Um novo método para determinação simultânea de íons paládio, platina e ródio, como quelatos metal-DHBTR foi desenvolvido. Os íons paládio, platina e ródio foram derivatizados (pré-coluna) com 2,4-dihidroxibenzilidenotiorodanina (DHBTR) para formar quelatos coloridos. Os quelatos Pd-DHBTR, Pt-DHBTR e Rh-DHBTR são absorvidos na coluna de enriquecimento, quando injetados e transportados por uma fase móvel composta por solução tampão de ácido acético-acetato de sódio 0,05 mol L -1 (pH 3,5). Após o término do enriquecimento, ao acionar uma válvula de seis vias, os quelatos retidos foram carregados pela fase móvel, para a coluna analítica. A separação dos quelatos na coluna analítica foi satisfatória com acetonitrila 62% (v/ v) (contendo solução tampão de ácido acético-acetato de sódio (0,05 mol L -1 , pH 3,5) e 0,1% (m/v) de tritonX-100) como fase móvel. Os limites de detecção de paládio, platina e ródio são 3,6 ng L -1 , 3,2 ng L -1 e 4,5 ng L -1 , respectivamente. Este método foi aplicado para a determinação de paládio, platina e ródio em água, urina e amostras de solo, com bons resultados.A new method for the simultaneous determination of palladium, platinum and rhodium ions as metal-DHBTR chelates was developed. The palladium, platinum and rhodium ions were pre-column derivatized with 2,4-dihydroxybenzylidenethiorhodanine (DHBTR) to form colored chelates. The Pd-DHBTR, Pt-DHBTR and Rh-DHBTR chelates can be absorbed onto the front of the enrichment column when they were injected into the injector and sent to the enrichment column with a 0.05 mol L -1 sodium acetate-acetic acid buffer solution (pH 3.5) as mobile phase. After the enrichment had finished, by switching the six ports switching valve, the retained chelates were back-flushed by mobile phase and traveling towards the analytical column. These chelates separation on the analytical column was satisfactory with 62% (v/v) acetonitrile (containing 0.05 mol L -1 of pH 3.5 sodium acetate-acetic acid buffer salt and 0.1% (m/v) of tritonX-100) as mobile phase. The Limits of detection of palladium, platinum and rhodium are 3.6 ng L , respectively. This method was applied to the determination of palladium, platinum and rhodium in water, urine and soil samples with good results.Keywords: palladium, platinum, rhodium, 2,4-dihydroxybenzylidenethiorhodanine, high performance liquid chromatography, on-line enrichment
IntroductionEnvironmental contamination by the platinum group elements (PGEs), mainly related to automotive catalytic converters, is exponentially increasing and reliable and accurate quantification is a mandatory task. [1][2][3][4] The wide use of palladium, platinum and rhodium not only in automotive catalytic converters but as a drug (Pt) and in food production (Pd) 5 has led to a more uncontrolled release of those metals in the environment, with respect to the one due to the traditional chemical industry. Moreover, the platinum group elements derived from automotive catalytic converters are released as nanocrystallites (particles with less than 3 mm in ...