Design, development and optimization of a fluorometric reaction-rate instrument and method of analysis for metal ions Public Deposited

http://ir.library.oregonstate.edu/concern/graduate_thesis_or_dissertations/9g54xm605

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  • The design, construction and operation of a fluorometric reaction rate instrument is described. The instrument is designed for simple operation with maximum versatility. Advantages and modes of operation of the system are discussed in detail. The instrument is used for the kinetics-based determination of trace levels of Ag and Al. Evaluation of the instruments! transfer function and SiN characteristics is also presented. The fluorescence spectrometer is shown to possess excellent S/N characteristics with a detection limit of 1 part-per-trillion for quinine sulfate. Signal-to-noise ratio studies allow the factors which limit precision to be identified. The versatile reaction ratemeter provides high resolution, digital readout of the measured rate and possesses excellent signal averaging capabilities. A new ratemeter testing circuit is described which allows a much better evaluation of a ratemeterts noise immunity and performance in a real situation. The development and optimization of fluorometric reaction rate methods of analysis is described in detail for silver and aluminum. These techniques provide large dynamic linear ranges of 6 ppb to 30 ppm and 0.4 ppb to 10 ppm, for the trace determination of Ag and Al, respectively. The relative standard deviation for the Ag analysis is less than 0. 5% for the whole concentration range whereas for Al the relative standard deviation is 0. 4% at the high end of the concentration range and increases to 2% at the detection limit. A complete interference study is described for both Ag and Al. For the analysis of Ag in real samples, a dithizone extraction procedure is developed to eliminate interferences and this procedure is applied to N.B.S. Zn spelter samples.
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