Title

Laser-Induced Breakdown Spectroscopy: Simultaneous Multi-Elemental Analysis and Geological Applications

Advisor

Singh, Jagdish P.

Committee Member

Arnoldus, Hendrik F.

Committee Member

Monts, David L.

Committee Member

McIntyre, Dustin L.

Committee Member

Srinivasan, Kalyan K.

Date of Degree

1-1-2017

Original embargo terms

Visible to MSU only for 3 years

Document Type

Dissertation - Open Access

Degree Name

Doctor of Philosophy

College

College of Arts and Sciences

Department

Department of Physics and Astronomy

Abstract

Under high irradiation, a fourth state of matter named plasma can be obtained. Plasmas emit electromagnetic radiation that can be recorded in the form of spectra for spectroscopic elemental analysis. With the advent of lasers in the 1960s, spectroscopists realized that lasers could be used simultaneously as a source of energy and excitation to create plasmas. The use of a laser to ignite a plasma subsequently led to laser-induced breakdown spectroscopy (LIBS), an optical emission spectroscopy capable of analyzing samples in various states (solids, liquids, gases) with minimal sample preparation, rapid feedback, and endowed with in situ capability. In this dissertation, studies of LIBS for multi-elemental analysis and geological applications are reported. LIBS was applied to cosmetic powders for elemental analysis, screening and classification based on the raw material used. Principal component analysis (PCA) and internal standardization were used. The intensity ratios of Mg/Si and Fe/Si observed in talcum powder show that these two ratios could be used as indicators of the potential presence of asbestos. The feasibility of LIBS for the analysis of gasification slags was investigated and results compared with those of inductively-coupled plasma−optical emission spectrometry (ICP-OES). The limits of detection for Al, Ca, Fe, Si and V were determined. The matrix effect was studied using an internal standard and PLS-R. Apart from V, prediction results were closed to those of ICP-OES with accuracy within 10%. Elemental characterization of outcrop geological samples from the Marcellus Shale Formation was also carried out. The matrix effect was substantially reduced. The limits of detection obtained for Si, Al, Ti, Mg, Ca and C were determined. The relative errors of LIBS measurements are in the range of 1.7 to 12.6%. Gate delay and laser pulse energy, have been investigated in view of quantitative analysis of variation of trace elements in a high-pressure environment. Optimization of these parameters permits obtaining underwater plasma emission of calcium with quantitative results on the order of 30 ppm within a certain limit of increased pressure. Monitoring the variation of the trace elements can predict changes in the chemical composition in carbon sequestration reservoir.

URI

https://hdl.handle.net/11668/17711

Comments

carbon sequestration||multivariate analysis||trace analysis||Internal standardization||Multi-elemental analysis||Marcellus shale formation||Elemental analysis||Slag analysis||Partial least squares regression||Principal component analysis||Samples classification||Optical emission spectroscopy||ICP-OES||Laser induced breakdown spectroscopy

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