the main window displays a graphical presentation of the above temperature
program. The programmed ramp steps and hold stages are displayed.
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4.4.4 Preferences
The Preference dialog comprise options controlling the graphics layout and the logging options of the application.
The Look sheet gives the user the facility to change the
temperature unit and colour of the displayed temperature curves.
The user can change the temperature unit at any time between
Celsius ( mostly in case of high temperature measurement ) and
Kelvin (common for low temperature measurements).
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The Logging sheet gives access to the applications logging options. System logging will control the creation of a
system logging file: normal and verbose will activated the creating
of such a file. In generally this file is only needed for diagnostic
reasons ( ie. in case of hardware or communication problems ). The
file contains all executed temperature steps, error messages and
other diagnostic infos. none will inhibit the creation.
Caution: when setting to verbose the application will keep a
complete log of the communication between application and
temperature controller resulting in a rapidly growing log file. This
option should only be used temporarily to debug communication or
controller related issues and should be deactivated during regular
measurements!
Temperature logging: if enabled the application will write a
second log file with temperature readings. The file contains the
current time, the runtime, the target and actual temperature, the
temperature error and the controller status in csv-format. This file is
suitable for further processing with, for example, a spreadsheet.
4.4.5 HTC Measurement, Run and Control

To start the programmed HTC measurement press the Execute option in the above menu or click on the Execute
button in the lower part of the main window.
Start the HTC measurement with OK. The HTC controller is initialised and ramping to the first temperature starts.
The window shows the status of the HTC data collection, the actual step (Ramp or Hold), Temperature, the
Power used, the current Error, meaning the difference between the actual temperature and the setpoint chosen by
the temperature controller. Step Time is counted down and indicates the remaining measuring/ramp time and might
show negative values if a step takes longer then expected. The time for a Hold step is the sum of the waiting time
and the measuring time. Total Time shows how long the program will still be running.
During the experiment the shown diagram is constantly updated, the measured temperature will be displayed in red,
following the temperature program, displayed in blue. These default colours could be changed with the Preference
dialog ( 4.4.3 ) to any desired colour.
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As soon as the first measuring hold has been reached and the temperature is stabilised (for 10 sec the error must be
less than a software - calculated Delta T) within an appropriate time (10 min), (otherwise the controller is shut down
and a warning message is displayed), the data collection menu is called and starts the data collection with respect to
the selected range(s) automatically.
As in the normal data collection, the raw data file is automatically updated with counts after a certain time has
elapsed. Data which have already been saved to the file are displayed in blue, unsaved data in red. The Stop button
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of the small info window may be used to interrupt data collection at any time. Red datapoints will in this case be lost,
blue datapoints will be kept in the raw data file.
The HTC program can always be stopped during the various steps by pressing the Shutdown button in the lower
part of the HTC data collection main menu. The application will
After the end of the experiment the HTC data collection menu shows how well the temperature has followed the
programmed temperature diagram. The data collection menu will display the diagram collected during the last hold /
measurement state
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5 Graphics
5.1 Introduction
The Graphics program is accessible from the Raw Data pull-down menu of the WinXPOW main menu.
It can display raw data and peak lists and perform peak search, background correction and raw data smoothing.
Intensity scaling can be chosen from linear, square root or logarithmic axes displaying total counts, counts per second
or relative intensities; x-axis scaling can be 2theta, 1/d or 1/d2 ( == Q ). The number of windows is nearly unlimited as
is the number of diagrams in a window.
The graphics program is a multi-document application; the windows standards are the same as in applications like
Word, Excel etc.. The most important windows properties are described in chapter 5.5.7.
WinXPOW 3.05 Software Manual - Graphics 5-1

5.2 Files
The menu item File offers the standard Windows utilities to read and write files, to re-open recently used files and to
print the graphics.
The file formats that the program can handle are :
the standard STOE peak files in ASCII format with default extension *.pks or *.pth.
the standard STOE binary raw data files with default extension *.raw or *.rth.
STOE graphic files (default extension *.grs) containing the complete information about the state of the graphics
program. These files can be used for storing the current graphics and recalling the exact look of the graphics at a
latter time.
Immediately after the start of the program, only the Open and Recent files options are available from the pull-down
menu.
The Open command loads the contents of an existing file - either a raw data or peak file - into the program and
displays the file contents in a new window.
The Load Graphic and Save Graphic' commands lets the user write and read graphic files (*.grs).
With the Load and Print Graphic command the user could load a previously saved graphics file (*.grs) and
immedeatly print it out.
With the Setup command the user could access a dialog in which certain aspects of the program could be edited.
The Printing sheet is used to define some aspect of printing. When
choosing output file header info the diagram will be printed together
with all data collection parameters at the bottom. With Frame pen
width the user can control the thickness of the frame surrounding the
data and header info. With Data format and Time format the user can
control the output of the current date and time which will be printed if
not suppressed by choosing no output - in the upper right area of the
surrounding frame. By clicking the Defaults button the options will be
reset to default values.

The Colour Setup sheet is used to define the various colours
associated with the loaded data, labels, background etc. The
colour selection may either be done via the RGB formalism (if a
button is clicked, the edit windows or spinner buttons of the
basic colours red, green and blue may be used to change the
current colour settings) or by the Choose Colors button which
opens the standard Windows colour dialog. If more than 16
curves are loaded in a window, the colour coding is repeated
starting from the colour associated with curve 1.
Export Graphic provide an opportunity to create files in different formats for importing the display into other
Enhanced Metafile (which will be the most adequate format when importing the display into other applications), TIFF-,
JPG- and Windows Bitmap file. With deactivated option only Diagram(s) the output will be identical to the printed
version, otherwise only the diagram itself will be exported. The default behaviour is to rescale the display to a DIN-A4
page, regardless of the current aspect ratio of the display. To maintain the current screen aspect ratio the keep
aspect ratio option should be activated.
The Print, Print Preview and Print Setup commands control and format the output of the programs main window
to the system printer.
The Exit command terminates the application and returns control to the WinXPOW main menu.

5.3 View
This menu comprises several options controlling the graphics layout. Activated options will be marked with an leading
checkmark.
Whole Diagram resets a former zoom command by displaying both axes starting from the minimum value of all
loaded diagrams to their respective maximum value. The tool button remains depressed as long as the complete
diagram is displayed. By clicking on the Whole button again, the zoomed-in state may be recalled.
Position Info switch on or off the display of the current cursor position (position and intensity) in the left part of the
main windows status bar.
Crosswire Changes the cursor to a crosshair extending over the whole active window. This representation is useful
for comparing peak positions of diagrams loaded into the same window.
Grid Lines adds or removes a rectangular pattern to and from the window.
If the option Rescale on Load is activated.the program will automaticly rescale the axes to fit the new data. If
deactivated the axis will be left unchanged, even if the new data wont fit into the actually axes.
The options File Names switch on or off whether the file names will be displayed in the upper left corner of the
diagram.
The options File Titles switch on or off whether the file titles will be displayed in the upper left corner of the diagram.
The options Title Left Aligned, Titles in Reverse Order and Show Range Number control the way the titles are
actually displayed. The default behaviour of displaying the title right align could be changed with the option Title Left
Aligned. The file titles are displayed from top to bottom in the order the curves are loaded, the activated option
Titles in Reverse Order will invert this order. The option Show Range Number switch on and off the display of
range numbers.
Toolbar removes / brings back the toolbar with shortcut buttons above the main window.
Status bar removes / brings back the status bar beneath the main window.

The Position Info, Whole Diagram, and Grid Lines commands are also available from these toolbar buttons:
When the cursor is not in the Position Info mode, it may be used to define a zoom-in window by moving it to any
point in the diagram, pressing the left mouse button and holding it depressed while moving the opposite corner of the
rubber box to the requested position. Releasing the left mouse button will change the display to an enlarged
representation of that diagram part which was contained in the rubber box. Scroll bars will be added to the diagram
enabling the user to move the diagram horizontally and vertically, if necessary.

5.4 Options
This menu item comprises commands which changes the appearance of the graphics windows as well as tools for
editing and manipulating peak and raw data.
Scaling Axes allows the user to input exact values for the viewport and to choose from several scaling modes for
the intensity and angle axis. The data limits in the bottom right part of the dialog box are given for comparison.
Whereas 2Theta (or Omega in the case of a rocking curve with the detector kept at a fixed position) is the most
popular scaling for the x-axis of a diffractogram, the 1/d or 1/d**2 - scaling is useful for comparing data sets collected
with different wavelengths. The x-axis will be automatically reset to the maximum viewport necessary for the curves
currently loaded if the type of scaling is changed.
The intensity scaling will usually be done on a linear scale. Square root scaling gives a better representation of the
background and leads to error bars of identical absolute size for every data point. Logarithmic scaling is used for
high-resolution diffractograms or reflectograms from thin films, wafers etc..
Absolute intensity scaling will label the intensity axis with the counts accumulated over the respective count time of
the data collection. Counts / sec normalizes these counts to a count rate per sec and is thus useful for comparing
diagrams collected with different measuring times. Relative intensity scaling sets the strongest intensity in every
diagram to 100%.
The Y offset may be used to shift diagrams displayed in one window vertically by a certain amount. This mode
increases the visibility, but should be switched off if correct intensity information is to be taken from the display as the
offset is not taken into account when the Position info is invoked.

The Absolute / Relative / Linear / Square Root / Logarithmic scaling options are also
available from these tool bar buttons :
The Fonts option is used to select the lettering type and size used for the title axes labels, notes.
Labels Is used to add d-spacing - , index - or other labels to the diagram. The option needs at least one peak file
loaded from which the data for labelling can be taken.
hkl-labelling can only be done if a peak file containing peak indices has been loaded.
2Theta - and d-value labelling can be chosen independently from the x-axis scaling, whereas 'same as axis'
automatically writes the peak positions in 2theta, 1/d or 1/d**2 depending on the setting for the x-axis.
The Find Peaks tool opens a dialog box from which a peak search in the loaded raw data can be started. It is
disabled if no or more than one raw data file is loaded in the active window or if a peak list is loaded together with the
raw data.

Estimated Halfwidth : An approximate value for the peak halfwidth must be given. This parameter can be used to
discern between sharp and broad peaks. When both kinds of peaks are present in a diagram, it is usually impossible
to identify both classes of peaks in one run of the peak search. For data collected with the linear PSD or IP-PSD
0.15, for data collected with the Mythen1K detector 0.08 will be usually a good value.
Significance Level : The significance level sets a lower limit to the peak heights; it is defined as the ratio of the
maximum peak intensity to background. Peaks which are found by the slope criterion, but have a peak height below
the given significance limit, will be discarded.
Intensity Limit : The intensity limit is an additional criterion applied to a peak identified in the peak search algorithm.
All peaks having an absolute height less than the input value will be discarded. Setting it to 0 will accept all peaks
matching the significance criterion, values above 0 will increasingly reduce the number of peaks
Remove Alpha2 Peaks : Checking this box will scan the peak list for pairs of Alpha1/Alpha2 peaks and discard the
Alpha2 reflection. To match the Alpha1/Alpha2 criterion, the peak position of the second peak must be within 0.02 of
the theoretical Alpha2-reflection as calculated from the Alpha1-position and its intensity must be between 45 and 55
% of the corresponding Alpha1 peak.
Remove Spikes : When this box is checked, a search for peaks of abnormal halfwidth will be performed in the peak
list which passed the other criteria. Peaks of a halfwidth less than 25% of the estimated halfwidth defined above will
be discarded as spikes.
The Defaults button loads approximately correct parameters for most problems in case the user has completely lost
track of the parameter settings meaning and effects.
By pressing the OK button the peak search is started. When it is finished, the number of found peaks is displayed in
a message box and the menu bar layout changes. In this mode, the user may add peaks at any position by pointing
the cursor to the desired peak position and clicking on the left mouse button. Accordingly, peaks may be removed by
moving the cursor onto the bar of a peak and clicking on the right mouse button. Peaks may also be moved in the
drag-and-drop way : When the cursor changes to a cross ( whenever the cursor is close enough to a peak in x and
within the peak height in y ), a peak may be picked up by left-clicking and moving it to the required position and
intensity and placing it there by releasing the mouse-button. In order to invoke the standard zoom-in option, it is
advisable to keep the cursor above peaks in the diagram or below the x scale, so that peaks are not inadvertedly
shifted instead of zooming in.
Exit brings the user back to the normal graphics mode.

The menu bar item Write Peakfile saves the peak list to file.
Restart brings the dialog box Peak Search Parameters back on the screen so that the user may restart the peak
search with a different set of parameters.
Next Range and Prev. Range are enabled only if the raw data file contains more than one scan range and are
used to switch to the next / previous scan range for peak identification.
The Edit Peaks option opens the same edit window as the Find Peaks command does after the peak identification
with the same possibilities to add or remove peaks by mouse-clicks.
The Smooth Raw Data is option opens a dialog box which asks for the number of data points which are to be
averaged. It is only enabled if one raw data file is loaded in the
current window. The smoothing is done after an algorithm
described by Allmann (see below). This value may either be
input as the average peak halfwidth (in degrees 2theta) from
which the program calculates the number of points by dividing it
by the data step width or directly as the number of data points to
be used. After pressing the OK button, the smoothed curve is
displayed together with the original raw data.
R.Allmann, Smoothing by digital filters and a new peak search routine. EPDIC 2, Mat.Sci.Forum 133-136, 323 (1993)
R. Allmann, Rntgenpulverdiffraktometrie, Clausthaler Tektonische Hefte 29, Verlag Sven von Loga, Kln 1994
The Background tool starts an automatic background-removal routine which may as well be altered by the user.
The option is only available if only a single raw data file is loaded in the current window.
If the option is selected, the menu layout is changed and the program displays a background-spline function
calculated from a number of automatically selected background points. There are three options for the user to change
the background generated by the program :
By left-clicking on one of these points, they may be moved to any position in the diagram and - by releasing the
mouse button again may be placed at a different location. The spline function will be automatically re-calculated.
The very first and very last point of the diagram may not be shifted in their position, but may only be altered in their
height.
By double-clicking anywhere in the diagram, an additional background point is inserted and the background - spline
re-calculated.
By either clicking on the Inc.Smo. / Dec.Smo. menu items or by hitting the + / - keys on the numeric keypad, the
degree of smoothing of the spline function is changed. By increasing the smoothing further and further, a straight
background in the form of a linear regression will be obtained. By decreasing the smoothing factor further and further,
the background will follow exactly through all background points, sometimes tending to overshoot between the points.

When the background line has been defined, the Subtract BG option may be used to create a raw data file with the
background-corrected data. The default extension for background-subtracted data is *.rmb.
When the Exit option is selected, the background selected so far is written to the original raw data file (without
changing the original data) and may e.g. be used in the fitting routine (see chapter 8). Subsequently, the normal
graphics menu bar is restored.
The Sign file command allows to sign a GMP raw data file. An entry File signed will be appended to the files
Audit Data, including name of the user who signed the file and the date he signed.
Only users that have the Sign privilege are allowed to sign a file: this privilege can
be given or removed using the User Management functionality in MainMenu. After
choosing this command, the user is asked to enter his username and password.
This functionality is disabled if WinXPOW is not running in an GMP controlled
environment, or the data where not measured under GMP. A file can only be
signed once.

5.5 Window
comprises commands concerning either a particular window of the graphics display (Add Raw Data, Add Peak
Data, Add ICDD data, Delete Curve, Split) and commands regarding the order and shape of all currently opened
graphics windows (Cascade, Tile Horizontally, Tile Vertically, current window list).
Whereas data loaded with File-Open are always displayed in a window of their own, the Add Raw Data command
displays a newly loaded file in the currently active window together with all other already loaded curves. The default
extension for files shown in the standard windows Open menu is *.r*.
If a window has been split (see chapter 5.5.5), the diagram will be displayed in the currently selected upper or lower
part of the window.
Add Peak Data has the same functions as Add Raw Data for the opening of peak files. The default extension for
files shown in the standard windows Open menu is *.p*.
The Add ICDD Data tool loads peak lists from the ICDD data base into the current graphics. The dialog will asked
the user for the requested PDF card number (Product ID). The format of this
card number was changed and dependes on the installed database. However
the program recognizes which version of the ICDD data base is installed and
asks the user to input the card number using either the older 6-digit [nn-nnnn]
or the newer 9-digit [nn-nnn-nnnn] format. For both formats only digits, hyphens
(as separator) and blanks (ignored) are acceptable characters: the PDF card
[01-082-0505] should be therefore entered as 01-082-0505
The Edit Curve option opens a list box showing all curves in the currently selected part of the window. By clicking on
one line and then pressing the Delete button, the corresponding diagram is flagged for removal from the display.
When the window is closed using the OK button, the flagged curves will be removed (and the colours newly
assigned to the remaining diagrams). By pressing the Cancel button, the changes will not become active. By

selecting one entry with a left-mouse-click and moving the mouse up- or downwards, still pressing the left mouse
button, the order of the curves, and with it the order they are drawn, can be altered.
The scale factor and title of each curve may be changed by double-left-clicking on the corresponding line. A dialog
box is opened which shows an edit box with the current title for the selected curve and a checkbox for curve scaling.
By default, the check mark 'scaling' is not checked and the corresponding intensity set to 100, which means that the
intensities are displayed as read from the respective files. If the user checks this mark, the maximum intensity of the
curve may be scaled to any required value (the intensity input in the edit box must always be in ABSOLUTE count
rate regardless of the y-scaling currently selected).
Using the Split option, every window may be split into two parts separated horizontally. By using the toolbar buttons
shown below that part of the window, which is to receive all keyboard and mouse input, may be selected. The border
line between the two window parts may be moved when the cursor is close to it and changes to a double-arrow.
Cascade aligns all windows which are currently not minimized one on top of the other with only the title bar being
visible above the other diagrams.
Tile Horizontal aligns all windows which are currently not minimized one above the other in landscape format, while
Tile Vertically aligns all windows which are currently not minimized one beside the other in portrait format.
Current window list lists all graphic windows which are open at the moment either minimized, maximized or in any
other state. Clicking on its name makes it the active window.

5.5.1 Window handling
Every graphics window has a title bar of its own with a document icon in its top left corner. By clicking on this icon, a
pull-down menu is opened which contains the Windows standard windows control commands. As this menu is
provided by the operating system, it will be in the language defined in the appropriate System Setup routine. When
the window is maximized so that it fills the whole main window, the document icon is moved
to the leftmost position of the main windows menu bar.
By right-clicking on the mouse anywhere in the window area a formatting window may be
opened which allows a short-cut to functions like Add ... Data , Split , Edit Curve, Insert
Note and Scaling Axes which have been explained above in the context of their
respective pull-down-menus.
The 'Insert Note' option, however, is not available from the pull-down-menus as the cursor
position at which the right mouse-click is executed is taken as the top left corner of the
position of the text to be entered. The corresponding dialog box and the handling of user-
defined notes are explained in the next chapter.
5.5.2 Editing user notes

When the 'Insert note' option has been invoked from the above window, a dialog box is opened which allows the input
of any text which will be positioned in the diagram in such a way that the top left corner of the note will be at the
cursor position at which the formatting window was opened by right-clicking. The colour of the notes text could be
controlled by clicking in the coloured rectangle.
Existing notes may be moved by left-clicking on the text and dragging- and dropping to their new positions. They may
also be edited by double-left-clicking on the text in which case the above dialog window opens again. The text and
the color may then be altered or the 'Delete' button pressed to remove the whole note from the diagram. To copy text
to another position, the clipboard function may
be used: The existing text in the above
window is selected with the cursor and Ctrl-C
pressed. On opening the window at another
position, the standard text is again selected
and Ctrl-V pressed. This will overwrite the
standard text with the one selected before.
To save the text inserted into the diagram, the
'Save Graphic' option described in chapter 5.2
can be used.

