TOTAL X-RAY POWDER PATTERN ANALYSIS. X Pert HighScore and X Pert HighScore Plus

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1 TOTAL X-RAY POWDER PATTERN ANALYSIS X Pert HighScore and X Pert HighScore Plus

2 X PERT HIGHSCORE AND HIGHSCORE PLUS Overview X Pert HighScore and X Pert HighScore Plus are software packages that incorporate the latest technology and algorithms for X-ray powder diffraction data analysis. X Pert HighScore is a comprehensive phase identification program for powder diffraction data, while X Pert 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 today s 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 PANalytical s 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. X Pert 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 X Pert HighScore and HighScore Plus

3 X Pert 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 X Pert 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

4 X PERT 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. X Pert 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. 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. 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. 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.

5 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 Kα 2 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.

6 X PERT 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. PANalytical s cluster analysis module uses several algorithms from common statistical packages, from the literature, and also some that are proprietary to PANalytical. X Pert HighScore Plus supports the cluster analysis of an unlimited number of scans, while X Pert 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 non- XRD (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. 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. 1. Correlation matrix 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

7 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

8 ONLY IN X PERT 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. PANalytical s 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.

9 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 exalf 3 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.

10 ONLY IN X PERT HIGHSCORE PLUS Crystallographic analysis Solutions for the catalyst industry Crystallographic analysis consists of two basic tasks: unit cell search (indexing) unit cell refinement (lattice parameter determination) 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. 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. X Pert 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.

11 Structure solution by charge flipping 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. HighScore Plus uses the Superflip algorithm developed at the EPFL, Lausanne, which can be set up and started easily. Structure viewing 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. 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. Lead and sulfur atom positions of lead sulfate found by the charge flipping algorithm. The marked atom indicates the actually selected position. Ball and stick model view of Linde A zeolite 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.)

12 Tools for XRD X Pert 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 Global and near PANalytical PANalytical is the world s 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. PANalytical s 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 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 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) F +31 (0) Regional sales offices Americas T F Europe, Middle East, Africa T +31 (0) F +31 (0) Asia Pacific T F Although diligent care has been used to ensure that the information herein is accurate, nothing contained herein can be construed to imply any representation or warrantee as to the accuracy, currency or completeness of this information. The content hereof is subject to change without further notice.please contact us for the latest version of this document or further information. PANalytical B.V. [2009] PN6999

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