ARL X'TRA Brochure - Thermo Scientific

e l e m e n t a la n a l y s i sThermo Scientific ARL X’TRAPowder X-ray Diffraction SystemUncompromised Intensity and ResolutionPart of Thermo Fisher Scientific

ARL X’TRAPowder X-ray Diffraction SystemARL X’TRAHigh performance powder X-ray diffraction systemThe Thermo Scientific ARL X’TRA is anadvanced multi-purpose system designed foracademic or industrial analyticallaboratories. It is ideal either for routineanalysis or highly demanding applicationsrequiring dedicated accessories. Analyticalperformance, ergonomics and safety are themajor characteristics of this outstandinginstrument.With 20 years of experience in theNorth America market and high precisionengineering with excellence in X-rayspectroscopy, the ARL X’TRA offers aleading edge in the field of X-ray powderdiffraction technology.The design of the ARL X'TRA is basedon a vertical θ-θ Bragg-Brentano geometryfor convenient sample preparation andsample handling. With the unique Peltierdetector technology, ultimate performancein both angular and energy resolution canbe achieved without using β-filters ormonochromators. This elegant designyields higher diffraction intensities andsuperior resolution compared to traditionalpoint detectors.Depending on the type of analysis orsample type, the system can be easilyreconfigured using pre-aligned Plug & Playaccessories such as temperature chambers,parallel beam optics, transmission stage.The modular approach of the ARL X’TRApowder diffraction instrument provides fullflexibility without any compromise inperformance for a large range ofapplications covering both inorganic andorganic polycrystalline materials.A wide range of analyticaltechniquesX-ray diffraction is a versatile and nondestructivetechnique that reveals detailedstructural and chemical information aboutthe crystallography of materials.• Identification of single or multiple phasesin an unknown sample• Quantification of known phases of amixture• Crystallography – solving crystal structure• Non ambient analysis – crystal structurechanges with temperature, pressure orgas phase• Surface and thin film analysis• Texture analysisA broad range of materialsNatural or manufactured materials oforganic or inorganic chemistry can becharacterized with this technique. Sometypical materials are listed here:• Chemicals• Pharmaceutical substances• Environmental dusts• Asbestos• Rocks• Clay minerals• Zeolites• Polymers• Metals• Cement and building materials• Forensics• PigmentsPharmaceuticals Geology Ceramics

Environment Building materials Chemicals

ARL X’TRAPowder X-ray Diffraction SystemTechniqueThe most flexible goniometer geometryIt is now well accepted that for the majority ofthe powder X-ray diffraction experiments, thevertical θ-θ Bragg-Brentano setup replaces thetraditional vertical or horizontal θ-2θ geometry.The main reason is that the sample stage doesnot move during the scan and therefore evenloose powders or liquids can be analyzed.In this geometry, the ARL X’TRA offersthe best configuration providing superiorflexibility for future upgrades orreconfigurations with optional accessories.The reliability and accuracy of this systemis achieved thanks to closed loop servo motorswith optical encoders.Choose the best trade-off betweenintensity and resolutionThe continuous slit aperture capability of theARL X’TRA system allows an instrumentoperator to choose the optimum balancebetween intensity and angular resolution.Continuous adjustment capability allowsinstrument operators to optimize the slitsettings in accord with the crystallographicquality of the materials.As shown in Figure 3, an angularresolution < 0.04° FWHM can be measuredeasily in standard configuration without usingbeam path accessories and with a normalscan speed (0.1° 2θ/s).A precise control of the radial and axialcollimation of the beam is ensured withmicrometer-controlled slits and anexchangeable/removable set of soller slits.Precise “zero plane” adjustmentSample height is critical to get accurate datain Bragg-Brentano geometry (standard setup)and to get best intensity in parallel beamconfiguration.The standard sample stage on the ARLX’TRA includes a micrometer based stagewith height adjustment and height positionblock. Depending on the shape and dimensionof the sample, the micrometer adjustment canbe used to precisely adjust the specimenheight at the scale of 10 µm. The precision inthe micrometer adjustment also yieldsnumeric traceability of the aligned position.Modular stage designThe modular design or so called “Plug & Play”of the ARL X’TRA allows users to exchangepre-aligned sample stages without requiring alengthy realignment procedure. The standardsample stage incorporates one mechanical pinthat precisely orient both the translational androtational orientation of the stage relative tothe goniometer. Complete reconfiguration ofthe diffractometer is now achievable inseveral minutes instead of hours.Unique Peltier cooled Si(Li) solid-statedetectorFor more than 20 years, solid-state detectorshave been a popular detection option on ourinstruments. The latest version is a Peltiercooled Lithium drifted Silicon solid-stagedetector (see Figure 1). It is sealed under highvacuum with passive getters that ensure thelong term stability of the vacuum.The 5 stage Peltier pyramid allows tocool down the Si(Li) crystal down to atemperature close to -100°C and therefore,the internal noise of this detector is extremelylow:

