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The XRF method: Development and Applications. Ch. Zarkadas and A.G. Karydas N.C.S.R. “Demokritos”, Institute of Nuclear Physics, Aghia Paraskevi, 15310, Athens Greece. Workshop PET/SPECT/RADIO-ISOTOPES in Greece. 26 June 2006. Outline. The X-ray Fluorescence technique.
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The XRF method: Development and Applications Ch. Zarkadas and A.G. Karydas N.C.S.R. “Demokritos”, Institute of Nuclear Physics, Aghia Paraskevi, 15310, Athens Greece Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Outline • The X-ray Fluorescence technique • State of the art instrumentation • XRF facilities at the I.N.P of “Demokritos” • Applications • Conclusions Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
E0 Ka Physics of the XRF technique L Κ M Nucleus Electrons Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
A typical ΧRF setup Substrate Sample Source X-rays Detector Preamp Computer Amp ADC MCA Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Digital Electronics X-ray Optics X-ray Detectors X-ray Tubes Polycapillary lenses LN cooled Si(Li) Rotating anode (18kW) High power (3kW) HOPG crystals Thermoelectrically cooled SDD, Si-PIN Low power (50W) State of the art instrumentation • Provide/Enable: • Intense exciting X-ray beams • Energy resolution down to 135 eV • High count rate handling capabilities (106 cps!!!!) • Low Z detection (B,C,O,N) • Formation of focused intense beams – microbeams (10μm-100μm) • In depth analysis combining two polycapillaries (3D confocal XRF) Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Detector guide Sample Filters Shutter Crystal Secondary target Be window XRF instruments at the I.N.P STXRF (Secondary Target XRF) • Provides: • Selectable almost monochromatic excitation • Polarized doubly scattered continuum Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
XRF instruments at the I.N.P TXRF (Total Reflection XRF) Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
The demokritos portable milli beam XRF spectrometer • Features: • Rh, side window, 50W, air cooled tube, 75μm Be window • PIN diode detector, FWHM = 165 eV MnKα, 500 μm thickness • Electromagnetic beam shutter • Rotatable filter wheel • Lasers for sample positioning • Collimating parts, Beam spot • ~ 3mm at sample position • Control unit Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Handheld XRF spectrometer (under design) Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
The demokritos μXRF spectrometer X-Y-Z stage 10μm steps 30W, Rh anode μfocus (50μm x 50μm) X-ray tube Camera 10mm2SDD Polycapillary lens 41MLS03 Focal spot 60-80 μm Optimized for higher energies Output focal distance 21.2 mm Minimum Halo effect He filled Polycapillary lens Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Biomedical Applications (I) Determination of Trace Elements in Human Blood serum MDL’s: 12 ppb Yttrium secondary target excitation Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Biomedical Applications (II) Determination of cis-Pt in mice Blood Yttrium secondary target excitation Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Biomedical Applications (III) Determination of Uranium in urine 5 ppb U MDL’s: 250 ppt Total reflection + chemical treatment Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Environmental Applications (I) Determination of Trace Elements in potable water Bottled water Tap water MDL’s: 6 ppb Total reflection, direct measurement Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Environmental Applications (II) Determination of Trace Elements in airborne particulates The case of “Sahara rain” Mo secondary target excitation Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Organic Orpiment Ochre Celadonite Jarosite Sulfur Flower Egyptian Blue Organic Black Ochre Celadonite Ochre Orpiment (As2S3) Ochre Ochre Sulfur Orpiment Egyptian Blue (CuCaSi4O10) Cultural Heritage Applications (I) Determination of pigments on marble statues Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Linear scan in a paint layer section 10-15 μm cinnabar 20-30 μm red ochre Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Linear scan in a paint layer section 10-15 μm Egyptian Blue 100-140 μm Black 30-50 μm Kaolinite 10-20 μm Cinnabar Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Cultural Heritage Applications (II) Chemical discrimination of gold alloys 34 gold jewels Benaki Museum Rh direct excitation Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
μXRF spectrum of a tin-lead Copper alloy Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006
Summary - Conclusions - Perspectives • X-ray Fluorescence is nowadays a dynamic and well established technique for quantitative and/or qualitative analysis (non destructive if necessary) • Offers multielemental and sensitive analysis in a wide variety of different samples in the interdisciplinary field • A new generation of XRF spectrometers is currently available at Demokritos • In depth analysis has been already achieved (3D confocal setups) and will be the trend in the near future Workshop PET/SPECT/RADIO-ISOTOPES in Greece 26 June 2006