A simple electroanalytical procedure for the determination of calcium in biodiesel

Voltammograms showing the qualitative reactivity for the Ca–EDTA system in pH9.4 (ammonium buffer 0.01molL−1) on the glassy carbon electrode surface (υ=100mV/s; (a) bare electrode; (b) 4×10−3molL−1EDTA on the CGE; (c)=(b) after addition of 1×10−4molL−1Ca2+. [Display omitted] •Alternative analytical...

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Bibliographic Details
Published in:Fuel (Guildford) 2014-01, Vol.115, p.658-665
Main Authors: Almeida, Joseany M.S., Dornellas, Rafael M., Yotsumoto-Neto, Sakae, Ghisi, Mirela, Furtado, Jethânia G.C., Marques, Edmar P., Aucélio, Ricardo Q., Marques, Aldaléa L.B.
Format: Article
Language:English
Subjects:
Applied sciences
Biodiesel
Calcium
Deposition
EDTA
Electrodes
Energy
Energy. Thermal use of fuels
Exact sciences and technology
Fuels
Glassy carbon electrode
Microwaves
Optimization
Reproducibility
Square-wave anodic stripping voltammetry
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Summary:Voltammograms showing the qualitative reactivity for the Ca–EDTA system in pH9.4 (ammonium buffer 0.01molL−1) on the glassy carbon electrode surface (υ=100mV/s; (a) bare electrode; (b) 4×10−3molL−1EDTA on the CGE; (c)=(b) after addition of 1×10−4molL−1Ca2+. [Display omitted] •Alternative analytical procedure for the determination ofcalcium in biodiesel.•Quality of biodiesel.•Interference of magnesium in the determination of calcium.•Calcium–EDTA complex. An alternative method is proposed for the determination of calcium in biodiesel samples using square-wave voltammetry and a glassy carbon electrode in a solution containing EDTA. A microwave assisted acid digestion of the biodiesel samples was carried out before analysis. Experimental parameters such as deposition potential, deposition time, frequency, amplitude, step potential, were optimized for the purpose of determination of trace calcium ion in 1×104μmolL−1 ammonium buffer solution (pH9.4) in the presence of 400μmolL−1 of EDTA. Under optimal conditions, the limit of detection was 1.6×10−3μmolL−1 for Ca2+ with a 2min preconcentration time. In addition, the EDTA/GCE displayed good reproducibility (CV maximum of 0.70%) and accuracy (recovery around 102%) making it suitable for the determination of Ca2+ in real biodiesel sample.
ISSN:0016-2361
1873-7153
DOI:10.1016/j.fuel.2013.07.088