Um novo método para extração líquido-líquido, separação e pré-concentração de cério(IV) com um derivado ácido do calix [4]resorcinareno [C4RAHA] é descrito. Cério foi extraído em pH 9 com etilacetato, e recuperado de areias monazíticas, na presença de tório, urânio, lantânio e um grande número de cátions e ânions. Cério(IV) forma um complexo colorido, amarelo, λ max 381 nm, absortividade molar de 1,06 × 10 4 L mol -1 cm -1 e obedece a lei de Beer no intervalo entre 0,4 e 15 mg mL -1 . A razão metal-ligante encontrada para cério(IV) foi de 4:1 (M:L). Estudos de transporte foram realizados em um sistema de três fases, através de uma membrana líquida contendo C4RAHA. Para medidas por ICP OES, o extrato pode ser diretamente aspirado, o que aperfeiçoa a sensibilidade em 25 vezes e os limites de estimativa são 5-150 μg L -1 de cério. O método foi aplicado para a determinação de cério em materiais geológicos de referência, areia monazítica e amostras de água de mar.A new method for liquid-liquid extraction, separation and preconcentration of cerium(IV) with a calix[4]resorcinarene acid derivative [C4RAHA] is reported. Cerium was extracted at pH 9 in ethyl acetate and recovered from monazite sands in the presence of thorium, uranium, lanthanum and large number of cations and anions. Cerium(IV) forms yellow coloured complex, λ max 381 nm, molar absorptivity 1.06 × 10 4 L mol -1 cm -1 and obeys Beer's law over the range 0.4-15 mg mL -1 . The metal ligand ratio for cerium (IV) was found to be 4:1 (M:L). Transport studies were carried out in a three phase system across a liquid membrane containing C4RAHA. For ICP OES measurements, the extract can be directly aspirated, which enhances the sensitivity 25-fold and the limits for estimation are 5-150 μg L -1 of cerium. The method was applied for the determination of cerium in standard geological samples, monazite sand and sea water samples.Keywords: cerium(IV), calix [4]resorcinarene-N-fenil-acetohydroxamic acid(C4RAHA), transport studies, spectrophotometry
IntroductionThe chemistry of bowl shaped macrocyclic compounds that can complex organic and inorganic guests has been receiving significant attention in the field of supramolecular chemistry. 1 Among the different macrocyclic compounds, calix[4]resorcinarenes and calixarenes 2 have been widely employed as changeable units with a well defined structure and easy accessibility. The calixresorcinarenes are unique three-dimensional cyclic tetramer and hexamer that belong to a class of metacyclophanes in which resorcinol units are linked by methylene bridges. 3 The interest towards this class of compounds which are capable of forming host guest complexes is stimulated by the development of supramolecular chemistry which uses them for the possible creation of synthetic receptors and carriers of cations, anions and neutral molecules. 4 The host properties of calix[4]resorcinarenes continue to draw research interests due to its potential application as macrocyclic receptors, 5 as dendrimers in biological systems, 6 nano-capsule, 7 na...