Transcript Future versions HighScore (Plus)

NEW FEATURES IN ANALYSIS SOFTWARE FOR POWDER DIFFRACTION
Jakob Noreland
Nordic XRF & XRD Application Specialist
Norwegian X-ray Conference
Fevik, Norway
September 2, 2014
J.Noreland
July 8, 2015
1
Phase mixture
Characteristic diffractograms
Quartz (SiO2)
+
Salt (NaCl)
Superposition of the peaks
SiO2 + NaCl
J.Noreland
July 8, 2015
2
Phase identification
Counts
SiO2 + NaCl
10000
Collect the diffraction pattern
for the unknown sample
5000
0
50
Comparison with a database of known
diffraction patterns
• ICDD – Int. Centre for Diffraction data
• PAN-ICSD, or free alternatives
100.000 – 500.000 possible patterns
Phase = crystalline
material with a typical 3D
atomic arrangement
J.Noreland
Phase
identification:
July 8, 2015
55
60
65
70
75
Position [°2Theta] (Copper (Cu))
Determination of peak
positions and intensities
SiO2
NaCl
3
Reference Databases
• A reference database with known
diffraction patterns of pure phases is
mandatory for phase identification.
• There are several commercial or free
possibilities:
1. Commercial ICDD reference databases
2. Commercial PAN-ICSD ref. database
3. The free COD reference database
4. Special, user-made reference databases
J.Noreland
July 8, 2015
4
ICDD Reference Databases
ICDD = International Centre for Diffraction
Data
• Offers time-restricted licenses for several
database products without (PDF-2) or with
(PDF-4) crystal structure data, for single or
multiple PC’s.
• Best data quality, good coverage of old and
new phases, high price, yearly license
• Inorganic, organic and mineral databases
available
• Link: http://www.icdd.com/
J.Noreland
July 8, 2015
5
PAN-ICSD Reference Database
ICSD = Inorganic Crystal Structure Database
• The PAN-ICSD is a PANalytical reference
database derived from the ICSD.
• It contains reference patterns and crystal
structures from inorganic (and some mineral)
phases.
• Licensing is the same as for PANalytical
analysis software
•
Original link: http://www.fizkarlsruhe.de/icsd.html
J.Noreland
July 8, 2015
6
COD = Crystallography Open Database
• Contains crystal structures from literature
(inorganic, organic, minerals)
• PANalytical has calculated a reference database
for search-match from this data, including
crystal structure data.
• This database is available free-of-charge! No
limits on the number of PC’s or usage time!
 Download adress:
www.crystallography.net/archives/2013/PANalyti
cal/
J.Noreland
July 8, 2015
7
COD = Crystallography Open Database
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
Dear PANalytical HighScore (Plus) User:
Purpose:
The COD database file you find here is meant to be used with version 3.0a or higher of the PANalytical HighScore or
HighScore Plus software packages.
ATTENTION:: This database can NOT be used with previous versions (1.0, 2.0, 2.1, 2.2, 3.0) of this software.
Procedure:
* Install the database file (COD_2013.hsrdb) on your PC by simply unzipping it from the downloaded COD_May2013_4HS.ZIP file.
You better ‘Defragment’ your disk before putting such a large file on it. (It is recommended to put such a database file NOT on the C:
drive.)
* Announce the new database for use in the software. Use the ‘Customize, Manage Databases, Add HighScore database...’
function or the ‘Search for databases’ function.
Details
The file ‘COD_2013.hsrdb’ contains a total of 223339 calculated reference patterns.
This conversion is based on revision 79023-2013.04.04 of the original COD.
The reference patterns are subdivided into 4 subfiles:
a)
b)
c)
d)
J.Noreland
User Organic
User Inorganics
Metallic
User Mineral
190129
33210
1953
11795
patterns
patterns
patterns
patterns
(C-H bond present in CIF)
(all other CIFs)
(only metals present in CIF)
(mineral name is present in CIF)
July 8, 2015
8
COD = Crystallography Open Database
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
These 4 subfile properties are automatically assigned, depending on criteria tested for each CIF entry. With the
introduction of subfiles a separate minerals database file is no longer available.
Changes:
No significant changes with respect to previous versions. The number of entries in the COD is growing fast.
Citation
Please use the following text, when you publish results achieved with a COD reference database:
Gražulis, S., Daškevič, A., Merkys, A., Chateigner, D., Lutterotti, L., Quirós, M., Serebryanaya, N. R., Moeck, P.,
Downs, R. T. & LeBail, A. (2012) "Crystallography Open Database (COD): an open-access collection of crystal
structures and platform for world-wide collaboration". Nucleic Acids Research 40, D420-D427.
COD reference database 2012:
Gražulis, S.; Chateigner, D.; Downs, R. T.; Yokochi, A. F. T.; Quirós, M.; Lutterotti, L.; Manakova, E.; Butkus, J.;
Moeck, P. & Le Bail, A.; Crystallography Open Database - an open-access collection of crystal structures, J. Appl.
Cryst., 2009, 42, 726-729.
When your research relies only the subset of COD containing mineral data
from AMCSD (the range 9* datasets), then please mention this source database:
Downs, R. T. & Hall-Wallace, M. (2003). "The American Mineralogist
Crystal Structure Database" American Mineralogist 88, 247-250."
J.Noreland
July 8, 2015
9
Possibilities and limitations
• It is often possible to identify up to 10 phases
in a phase mixture
• Typical detection limits are in the order of 0.1
to 1 % per phase
Other parameters can also be determined:
• Degree of crystallinity
• Crystallite size
J.Noreland
July 8, 2015
10
Typical samples
Powder specimen from
• Cement
• Pharmaceuticals
• Minerals
• New materials
•…
J.Noreland
July 8, 2015
11
Typical configuration
• Pre-aligned optics
• Measurement in
transmission or
reflection
• Sample in glass
capillary if sensitive
to air
• Option for nonambient conditions
J.Noreland
July 8, 2015
12
Current PANalytical SW used for phase analysis
• Highscore (Plus) for phase ID (+Rietveld)
– Database is also needed: ICDD, ICSD, …
• Quantify for quantification using a calibration
model, selected from 10 available models
• Industry for quantification using calibrations in
a more flexible way
• Examples from the Nordic countries:
– Respirable silica
– Potflux (Al production)
– Cutting tools (hard metal with coating)
J.Noreland
July 8, 2015
13
Typical phase ID analysis in Highscore
J.Noreland
July 8, 2015
14
HS(+) version 4.0 is a true “next major version”:
1. Many things are programmed new from
scratch
2. Some things are re-done from scratch
3. Few things are done in a different way (in the
code, NOT visible from the outside)
J.Noreland
July 8, 2015
15
What’s new in HighScore (Plus) version 4.0?
1. Partial Least-Squares Regression (PLSR)
2. Merging of all refinement modes
3. Wavelet based adaptive de-noising
4. XRF data integration: Calculator & Restrictions
5. Bitmap to scan converter
6. Scripting improvements
7. MS Windows Explorer integration
For further details on all these topics please go to
our website www.panalytical.com, register and
download the webinar ”What’s new in HighScore
(Plus)?” presented by Thomas Degen (recorded on
November 12, 2013).
J.Noreland
July 8, 2015
16
For existing HighScore (Plus) users
J.Noreland
July 8, 2015
17