How to overcome the difficulty in assaying Ni in biodiesel samples? Extraction induced by microemulsion breaking and square wave adsorptive stripping voltammetry could be the answer

Talanta. 2024 May 15:272:125776. doi: 10.1016/j.talanta.2024.125776. Epub 2024 Feb 15.

Abstract

Herein, a simple, green, and relatively inexpensive approach to determine nickel (Ni) in biodiesel samples by square wave adsorptive cathodic stripping voltammetry (SWAdCSV) is presented. A method based on the accumulation of Ni as Ni(II)-dimethylglyoxime (Ni(II)(HDMG)2) on the glassy carbon electrode was carried out in a solution containing the aqueous phase extract (APhEx) obtained from an extraction induced by microemulsion breaking (EIMB), which was achieved by adding a few microliters of ultrapure water to a microemulsion composed of biodiesel, n-propanol and a diluted HNO3 solution. The LOD and LOQ were 0.2 μg L-1 and 0.8 μg L-1, respectively, and the accuracy was evaluated by recovery assays of spiked samples and by analyzing a standard reference material. Results obtained from a comparative method (HR-CS GF AAS) were also used for this evaluation. The method was applied to biodiesel samples produced from different feedstocks. To the best of the authors knowledge, it is the first time that: 1) Ni in biodiesel is determined by a voltammetric method; 2) EIMB is applied to extract Ni from this matrix and 3) this type of sample preparation method is used with adsorptive stripping voltammetry.

Keywords: Adsorptive stripping voltammetry (AdSV); Biofuel; Extraction induced by micromulsion breaking (EIMB); Nickel.