Abstract

An "oil in water" formulation was optimized to determine chromium in heavy crude oil (HCO) and bitumen-in-water emulsion (Orimulsion-400®) samples by transversally heated electrothermal atomic absorption spectrometry (TH-ET AAS) using Zeeman effect background correction. The optimum proportion of the oil-water mixture ratio was 7:3 v/v (70 ml of oil as the internal phase) with a non-ionic surfactant concentration (lntan-l00) in the emulsion of 0.2% w/w. Chromium was determined in different crude oil samples after dilution of the emulsions 1:9 v/v with a 0.2°/, w/w solution of surfactant in order to further reduce the viscosity from 100 to 1.6 cP and at the same time to bring the concentration of chromium within the working range of the ET AAS technique. The calibration graph was linear from 1.7 to 100 gg Cr 1- t. The sensitivity was of 0.0069 s 1 µg- ', the characteristic mass (mo) was of 5.7 pg per 0.0044 s and the detection limit (36) was of 0.52 pg 1-'. The relative standard deviation of the method, evaluated by replicate analyses of three crude oil samples varied in all cases between 1.5 and 2.6%. Recovery studies were performed on four Venezuelan crude oils, and the average chromium recovery values varied between 95.9-104.8, 90.6-107.6, 95.6-104.0 and 98.8-103.9% for the Cerro Negro, Crudo Hamaca and Boscan crude oils and for the Orimulsion®-400, respectively. The results obtained in this work for the Cerro Negro, Crudo Hamaca and Boscan crude oils and for the Orimulsion('~-400 following the proposed procedure were of 0.448±0.008, 0.338±0.004 0.524±0.021 and 0.174±0.008 mg Cr 1-t, respectively, which were in good agreement with the values obtained by a tedious recommended standard procedure (respectively: 0.470±0.05, 0.335±0.080, 0.570±0.021 and 0.173±0.009 mg Cr 1-t). CC) 2003 Elsevier B.V. All rights reserved.

Artículo publicado en: Talanta 61 (2003) 353-361