A series of studies was carried out on the direct analysis of solid samples with inductively coupled plasma atomic emission spectrometry (ICP-AES) and mass spectrometry (ICP-MS). Samples were first vaporized by modified electrothermal vaporization (ETV) systems and the vapor was introduced into the ICP. Inert gas flows were used to increase analyte transport efficiency and to reduce matrix effects. / Halogenation reactions were used to improve solid sample vaporization in one of the modified ETV systems. At temperatures ranging from 1000$ sp circ$C to 2400$ sp circ$C pure oxides and carbides were converted to lower boiling point halides and evaporated. Experimental results showed that, with the use of Freon-12 as a gas phase halogenation reagent, nearly 100% vaporization was achieved for $ rm Al sb2O sb3$ (B.P. 2980$ sp circ$C, particle size $<$10 $ mu$m), SiO$ sb2$ (B.P. 2230$ sp circ$C, particle size $<$44 $ mu$m), ZrO$ sb2$ (B.P. 5000$ sp circ$C, particle size $<$74 $ mu$m) and TaC (B.P. 5500$ sp circ$C, typical particle size 5 $ mu$m). The same was true for WC (B.P. 6000$ sp circ$C, particle size $<$10 $ mu$m) if BaCl$ sb2$ was used as a second halogenation reagent. These lead us to believe that we would be able to vaporize samples with almost any inorganic matrix. When the same ETV system was used to analyze four marine sediment reference materials and one coal fly ash reference material, a linear relationship was found between the background corrected peak area and the reference concentration for six of the eight elements monitored.
| Identifer | oai:union.ndltd.org:LACETR/oai:collectionscanada.gc.ca:QMM.41752 |
| Date | January 1994 |
| Creators | Ren, Jian Min |
| Contributors | Salin, Eric D. (advisor) |
| Publisher | McGill University |
| Source Sets | Library and Archives Canada ETDs Repository / Centre d'archives des thèses électroniques de Bibliothèque et Archives Canada |
| Language | English |
| Detected Language | English |
| Type | Electronic Thesis or Dissertation |
| Format | application/pdf |
| Coverage | Doctor of Philosophy (Department of Chemistry.) |
| Rights | All items in eScholarship@McGill are protected by copyright with all rights reserved unless otherwise indicated. |
| Relation | alephsysno: 001401259, proquestno: NN94705, Theses scanned by UMI/ProQuest. |
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