6 3D-Graphics
6.1 Introduction
The 3D-Graphics program is accessible from the Raw Data pull-down menu of the WinXPOW main menu.
It can display sets of raw data from high-temperature runs, time-resolved experiments or any other combination of
powder data on linear, square root or logarithmic scale in a user-defined perspective. The program also offers the
option of a Pseudo-Guinier-film representation where peak intensities are colour-coded.
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WinX 3.05 Software Manual 3D Graphics 6-1
6.2 Files
The menu item File offers the standard Windows utilities to read and write files, to re-open recently used files and to
print the current 3D graphics.
The program can handle STOE raw data files and 3DGrafix files.
Open reads the contents of existing raw data files into the program and displays their contents. As long as no data
have been loaded, a dummy picture is displayed. There are two ways to load a set of raw data into the program : One
is to load a single raw data file which has been used as a master file for a multi-file data collection e.g. with a high-
temperature attachment, sample changer or sample position control (see chapter 3.5.3 ). This master file is
accompanied by a set of corresponding data files (usually with the same name but extensions ranging from *.001 to
.nnn) which are automatically read into the program once the master file is opened. The second possibility is to open
several raw data files which are then single-sample files and contain raw data. All these data are then read in and
displayed. If they contain z information (see chapter 7) they may subsequently be aligned in the order of z. By
pressing the right mousebutton while the cursor is inside the main window, the z order may be reversed.
Save Metafile lets the user write the current graphics to an *.emf file ready for import into other programs.
'Load Graphic' reads an existing 3DGraphics file restoring the display saved in this file.
'Save Graphic' stores all information about the current display status to a file with default extension *.g3s. This file
may be read in at a latter stage to restore the graphics in the way they were when saved. The raw data are NOT
stored in the 3DGraphics file and may therefore not be deleted even if the display has been saved.
Print - Print Preview - Print Setup control and format the output of the programs main window to the system
printer.
The Recent file list contains the last eight files which have been opened.
Exit terminates the 3D graphics routine and returns control to the STOE main menu.
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6.3 View
allows the user to change the graphics layout.
Centre moves the cube in its current orientation to the centre of the window and, if necessary, re-sizes it to fill the
window. This command is also available from the toolbar button .
Default Cube resets the perspective to a standard view and is useful if the cube has been manually twisted beyond
repair.
Cube Mode switches to a representation of a flexible cube which defines the perspective of the drawing. When the
user presses the left mouse-button on one of the squares in the middle of the cube edges, the corresponding edge
changes its colour and may be moved until the mouse-button is released again. The front and back face of the cube
may also be shifted as one block when the cursor is moved to the centre of the crosshair and the left button is
pressed.
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To move the cube around within the window, click on the arrow-crosshair in the middle of the cube. When it changes
its colour, the cube may be shifted within the window until the left mouse-button is released again. The Centre
command described above is also available in this display mode.
To go back to the normal 3D representation, remove the check mark from this menu item or use the toolbar
button described below. The same procedure has to be followed by scaling the x,y and z-axis. Check the
corresponding button, scale the x,y, z-axis or the cube and uncheck the button again.
Note : It is possible to make two cube edges exactly coinciding. The singularity thus produced may only be resolved
by using the Default Cube command.
Cube Mode and Top View may be invoked and switched off by the toolbar buttons , respectively.
Top View switches to a two-dimensional representation of the data in the form of a moving Guinier-film experiment.
The size and position of the rectangle correspond to the size and position of the cubess front face in the cube mode
representation. Intensities are colour-coded as defined in the Colour Setup dialog box. The scaling mode currently
selected (linear, square root or logarithmic) is maintained. The intensities of the lines are indicated above the Top
View window.
Recolour applies the colour definition as set up in the Options Colour dialog box to the currently selected range
of raw data. Start colour will be assigned to the first diagram in the display, end colour to the last diagram displayed
and the diagram colours in between will be interpolated taken into account the middle colour definition. This option
need only be selected if the z-Range of the display has been changed by the Scale - Z-Range option. This option is
also accessible from the toolbar button .
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6.4 Options
This menu item comprises commands which change the appearance of the graphics without changing the
perspective of the drawing : Colour, Font , Labels , Scaling , and Title.
6.4.1 Colour
The colour scheme is defined by the three colours which are assigned to the first, middle and last diagram in the raw
data set. For every diagram in the graphics, the appropriate colour is calculated by linear interpolation between the
colours defined. All colours including those for background, text and grid lines are defined by their RGB values which
may either be entered in the edit box via the keyboard or by using the attached spin buttons.
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The check boxes Draw filled diagrams and Use Border pen for diagram define the look of the graphics. If Draw
filled diagrams is not checked, every diagram will be displayed as a polygon built from all count rates; otherwise the
area between the zero-level and the count rate will be filled with the appropriate colour. If the Border pen is not
checked, the polygon will be drawn in the appropriate diagram colour, otherwise in the colour used for text and border
(usually black).
6.4.2 Font
This option opens the standard Windows dialog box from which the user may select the type and size of the label
lettering. The language used in this box depends on the users systems settings.
6.4.3 Labels
This option allows the user to define the layout of the outer part of the cube.
By using the spin buttons Label Position X, Label Position Y and Label Position Z the cube edge which will receive
the labelling of the axis may be selected. The edge currently selected is highlighted in the drawing in the right-hand-
side of the dialog box. When no edge is highlighted, labelling for the corresponding axis will be omitted.
The radio buttons Z axis mode allow the user to define the aligning criterion used to order the diagrams along the z
axis. N will stack the diagrams starting with the file having the smallest number as extension and ending with the
largest. Time will start with the oldest file and end with the most recently measured one and so displays the duration
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of the experiments. The labelling of the second button depends on the kind of measurement performed. It may e.g. be
Temperature, Sample position or the like.
The check box Draw grid lines switches the display of grid lines on and off.
If Draw Box is not checked, all of the outer part of the cube including labels and grid lines will be omitted from the
display.
The 'Axis' edit windows may be used to change all axis titles and to define the labelling of the z-axis.
6.4.4 Scaling
This option sets the viewport limits for all three axes and the scaling mode for the intensity ( = Y ) axis.
The edit boxes X-Range, Y-Range and Z-Range are used to define the actually displayed part of the raw data set.
The X-Range values are given in degrees, the Y-Range is the intensity axis and the meaning of the Z-Range values
depends on the setting of the Z-axis mode described in the previous chapter. If a file contain z information (see
chapter 7) they may subsequently be aligned in the order of z. By pressing the right mousebutton while the cursor is
inside the main window, the z order may be reversed.
The truncation of the visible portions may also be performed with the toolbar buttons . Using
these buttons a representation of a flexible cube appears, similar to the one in the cube mode . The different axis
may be scaled according to the needs. In the case of the x-axis the adjusted section then can be moved through the
cube by pressing the left mouse button on the centre of the crosshair.
They offer graphical support for the selection of the viewport in the same way as the cube mode does. Clicking on
the button labelled with the arrow-crosshair resets the display to the full range of the data set.
The radio buttons Scaling allow the selection of a function for the intensity axis. The same may be done from the
toolbar using the buttons .
If the check box Individual is checked, all diagrams are shown on a relative scale, i.e. the maximum intensity of
every diagram is scaled to 100 %.
6.4.5 Title
opens a dialog box allowing the user to enter a title describing the displayed experiment which is shown in the bottom
left corner of the window.
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7 Raw Data Handling
7.1 Introduction
The Raw Data Handling routine provides tools for the modification and conversion of the binary STOE raw data files
*.raw like absorption correction or conversion of the raw data for Rietveld analysis.
After selection of the Raw Data Handling from the pull down menu item Raw Data the following window is
displayed.
Title Bar
Menu Bar Tool Bar
Caption Bar
Range View Window

Layer Panel
Report Panel
History Panel
Status Bar
The program window is split into five separate areas. In the upper area the Menu, Tool and Caption Bar are
positioned. All basic operations can be started with these panels. The Caption Bar will show important messages
(such as position info of the mouse pointer or operating mode of the program etc.).
Most important area of the window for working with raw data files is the Range View Window (centre / right of the
program window). The changes to the raw data loaded will be displayed in this window.
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WinX 3.05 Software Manual Raw Data Handling 7-1
On the left hand side of the program window the Layer Panel and the History Panel are located. The Layer Panel
enables a quick and comfortable way to edit separate ranges and their display properties.
The History Panel will list all operations done by the user. In the basic working mode all of these operations can be
reversed and macros can be applied or edited.
On the bottom of the program window the Report Panel is placed. All info from the source file or the working copy
and program errors are displayed here.
7.1.1 Menu-, Caption-, Status- and Toolbars
File Toolbar Range View Toolbar Operations Toolbar
The Menu Bar will be explained in detail in chapter 7.2. In the basic working mode three toolbars (see above) are
displayed.
The File Toolbar contains the buttons New File, Open File, Multiple Open, Import File, Export File, Merge Files,
Page Setup, Print Preview, Print and Info. All functions of the buttons are identical to the same named functions
in the Menu Bar (see below).
The Range View Toolbar contains the buttons Position Info, Crosshair, Grid, Show All, Move, Separate View
and Axes Scale. Again the functions of the buttons are identical to the functions in the Menu Bar.
The Operations Toolbar contains the buttons Absorption Correction, Angle Correction, Alpha 2 Stripping, Dead
time Correction, Fold Diagram, Background and Smooth. All functions are explained below in detail.
All Toolbars can be moved from its position. To align them in their original position select Restore Original Layout
from the View drop down menu from the Menu Bar
The Caption Bar and the Status Bar will show important information during the work with the program. The Caption
Bar will display mostly the current working mode or the position info of the mouse pointer. The Status Bar is used to
show a progress bar during applying operations in the master- or batch- working mode.
7.1.2 Layer Panel

The Layer Panel consists of a Layer Panel Toolbar (functions of this toolbar are
equal to the ones which can be selected from the Menu Bar see chapter 7.5 for
more info) and a tree figure of all the ranges loaded. The basic entry of the tree is
the loaded raw data file. The two separate range arrays Source and Working
Copy correspond to the original loaded, unedited data and the current edited data.
With the check boxes at the left side of the ranges the ranges can be hidden or
shown in the Range View Window. A right click on a range will open a context
menu to edit properties of the range. With a right click on a source range the
range display properties (line width and colour) can be edited and the range can
be selected.
If a range is selected all the data points in the raw data file will be shown as black
dots in the Range View Window. Ranges can be selected through the context
menu or by clicking the number of the range on the keyboard.
A right click on a working copy will open a context menu where, besides the options of the context menu of the source
files, all range operations can be selected. A double click on one of the ranges will open the properties dialog directly
and displaying parameters can be set. With a double click on the Working Copy or Source entry of the tree all viewing
properties of the ranges which belongs to the entry can be altered altogether.
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7.1.3 History Panel
The History Panel consists of a History Panel Toolbar and a list of operations done to
the loaded raw data file.
The toolbar contains the three buttons Save History, Play Macro File and Edit Macro.
When a raw data file is loaded by the program a temporary history file will be created. In
this history file all operations will be logged. If a file is closed (due to the exit of the
program or loading another file etc.) the temporary history file will be deleted. With the button Save History the
current history file can be saved to a user selected location. The default extension of a history file is *.hst.
A macro can be applied to the loaded raw data file. The macro must be saved as a macro file first. A macro file has to
be created with the Macro Editor. The Macro Editor can be started be the Edit Macro button in the History Panel
Toolbar.
The list of applied operations in the History Panel can be used to reverse operations. To reverse the operations just
click twice on an entry of the list, to reverse to the state of the data right after the operation connected to this entry
was applied. To receive further information to the applied operation move the mouse pointer over the entry and read
the displayed tooltip.
If an operation of a macro file could not been carried out, it will be shown in red in the history list. Errors occurred
during the playing of the macro will be listed in an error report which will be displayed in the Report Panel.
Operations which caused an error cannot be reversed.
7.1.3.1 The Macro Editor

The Macro Editor will hold a list with the previous
applied operations (file operations like save and
load and extract to file are removed from this list
because of their incompatibility with the macro
function). With the New Macro, Open Macro and
Save Macro button on the upper right side of the
Macro Editor the handling of the macro file can be
accomplished. The default extension of a macro
file is *.hmc.
The list of operations on the left side of the editor
can be altered by drag and drop of the list entries
to change the sequence of the operations, by
double click to change important parameters of
the operations and by adding operations by
clicking the symbols of them on the right side of
the dialog. After entering a new operation from the
toolbar the parameters of this option will be asked for. After the editing of the list the macro file should be saved and
can be applied to raw data files by pushing the Play Macro File button.
7.1.4 Range View Window

The Range View Window displays the current data. The user is able to zoom into the diagrams, display a crosshair
and/or a grid, give out the position info of the mouse pointer, pan, show all, separate the source and the working data
etc. All of these operations can be selected from the Menu Bar or through the Range View Toolbar. If the diagram is
zoomed a double click will display the whole diagram.
With a right mouse click a context will be shown, which contains the most important operations for the displaying of
the data.
If a range is selected from this context menu all other ranges will be hidden and only the original source range and
the edited working range will be shown. Both ranges will be selected (see chapter 7.1.2 for more info).
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7.1.5 Report Panel
The Report Panel contains a toolbar and the
report of the loaded data. In the report all
important settings of the raw data file loaded and
edited are summarized.
With the toolbar important file, print, search, copy
and format operations can be selected.
With Save as the report can be saved as an
ASCII text file (*.txt) or in the rich text format
(*.rtf). If the text is saved to an ASCII text file, all
format settings will get lost. To keep the font
settings the report must be saved in the rich text
format.
The Print Preview button will open a preview of
the text as it will be set on a print out.
In Page Setup important settings for the margin
of the print page can be set. The properties sett
here, are independent of the page setup done
from the File Toolbar or from the Menu Bar. If a
different printer should be chosen, it must be
done in this Page Setup dialog.
Print will print out the report without showing the usual printer dialog. All important settings must be done from the
Page Setup dialog.
With Font, Font Size, Bold and Italic the font used in this report and its properties can be altered.
The Report Form can be chosen on the upper right side of the panel. The short report contains only the information
of the settings of the given ranges but not the data of the ranges themselves. This data will only been shown if the full
report is selected.
If an error occurred during the work (mostly in the batch- or master working mode) an error report will be created, if
desired and set in the preferences (see chapter 7.2.3. for more details). An operation which could not been carried
out while playing a macro file, will write the error as well to the error report. To show the error report the Error
Report can bee selected from the Report Form menu.
While working with protected files (GMP mode) the Audit Data of the file can be displayed in the full or short report.
The user can select if the working data of the raw data file or the loaded unedited data from the file should be shown.
To select the source of the report the menu items From Working or From Source can be chosen.
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7.2 File
The menu item File offers the standard Windows utilities to reset to a new document, to read and write files, to re-
open recently used files, to import or export files, to merge ranges of different raw data files and to print and export
graphics shown in the Range View Window.
New resets the program to the clean state as if the program was started. The list of
operation done, stored in the History Panel and the Report Panel will be cleaned and
the raw data file will be removed from memory.
Open reads the contents of an existing raw data file, with the default extension
*.raw, smoothed raw data files (*.rsm), background subtracted raw data files (*.rmb),
calculated raw data (*.rtf) and other files in the raw data file format (like repetition files
etc.). By opening a raw data file containing more than one measured range, all these
ranges will be loaded into the current raw data handling procedure. If a file is opened
which is currently being measured, a warning message is displayed. It is not possible
to assess and alter the data during measurement. To check data and work with
currently measured ranges anyway, a working copy of the file must be created. The
warning dialog displaying will ask you if such a file should be created. The copy, if
created, will be loaded afterwards.
After opening a raw data file, its name is displayed in the Title Bar of the raw data
handling main menu, the Range View Window and the Layer Panel will display the
different ranges, the History Panel will show that a file was loaded an the Report
Panel will report measurement parameters, background points as well as further
information about the experiment.
Multiple Open will open a list of files in a batch operating mode (see chapter 7.2.1
for more information).
Save and Save As are only activated if a parameter file has been loaded from
which the file name can be taken. The program lets the user write the modified raw
data file to a file of the same or a different name, still in the STOE binary format.
Import formats and loads files with a different but specific raw data file format.
Export provides the user with the possibility to convert the raw to an ASCII, GSAS, Fullprof, XFIT, CSD; UDF,
ICDD PDF3, and MSI format compatible with other crystallographic software, especially Rietveld-Programs (see
chapter 7.2.2 for more info).
Merge writes two different raw data files into one file as consecutive ranges. Of course, files which are to be
merged must have the same wavelength, detector and diffractometer type used.
Print will print out the graphic currently shown in the Range View Window.
Print Preview will show a preview of the graphic which will be printed.
Page Setup enables the user to set individual settings for the print out of graphics.
Export Graphic will export the graphic into the following formats: Windows Enhanced Metafile (*.emf), TIFF file
(*.tif); Windows Bitmap (*.bmp) and JPG image (*.jpg). Additionally it can be decided if only the diagram should be
exported and if the aspect ratio should be kept. When the JPG image format was chosen, the compression quality
can be set.
Preferences let the user set individual preferences of the program layout, and behaviour (see chapter Fehler!
Verweisquelle konnte nicht gefunden werden. for more info).
The Most Recent File List contains the names and directories of the files most recently opened.
Exit terminates the raw data handling routine and returns control to the STOE main menu. If the raw data file has
been modified by the user, but not stored yet, the user is prompted whether he wants to update the current file or not.
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7.2.1 Different Working Modes
- If a single raw data file (which was not saved under secured GMP protection) is loaded the program will work in
the basic working mode. An original unchanged raw data diagram and a diagram which shows the result of the
chosen operation on these raw data will be displayed. All ranges can be edited separately and correction
operations will affect all ranges. The history of operations done to the original file is reversible. A defined macro
file can be used to perform defined operations automatically. Only saving the file will finalize all the done
processes. After saving the file and opening it again, the operation done to the original file are irreversible.
- If a master file (in which all data of temperature or repetition measurements will be stored) is loaded, the program
will switch to the master working mode.
NOTE: In this mode the operations done to the files are irreversible. All corrections
and adaption of the separate ranges will be stored directly in the files which are
selected. It is therefore highly recommended to make a backup copy of all the
files of the serial measurement.
The program will perform this for the user, if the user selects the option that the program should work with a
backup copy of the serial measurement.
After loading the files, a different toolbar will be shown.
File select Stop Accumulate Master

Ranges Combine
In the first (left) part of the toolbar a specific file (with a selected index) can be chosen for displaying from the
serial measurement.
The Stop button will terminate operations currently performed. The Accumulate Ranges button and the Master
Combine button will perform special operation only valid in the master working mode. The other button will
perform operations as described below to all the files of the serial measurement. Both operations will create new
raw data files.
Accumulate Ranges will accumulate all the intensities of the ranges in the selected files.
For instance:
The intensities of the range 1 from file 1 will be added to the intensities of the range 1 from file 2; range 2 from file
1 will be added to range 2 of file 2 and so on. The resulting summated intensities will be saved to a selected file.
Master Combine will do the equal operation as Accumulate Ranges. Instead of the addition of the intensities the
combine algorithm will be used as described below.
NOTE: The usage of Accumulate Ranges and Master Combine is mostly reasonable
for repetition measurements.
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- If more than one single file is loaded by the Multiple Open option
from the File menu the program will switch to the batch working
mode. The files loaded to this mode can be chosen in the batch
select file dialog. In this dialog a list of the file to load are stored.
This list can be extended with new files (Add Files) and can be
cleaned (Clear List). In the file dialog, opened after pushing the Add
Files button more than one file can be selected.
The batch working mode is identically to the master working mode
in most parts. The history is as well irreversible and all changes will
be saved to the individual files directly. Different to the master
working mode, in the batch working mode ranges could not be
accumulated and a master combine procedure can not be
performed.
This program mode should be used as a quick and easy way to
perform corrections to a list of files.
7.2.2 Export Files

