Multivariate optimization of the determination of zinc in diesel oil employing a novel extraction strategy based on emulsion breaking

This paper describes the extraction/pre-concentration of Zn from diesel oil and its determination by Flame Atomic Absorption Spectrometry (FAAS), proposed as a novel approach for these kinds of analyses and the multivariate optimization of the proposed procedure. The extraction of Zn is based on the emulsification of an aqueous solution containing Triton X-114 and HNO₃ with diesel oil samples followed by breaking of the emulsion by heating. The aqueous phase obtained after the emulsion breaking was collected and used for Zn quantification by FAAS. The methodology was optimized using a Doehlert design and the system variables were the concentrations of surfactant and HNO₃ in the solution employed in the emulsification and the temperature used in the emulsion breaking. The ratio between absorbance and the time required to break the emulsions was taken as response. Two sets of experiments, using different emulsifier agents, were run: the first one using Triton X-100 and the second one using Triton X-114. At optimized conditions, the emulsions were prepared by mixing 10 mL of diesel oil with 2 mL of a solution containing 5% w/v of Triton X-114 and 15% v/v of HNO₃ and broken by heating at 80 °C. The proposed analytical procedure was applied in the analysis of six real samples of diesel oil and a recovery test was carried out by spiking the samples with known amounts of Zn (25 and 50 μg L⁻¹), added as organometallic oiled standard. Recovery percentages achieved in this test were between 92 and 109%.