TOTAL X-RAY POWDER PATTERN ANALYSIS

XPert HighScore
and
XPert HighScore Plus

XPERT HIGHSCORE AND HIGHSCORE PLUS

Overview
XPert HighScore and XPert HighScore
Plus are software packages that
incorporate the latest technology and
algorithms for X-ray powder diffraction
data analysis. XPert HighScore is a
comprehensive phase identification
program for powder diffraction data,
while XPert HighScore Plus has the
additional functionalities of profile
fitting, Rietveld, crystallographic
and extended cluster analysis. These
packages are specifically designed
to meet the demands of todays
materials analysis, whether identifying
complex phase mixtures, performing a
standardless quantitative analysis using
Rietveld, or simultaneously analyzing a
large number of scans to look for similar
composition, or clustering.

Solutions for geology

PANalyticals software development

engineers are dedicated to bringing
you the latest advances in analysis
technology, together with tools
and features that make diffraction
data interpretation easier and more
accurate than ever. XPert HighScore
and HighScore Plus utilize all the
conveniences of the modern Microsoft
Windows platforms: the interface can
be customized by each individual user;
analysis procedure batches can be saved
to toolbar buttons for one-touch, fully
automated data analysis, tuned to a
variety of materials; report formats can
also be customized; thumbnails and
preview pictures support you to select
any existing measurement or analysis
file.
PANalytical software licensing is
designed to support the way you work.
Multiple software installations* allow
you to transfer data from the lab to
your office or laptop - wherever is most
convenient.
*Please see the Terms and Conditions of the
Software License Agreement for details.
Automatic phase identification and semi-quantitative analysis of a mineral mixture - a one-button
operation in both XPert HighScore and HighScore Plus

XPert HighScore features

A third generation search-match
algorithm working on profile and
peak data, either simultaneously or
individually, including an automatic
residue search and automatic phase
identification, thus greatly improving
phase analysis
Grouping of similar or nearly identical
candidate patterns
Fast search and retrieval for the ICDD
PDF2/PDF4 reference databases
Simultaneous support of multiple
reference databases
Possibility of separate, multiple user
reference databases
Extended profile fitting functions
using a state-of-the-art, fast and
stable BCPE mathematical solver
A multiple document interface
displaying any number of scans, which
allows simultaneous batch processing
of all open scans
Line profile analysis
User-defined batches and parameter
sets plus a command line interface to
allow the complete automation of the
analysis

Automatic semi-quantitative analysis

based on the RIR method
Full pattern autoscale analysis after
BISH & CHIPERA
Percent crystallinity determination
Fully customizable graphical user
interface
Add, subtract, merge and simulate
scans
Advanced reporting options in MS
Word and RTF
Full pattern cluster analysis, which
automatically sorts closely related
scans of an experiment into clusters
Support for XRDML file format (based
on XML technology), as well as other
PANalytical and many proprietary file
formats
A complete on-line Quick Start Guide,
a tutorial with practical examples, and
a comprehensive HTML-based help
system

Note: Software incorporating audit trail functionality for GLP and 21

CFR Part 11 compliance is also available

XPert HighScore Plus enhancements

Automated and semi-automated
Rietveld analysis, Pawley and Le Bail
fits
Rietveld control file customization for
industrial automation
Crystallographic analysis by four
methods DICVOL, TREOR, ITO, and
McMaille
Expanded cluster analysis
Integrated Superflip charge flipping
algorithm and live electron density
display

XPERT HIGHSCORE AND HIGHSCORE PLUS

Phase identification

Search - match
Identification of the crystalline
components or phases in a sample or
mixture is a primary application of
X-ray diffraction. XPert HighScore and
HighScore Plus both use a powerful
search-match algorithm that combines
peak and profile data and instantly
re-scores an existing candidate list
based on whatever input is preferred.
Each method has its advantages: peak
data more accurately identify major
phases, while profile data more readily
elucidate minor phases. A skillful
combination of both often produces the
most reliable results.
Candidates groups
On demand candidates are put into
distinctive groups by agglomerative
cluster analysis, based on their similarity.
This results in a much better overview
in case many very similar or nearly
identical candidates are found.

