Investigation of chromatographic procedures for the analysis of cationic impurities in uranium and plutonium matrices by ICP-OES and ICP-MS

Abstract

Four different separation protocols were tested to analyze several cations in a U-Pu matrix by inductively coupled plasma – optical emission spectrometry (ICP-OES) or mass spectrometry (ICP-MS): UTEVA resin with HNO₃ eluent, UTEVA resin with HNO₃/H₂C₂O₄ eluent, UTEVA resin with HNO₃/H₂O₂ eluent and TEVA resin with HNO₃ eluent. It was shown that none of the twenty nine tested cations (Al, Ag, B, Ca, Cd, Ce, Cr, Cu, Fe, Ga, La, Mg, Mn, Mo, Na, Nd, Ni, Pb, Pd, Rh, Sb, Se, Si, Sn, Sr, Ti, V, Y and Zn) was retained onto the resin, with recovery yields between 80 and 120 %. Meanwhile, the U-Pu matrix was retained onto the resin and was eliminated from the fraction containing the cations. After initial testing, two of the protocols were chosen: UTEVA resin with HNO₃/H₂C₂O₄ eluent and UTEVA resin with HNO₃/H₂O₂ eluent thanks to their efficacy and practicality. Then, the two selected protocols were applied to a uranium oxide certified reference material to validate them. Twenty three out of the thirty one impurities presents in the material (Ag, Ba, Be, Bi, Cd, Co, Cr, Cu, Dy, Eu, Fe, Gd, In, Li, Mo, Ni, Pb, Sm, Sn, Ti, V, W and Zr) were determined with good recoveries. Th was fixed onto the resin. Based on theses results, it seems possible to analyze the forty one impurities in a U-Pu material by optimizing the operating conditions. These two protocols were used to study the presence of impurities in a Pu-based material to ensure the purity of the materials. Detection limits in the order of μg g⁻¹ powder were obtained.