Files loaded can be converted into different file formats. If
Export is chosen form the File menu, an export file dialog with
further parameters is opened. The output file which will contain
the converted data will have the same name as the basic raw data
file with a different extension corresponding to the output format.
The directory in which the output file will be stored can be chosen
in the upper field of the export dialog. In the editable drop down
list field the output format can be selected. The settings for the
different formats are selected in the Settings field in of the dialog.
The first three options are identical for all output formats.
- If avoid negative intensities is selected, all the data of the
original file is increased automatically till all intensities are greater than zero.
- If convert intensities to counts/seconds is selected, all the measured intensities will be divided by the
measuring time in seconds needed to measure these intensities.
- If overwrite files without asking is selected newly created export files will overwrite existing files if present in
the selected output directory.
Individual Format Settings:
- Format of the X/Y files: output file can remain X and Y values or only Y values.
- Format of GSAS files: the instrument parameter information in the *.gda file will be set to STADIP.PRM or different
selected values.
- Format of Fullprof files: two different formats can be selected (Id=0 and Id=10). For more information about these
formats please refer to the Fullprof manual.
Exporting Files can as well be performed in the different working modes.
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7.2.3 Preferences
In the Edit Preferences Dialog the general behaviour, the graphical layout of the diagram and printing preferences
can be changed.
The general program settings define the behaviour of the
error handling, warning management and other prompt
messages given out by the program.
The drop down list after Old File Format Handling
describes the interaction with old raw data files. The
possible options are Do not care to open old files
without warning prompt, Prompt warning to give out a
warning on loading the old format, and Do not process
old files.
If the check for unsaved data is disabled, the program
will not check if any raw data file is edited but not saved
before closing the file.
In the next drop down field the behaviour of creating
backup copies in the master working mode can be
defined. The possible choices are Always ask to show a
message prompt after opening a master file, Create
Backup without asking for the creation of the backup
files without a message prompt, or Never create
Backup.
With the next drop down list the error handling in the
master working mode can be altered. It can be chosen between Write to Error Report to give out every error to a
report which will be displayed in the report panel, Show Error Prompt to give out an error warning without stopping
the process, Break to get an error warning and stop the process afterwards, and Do not care to work without any
prompt or report.
If Ask to open Masterfile is enabled, the program will recognise if the file to be opened is part of a series and will
send an message to ask the user if the master file should be opened instead.
The enabling of the Apply calculations always to all files
will disable the dialog to select special files to apply
operations to, when working in the master mode.
The properties of the batch working mode can be
changed with the last two check boxes Do not prompt
errors and Overwrite files. When the first is checked,
the error prompt which will be displayed if incompatible
files are added to the batch file list will be suppressed.
The second check box suppresses the warning
messages in the batch working mode.
The diagram appearance defines output of diagrams on
the screen and in print outs. In the box drawing settings
the basic colours, the line width of the diagram and the
showing of a zero line can be altered.
In the next drop down list the position of the filename can
be aligned and the title of the top diagram (which shows
the original raw data file before alteration) and the below
diagram (which shows the current altered raw data file)
can be edited. The locations of the diagrams correspond
here to the split view.
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The printer settings can be used to alter the appearance of the graphic print out.
Date and Time of

the Print Out
STOE-Frame
On every printed diagram the STOE-Frame will be shown. This

STOE-Frame consists of a box around the diagram and a title
field at the top of the page.
If the date or the time is enabled in the preference dialog, on the
right side of the title the date and/or the time of the print out is
given. The field in the middle of the title shows an editable text,
which can be defined in the WinXPOW MainMenu.
The orientation, the margin of the frame and the settings for the
Bundsteg (with possible Lochermarke) can be set in the
Page-Setup-Dialog which is assessable through the toolbar
button or the File-menu see above.
All settings can be reset to the default values by clicking the
Reset button.
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7.3 View
The pull down menu View changes the display of the file contents on the screen.
If Position Info is checked, the 2 and the intensity position of the mouse
pointer will be displayed in the caption bar. Crosshair will connect the mouse
pointer with the diagram frame, forming a crosshair. If Show Grid is enabled a
grid will be displayed over the diagram.
With Zoom all and Pan a zoomed diagram can be handled. With Split the two
files (original loaded before the editing and the current working file) can be viewed
in a split or in an overlay mode. In the split view the diagrams of the source and of
the working file will be separated. The top diagram displays corresponds to the
source file and the lower button diagram shows the edited ranges. To enable the
split view, both files must be displayed with at least one range. If all ranges of one
file are hidden, only the other file will be displayed in the overlaid mode.
With X-Axis Scale and Y-Axis Scale the scale of the axes can be altered. The
X-Axis can be scaled to 2, 1/D and 1/D2. The Y-Axis can be scaled to relative and absolute values.
In the last three menu entries the layout of the whole program can be altered. With Restore Original Layout the
layout of the program before the alteration can be restored.
7.4 Parameter
This option activates the pull down menu shown on the right side.
- Title allows the user to change the raw data file title.
- Wavelength allows to change the wavelength used for the data collection to a
different standard wavelength or to user defined one.
NOTE: Obviously, this needs only to be done if the data has been accidentally
collected with an incorrect instrument parameter file setting. Input of an
incorrect wavelength will lead to disastrous results when observed 2- values
are converted to d-spacing by any of the evaluation programs!
- Generator allows to change the generator-settings stored in the raw data file.
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7.5 Ranges
The menu item Ranges activates the pull down menu shown on the right, with the
options to combine, delete etc. ranges of collected powder patterns as well as to add,
subtract or divide ranges from an other file.
All of this operations can be chosen as well from the toolbar in the Layer Panel or in the
context menu if a range in the Layer Panel is clicked by a right click on a range.
NOTE: If a range operation is selected in the Ranges menu or in
the Layer Panel toolbar a range must be chosen first to
proceed. To choose the operation in the context menu
requires no selection of specific ranges.
When working in master working mode or batch working mode the operation selected will
be applied to all selected files (which can be selected in the file select dialog in the master
working mode which is only displayed if it is enabled in the preferences of the program). In master or batch mode all
icons shown in the pull down menu got a -symbol at the upper left corner.
Add Ranges performs the requested operation between a scan range

of the current raw data file and a scan range of another range or ranges
of the same raw data file.
One or more ranges can be activated by a mouse click and using the
CTRL-key. These ranges will be added by pressing OK to the range
specified in the Select Range to add to drop down list in the upper right
corner of the displayed window. All ranges could be added to the
selected range by pushing the All Ranges button in the lower left corner
of the dialog.
The tool Combine Ranges creates a single range from two ranges with different 2 ranges. The option requires two
ranges collected with the same scan mode; otherwise an error message is given. If the scan ranges overlap, the
intensities in the overlapping region will be added with weights linearly proportional to their angular position:
x1 x x x2
I( x )=I1 ( x ) + I 2 (x )
x1 x2 x1 x2
I(x) : new intensity at x

I1(x) : intensity at x in the first range
I2(x) : intensity at x in the second range
x1 : end of first range
x2 : start of second range
If the two scan ranges do not overlap, a warning message will be displayed and a zero line will be inserted in the
region between the end of the first range and the start of the second range.
If the number of points for the new range exceeds the maximum permitted number per range, i.e. 16384, the new
range will be truncated at this point and a warning message will be displayed.
Delete Ranges removes a range from the current raw data file.
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The option Truncate Ranges reduces the angular range for a selected
scan range in order to eliminate useless data points (i.e. shadowing
effects from sample holders etc.).
Adapt Intensities is used to either multiply all intensities in a range by a

user-defined factor, to set the maximum intensity in a range to a certain
value with all the other intensities being changed accordingly maintaining the
relative intensity relations, to cut the smallest intensities to a minimum value
or to slide the range(s) to a defined value. This option may be useful for
comparison reasons, or to avoid negative intensity values, but invalidates the
counting statistics.
NOTE: Data manipulated in this way should therefore

never be used for quantitative work.
Add Points is useful to gain intensity at the expense of data

resolution. When two points are added up to one data point in the
raw data file, the nominal step width of data points is doubled and
the intensity per data point is approximately doubled, too. For very
badly diffracting samples this value may be increased up to a point
where the nominal data step width is about a third of the expected
peak half widths. Otherwise this option may be used to reduce the
amount of collected data points in order to save disk space or load
this modified file after conversion into older shareware programs.
One or more ranges out of a multi range raw data file may be extracted to another file using the option Extract
Ranges.
Add File, performs the requested operation between a scan range of the
current raw data file and a scan range of another or the same raw data file.
The scan parameters of the two ranges have to be identical otherwise a
warning message is displayed and the operation is aborted. When the
second file has been accepted by the software the relative intensity of the first
range with respect to the second range and vice versa can be influenced by
the multiplication factors (m1 for the first and m2 for the second range).
These ranges will then be added in the specified ratio by pressing OK.
Subtract File performs the same operation between a scan range of the current raw data file and a scan range of
another or the same raw data file only in the reverse case. The second range will be subtracted from the first range
according to the chosen ratio.
Divide File performs the division of a scan range of the current raw data file by scan range of another or the same
raw data file after choosing a specific factor ratio.
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7.6 Operations
The menu item Operations activates the pull down menu shown on the right,
with options like Absorption Correction, Angle Correction etc. These
operations can be performed to all the files of serial measurement or to files
selected in the batch file list. When the operation menu item are displayed in
the batch working mode or in the master working mode the icons will display a
small -symbol in the upper left corner. All the menu items can be selected
directly from the operations tool bar or the batch/master toolbar and will affect
all ranges of the opened files.
The option Absorption Correction calculates the effect of the

transmission factor input for the data collection geometry
(Transmission, Reflection or Debye-Scherrer).
The applied formulas are:
I(corr) = I(obs) . exp ( .t / cos ) for transmission
I(corr) = I(obs) / [ 1 - exp ( - 2..t / sin ) ] for reflection
For the Debye-Scherrer geometry, the tables of Weber (K. Weber, Acta Cryst. 23, 720 (1967)) are used. A cubic
spline is used twice for the interpolation between the tabulated q-values and between the tabulated R-values.
Note: The absolute intensities will be strongly affected by the absorption correction.
The usual Poisson counting statistics are no longer valid for the corrected
raw data.
If the raw data collection has been done in Transmission-mode, where the transmission coefficient can be determined
experimentally, the parameter expected by the program is I/I0, the ratio of the attenuated primary beam intensity by
the sample to the not attenuated intensity of the primary beam.
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To obtain I and I0 the user has to execute the following procedure:
1. The settings of the current (mA) and voltage (kV) have to be reduced to 20 mA and 40 kV before or after the
normal measurement.
2. The small plate in front of the PSD with the 6 aperture has to be exchanged against the one with the brass filter
by unscrewing the plastic screws and introducing the attenuator instead.
3. The primary beam stop has to be removed.
3. The sample in the flat sample holder has to be measured for at least 60 sec. with the PSD stationary at 2 = 0,
the obtained count rate is I.
4. The same measurement with an empty sample holder and the fixing ring of same diameter as the one used for
the sample has to be repeated for the same period of time. The count rate is then I0.
If the data collection was done in reflection or Debye-Scherrer-mode, the value expected by the program is R,
which has to be calculated from attenuation coefficients (one can get this value easily by using the Program
Theoretical pattern), sample density (which has to be assumed between 0.5 and 0.7, depending on how easily the
sample could be inserted into the capillary) and sample thickness (which is R, half the diameter of the capillary). R
is then calculated by * sample density * R.
Angle Correction provides a possibility to correct the angular scale of the raw data a posterior. If the user file
contains a correction polynomial created and chosen by the Peak Calibration routine, this polynomial will be applied
to the RAW data file.
Alpha2-stripping performs the Rachinger correction for data which have not been collected with monochromatic
K1-radiation. This correction removes all K2-peaks from the diagram. The option is not activated if the data have
been collected using a primary monochromator.
Deadtime correction provides a possibility to apply a dead time correction to the data. This is normally done by the
data collecting software when a scintillation counter has been used for data collection. If such a correction has
already been applied the program will give an error message. The applied formula is:
I (obs )
I (corr ) =
1 I (obs )
Fold diagram provides a possibility to fold the data, collected with an IP-PSD in symmetrical setting, around zero.
In such a way a scan range with an angular range of -55 to +60 degree 2theta resulting a scan range with an angular
range of 0 to 55 degree 2theta and doubled intensity. This option is only accessible if data collected with an IP-PSD
have been loaded.
Edit Background starts an automatic background-removal routine which may as well be altered by the user. If the
option is selected, the menu layout is changed (the Layer- , the Report- and the History panel will be hidden) and
the program displays a background editing toolbar (see below) and a background-spline function calculated from a
number of automatically selected background points.
Increase/Decrease
Smoothing Factor Stop Button
Subtract Range
Background Selection Tools
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With the first button on the toolbar a modified background file will be saved. With the next two buttons the smoothing
of the background spline can be altered. The Range to be edited can be chosen with the next buttons. The Ok
button on the right side of the toolbar will end the editing of the background. If the background was edited, the user is
asked if the changes should be kept.
There are three options for the user to change the background generated by the program:
By left-clicking on one of these points, they may be moved to any position in the diagram and - by releasing the
mouse button again may be placed at a different location. The spline function will be automatically re-calculated.
The very first and very last point of the diagram may not be shifted in their position, but may only be altered in their
height.
By double-clicking anywhere in the diagram, an additional background point is inserted and the background - spline
re-calculated.
By either clicking on the toolbar buttons or by hitting the + / - keys on the numeric keypad, the degree of smoothing
of the spline function is changed. By increasing the smoothing further and further, a straight background in the form of
a linear regression will be obtained. By decreasing the smoothing factor further and further, the background will follow
exactly through all background points, sometimes tending to overshoot between the points.
When the background line has been defined, the Subtract Background button may be used to create a raw data file
with the background-corrected data. The default extension for background-subtracted data is *.rmb.
When the Stop button is pushed, the background selected so far is stored in the original raw data (without changing
the original data). Subsequently, the normal graphics menu bar is restored.
Note: The .background points will be lost after applying other operations. To store
the background points for using them in other programs like Fit, the file has to
be saved directly after calculation and editing the background points.
If background editing is selected in the batch- or master working mode only a dialog
will appear (shown on the right) where a Background Smooth Factor can be defined
and it can be selected if the background correction should be applied directly to the
file (a background spline will be calculated and subtracted from the data of the file
and the file will be saved afterwards) or if only background points will be calculated
and saved in the file (to edit the background afterwards with programs like Fit).
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If the option Smooth Diagram is selected, the menu layout is changed (the Layer , the Report and the History
panel will be hidden), the program displays a smooth editing toolbar (see below) and a preview of the range data after
applying the smooth function.
Editing Tools for
Parameters Stop Button
Apply Smooth Range

Function Selection Tools
The smoothing is done according to an algorithm described by Allmann (see below). The parameter for this algorithm
may either be input as the average peak half width (in degrees 2) from which the program calculates the number of
points by dividing it by the data step width or directly as the number of data points to be used.
With the Apply Smooth Function button the algorithm will be applied to the data and the newly created data will be
saved. The default extension for a smoothed raw data file is *.rsm. When the Stop button is pushed the program will
end the preview mode for smoothing.
If Smooth is selected in the batch- or master working mode only a dialog will
appear (shown on the right), where the two factors can be defined. After pressing
the OK button the smooth algorithm will be applied to all selected files.
R. Allmann, Smoothing by digital filters and a new peak search routine. EPDIC 2, Mat.Sci.Forum 133-136, 323 (1993)
R. Allmann, Rntgenpulverdiffraktometrie, Clausthaler Tektonische Hefte 29, Verlag Sven von Loga, Kln 1994
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8 Pattern Fitting
8.1 Introduction
The Pattern Fitting routine is used to determine profile parameters and integrated intensities from observed powder
patterns. A variety of constraints makes it possible to achieve meaningful results even for complicated patterns. The
program is started from the Raw Data pull-down menu of the WinXPOW main menu.
The menu items of the Pattern Fitting routine comprise File, Parameters, Operations, View, Options, and Help.
The left-hand side of the status bar usually displays the cursor position, the right-hand side the statistical descriptors
of the most recently run least-squares-fitting.
8.2 File
The File-menu item offers the standard Windows utilities to read and write files, to re-open recently used files and to
print the results.
WinXPOW 3.05 Software Manual Pattern Fitting 8-1

8.2.1 New
Deletes all loaded data from memory but keeps parameter settings like Overall Parameters or view parameters.
8.2.2 Open
Reads the contents of an existing file - either a peak or raw data file - into the program. After opening a file, its name
is displayed in the title bar of the main program window. To perform a pattern fitting, at least a raw data file must have
been opened. If no peak file is read, a peak list can be generated with the Find Peaks option described in chapter
8.4.1.
8.2.3 Read ICDD Data

Importing a peak list from an installed ICDD database. This item is activated only if an ICDD database is installed.
8.2.4 Save As
Lets the user write the current peak list to a file. This may either be an existing or new *.pks file or a file having the
STOE peak file format but the extension *.pft denoting that the contents of this file have been generated by the
pattern fitting routine. Also, the calculated step intensities may be written to a raw data file with extension *.rft.
8.2.5 Update Raw File

Can be used to store the background line defined with the option described in chapter 8.4.3. to the raw data file
currently loaded. This item is disabled if a raw data file which was measured under GMP was opened in an not GMP
controlled enviroment.

8.2.6 Print / Print Preview / Print Setup
Control and format the output of the current graphic display to the system printer.
8.2.7 Export Graphics

Provide an opportunity to create files in different formats for importing the display into other applications. The user
can choose the desired format with the combo box Save as type. The available formats are Enhanced Metafile
(which will be the most adequate format when importing the display into other applications), TIFF- and Windows
Bitmap file. With deactivated option only Diagram(s) the output will be identical to the printed version, otherwise
only the diagram itself will be exported. The default behaviour is to rescale the display to a DIN-A4 page, regardless
of the current aspect ratio of the display. To maintain the current aspect ratio the keep aspect ratio option should be
activated.
8.2.8 Recent File List

The most recent file list contains the names of the eight most recently used file names for quick re-loading.
8.2.9 Exit
Terminates the Profile Fitting routine and returns control to the WinXPOW main menu.

8.3 Parameters
provides input facilities for all parameters concerning the fit of modelled data to observed data.
8.3.1 Overall Parameters

This dialog box is used to define the kind of background function, the kind of wavelength used to collect the diagram
nd the 2theta-dependent asymmetry function of the peak profiles.

The background function of the diagram may be defined either as a series of Tschebyschev polynomials or as a
conventional power series, which may be selected by radio buttons. The Tschebyschew polynomials are usually more
robust and mathematically better behaved than a power series representation.
The maximum order for both kinds of function is proposed by the program as the 2theta-range of the diagram
divided by 20, but not exceeding 6. It may be changed by the user and should, if in doubt, rather be given too small
than too large. For short 2theta regions ( 5-10 ), the maximum order should be set to 1 (= linear background) to
avoid artefacts of the background function. For a strictly horizontal background line varying only in height but not in
inclination, max. order is set to 0.
Usually, there will be no need to change the background coefficients and their fixation. In the beginning, all
coefficients should be allowed to vary. If a convincing background representation has been found, but the refinement
is not quite stable, all coefficients may be fixed with the Fix all button leading to a background line not varying with
the peak parameters. Individual terms of the background representation may be fixed as well using the corresponding
check boxes.
The empirical background as defined with the Operations Background option (see chapter 8.4.3) may be taken
into account during refinement or not. If Add empirical background is checked, this user-defined background line
will be added to all calculated intensities thus preserving correct counting statistics and weights. The user-defined
background line will never be refined. If the user-defined background alone shall be used to account for the
background line, the (refineable) polynomial representation may be switched off by setting its maximum order (see
above) to -1.
The monochromatisation of the primary beam may be selected with the Add Alpha2 peaks checkbox. For
diagrams collected with a primary monochromator and thus pure Kalpha1-radiation, it must not be checked. If it is
checked, the intensity ratio alpha2/alpha1 may be entered (usually 0.5) and may be either fixed or refined. Having the
intensity ratio refined usually leads to a smaller R-value, but is only advisable if a large portion of a diagram is fitted
simultaneously. If the fitting region contains only a few peaks, closely spaced peaks may be missed and ascribed to
an incorrect intensity ratio.
Peak asymmetry is described by a modification of the method of Finger et al. (Finger, J.Appl.Cryst., 31, 111, (1998)
and Finger,Cox & Jephcoat, J.Appl.Cryst. 27, 892 (1994)). Finger's original approach uses two (physically significant)
parameters H/L and S/L to describe the 2theta-dependent asymmetry of all peaks. For data collected on the STOE
diffractometers, one parameter defined as the average of the two original terms was found to describe the asymmetry
equally well: the value of this parameter must be between 0 and 1. Values outside this range written in the user file
will be reset to 0 on the successive start of the application. As the algorithm involves convolution of profiles, it is quite
time-consuming. Therefore, the number of steps used for the numerical integration of every data point of a peak
profile may be varied. Usually, values around 50 work both reasonably accurate and reasonably fast. In the early
stages of refinement, the asymmetry parameter should either not be used or be fixed to a known value specific for the
measuring parameters.
8.3.2 Peaks
The dialog box Edit Peaks is used for the definition of profile parameters for individual peaks or a set of peaks
defined as a group. A group has identical profile shape and other relevant group-properties described in 8.3.3. Every
peak belongs to exactly one group; a group number of 1 assigned to a peak will exclude this peak from all
calculations during the refinement.
The main list box in the centre of the dialog box displays all peak data for the current refinement problem. The
refinement flags are indicated by V (for variable) or F (for fixed) after the parameters. By left-clicking on one of the
lines it becomes highlighted and the peak data from that line are transferred to the four edit boxes and three
corresponding check boxes at the top of the dialog box. In these boxes, the parameters and their refinement flags
(fixed or not) may be changed. When the changes are done, pressing the Replace button moves the new
parameters back into the main list box. Pressing the Delete button while one of the peaks is highlighted removes it
from the peak list. Clicking on the Insert button adds the peak data currently in the edit boxes to the peak list.
Caution : Having two identical peaks in the peak list will result in a singular least-squares matrix.

