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Emission Spectrometry For The Determination Of Uranium And Oxalate Based On Sulfosalophen Complex

Posted on:2015-11-29Degree:MasterType:Thesis
Country:ChinaCandidate:L ChenFull Text:PDF
GTID:2181330434955215Subject:Analytical Chemistry
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In the first part of this paper, the research significance and developments in thedetermination of uranium and oxalate are reviewed. The functional properties andapplication of salophen and its complexes are also introduced. After that the principleand application of supramolecular chemistry and resonance light scattering techniqueare described.In the second chapter, sulfo-salophen, a water-soluble tetradentate Schiff baseligand of uranyl, was synthesized by the reaction of5-sulfo-salicylaldehyde with1,2-phenylenediamine. The coordination reaction of sulfo-salophen with uranyl toform complex uranyl-sulfo-salophen was studied by fluorescence spectroscopy. Thereaction of sulfo-salophen with uranyl results in a remarkable enhancement offluorescence intensity. The maximum emission wavelength of the fluorescence is at428nm. The reaction was used to establish a fluorescence method for thedetermination of uranyl ion in aqueous solution. Under optimum conditions, the linearrange for the detection of uranyl is0.03to4.0nmol/mL. The detection limit is0.015nmol/mL. The proposed fluorescence method has been successfully applied for thedetermination of uranyl in environmental water samples with the recoveries of97.0%to104.0%.In the third chapter, a resonance light scattering (RLS) method for the directdetection of uranium (VI) or uranyl in aqueous solution without separation procedurehas been reported in this paper. Sulfo-salophen, a water-soluble tetradentate Schiffbase ligand of uranyl, reacted with uranyl to form a complex. The complex reactedfurther with oxalate to form supramolecular dimer with large molecular volume,resulting in a production of strong RLS signal. The amount of uranium (VI) wasdetected through measuring the RLS intensity. A linear range was found to be0.2to 30.0ng/mL under optimal conditions with a detection limit of0.15ng/mL. Themethod has been applied to determine uranium (VI) in environmental water sampleswith the relative standard deviations of less than5%and the recoveries of98.8to105.8%. The present technique is suitable for the assay of uranium (VI) inenvironmental water samples collected from different sources.In the fouth chapter,we report a resonance light scattering method for thedetermination of oxalate based on a water-soluble salophen and uranium.Sulfo-salophen, a water-soluble tetradentate Schiff base ligand of uranyl, reacted withuranyl to form a complex. The complex reacted further with oxalate to formsupramolecular dimer with large molecular volume, resulting in a production ofstrong RLS signal. The amount of oxalate was detected through measuring the RLSintensity. A linear range was found to be0.04to5.0nmol/mL under optimalconditions with a detection limit of0.018nmol/mL. The method has been applied todetermine oxalate in environmental water samples and the recoveries of98.3to104.5%.
Keywords/Search Tags:Uranyl, oxalate, Sulfosalicylic salophen, emission spectrometry, resonance light scattering, fluorescence
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