600050004000A.U.30002000Speed of acquisition with the ARL X’TRA on1000a Zeolite 4A sample: In green, the datameasured in less than 5 minutes and in red,the data measured in 20 minutes05 15 25 35 45 552Θ0.2Raw dataFWHM dataFWHM Cagliotti fit0.16A.U.0.120.08FWHM °Figure 3: Full Width at Half Maximum (FWHM) of the NISTLaB6 (SRM660a) reflections as a function of 2θ CuKα. Thered curve shows the Cagliotti fit and in blue, the XRD rawdata measured in 2 hours without primary or secondarybeam monochromator0.04010 60 110 1602Θ°

ARL X’TRAPowder X-ray Diffraction SystemWinXRD for data acquisition anddata analysisBest performance from the X-ray diffractionsystem is ensured with WinXRD, a Windows ®XP based software. This comprehensivesoftware package is fully integrated andfacilitates a smooth progression from datacollection through analysis and report writing.Data can be handled with convenienceand efficiency thanks to audit trails, useraccess controls and export functions.The data collection part offers thepossibility to perform different types ofmeasurements:• Symmetric θ:θ normal scans• Asymmetric θ scans (e.g. for grazingincidence)• And finally ω rocking scans.Data analysis software includes variousanalytical features like:• Basic data treatment (backgroundsubstraction, smoothing, peak extraction,profile fitting, etc.)• Search-match routine using the ICDD oruser database• Quantitative Phase Analysis• Crystallite size determination• Crystallographic analysis (indexing andunit cell refinement)• 2D and 3D graphic display formultiple graphs• Texture analysis with 2D and 3Dpolefigure displayAdvanced third party software allowmore specific data analysis like:• SIROQUANT for routine mineralsquantification based on the Rietveldmethod• Visual CRYSTAL ® for full patternqualitative and quantitative analysis.Enhanced capabilities withaccessoriesIn addition to the superior performance ofthe standard instrument configuration mainlydedicated to phase identification & phasequantification, the system can be quicklyreconfigured with accessories providingsuperior analytical capabilities like:• Batch mode for routine measurementswith the multi-position sample changer• Texture analysis in transmission modewith the transmission stage• Non-ambient experiments from lowtemperature to very high temperatureconditions under vacuum, air, inert gasesor controlled humidity conditions• Air sensitive material analysis using thecapillary stage• Reactive materials with theenvironmental stage• Low Z materials, small samples,irregularly shaped samples can all becharacterized with great efficiency usingthe parallel beam setup consisting of theparabolic mirror and the thin filmcollimator and more.Rapid & reproducible accessoryexchangeRecent developments in high precisionmechanics significantly enhanced thepositioning reproducibility of the accessories.With the ‘Plug & Play’ system, it is nowpossible to quickly exchange stageaccessories and optical configurationswithout requiring time consuming realignment.Moreover, the softwareconfiguration manager stores all specificsettings so that the user only has to selectthe pre-aligned optical and stage accessoriescurrently installed from software menus. Allinstrument configuration details are recordedand associated with the data.From the left to the right (Figure 1), theexchangeable components on thegoniometer are:• X-ray tube• Primary beam path accessories: divergentslits, soller slits, anti-scatter slits,parabolic mirrors, pinhole collimator, filters• Sample stages: basic stage, singlesample spinner, sample changer,environmental chamber, capillary stage,transmission stage, temperature stages(low temperature to high temperature),pressure reactor• Secondary beam path accessories: antiscatterslits, soller slits, receiving slits,thin film collimator, monochromators• Detectors: Peltier cooled solid-statedetector or Scintillation detectorFigure 1: Schema of the geometry of the theta:theta goniometerPeak position extraction by profile fitting, an example ofRanitidine analysisPhase identification by the search-match method using theICDD database