Automatic identification
When a list of candidates is determined,
the best matches can be automatically
accepted using a sophisticated filter.
This filter combines several criteria
to select the most likely phase(s).
Automatic identification can be
switched on and off, and the filter can
be tuned as needed.
Push-button operation
Batch buttons, located on the toolbar,
can be programmed to handle certain
types of samples. New buttons are easily
created, with a user-defined sequence
of analysis steps as required. These
batch programs can also be started by
other applications to automate tasks.

Reference databases
Reference databases e.g. from the
International Centre for Diffraction
Data (ICDD) are supported, including
the portable Web-PDF 4+ file. User
reference patterns are stored in
separate, dedicated user reference
databases. Multiple databases can be
used in any combination for phase
identification. Measured reference scans
form an integral part of some reference
databases.

Complete integration
The search-match algorithm is
completely integrated in the graphics.
Whenever data is changed, for example
by adding or deleting peaks, the scores
of all candidates and matches are
dynamically recalculated.

Semi-quantitative analysis
RIR (Reference Intensity Ratio) data can
be used to estimate the quantity of all
identified phases.
RIR data (or I/Icorundum data) can be
added or edited for every reference
pattern. This can be useful as an
approximate analysis for a sample, if
good calibration samples or structure
information are not available.

Restrictions based on chemistry, quality, subfile, crystallography or any reference card

information (such as color) are possible.

Pattern treatment
functions
Solutions for mining
The software incorporates a full range
of pattern treatment functions to aid
diffraction data analysis including:
Background determination
Peak searching
Profile fitting and LP analysis
K2 stripping
Smoothing
Correction functions:
- Systematic error
- Automatic/fixed slit conversion
- Outlier correction
Math functions:
- Add
- Subtract
- Sum measured diffraction patterns
and simulated scans

A mining sample diffraction pattern was processed using a batch button programmed for
mineral analysis.

Profile fit
Highlights:
State-of-the-art,
proprietary mathematical
BCPE solver (bound
constraints parameter
estimation)
Three profile functions,
each either unsplit, single
or double split
- pseudo-VOIGT
- PEARSON 7
- VOIGT

Profile fitting is
most often used to
deconvolute severely
overlapping peaks
into single peaks. It
calculates peak profile
characteristics by
applying adjustable,
mathematical profile
functions. These
functions obtain
more accurate
information on peak
parameters such as
position, intensity,
width and shape.
The peak parameters
can be used to derive
crystallite size and/
or microstrain data
through line profile
analysis.

XPERT HIGHSCORE AND HIGHSCORE PLUS

Cluster analysis is
a four step process
that automatically
produces:
a correlation matrix
a dendrogram
a principal components
analysis 3-D score plot
and individual clusters

Cluster analysis automatically sorts all

closely related scans of an experiment
into clusters, and marks the most
representative scan of each cluster as
well as outlying patterns. It is useful
for non-ambient experiments, mining
samples and soil mapping, for synthesis
experiments such as zeolites, and for
finding polymorphs and solvates in drug
development.
PANalyticals cluster analysis module
uses several algorithms from common
statistical packages, from the literature,
and also some that are proprietary
to PANalytical. XPert HighScore Plus
supports the cluster analysis of an
unlimited number of scans, while XPert
HighScore can cluster up to a maximum
of 50 scans per analysis.
XRD data can now be cross-linked with
other data. Spearmans Rho, Pearsons R
and overall rank correlation methods
are used to compare and cluster nonXRD (eg. Raman) data. The overall speed
of cluster analysis is 8 - 10 times higher
than in previous versions.

Cluster analysis greatly simplifies the analysis

of large amounts of data
1. Cross-comparison of all scans in an
experimental group, resulting in a
color-coded matrix of similarities.
2. Agglomerative hierarchical cluster
analysis puts the scans in different
classes defined by their similarity,
producing a dendrogram. The
number of clusters is determined
by statistical methods or manually,
and the most representative scan
within each cluster is determined.
The representative scans can then
be further processed for phase
identification, quantification and so
on.

1. Correlation matrix

3. Principal components analysis (PCA)

can be carried out as a separate and
independent method to visualize and
judge the quality of the clustering.
4. Individual clusters of scans are
displayed on separate tabs, as well as
any unclustered or outlying scans.

