Nanoplastics (NPs) are considered emerging pollutants, namely unregulated contaminants whose toxic effect on humans and the environment has been demonstrated or suspected. They are the result of the physical fragmentation of the plastics that over time reach smaller dimensions (<100 nm). The issues related to the characterization and quantification of NPs in the environmental matrices are mainly related to the infinitepsimal size, to the fact that they are found in bulk, and to the different physico-chemical forms in which the same polymer can evolve over time by degradation. To deal with the study of a new class of pollutants it is necessary to assess the entire analytical method, carefully considering every single step (sampling, cleanup, qualitative, and quantitative analysis) starting from the validation method in the laboratory. This paper reviews the analytical method steps, focusing on the first ones, which the current literature often underestimates: laboratory tests, sampling, and sample processing; in fact, most errors and the quality of the analyses often depend on them. In addition, all newly introduced sample processing methods were examined.

Agricultural activities lead to the production of large quantities of pruning and residual biomass, the correct disposal of which is a topic of great interest. Unfortunately, although it is an environmentally unacceptable practice, disposal often takes place with uncontrolled combustion in field (open burning). Disposal using biomass boilers produces energy from controlled combustion and the use of abatement systems reduces emissions that are inevitably generated in the combustion processes of solid fuel (CO, CO₂, NOx, SO₂, PM, etc.). Among the pollutants produced in combustion processes, Persistent Organic Pollutants (POPs) are one of the most relevant groups of chemicals that must be monitored for their effect on human health and the environment. This paper reports the data obtained for the emissive characterization of POPs of three different wood biomass prunings (Olive, Citrus and Grapevine) focusing on VOCs, PAHs, PCBs, PCDD/Fs. Emissions samplings were performed at the stack during combustion in a 30 kW_th boiler equipped with a multicyclone filter bag for PM abatement in an isokinetic mode in accordance with the CEN and ISO standards methods. Through this work, a complete emission profile of VOCs, PAHs, PCBs, and PCDD/Fs of three different biomass types is provided for the first time, showing that the use of biomass boilers produces quantities of pollutants below the regulatory limits and still lower than those produced by open burning phenomena. Citrus has shown, regarding the other two essences, elevated concentrations in terms of Σ PAH = 174.247 ng/m³, while Olive gave higher results in terms of PCBs and PCDD/Fs (respectively, 39.769 and 3390.63 TEQ pg/Nm³). This is probably due to the high concentration of iron in this biomass (711.44 mg/kg), which during combustion is a catalyst (together with copper) of PCDD/Fs.

Active carbon-based sorbents are well known and are used in analytical chemistry. Activated carbon fibers (ACFs) are mainly used as abatement systems in industrial emission pollution control. The objective of this study was to extend the use of ACFs in analytical chemistry for the analysis of polychlorodibenzo-p-dioxins (PCDDs), polychlorodibenzofurans (PCDFs), dioxin-like polychlorobiphenyls (PCBs), and chlorobenzenes (CBs). For this purpose, the extraction efficiency was evaluated based on the QA/QC criteria defined by EPA/ISO reference methods on ¹³C-standards recovery rates. The procedures tested were ultrasonic assisted extraction (UAE), Soxhlet extraction (SE), accelerated solvent extraction (ASE), and microwave-assisted extraction (MAE). Each experiment was performed in triplicate to ensure the repeatability of the results, and a second extraction assessed the complete extraction. The comparison of the results of each set of experiments with the minimum requirements of the reference methods for each class of compounds led to SE being chosen as the best technique. SE with toluene resulted in a reduction of time and costs and with respect to the other investigated techniques. The present work demonstrated that ACFs can be used in environmental fields means of both prevention and control (exploiting the adsorbent characteristics) and for analytical purposes (exploiting the desorption) for the described chlorinated classes of pollutants.

Among all the emerging contaminants, fragrances are gaining more relevance for their proven allergenic and, in some cases, endocrine-disrupting properties. To date, little information exists on their concentration in the air. This study aims to fill this gap by developing a method for the determination of semivolatile fragrances in the indoor gaseous phase with sampling protocols usually adopted for the collection of atmospheric particulate matter (sampling time 24 h, flow rate 10 L min⁻¹) and instrumental analysis by gas chromatography coupled with mass spectrometry. The method was developed on 66 analytes and tested at three concentration levels: 20 compounds showed analytical recoveries ≥72% with percentage standard deviations always better than 20%. For most compounds, negligible sampling breakthroughs were observed. The method was then applied to real samples collected in a coffee bar and in a private house. Considering the fragrances for which the method has shown good effectiveness, the highest concentrations were observed for carvone in the coffee bar (349 ng m⁻³) and camphor in the house (157 ng m⁻³). As concerns certain or suspected endocrine disruptors, lilyal and galaxolide were detected at both sites, α-isomethylionone was the second most concentrated compound in the house (63.2 ng m⁻³), musk xylene and musk ketone were present at lower concentration (≈ 1 or 2 ng m⁻³).