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Title: Determination of elemental composition of shale rocks by laser induced breakdown spectroscopy

Laser induced breakdown spectroscopy (LIBS) is used for elemental characterization of outcrop samples from the Marcellus Shale. Powdered samples were pressed to form pellets and used for LIBS analysis. Partial least squares regression (PLS-R) and univariate calibration curves were used for quantification of analytes. The matrix effect is substantially reduced using the partial least squares calibration method. Predicted results with LIBS are compared to ICP-OES results for Si, Al, Ti, Mg, and Ca. As for C, its results are compared to those obtained by a carbon analyzer. Relative errors of the LIBS measurements are in the range of 1.7 to 12.6%. The limits of detection (LODs) obtained for Si, Al, Ti, Mg and Ca are 60.9, 33.0, 15.6, 4.2 and 0.03 ppm, respectively. An LOD of 0.4 wt.% was obtained for carbon. Finally, this study shows that the LIBS method can provide a rapid analysis of shale samples and can potentially benefit depleted gas shale carbon storage research.
Authors:
 [1] ;  [2] ;  [3] ;  [2] ;  [4] ;  [3]
  1. Mississippi State Univ., Mississippi State, MS (United States). Inst. for Clean Energy Technology
  2. National Energy Technology Lab. (NETL), Pittsburgh, PA (United States)
  3. Applied Spectra, Inc., Fremont, CA (United States)
  4. National Energy Technology Lab. (NETL), Morgantown, WV (United States)
Publication Date:
Type:
Accepted Manuscript
Journal Name:
Spectrochimica Acta. Part B, Atomic Spectroscopy
Additional Journal Information:
Journal Volume: 122; Journal ID: ISSN 0584-8547
Publisher:
Elsevier
Research Org:
National Energy Technology Lab. (NETL), Pittsburgh, PA (United States)
Sponsoring Org:
USDOE
Country of Publication:
United States
Language:
English
Subject:
58 GEOSCIENCES; LIBS; shale rock; elemental analysis
OSTI Identifier:
1480827
Alternate Identifier(s):
OSTI ID: 1359838

Sanghapi, Hervé K., Jain, Jinesh, Bol'shakov, Alexander, Lopano, Christina, McIntyre, Dustin, and Russo, Richard. Determination of elemental composition of shale rocks by laser induced breakdown spectroscopy. United States: N. p., Web. doi:10.1016/j.sab.2016.05.011.
Sanghapi, Hervé K., Jain, Jinesh, Bol'shakov, Alexander, Lopano, Christina, McIntyre, Dustin, & Russo, Richard. Determination of elemental composition of shale rocks by laser induced breakdown spectroscopy. United States. doi:10.1016/j.sab.2016.05.011.
Sanghapi, Hervé K., Jain, Jinesh, Bol'shakov, Alexander, Lopano, Christina, McIntyre, Dustin, and Russo, Richard. 2016. "Determination of elemental composition of shale rocks by laser induced breakdown spectroscopy". United States. doi:10.1016/j.sab.2016.05.011. https://www.osti.gov/servlets/purl/1480827.
@article{osti_1480827,
title = {Determination of elemental composition of shale rocks by laser induced breakdown spectroscopy},
author = {Sanghapi, Hervé K. and Jain, Jinesh and Bol'shakov, Alexander and Lopano, Christina and McIntyre, Dustin and Russo, Richard},
abstractNote = {Laser induced breakdown spectroscopy (LIBS) is used for elemental characterization of outcrop samples from the Marcellus Shale. Powdered samples were pressed to form pellets and used for LIBS analysis. Partial least squares regression (PLS-R) and univariate calibration curves were used for quantification of analytes. The matrix effect is substantially reduced using the partial least squares calibration method. Predicted results with LIBS are compared to ICP-OES results for Si, Al, Ti, Mg, and Ca. As for C, its results are compared to those obtained by a carbon analyzer. Relative errors of the LIBS measurements are in the range of 1.7 to 12.6%. The limits of detection (LODs) obtained for Si, Al, Ti, Mg and Ca are 60.9, 33.0, 15.6, 4.2 and 0.03 ppm, respectively. An LOD of 0.4 wt.% was obtained for carbon. Finally, this study shows that the LIBS method can provide a rapid analysis of shale samples and can potentially benefit depleted gas shale carbon storage research.},
doi = {10.1016/j.sab.2016.05.011},
journal = {Spectrochimica Acta. Part B, Atomic Spectroscopy},
number = ,
volume = 122,
place = {United States},
year = {2016},
month = {5}
}