Novel extraction induced by emulsion breaking as a tool for the determination of trace concentrations of Cu, Mn and Ni in biodiesel by electrothermal atomic absorption spectrometry

• Published in: Talanta (Oxford) 2013-12, Vol.117, p.32-38
• Main Authors: Pereira, Fernanda M., Zimpeck, Renata C., Brum, Daniel M., Cassella, Ricardo J.
• Format: Article
• Language: English
• Subjects: agitation; aqueous solutions; Atomic absorption analysis; atomic absorption spectrometry; Biodiesel; Breaking; Copper; emulsifiers; Emulsions; Extraction; Extraction induced by emulsion breaking; GFAAS; Manganese; Metals; mixing; Nickel; nitric acid; octoxynol; surfactants
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2013.08.042

This work proposes a novel method for the determination of trace concentrations of Cu, Mn and Ni in biodiesel samples by electrothermal atomic absorption spectrometry. In order to overcome problems related to the organic matrix in the direct introduction of the samples, a new extraction approach was investigated. The method was based on the extraction induced by emulsion breaking, in which metals were transferred from the biodiesel to an acid aqueous phase after formation and breaking of a water-in-oil emulsion prepared by mixing the biodiesel sample with an aqueous solution containing surfactant and nitric acid. Several parameters that could influence the performance of the system were evaluated. Quantitative extractions of the analytes were obtained when the extraction was performed using an emulsifier solution containing 2.1molL−1 of HNO3 and 7% m/v of Triton X-100. The extraction time had remarkable influence on the efficiency of the process, being necessary an agitation time of 60min to achieve maximum extraction. The limits of quantification were below 1µgL−1 for the three analytes under study. The accuracy of the method was tested by application of a recovery test (recovery percentages between 89% and 109% were observed) and by comparison with a well-established method, taken as reference. •A novel approach was developed for the determination of Cu, Mn and Ni in biodiesel.•The use of Triton X-100 and HNO3 in the extractant solution improved the process.•Extraction time had remarkable influence on the extraction efficiency.•Calibration could be performed with aqueous standard solutions.