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This paper reports the development of a method based on the extraction induced by emulsion breaking (EIEB) for the determination of Cr, Cu and Mn in asphalt by high-resolution continuum source atomic absorption spectrometry. In optimized conditions, the extraction efficiency ranged from 88.6 for Cu to 104.5% for Mn. Measurements were carried out at the primary lines of the three analytes. The limits of detection were 0.02 µg g-1 for Cr, 0.01 µg g-1 for Cu and 7.11 ng g-1 for Mn. The precision, expressed as the relative standard deviation, ranged from 1.0 for Cu to 9.1% for Cr. The performance of the proposed method was compared to previously reported sample preparation procedures, including microwave-assisted acid digestion (MW-AD), ultrasound-assisted acid extraction (USE), emulsification (E), and direct dilution in organic solvent (DD). The parameters evaluated were matrix effects, limits of detection and quantification, characteristic mass, precision, accuracy, sample stability and applicability for routine analysis. The methods most suitable for Cu determination were EIEB, MW-AD, USE and E. For Cr and Mn, the best results were obtained by EIEB, MW-AD and DD procedures.
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Hidrocarburos , Emulsiones , Espectrofotometría AtómicaRESUMEN
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.
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Hidrocarburos , Azufre , Cromatografía Líquida de Alta Presión , Cromatografía LiquidaRESUMEN
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.
Asunto(s)
Bario/análisis , Cobalto/análisis , Hierro/análisis , Níquel/análisis , Nueces/química , Espectrofotometría Atómica/métodos , Emulsiones , Reproducibilidad de los Resultados , AguaRESUMEN
The interaction between aluminium and cysteine and cystine was evaluated by means of ion-exchange experiments and potentiometry. Ion-exchange experiments included other ligands with affinity for aluminium and two kinds of resins, either a Na+ -form or an Al3+ -form exchanger. The ability of the ligands to keep aluminium in solution in the presence of the Na+ exchanger or to withdraw it from the Al3+ -form resin was evaluated. Aluminium quantification was carried out by either graphite-furnace or flame atomic absorption spectrometry. Aluminium extraction isotherms were linearised using the Scatchard plot, and stability constants were obtained from the curves' slopes. The experiments showed that the ability of the ligands to withdraw aluminium from the Al3+ -form resin increased following the order cysteine < oxalate < citrate = cystine < nitrilotriacetic acid < ethylenediaminetetraacetic acid. Potentiometric titrations, carried out in aqueous solution with constant ionic strength and temperature, showed that the predominant species in solution have a metal-ligand proportion of 1:1 for both amino acids. The main species are Al(OH)3L, with log K of 6.2 for cysteine, and AlL and Al(OH)L, with log K of 10.3 and 1.7, respectively, for cystine. Stability constants obtained from the Scatchard plots showed a linear correlation with the stability constants obtained by potentiometry for cystine and cysteine in this work and those collected from the literature for the other ligands. These results show that cysteine and cystine extract and maintain aluminium in solution, which may explain elevated concentrations of aluminium in parenteral nutrition solutions containing these amino acids.