The refinement flags may also be changed en-suite: While a peak ( or several peaks selected by Shift- or Strg-
leftclicking ) is highlighted, the Free Peak button will set all three individual refinement flags for position, intensity
and width to variable, whereas the Fix Peak button will fix all three parameters. The Fix all and Free all buttons
refer to the parameter in the column beneath which they are positioned; pressing the first Fix all button will e.g. set
the position of all peaks in the list to fixed; whereas pressing the last Free all button will set all FWHMs to variable.
The Delete - button is used to remove all peaks having a group number of 1 (and therefore excluded from
calculations) permanently from the list. The Reset - button changes all group numbers from 1 to 1 thus including
these peaks into calculations again.
Edit Group provides a shortcut to the Edit Group dialog box described in 8.3.3.
Set Group is useful to assign a group number to several peaks simultaneously: After selecting the peaks by Shift- or
Strg-leftclicking, a group number may be entered into the group number edit box which will be transferred to all
currently highlighted peaks when pressing the Set Group button.
The Go To button is only active if the graphic display has been zoomed and does not show the whole diagram. By
clicking on the GoTo button the graphics display will be scrolled so that the currently highlighted peak in the list box
is within the visible part of the diagram.
The 'Close' button closes the dialog box. It may, however, be left open during refinement. The peak data are then
automatically updated during cycles.
8.3.3 Groups
The Edit Groups dialog box is used to define group properties which are common to all peaks within this group.
The profile function may be selected from the radio-buttons either as Pearson or Pseudo-Voigt. The simpler
Lorentzian, squared Lorentzian and Gaussian functions may be chosen by selecting a Pearson type profile with a
fixed profile parameter of 1, 2 or above 10, respectively. For the mathematical definitions of these functions see
chapter 11.3.3.

The edit boxes and check boxes are used to enter parameters and refinement flags. These settings are transferred to
the currently selected and highlighted group by pressing the Replace button. Pressing the Insert button will add a
new group to the list with the properties defined in the edit and check boxes. Delete removes the highlighted
group(s) only if the group number is currently not assigned to any peaks.
The Fix Group and Free Group buttons are used to change all refinement flags of the group simultaneously. In
contrast to the change of individual refinement flags using the check boxes, these changes are automatically
tranferred to the group list box and need not be activated by Replace.
The Profile Parameter is either the Pearson exponent (which must exceed 0.5) or the Gauss mixing parameter
(between 0 and 1) depending on the choice of the profile function (see chapter 10.3.3 for the respective formulas).
The profile shape is always the same for all peaks in a group and may be either be set to Fixed or varied during
refinement.
The Intensity factor, Zeroshift and Halfwidth of a group are only refined if peak intensities, positions and halfwidth
of all peaks in this group have been respectively fixed in the Edit Peaks dialog box regardless of the setting of their
group refinement flags. These three parameters are used together with the individual peak parameters, i.e. the
integrated intensity of a peak is the individual peak intensity multiplied by the group intensity factor; its position is the
individual position plus the group zeroshift; and its FWHM is the sum of the individual halfwidth and the group
halfwidth. The interplay between individual peak parameters and group parameters allows e.g. the fixation of an
intensity ratio of two peaks by assigning only these peaks to one group, entering their intensities manually, fixing the
intensities in the Edit Peaks dialog box and then refining the intensity factor for the corresponding group.
The Normalize buttons allow the transfer of the group parameters to the individual peak parameters of all peaks
belonging to the selected group; i.e. normalizing the intensity factor will multiply all individual peak intensity by the
factor and reset it to 1; normalizing the zeroshift (halfwidth) will add the zeroshift (group halfwidth) to all peak
positions (peak halfwidths) and reset it to 0. The only exception from this rule is described below.
The peak halfwidths of all peaks in a given group may also be refined as a function of 2Theta using the Cagliotti
formula if Halfwidth as function is checked. In this case, the individual halfwidths of peaks belonging to the group
are totally ignored. When normalizing the halfwidths, the individual halfwidths are therefore discarded and replaced by
the halfwidths calculated from the formula. The three parameters, which may also be individually fixed or varied,
correspond to U, V, and W in the formula

FWHM 2 = U . tan2 + V . tan + W
8.3.4 Regression
This dialog box defines some optional properties of the non-linear refinement.
Termination of the refinement is controlled by the Convergence
limit and the Maximum number of cycles. The convergence limit
is the maximum relative difference of 2 - values of two subsequent
cycles so that the refinement is considered converged and
terminated.
If Linear regression before nonlinear is checked, one linear cycle
is calculated every time a non-linear refinement is started. This
option helps to keep refinements stable.
Draw diagram after each cycle may be used to switch on and off
the on-line display of calculated curves after each refinement cycle.
Add empirical background is used to include background
previously defined using the View-Background option. This check
box is the same as in the Overall Parameters dialog box and is
explained there (chapter 8.3.1).
The Weighting scheme can be chosen from unit weights, 1/I and
1/I. The usual weighting scheme arising from the Poisson counting
statistics is 1/I.
The Stepwidth for simulated pattern affects only the Simulation operation, i.e. the calculation of a raw data
diagram from given peak and overall parameters without taking into account observed raw data.
The edit and check boxes belonging to the Check abnormal FWHM field are used to set up an automatic exclusion
of those peaks from further calculations, which have been distorted during the refinement. All peaks having a
halfwidth less than Min.(%) of the average halfwidth or exceeding Max.(%) of the average FWHM are assigned a
group number of 1, if Exclude abnormal peaks is checked. The group number of 1 indicates a peak which is not
to be used in further calculations (see 8.3.2).
The same happens to peaks below a certain integral intensity level, if the box Exclude peaks with intensity < is
checked. The required minimum intensity is entered in the corresponding edit box.

8.3.5 Regions
The default fit region is the whole measured pattern. If however, only portions of the diagram shall be fitted, the
Regions dialog box is used to define them. The list box contains the currently defined regions, which may be selected
using the left mouse button. The region input into the edit box at the top may be moved into the list box by three
possible actions:
Insert adds the new region to the others taking into

account possible overlap and combining two
overlapping regions into one larger region.
Replace discards the currently highlighted region and
replaces it with the new region again testing for
overlap with other regions.
Exclude cuts the region in the edit box from the appropriate
region(s) in the list box creating if necessary two
regions out of one.
Delete removes the highlighted regions from the list.
Delete All removes all regions.
The 2theta and D-space buttons are used to define the units in
which the regions are defined and displayed.
8.3.6 Load / Save Parameters
The Save Parameters could be used to store a set of parameters ( peaks, regions, background, groups ) for later
use. The parameters are stored in files having the extension *.par. A previous stored parameter set could be reload
with the Load Parameters option, overwriting all current parameters.

8.4 Operations
The Operations pull-down menu comprises all commands starting calculations with peak or raw data.
Most of these commands are also available from the following toolbar buttons :
Si = Simulation = Edit Peaks
S = Scaling
L = Linear Regression = Edit Background
N = Nonlinear Regression
N1 = one cycle of nonlinear regression

8.4.1 Find Peaks
Find Peaks opens a dialog box from which a peak search in the loaded raw data can be started. Peaks previously
loaded are discarded.
Estimated Halfwidth : An approximate value for the peak halfwidth
must be given. This parameter can be used to discern between sharp
and broad peaks. When both kinds of peaks are present in a diagram, it
is usually impossible to identify both classes of peaks in one run of the
peak search. A good value for data collected with the linear PSD or IP-
PSD is 0.15, while for data collected with the Mythen1k detector a
good value is 0.08.
Significance Level : The significance level sets a lower limit to the
peak heights; it is defined as the ratio of the maximum peak intensity to
background. Peaks which are found by the slope criterion, but have a
peak height below the given significance limit, will be discarded.
Intensity Limit : The intensity limit is an additional criterion applied to a
peak identified in the peak search algorithm. All peaks having an
absolute height less than the input value will be discarded. Setting it to
0 will accept all peaks matching the significance criterion, values above 0 will increasingly reduce the number of
peaks found.
Remove Alpha2 Peaks : Checking this box will scan the peak list for pairs of Alpha1/Alpha2 peaks and discard the
Alpha2 reflection. To match the Alpha1/Alpha2 criterion, the peak position of the second peak must be within 0.02 of
the theoretical Alpha2-reflection as calculated from the Alpha1-position and its intensity must be between 45 and 55
% of the corresponding Alpha1 peak.
Remove Spikes : When this box is checked, a search for peaks of abnormal halfwidth will be performed in the peak
list which passed the other criteria. Peaks of a halfwidth less than 25% of the estimated halfwidth defined above will
be discarded as spikes.
The Defaults button loads reasonable values for the above edit boxes.
By pressing the OK button the peak search is started. When it is finished, the peaks found are displayed in the
graphics window and are written to the peak list accessible from the Parameter - Peaks option.
8.4.2 Edit Peaks

If the Edit Peaks option is activated (visible either by the depressed tool button or the check mark in front of the pull-
down menu option) interactive changes to the peak list may be made by mouse-clicks on the diagram. The relevant
conventions are as follows :
Double-clicking anywhere in the diagram while the cursor is the usual arrow inserts a new peak with the according
2theta - position and intensity and the average FWHM of all peaks in the region into the peak list.
Moving the cursor in the vicinity of an existing peak changes it to a cross. As long as the cursor is in this shape, the
peak may either be moved by drag-and-drop to change peak position and/or intensity or can be deleted from the peak
list by right-clicking.
Caution : When trying to zoom in while this option is active may lead to accidental movement of peaks when the fact
that the cursor changes his shape to a cross is ignored.

8.4.3 Edit Background
This option is used to define a background line independent from the polynomial representations used for refinement.
This empirical background line may then either be used in addition to the refineable background or instead of it (see
Overall Parameters, chapter 8.3.1).
If the Background option is applied for the first time during a session, the program proposes reasonable background
points. The number of these points differs between 2 and 16 depending on the number of pattern data points. The
maximum number of background points is 64. If the raw data file already contains background information from a
previous background run ( either in Graphics or Profile Fitting ), the stored background points will be loaded and
displayed.
If there are at least 3 background points a background curve is shown which is computed by a smoothing cubic spline
interpolation routine.
The number, positions and intensities of the background points may be changed by mouse-click. The two points at
the left and right border of a pattern are not deletable, but they can be moved vertically. Double-clicking anywhere in
the diagram while the cursor is the usual arrow inserts a background point at the cursor position and recalculates the
spline function. Moving the cursor in the vicinity of an existing background point changes the cursor to a cross. As
long as the cursor is in this shape, the background point may either be moved by drag-and-drop to change its position
or may be deleted by right-clicking. The background function will again be recalculated.
Pressing the key of the numeric keypad reduces the smoothing of the background curve. The smallest possible
smoothing causes the background curve to match the background points exactly.
Pressing the + key of the numeric keypad increases the smoothing of the background curve. The largest possible
smoothing causes the background curve to be a straight line which need not match the background points.
When the background has been described in a satisfying way, it is possible to store the background function in the
raw data file using the Update Raw File command from the File pull-down menu.
8.4.4 Clear Background

removes the information set up in the 'Edit Background' option; i.e. zeroes the observed background line.

8.4.5 Simulation
This option calculates a diagram using the overall, peak, and group parameters as currently defined and displays it.
No changes to the parameters are done. The option is useful if the type of peak profile or background line are totally
unknown. Trying different settings out helps in getting reasonable starting values before starting the refinement
cycles.
8.4.6 Scaling
This option refines only the background line but takes into account overall, peak, and group parameters as currently
defined. The option can be used at the beginning of a refinement to provide the program with a reasonable
background estimate. The background parameters must of course have been allowed to vary in the Overall
Parameters dialog box.
8.4.7 Linear Regression

This option refines only peak intensities and background but leaves peak positions, halfwidths and profile parameters
fixed. This kind of refinement should be run between the scaling and the nonlinear routine thus eliminating the danger
of oscillations during the early stages of refinement.
8.4.8 Nonlinear Regression

This option starts the complete refinement of all parameters which have not be fixed explicitly or which are fixed by
group considerations ( see 8.3.3 ). Depending on the settings in the Regression dialog box explained in 8.3.4
additional actions will be taken, e.g. eliminating peaks of a too narrow or too large halfwidth from consideration.
During calculation, the statistical descriptors of the refinement will be updated in the right-hand side status bar. To
interrupt calculation, click on the red traffic light button in the tool bar.
8.4.9 Integrate regions

This option opens a dialog window similar to the Regions
window described in 8.3.5. The regions selected so far are
displayed in a list together with the integrated peak intensity
in this region which is calculated as the sum of all intensity
values in the region minus a linear background calculated
from the n leftmost and rightmost points of the region. The
parameter n may be entered in the edit box below the list box.
The default value for n is 10. After changing the number of
background points, the integral intensities are re-evaluated if
the Calculate button is pressed.
Save Result lets the user save the integration results in a
text file.
This option is useful, if peak shapes are quite irregular and
cannot be simulated by any of the analytical peak shape
functions.

8.5 View
In the pull-down menu View commands affecting the layout of the window are combined.
8.5.1 Clear
removes all calculated lines from the display leaving only the observed raw and peak data.
8.5.2 Regions
must be checked if a bar beneath the x-axis shall display the regions defined as explained in 8.3.5. If this mode is
active, it is also possible to re-define the regions by moving the cursor to the region bar. When the cursor is
positioned on the beginning or end of a region, it turns into a bidirectional arrow and moving it by drag-and-drop
extends or truncates the region accordingly. If the cursor is positioned inside a region, it turns into a cross and similar
drag-and-drop action will remove the defined parts from the region.
8.5.3 Difference
must be checked so that a splitter window beneath the diagram shows the difference plot.
8.5.4 Position Info

must be checked in order to have the cursor position continuously updated in the left pane of the status bar. This
option is also accessible through the toolbar button .
8.5.5 Grid Lines

switches an underlying grid for the diagram on and off. This option is also accessible through the toolbar button .

8.5.6 Whole Diagram
resets a zoomed image to the display of the complete pattern. As long as the button is depressed, it is possible to go
back to the zoomed state by releasing the button by clicking on it. This option is also accessible through the toolbar
button .
8.5.7 Toolbar
switches the toolbar on and off.
8.5.8 Status Bar

switches the status bar on and off.

8.6 Options
The Options menu comprises commands affecting the display of the main window as well as tools for recalling
parameters from previous fit runs and storing parameters temporarily.
8.6.1 Edit File Title

allows the user to change the diagram title which is displayed and printed. The File Title will be also used as title for
the .rft file. If the checkbox Copy File Title to RAW file is checked ( ), the title will be copied also in the .raw
file the next time the user performs an Update Raw File.
8.6.2 Set fit. as obs. Pks

replaces the observed peak list with the refined peak list. The observed peak list are the starting values provided
either by reading a peak file or by executing the PeakSearch option. This list is not accessible to the user after
refinements, but may be displayed in the graphics depending on the Window settings shown below. It is only kept
for comparison reasons of the type before / after refinement.
8.6.3 Save FitParam

produces a copy of the current parameter list in the memory which may later be re-loaded. This is useful to recover
parameters which have become unreasonable during a refinement run.
8.6.4 Reset FitPara_X

The X in the command may be one of the characters P, S, L, N or 1 referring to the resetting of parameters
before a simulation, scaling, linear, non-linear or 1 cycle of non-linear run.

8.6.5 Graphics
opens a dialog box where the layout of the program window can be set up. The display of all curve types may be
switched off and on and the size and viewport of the splitter windows defined.
.
8.6.6 Colours
opens a dialog box where the colours associated with the different observed and calculated curves may be edited.
The functionality is the same as in the Colours option of the graphics program described in 5.4.2.

9 Peak Calibration
9.1 Introduction
The module Calibrate Peaks allows the user to calculate correction terms for the 2theta scale of data collected with
an internal standard or otherwise known peak positions. While the program deals only with peakfiles, it can however
store a correction term in the userfile which may be used to correct raw data files with the Raw data handling module,
which is accessible from the Raw Data - pull -down - menu of the WinXPOW main menu.
The 2theta errors and the correction curves are shown in a diagram. The program can use polynomals up to order
four or splines to calculate correction terms.
9.2 Files
comprises options to load peak files into the program, to save corrected peak lists and to print out data from the
program.
Open is used to load the two required peak-sets into the program: One peak file containing the observed peak data
and one set containing the standard peak-set ( or the whole
sample in case the correction polynomial is to be used as
an external standard ). By choosing Peak file the standard
peak-set is read from a peak file, while choosing ICDD
Database this set could be loaded from an ICDD database.
The browse-buttons provide the standard Windows
function for file selection.
Save and Save As lets the user write the calibrated peak list either to the very peak file from which the observed
data have been read or to a peak file of another name. Both items are only activated if the observed peak list has
been changed either by the automatic calibration routine or the Calibrate Peakfile command.
Print - Print Preview - Print Setup control and format the output of the current graphic display to the system
printer.
Export Graphics provide an opportunity to create files in different formats for importing the display into other
Enhanced Metafile (which will be the most adequate format when importing the display into other applications), TIFF-
and Windows Bitmap file. With deactivated option only Diagram(s) the output will be identical to the printed version,
otherwise only the diagram itself will be exported. The default behaviour is to rescale the display to a DIN-A4 page,
WinXPOW 3.05 Software Manual Peak Calibration 9-1

regardless of the current aspect ratio of the display. To maintain the current aspect ratio the keep aspect ratio
option should be activated.
The most recent file list contains the names of the six most recently used file names for quick re-loading.
Exit terminates the peak calibration routine and returns control to the STOE main menu.
9.3 Match Peaks
This command scans the two peak lists calibration peaks and observed peaks - for peak pairs which lie within a
given 2 window. A dialog box allows the input of two parameters :
The Intensity limit is a cutoff-value below which the

program will ignore all peaks from both the calibration
and the observed peak files. The 2 window is the 2
range around a calibration peak which the program will
search for matching observed peaks. If more than one
observed peak is within the 2theta window, the peak
closest to the calibration peak will be assigned to it.
Clicking the OK Button will start the matching routine.
When the program has assigned pairs of calibration / observed peaks, the results are displayed in the main window
and may be altered manually by the user ignoring the parameters described above. In addition, the resulting peak
pairs and their deviations are shown in a child text window :
The File menu of this text window contains the standard Windows Print, Print Preview and Print Setup printing
commands.

In the upper part of the main program window the matching peaks from the measured peakfile will be shown in red
while the rest of the observed peaks will be drawn in gray. The calibration peaks will all be drawn in blue. Around the
calibration peaks the 2 window is shown as a light gray rectangle.
Zooming can be performed by leftclicking and dragging the appearing rectangle to the required size, then releasing
the left mouse button. The toolbar buttons with the arrow and crosshairs provide the possibility to switch on position
information output in the left status pane and to go back to the display of the full 2 /intensity range from a zoomed-in
state, respectively.
The peak pairs thus displayed may be edited in a very easy way by pointing the cursor at them and clicking on the left
or right mousebutton :
If you wish to connect a measured peak to a calibration peak, first
select the calibration peak by pointing at it with the cursor and
pressing the left mouse button. The cursor shape will be altered
indicating that you are now editing a peak pair. In addition, the text
in the status bar will tell you so.
Now select the measured peak to which you want to attach the
calibration peak by pointing at it and pressing the left mouse button
again. This operation may as well be used for peaks already in use
as for peaks which are yet unassigned. In the former case, the new
manual assignment will override the old one. CAUTION: you are
not limited in your assignments by the parameters you entered for
the peak matching routine!
To delete a connection between a calibration and a measured peak
point at the calibration peak und press the right mouse button.
If peak pairs have been edited, the calibration polynomials have to

be re-calculated as described in the next chapter.

