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A Comparative Study of Thin-Film Coated Silicon Wafer Surfaces for Laser-Induced Breakdown Spectroscopic Analysis of Liquids
(01. Izmir Institute of Technology, 2021) Aras, Nadir; Yalçın, Şerife Hanım
Laser-Induced Breakdown Spectroscopy, LIBS, is a relatively new atomic emission spectroscopic technique that shows rapid growth due to its many special peculiarities, like its ability to provide spectral signatures of all chemical species at the same time, in all environments of solid, liquid, or gas. Liquid sample analysis by LIBS is more troublesome compared to analysis of solids. Therefore, liquid analysis by LIBS requires some pretreatment steps to be applied before direct analysis of the samples. In the literature, a variety of approaches has been successfully applied and there is still plenty of room to improve methodologies used in the liquid-LIBS analysis. The main purpose of this thesis study was to perform studies for the development of a LIBS-TARGET for sampling liquids on it, after drying, by repetitive laser pulses. With this purpose, silicon wafer-based substrates with differing surface compositions; uncoated (crystalline silicon, c-Si), oxide-coated silicon, SiO2, and nitride coated silicon, Si3N4, were tested for several experimental parameters. Within the content of this study, a fast and accurate methodology for direct analysis of aqueous samples by LIBS is proposed. This methodology has two important attributes: one is the use of the non-metal substrate, silicon wafer, for the first time for direct analysis of aqueous samples dried on, and two is the use of high energy laser pulses focused outside the minimum focal point of a plano-convex lens at which relatively large laser beam spot covers the entire droplet area for plasma formation. Si-wafer-based substrates were used for both qualitative and quantitative analysis of Cd, Cr, Cu, Mn, and Pb elements, and analytical figures of merit were determined. The analytical performance of each substrate was evaluated from the experiments performed with aqueous standards and real water samples. Silicon nitride-coated substrate has shown superior properties in terms of enhancing the LIBS signal and as low as 11 pg detection limits for Pb were obtained.
Design, Construction and Optimization Studies of a Hydride Generation Laser-Induced Breakdown Spectrometric System, (hg-Libes), for the Determination of Toxic Elements in Aqueous Samples
(Izmir Institute of Technology, 2013) Ünal Yeşiller, Semira; Yalçın, Şerife Hanım
In this thesis study, design, construction and optimization of a continuous flow hydride generation laser-induced breakdown spectroscopic system, HG-LIBS, for the determination toxic and environmentally important elements: arsenic, selenium, lead, antimony, tin, bismuth, germanium and tellurium, has been performed. The HG-LIBS system, which has been constructed from its commercially available components, consisted of four main parts: a laser source, a hydride generation unit, a sample/plasma cell and a detection unit. In order to maximize LIBS emission signal, some instrumental parameters such as laser energy and detector gating parameters were investigated. Some chemical parameters such as acid/reductant concentration and flow rate, carrier gas type and flow rate, presence of pre-reducing/oxidizing agent that effect hydride generation efficiency and transportation of hydrides were also studied. Under optimized conditions detection limits of 0.2 mg L-1, 1.1 mg L-1, 1.0 mg L-1, 1.3 mg L-1 and 0.2 mg L-1 were obtained for Sn, As, Sb, Pb and Ge, respectively. No analytical signal could be detected from Se and Te elements with the system developed. The applicability of the HG-LIBS system for the determination of As, Sb, Pb and Ge in aqueous environments has been tested on several real water samples including tap water, drinking water and reference river water standard. Temporal variation of electron temperature and electron density values for tin and germanium hydride plasma was determined under argon and nitrogen environment. Electron temperatures were calculated by making use of neutral atomic lines in Boltzmann equation. Plasma electron density was evaluated from the Stark-broadened line shapes of Hα line at 656.3 nm. In order to investigate the main cause of increase in germanium signal under argon environment, physical plasma parameters were evaluated in argon and nitrogen gas mixtures. With this thesis study, the applicability of the HG-LIBS system for on-line monitoring of environmental pollutants has been shown.

Phd Degree / Doktora

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