Application of microwave energy to speed up the alkaline extraction of humic and fulvic acids from marine sediments Original Research Article

The feasibility of microwave energy to speed up the alkaline extraction of humic substances (humic acid, HA, and fulvic acid, FA) from marine sediments has been checked. Extractions were performed by using 20 mL of sodium hydroxide at 0.1 M (two repeated extractions) after an ultrasound-assisted acid pre-treatment of samples to remove the carbonate fraction (ultrasound power at 17 kHz, 10 mL of 6.0 M hydrochloric acid for 15 min). After separation of HA and FA fractions by acidifying with 6 M HCl, the FA fraction (supernatant) was purified by passing the solution through a column of Amberlite XAD-8. Both HA and FA extracts were measured by UV–visible spectrophotometry. All variables affecting the extraction process (sodium hydroxide concentration and volume, ramp and hold times, temperature and number of repeated extractions) have been screened by using a Plackett–Burman design (PBD) as multivariate approach. The variables temperature and number of repeated extractions were the most significant factors (P = 95%) affecting the extraction of both FA and HA from marine sediments. These two variables have led optimum values of 150 °C and two repeated extractions. The developed method has been found precise (R.S.D.s of 9% for HA and 12% for FA, for 11 determinations) and its results were comparable in terms of elemental (C, H and N) composition to those obtained after applying methods based on mechanical stirring and ultrasounds assisting. However, higher HA and FA concentrations than those obtained after conventional stirring and ultrasound irradiation were obtained when applying microwave energy. This means a higher efficiency of microwave energy than ultrasounds or mechanical stirring to extract HA and FA fractions from marine sediments. The method was finally applied to different surface marine sediments from the Ría de Arousa estuary.