1 2 3 45 6 7 81. High temperature chamber with samplespinner (Anton Paar HTK 1200)2. Parabolic mirror and thin film collimator3. Capillary stage for small and/orreactive samples4. 12 position sample changer forautomated batch processing5. Pinhole collimator for point focus forsmall samples6. High temperature chamber for thermalproperty analysis (Anton Paar HTK 16/20)7. Environmental chamber for reactivesamples analysis8. High/Low temperature chamber withliquid nitrogen Dewar (Anton PaarTTK 450)9. Pressure and temperature reactor chamberwith sample spinner (Anton Paar XRK 900)9Temperature transition diagram of TiO2 polymorphicphases: Anatase and Rutile3D Polefigure of an NBT film

Technical specifications for the ARL X’TRAElectrical requirementsSingle phase 200-250V, 32A, 50-60 HzShipping weight600 kilograms, including packaging.Water requirements4.0 liters per minute, 4 - 6 bars, 16°-24° CTemperature:18º to 32º CFilterFive-micron filter system is recommended to remove particles from water supply.Dimensions of the instrument(Red: dimensions for shipment)986 mm1220 mm1483 mm1956 mmIn addition to these offices, ThermoFisher Scientific maintains a networkof representative organizationsthroughout the world.Australia+61 2 8844 9500 • analyze.au@thermo.comAustria+43 1 333 50340 • analyze.at@thermo.comBelgium+32 2 482 30 30 • analyze.be@thermo.comCanada+1 800 532 4752 • analyze.ca@thermo.comChina+86 10 5850 3588 • analyze.cn@thermo.comDenmark+45 70 23 62 60 • analyze.dk@thermo.comFrance+33 1 60 92 48 00 • analyze.fr@thermo.comGermany+49 6103 408 1014 • analyze.de@thermo.comIndia+91 22 6742 9434 • analyze.in@thermo.comItaly+39 02 950 591 • analyze.it@thermo.comJapan+81 45 453 9100 • analyze.jp@thermo.comLatin America+1 608 276 5659 • analyze.la@thermo.comNetherlands+31 76 587 98 88 • analyze.nl@thermo.comSouth Africa+27 11 570 1840 • analyze.sa@thermo.comSpain+34 91 657 4930 • analyze.es@thermo.comSweden / Norway / Finland+46 8 556 468 00 • analyze.se@thermo.comSwitzerland+41 21 694 71 11 • analyze.ch@thermo.comUK+44 1442 233555 • analyze.uk@thermo.comUSA+1 800 532 4752 • analyze.us@thermo.com825 mm1154 mmwww.thermo.comLaboratory Solutions Backed by Worldwide Service and SupportTap our expertise throughout the life of your instrument. Thermo Scientific Servicesextends its support throughout our worldwide network of highly trained and certifiedengineers who are experts in laboratory technologies and applications. Put our teamof experts to work for you in a range of disciplines – from system installation, trainingand technical support, to complete asset management and regulatory complianceconsulting. Improve your productivity and lower the cost of instrument ownershipthrough our product support services. Maximize uptime while eliminating theuncontrollable cost of unplanned maintenance and repairs. When it’s time toenhance your system, we also offer certified parts and a range of accessories andconsumables suited to your application.Thermo Electron SA, Ecublens,Switzerland is ISO certified.©2007 Thermo Fisher Scientific Inc. All rights reserved.Windows ® is a registered trademark of Microsoft corp.Visual CRYSTAL ® is a registered trademark ofCorporation Software sprl. All other trademarks arethe property of Thermo Fisher Scientific Inc. andits subsidiaries.Specifications, terms and pricing are subject to change.Not all products are available in all countries. Pleaseconsult your local sales representative for details.BR41188_E 07/07CTo learn more about our products and comprehensive service offerings,visit us at www.thermo.com.