9.4 Calculate
9.4.1 Calculate polynomials
This command calculates the 2-offset defined as the position of a calibration peak minus the position of the
matching observed peak for all peak pairs and performs a least - squares fit to the 2-offset against 2 with
correction polynomials up to order 4.
If there are less than 3 pairs of peaks the program will refuse to calculate any polynomals and issue an error
message.
In this case, after clicking the OK-Button, another Match Peaks run with a different set of parameters may be started
or more peak pairs may be added manually.
After calculation of the correction polynomials, the results are shown in the lower part of the main window. The 2theta
offsets for all peak pairs are shown as black squares and the calculated correction polynomials as curves of different
colours. The data should be checked for consistency; e.g. the example below might require checking of the two peak
pairs around 2 = 50 as they look like outliers on the polynomial curves.
9.4.2 Calculate spline
This command calculates the 2 - offset defined as the position of a calibration peak minus the position of the
matching observed peak for all peak pairs and performs a least - squares fit to the 2-offset against 2 with a spline.
This method is used to calculate a 2theta correction for a IP-PSD detector.

After calculation of the correction spline, the results are shown in the lower part of the main window. The 2theta
offsets for all peak pairs are shown as black squares and the calculated correction splines as a blue curve. The spline
smoothing factor could be adjusted with a floating dialog. The factor could be changed by moving the arrow or by
typing a factor into the dialog an pressing the C-button.

9.5 Calibrate peakfile
This command applies the correction polynomial selected by the user to

all peaks in the loaded range of the observed peak file. The polynomial
showing the smallest 2 value ( i.e. the best fit with the smallest number
of parameters ) is highlighted as the default in the edit list. The user
may, however, choose any polynomial from the list to be applied. By
clicking on the OK-button, the 2 - and d-values of all peaks in the
selected range will be shifted by the amount calculated from the
selected polynomial.
The modified peak list will not be written directly to the file, but must be
saved using the Files suboption Save or Save As.
In addition, the selected polynomial is automatically written to the user
file and may be used in the Raw Data Handling module to correct the
raw data file ( from which the observed peak data have been taken ) as
well by selecting the 2Theta correction option. If the polynomial is to be used as an external standard, it may also be
applied to other raw data files.
9.6 Auto calibrate
This option performs all three steps described above automatically. No user input is allowed / required. The
calibration polynomial used to re-calculate the observed peak list ( which is also automatically written to the user file
for subsequent 2-correction of the corresponding raw data ) is the one showing the smallest 2 value of all
calculated polynomials. The user file is updated with the polynomial with minimum 2, too, but the peak file will not be
updated automatically and requires saving using the Files suboption Save or Save As.
9.7 Write IP calibration
This option is only available if a spline had be used to calculate a calibration curve. With this option the calculated
spline could be stored into the Instrument Parameter file (IPR-file) to be used as a IP-PSD calibration. This command
only stores the spline into the Instrument Parameter file but did not activate the use of the calibration. This is be done
with the program Instrument Parameters.

10 Index & Refine
10.1 Introduction
The Index & Refine module comprises three indexing routines and a lattice parameter refinement option.
The implemented indexing algorithms are based on
Werners TREOR program (see e.g. P.-E.Werner, L.Eriksson, M.Westdahl, Journal of Applied
Crystallography 18, 367 (1985) )
Vissers ITO routine (see e.g. J.W.Visser, Journal of Applied Crystallography 2,89 (1969) )
Lours DICVOL program (see e.g. A.Boultif, D.Lour, Journal of Applied Crystallography 37, 724
(2004) ).
File contains the standard Windows options for opening, saving and printing files and.
View is used to control the layout of the main window.
Index contains a property page for the setting of the indexing parameters and the starting commands for
the indexing routines.
Refine opens a dialog box for the definition of the lattice constants refinement parameters and starts the
refinement routine.
WinXPOW 3.05 Software Manual Index & Refine 10-1

10.2 File
10.2.1 Open
reads the contents of an existing peak file (default extension *.pks or *.pth) into the program. When a peak file has
been opened, its name is displayed in the title bar of the programs main window.
10.2.2 Save As
stores the outcome of the lattest indexing / refining to a peak file and a list file. The peak file name may be the same
as the one used for reading the observed peaks. The list file contains all results as displayed in the child text window
and has the same file name as the peak file and an extension signifying the type of routine used to produce the
output : Output from Werners routine is called *.lwr, output from Vissers routine *.lvs, output from Lours routine *.llr,
output from lattice constants refinement *.lrf.
In the case of Werner indexing or lattice parameter refinement the peak file is updated by the symmetry and
spacegroup information, the calculated lattice constants and the peak indices.
10.2.3 Print List File

sends the current contents of the text child window to the default printer.
10.2.4 Most Recent File List

the Most Recent File List contains the names of the files most recently opened.
10.2.5 Exit
terminates the application and returns control to the WinXPOW main menu.

10.3 View
The View menu contains options controlling the layout of the application.
10.3.1 List File

is used to open and close the child text window containing the results from the indexing or refining routines.
10.3.2 Graphics Update

when not activated, Werners algorithm will not update the lower window with the currently checked solution during
the indexing. This will speed up the search a little.
10.3.3 Toolbar
is used to switch off and on the display of the windows toolbar.
10.3.4 Status Bar

is used to switch off and on the display of the windows status bar.

10.4 Index
Parameters opens a property page for the input of the control parameters for the three indexing routines.
Run Werner, Run Visser and Run Lour start the selected indexing routine. These commands are
also available from the toolbar buttons W,V and L.
10.4.1 Indexing Parameters for Werners algorithm (TREOR)

The control parameters defining Werners algorithm are :
Max.cell edge defines the maximum length of a,b or c (in Angstrom) which a possible solution may
have.
Max.cell volume defines the maximum volume (in Angstrom3) which a possible solution may have.
Together with the Max. cell edge this parameter strongly influences the number of
possible solutions and thus the execution time of the routine.
Max. # of peaks allows the user to limit the number of peaks used for the trial indexing to the first n
peaks with the smallest 2Theta-values in the peak list. As peak positions at higher
angles may be incorrect due to peak overlap, it may be advisable to use a smaller
number of peaks.
Independent of the number of used lines, the algorithm uses only the first 20 lines to
find a possible solution. After refinement of a possible solution against these 20 lines
the observed and calculated peak positions are compared again, this time using ALL
lines in use. Then the number of unindexed lines (calculated from ALL used peaks)
and the figure-of-merit used peaks are checked against the requested input values.
Only if the number of unindexed lines is smaller and the figure-of-merit larger than
requested, the solution is displayed.
2Theta window defines a matching pair of observed and calculated peaks. If the absolute difference
between an observed peak position and a calculated peak position is less than the
2Theta window (in degrees), the observed peak will be considered indexed. This
parameter strongly influences the number of possible solutions and thus the
calculation time. 0.05 is usually a good value.
Unindexed lines is the permissible number n of peaks which do not match any calculated peak
belonging to a certain solution. If more than n observed peaks are unindexed, the
solution will not be displayed. The value should not exceed 5 and should be set to 2
for standard data.
Peak intensity limit eliminates all peaks with a relative intensity less than the Peak intensity limit from the
calculations regardless of their 2theta position. This option is useful for obtaining at
least a sub-cell of a superstructure by eliminating the weak reflections or to index a
sample with a suspected high number of spurious lines.
The reason for eliminating peaks must of course be a good one and the outcome of
the indexing treated as a possible approximation of the correct solution !
This parameter is the only one which is automatically transferred to the property
sheets of the other indexing algorithms as it is more a function of the quality of the
input list as of the algorithm.
Required FOM is the minimum figure-of-merit as defined by de Wolff (Journal of Applied
Crystallography 1 (1968) 108) which a solution must have in order to be displayed on
the screen. The de Wolff - FOM is calculated by M20 = Q20 / ( 2 * * N20 ) where
Q20 is the Q (=1/d2) - value of the twentieth observed line, the average deviation
between observed and calculated Q-value of the first 20 lines and N20 the number of
calculated lines up to the twentieth observed line. Due to the lattest parameter, the
FOM is inversely proportional to the cell volume. Therefore, very large cells like
zeolites will seldom have FOMs larger than 1 or 2 regardless of the data quality. In
these cases, the required FOM must be lowered to 1, whereas in normal cases 5 is a
good choice for this parameter.

Crystal system is the crystal system in which a solution is initially sought. If no solution matching the
criteria is found in this system, the next one will be searched in the order cubic-
hexagonal-tetragonal-orthorhombic.
10.4.2 Indexing Parameters for Vissers algorithm (ITO)
The control parameters defining Vissers algorithm are :

Max. # of peaks allows the user to limit the number of peaks used to the first n peaks with the smallest
2Theta-values in the peak list. As peak positions at higher angles may be incorrect
due to peak overlap, it may be advisable to use a smaller number of peaks.
Vissers algorithm treats only the first 40 lines of the input as observed data. All lines
exceeding this limit will be ignored. On the other hand, Vissers routine needs a
MINIMUM of 20 observed lines and will yield an error message when tried to be run
with an input of less than 20 lines.
calculation time. 0.05 is usually a good value.
Unindexed lines is the permissible number n of peaks which do not match any calculated peak
belonging to a certain solution. If more than n observed peaks are unindexed, the
solution will not be displayed. The value should normally be in the range from 1 to 5.

the indexing treated as a possible approximation of the correct solution ! Bear in mind
that at least 20 input peaks are necessary for Vissers algorithm.
This parameter is automatically transferred to the property sheets of the other indexing
algorithms as it is more a function of the quality of the input list as of the algorithm.
the screen. The de Wolff - FOM is calculated by M20 = Q20 / ( 2 * * N20 ) where
Q20 is the Q (=1/d2) - value of the twentieth observed line, the average deviation
between observed and calculated Q-value of the first 20 lines and N20 the number of
calculated lines up to the twentieth observed line. Due to the lattest parameter, the
FOM is inversely proportional to the cell volume. Therefore, very large cells like
zeolites will seldom have FOMs larger than 1 or 2 regardless of the data quality. In
these cases, the required FOM must be lowered to 1, whereas in normal cases 5 is a
good choice for this parameter.
Formula weight and Observed density are optional input. If the formula weight is given, the program
calculates the number of formula units per unit cell Z for each solution and writes it to
the extended output file named visser.out which is not automatically displayed on the
screen but written every time the routine is run.
These two parameters are automatically transferred between the Visser and Lour
property sheet as they are characteristics of the sample and not of the indexing
algorithm.
2Theta zero error allows the input of a known systematic zero-offset of the observed peak positions.
Even if such a shift is present, this value need usually not be given as the program
refines the 2Theta zero-point automatically and is quite robust against zero-offsets of
up to some hundredths of a degree.
10.4.3 Indexing Parameters for Lours algorithm (DICVOL)
The control parameters defining Lours algorithm are quite extensive but do not allow for any unindexed
lines. All used lines ( = lines in the peak file with a relative intensity above the peak intensity limit and
among the first n peaks where n is the user-defined maximum number of peaks ) must therefore belong to
one phase so that this algorithm can succeed.

Max.cell edge 1 2 3 define the maximum length in Angstrom for the three cell edges respectively which a
possible solution may have.
Min.cell volume defines the minimum volume (in Angstrom3) which a possible solution may have. If no
clues to the approximate volume are available, it should be set to 0.
Max.cell volume defines the maximum volume (in Angstrom3) which a possible solution may have.
Together with the Max. cell edge this parameter strongly influences the number of
possible solutions and thus the execution time of the routine.
Min. mono. angle and Max. mono. angle define the range for the monoclinic angle. A range between 90 and
125 will usually be sufficient if no clues are available.
Max. # of peaks allows the user to limit the number of peaks used for indexing to the first n peaks with
the smallest 2Theta-values in the peak list. As peak positions at higher angles may be
incorrect due to peak overlap, it may be advisable to use a smaller number of peaks.
In the case of low-symmetry patterns, this parameter is closely related to the 2Theta
window. As more and more peaks are input increasing the 2theta value of the last
peak, the program will require the 2Theta window to become smaller and smaller. If
the error message Experimental error too large! is issued from the algorithm after the
list of input lines or the output list contains no solutions at all the user may either
reduce the 2theta window or the number of lines used.

calculation time. As Lours algorithm usually needs higher-precision data than the
other two routines, 0.03 is the standard value.
the indexing treated as a possible approximation of the correct solution !
This parameter is automatically transferred to the property sheets of the other indexing
algorithms as it is more a function of the quality of the input list as of the algorithm.
the screen. Lours version of the de Wolff - FOM is calculated by Mn = Qn / ( 2 * *
Nn ) where Qn is the Q (=1/d2) - value of the last observed line, the average
deviation between observed and calculated Q-value of all lines and Nn the number of
calculated lines up to the last observed line. Due to the fact that this FOM takes into
account ALL used lines whereas Werner and Visser only make use of the twenty
innermost lines, Lours FOM usually differs significantly from the other FOMs;
however, the FOM is not an important criterion for Lours routine and may be set to 0.
Formula weight and Observed density are optional input. In contrast to Vissers algorithm, these values if
both are given - have a dominant influence on the output : the program calculates the
expected volume for one formula unit and discards all solutions which are not within a
certain error limit from a multiple of this volume ! Thus, these input values have to be
correct or should not be entered at all. If only one of these values is given, it is ignored
and the possible solutions are not narrowed down by Z considerations.
These two parameters are automatically transferred between the Visser and Lour
property sheet as they are characteristics of the sample and not of the indexing
algorithm.
Max impurity lines this is the max. number of lines the algorithm will accepted as impurity or spurious
lines. The algorithm will remove this lines and recalculate a solution.
Search for zero-point error check this parameter to let the algorithm check for an zero point error in the
input data
Refine zero point check tis parameter to perform a least-square refinement of the zero-point error
Do extended search check this parameter to perform an extended (exhausted) search in volume domains
(this option will increase the CPU time needed)
Search crystal systems : These check boxes are used to select the crystal system for which a solution to
the indexing problem is sought. Multiple choices are possible, but lead to rather long
computation times if more than one of the selected systems is lower than
orthorhombic.

10.4.4 Output from the indexing routines
Due to different implementations of the three indexing algorithms, their output handling is slightly different :
When Vissers and Lours routines have finished, they open a child window displaying their output.
Werners algorithm may be interrupted anytime by clicking the toolbar button with the red traffic light.
The possible solutions of all three routines are written into the main window and after completing the
search - the user may double-click on any of them to open a child window showing the indexing of the data
with the currently selected cell (highlighted in red in the main window).
The relevant data contained in this window like Cell parameters and Crystal System can be directly
transferred into the applications Theoretical pattern (Theo) Setup Crystal Parameters dialog box through a
Copy&Paste or a Drag&Drop operation. This operation is described at paragraph 11.3.1 of this manual.

10.5 Refine
The parameter input for the Lattice constants refinement tool looks like this :
Symmetry information may either be entered as Crystal system plus Bravais type or as the phases space
group (either in abbreviated Herman-Mauguin notation or as the space group number as defined in the
International Tables). In the Space group edit box blanks must be used to separate symmetry elements
(e.g. F 21 21 21). The monoclinic crystal system requires the unique axis being b. Rhombohedral axes are
not supported and must be transformed to hexagonal ones and the Bravais type R-Centred .
From the Lattice parameters edit fields only those necessary for the given crystal system are accessible.
Lattice constants have to be given in Angstroms.
The 2Theta window defines a matching pair of observed and calculated peaks. If the absolute difference
between an observed peak position and a calculated peak position is less than the 2Theta window (in
degrees), the observed peak will be considered indexed. During refinement, the program will try to reduce
the window as much as is possible without observed peaks becoming unindexed.
2Theta zero allows the input of a constant 2theta-error introduced by poor 2Theta-calibration of the
diffractometer. The check box Refine 2Theta zero is used to enable or disable refinement of this value
together with the cell parameters.
If Use peak file indices is checked, the starting values for refinement are not taken from the Lattice
parameter edit fields but are generated from all peaks in the peak file which are single-indexed (i.e. which
have an index triple in the line after their FWHM and do not have an M (=multiple) flag following these
indices).
Pressing the OK button starts the refinement. The results will be displayed in an automatically opened
child window. To produce a list file with the same name as the peak input file and the extension .lrf, select
the Save option of the File pull-down menu.

The refined Cell Parameters, the Symmetry information (Spacegroup if given or Crystal System and Lattice
Type) and other relevant data can be transferred through Copy&Paste or Drag&Drop to the Setup Crystal
Parameters dialog box of Theo. This operation is described at paragraph 11.3.1 of this manual.

11 Theoretical Pattern
11.1 Introduction
The Theoretical Pattern program can calculate peak positions and Miller indices from lattice constants and symmetry
information (either crystal system, Laue group or space group) as well as the full pattern from cell metrics and atomic
coordinates. To generate a full pattern, the atomic structure may be entered via the programs editing options as well
as loaded from a file.
The program is started from the pull-down menu of the main menu item Cell
WinXPOW 3.05 Software Manual Theoretical Pattern 11-1

11.2 File
The menu item File offers the standard Windows commands to read and write files, to re-open recently used files
and to print data or graphics.
The file formats that the program can read are
standard STOE parameter files for THEO with default extension *.tin (see chapter 11.2.2)
standard STOE single crystal parameter files with default extension *.crs (a slightly modified version of the TIN
format containing no atomic parameters but spacegroup and cell metrics produced by the STOE Stadi4 and IPDS
control programs)
Shelx instruction files with default extension *.ins (please refer to the original Shelx manuals for a description of
the format) are fully supported (e.g. FVAR, long form of SFAC (12 coefficients), riding hydrogens with negative U).
The spacegroup symbol is recognized from the CELL information and SYMM instructions. The CELL constants
must therefore conform to the crystal system (e.g. orthorhombic phases require all angles equal to 90.00 and
tetragonal systems require a being identical to b).
CIF files *.cif as defined by the IUCr. For an example, see chapter 11.2.1. If the file contains multiple data
blocks, that is, multiple data_datablockname keywords, only the crystal structure contained in the last
data block is used as input for the calculation. Multiple data blocks can be found occasionally in CIF files
exported by the CCDC databank.
File formats written by the program are
STOE binary raw data with extension *.rth (raw data from theoretical calculation)
STOE peak files with extension *.pth (peak data from theoretical calculation). This file contains only the peaks
whose relative intensity is larger than 0.01
plain ASCII text files containing all relevant information about peak intensities, indices, Lorentz-, polarisation-, and
absorption corrections with extension *.lth (listing from theoretical calculation)
standard STOE parameter files for THEO with default extension *.tin.

Open reads the contents of an existing parameter file - either a *.tin, *.ins, *.crs or *.cif file - into the program. After
opening a parameter file, its name is displayed in the title bar of the main program window.
Save is only activated if a parameter file has been loaded from which the file name can be taken. The program will
write / update the following files after the theoretical pattern generation has been performed:
the *.tin parameter file
an ASCII list file of the same name as the *.tin file and extension *.lth
a peak file of the same name as the *.tin file having the extension *.pth
if a full patter was generated, a raw data file of the same name as the *.tin file having the extension *.rth.
Save As lets the user write the current parameters and generated peaks (and raw data) to files of a different name.
Export lets the user generate a NBS*AIDS32 file (*.nbs) from the calculated intensities. This file can be added as a
User Card to a PDF2 database (
please refer to the Search/Match
manual for more details about PDF2
databases and User Cards ). In the
opening dialog the user can choose
the cards file and subfile attribute. Its
possible to choose more than one file
or subfile. When choosing Mineral a
Mineral name must be given.
Print Graphics - Print Preview - Print Setup control and format the output of the programs main window to the
system printer.
'Print List File' sends the current contents of the text child window to the default printer.
'Export Graphics' provide an opportunity to create files in different formats for importing the display into other
The Most Recent File List contains the names of the files most recently opened.
Exit terminates the pattern generation routine and returns control to the WinXPOW main menu.

