Optimisation of the extraction of polycyclic aromatic hydrocarbons and their nitrated derivatives from diesel particulate matter using microwave-assisted extraction |
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Authors: | F Portet-Koltalo K Oukebdane F Dionnet P L Desbène |
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Institution: | (1) Laboratoire d’Analyse des Systèmes Organiques Complexes, UPRES 3233-IRCOF et IFRMP, Université de Rouen, 55 rue Saint Germain, 27000 Evreux, France;(2) CERTAM, Technopole du Madrillet, 1 rue Joseph Fourier, 76800 Saint Etienne du Rouvray, France |
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Abstract: | Pressurised microwave-assisted extraction was used to extract a complex mixture containing polycyclic aromatic hydrocarbons
(PAHs), nitrated PAHs and heavy n-alkanes from a particularly refractory carbonaceous material resulting from the combustion in a diesel engine. A second-order
central composite design was used to determine the optimal conditions of extraction in terms of time, temperature, volume
and nature of extracting solvent from spiked diesel soots. To begin, methylene chloride, tetrahydrofuran and chloroform were
tested for extracting the spiked diesel particulates; however, the nature of these solvents was not really an influential
factor. Volume was the most influential factor and was kept at a medium level to enhance the extraction of heavy PAHs without
introducing an important dilution factor. Temperature and time were not influential as main factors but interacted with the
other factors. Finally, high temperature and duration associated with a medium volume of methylene chloride were better for
the extractions. After this optimisation, five-ring and six-ring PAHs were nevertheless not satisfactorily desorbed. Other
solvents were therefore tested. Only aromatic ones, and particularly heterocyclic aromatic solvents, managed to desorb the
heaviest PAHs. Pyridine, with its both aromatic and its basic character, was the most successful solvent. Desorption was even
complete with an addition of 17% of diethylamine into pyridine. So, using MAE, we succeeded in extracting quantitatively,
from the spiked refractory diesel soot surface, two-ring to six-ring PAHs, heavy n-alkanes and short nitrated PAHs. However, heavy nitrated PAHs were better extracted with a small addition of acetic acid
(1%) into pyridine instead of a basic cosolvent. |
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Keywords: | Polycyclic aromatic hydrocarbons Diesel particulate matter Microwave-assisted extraction Factorial design |
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