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Developments in the application of atomic spectroscopy to trace metal analysis

Thesis/Dissertation ·
OSTI ID:5739385

A method is described for the determination of selenium in horse blood by generation, atomization and analysis of the selenium hydride. A pooled horse blood sample which contained 8.8 ..mu..g 1/sup -1/ of selenium exhibited a precision of analysis of 4.32% for ten replicate analyses. A study of the sensitivity of nonresonance and resonance lines of ytterbium utilizing microboat and platform atomization was investigated. Increases of at least twofold for all nonresonance lines were observed. Microboat sensitivity fell between that of the wall and the platform. Alternative surfaces of electrothermal atomization atomic absorption spectrophotometry (ETAAS) and the thermodynamic process for atom formation in ETAAS were investigated. Sensitivities for carbide-formation elements such as ytterbium and molybdenum and other noncarbide formation elements were determined by precoating graphite tubes and inserting collars. An improvement in analytical sensitivity and reduction in memory effect compared to commercially available pyrolytic graphite tubes were observed for all except the molybdenum analyte where a depression in analytical sensitivity resulted. The useful lifetime (analysis cycles) of all surfaces (except metal collars) were recorded at 250 to 400 cycles with acceptable and comparable precisions. A method is described for proposing the thermodynamic process in IL655 ETAAS. Appearance temperatures of analytes and free energy were studied and two major pathways were found operative: 1) thermal dissociation of the analyte oxide; 2) carbon reduction of the oxide followed by atomization of the free metal.

Research Organization:
New Mexico State Univ., Las Cruces (USA)
OSTI ID:
5739385
Country of Publication:
United States
Language:
English