Instructions for the ICDD PDF-4+ and Sieve+ Software

Instructions for the ICDD PDF-4+ and Sieve+ Software
Contents
Searching the Database .............................................................................................................. 2
Comparing experimental data against the PDF-4+ database using SIeve+ ............................... 4
Data preparation ....................................................................................................................... 4
Starting SIeve+ and loading your data ...................................................................................... 5
Filtering your results ................................................................................................................. 7
Multi-phase samples .................................................................................................................. 8
Publishing your final analyses ................................................................................................... 9
This software is only licensed for use on one computer. It is not available for
users to install on other computers.
Last updated: NRM, 16/12/2011

Searching the Database
The database can be accessed by clicking on the ‘PDF-4+ 2011’ icon on the
desktop of the computer.
There are a multitude of search criteria – I would encourage you to play
around and see what things do. As a brief summary, you can search by the
following general criteria:
Database (there are actually several included)
Ambient or non-ambient temperature/pressure
Quality Mark
Subclass (e.g. cements, ceramics…)
Elements (using Boolean logic or Yes/No/Maybe)
Formula, composition & number of elements
Name (compound, common, mineral)
Zeolite or Mineral Classification
References (author, journal, title, etc.)
Structures (symmetry, space group, unit cell dimensions,
(non)centrosymmetry, atomic environment (e.g. tetrahedral, etc.))
Density
Melting point
I/Ic (for RIR method of quantitative phase analysis)
Organic functional groups…
To filter through the database:
1. Go to the main ‘Search’ window (move the SIeve+ plus window if
necessary).
2. Choose your filtering criteria – a good starting point might be to select
those elements present in your sample. To do this:

a. Select either the Boolean or Yes/No/Maybe tab; I prefer the
latter, so we’ll do that here.
b. Click Set Unselected to ‘No’ – this will deselect all elements
c. Click an element to add it to the ‘Maybe’ list (i.e. this element
may or may not be in the phases in your sample). Clicking it
again will add it to the ‘Yes’ list (i.e. this element must be in all the
phases in the sample). A third click will return it to the ‘No’ list.
d. Repeat for all elements as appropriate.
3. Repeat for other search criteria if and where appropriate.
4. Once you are happy with the search criteria, click Search at the
bottom of the ‘Search’ window. A ‘Results’ list will appear in a new
window.

Comparing experimental data against the PDF-4+ database
using SIeve+
This is the analogous process to that we can perform in the STOE WinX POW
software’s Search/Match program to access the 2004 edition of the PDF-2
database. However, the SIeve+ software that can access the 2011 edition is
much more powerful, and obviously has access to a much larger, more up-
to-date database. SIeve+ is built in to the database software, and is
accessed from within it.
Data preparation
In order to load your experimental data in to the SIeve+ software, it must first
be in one of the following data formats:
- Sietronics *.cpi (as output by the Siemens D500 and Philips PW1825)
- *.xyd (for all other instruments)
To convert your data in to *.xyd format, follow these steps:
For data collected on the Siemens D5000:
1. Open WinX POW
2. Go to Raw Data/Raw Data Handling
3. Go to File/Import
4. Change to ‘Files of Type’ = Diffrac Raw Files
5. Select your Siemens *.raw file
6. Save, WITH A DIFFERENT FILE NAME, as a STOE *.raw file
7. Change the Wavelength to Cobalt.
8. Click File/Save As, and overwrite the STOE *.raw file.
9. Click File/Export, and select the *.xyd file format option.
Note: it may be appropriate to have 1 folder for your raw data, and 1 for your
imported data – otherwise things will get pretty complicated!

For data collected on the STOE Image Plate:
1. Go to Raw Data/Raw Data Handling
2. Go to File/Open, and select your file
3. Click Ranges/Add Ranges – add ranges 2 and above to range 1
4. Click Ranges/Extract Ranges – extract range 1, to a file with format
.ra1
5. Click File/Export, and select the *.xyd file format option
For data collected on the STOE PSD systems:
1. Go to Raw Data/Raw Data Handling
2. Go to File/Open, and select your file
3. Click File/Export, and select the *.xyd file format option
You can also import data in GSAS format by specifying the start and stop
angles, step size, the number of data points per line, the line number where
data start, and the wavelength.
Starting SIeve+ and loading your data
1. Clicking on the ‘PDF-4+ 2011’ icon on the desktop of the computer.
2. At the top of the screen, Click Edit and then Preferences
3. In the PDF Card tab, ensure that the ‘Wavelength’ matches that of your
experiment.
4. Click on the Simulated Profile tab and make sure that again the Type
and Anode match your experiment (i.e. Type = Ka1 or Ka1+2 and
Anode = Co, Cu or Mo as appropriate).
5. Click OK.
6. At the top of the screen, click Tools, and then SIeve+
7. Choose File, then Import Session and From Experimental Data
8. Change ‘Files of Type’ to match your Sietronics (*.cpi) filetype or All
Files to see your *.xyd file.

