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Hydride Generation and Laser Spectroscopy Techniques for Trace Analytical Measurements of Antimony and Selenium

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Degree
Master of Science in Chemistry, Youngstown State University, Department of Chemistry, .
Abstract
Hydride generation (HG) sample introduction increases the sensitivity for certain metal species by converting them to their gaseous forms for measurement by atomic spectrometry techniques. In this work, measurement methods have been developed for the trace analysis of antimony (Sb) and selenium (Se) using HG coupled to Laser Induced Fluorescence (LIF) or Laser Induced Breakdown Spectroscopy (LIBS) detection techniques. In the LIF studies, aqueous samples of Sb are subjected to HG and the Sb hydride is carried to the flame which acts as an atomization source. The wavelengths of absorption and fluorescence emission for Sb were found to be 212.7 nm and 259.8 nm, respectively. The intensity of fluorescence was plotted against the concentration of Sb used. It was found that the intensity was linearly related to the concentration of Sb in the range 0.3-10 ppb. The limit of detection (LOD) was found to be 0.003 ppb. A similar technique has been used for the determination of Sb and Se in aqueous samples using LIBS. In this approach, a plasma instead of a flame is used to excite Sb and Se atoms and the atomic emission is measured at wavelengths of 259.9 nm and 196.1 nm, respectively. Using these wavelengths, calibration curves were plotted for intensity of emission against different concentrations of Sb and Se. From the calibration curve, the slope and LOD have been determined. The results of the studies have been evaluated to show the relative performance of each technique.
Subject Headings
Analytical chemistry; Chemistry
Keywords
Hydride generation; Laser spectroscopy; Trace analytical measurements; Antimony; Selenium
Committee / Advisors
Josef Simeonsson, PhD (Advisor)
Timothy Wagner, PhD (Committee Member)
Daryl Mincey, PhD (Committee Member)
Pages
xvi, 79 p.

Document number: ysu1219424557
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