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Uncompromised Intensity and Resolution
Thermo Scientific ARL X’TRA Powder X-ray Diffraction System
Part of Thermo Fisher Scientific
e l e m e n t a l a n a l y s i s
The 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 design yields 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 non-destructive technique that reveals detailedstructural and chemical information aboutthe crystallography of materials.• Identification of single or multiple phases
in an unknown sample • Quantification of known phases of a
mixture • Crystallography – solving crystal structure• Non ambient analysis – crystal structure
changes with temperature, pressure orgas phase
• Surface and thin film analysis• Texture analysis
A 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• Pigments
ARL X’TRAHigh performance powder X-ray diffraction system
Pharmaceuticals Geology Ceramics
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Environment Building materials Chemicals
Technique
The 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 position
block. 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: <0.1 CPS.
Quantitative phase analysis in the rangeof 0.1 weight % (depending on the sample) ispossible due to very low detector noise level.
This solid-state detector allows the userto electronically select photons based upontheir energy signature thereby eliminating theneed for beta filters or diffracted beammonochromators to remove unwanted sourceof X-ray intensity (e.g. diffraction from beatwavelengths, Bremsstrahlung and/or samplefluorescence as shown in Figure 2).
The fluorescence efficiency for Fe with Curadiation is very high so if we look at a Fe
powder, a conventional scintillation detectorshows about 5,000 cps of Fe fluorescence. It isalso showing Kβ contributions for the strongerdiffraction peaks (green curve in Figure 2). Thisis a big problem with conventional detectorsbecause while the β filter can get rid of Kβ, Fefluorescence cannot be discriminated. Theonly way to get rid of the Fe fluorescencebackground is to use secondary beammonochromators but this strongly reducesoverall intensities. The Si(Li) Peltier detectorhas no problem removing these interferences.
This resolution in energy can also beexploited to tune the wavelength andtherefore the energy. To get simplified XRDpattern with minimum peak overlaps, one canfor instance collect a pattern in Kβ modeinstead of Kα which shows its characteristicKα1/2 doublet. The optical mount designallows both a para-focussing slit optic andthin film collimator optic to be mounted inaligned positions simultaneously. The detectoris mounted on a double pinned bracket thatallows it to be moved from behind one optic tothe other. This design feature allows it toswitch to optical configurations in less thanfive minutes without having to re-align theinstrument. In addition, this solid-statedetector produces superior quality XRDpattern in both para-focusing and parallelbeam optics. There is no compromise inresolution or quality of XRD data whenparabolic mirrors are employed.
Figure 2: Two measurements of iron powdershowing the effect of sample fluorescencesuppression and Kβ removal with Peltierdetector. All peaks have the same net intensity.
Figure 1: Crosssection of thesealed head of thePeltier detector
The unique design of the Peltier detector isabsolutely maintenance free and has a longterm stability guarantee
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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 monochromator
Speed of acquisition with the ARL X’TRA ona Zeolite 4A sample: In green, the datameasured in less than 5 minutes and in red,the data measured in 20 minutes 0
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WinXRD 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 grazing
incidence)• And finally ω rocking scans.
Data analysis software includes variousanalytical features like:• Basic data treatment (background
substraction, smoothing, peak extraction,profile fitting, etc.)
• Search-match routine using the ICDD oruser database
• Quantitative Phase Analysis• Crystallite size determination• Crystallographic analysis (indexing and
unit cell refinement) • 2D and 3D graphic display for
multiple graphs• Texture analysis with 2D and 3D
polefigure display
Advanced third party software allowmore specific data analysis like:• SIROQUANT for routine minerals
quantification 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 measurements
with the multi-position sample changer• Texture analysis in transmission mode
with the transmission stage• Non-ambient experiments from low
temperature 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 re-alignment. 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: divergent
slits, 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: anti-scatter slits, soller slits, receiving slits,thin film collimator, monochromators
• Detectors: Peltier cooled solid-statedetector or Scintillation detector
Figure 1: Schema of the geometry of the theta:theta goniometer
Peak position extraction by profile fitting, an example ofRanitidine analysis
Phase identification by the search-match method using theICDD database
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1. High temperature chamber with samplespinner (Anton Paar HTK 1200)
2. Parabolic mirror and thin film collimator3. Capillary stage for small and/or
reactive samples 4. 12 position sample changer for
automated batch processing5. Pinhole collimator for point focus for
small samples
6. High temperature chamber for thermal property analysis (Anton Paar HTK 16/20)
7. Environmental chamber for reactivesamples analysis
8. High/Low temperature chamber withliquid nitrogen Dewar (Anton Paar TTK 450)
9. Pressure and temperature reactor chamber with sample spinner (Anton Paar XRK 900)
Temperature transition diagram of TiO2 polymorphicphases: Anatase and Rutile
3D Polefigure of an NBT film
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Technical specifications for the ARL X’TRA
Electrical requirements Single phase 200-250V, 32A, 50-60 HzShipping weight 600 kilograms, including packaging.Water requirements 4.0 liters per minute, 4 - 6 bars, 16°-24° CTemperature: 18º to 32º CFilter Five-micron filter system is recommended to remove particles from water supply.
Dimensions of the instrument(Red: dimensions for shipment)
1154 mm
1956
mm
825 mm
1483
mm
1220 mm986 mm
BR41188_E 07/07C
©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. and its subsidiaries.
Specifications, terms and pricing are subject to change.Not all products are available in all countries. Pleaseconsult your local sales representative for details.
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engineers who are experts in laboratory technologies and applications. Put our team
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and technical support, to complete asset management and regulatory compliance
consulting. Improve your productivity and lower the cost of instrument ownership
through our product support services. Maximize uptime while eliminating the
uncontrollable cost of unplanned maintenance and repairs. When it’s time to
enhance your system, we also offer certified parts and a range of accessories and
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visit us at www.thermo.com.
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