2. Dendrogram and cut-off value

3. 3D score plot from principal components

analysis allows visual confirmation of the
observed clusters with confidence spheres

4. Similar scans sorted into one cluster

Solutions for the pharmaceutical industry

A large number of scans can
be processed simultaneously
to identify the presence
of solvates, hydrates and
polymorphs in an active
pharmaceutical ingredient
(API). The sampling grid can
be generated to visualize the
results from a well plate

Line Profile analysis

Information on the
microstructure of crystalline
materials is obtained
from the width and the
shape of X-ray single peak
profiles. Before the analysis
HighScore corrects the
profiles for instrumental
broadening.
The results are microstrain
and / or crystallite size
information for each peak.
For multiple peaks a
WILLIAMSON-HALL plot
shows the average results.
Fitted profile and peak list with FWHM and integral breadth numbers on top,
net GAUSS and LORENTZ broadening, WILLIAMSON-HALL plot and size-strain results at the bottom

ONLY IN XPERT HIGHSCORE PLUS

Rietveld analysis
Solutions for the building
materials industry

The Rietveld method is a full-pattern

fitting method in which a measured
diffraction profile and a calculated
profile are compared and, by varying
a range of parameters, the difference
between the two profiles is minimized.
A standard Rietveld refinement requires
crystal structure data, such as atom
positions. In addition to structural
information, the scale factors calculated
for a mixture of phases are proportional
to weight fractions, making standardless
quantitative analysis possible.
PANalyticals Rietveld algorithm is an
advanced implementation of widely
accepted and proven technology,
continuously developed over the past
few decades. The combination of

reference patterns, linked to a choice of

structures for Rietveld analysis, allows
a user to create a batch file for the
complete analysis of materials.
Rietveld can answer:
How much of each phase is present?
Is preferred orientation present in the
sample?
What are the precise lattice
parameters for the material?
How much of one atom is substituted
for another?
How small are the crystallites, or is
microstrain contributing to peak
broadening?
How much amorphous material is
there?

Automatic quantification of phases in clinker and cement products provides the cement industry
with accurate information for process control from a five minute scan.

Aluminum electrolytic bath analysis

Potflux

Rietveld analysis of a standard electrolytic bath showing

phase concentrations, including two different Ca-Cryolite
phases from a 3 minutes scan

Potflux analysis with the

standardless Rietveld
method has several
advantages: You can
distinguish between and
determine the different
Ca-Cryolite phases. Crucial
process parameters like
exAlF3 or bath ratio are
calculated directly from the
phase quantification and
total calcium data. Line
overlaps, sample height
and preferred orientation
do not influence the
results. The method can be
extended to non-standard
bath chemistry.

Additional functionality
Scripting
All HighScore Plus functions can
be changed and combined in
new ways by scripts. These small
external programs allow to write
dedicated output, to read and
process other input data and to
perform specific calculations. Every
property of all objects handled by
the software can be influenced this
way.

Crystallite size / micro strain analysis

Le Bail fit - to confirm the unit cell
and space group and to extract
structure factors
HKL file fit - to work with phases of
unknown structures
Determination of the amorphous
content
Automatic or semi-automatic
refinement: from remote control
(LIMS) through push-button operation
to refining individual paramaters,
the software makes Rietveld easy for
novices and experts alike
Batch files for the automation of data
analysis and reporting

Roboriet
Another version of the software
- RoboRiet - executes preprogrammed Rietveld analyses
in a production environment.
It acts automatically on the
presence of new measurements
and communicates the results to a
printer, a disk drive, Excel lists or
directly to a LIMS system.

ONLY IN XPERT HIGHSCORE PLUS

Crystallographic
analysis
Crystallographic analysis consists of two
basic tasks:
unit cell search (indexing)
unit cell refinement (lattice parameter
determination)

Solutions for the catalyst

industry

Exact lattice parameters and relative

peak heights are crucial parameters of
many zeolites used in industrial processes. A Le Bail fit with HighScore Plus
determines the lattice parameters and,
optionally, the sample height. In contrast to the ASTM norm it uses all peaks

of the measurement, and simultanously

determines the relative peak intensities. The calculation of the crystallinity
percentage is easily integrated and the
whole process can be automated at will.

