Edme H. Hardy - KIT...Edme H. Hardy 2 2.11.2009 Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical...

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KIT – University of the State of Baden-Wuerttemberg and National Laboratory of the Helmholtz Association Institute for Mechanical Process Engineering and Mechanics www.kit.edu m = ½ m = -½ ħ ω = ΔE = ħ γB 0 B o E m 0 ΔE up down NMR and MRI in Chemical and Process Engineering Edme H. Hardy

Transcript of Edme H. Hardy - KIT...Edme H. Hardy 2 2.11.2009 Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical...

  • KIT – University of the State of Baden-Wuerttemberg and National Laboratory of the Helmholtz Association

    Institute for Mechanical Process Engineering and Mechanics

    www.kit.edu

    m = ½

    m = -½

    ħ ω = ΔE = ħ γB0

    BoEm

    0 ΔE

    up

    down

    NMR and MRI in Chemical and Process EngineeringEdme H. Hardy

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics2 2.11.2009

    Contents

    1 Basics of NMR and MRI2 Examples of in situ applications3 Requirements, limitations4 Compact, mobile systems5 Contact

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics3 2.11.2009

    1 Basics of NMR and MRI

    For dN NMR-active nuclei in a volume dV in an external flux density B a nuclear magnetization M is observed in thermal equilibrium.

    The nuclear magnetization is proportional to the density of nuclear spin I:

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics4 2.11.2009

    1 Basics of NMR and MRI

    In an external field B the magnetization experiences a torque density T:

    The torque density results in a change of density of spin:

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics5 2.11.2009

    1 Basics of NMR and MRI

    These three relations lead to the classical equations of motion:

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics6 2.11.2009

    1 Basics of NMR and MRI

    NMR, MRI: manipulation of magnetization dynamics via B(r, t)Sample: NMR-relevant parameter vector

    and associated distribution („spin density“)

    NMR signal and sample properties: integral transform

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics7 2.11.2009

    2 Examples of in situ applications

    Solid-liquid separationDust separation Microwave heating and dryingTrickle bed

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics8 2.11.2009

    2 Examples of in situ applications

    Solid-liquid separation

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics9 2.11.2009

    2 Examples of in situ applications

    Solid-liquid separation

    Filter-cake buildup, SimulationFilter-cake buildup, MRI

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics10 2.11.2009

    2 Examples of in situ applications

    Dust separation

    Structure of fibrous filter(MRI, detail, 30 µm resolution)

    Oil-filled microcapsules as test particles,6 µm diameter (SEM)

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics11 2.11.2009

    2 Examples of in situ applications

    Dust separation

    Dust-loading profile after 2 hours Dust-loading profile after 8.5 hours

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics12 2.11.2009

    2 Examples of in situ applications

    Microwave heating and drying

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics13 2.11.2009

    2 Examples of in situ applications

    Microwave heating and drying

    Simulation

    Messung

    x / mm y / mm

    z / m

    m

    x / mm y / mm

    Simulation

    Experiment

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics14 2.11.2009

    2 Examples of in situ applications

    Trickle bed

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics15 2.11.2009

    2 Examples of in situ applications

    Trickle bed

    Structure for Spheres and Trilobes Radial Porosity Profiles

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics16 2.11.2009

    2 Examples of in situ applications

    Trickle bed

    Velocity field (mm/s) for one-phase liquid flow through a ceramic sponge

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics17 2.11.2009

    2 Examples of in situ applications

    Trickle bed

    Identification of individual particles Differentiation of catalyst and supportvia NMR-Relaxation

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics18 2.11.2009

    3 Requirements, limitations

    NMR-active nuclei (1H, 19F, 31P, …)Transparency for radio waves (not optical waves)No electrically conducting material within the measuring zoneNo ferromagnetic devices near a superconducting magnetSample must fit into the magnet (KIT: ~ 5 to 65 mm)Tomography is difficult for dry, solid samples

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics19 2.11.2009

    3 Requirements, limitations

    Spatial resolution: typically up to 256x256x256 sampling pointsTemporal resolution: ~second to hoursVelocity range: ~mm/s to cm/sTemperature resolution: ~K

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics20 2.11.2009

    4 Compact, mobile systems

    Ferromagnetic devices permitted close to the permanent magnetNMR apparatus can be brought to the samplePossibilities for single-sided and inside-out NMR

    NMR-based Capillary RheometryRheo-TD-NMRMoisture ProfilesMedium ResolutionDroplets Size DistributionSFC, Oil and Water Content, Spin finish, H content,…

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics21 2.11.2009

    4 Compact, mobile systems

    NMR-based Capillary Rheometry: in situ Velocimetry

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics22 2.11.2009

    4 Compact, mobile systems

    NMR-based Capillary Rheometry: in situ Velocimetry

    Velocity Probability Density FunctionOlive Oil (∇) and Mayonnaise (◊)

    Viscosity Function (Olive Oil,Mayo., PVP Solution, Dispersion)

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics23 2.11.2009

    4 Compact, mobile systems

    Rheo-TD-NMR

    T p ω

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics24 2.11.2009

    4 Compact, mobile systems

    Moisture Profiles

    Test sample

    Experiment

  • Dr. E. H. Hardy, Lv-Nr: 22954 Inst. f. Mechanical Process Engineering and Mechanics25 2.11.2009

    5 Contact

    Spokesperson tomography group:Prof. R. Reimert, CIW-VT, EBI-GEK, KIT CSLocal contact tomography laboratory:Dr. G. Guthausen, CIW-VT, IMVM, SRG 10-2, KIT CSLow-field NMR Medium Resolution and Droplets-Size Distribution: Dr. G. GuthausenLow-field NMR-based Capillary Rheometry, Rheo-TD NMR and Imaging: Dr. E. H. Hardy, CIW-VT, IMVM, KIT CS

    Thanks to D. Mertens, R. Reimert, H. Nirschl, H. Buggisch, DFG, SRG 10-2 C2F Excellence Initiative