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Title: Analysis of slags using laser-induced breakdown spectroscopy

The feasibility of laser-induced breakdown spectroscopy (LIBS) for the analysis of gasification slags was investigated by comparing LIBS results to the results of an ICP-OES analyzer. A small amount of slag sample was placed on a piece of double sided adhesive tape attached to a glass microscope slide and analyzed for Al, Ca, Fe, Si, and V which are major elements found in slags. The partial least squares regression (PLS-R) and univariate simple linear regression (SLR) calibration methods indicated that apart from V (accuracy up to + 20%) the accuracy of analysis varies within 0.35–6.5% for SLR and 0.06–10% for PLS-R. A paired-sample t-test within the 95% confidence level yielded p-values greater than 0.05, meaning no appreciable statistical difference was observed between the univariate SLR with internal standardization and the multivariate PLS-R for most of the analytes. From the results obtained in this work, LIBS response varies depending on the element and the technique used for quantitative analysis. Simultaneous use of the univariate calibration curves with internal standard (intensity ratio) and PLS regression in multi-elemental analysis can help reduce the matrix effect of slags associated to their high variation in concentration. Overall, these results demonstrate the capability of LIBS asmore » an alternative technique for analyzing gasification slags. Estimated limits of detection for Al, Ca, Fe, Si and V were 0.167, 0.78, 0.171, 0.243 and 0.01 wt.%, respectively.« less
Authors:
 [1] ;  [1] ;  [1] ;  [2] ;  [3] ;  [3] ;  [3]
  1. Mississippi State Univ., Mississippi State, MS (United States). Inst. for Clean Energy Technology
  2. Mississippi State Univ., Mississippi State, MS (United States). Inst. for Clean Energy Technology; King Saud Univ., Riyadh (Saudi Arabia). Dept. of Physics
  3. National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States)
Publication Date:
Grant/Contract Number:
FE0004000
Type:
Accepted Manuscript
Journal Name:
Spectrochimica Acta. Part B, Atomic Spectroscopy
Additional Journal Information:
Journal Volume: 115; Journal Issue: C; Journal ID: ISSN 0584-8547
Publisher:
Elsevier
Research Org:
National Energy Technology Laboratory (NETL), Pittsburgh, PA, Morgantown, WV, and Albany, OR (United States)
Sponsoring Org:
USDOE
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; 36 MATERIALS SCIENCE; LIBS; ICP-OES; Slag; Internal standard; Multivariate analysis-partial least squares regression (PLS-R)
OSTI Identifier:
1480841
Alternate Identifier(s):
OSTI ID: 1359833

Sanghapi, Hervé K., Ayyalasomayajula, Krishna K., Yueh, Fang Y., Singh, Jagdish P., McIntyre, Dustin L., Jain, Jinesh C., and Nakano, Jinichiro. Analysis of slags using laser-induced breakdown spectroscopy. United States: N. p., Web. doi:10.1016/j.sab.2015.10.009.
Sanghapi, Hervé K., Ayyalasomayajula, Krishna K., Yueh, Fang Y., Singh, Jagdish P., McIntyre, Dustin L., Jain, Jinesh C., & Nakano, Jinichiro. Analysis of slags using laser-induced breakdown spectroscopy. United States. doi:10.1016/j.sab.2015.10.009.
Sanghapi, Hervé K., Ayyalasomayajula, Krishna K., Yueh, Fang Y., Singh, Jagdish P., McIntyre, Dustin L., Jain, Jinesh C., and Nakano, Jinichiro. 2015. "Analysis of slags using laser-induced breakdown spectroscopy". United States. doi:10.1016/j.sab.2015.10.009. https://www.osti.gov/servlets/purl/1480841.
@article{osti_1480841,
title = {Analysis of slags using laser-induced breakdown spectroscopy},
author = {Sanghapi, Hervé K. and Ayyalasomayajula, Krishna K. and Yueh, Fang Y. and Singh, Jagdish P. and McIntyre, Dustin L. and Jain, Jinesh C. and Nakano, Jinichiro},
abstractNote = {The feasibility of laser-induced breakdown spectroscopy (LIBS) for the analysis of gasification slags was investigated by comparing LIBS results to the results of an ICP-OES analyzer. A small amount of slag sample was placed on a piece of double sided adhesive tape attached to a glass microscope slide and analyzed for Al, Ca, Fe, Si, and V which are major elements found in slags. The partial least squares regression (PLS-R) and univariate simple linear regression (SLR) calibration methods indicated that apart from V (accuracy up to + 20%) the accuracy of analysis varies within 0.35–6.5% for SLR and 0.06–10% for PLS-R. A paired-sample t-test within the 95% confidence level yielded p-values greater than 0.05, meaning no appreciable statistical difference was observed between the univariate SLR with internal standardization and the multivariate PLS-R for most of the analytes. From the results obtained in this work, LIBS response varies depending on the element and the technique used for quantitative analysis. Simultaneous use of the univariate calibration curves with internal standard (intensity ratio) and PLS regression in multi-elemental analysis can help reduce the matrix effect of slags associated to their high variation in concentration. Overall, these results demonstrate the capability of LIBS as an alternative technique for analyzing gasification slags. Estimated limits of detection for Al, Ca, Fe, Si and V were 0.167, 0.78, 0.171, 0.243 and 0.01 wt.%, respectively.},
doi = {10.1016/j.sab.2015.10.009},
journal = {Spectrochimica Acta. Part B, Atomic Spectroscopy},
number = C,
volume = 115,
place = {United States},
year = {2015},
month = {10}
}