Analysis of tert-butyldimethylsilyl derivatives in heavy gas oil from brazilian naphthenic acids by gas chromatography coupled to mass spectrometry with electron impact ionization

Naphthenic acids, CnH2n+ZO2, are a complex mixture of alkyl-substituted acyclic and cycle-aliphatic carboxylic acids. The content of naphthenic acids and their derivatives in crude oils is very small, which hinders their extraction from matrixes of wide and varied composition. In this work, liquid-liquid extraction, followed by solid phase extraction with an ion exchange resin (Amberlyst A-27) and ultrasound desorption were used to isolate the acid fraction from heavy gas oil of Marlim petroleum (Campos, Rio de Janeiro, Brazil). The analysis was accomplished through gas chromatography coupled to mass spectrometry with electron impact ionization, after derivatization with N-(tert-butyldimethyslsilyl)trifluoracetamide (MTBDMSTFA). The results indicate the presence of carboxylic acids belonging to families of alicyclic and naphthenic compounds which contain up to four rings in the molecule. (c) 2005 Elsevier B.V. All rights reserved.