X-RAY ABSORPTION SPECTROSCOPY
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1 II Workshop Integra: Desafios da Gestão de Recursos Hídricos X-RAY ABSORPTION SPECTROSCOPY Principles and Environmental Applications Thiago A. Formentini, Dr. Curitiba, Dez 2016
2 2 Outline Brainstorm: Application What s Next? XAS Principles
3 3 How X-rays are absorbed by an atom at energies near and above the core-level energies Variation of the x-ray absorption coefficient as a function of the energy 1s2 2s2 2p6 3s2 3p6 3d6 4s2 All atoms have core-level electrons with different binding energies parts per million level ideal for investigating contamination in the environment
4 4 X-ray absorption near edge structure Extended X-ray absorption fine structure Depends on: Oxidation state (XANES) Distances, coordination number and species of the atoms immediately surrounding the selected element (EXAFS)
5 5
6 6 XANES X-ray Absorption Near Edge Structure Valence of the absorber Qualitative structural information Interpreted often by simulation
7 7
8 Extended X-ray Absorption Fine Structure X-RAY ABSORPTION EXAFS 8 Detailed information about the local atomic structure Analyzed by curve fitting Weighted Fingerprint Fourier Transform isolate and identify different coordination spheres around the absorbing atom
9 9 X-rays Energy: 0.5 kev to 500 kev WL: 25 to 0.25 Å 12.4 kev = 1 Å HIGHLY intense and energy-tunable source of x-rays: synchrotrons ESRF - Grenoble 844 m - 6 GeV LNLS - Campinas 93 m GeV Sirius 520 m - 3 GeV
10 10 Linear acelerator (LINAC): high voltage power supply Intermediate synchrotron Synchrotron: magnetic field to turn the particles in the circle electric field to accelerate the particles Optics Hutch Experimental Hutch Control Cabin Beamlines
11 ESRF - Grenoble X-RAY ABSORPTION 11
12 12 47 synchrotron radiation research facilities in 23 countries (lightsources.org)
13 Radical change of Zn speciation in pig slurry amended soil: key role of nano-sized sulfide particles 13 TA Formentini, S Legros, CVS Fernandes, A Pinheiro, M Le Bars, C Levard, FJK Mallmann, M Veiga, E Doelsch
14 Radical change of Zn speciation in pig slurry amended soil: key role of nano-sized sulfide particles 14
15 Radical change of Zn speciation in pig slurry amended soil: key role of nano-sized sulfide particles 15
16 Radical change of Zn speciation in pig slurry amended soil: key role of nano-sized sulfide particles 16
17 Radical change of Zn speciation in pig slurry amended soil: key role of nano-sized sulfide particles 17
18 Radical change of Zn speciation in pig slurry amended soil: key role of nano-sized sulfide particles 18
19 Radical change of Zn speciation in pig slurry amended soil: key role of nano-sized sulfide particles 19 ZnS made up 100% of the Zn speciation in the pig slurry (the highest proportion of ZnS ever observed in organic waste) ZnS aggregates were about 1-μm diameter (the smallest particle size ever reported in pig slurry) Zn in the pig slurry consisted of nano-sized ZnS crystallites that further aggregated The low stability of ZnS nanoparticles in oxic and complex environments such as the studied soil was the key explanation for the radical change in pig slurry-borne Zn speciation after long-term amendments
20 Slurry, Manure, Sludge, etc... X-RAY ABSORPTION 20 N P Cu Zn, others Groundwater Contaminant plume Groundwater wells Poisoning? Spread of disease? Streams Drinking water Recreation Biotic communities Toxicity? Soil accumulation Phytotoxicity? Plant uptake? Food chain? Fate, behavior, bioavailability, toxicity (where? how?)
21 Slurry, Manure, Sludge, etc... X-RAY ABSORPTION 21 N P Cu Zn, others SEASONAL (Precipitation, temperature) TYPE OF SOIL (Sandy, clayey) EFFLUENT (Manure, sewage, sludge)
22 Slurry, Manure, Sludge, etc... X-RAY ABSORPTION 22 N P Cu Zn, others Characterization Integrated monitoring Integrated modeling Desafio da Gestão de Recursos Hídricos
23 23 #FORATEMER
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