Author(s) |
Kelkar, A.; Prakash, A.; Afzal, M.; Panakkal, J. P.; Kamath, H. S. |
An ion chromatographic method has been developed for the determination of traces of
Li+, Na+, K+, Ca2+, Mg2+,
Sr2+, Fe3+, Cu2+, Ni2+,
Co2+, Zn2+, Cd2+, Mn2+ in
UO2, ThO2 powders and sintered (Th,U)O2 pellets. This new method utilizes poly-(butadiene-maleic acid) (PBDMA) coated silica cation exchange column and mixed functionality column of anion and cation exchange to achieve the separation of alkali, alkaline earths and transition metal ions, respectively. It involves matrix separation after sample dissolution by solvent extraction with TBP (tri butyl phosphate)-TOPO (tri octyl phosphine
oxide)/CCl4. Interference of transition metal ions in the determination of alkali, alkaline earth metal ions are removed by using pyridine 2,6-dicarboxylic acid (PDCA) in the tartaric acid mobile phase. Mobile phase composition is optimized for the base line separation of alkali, alkaline earth and transition metal ions. Linear calibration graphs in the range 0.01-20
µg mL-1 were obtained with regression coefficients better than 0.999. The respective relative standard deviations were also determined. Recoveries of the spiked samples are within
± 10% of the expected value. The developed method is authenticated by comparison with certified standards of
UO2 and ThO2 powders. |