11.2.1 Example CIF file
The following CIF file was generated by the ICSD Retrieve software and shows some typical features of the CIF
structure:
data_75107-ICSD Note: if more than one datablock (keyword data_datablockname)

is present in the CIF file, only the information present
in the last one is used by Theo
_audit_creation_date 98-12-03
_audit_creation_method 'generated by RETRIEVE 2.0'
_database_code_ICSD 75107
_chemical_name_systematic 'Dicalcium chromium tantalum oxide'

_chemical_formula_structural 'Ca2 (Cr Ta) O6'
_chemical_formula_sum 'Ca2 Cr O6 Ta'
_publ_section_title
;
Competition of covalency between Cr^III^-O and Ta^V^-O bonds inthe
perovskites Ca~2~CrTaO~6~ and Sr~2~CrTaO~6~
;
loop_
_publ_author_name
'Choy, J - H'
'Park, J - H'
'Hong, S - T'
'Kim, D - K'
_journal_name_full 'Journal of Solid State Chemistry'
_journal_coden_ASTM JSSCBI
_journal_volume 111
_journal_year 1994
_journal_page_first 370
_journal_page_last 379
_cell_length_a 5.4199(1)
_cell_length_b 5.4936(1)
_cell_length_c 7.7108(2)
_cell_angle_alpha 90
_cell_angle_beta 90.02(1)
_cell_angle_gamma 90
_cell_volume 229.6
_cell_formula_units_Z 2
_symmetry_space_group_name_H-M 'P 1 21/n 1'

_symmetry_Int_Tables_number 14
_symmetry_cell_setting monoclinic
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'1/2+x,1/2-y,1/2+z'
'-x,-y,-z'
'1/2-x,1/2+y,1/2-z'
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ca2+ 2.000
Cr3+ 3.000
Ta5+ 5.000
O2- -2.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol

_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Ca1 Ca2+ 4 e 0.007(2) 0.0390(4) 0.7504(8) 1. 0 d
Cr1 Cr3+ 2 c 0. 0.5 0. 0.726(3) 0 d
Cr2 Cr3+ 2 d 0.5 0. 0. 0.274(3) 0 d
Ta1 Ta5+ 2 c 0. 0.5 0. 0.274(3) 0 d
Ta2 Ta5+ 2 d 0.5 0. 0. 0.726(3) 0 d
O1 O2- 4 e 0.278(2) 0.301(3) 0.958(3) 1. 0 d
O2 O2- 4 e 0.299(3) 0.279 0.540(3) 1. 0 d
O3 O2- 4 e 0.919(2) 0.477(1) 0.739(2) 1. 0 d
_refine_ls_R_factor_all 0.038
11.2.2 TIN file format
The most convenient way to set up a .tin parameter file is to use the Setup options of the program and to store these
data to file. In this case, the user need not know the exact file structure. If, however, the file shall be prepared by
external programs or editors, the ASCII file format is described in this chapter.
The input file useful to perform a full pattern generation with THEO is an ASCII file of a similar format as the '*.INS' file
in the SHELX system (exception: keyword SYMM - see below). The first four characters in each line are regarded
either as a keyword or as the name of an atom in the structure. Valid keywords are:
TITL followed by a blank and any string containing up to 75 characters
WAVE followed by a blank and a chemical symbol (either Ag,Mo,Cu,Co,Cr or Fe) and the string 'a1' if K1 is to be
used or 'a2' if K2 is to be used. Alternatively, any wavelength may be given in Angstrom units.
CELL followed by the lattice constants in the order a,b,c,alpha,beta,gamma. All six lattice constants must be given
even for high-symmetry-lattices. Cell edges must be given in Angstrom units. The default setting for the
monoclinic crystal system is the unique axis being b. Rhombohedral axes may be entered if the letter R (
not case sensitive ) is appended to the space group symbol. R 3 m expects hexagonal axes and R 3 m r
rhombohedral lattice constants.
SPGR followed by a blank and a valid space-group symbol (Herman-Mauguin short form symbols as used in the
International Tables). Alternatively, the number of the spacegroup corresponding to the International Tables
may be given. The program supports all possible Bravais settings. For details of origin selection etc. see
chapter 11.3.1. For compatibility with the Visual XPOW package, the keyword SYMM may be used
synonymously.
SFAC followed by a blank and a list of up to ten chemical symbols identifying the kind of atoms present in the
structure.
UNIT followed by as many numbers as there are symbols in the SFAC line identifying the total number of atoms of
each type within the unit cell (in the same sequence as in line SFAC ).
ZERR followed by an integer identifying the number of formula units in the unit cell.
END will instruct the program to ignore any lines following this keyword.
-XYZ Any line beginning with characters which are not a keyword will be assumed to be an input line for one atom
in the structure. Following the atom identifier (1 to 4 characters) 6 values are required in the order listed
below:
n(sfac) is the position number of the atom type in the SFAC list.
xyz are the fractional coordinates of the atom.

SOF is the site occupation factor (multiplicity of the atom's site divided by the multiplicity of the general
position in the given space group). Statistical occupancy of sites may be multiplied by the SOF to be
taken into account, too.
U is the isotropic temperature factor. To convert from B to U, divide B by 82.
Keywords may be omitted from the '*.TIN' file and the corresponding parameters entered via the Crystal parameter
and Atom list dialog boxes.
Examples for valid '*.TIN' files :
1) TITL Silicon
SYMM F d 3 m z
WAVE Cu A1
CELL 5.4309 5.4309 5.4309 90 90 90
SFAC Si
SI1 1 .125 .125 .125 .041667 .015
END
2) SFAC Ca W O
Ca1 1 0 .25 .625 Missing SOF and displacement parameters will be set
W(1) 2 0 .25 .125 to the site multiplicity and a default value of 0.01,
O(1) 3 0.150 0.009 0.211 respectively.
Examples for invalid '*.TIN' files :
1) TITL Silicon
SYMM F d 3 m s
WAVE Cu A1 Keyword SFAC missing
CELL 5.4309 5.4309 5.4309 90 90 90
SI1 1 .000 .000 .000 .041667 .015
END
2) TITL Silicon
SYMM F d 3 m z
WAVE Cu A1
CELL 5.4309 5.4309 5.4309 90 90 90
SI1 .125 .125 .125 .041667 .015 No atom type (referring to the SFAC list) given atom
SFAC Si will be omitted
END

11.3 Setup
From the menu item Setup all information required for the pattern calculation may be entered.
Crystal Parameters opens a dialog box for the input of the basic cell parameters. Atom List opens a dialog box
with editing options for atom types, atomic positions, displacement parameters and occupancy factors. Pattern
Parameters allows the definition of diffractometer geometry and peak shape.

11.3.1 Crystal Parameters
Crystal Parameters : using this dialog box the user can input cell parameters, cell contents and other basic
parameters.
The edit box Title is used to input a string describing the project.
Formula is the sum formula of the substance; ions like Fe3+ ( NOT Fe+3 ! ) may be input as well. In the case of
ions, the stoichiometric factor must be separated by a blank from the charge number. From the formula string,
element (or ion) symbols are extracted and available as atom types in the Atom list dialog box. This means that all
atom types for which atomic positions are to be entered must be given in the formula. If the parameters are
read from a *.tin file, the formula is calculated by dividing the UNIT numbers for every atom type by the ZERR
number (see chapter 10.2.1). If structure information has been read from an *.ins file containing the 'old' SFAC
format with full scattering factor information, the 'Formula' edit box is disabled as any elemental input in this window
would replace the loaded scattering factors with their 'built-in' standard values.
The edit box Mol.Wt. displays the molecular mass of the substance when a formula is present. If the formula is
changed, the mol.weight window is updated. The user may however override the calculated value by entering a figure
in this edit box (note that a user-defined mol. weight will be overridden again by choosing a different wavelength as
the elemental information is updated in this case).
Z is the number of formula units per unit cell. From this figure, the molecular mass, the cell constants and the
formula the density and attenuation factor are calculated.
Laue Symmetry is a list box containing the 12 Laue groups (plus 2 groups Trigonal R -3 and Trigonal R 3 m'
defining rhombohedral groups on rhombohedral axes and 'Monoclinic 2/m C' allowing the choice of c as the unique
axis).
Lattice type is a list box containing all permissible lattice centrings for the selected Laue symmetry.
The Space group edit box accepts Herman-Mauguin short form symbols as well as the space group numbers
according to the International tables. Blanks may be input, but are are not considered by the verification routine.

Neither is the input case-sensitive. The symmetry information is taken from a table containing all space groups in
all possible settings except monoclinic cells with unique axis a and multiple cells like C4.
The monoclinic crystal system defaults the unique axis to b. To select c as the unique axis, it is either sufficient to put
in a space group like P21/b from which the selected setting is evident or a 'c' has to be appended to the space group
symbol (e.g. P 21 c). The same effect may be achieved by entering the full symbol P 1 1 21.
Spacegroups with two possible choices of origin like P m m n require an additional character 's' or 'z' following the
name of the space group : 'Z' denotes the origin on the center of symmetry, 'S' the origin selected off-center. If such a
spacegroup is entered by its spacegroup number without further information, 's' will be used as the default setting.
The spacegroup number may also be followed by one of the characters '1' or '2' to force the program to use the
settings 'S' or 'Z', respectively (according to the numbering in the International Tables).
Rhombohedral axes may be entered if the letter R is appended to the space group symbol. R 3 m expects
hexagonal axes and R 3 m r rhombohedral lattice constants (in the case of rhombohedral axes, the lattice centring
will also be changed from R to primitive).
Only those edit boxes of the Cell Parameters edit field are enabled which are necessary for the given crystal
system and setting. Lattice constants have to be given in Angstroms.
The list box Radiation is used to define the wavelength for which the diagram is to be calculated.
Generate Full Pattern is a check box which is only enabled if atoms have been input in the Atom List dialog box.
2Theta (Min, Max) describes the begin and end of the 2theta range for which peak positions will be calculated.
The data necessary to fill this dialog box can also be dropped or pasted from the main window of Index or from the
Results From Lattice Parameter Refinement window of Index onto the Setup Crystal Parameters dialog box.
To perform a Drag&Drop from the Index main window to Theo
a) The user starts Index, loads a .pks or .pth file (manual at paragraph 10.2) and performs an indexing using
one of the algorithms available (paragraph 10.4). A set of solutions is displayed on the main window of the
Index application
b) The user left-clicks on a solution to highlight it (see picture below) and, keeping the mouse left button
pressed, drags the solution over the Setup Crystal Parameters dialog box. When the cursor is on the
dialog box, the user drops the solution by releasing the mouse left button
To perform a Copy&Paste from Index main window to Theo:
a) The user starts Index, loads a .pks or .pth file and performs an indexing
b) The user right-clicks on a selected solution. A context menu appears with a single command Copy
unrefined cell params to Theo. The user performs the Copy operation. He then right-clicks on the Setup
Crystal Parameters dialog box. Another context menu appears with a single command Paste cell params
from Index. The user performs the Paste operation.
To perform the Paste operation correctly, it is important not to right-click on any of the edit boxes or controls
but on a region of the dialog box where there are no controls, for example, on the title bar where the window
title Setup Crystal Parameters appears
When transferring data from Index main window to Theo, only the unrefined Cell Parameters, the Crystal System,
the Wavelength and the .pks .or .pth file Title are going to be transferred. The Laue symmetry is set to the lowest
Laue symmetry compatible with that Crystal System and the lattice type is set to Primitive.

Drag&Drop or Copy&Paste operations can be performed also from the Index Results From Lattice Parameter
Refinement window as shown in the figure above: this window appears after the successful completion of a
refinement. In this case the refined cell parameters are transferred to Theo with the number of significant figures
compatible with the standard deviation obtained at the end of the refinement. Also, if the refinement was run using a
specific Crystal System / Lattice Type combination or a specific Spacegroup, this information is also transferred to
Theo.
11.3.2 Atom List

The Atom List option in the pull-down menu is only enabled if a formula has been defined in the Crystal
Parameters dialog box.
When defining atom positions in spacegroups with ambiguous setting of the origin, it is important to have
the parameters in accordance with the choice of origin defined by the space group identification.

To input a new atom, first press the New Atom button, then select an atom type from the list box, press Set Type
and proceed with defining the atom name, positions etc. To change an atomic parameter of an existing atom, click on
the atom in the atom list box which will transfer all atom data to the edit boxes above. These may then be changed.
By pressing the enter key in any of these edit boxes the parameters will be transferred back to the atom list box. To
delete an atom, click on the appropriate line in the atom list box and then the Delete button.
Name is a unique identifier for every atom in the structure.
Type can either be selected from the atom types list box and written to this edit box by pressing the Set type button
or typed into the edit box. Only atom types shown in the atom type list box which are part of the formula are accepted
as input.
x/a, y/b, z/c are the fractional coordinates of the atom. The site multiplicity for the atom's position is calculated
automatically. For atoms on special positions like 1/3 or 2/3, it is important to input at least 5 significant digits
(0.33333 and 0.66667) so that the program recognizes the correct multiplicity.
Occupancy is by default set to 1 for every new atom and needs only to be changed if the site is occupied statistically,
either sharing the position with another atom type or with a lattice vacancy. Occupancy multiplied by the Multiplicity
of the site gives the site occupation factor SOF used in the .tin files.
U11,U22,U33 and U12,U13,U23 are the components of the anisotropic temperature factor. When a number is
entered in any of these edit boxes other than U11 the atom is automatically labelled anisotropically. The change from
isotropic to anisotropic temperature factors may also be done by pressing the Anis/Iso button which will change the
corresponding flag of the currently highlighted atom in the atom list box. To convert from B to U, divide B by 82.

11.3.3 Pattern Parameters
This dialog box can only be opened if the Generate Full Pattern box of the Crystal Parameter dialog box has been
checked as the parameters set in this box are only important for the calculation of raw data.
The Geometry radio buttons are used to select the sample type and beam path for the experiment. This parameter
especially influences the absorption correction if a Mu*T other than zero is entered, otherwise the effect on relative
peak intensities is only significant at high angles. If absorption is not taken into account, the intensities for a Debye-
Scherrer (=capillary) sample and a reflection sample measured with fixed slits (Constant Sample Area not checked)
are identical as the irradiated volume remains constant over 2Theta, whereas high-angle peaks measured in
transmission geometry (2:1 coupling between 2Theta and omega) have a higher relative intensity due to the increase
of irradiated volume with 1/cos.
The Monochromator buttons are used to define the kind of primary monochromator used. The knowledge of the d-
spacing of the monochromators reflecting plane is necessary for the polarization correction factor. For Germanium,
the (111) plane is assumed to be the monochromator surface, for quartz the (101) reflection.
The Profile Function used for calculation of the raw data curve from the integrated intensities may be chosen from
five alternatives :
Lorentz (= Cauchy): Y = Yo . [ 1 + CL1 . ( (x - xo) / h )2 ]-1
Squared Lorentz: Y = Yo . [ 1 + CL2 . ( (x - xo) / h )2 ]-2
Gauss: Y = Yo . exp[ -CGS . ( (x - xo) / h )2]
Pearson VII: Y = Yo . [ 1 + CPS . ( (x - xo) / h )2 ]-m
Pseudo-Voigt: Y = Yo . ( 1 - n ) . [ 1 + CL1 . ( (x - xo) / h )2 ]-1
+ Yo . n . CLG .exp [ - CGS . ( (x - xo) / h )2 ]
xo: Peak position

Yo: Maximum counting rate (at xo )
h: Full width at half maximum (FWHM)

m: Pearson exponent of the Pearson VII function
n: Gauss component of Pseudo-Voigt profile
Cx: Constant coefficients specific to each profile
For the Pearson VII and Pseudo-Voigt functions, the variable profile parameter may be input in the edit box beneath
the Profile Function buttons either labelled Pearson Exponent or Gauss Component depending on the profile
type selected.
Using the Peak asymmetry radio buttons and edit boxes the user can simulate the peak asymmetry observed in
diffraction patterns when detector and sample heights are not small compared with the detector-to-sample separation.
Following the original method of Finger et al (van Laar, Yelon J. Appl. Crys. (1984), 17, 47; Finger, Cox, Jephcoat J.
Appl. Crys. (1994), 27, 892 and Finger J. Appl. Crys. (1998), 31, 111), the peak asymmetry that arises from axial
divergence can be described in terms of two physically relevant parameters H/L and S/L, where H is the detector
half-height, S is the sample half-height and L is the sample-to-detector distance. A modification of this approach here
used, implemented also in the pattern fitting program Fit (see paragraph 8.3.1), uses a single parameter equal to the
average of the H/L and S/L parameters, that is, (H/L+S/L)/2. The Approx. integration points per degree box
determines the approximate number of integration points and therefore the accuracy in the evaluation of the peak
asymmetry (see Finger 1994): large values might slow down the calculation of the theoretical pattern. The standard
value of 100 points per degree is acceptable. The checkbox Abort integration if accuracy can not be maintained
is a sort of safeguard against meaningless input in the (H/L+S/L)/2 parameter which might lead to long and not
correct calculations: if the program can not perform the integration with the same number of points per degree for all
peaks, the calculation is aborted. This is normally an indication that the value of the asymmetry parameter is not
reasonable or that too many integration points per degree were chosen. This checkbox should always be left checked
(as in the picture).
Only the .rth file is corrected for peak asymmetry: the .pth file, the theo.log file and the .lth file contain the
uncorrected peak positions and intensities. Also the peak positions shown at the bottom of the pattern as
short magenta lines correspond to the uncorrected peak positions (see paragraph 11.4). If the user wishes
to create a peak file which contains the shifted position of the peaks caused by the introduction of
asymmetry, he must load the asymmetry corrected .rth file using Graphic or Fit, perform a peak search and
save the resulting peak file.
When calculating the peak integrated intensity in presence of asymmetry, the conventional Lorentz factor for
powder diffraction measurements is used.
The edit box 2Theta ( Min,Max,Step) is used to define the 2theta range in which the raw data are to be collected
and the step width defining the angular distance between adjacent data points.
Mu*T allows the input of the samples attenuation factor for the calculation of the absorption correction
(transparency correction in the case of reflection geometry). The intensities calculated from the structure I(uncorr)
are multipied by the absorption factor appropriate for the geometry selected :
Transmission : I(abs) = I(uncorr) . exp ( - t / cos )
Reflection : I(abs) = I(uncorr) . [ 1 - exp ( - 2 t / sin ) ]
Debye-Scherrer : The cylinder absorption tables ( International Tables and references therein ) are
interpolated twice by a cubic spline between the tabulated q-values and between the
tabulated R-values.
Halfwidth defines the variation of peak halfwidth (in degrees) with 2theta as FWHM() = x1 + x2 * tan.
Max.Intensity is the count rate which will be assigned to the data point of the highest intensity in the diagram.
If Generate Alpha2 Peaks is checked, every generated reflection will be calculated for the selected alpha1 radiation
as well as for the corresponding alpha2 wavelength. The intensity ratio is taken as 2:1.
Constant Sample Area is only significant if Reflection geometry is selected. It multiplies all intensities by a factor
sin to simulate data collection with a variable divergence slit which keeps the irradiated sample area but not the
sample volume constant.

11.3.4 Load from ICDD
Load from ICDD allows the user to copy crystallographic data like cell parameters, chemical formula and
spacegroup from a PDF2 card directly into the application. Please note, that PDF2 cards dont contain atom site infos
at all and that not all cards contains all required datas.

11.4 View
Whole Diagram resets a former zoom command by displaying both axes starting from the minimum value of the
calculated diagram to its maximum value.
Position Info changes the cursor to a crosshair and displays the current crosshair position in the left part of the
main windows status bar.
'Labels' is used to select the labelling of the generated peaks in the main window. The peaks may either be identified
by their 2theta-position, their d-spacing or their Miller indices.
Grid Lines adds or removes a rectangular pattern to and from the window.
'List File' opens and closes the child text window containing the list of calculated peaks.
The Position Info, Whole Diagram, and Grid Lines commands are also available from these toolbar buttons:
When the cursor is not in the Position Info mode, it may be used to define a zoom-in window by moving it to any
point in the diagram, pressing the left mouse button and holding it depressed while moving the opposite corner of the
rubber box to the requested position. Releasing the left mouse button will change the display to an enlarged
representation of that diagram part which was contained in the rubber box. Scroll bars will be added to the diagram
enabling the user to move the diagram horizontally.

