The speciation of Tc after the extraction of Tc(IV) from HO and 1 M HNO by dibutylphosphoric acid (HDBP) in dodecane has been studied by X-ray absorption fine structure (XAFS) spectroscopy. Results show the formation of dimeric species with TcO and TcO units, and the formulas [TcO(DBP·HDBP)] (1) and [TcO(NO)(DBP)(DBP·HDBP)] (2) were, respectively, proposed for the species extracted from HO and 1 M HNO. The interatomic Tc-Tc distances found in the TcO and TcO units [2.55(3) and 3.57(4) Å, respectively] are similar to the ones found in Tc(IV) dinuclear species. It is likely that the speciation of Tc(IV) in dodecane is due to the extraction of a species with a TcO unit for (2) and to the redissolution of a Tc(IV)-DBP solid for (1). The XAFS results for (1) and (2) were compared to that obtained for the extraction of Tc(IV) with TBP/HDBP/dodecane from 0.5 M HNO, (3) which highlight the formation of Tc mononuclear nitrate species {i.e., [Tc(NO)(DBP)] or [Tc(NO)(DBP·HDBP)]}. These results confirm the importance of the preparation and speciation of the Tc(IV) aqueous solutions prior to extraction and how much this influences and drives the final Tc speciation in organic extraction. These studies outline the complexity of Tc separation chemistry and provide insights into the behavior of Tc during the reprocessing of used nuclear fuel.
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