Concept differences in WD-XRF goniometer systems
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1 X-Ray Conference Norway 14 september 2010 Concept differences in WD-XRF goniometer systems Didier Bonvin & Renaat Van Geel Thermo Fisher Scientific, Ecublens, Switzerland Renaat Van Geel SID Commercial Marketing Manager BEA EMEA
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8 GOLDD Technology Thermo Scientific is introducing the new Niton XL3t XRF Analyzer with GOLDD Technology This new analyzer delivers Light element detection (Mg, Al, Si, P, S) without helium or vacuum purging The lowest limits of detection and the fastest analysis available True lab-quality performance in a handheld instrument (Geometrically Optimized Large Area Drift Detector) 8
9 UCCO: Ultra Closely Coupled Optics for WD 50W 9
10 Thermo Scientific ARL 9900 Total Cement Analyzer Coal (Ash) Hot meal degree of calcination Clinker (Free Lime, C 3 S + Other Clinker phases) Environmental (Heavy metals in dust) Raw Materials + others (Limestone, Clay, Iron Ore etc. + Bypass samples) Raw Meal (LSF, SM, AM) Additives (Slags, Fly Ash, Limestone, etc.) Cement 10
11 Detection limits and dynamic range element analysis Solids Liquids ICP-MS GFAAS ICP-0ES AAS XRF TOC; TN / TS / TX 1 ppq 1 ppt 1 ppb 1 ppm 1,000 ppm 100% TRACE BULK 11
12 Intensity (kcps) Intensity (kcps) XRF, ED or WD, that s the question Cu and Zn peaks on WDXRF instrument Cu and Zn peaks on EDXRF instrument Cu k Zn k Cu k Zn k Cu k Zn k Cu k Zn k Energy (kev) Energy (kev) WDX has 10 times better resolution compared to EDX 8 to 10 times higher count rates 12
13 Wavelength Dispersive X-ray Fluorescence (WDXRF) Multi-element technique for solids, liquids, loose powders, etc. Up to 84 elements of the periodic table (from Be to U) H He Li Be B C N O F Ne Na Mg Al Si P S Cl Ar K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe Cs Ba La Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn Fr Ra Ac Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lw Standard elements Ultra light elements require synthetic multilayer crystals Not measurable Unstable elements Rare gases 13
14 Role of the Goniometer at WD-XRF Ensures the accurate angular positioning of crystal and detectors Must meet Bragg s law l 14
15 Role of the Goniometer at WD-XRF Accurate angular positioning of crystal (1 theta) and detector (2 theta) precision retained over lifetime of the instrument 15
16 Role of the goniometer at WD-XRF 16 FEATURE Sensitivity Resolution K Spectra Elements Be B C N O -F -Na Mg Al Si P -S -Cl K Ca...Ti Fe Choice L Spectra of various crystals depending on required elements Sn...Yb and COLLIMAT. applications X-Coarse 2.6 V.High Low Coarse 0.6 High Fair FEATURE Medium 0.25 Sensitivity Good Resolution Good Elements K Fine Spectra 0.15 Low High Be B C N O -F -Na Mg Al Si P -S -Cl K Ca...Ti Fe L CRYSTAL Spectra Sn...Yb COLLIMAT. AXBeB High Low Be X-Coarse AX V.High Good Low B Coarse AX High Fair Low C Medium AX Good Good Low N Fine AX Low High High Low O CRYSTAL AX03 AXBeB TlAP Good High Good Good Low Good Be O O AX20 ADP Good Low Low High B Mg AX16 PET High Good Low Fair C Al AX09 InSb Good High Low High N Si AX06 Ge111 High Good Low High O P AX03 LiF 200 Good Good Good Good O K LiF 220 Fair High TlAP Good Good O LiF420 Low V.High ADP Low High Mg DETECTOR PET Good Fair Al FPC InSb High High Si Scintillation Ti Co...Zn Sn Hf...U Co...Zn Sn Hf...U Zn
17 Universal Goniometer Electro-optical angular positioning High precision of positioning Direct drive No wear with usage Up to 9 crystals Up to 4 collimators Two detectors Standard elemental coverage Fluorine to uranium With appropriate crystals Extension for beryllium to oxygen 17
18 Universal Goniometer Capability for Four Programmable Collimators Choice of collimators in order to optimize resolution or sensitivity Standard collimators : Medium : 0.25 divergence Coarse : 0.6 divergence Optional collimators : Fine : 0.15 divergence Extra-coarse : 2.5 divergence Front view of the goniometer with its four collimator changer 18
