A new simpler and reliable method for determining mineral oil in sewage sludge: Influence of biogenic compounds for the quantitative analysis of C10-C40 hydrocarbons

Abstract

The characterization of organic contaminants in sewage sludge is a fundamental step to address the relevant most appropriate management practice. In this perspective, C10-C40 hydrocarbon content was considered in Italy a crucial parameter to be considered, in spite of its irrelevance in the literature. The very complex mixture of organic substances of both biogenic and anthropogenic origin the sludge is made up of makes sewage sludge a matrix of uniqueness nature, and the analytic determination of hydrocarbon content through conventional procedures may be subjected to overestimation. In this work, optimization of two conventional protocols for the determination of mineral oil (EN14039 and IRSA CNR gravimetric method) were run with attention to anthropogenic compounds potentially affecting the C10-C40 mineral hydrocarbons determination. Effects from the first manipulations of sewage sludge samples to extraction procedure and clean-up operations were investigated. A new simple procedure was set up and tested on 30 samples from different wastewater treatment plants (WWTPs). Through a simple extraction with hexane (12 mL per 2 g of dried sludge, acidified with HCl conc.) at room temperature for 2 h, followed by a clean-up on Florisil column (10 mL-2 g) a confident determination of C10-C40 were obtained with respect to conventional optimized procedures. Variability within the range 0.06-9.49% was calculated with respect to the average value determined using three different methods, with an average value of 2.48 ± 2.37%, demonstrating the robustness of the determination. Up to 3% of the total hydrocarbons were identified as naturally occurring, namely terpenes, squalenes and deoxygenized sterols, passed through the clean-up Florisil column. A significant incidence (up to 75%) of the final overall C10-C40 content was found to be related to the C10-C20 component, originally present in the commercial polyelectrolytes in emulsion, widely used for conditioning before mechanical dewatering.

Keywords: C10–C40 determination; EN14039; Hydrocarbons; Mineral oil; Sewage sludge.