spectroscopic and microscopic characterization of oil shale · spectroscopic and microscopic...
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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.
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● 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
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Introduction
Samples
Methods− Millimeter wave spectroscopy− Scanning acoustic microscopy− Thermal gravimetric analysis− QemScan
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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
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Sample Conditions II
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Sample Conditions III
Control Sample T= 310 °C T =330°C
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Techniques
1. Millimeter Wave Spectroscopy
2. Thermal Gravimetric Analysis
3. Scanning Acoustic Microscope
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Millimeter Wave Spectroscopy I
Scales & Batzle (2006)
Harmonic Multiplier
Teflon Probes
Vector NetworkAnalyzer
Harmonic Detector
HarmonicDetector
MotorMotor Control
Scalar Horn
Computer
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Millimeter Wave Spectroscopy II
Lens
Lens
Scalar Horn
Sample
Transmitted Field ET
Reflected Field ER
Emitted Field EI
Standing Waves
Scalar Horn
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Millimeter Wave Spectroscopy VRaw Data – Transmitted Phase Angle
+180 °
0°
-180 °
2.7 cm
Phas
e A
ngle
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Control T = 310°C T = 330°CSamples : :
Transmitted Phase Data
+180 -180°-90°+180° +90° 0°PhaseAngle:
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Dielectric Permittivity Map
Low High2 4
Before Hydropyrolysis After Partial Hydropyrolysis
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Thermal Gravimetric Analysis
http://www.nd.edu/~pmcginn/IMG_1494.jpg
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TGA Data Example
Temperature Increasing
Sample Weight Decreasing
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TGA Display Format
Temperature [°C]
Organic Material Loss-dTg/dT
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1 mm
Sample A
Sample B
Sample C
X-ray energy dispersive analysis
““Qemscan”Qemscan”
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Layer Locations
RedRed
LightLightDarkDark Section Section
LocationLocation
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TGA
0 100 200 300 400 500 600 700 8000
0.5
1
1.5
2
2.5
3TGA Light Layer Comparison
0 Light290 Light330 Light
T [°C]
-dTg
/dT
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TGA
0 100 200 300 400 500 600 700 8000
0.5
1
1.5
2
2.5
3
3.5
TGA Red Layer Comparison
Red 0Red 290Red 330
T [°C]
-dTg
/dT
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TGA
0 100 200 300 400 500 600 700 800012345678
TGA Dark Layer Comparison
0 Dark290 Dark330 Dark
Temperature [°C]
-dTg
/dT
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Scanning Acoustic Microscopy
Control Sample
T = 330 ° C
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Scanning Acoustic Microscopy
~1.1mm
~1.4mm
~1.5mm
Acoustic Two-Way Travel Times:
17943 [ns]
17914 [ns]
17987 [ns]
Control Sample
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Scanning Acoustic Microscopy
Acoustic Two-Way Travel Times:
17956[ns]
17913 [ns]
17953 [ns]
Sample T = 330 °C
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Control T = 310°C T = 330°CSamples : :
Transmitted Phase Data
+180 -180°-90°+180° +90° 0°PhaseAngle:
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Dielectric Profile Comparisonbefore T-processed
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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
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Implications
Dielectric logging can assess the degree of pyrolysis in the lab and in situ.
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AcknowledgmentsMillimeter Wave Spectroscopy
Nathan GreensEngineering Physics Department, CSM
Scanning Acoustic MicroscopeManika Prasad Ph.D.
Petroleum Engineering Department, CSM
Thermal-gravimetric AnalysisMatthew Liberatore Ph.D.
Chemical Engineering Department, CSM
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Acknowledgments
Marisa RydzyDepartment of Geophysics, Colorado School of Mines
Aaron McEvoyDepartment of Physics, Los Alamos National Laboratory
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Dielectric Constant
=2d
¿2¿
= 2d
Dielectric Permittivity
Wave Length
Sample thickness
Transmitted Phase Difference
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Extra Slides: MMW Connections
Scales & Batzle 2006
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Extra Slides: MMW
Gas Hydrate Research at CRA
Reflected
Transmitted
Fabry-Pérot Fit
Measurementsa) Frequency 75-100GHz b) Phase & Amplitude c) MMWref and MMWtransd) Data fit with Fabry-Pérot
ModelFabry-Pérot Model: Phase and Amplitude of transmitted and reflected wave depend on the sample thickness and the dielectric permittivityDielectric Constants at 273 K:Ice 94GH 58
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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