Improvement of the capabilities of inductively coupled plasma optical emission spectrometry for the analysis of complex matrices and for single particle analysis

Abstract

The objective of this thesis is to explore new applications of inductively coupled plasma optical emission spectrometry (ICP-OES).

The first application involved the development of a method for the direct bulk analysis of a 12 M KOH zincate electrolyte fuel, which is used for green energy backup systems. By using flow injection analysis in combination with an inert sample introduction system, the concentrations of additives (Al, Fe, Mg, In, Si) and corrosion products (Zn2+ and CO32-) were quantified. However, accurate determination of all elemental concentrations was unsuccessful due to suppression from the matrix. The second application focused on exploring and enhancing the capabilities of single particle ICP-OES analysis for the characterization of the particles filtered from the 12 M KOH zincate electrolyte fuel. A conventional pure argon plasma and Ar-N2-N2/H2 mixed gas plasma were compared with regards to sensitivity, detection limit, and robustness to establish which operating conditions minimize the detectable particle mass. The effect of infrared heating the sample aerosol in the spray chamber and base of the torch was explored to increase transport efficiency and reduce the noise arising from aerosol processing within the plasma that would degrade detectable particle mass. Two surfactants were also explored to stabilize and disperse particles in solution.