INFLUENCE OF SAMPLE SURFACE PREPARATION ON TIR ...
Transcript of INFLUENCE OF SAMPLE SURFACE PREPARATION ON TIR ...
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INFLUENCE OF SAMPLE SURFACE PREPARATION ON TIR SPECTROSCOPY RESULTS
CHRIS HECKER, EVELIEN ROST, FREEK VAN DER MEERMARTIN SCHODLOK, BGR
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LABORATORY TIR SPECTROSCOPY
Directional – hemispherical reflectance measurementsBruker Vertex 70 and integrating sphere
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THE ISSUE
TIR spectra influenced by e.g.: grain size, packing density, solid solution, crystallographic
orientation, surface roughness, exsolution …
Curse and a blessing Changes results but also contains additional information
Some issues intuitively known but not well characterized e.g. roughness, orientation (work in progress)
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WHY NOW?
Mineral spectroscopy from point measurement to image
Issues always there but now more visible
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PHD TOPIC EVELIEN
Determine (and correct) effects of: surface preparation Split Cut Grind Polish
Orientation of crystal axes Possibly pyroxenes, plag feldspars?..
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PHD TOPIC EVELIEN
Determine (and correct) effects of: surface preparation Split Cut Grind Polish
Orientation of crystal axes Possibly pyroxenes, plag feldspars?..
On “simple” rock samples
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ROCK SAMPLES - CONDITIONS
Simple modal mineralogy Spatially homogeneous (@3 cm sample spot) Uniform mineral size (non-porphyritic) LWIR active mineralogy 20x20x20 cm minimal => enough for several tests
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ROCK SAMPLESGildehaus SStFontainebleau SSt Shanxi gabbro
Fine grained• Quartz• 6% porosity
Medium grained• Quartz• Kaolinite• ~20% porosity
Fine grained• Feldspar, pyroxene• intergranular
• Quartz, cummingtonite, hornblende
• No porosity except microcracks.
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METHODS – ROUGHNESS
Surface roughness differences:
Split, Saw, Polish (grit of 4000)
washed, compressed air, oven dried @50°C for ~8 h.
Cooling in desiccator for ~12h
Used same surface of block, <20cm distance => avoid even unlikely anisotropy / inhomogen.
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METHODS – SPECTRAL MEASUREMENTS
Bruker Vertex70 FTIR with DHR integrating sphere Measured range: 5000 – 500 cm-1
Spectral resolution: 4 cm-1
3 scans/sample surface
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PRELIMINARY RESULTS - GABBRO
General shape is same Amplitude of signal
changes: Splitting: darkest Sawing: brighter Polished: brightest
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PRELIMINARY RESULTS - GABBRO
Normalized from 0.0 to 1.0 Shape not exactly the
same Some of the shoulders
(e.g. [email protected]) are lower/higher, resp.
Relative peak heights slightly change
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PRELIMINARY RESULTS – GILDEHAUS SST
Amplitude of signal changes: Splitting: darkest Sawing: brighter Polished: brightest
Shape of 8.2micron quartz lobe changes
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PRELIMINARY RESULTS – GILDEHAUS SST
Normalized from 0.0 to 1.0 Shape of 8.2 feature
clearly different But not on second lobe
(asymmetric)
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PRELIMINARY RESULTS – FONTAINEBLEAU SST
Inverse to Gildehaus: Splitting now brighter
than sawing Lobe shape of splitting
now sloping down to left (Polished not measured
yet)
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INTERPRETATIONS
Explanations through traditional dispersion theory? (refractive index and ext coeff for ord and extord ray)
Differences in two sandstones: Porosity Cementation (Kaol vs ?amorphous quartz phase)
Instrument effects? Preferred reflection (polarization) on polished surfaces? Different results for polarized/specular light even with integr. sphere?
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NEXT STEPS
Characterize the sample composition better (XRD, ?micro-XRF)
Characterize the sample surface better Morphology scanner Electron microscopy
See which parts can be explained by dispersion theory
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INFLUENCE OF SAMPLE SURFACE PREPARATION ON TIR SPECTROSCOPY RESULTS
CHRIS HECKER, EVELIEN ROST, FREEK VAN DER MEERMARTIN SCHODLOK, BGR