Rapid and greener vortex-assisted deep eutectic solvent-based dispersive liquid-liquid microextraction for spectroscopic determination of Hg in fuels
Year: 2025
Type: article
Abstract: • Rapid and greener microextraction of Hg in fuels was successfully developed. • Confirmed optimum conditions were 4.5 pH, 5 mins extraction time, 164 µL volume and 665 µL disperser solvent. • The VA-DLLME was precise (2.3 %), rapid (5 mins) and accurate (99.9 %). • The AGRREEprep assessment tool confirmed the greenness of the proposed VA-DLLME. • The Hg concentrations obtained in real fuels were < 1 µg/g which implied no risk. Mercury is considered a global pollutant and occurs naturally at trace levels in fuel oils such as crude oil and its derivatives. The former is released into the environment during the processing of these energy sources. Due to its high toxicity, there is a global concern regarding human exposure to this element. Three distinct deep eutectic solvents (choline chloride + ethylene glycol, choline chloride + levulinic acid, and betaine + levulinic acid) were synthesized and characterized using Fourier Transform infra-red spectroscopy (FT-IR), Thermogravimetric analysis (TGA), and 13 C nuclear magnetic resonance (NMR) for the preconcentration of Hg in fuel oils prior to quantification using inductively coupled plasma-optical emission spectroscopy (ICP-OES). Multivariate optimization tools were used for the optimization of the vortex-assisted deep eutectic solvent based dispersive liquid-liquid microextraction (VA-DES-DLLME) procedure. The optimum conditions for the newly developed method were 4.5 pH, 5 mins extraction time, 164 µL extractant volume and 665 µL disperser solvent. The optimized method was validated using NIST SRM 2778 with certified mercury concentration of 38.98 µg/kg ± 1.10 µg/kg. The method provided enrichment factor (EF), precision (%RSD), and limit of detection (LOD) of 234, 2.3 %, and 0.025 µg/L, respectively. Additionally, the newly developed method demonstrated good accuracy 97–99.9 %. The newly developed method was successfully applied in real crude oil, kerosene, diesel, and gasoline. The concentrations obtained were 0.390 ± 0.01–0.510 ± 0.09 µg/g for crude oil samples, 0.308 ± 0.05–0.402 ± 0.05 µg/g for gasoline samples, 0.370 ± 0.35–0.510 ± 0.080 µg/g for diesel oil samples and 0.09 ± 0.09–0.098 ± 0.02 µg/g for kerosene samples. The environmental impact of the newly developed method was assessed using AGREEprep software and a score of 0.72 was obtained.
Source: Green Analytical Chemistry
Institutions: University of South Africa, University of Johannesburg
Language: English
Subfield: Analytical Chemistry
Field: Chemistry
Domain: Physical Sciences
Open Access status: gold
Estimated APC paid: $1,550
Funder: National Research Foundation
Award: G127616651
OpenAlex ID: W4407874175