RESUMO
A chromatographic method is described for the separation and quantification of polycyclic aromatic sulfur heterocycles (PASHs) using liquid chromatography coupled with diode array detection (DAD). The PASHs that were investigated in this study were chosen based on their similarity in molecular weight, volatility and polarity of their PAH analogues. The chromatographic separation of the compounds was optimized, and their analytical characteristics were evaluated. The limits of detection and quantification ranged from 0.05 for 2,3,4,7-tetramethylbenzothiophene to 2.16 µg L-1 for thieno[2,3-b]thiophene and from 0.16 for 2,3,4,7-tetramethylbenzothiophene to 6.53 µg L-1 for thieno[2,3-b]thiophene, respectively. Recoveries ranged from 84.9 for benzo[b]benzo[4,5]thieno[2,3-d]thiophene to 110% for dinaphtho[2,1-b:1',2'-d]thiophene. Intermediate precisions and repeatabilities lie between 1.4 and 3.0%, and 0.3 and 1.7%, respectively. The chromatographic method was applied for determination of PASHs directly in asphalt fumes, which were obtained by heating asphalt samples in a homemade closed system. The mutual interference of PAH analogues was also discussed. The method was successfully used for PASH determination in asphalt samples obtained from three different oil refineries in Brazil.
Assuntos
Hidrocarbonetos , Enxofre , Cromatografia Líquida de Alta Pressão , Cromatografia LíquidaRESUMO
This paper describes the simultaneous determination of Ba, Co, Fe, and Ni in nuts by high-resolution continuum source atomic absorption spectrometry after extraction induced by solid-oil-water emulsion breaking. Extraction yields ranged from 94.9 for Ba to 109.8% for Fe. Simultaneous measurements were carried out at secondary lines of Ba, Co, Fe, and Ni. The limits of detection and quantification were, respectively, 3.819 and 1.146 mg L-1 for Ba, 2.274 and 7.421 µg L-1 for Co, 0.095 and 0.285 mg L-1 for Fe, and 2.138 and 6.614 µg L-1 for Ni. The precision ranged from 3.1 to 4.2%, 1.5 to 8.0%, 1.6 to 6.6%, and 0.4 to 6.1% for Ba, Co, Fe and Ni, respectively. The method accuracy was assessed by recovery tests and comparison of the results obtained by the proposed extraction method with those obtained after acid digestion. Recoveries ranged from 93.5 for Ni to 104.5% for Co.