Leaching of rare earth elements from phosphogypsum.

High amounts of phosphogypsum (PG) are generated in the production of phosphoric acid. Previous literature demonstrates that obtaining rare earth elements (REE) from PG is a promising alternative to managing this waste. However, the reported leaching efficiencies are low in most cases, or drastic leaching conditions are required. Therefore, this work aimed to study the leaching conditions of REE from PG to obtain high leaching efficiency values. Initially, a 24 factorial experimental design investigated the factors that affect the conventional acid leaching of REE from PG (leaching acid (citric and sulfuric acid), solid/liquid ratio, acid concentration, and temperature). Better leaching efficiency values of the sum of all REE (62.0% and 89.7% for citric and sulfuric acid, respectively) were obtained using an acid concentration of 3 mol L-1, solid/liquid ratio of 1/20 g mL-1, and temperature of 80 °C. Subsequently, the experiments optimization, performed through a central composite rotational design, indicated that the maximum leaching efficiency was achieved using a sulfuric acid concentration of 2.9 mol L-1, solid/liquid ratio of 1.7/20 g mL-1, and 55 °C. Under these conditions, the leaching efficiency of the sum of all REE was 90.0%. Leaching kinetics results showed that the equilibrium was reached in about 20 min for most REE. The mechanism investigation suggested that surface chemical reaction and diffusion through the boundary layer controlled the leaching.

Microwave-based strategies for sample preparation and halogen determination in blood using ICP-MS.

In this work, two microwave-assisted sample preparation methods based on combustion and ultraviolet digestion for futher determination of Br, Cl, and I in blood by inductively coupled plasma mass spectrometry were proposed. For microwave-induced combustion (MIC), blood was spotted on square pieces of Munktell TFN paper, and water and diluted NH4OH were evaluated as absorbing solutions. The stability of the analytes in the spotted blood was also evaluated. During 90 days, no changes of halogen content were observed for samples (with and without anticoagulant) on paper stored in a desiccator at 20 ± 5 °C. Whole blood was also digested by microwave-assisted ultraviolet digestion (MAD-UV). Some parameters as the volume of HNO3 solution, the influence of H2O2, and the effect of UV radiation were investigated. The interferences caused by C and K on halogen determination were carefully investigated. The results for MIC and MAD-UV and Br, Cl and I determination by ICP-MS presented no difference. The accuracy of MIC and MAD-UV was also evaluated by analyte spike with reference solutions of Br, Cl and I using inorganic species and also organic I standard (T4-levothyroxine). For both methods, recoveries were 94 and 108% for Br, 96 and 103% for Cl, and 104 and 97% for I. In case of organic I, recoveries were 99 and 111% for MIC and MAD-UV, respectively. The limits of quantification for MIC and MAD-UV after ICP-MS determination were 0.06 and 0.04 µg g-1 for Br, 14 and 30 µg g-1 for Cl and 12 and 8 ng g-1 for I, respectively. The proposed methods provide a suitable digestion approach, assuring safety and high digestion efficiency for further halogen determination in blood, with the possibility to use in clinical analysis.