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U of U PHYS 5739 - Eagle III — Micro-EDXRF System

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Slide 1Eagle System SchematicXRF AdvantagesAdvantages to EDS (Matt’s addition)Non-Destructive Testing“As Delivered” Sample AnalysisHigh SensitivitySlide 8Configuration — Standard Eagle IIIConfiguration — Eagle III - OPTIONSSample Illumination: White LEDsColor Low-Magnification Image (single)Color Low-Magnification Image (montage)Hi-Magnification Image - Montage 5×5Hi-Magnification Image - Montage 3×3Hi-Magnification Image (Single) + Digital ZoomTransmission Sample BacklightingSlide 18Si(Li) Detector propertiesDetector’s relative low energy performancesSi(Li) CoolingCapillary X-ray OpticsIncident X-Ray Spectral Distribution (Modified Excitation Spectrum)Multilevel Sample AnalysisFilter BenefitsExample: Ni FilterExample: Ni Filter – Improve Limits of Detection“Vision” Software: Modes of Operation“Vision” Software: Applications“Vision” Software: Applications (cont’d)Manual Control and AnalysisAutomated Multiple Point AnalysesAutomated Multi-Point Analysis:Foreign Particulates in SilicaFP “Standardless” Analysis: Particle 1FP “Standardless” Analysis: AccuracySlide 38Slide 39Slide 40Multi-Point Analysis: Chemical DistributionSpectral Mapping DefinitionSpectral Mapping: Search and Use of DataSpectral Mapping:Elemental Spatial Distribution Maps: PaperSpatial Distribution Maps: Facial TissueSlide 47Slide 48Quantitative Mapping: Geological SampleSlide 50Slide 51Multi-Field Mapping: Geological SampleSpectral Mapping - Bone FossilizationMap Image Overlays: Bone FossilizationMetal Analysis: Coins (Non-Destructive)Eagle ApplicationsEagle III — Micro-EDXRF SystemEagle System SchematicEagle System SchematicXRF AdvantagesXRF AdvantagesNon-destructive: No beam damage or coating of sampleMinimal Sample Preparation:•conductivity not required•sample shape can be irregularLow Vacuum (~ 100 mTorr) or No Vacuum (Air)Navigation by Optical MicroscopeDetection limits improve: 10x or better (vs. SEM-EDS)X-rays are penetrating (microns to millimeters)Advantages to EDS (Matt’s addition)Advantages to EDS (Matt’s addition)Cheaper to add EDS to a microscope than to buy an XRF systemOrders of magnitude better image quality•CCD camera in XRF has magnification of 150 – 200X•Resolution comparable to XRF: about 10 nm•SEM image quality can be orders of magnitude betterSmaller analytical volume•One order of magnitude always•Another order of magnitude if you can live with lower voltageNon-Destructive TestingNon-Destructive Testing10x Eagle Video (B/W)100x Eagle Video (color)Small Fracture in Diamond Table? Glass-Filled ?Small Fracture in Diamond Table? Glass-Filled ?* Rh Tube* Aperture/Rh filterConclusion: Yes!Conclusion: Yes!“As Delivered” Sample Analysis“As Delivered” Sample AnalysisChemical Residues from suspected drug labX-ray Excitation minimizes sample preparationQualitative answer in < 2 minutesHigh SensitivityHigh SensitivityReduced backgroundEagle System SchematicEagle System SchematicStandard features•Rh or Mo tube (40kV, 40W)•300µm monocapillary•Video: 10× colour; 100× colour (plus 2× digital zoom)•Sapphire™ 80 mm2 Si(Li) detector•Genesis 2000 (Windows XP)•Vision32 version 4 software (patented FP and Comb32)Configuration — Standard Eagle IIIConfiguration — Standard Eagle IIIConfiguration — Eagle III - OPTIONSConfiguration — Eagle III - OPTIONSOptions•100µm monocapillary in lieu of the 300µm•collimators (1 & 2mm)•manually interchangeable filters (for collimator only)•40kV, 20W Cr-anode X-ray tube•50 kV, 50W X-ray tube (Mo, Rh or W anodes)•30 mm2 Si(Li) detector•rotation table OR sample backlighting•LineScan, Mapping & Image processing softwareSample Illumination: White LEDsSample Illumination: White LEDsDirectionally adjustable LED arraysIndividual arrays for both Low- & High-mag image viewsIndividual light output adjustment to both arrays at both magnification viewsLow-magHigh-mag$20 banknote (US)Color Low-Magnification Image (single)Color Low-Magnification Image (single)$20 banknote (US)Color Low-Magnification Image (montage)Color Low-Magnification Image (montage)Hi-Magnification Image - Montage 5×5Hi-Magnification Image - Montage 5×5Hi-Magnification Image - Montage 3×3Hi-Magnification Image - Montage 3×3Hi-Magnification Image (Single) + Digital ZoomHi-Magnification Image (Single) + Digital ZoomNormal (100×) Digital Zoom (2× “normal”)Blue security-fibre in banknoteTransmission Sample BacklightingTransmission Sample BacklightingReflective lightingTransmission lightingFine “Hi-Purity” Silica particlesTransmission Sample BacklightingTransmission Sample BacklightingTransmission lighting (Low Mag View)Transmission lighting (High Mag View)Si(Li) Detector propertiesSi(Li) Detector propertiesActive area(mm2)Be(coated)windowProcessing TC(µsec)Countrate(cps)Resolution @MnKa (eV)30nominal8µm35 5000 ≤14510 15000 ≤16580nominal12µm35 5000 ≤15510 15000 ≤185100,000cps processing capabilityAbsolute intensities: I30 ≈ I80× 55%30mm280mm2NaK MgK AlK SiK500 700 900 1100 1300 1500 1700 1900 (eV)Glass sample (srm620)Spectra normalised to CaK (3690eV)Detector’s relative low energy performancesDetector’s relative low energy performancesSi(Li) CoolingSi(Li) CoolingStandard: Liquid Nitrogen•30 mm2 or 80 mm2•5 L dewar•≥ 3 day hold time•Detector can be allowed to warm when not in use. Detector High Voltage bias is switched off when detector warms.Capillary X-ray OpticsCapillary X-ray Optics“Total” Reflection of X-rays inside glass capillaryc = f(1/E)Incident X-Ray Spectral Distribution(Modified Excitation Spectrum)Incident X-Ray Spectral Distribution(Modified Excitation Spectrum)Multilevel Sample AnalysisMultilevel Sample AnalysisFilter BenefitsFilter BenefitsImprove Limits of DetectionMake analysis possibleRemove Tube Characteristic LinesReduce Bremsstrahlung in limited regionEliminate Bragg Diffraction Peaks in limited regionThis is accomplished by …Example: Ni FilterExample: Ni FilterHigh Sensitivity RegionUseful RegionNi Absorption EdgeFilter Band PassExample: Ni Filter – Improve Limits of Detection Example: Ni Filter – Improve Limits of Detection“Vision” Software: Modes of Operation “Vision” Software: Modes of Operation Manual point to pointAutomated multiple point, lines or matricesAnalyze within an area and add spectra togetherLine Scan (generates a


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U of U PHYS 5739 - Eagle III — Micro-EDXRF System

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