Spectroscopic and Microscopic Characterization of Oil Spectroscopic and Microscopic Characterization

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  • Spectroscopic and Microscopic Characterization of Oil Shale

    Tracy Elizabeth McEvoy1, Michael Batzle1, Jeremy Boak3,5, Earl D. Mattson4, John Scales2,

    George Radziszewski2,3

    1Department of Geophysics, Colorado School of Mines, Golden, Colorado, U.S.A., 2Department of Physics, Colorado School of Mines, Golden, Colorado,

    U.S.A., 3Center for Oil Shale Technology and Research (COSTAR), Golden, Colorado, U.S.A., 4Energy Resource Recovery and Management Department, Idaho National Laboratory, Idaho Falls, Idaho,U.S.A. 5Department of Geology,

    Colorado School of Mines, Golden, Colorado, U.S.A.

  • ● Earl Mattson – Research Scientist, Energy Resource Recovery & Management

    Department, Idaho National Laboratory

    ● George Radziszewski – Research Scientist, Department of Physics, Colorado School of

    Mines

    ● Michael Batzle – Professor, director of Center of Rock Abuse, Department of

    Geophysics, Colorado School of Mines

    ● John Scales – Professor, Department of Physics, Colorado School of Mines

    ● Jeremy Boak – Chair of the Oil Shale Symposium and the Director of the Center for

    Oil Shale Technology and Research (COSTAR) at the Colorado School of Mines

  • Introduction

     Samples

     Methods − Millimeter wave spectroscopy − Scanning acoustic microscopy − Thermal gravimetric analysis − QemScan

  • Sample Conditions

    Prepared by: Earl D. Mattson, Idaho National Laboratory

    Hydropyrolysis Four Stages of Extraction:

    - Control - T = 290°C - T = 310°C - T = 330°C - T = 350°C

  • Sample Conditions II

  • Sample Conditions III

    Control Sample T= 310 °C T =330°C

  • Techniques

    1. Millimeter Wave Spectroscopy

    2. Thermal Gravimetric Analysis

    3. Scanning Acoustic Microscope

  • Millimeter Wave Spectroscopy I

    Scales & Batzle (2006)

    Harmonic Multiplier

    Teflon Probes

    Vector Network Analyzer

    Harmonic Detector

    Harmonic Detector

    MotorMotor Control

    Scalar Horn

    Computer

  • Millimeter Wave Spectroscopy II

    Lens

    Lens

    Scalar Horn

    Sample

    Transmitted Field ET

    Reflected Field ER

    Emitted Field EI

    Standing Waves

    Scalar Horn

  • Millimeter Wave Spectroscopy V Raw Data – Transmitted Phase Angle

    +180 °

    -180 °

    2.7 cm

    Ph as

    e A

    ng le

  • Control T = 310°C T = 330°CSamples : :

    Transmitted Phase Data

    +180 -180°-90°+180° +90° 0° Phase Angle:

  • Dielectric Permittivity Map

    Low High2 4

    Before Hydropyrolysis After Partial Hydropyrolysis

  • Thermal Gravimetric Analysis

    http://www.nd.edu/~pmcginn/IMG_1494.jpg

  • TGA Data Example

    Temperature Increasing

    Sample Weight Decreasing

  • TGA Display Format

    Temperature [°C]

    Organic Material Loss -dTg/dT

  • 1 mm

    Sample A

    Sample B

    Sample C

    X-ray energy dispersive analysis

    ““Qemscan”Qemscan”

  • Layer Locations

    RedRed

    LightLight DarkDark Section Section LocationLocation

  • TGA

    0 100 200 300 400 500 600 700 800 0

    0.5

    1

    1.5

    2

    2.5

    3 TGA Light Layer Comparison

    0 Light 290 Light 330 Light

    T [°C]

    -d Tg

    /d T

  • TGA

    0 100 200 300 400 500 600 700 800 0

    0.5

    1

    1.5

    2

    2.5

    3

    3.5

    TGA Red Layer Comparison

    Red 0 Red 290 Red 330

    T [°C]

    -d Tg

    /d T

  • TGA

    0 100 200 300 400 500 600 700 800 0 1 2 3 4 5 6 7 8

    TGA Dark Layer Comparison

    0 Dark 290 Dark 330 Dark

    Temperature [°C]

    -d Tg

    /d T

  • Scanning Acoustic Microscopy

    Control Sample

    T = 330 ° C

  • Scanning Acoustic Microscopy

    ~1.1mm

    ~1.4mm

    ~1.5mm

    Acoustic Two-Way Travel Times:

    17943 [ns]

    17914 [ns]

    17987 [ns]

    Control Sample

  • Scanning Acoustic Microscopy

    Acoustic Two-Way Travel Times:

    17956[ns]

    17913 [ns]

    17953 [ns]

    Sample T = 330 °C

  • Control T = 310°C T = 330°CSamples : :

    Transmitted Phase Data

    +180 -180°-90°+180° +90° 0° Phase Angle:

  • Dielectric Profile Comparison before T-processed

  • Decreased impedance contrast, scanning acoustic microscope.

    Dielectric constants of organic rich layers in the samples studied were low in comparison to the dielectric constants of the organic poor layers.

    Conclusions

  • Implications

    Dielectric logging can assess the degree of pyrolysis in the lab and in situ.

  • Acknowledgments Millimeter Wave Spectroscopy

    Nathan Greens Engineering Physics Department, CSM

    Scanning Acoustic Microscope Manika Prasad Ph.D.

    Petroleum Engineering Department, CSM

    Thermal-gravimetric Analysis Matthew Liberatore Ph.D.

    Chemical Engineering Department, CSM

  • Acknowledgments

    Marisa Rydzy Department of Geophysics, Colorado School of Mines

    Aaron McEvoy Department of Physics, Los Alamos National Laboratory

  • Dielectric Constant

    

    = 2d 

    ¿ 2¿

    = 2d 

    

    Dielectric Permittivity

    Wave Length

    Sample thickness

    Transmitted Phase Difference

  • Extra Slides: MMW Connections

    Scales & Batzle 2006

  • Extra Slides: MMW

    Gas Hydrate Research at CRA

    Reflected

    Transmitted

    Fabry-Pérot Fit

    Measurements a) Frequency 75-100GHz b) Phase & Amplitude c) MMWref and MMWtrans d) Data fit with Fabry-Pérot

    Model Fabry-Pérot Model: Phase and Amplitude of transmitted and reflected wave depend on the sample thickness and the dielectric permittivity Dielectric Constants at 273 K: Ice 94 GH 58

  • Image Sources

    ●TGA photograph - http://www.nd.edu/~pmcginn/IMG_1494.jpg, University of Notre Dame Department of Chemical Engineering, Last Accessed: Monday, Oct 12, 2009

    http://www.nd.edu/~pmcginn/IMG_1494.jpg

    PowerPoint Presentation Slide 2 Slide 3 Slide 4 Slide 5 Slide 6 Slide 7 Slide 8 Slide 9 Slide 10 Slide 11 Slide 12 Slide 13 Slide 14 TGA Display Format Slide 16 Slide 17 Slide 18 Slide 19 Slide 20 Slide 21 Slide 22 Slide 23 Slide 24 Slide 25 Slide 26 Slide 27 Acknowledgments Slide 29 Slide 30 Slide 31 Slide 32 Slide 33