A procedure for the simultaneous separation and determination of fission products (lanthanides) and actinides (Pu, Np, U, Am and Cm) is described. The method is based on the use of an anionic/cationic mixed bed chromatographic column (CS5A, Dionex), coupled on-line to an ICP-MS detector. Optimisation of the parameters was carried out with standard solutions containing actinides and lanthanides at the 50 ng ml 21 concentration level. The effects of different oxidising/reducing agents as well as different mobile phases on the intensity and position of the chromatographic peaks were investigated. The analytical procedure was validated by the use of certified materials as well as by other independent techniques. Analytical figures of merit resulting from the procedure were compared with those obtained using other commercially available ion-exchange stationary phases. The procedure developed was applied to the inventory of spent nuclear fuel samples. Detection limits of 0.25 ng ml 21 and 0.45 ng ml 21 were obtained for lanthanides and actinides, respectively. Analytical precision was typical better than 5% over seven repeated measurements.
A novel sample cleanup procedure for the Am determination in environmental samples by alpha-spectrometry is described. The method is based on the use of three analytical chromatographic columns. TEVA-Spec. from Eichrom has been packed in an analytical chromatographic column to carry out the lanthanide/actinide separation. A CS5A mixed-bed column from Dionex was used to separate Am from lanthanide impurities and other actinides. A TCC-II column from Dionex was used to connect the TEVA to the CS5A and act as a preconcentrator column for the trivalent ions. The behavior of the columns was studied by coupling the chromatograph to an ICPMS detector. A chromatographic fraction has been used for sample preparation for alpha-spectrometric determination of 241Am. The analytical procedure has been validated with certified reference materials (sediment and soil) and was applied to sediment core samples from the Irish Sea and compared with the classical radiochemical separation of Am.
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