In order to determine sterols and stanols in freshwater sediments to reconstruct the past presence of humans and pastoral animals, we developed an analytical method based on pressurised liquid extraction (PLE), clean-up performed using solid phase extraction (SPE) and sterol determination using gas chromatography-mass spectrometry (GC-MS) analysis. PLE extraction conditions were optimised using dichloromethane (DCM) and DCM/methanol mixtures. Clean-up was performed with 2 g silica SPE cartridges, and the concentrated extracts were eluted with 70 mL DCM. Extraction yield was evaluated using an in-house reference material spiked with (13)C-labelled cholesterol and aged for 10 days. In comparison with pre-extraction, where the sediment is extracted and then spiked with a known analyte concentration, this approach preserves the original composition of the sediment. DCM and DCM/methanol mixtures resulted in high extraction yields ranging from 86 to 92 % with good reproducibility (relative standard deviation (RSD) 5-8 %). PLE extraction yields obtained with DCM as the extracting solvent were about 1.5 times higher than extractions using an ultrasonic bath. The solvent extraction mixture and matrix composition strongly affected the solvent extraction composition where higher overall recoveries (70-80 %) for each compound were obtained with DCM. The extraction mixture and matrix composition also affected the analyte concentrations, resulting in a method precision ranging from 1 to 18 %. Diatomaceous earth spiked with 10 to 100 ng of sterols, and environmental samples fortified with suitable amounts of sterols provided apparent recovery values ranging from 90 to 110 %. We applied the method to environmental samples both close to and upstream from sewage discharge zones, resulting in substantially higher faecal sterol (FeSt) concentrations near the sewage. In addition, we also applied the method to a 37-cm freshwater sediment core in order to evaluate its applicability for obtaining vertical sterol profiles.
Open burning of agricultural waste is still a common practice as it is a rapid method for waste disposal, although natural biomass, including agriculture residues, can be exploited as a renewable energy source. We assessed the viability and sustainability of using vineyard pruning residues, as wood chips, for energy conversion. Wood chips, obtained from vineyards in the Prosecco DOCG region (Italy), were characterized in terms of chemical composition, calorific value, ash content and humidity. Combustion tests were performed in a medium-size biomass boiler (maximum power 500 kW) to assess the viability of the approach in terms of sustainable steady-state combustion. Primary emissions of both macro-and micro-pollutants were measured to assess the environmental impact.An analytical method was purposely developed for the determination of polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) in three matrices: fly ashes, condensate and gas. The results showed that vineyard pruning residues can be used for energy conversion in medium-and large-scale biomass boilers. Primary emissions of measured pollutants were all below limit values set by current European legislation except for particulate matter, for which current available abatement technologies are required to contain emissions, thus making the use of vineyard pruning residues unsuitable for combustion in domestic appliances where such technologies are not installed. Bottom ashes produced during combustion were also characterized to assess whether they can be recycled in the vineyard as soil amendments/fertilizers. Copper content in combustion ashes exceeded limit values for ashes to be used as fertilizers in agricultural fields for some European countries but not for others, indicating that ashes may need to be disposed as waste.
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