Organic solvent effects on sulfur and phosphorous band emissions and direct isotipic analysis by atomic fluorescence flame spectrometry

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1971

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In this dissertation, two parts of study undertaken are presented. In the first part, the analytical applicability of sulfur and phosphorous band emission in aqueous and organic solvents has been investigated. Although the sulfur and phosphorous molecular band emissions were affected by quenching actions and with flame temperature with organic solvents, the observed maximum emission intensity was established to be useful for sulfur and phosphorous determination. It has been postulated in the literature that efficient atomization with organic solvents and the temperature of a flame are responsible for an increased emission intensity of metal atoms in organic solvents. However, the role of flame temperature appears to be a determining factor influencing the emission intensity in flame emission spectrometry. During this investigation, it was necessary to develop a correct calibration procedure for rotameter-type gas flow measuring devices. Hence, a newly developed calibration procedure is presented. In the second part, a possibility of isotopic analysis is investigated. The analysis has been carried out with mercury, zinc, copper, and indium isotopes by using electrodeless discharge lamps containing a single isotope as a light source. Of many factors, temperature of the atomic vapor in the flame cell and of the lamp is found to be very critical. Furthermore, with the present technique of atomic fluorescence flame spectrometry, temperature of atomic vapors appears to be the limiting factor for isotopic analysis. Among those isotopic elements studied, only mercury gives separations with adequate separation (10 to 20% overlap) between isotopic lines. Comparison of atomic fluorescence with atomic absorption flame spectrometry for the isotopic analysis is also made.

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