Zr and U determination at trace level in simulated deep groundwater by Q ICP-MS using extraction chromatography

Abstract

In the framework of trace element analysis by Q ICP-MS in a simulated deep Callovo-Oxfordian groundwater, separation procedures based on extraction chromatography were developed to eliminate the high salt contents and to concentrate Zr and U simultaneously. Theoretical and experimental speciation studies showed the importance of adjusting the medium to HNO3/HF (0.5M/0.005M) to guarantee the stability over time of the analytes before removal of the matrix. Two preconcentration methods based on TRU® and TODGA® resins were optimized for the simultaneous isolation of Zr and U prior to Q ICP-MS measurements. Using TRU resin, alkali and alkali earth metals contained in the deep groundwater were removed with 2M HNO3 whereas Zr and U were recovered with a HNO3/NH4HC2O4 (0.02M/0.05M) medium. For the separation protocol based on TODGA resin, alkali and alkali earth metals were eliminated with 3M and 11M HNO3 while Zr and U were simultaneously stripped with a HNO3/HF (0.5M/0.2M) medium. The procedure optimized on TODGA resin was validated with the French AFNOR NF T90-210 standard by studying linearity, limits of quantification (LOQ) and separation yields. The LOQ was determined at 0.008μgL−1 for Zr and U after the separation. Both analytes were recovered quantitatively. Compared to a sample dilution implemented to reduce the matrix effects, the developed preconcentration method allowed improving the sensitivity up to a 20 fold factor for Zr and U measurements at trace level by Q ICP-MS.