Separation Behavior of U(VI) and Th(IV) on a Mixed Ion Exchange Column Using 2,6-Pyridine Dicarboxylic Acid as a Complexing Agent and Determination of Trace Level Thorium in Uranium Matrix Employing High Performance Ion Chromatography

Abstract

Retention behavior of U(VI) and Th(IV) as their 2,6-pyridine dicarboxylic acid (PDCA) complexes on reversed phase and ion exchange (cation, anion and mixed ion exchange) columns was studied and based on the results, a simple ion chromatography method for the determination of trace level thorium in uranium oxide using 0.075 mM 2,6-pyridine dicarboxylic acid (PDCA) and 1 M KNO 3 in 1.2 M HNO 3 as eluent (flow rate 1 mL/min) was proposed. The advantage of the developed method is that the separation of uranium matrix is not required prior to the ion chromatographic determination of trace Th. Separation was carried out on a mixed ion exchange stationary phase and a 10 −4 M arsenazo (III) solution was used as post column reagent for detecting the separated metal ions. The separation of Th from uranium using PDCA in the present investigation is attributed through cation exchange mechanism. A calibration plot was constructed by following the standard addition method over the concentration range of 0.25 to 10 ppm of Th in the presence of uranium matrix, which resulted in a linear regression coefficient of 0.9978. The precision of the method was better than 5% and the LOD for Th was found to be 0.1 ppm (S/N = 3). The method has been validated by comparing the results with the results obtained from ICP-MS analysis where the Th is separated from the uranium matrix. The proposed method is simple, rapid, accurate and cost effective compared to techniques like ICP-MS or ICP-AES and is suitable for the routine kind of analysis.

Fast and selective reversed-phase high performance liquid chromatographic separation of UO22+ and Th4+ ions using surface modified C18 silica monolithic supports with target specific ionophoric ligands

“… 42 Similar studies were also conducted by Raut et al , which were based on both ion exchange and reverse phase behavior of 2,6-pyridine dicarboxylic acid for the complexation of UO 2 2+ and Th 4+ . 43 In addition, Datta et al have conducted extensive studies on the chromatographic separation of UO 2 2+ and Th 4+ using short columns with small particle sizes to separate UO 2 2+ from Pu 3+ and Pu 4+ . 44 Inspired by the results obtained, they have used monolithic supports modified with bis-2-ethylhexyl succinamic acid as a stationary phase for burn-up measurements of fast reactor fuels.…”