12 Crystallinity
12.1 Introduction
The module Crystallinity is used to determine the crystallinity index of an unknown sample, either by comparing the
diagram obtained from it with diagrams obtained from two other samples of known crystallinity or by first-principles
calculation.
The application is started from the pull-down menu of the WinXPOW main menu item Crystallinity
Standards method :
Ideally, the two standards should have a crystallinity of 100% (crystalline standard) and 0% (amorphous standard),
respectively. As such samples are not always available, the program provides the possibility to use standards of
another (but in any case well-known) crystallinity indexes. It requires four measurements to be performed with exactly
the same data collection setup and parameters including the generator settings : the two standard samples, the
unknown sample and a blind run for air scatter correction.
WinXPOW 3.05 Software Manual Crystallinity 12-1

The program calculates a least-squares fit for all data points in the three diagrams ( which have been corrected for air-
scatter ) according to the equations :
I(2) = m . ( xc . Ic(2) + (1-xc) . Ia(2) )
m ....... sample mass
xc ....... crystallinity index ( 0...1 )
I(2).... count rate for the unknown sample at a given 2
Ic(2)... count rate for the 100% crystalline standard at the same 2
Ia(2)... count rate for the 100% amorphous standard at the same 2
In the case non-ideal standards their ( known ) crystallinity index may be taken into account :
I(2) = m . ( x . Ic(2) + (1-x) . Ia(2) ) and xc = a + x . ( b - a )
m ....... sample mass
xc ....... crystallinity index ( 0...1 )
x ....... apparent crystallinity index
I(2).... count rate for the unknown sample at a given 2
Ic(2)... count rate for the standard having xc = b at the same 2
Ia(2)... count rate for the standard having xc = a at the same 2
Single-sample method :
The single-sample-method requires the user to define the portions of the diagram due to air scatter and inelastic
scattering, amorphous scattering and Bragg scatter. If Ic(2) and Ia(2) are known for the whole diagram, the
crystallinity index is calculated from
xc = Ic(2) / ( LP * F * T ) / { Ic(2) / T + Ia(2) } / ( LP * F ) summing over 2.

The Lorentz-Polarization factor LP, the average formfactor F, and the temperature factor T are all 2-dependent
functions :
LP(2) = ( 1 + cos**2 (2) ) / ( sin**2 () * cos () )
F(2) = f (n,2) summing over all atoms n in the formula unit
T(2) = exp ( - 2* B sin**2 () / **2 )
The samples overall formula and average temperature factor have to be known and to be entered into the program in
order to be able to apply the single-sample method.
Note : Sample absorption is always neglected, the program thus only works well ( xc within +/- 3 % of the true
crystallinity ) for transmission data of organic samples or reflection data.

12.2 File
comprises options load data files into the application and to print out the graphical representation of the calculations.
Open is used to select the desired algorithm and load the required raw data files for the selected algorithm into the
application
By choosing the Standards method the four required raw data files are
loaded: The Raw data file of the unknown sample, both crystalline
standard files and the air scatter file. For the two standard files, their
respective crystallinity indices must be entered. For ideal standards, the
parameter Crystallinity (%) is 100 for the crystalline standard and 0 for
the totally amorphous standard.. Editing the values 2Theta(min) and
2Theta(max) gives the option to exclude parts of the diagram from
calculation. By default the application calculate the crystallinity from the
total overlapping range of all files.
On pressing the OK button, the fit described above is performed. The
result is displayed in an info box and written to a text file having the
same name as the raw data file and extension *.lcr. In addition, a raw
data file is created with the same name but extension *.rcr which
contains the intensities calculated from the intensities in both standard
files multiplied by their respective contributions to the pattern of the
unknown sample. This diagram is also displayed in the main window
together with the original unknown raw data.

In the case the Single-sample algorithm is to be used, only two input
boxes remain active after checking the appropriate radio button.
Both files must have been created before starting the crystallinity
analysis module using the Background option in the Graphics program.
The background-corrected raw data file is generated from the original
raw data by fitting a rather straight line to the background (thus
eliminating air scatter and inelastic scattering) and saving the remaining
diagram to file. This file is then background-corrected for a second time,
now fitting the background to the amorphous hump. After subtracting this
hump, the remaining Bragg-only diagram is stored to another file name,
which is subsequently loaded as the crystalline scatter file.
On pressing the OK button, another dialog box is opened which

prompts the user for the formula unit and the average temperature
factor B of the sample. For organics, B is usually around 4; for
inorganics values between 1 and 2 are usually correct. The exact
formula has usually little influence on the result, whereas the
temperature factor can affect the crystallinity to within some percent.
The result is displayed in an info box and written to a text file having
the same name as the raw data file and extension *.lcr.
,Export Graphic provide an opportunity to create files in different formats for importing the display into other
Print - Print Preview - Print Setup control and format the output of the current graphic display to printer.
The most recent file list contains the names of the most recently used file names for quick re-loading.
Exit terminates the application and returns control to the WinXPOW main menu.

13 Size / Strain
13.1 Introduction
The module Size / Strain allows the user to calculate crystallite size and microstrain from peak widths.
The application is started from the pull-down menu of the WinXPOW main menu item Size / Strain.
The algorithms provided range from the simple and robust Scherrer- and Wilson-formulas to Williamson-Hall-plots
and profile decomposition into Lorentz- and Gau-portions using the procedure of de Keijser, Langford, Mittemeijer et
al.. All algorithms are based on the variation of the integral breadth over 2theta.
The two fundamental equations are :
K
Particle-size-broadening : Scherrer-equation (1) =
L cos
Microstrain-broadening : Wilson-equation (1) = 4 e tan
POW
WinX 3.05 Software Manual Size / Strain 13-1
with = integral peak breadth
K= size factor
= wavelength
L= volume-average particle size ( = D<v>)
e= 'upper-limit' mean strain
If both broadening effects are present, the Williamson-Hall plot (2) usually gives a good indication of the extend of
these effects:
K sin 2
cos = + 16 e
L cos
The size factor K which differs with particle shape (spheres, cubes, octahedral or the like) is set to unity in this
program.
For all three formulas, is the integral breadth of the pure specimen broadened profile function F(x). This is the
measured (observed) profile H(x) corrected for the instrumental resolution G(x). As the observed profile H(x) is the
result of a convolution of F(x) with G(x), this correction is not easily performed. The effect that the convolution of F(x)
with G(x) has on the halfwidths of H(x) depends on the profile functions (Gau, Lorentz or any intermediate) for F(x)
and G(x). The instrumental resolution function G(x) varies smoothly with 2theta. Hence this function can be obtained
by measuring a suitable standard with lines as sharp as possible like Si, LaB6 or Scheelite.
In the case that the profiles can be described by a Voigt- or pseudo-Voigt shape, a practical way of solving this
problem was developed by de Keijser and co-workers (3,4). Within this method, the integral breadths of the Lorentz-
and Gau- components of the measured H(x) and G(x) profiles are extracted using the ratio of integral breadth
(=beta) to full-width-at-half-maximum (=gamma) and accurate polynomial approximation formulas. The calculation of
the F(x) profile is then done for the Gau- and Lorentz-part of the Voigt-function separately :
F,Lorentz = H,Lorentz - G,Lorentz and F,Gau2 = H,Gau2 - G,Gau2 .
As particle-size-broadening leads to a Lorentzian shape of F(x) and strain-broadening to a Gaussian profile for F(x)
(5),
the deconvolved Lorentzian breadth of F(x) can subsequently be used in the Scherrer-equation to determine the
particle size and the Gaussian breadth of F(x) may be inserted into the Wilson-formula to calculate the microstrain.
The literature cites at least three parameters describing the amount of microstrain : the 'apparent strain' , the 'upper
limit' strain e and the root-mean-square strain <e2> which may be related to each other by
= 4 . e = 2 . (2) . <e2> and thus e = 1.25 . <e2>.
The program lists both e and <e2>.
Peak data input into this program must have been fitted by the 'Profile Fitting' module using Pseudo-Voigt functions
and individual peak widths not represented by the Caglioti formula !
(1) H.P.Klug, L.E.Alexander, X-Ray Diffraction Procedures, John Wiley & Sons, New York 1974, 655ff.
(2) G.K.Williamson, W.H.Hall, Acta Met. (1953) 1, 22
(3) Th.H.de Keijser, J.I.Langford, E.J.Mittemeijer, A.B.P.Vogels, J.Appl.Cryst. (1982) 15, 308
(4) Th.H.de Keijser, E.J.Mittemeijer, H.C.F.Rozendaal, J.Appl.Cryst. (1983) 16, 309
(5) R.A.Young, The Rietveld method, Oxford University Press 1993, 163ff.
POW
13.2 File
comprises options to load peak files into the program, to save a list file and to print out data from the program.
Open is used to load the two required kinds of peak files into the program : One peak file containing (fitted) peak
data from a standard sample reflecting the instrumental G profile and one containing the observed = broadened peak
data, the H profile. These peak files are generated using the 'Profile Fitting' module. The Browse buttons provide the
standard Windows function for file selection.
When both files have been read, the program displays

the list of observed peaks with all of these peaks
selected. The user may either accept all peaks or
discard those peaks from the list by clicking on them
which shall not be used for the size / strain evaluation.
Pressing the 'OK'-button will continue the program by
opening the 'Options' dialog box. If the 'Cancel'-button
is pressed, no peaks are loaded and the user has to
supply new peak data by using the 'File'-'Open' option
again.
Save Report lets the user write the program output
to a text file which receives a default file name
identical to the observed peak file but with extension
*.lsz. The item is only activated if data have been
loaded and evaluated.
Print - Print Preview - Print Setup control and
format the output of the current graphic display to the
system printer.
The most recent file list contains the names of the
six most recently used file names for quick re-loading.
Exit terminates the routine and returns control to the
WinXPOW main menu.
POW
13.3 View
This menu comprises commands affecting the layout of the main window and the visibility of the text child window.
'Toolbar' removes / brings back the

toolbar with shortcut buttons above the
main window.
'Status bar' removes / brings back the
status bar beneath the main window.
'Split' invokes the cursor used to shift the
limits of the main window's three splitter
windows.
'ListFile' switches off and on the display of
a child window listing the results.
13.4 Options
This dialog box allows the user to select the algorithm for the size / strain evaluation.
The 'Calculation' radio buttons allow the user to choose
between two different evaluations of the 2theta-dependance of
the peak broadening effect. 'Use functions' will perform a least-
squares-fit according to the Scherrer- and Wilson-formula to
the F breadths (using the breadth parameter selected with the
next two input options). 'Use mean value' will apply the two
formulas independently for every peak, calculate a size- resp.
strain-parameter for each line and take the average of these
parameters. The difference between the results obtained with
the two methods is usually small (typically 1-10% of the
calculated value depending on the number of peaks
evaluated); if the difference exceeds about 20%, this is an
indication that the data do not follow the theoretical prediction
at all. The setting of these radio buttons do not influence the
Williamson-Hall-Plot.
The check box 'Use Deconvolution' is usually checked as the
profile decomposition procedure described in 13.1. is the most
accurate way of separating the size and strain broadening
effects. However, the raw data must be of very good quality
and the fitting performed as accurately as possible; especially
the background must be defined unambiguously and the peak
counting statistics have to be excellent. If these prerequisites
cannot be met for some reason, it is preferable to retreat to a
POW
simpler size / strain estimation (i.e. use the Scherrer-, Wilson- and Williamson-Hall-formulas with the total breadths of
the H profile minus the total breadths of the G profile) rather than expect correct results from an advanced algorithm
fed with insufficient data. Therefore, this box should not be checked for poor data.
The 'Breadth' radio buttons are only enabled if the 'Use deconvolution' check box is not checked; i.e. if no separation
of the peak profiles in Lorentz- and Gau-components is to be performed. This crude particle size estimation is
usually done when the data are noisy, peaks are overlapping or the background is ill-defined. In these cases, the
FWHM of peaks is less prone to errors than the integral breadth and should be used in the Scherrer- and Wilson-
equations instead of the integral breadths.
The '2Theta window for deconvolution' controls the assignment of observed peaks to standard peaks. As the peak
width as well as the peak shape usually change with 2theta for F-, G- and H-profiles, the standard peak used to
correct the H profile for instrument broadening must be in the same 2theta region as the broadened peak. Ideally, the
standard is the same substance as the broadened sample but showing no peak broadening effects. In this case,
every broadened peak may be corrected with its unbroadened analogon in the standard. Peak positions would vary
very little and a small 2Theta window can be used. The use of the very same substance as a standard is, however,
not always feasible and laboratory standards like Si or LaB6 must be used. In these cases, the permissible width of
the 2theta window depends on the size of the broadening effect and may be the larger the larger the broadening is;
i.e. the less important the G contribution becomes. If the instrumental FWHM is e.g. in the range of 0.1 and the
broadened peaks are more than 2 wide, the 2theta window may be up to 10 without introducing a significant error
(of course presuming a 'normal' variation of peak width and peak shape with 2theta for the instrumental profile).
Pressing the 'OK' button will start the calculation and display the results on the screen.
'Cancel' will discard all changes which have been entered and return to the main menu.
13.5 Output
The result of the calculations is displayed graphically in the three splitter windows of the main window. The top left
display shows the results of the particle-size evaluation, the top right window the results of the strain calculation, and
the lower window the Williamson-Hall-plot.
Depending on the setting of the 'Calculation' option, the top left window either shows the variation of the breadth
measure with /cos ( if 'use functions' has been selected) or the variation of the calculated particle size D<v> with
2 ( if 'use mean value' has been selected). Accordingly, the top right window either shows the breadth / tan -
variation or the strain e over 2, respectively.
For a perfect fit to the Scherrer- or Wilson-equation, D resp. e should be the same for all peaks, i.e. constant with 2,
if the calculation mode 'use mean value' is selected.
The parameter calculated for the particle size is the volume-averaged particle size D<v>; the strain parameters output
are the strain e and the r.m.s. strain (for definitions, see 13.1 and the literature cited therein).
A child text window displays all information relevant for the task performed. This output may be written to file using
the 'Save Report' option in the 'File' pull-down menu.
POW
14 System-Evaluation
14.1 Introduction
The System-Evaluation module is a graphic interface to observe powder pattern and calculate their refining
lattice parameters. For a better description it has been (sub-)divided to the following parts:
1. graphic interface to display powder pattern, define background points and allocate peaks,
2. pattern fitting, using the Fit-module of the WinXPOW software suite,
3. indexing via the programs ITO1, TREOR2 and DICVOL3 and the refining routine (see index & refine
module of the WinXPOW software suite),
4. space group determination of crystallographic powder data (ExtSym4).
The module provides an easy way for data processing and preparing data for further analyses.
Menu and Tool Bar

Caption Bar
Display Window
Operation Bar
Report Bar
1
J.W.Visser, Journal of Applied Crystallography 2,89 (1969)
2
P.-E.Werner, L.Eriksson, M.Westdahl, Journal of Applied Crystallography 18, 367 (1985)
3
J.W.Visser, Journal of Applied Crystallography 2,89 (1969)
4
A.J.Markvardsen, K.Shankland, W.I.F.David, J.C.Johnston, R.M.Ibberson, M.Tucker, H.Nowell, T.Griffin,
Journal of Applied Crystallography. 41, 1177(2008)
WinXPOW 3.05 Software Manual System Evaluation 14-1

The program main window is split into five parts:
- The menu- and tool-bar
- The operations-bar
- The caption-bar
- The display window
- The report bar.
These five parts should be described in the following chapters.
14.2 The menu- and tool-bar
14.2.1 File
The File-menu item offers the standard Windows utilities to read and write files, to re-open recently used
files and to print the results. For further information please consult the RawDat chapter 7.2.
14.2.2 View
The View-menu item provides the utilities for the control of the display. Their closer description has been
documented in the chapter 7.3 of the RawDat documentation.
14.2.3 Operations
The Operations-menu item contains two basic editing functions. The first function is the editing of the
background points and the manipulation of the background curve, the second is a smoothing operation
which can be performed to the data points. Both operations are described in the RawDat manual section
(see chapter 7.6).
14.2.4 Peaks
The Peaks-menu item lists the operations for peaks, phases and regions alignment.
Search Peaks starts the peak search algorithm, scanning the raw data for significant peaks. For this
operation the current search parameters will be used. After loading a powder-diffraction file (Stoe RAW-file),
these parameters will be set to default values, depending on the measurement conditions. Following peak
searches will add the found peaks to the existing peak list. This can lead to double entries. The peaks found
by the algorithm will be grouped in the phase called PeakSearch. To prevent double entries, it is highly
recommended to clear the current peak list before searching.
Clear Peak List deletes all current peaks, not concerning their properties like phase or if indexed.
Edit Peaks starts the peak editing mode as described below.

Edit Peaks Dialog displays the peak list dialog (see below).
Range Selector
Lock Columns
Edit Buttons
In Stoe RAW-files more than one measurement range can be stored. On top of the dialog one of these
ranges can be chosen. Changes in this selection will display the corresponding peaks to this range.
The header line of the peak list table can be clicked for sorting or to switch on/off all values below the
values in the corresponding column below. An unlocked/locked-icon indicates if the value before the icon
will be free or fixed for refinement in the next fit cycle.
2Theta, Half-width, Intensity and Phase values can be edited manually. Negative or zero values are not
allowed in the phase fields. Gabs in the phase list must be prevented.
New peaks can be entered through clicking the New Peak button at the bottom of the dialog or through the
context menu (right mouse button). Peaks can be selected through the usual mouse clicks. Holding down
the shift-key will select all peaks between the first and the last click. Every left click will select one single
peak, while unselect the last selected one. Holding down the ctrl-key while clicking, enables the users to
select more than one entry. Selected peaks can be deleted through the Delete Peak-button or through the
context menu.
Edit Region starts the region editing mode as described below.
Edit Regions Dialog displays the regions dialog.
This dialog can be handled similar to the Edit Peaks Dialog above. New entries can be made by a click on
the corresponding button or from within the context menu, displayed after clicking the right mouse button.
Selected entries can be deleted by the button or context menu. Values in the Begin column must be
smaller than values in the End column. Overlaps of regions should be prevented. A warning will indicate an
overlap which will be truncated or deleted after closing the dialog by clicking the OK button.

Edit Phases starts the region editing mode as described below.
Edit Phases Dialog displays the phases-dialog.
Color Selector Field
Use/Refuse Phase
Show/Hide Phase
Name of the Phase
Selected Phase
The handling of this dialog is similar to the regions dialog described above. The columns Index and
NPeaks displays only information and can not be edited. By pressing the corresponding Sel. field, a
working phase can be defined. This selected phase will be used to proceed with further processes. A
name for the specific phases can be set. This names will be displayed in the phase editing modus, see
below for further information. To show or hide phases in the display can be chosen by clicking the
corresponding field in this dialog.
If phases are refused for further process, the peaks belonging to this phases within the defined regions will
be removed before the next pattern fitting cycle. In the last column the color of the peaks belonging to this
phase can be edited.
Through the context menu (pressing the right mouse button) selected phases can be merged. All selected
phases will be merged to the first selected phase in this list.
After a pattern fitting cycle peaks with abnormal parameters will be sorted out into refused-phases,
indicating that these peaks could not be well fitted. It is recommended not to use this peaks for further
process.
14.2.5 Help
The Help-menu item list displays information about the program.
14.2.6 Tool-Bar
Most of the commands described above can be called directly by clicking the corresponding button in the
toolbar.

14.3 The Caption-Bar
The caption bar displays current information and the state of the program. If Position Info is been enabled
in the menu- or in the tool-bar, the position (intensity and 2Theta) of the mouse pointer will be shown in the
caption bar.
14.4 The Operation Bar

Three operation tabs add up to the operation bar.
- the Guided Mode-tab,
- the Advanced Mode-tab,
- the Display-tab.
With the help of the commands- and entry fields in the first two tabs the program can be controlled.
Displaying options can be set in the third tab.
14.4.1 The Guided Mode-tab

In this tab the basic operations and settings are combined.
Tab Header
Command Button
Current state with state icon
Selector
Section Separator
Help Bar

In the list on the left side the buttons are stored. Pressing these buttons will execute external programs or
internal routines or change the editing modus. On the right side of the list the current states of the buttons or
a selection list are shown. On the very right side an icon will display the success of the performed
operations.
All of the command- and input- buttons are sorted into six sections. In the global section loading of the file
and basic operations are stored. The fit section consists of the button to start the external fit program. The
selection and execute button for the index routine has been put to the index section. In the GenHKL section
the execute button for the HKL file generating data fit is stored. Buttons for executing the external program
ExtSym and selecting the most probable extinction symbol, are placed in the ExtSym section. In the final
section RefineSG the button to refine the chosen space group with a final fit is placed. The buttons will
further be explained in detail.
Load File-button opens a file dialog. If this button is pressed and the warning for unsaved data is not
prevented in the preferences, the user will be asked to save the current unsaved data, which will be lost
otherwise. If a file has been loaded, the name of this file is shown in the information field on the right side of
the button.
Only displayed if more than one range is presented in the Raw-file the Select Range-button will open a
dialog where a working range can be chosen.
The Background-button starts or ends the background editing mode.
The Regions-button starts or ends the regions editing mode.
The Peaks-button starts or ends the peak editing mode.
Run Fit will execute the pattern fitting module. For more information to the fit program please read the
chapter 8 of this software manual.
If more than one phase is defined, the Select Phase entry will be displayed. By a mouse-click on the entry
the phase list dialog will be opened.
The Run Routine entry in the list will execute the on the right side of the entry selected external program.
To choose the external program, pressing the the switch-icon on the far right side of the entry.
If a cell suggestion has been selected and refined pressing the Generate HKL File button will fit the
generated theoretical peaks corresponding to the selected suggestion. After the fit an HKL file will be
generated and if not deactivated in the preferences, the user will be asked where to save this file.
Run ExtSym executes the external program ExtSym.
With the help of the Extinction Symbol-selector a possible extinction symbol can be selected.
With a click on the left side of the Refine SpaceGroup-button a final fit can be performed. After this fit a
final HKL-file will be created.
During the work with the Guide Mode-tab small information of the process is displayed at the right side of
the command buttons. At the right side of the section buttons an emotional icon will indicate the quality of
the results.
NOTE: The check for the quality of the results bases on distinct absolute values. The
result itself depends on many environment variables like the quality of the data
set. A bad indication must therefore not indicate that something went wrong
during the operation.
On the bottom of the bar a Help Bar will display an assisting text.

