Rapid separation of lanthanides and actinides on small particle based reverse phase supports

Abstract

This paper presents the results on the use of short columns (3-5 cm long) with small particle size (1.8 µm) for high performance liquid chromatographic separation of individual lanthanides and uranium from plutonium as well as uranium from thorium to achieve rapid separations i.e. separation time as short as 3.6 min for individual lanthanides, 1 min for thorium-uranium and 4.2 min for uranium from plutonium. These advantages can be exploited to significantly reduce analysis time, liquid waste generation as well as dose to operator when radioactive samples are analysed e.g. burn-up determination.In the present work, a dynamic ion-exchange chromatographic separation technique was employed using camphor-10-sulfonic acid (CSA) as the ion-pairing reagent and α-hydroxy isobutyric acid (α-HIBA) as the complexing reagent for the isolation of individual lanthanides as well as the separation of uranium from thorium.Uranium was separated from Pu(III) as well as Pu(IV) by reverse phase HPLC technique. The reverse phase HPLC was also investigated for the isolation and quantitative determination of uranium from thorium as well as lanthanide group from uranium.The dynamic ion-exchange technique using small particle support was demonstrated for measuring the concentrations of lanthanide fission products such as La, Ce, Pr, Nd and Sm in the dissolver solution of fast reactor fuel. Similarly, the assay of uranium in the dissolver solution of fast reactor was carried out using reverse phase HPLC technique. The rapid separation technique using reverse phase HPLC was also demonstrated for separation of lanthanides as a group from uranium matrix; samples of LiCl-KCl eutectic salt containing chlorides of lanthanides in uranium matrix (typically 1 : 2000) were analysed.

Burn-Up Measurements on Dissolver Solution of Mixed Oxide Fuel Using HPLC-Mass Spectrometric Method

“…The reversed phase monolith column was modified into a dynamic ion-exchange support using water soluble mod-ifier, e.g., ion-pairing reagent, camphor-10-sulfonic acid (CSA) [9][10][11]. The lanthanides were separated and eluted using alpha hydroxy isobutyric acid (α-HIBA).…”

Preferential removal of Sm by evaporation from Nd–Sm mixture and its application in direct burn-up determination of spent nuclear fuel

“…Isotopic ratio (IR) measurement by TIMS, by applying correction factors for interfering isotopes is not applicable for fission product monitor, as the isotopic composition of elements formed as fission products differ from their natural composition. Several HPLC based studies have been carried out & M. Joseph mj@igcar.gov.in to simplify and reduce the separation time [6][7][8]. The HPLC method offers reasonably accurate results for vital theoretical calculations for effective fuel management, but requires a minimum 5-10 lg of Nd/mL of aliquot (corresponding to *10 mg/mL of heavy elements) in the dissolver fuel solution for separation, resulting in a considerable volume of radioactive liquid waste and radiation exposure to the personnel.…”

Correlation of retention of lanthanide and actinide complexes with stability constants and their speciation

“…A separation procedure for the isolation of individual lanthanides was earlier reported from our laboratory [9,10]. In the recent past, small particle supports (1.8 µm) were employed for the rapid separation of lanthanides in about 3.7 min [11]. Separation time of lanthanides was further reduced to 2.8 min with monolith based support [12].…”

“…Separation time of lanthanides was further reduced to 2.8 min with monolith based support [12]. These rapid and high-resolution separation methods developed were demonstrated for burnup measurements on nuclear reactor fuel to minimise radiation exposure to the personnel [2,[10][11][12].…”