19 Collimator divergence Divergence of collimators depends on blade spacing and length of collimator Therefore should always be expressed as degrees of divergence and not as millimeters of spacing Φ 1 Φ 2 19
20 Influence of collimator on resolution Interference of Cr Ka on Mn Ka is best resolved with fine collimator: Coarse collimator should not be used for Mn analysis 20
21 Influence of collimator on intensity Scan on coarse and extra-coarse collimator on Nitrogen peak 21
22 Other influences on the performance The geometry of rotation of the goniometer can also have an influence on the XRF intensities obtained Goniometer rotation perpendicular to X-ray tube Goniometer rotation in same plane as X-ray tube 22
23 Optically driven, gearless SmartGonio Goniometer rotation in the same plane as the X-ray tube 3 crystals 2 detectors Fluorine to Uranium Crystals Collimator Detectors 23
24 Scan comparison of two geometries: Ba ka1,2 K line of heavy element short wavelength: 0.038nm Same crystal-detector combination: LiF200-Scintillation counter Small difference of collimators
25 Scan comparison of two geometries: Cu Ka1,2 K line of medium element: nm Same crystal-detector combination: LiF200-Scintillation counter Small difference of collimators
26 Scan comparison of two geometries: Ba La1,2 L line of heavy element - medium wavelength: nm Same crystal-detector combination: LiF200-Flow proportional counter Small difference of collimators
27 Scan comparison of two geometries: Al ka1,2 Light element - long wavelength: nm Same crystal-detector combination: PET-Flow proportional counter Small difference of collimators
28 SmartGonio vs. Universal Gonio: Sensitivity in Fe base 3600W medium collimator Better sensitivity with SmartGonio from all elements Much higher sensitivity at shorter wavelength (Nb to Sb) Sensitivity comparison SmartGonio vs Universal Gonio (Fe base) Cps/% for SmartGonio Cps/% with Universal Gonio Sensitivity (cps/%) Al Si P S Ca Ti V Cr Mn Co Ni Cu As Zr Nb Mo Sn Sb W Pb GonioF45 SmartGonio 28
29 Limit of detection (ppm) at 50kV-72mA SmartGonio vs. Universal Gonio: Limits of Detection in Fe base 3600W Better LoD with universal goniometer for lighter elements (Al to Ca) thanks to lower background Better LoD with SmartGonio for heavier elements from Cr due to better sensitivity LoD comparison Fe base - 20s counting time - medium collimator LoD with SmartGonio LoD with Universal Gonio Al Si P S Ca Ti V Cr Mn Co Ni Cu As Zr Nb Mo Sn Sb W Pb 29 GonioF45 SmartGonio
30 Make your choice depending on your applications Sample Changer Goniometer High Voltage Generator ARL ADVANT X Series - Side View with universal goniometer 30
31 Make your choice depending on your applications Sample Changer Goniometer High Voltage Generator ARL ADVANT X Series - Side View with SmartGonio 31
32 32 When you need the best of both worlds
33 Dual Goniometer configuration within the same instrument Cross Section of ARL 9900 Dual Goniometer version Vacuum Tank SmartGonio X-ray Tube Sample in Analysis Position Sample Changer Molecular Pump Rotary Vacuum Pump Electroni c Module Generator Water Cooling + Heat Exchange r 33
34 Dual Goniometer configuration within the same instrument XRF Universal Goniometer Sequential analysis X-Ray Tube XRF SmartGonio Sequential analysis XRF Fixed channels Fixed channels Elemental Fixed channels Elemental analysis analysis Elemental Information on analysis the elements in analysis the sample Sample 34
35 35 Flexible instrument for multiple applications
36 Thank you for your attention To keep informed on XRF products, visit our landing page;
B I N G O B I N G O. Hf Cd Na Nb Lr. I Fl Fr Mo Si. Ho Bi Ce Eu Ac. Md Co P Pa Tc. Uut Rh K N. Sb At Md H. Bh Cm H Bi Es. Mo Uus Lu P F.
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