14.4.2 The Advanced Mode-tab
The Advanced Mode-tab contains below the command buttons fields to edit important preferences for the
external and internal algorithms. With the help of the tool bar the sections can be switched. On the bottom
of the bar a Help Bar will display assisting information depending on the chosen field.
Tab Header
Tool-Bar
Command Buttons
Property Entries
Help Bar
The Command Buttons are similar to the buttons of the Guide Mode-tab. Indicators on the right side of the
entries show the process and the quality of the analyses. Below the command buttons Property Entries for
individual editing of settings are presented.
In the Global Prefs-section the min and max values of the regions can be edited. Additionally to the above
described guide buttons a Save PeakFile entry is placed in this section. A click on this entry will write a
Stoe-PeakFile.
In the Fit Prefs-section basic preferences for the external program
Fit can be edited. Additionally to the above described guide button a
Reset Settings-button is placed in this section. This button will reset
all individual settings done in this section and will reset all former
received fit results.
The lock-icon on the right side of a value indicates whether the
value is free for refinement. A click on this icon will change the
free/fixed behavior during refinement.
For more information about the values, which can be edited in this
section, please refer to chapter 8 of this manual.
If Fit is executed for the first time the 2Theta values of the peaks will
be fixed for refinement and only the intensities and the half-width of
the peaks will be free for refinement. In a second cycle the 2Theta
values of the peaks will be freed for refinement.

In the Index Prefs-section basic preferences for the external
indexing programs can be edited. Additionally to the above
described guide buttons a Reset Settings-button is placed in this
section. This button will reset all individual settings done in this
section and will reset all former received refine results.
With the top routine selecting button the below properties will be
changed depending on the routine chosen. All values are similar to
the values described in chapter 10 of this manual.
If an external indexing program is started by pressing the Run
Routine-button a status dialog will open which monitors the
external process and gives out a text which will be written by
executed process.
This dialog is closed if the OK button on this dialog (only enabled
if the external process has finished) or the Fixed-button on the
upper right side of the dialog has been set to Release and the
process has been finished.
In the Cell Setup section the refinement parameter and the cell
settings can be altered.
The first two values Zero Shift and 2Theta Ref.Window are
crucial for the internal refinement algorithm. An inaccurate zero-
shift will lead to false indexed peaks.
During the refinement the 2Theta window is minimized. The finally
reduced 2Theta window is saved for the next refinement cycle. This
window corresponds to the correlation between symmetry based
calculated peaks and the observed peaks from the peak search or
manual allocation. If this window is too small it can lead to a higher
number of peaks which could not be indexed.
NOTE: If the number of peaks which can not be indexed during refinement is getting
higher, please check the values for the Zero Shift and 2Theta Ref.Window. If the
zero-shift is too big or the 2Theta window too small, the values should be set back
to default values (0.0 for zero-shift and 0.08 for the 2Theta window) and
refinement should be repeated.

In the GenHKL Prefs section the settings for the fit of the symmetry
based calculated peaks can be altered. With a reset button all the
settings can be set back to default values.
Due to the theoretical calculations peaks are generated which are
located very near to each other, and can not be resolved with the fit
algorithm. To prevent faulty results these peaks will be filtered and
removed before fit and added back to the peak list afterwards (by
overwriting their parameters with fitted parameters from overlapping
peaks). The finally created HKL-file will contain all the theoretical
calculated peaks.
The filter Resolution Window can be defined in this section. If this
window is too big interactions between peaks can not bee detected.
With the choice of a too small window the fit of the peaks can lead to
typical artifacts. These artifacts lead to peaks which are excessively
huge, whereas the interacting peaks right next to this peak will be
negative.
The other parameters are well defined in chapter 8 of this manual.
If Generate HKL File is executed at the first fit cycle only the intensities and if set in the peak dialog, the
half-widths of the peaks are free for refinement. In a second fit cycle the cell data will be free for refinement.
In a third optional cycle the profile parameters u, v and w will be free for refinement (if fixed before).
The ExtSym Prefs section displays the settings which will be
send to the external program ExtSym. For more information
about these values please see the manual of ExtSym.
The additional entries Reset Settings and Save Generated
enables the user to reset to default values and to save the
generated peaks to a Stoe peak file.
The RefSG Prefs section corresponds to a final fit with a

selected space group. Again all settings can be set back to
default values by click on the Reset Settings entry.
A description of the displayed parameters is given in chapter 8
of this manual.

14.4.3 The Display-tab
Tab Header
Tool Bar
Show/Hide-Checkboxes
The Display-tab can be handled similar to the Layer Panel in RawDat specified in chapter 7.1.2 of this
manual. In difference to the Layer Panel show/hide buttons for special HKL values are shown in the tool bar
of the Display-tab. With the help of these buttons calculated peaks which fulfill discrete reflection
conditions can be displayed or hidden. The icon of the button corresponds to the special reflection
condition.
14.5 The Display Window

This window is a tool for displaying the basic raw data, for manual editing of data points and for monitoring
the progress.
In the basic raw data displaying mode the raw data curve, the resulting curves of the fit, the observed peaks
and the calculated reflections are shown. The curve offers valuable information about the quality of the
divergence fit last performed (see chapter 8 for further information). Tools for working with this window are
specified in chapter 7 of this manual. An additional tool for working with this display is the Zoom Diagram.

The Zoom Diagram contains two slider controls and a small
version of the whole diagram. With the help of the slider controls
at the bottom and on the right side of the window a zoom area
can be adjusted. A small rectangle represents the chosen zoom
area. This box can also be dragged around with the mouse
pointer. Moving the mouse pointer over the box and clicking into
it with the left mouse button, holding this button and moving the
mouse will shift the box in the diagram. During the movement the
main display window will show the chosen region.
14.5.1 Region Editing Modus

In this modus the regions can be defined. To edit these regions the mouse pointer has to be placed near
the end or the start of a region. If editing can be
performed the mouse pointer will change into a bar with
arrows at both sides pointing to the opposite directions.
If the left mouse button is clicked and hold down, the
region can be adjusted. If the mouse pointer will be
moved directly over the region bar at the bottom of the
diagram and is placed over the blue region representing
a defined region the mouse pointer will change into a
pointing hand. Clicking this region with the left mouse
button, holding down the button and moving the mouse
will shift the region. If a region collides with another
region both regions will be combined. A right pressed
button on a region will delete the selected region. All regions but one can be deleted. If the end or the start
of the region is outside the zoomed area, a white arrow will be shown (see diagram). A double click on the
blue region bar will open a dialog to edit this region by an input of discrete values.
14.5.2 Peak Editing Modus

In this modus peaks can be edited. A peak editing tool bar will be displayed above the diagram. Buttons of
this tool bar are explained below.
Seach Peaks will start the peak search algorithm
(chapter 14.2.4). Clear Peak List will delete all
current peaks not concerning their properties like
phase or if indexed.
The next five entries of the tool bar are well
documented in chapter 8.4.1 of this manual and
should not be explained here further.
The Consider Background button will delete
observed peaks which are not significant bigger than the background.
If the Automatic Mode button is checked, an algorithm will try to find best values for the parameters
above, to perform the best possible peak search.
A Reset button will set some of the parameters back to default values.

Peaks can also be allocated manually. For adding a peak-marker into the diagram double click the location,
were the peak should appear. After the double click the maximum in the raw data curve at this position will
be searched and the peak will be shifted to this maximized position. The automatic search for the best
position of a peak can be disabled by pressing the Sticky Add Peaks button in the Basic Operations
tool bar displayed in the upper right side of the program.
If the left mouse button kept pressed near an existing peak-marker, this peak-marker can be shifted to a
new position. A right click on an existing peak-marker will delete it.
Blue lines at the bottom of the diagram display the defined regions. If presented, the resulting cumulative
curve of a fit will be shown as well.
14.5.3 Background- and Smooth-editing Modes

These two modes have been specified in chapter 7.6 of this manual.
14.6 The Report Bar

The Report Bar contains two different panels, the Report-panel and the Index Result-panel.
14.6.1 The Report Panel

The report panel is similar to the report panel in RawDat (see chapter 7.1.5). Moreover this report panel
contains additional reports.
The Overview-report will display all the important results received during the processing of the Stoe RAW-
file. It contains the following eight sections:
- Current Info: most important results for indication of the quality of the results,
- File Info: header information of the loaded Stoe RAW-file,
- Selected Range Info: information about the selected range of the Stoe RAW-file loaded,
- Fitting Info: results from the first fit of the allocated peaks process,
- Index Info: results of the executed external or internal indexing routines,
- Selected Solution: information about the refined (and therefore selected) cell suggestion,
- HKL File Generation: results from the fit of the calculated peaks,
- ExtSym Overview: results form the external program ExtSym,

- SpaceGroup depending HKL File Generation: result of a final fit.
The RawDat-report is described in chapter 7.1.5 in this manual, as well as the possible selection of Audit-
Trail and Full Report.
In the Peak-File report the current allocated peaks will be listed as saved to a common Stoe peak-file.
The Fit Report contains all information of the last performed fit.
All errors during the operations will be stored in the Error Report.
The next two reports Index Report as output of the indexing program and Sel. Solution as overview over
the refinement of a selected cell suggestion, are the common output of the indexing programs (see chapter
10 for further information).
The Generated Peaks-report contains a list of all current generated peaks, calculated based on the cell
metric or the space group depending on the process of the work.
The ExtSym Report contains the output of the ExtSym program and a peak list.
NOTE: The list of peaks which has been calculated in the ExtSym Report contains only
the current displayed peaks. The list can therefore be altered by choosing the HKL
conditions which must be fulfilled by enabling/disabling this conditions in the
Display-tab tool bar (see above).
14.6.2 The Index Result-panel

In the Index Result-panel the cell suggestion for the peaks allocated in the loaded Stoe RAW-file are
displayed.
The tool bar on top of this panel can be used to reset to values and to sort the below listed suggestions. A
click on the Reset button will reset all suggestions to the values calculated by the indexing routine. All
refined results will be lost.
To sort the suggestions in this list, first the display has to be changed to alphabetical, by pressing the
corresponding button in the tool bar. After that, the suggestions can be listed depending on their occurrence
in the output of the indexing routine, on their FOM values, or on their cell volume. Clicking one of the
buttons more than once will change from ascending to descending order and back.
A mouse click with the left mouse button will refine the selected suggestion. Depending on if the zero-shift
should be fixed or free for refinement, one or a series of refinement cycle(s) will be performed. A context
menu, available by clicking an entry with the right mouse button, enables the user to delete or set back the
selected suggestion.

14.7 Example for Processing Data
1. After the start of the program a Stoe RAW-file has to be loaded. The SymEval program can not
process master files or a series of files.
1.1. To choose a range to proceed will only be necessary if more than one range is presented in the
Stoe RAW-file.
2. If background points are not provided by the Stoe RAW-file a new background has to be allocated.
To proceed, the background working mode has to be started. During this start a theoretical
background will be set. Background points can be altered or added or deleted afterwards to correct
the calculated background.
3. It is highly recommended to define the working region for further data procession. Beam-Stop areas
or high-angle areas without noticeable peaks should be cut off, to improve further results.
4. Most important to proceed is the allocation of peaks in the loaded curve. The first change to the
peak edit mode will perform an automatic search for peaks in which all search parameters will be
automatically adjusted to receive the best search results. To check this search by zooming in the
diagram and by allocating, deleting or adding peaks is highly recommended.
5. The next step in the processing of the data is a fit of the allocated peaks.
5.1. If the results of the fit indicates that peaks are missing or should be deleted, these peaks should be
edited by re-entering the peak edit mode. Peaks with abnormal shifts, half-width or intensities will
be rejected, set back to values before the fit and sorted out to additional phases. These phases
can be edited or deleted through the phase edit mode or the phase list dialog.
6. Next an indexing routine has to be started. If the indexing program does not deliver any cell
suggestions, the following points should be tried out:
- Change the max number and the max number of possible un-indexed peaks in the advanced
mode
- Change the indexing algorithm. Choices are:
- Werner algorithm (extern with TREOR program or use of the internal process)
- Louer algorithm (extern with DICVOL program)
- Visser algorithm (extern with ITO program)
7. Select and refine a suggestion by clicking on a list entry in the index result panel. The un-indexed
peaks will be flagged with a red UNINDEXED-label (if Peak Labels / X-Lables / HKL is enabled).
Please mind that too many un-indexed peaks may indicate a wrong symmetry, especially if
comparative strong peaks are un-indexed. Other explanation for un-indexed peaks may be fault
values for refinement (see chapter 14.4.2 for further information) or impurities in the sample.
8. Next a fit of the theoretical generated peaks and a generation of a HKL file should be proceeded. In
a first fit-cycle the 2Theta values are fixed and only the intensity of the peaks is free for the
structure refinement. The half width will be calculated as function during the refinement. A second
cycle will fit the peaks while freeing the cell parameters for the structure refinement. A third
recommended cycle will calculate the parameters u and v of the profile function (if not freed
before).
9. The generation of a HKL file should be followed by the execution of the program ExtSym. This
program will calculate the probability of extinction symbols describing the fitted peaks. These
symbols will be presented in a list box and can be chosen by the user.
10. After choosing an extinction symbol from the list and a corresponding space group, the new
settings can be used to generate peaks which can be fitted against the original data curve.

14.8 Preference Dialog
The preference dialog can be displayed by pressing the corresponding button in the tool bar or selecting the
menu entry in the menu bar. Five sections of preferences can be altered.
The General-section contains the more global settings for the
program behavior.
All Stoe RAW-files can be loaded with this program. Files created
with obsolete software suites can have a different internal
structure. This so called old format can be imported into the
SystEval program but not written back to disk. All Files saved by
SystEval will be written in the newest Stoe RAW-file format. The
handling of files in an old RAW-file format can be altered in the
corresponding field of the preferences.
New generated or edited background data for ranges will be saved
to the loaded files. If edited data should be kept, a warning
message will appear after changing background points. This can
be prevented by disabling the box in the preference dialog.
The program behavior during export and the display of warning dialogs during the fit process can be
changed in the corresponding fields of the preferences dialog.
In the Diagram-section, the colors and appearance of the
diagram presented in the program can be set. Entries in this
preference section are self explaining and similar to the
preferences described in the RawDat section of this manual.
In the Display-section the settings for the display of peaks can

be edited. In the first list box the origin of the peak data can be
set. The peak data can be loaded from file or created with the
usual peak search algorithm. Choices are as followed:
- Do nothing will only load the Stoe RAW-file.
- Ask for existing peak file will display a file dialog for
loading a peak file manually.
- Search for existing peak file will load a peak file with the
same name as the Stoe RAW-file loaded in the same
directory or will display the file dialog if no peak file with
the same name has been found.
- Automatic mode will search for an existing file and if no
file has been found or selected it will automatically perform
a peak search.
- Search for peaks automatically will perform a peak search
with automatic adjusted settings every time a Stoe RAW-
file is loaded.
Every theoretical peak will be calculated without a zero-shift
depending on the used diffraction system. To apply the zero-shift
in the display to the generated peak, enable the corresponding
checkbox in this dialog.

If peak labels should not be overwritten only the first label of a peak will be displayed if two labels are too
near each other and would overlap in the display.
The cumulative curve presented from a fit can be scaled on the total region or on the zoomed region
displayed on screen. This scaling behavior can be set in the corresponding field of this dialog.
In the Printing-section a few self explaining parameters for
the printout can be set.
In the Saving-section of the preference dialog the automatic

saving behavior of the program can be edited.
If the program is closed, while data were not saved, a warning
will be displayed. To avoid this warning, the corresponding
checkbox must be disabled.
In the edit field a project directory can be set up. In this project
directory all important data processed will be saved, without
asking the user. Opening of a Stoe RAW-file will save this file
into the project directory. All fit-result files (*.rtf), all peak files
(*.pks), all HKL-files (*.hkl), and all project file (*.exres) will be
saved automatically to this directory.
After the creation of an HKL-file and the execution of the Fit-
program the user is asked for a place and the name of the file
to be saved.
To save the HKL- and Fit-files without asking (giving them the
same filenames as the loaded RAW-file in the same directory),
the corresponding checkboxes must be enabled/disabled.
If the project file should be saved without a warning, every time
a file is closed a project file (*exres) will be written to the
location of the file loaded or in the project directory if defined.

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2 Instrument Parameters 2-1

3 Diffractometer Control 3-1

WinXPOW Software Manual 0-2

4 High-Temperature Data Collection 4-1

WinXPOW Software Manual 0-3

7 Raw Data Handling 7-1

7.2 File 7-5

8 Pattern Fitting 8-1

9 Peak Calibration 9-1

WinXPOW Software Manual 0-4

11 Theoretical Pattern 11-1

13 Size / Strain 13-1

WinXPOW Software Manual 0-5

WinXPOW Software Manual 0-6

1.1.1 General Remarks

1.1.2 Input Elements

The WinXPOW programs use three different kinds of dialog boxes :

User is used to select the users parameter file.

New User is used to create new user file entries.

Defaults allows the user to define default data collection parameters.

WinXPOW 3.05 Software Manual Instrument Parameters 2-1

WinXPOW 3.05 Software Manual Instrument Parameters 2-2

Dead time of Sci.Counter refers to the dead

WinXPOW 3.05 Software Manual Instrument Parameters 2-3

WinXPOW 3.05 Software Manual Instrument Parameters 2-4

In case of nonlinear characteristics of the

WinXPOW 3.05 Software Manual Instrument Parameters 2-5

WinXPOW 3.05 Software Manual Instrument Parameters 2-6

WinXPOW 3.05 Software Manual Instrument Parameters 2-7

WinXPOW 3.05 Software Manual Instrument Parameters 2-8

WinXPOW 3.05 Software Manual Instrument Parameters 2-9

WinXPOW 3.05 Software Manual Instrument Parameters 2-10

WinXPOW 3.05 Software Manual Diffractometer Control 3-1

WinXPOW 3.05 Software Manual Diffractometer Control 3-2

3.2.6 Print Preview

opens a Windows standard WYSIWYG window of the printout.

3.2.7 Print Setup

opens a Windows standard printer setup window.

3.2.8 Most Recent File List

WinXPOW 3.05 Software Manual Diffractometer Control 3-3

WinXPOW 3.05 Software Manual Diffractometer Control 3-4

3.3.4 Title / Comment

The Common property sheet contains two options : if the

The option erasing IP-PSD could be used when

WinXPOW 3.05 Software Manual Diffractometer Control 3-5

The Tasklist Setup sheet is described in in chapter 3.5.3 Scan Usage.

WinXPOW 3.05 Software Manual Diffractometer Control 3-6

3.4.1 Open Shutter

3.4.2 Close Shutter

3.4.3 Drive Circles

WinXPOW 3.05 Software Manual Diffractometer Control 3-7

3.4.4 Set Slit Width

WinXPOW 3.05 Software Manual Diffractometer Control 3-8

3.4.5 Sample Changer (Next Sample)

WinXPOW 3.05 Software Manual Diffractometer Control 3-9

3.4.6 Sample Position

WinXPOW 3.05 Software Manual Diffractometer Control 3-10

3.4.7 Erase IP-PSD

WinXPOW 3.05 Software Manual Diffractometer Control 3-11

3.5.1 Scan Mode

WinXPOW 3.05 Software Manual Diffractometer Control 3-12