Cation analysis by thin-layer chromatography and reflectance spectroscopy
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1968
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University of Hawaii at Manoa
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Abstract
A procedure whereby reflectance spectroscopy can be employed for the analysis of substances resolved on thin-layer plates was developed with the use of metal cation mixtures that had been separated on cellulose plates. A rapid method was devised whereby fourteen cations were separated and identified in situ by their reflectance spectra after chromogenesis with a mixture of dithizone and 8-hydroxyquinoline. Further studies were carried out on three of these cations: copper, nickel, and zinc. Copper and nickel were determined in the presence of eleven other cations without experiencing any interferences by employing neocuproine and dimethylglyoxime, respectively, as chromogenic reagents. In the case of zinc, the use of 3,3'-dimethylnaphthidine was equally successful except in the presence of tin, cadmium, and iron. The optimum concentration and reflectance ranges and the maximum accuracy of these analyses were then deduced by applying two graphical methods to the data obtained. A high-reflectance differential technique was developed for the measurement of micro-amounts of the above three cations. As the concentration of the reflectance standard was decreased, the lower limits of both the optimum reflectance range and optimum concentration range was extended to lower values. The probable percent error arising from an error of 1% reflectance was decreased significantly from 7% in the "ordinary" method to approximately 2-3% with the use of appropriate differential standards. Finally the utility of the procedure in the analysis of sea water was demonstrated. Precencentration of the trace metals was carried out using dithizone as the sequestering reagent. After back-extraction into the aqueous phase, the copper, nickel, and zinc were separated from each other and from interferences on cellulose chromatoplates. The were then determined by the methods developed employing both the ordinary and high reflectance techniques. The experimental methods were evaluated by enriching sea water samples with the three metal cations and carrying through the extraction, chromatographic separation, and reflectance measurements.
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Cations, Thin layer chromatography, Reflectance spectroscopy
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Theses for the degree of Doctor of Philosophy (University of Hawaii (Honolulu)). Chemistry; no. 164
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