A new cloud point extraction procedure has been developed for the quantification of plutonium(IV) in environmental samples. The separation procedure can be either coupled to inductively coupled plasma mass spectrometry (ICPMS) or α spectrometry for plutonium quantification. The method uses a combination of selective ligand (P,P'-di(2-ethylhexyl) methanediphosphonic acid (H2DEH[MDP])) and micelle shielding by bromine formation to enable quantitative extraction of Pu in highly acidic solutions. Cross-optimization of all parameters (nonionic and ionic surfactant, chelating agent, bromate, bromide, and pH) led to optimal of the extraction conditions. Figures of merit of the method for the detection using α spectrometry and ICPMS are reported (limit of detection, limit of quantification, minimal detectable activity, and recovery). Quantitative extractions (>95%) were obtained for a wide variety of aqueous and digested samples (synthetic urine, wastewater, drinking water, seawater, and soil samples). The method features the first successful coupling between α spectrometry and cloud point extraction and is the first demonstration of CPE suitability with metaborate fusion as a sample preparation approach, techniques used extensively in nuclear industries.
This study highlights a new type of extraction procedure combining a magnetic solid-phase support and a Schiff base ligand for the removal of uranium from rare earth leachates. After synthesizing and characterizing three Schiff base ligands (CH 3 Salen, H 2 Salophen, and MeOSalophen), they were combined with magnetic nanoparticles and assessed for the selective extraction of uranium. To optimize extraction, the effects of parameters such as the pH, the mass of the ligand, and extraction time, were explored. The maximum adsorption capacity for U(VI) using the magnetic MeOSalophen Schiff base was 63 ± 3 mg g −1 at pH = 6 with 25 mg of extracting agent for a contact period of 24 h. An acceptable extraction of U(VI) was also observed in more acidic conditions with a shorter extraction period. The magnetic ligand has shown a high selectivity toward U(VI) over a number of metals in a real rare earth element leaching solution.
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