Journal of the Brazilian Chemical Society
Print version ISSN 0103-5053
FERREIRA, Vânia R. et al. Optimization of an analytical protocol for the extraction, fractionation and determination of aromatic and aliphatic hydrocarbons in sediments. J. Braz. Chem. Soc. [online]. 2012, vol.23, n.8, pp. 1460-1468. Epub Aug 07, 2012. ISSN 0103-5053. http://dx.doi.org/10.1590/S0103-50532012005000010.
The main steps involved in the determination of aliphatic and aromatic hydrocarbons in sediments were evaluated in this work. In the extraction, factors such as the cooling system, time and solvent were evaluated. During the extraction and concentration, steps aspects such as time, extraction solvent and cooling system were evaluated. In the cleanup different solvents and elution mixtures were studied. The results were considered satisfactory (70-120%). Linearity and limits of detection and quantification were studied by means of calibration curves (R > 0.90) and the results demonstrated high sensitivity of the method. Precision and accuracy were studied by recovery tests using a certified reference material and sodium sulfate. In recovery tests, the standard deviations were below 20%, with percent recoveries for aliphatic and aromatics ranging from 59 to 105% and 55 to 113%, respectively. For the reference sediment, the standard deviations were lower than the certified values, with satisfactory recovery values. The present work provided a way of improving an already established method with high analytical reliability.
Keywords : hydrocarbons; Soxhlet extraction; sediment; gas chromatography; validation.