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Titel:Characterization of extraction chromatographic resins and method development for the separation and determination of Pd / Pt and 36Cl / 129I
Autor:Zulauf, Alexander
Weitere Beteiligte: Jungclas, Hartmut (Prof. Dr.)
URN: urn:nbn:de:hebis:04-z2010-07565
DDC: Chemie
Titel (trans.):Charakterisierung von extraktionschromatographischen Harzen und Methodenentwicklung für die Trennung und den Nachweis von Pd / Pt und 36Cl / 129I


Method developement and validation, Weight distribution coefficient, Palladiumion, Flüssigkeitsszintillati, ICP-MS, Methodenoptimierung, Platin, Chromatographie, Extraction chromatography (EXC), LSC, Charakterisierung, ICP-Massenspektrometrie, Validierung, Verteilungskoeffizient, Methodenentwicklung

The topic of the present work is the characterization of extraction chromatographic resins and method developments for the preconcentration, separation and detection of Pd and Pt and for 36Cl and 129I. Two newly developed resins (FClA and F49A, both TrisKem International) were at first characterized and compared with respect to the uptake of an elevated number of metal cations. Characterization studies were performed in batch experiments and included the determination of maximum uptakes, weight distribution ratios (Dw) and the influence of interferences on the uptake of the cations. Maximum uptakes were determined for Pd, Pt and Ag for varying acids at a fixed acid concetration. Weight distribution ratios were determined for several metal cations in different acids and acid concentrations with a main focus on Pd, Pt and Ag. The interferences caused upon the uptake of Pd and Pt was evaluated for an elevated number of cations and anions. Based on the results of the characterization studies a scheme for a method for the preconcentration and separation of Pd and Pt was developed. Also a method for preconcentration, separation and determination of 36Cl and 129I was developed. Therefore a new resin was prepared by loading FClA resin with silver ions (“silver loaded FClA resin”). The resin was also characterized by the determination of weight distribution ratios for chloride and iodide using 36Cl and 129I. Retention of both isotopes was tested in 1M H2SO4, elution conditions for chloride were tested using 0.01-0.2M KSCN solution and for iodide using 0.04-0.35M Na2S solution. Retention and elution conditions identified during the characterization studies were transferred to column geometry and further optimized. The method was validated with respect to its selectivity, linearity, trueness, precision, recovery and ruggedness. The method was also validated for different matrices (water, soil, filter and concrete).

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