9. Another window appears! Select the appropriate wavelength for your
data
10. Click Show Graph. Make sure that the graph matches what you
actually did (correct 2θ range etc.)
11. Click Process Data
12. Another window opens! Here you can remove the background,
smooth the data, and remove Ka2 peaks. So far, I have found using
the default options OK, though those with significant amorphous (e.g.
glassy) components may need to be more careful: press Remove, then
Smooth
13. If your data were collected on the PW1825, D500 or D5000s, press Strip
K2. If the data were collected on the STOEs, instead press Skip>
14. You should notice that the Plot Preview in the Import screen has
updated with tick marks indicating your peak positions. SIeve+ will use
these tick marks to try to identify what phase(s) are present in your
sample. If you’re happy with the tick marks chosen, press Accept
Peaks. If not, repeat the process or use the Manual Peak Selection
controls to add or remove peaks.
15. Press Import
16. Press Don’t Apply Filter and wait while the software searches for
matches
A list of results appears, ranking the database entries in the order in which
they most closely resemble your data by some ‘Goodness of Match’ score.
This does NOT mean that the top result is definitely a match for your sample –
just its XRD pattern most closely matches your experimental data. The
chemistry should match what is reasonable or expected for your sample!
Double-clicking any entry in the list will display the PDF database card for that
entry.

Filtering your results
Now that you have a list of results, you may wish to filter them so that you only
have those listed which are appropriate for your sample!
To do this, you will first need to prepare a filter:
5. Go to the main ‘Search’ window (move the SIeve+ plus window if
necessary, but don’t close it)
6. Choose your filtering criteria – there are loads, divided up in to various
subtabs – ‘Subfiles/Database Filters’, ‘Periodic Table’ and so on. A
good starting point might be to select those elements present in your
sample. To do this:
a. Select either the Boolean or Yes/No/Maybe tab; I prefer the
latter, so we’ll do that here.
b. Click Set Unselected to ‘No’ – this will deselect all elements
c. Click an element to add it to the ‘Maybe’ list (i.e. this element
may or may not be in the phases in your sample). Clicking it
again will add it to the ‘Yes’ list (i.e. this element must be in all the
phases in the sample). A third click will return it to the ‘No’ list.
d. Repeat for all elements as appropriate.
7. Repeat for other search criteria if and where appropriate.
8. Once you are happy with the search criteria, click Search at the
bottom of the ‘Search’ window. A ‘Results’ list will appear in a new
window.
9. Go back to the SIeve+ window.
10. In the centre of the screen, under ‘Matches Filter’, click Select
11. You will see a list of all recent (i.e. in the current session) filters. Check
the descriptions, and click on the appropriate filter.
12. Click Apply Filter
You will now have a list of possible matches to your sample, organised by the
‘Goodness of Match’ score – bear in mind that the software only knows what

you tell it about your specimen, and so the top answer is NOT necessarily
correct – garbage in, garbage out!
Multi-phase samples
Follow all the instructions in the previous sections!
If you have a multi-phase sample, you can then click on the ‘handshake’
button at the top of the SIeve+ window to accept a card that you think is a
good match for one of the phases in your sample. The software will then look
for the next best matching phase (assuming you have made your filter criteria
quite general).
Once all the peaks in the diffraction pattern have been accounted for, the
software may be able to use the RIR method to give an estimated of the
quantity of phases present – providing the cards you have selected all have
an I/Ic value entered – many do not.
I/Ic is the height of the strongest reflection in the pattern (the 100% reflection)
expressed as a ratio to that of corundum, a-Al2O3. I/Ic is obtained by
preparing a 50:50 mixture (by WEIGHT) of the phase with corundum and
measuring the strongest reflection from the phase and from corundum as
obtained from the mixture.
The RIR method is relatively easy, but can be very inaccurate. There is a
tutorial about it on the ICDD website here which those considering it should
probably read. You definitely need randomly orientated powder samples,
and it only gives ratios not absolute amounts. If you want a more accurate
quantification, you really need to use the Rietveld method.

Publishing your final analyses
Once you’ve satisfactorily finished your phase analysis, you should have a
fitted graph that you want to export in to some format that you can take
elsewhere and view as a picture or paste in to a report, etc.
The best way I have found to do this within the software is...
1. In the SIeve+ window, go to the Phases menu and Open Simulated
Profile with Experimental Data
2. In the window that appears, click Edit and then Preferences
3. In the PDF Card tab, ensure that the ‘Wavelength’ matches that of your
experiment. Click on the Simulated Profile tab and make sure that
again the Type and Anode match your experiment (i.e. Type = Ka1 or
Ka1+2 and Anode = Co, Cu or Mo as appropriate).
4. If you wish to export the selected PDF card(s) as simulated profile(s),
the easiest and quickest way to broaden the simulated profile peaks to
more closely match yours is to click on the Simulated Profile tab and
change the ‘Profile’ setting from Pseudo-Voigt to Crystallite Size and
change the Mean Crystallite Diameter from e.g. 25 to 250 – play
around and see. This does not imply anything about the crystallite size
in your specimen! Click OK.
5. If you wish instead to export the selected PDF card(s) as stick traces
(i.e. peaks with no width), click Plots and Add Stick Trace. Enter the
correct PDF Card number, and click Open. Click OK to accept the
default ‘Fixed Slit Intensity’ type. Finally, click Plots, Delete, and select
the entry for the full simulate profile – this will be the one with the full
stoichiometry, PDF card number AND comments about Experimental
Intensity). Click OK and then Delete.
6. Repeat if and as appropriate for other PDF card(s).
7. Once you are satisfied, click File, Save. Change ‘Files of Type:’ to JPEG
and give a file name. This JPEG will be an image file that you can then
view or import in to Word, Powerpoint etc. as a picture file.

Hopefully I can find a more streamlined way of doing all this – but at least for
now, it should work!