The determination of the unit cell and

a proper indexing of the measured
reflections is mandatory to characterize
a new, previously unknown phase. It is
also useful to check for minor variations
in a unit cell caused by solid-solution
effects, cation or anion exchange, or
absorption effects. Alternatives to the
traditional cell refinement are either a
LE BAIL or a PAWLEY fit.
Supporting functions include unit cell
reduction, unit cell transformation,
unit cell standardization and search
for possible space groups. Unit cell
refinement can be made part of a batch
of actions.

XPert HighScore Plus offers

four different indexing
methods:

Le Bail fit of a cubic zeolite with refined cell parameters

and specimen displacement. The peak list with relative peak
heights is shown too.

DICVOL
TREOR
ITO
McMAILLE
Crystallinity result.

Structure solution
by charge flipping
The results are presented as a three-dimensional electron density map with up to
three density levels. Routines to locate atoms, to standardize the structure and to
use difference Fourier maps are included.
Charge flipping is a fast ab initio
structure solution method. It was
developed for single crystal data in
2004, but was extended for powder
diffraction measurements later and is
used successfully for both small and
large, inorganic and organic structures.
Advantages of this method are: speed
(typically seconds to minutes), no need
for space group symmetry data, and no
chemical bond information required.
The only necessary input are lattice
parameters and reflection intensities.
Most of the time a LeBAIL or a PAWLEY
fit on good quality data is used to
extract the true net intensity of (even
overlapping) peaks.

Lead and sulfur atom

positions of lead
sulfate found by
the charge flipping
algorithm. The marked
atom indicates the
actually selected position.

HighScore Plus uses the Superflip

algorithm developed at the EPFL,
Lausanne, which can be set up and
started easily.

Structure viewing

Ball and stick model view of Linde A zeolite

The structure plot pane is a simple

means of displaying crystal structures.
It allows a user to choose the colors of
atoms, polyhedral viewing, and allows
the image to be shifted, turned around
an axis, rolled or zoomed for a better
view of the structure.

Polyhedral structure view of rutile

Structure solution of fayalite by a difference

Fourier map. The selected position (+) is a Si
atom site. (The real structure is overlaid for
comparison.)

Tools for XRD

XPert HighScore and HighScore
Plus contain the following useful
tools for XRD analysis
Mass absorption coefficient/
depth calculator
Bragg calculator
Periodic table
Symmetry explorer
Scherrer calculator

PANalytical
PANalytical is the worlds leading supplier of analytical instrumentation and
software for X-ray diffraction (XRD) and X-ray fluorescence spectrometry (XRF),
with more than half a century of experience. The materials characterization
equipment is used for scientific research and development, for industrial process
control applications and for semiconductor metrology.
PANalytical, founded in 1948 as part of Philips, employs around 950 people
worldwide. Its headquarters are in Almelo, the Netherlands. Fully equipped
application laboratories are established in Japan, China, the USA, and the
Netherlands. PANalyticals research activities are based in Almelo (NL) and on
the campus of the University of Sussex in Brighton (UK). Supply and competence
centers are located on two sites in the Netherlands: Almelo (development and
production of X-ray instruments) and Eindhoven (development and production
of X-ray tubes). A sales and service network in more than 60 countries ensures
unrivalled levels of customer support.
The company is certified in accordance with ISO 9001:2000 and ISO 14001.
The product portfolio includes a broad range of XRD and XRF systems and software
widely used for the analysis and materials characterization of products such as
cement, metals and steel, nanomaterials, plastics, polymers and petrochemicals,
industrial minerals, glass, catalysts, semiconductors, thin films and advanced
materials, pharmaceutical solids, recycled materials and environmental samples.
Visit our website at www.panalytical.com for more information about our
activities.
PANalytical is part of Spectris plc, the precision instrumentation and controls
company.

PANalytical B.V.
Lelyweg 1, 7602 EA Almelo
The Netherlands
T +31 (0) 546 534 444
F +31 (0) 546 534 598
info@panalytical.com
www.panalytical.com
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Although diligent care has been used to ensure that the information herein is accurate, nothing contained herein can be construed to imply any
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further notice.Please contact us for the latest version of this document or further information. PANalytical B.V. [2009]. 9498 702 16111 PN6999

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