Eduardo Pires Mateus

Although olive mill by-products and effluents (OMBP) are commonly regarded as potential environmental liabilities, they contain constituents that may offer recovery potential. This study proposes an integrated scheme combining dry (filtration, milling and sieving) and wet (distillation) fractionation, as well as thermochemical (carbonisation) processes, to stabilise and convert OMBP into solid and liquid fractions for potential applications. Mass and energy balances were established and the resulting products characterised. A preliminary technical and economic feasibility assessment was also conducted. The findings suggest that such an integrated valorisation framework could be implemented at local olive oil production sites. This could reduce resource losses (e.g., water and energy) and transport-related emissions while supporting local development opportunities.

Soil contamination by organic compounds such as pesticides poses a significant environmental challenge, requiring efficient and practical monitoring tools. Current analytical extraction methods such as QuEChERS, while sensitive and robust, often rely on costly and labor-intensive procedures involving sample collection, transport, and extraction. This study introduces a simpler and more cost-effective method for multiclass organic contaminant detection in soil using low-cost semi-disposable solid-phase microextraction (SPME) fibers for direct, non-invasive field extraction and portable sampling. The method consists of conditioning the fibers, after which they are directly inserted into the wet soil (water is added previously). After the extraction time, they are inserted into 120 µL of ethanol for retro-extraction. Finally, this extract is combined with an analyte protectant solution and injected into a GC-MS/MS system. The method was optimized for soil water content and extraction time, using two different soils with different textures and composition. The results show that it is not possible to reliably distinguish between close analyte concentrations (25, 50 and 100 µg/kg), meaning the method cannot be used quantitatively. Nevertheless, detection limits were in the range of 1–20 µg/kg while assuring (nearly) unbiased detection. Simplified and cheaper sample transport for analysis, following a mailing-kit concept, appears operationally feasible, as there were no differences between samples retro-extracted right after extraction and only 26 hours later (p = 0.05), assuming enclosed storage. Thus, the very small and light fibers can be transported to the lab themselves, rather than the liquid extract or a solid sample (as with traditional techniques). This technique presents a viable option for preliminary field monitoring and fast laboratory screening, providing a proxy for soil contamination levels and supporting informed decisions on subsequent targeted quantitative analyses. Future adaptation via e.g., DART-MS integration, may enhance throughput and field readiness with potential for commercial development in environmental diagnostics.

A new method is presented for the simultaneous determination of 13 multiclass pesticides along with glyphosate. The multiclass pesticides were extracted by creating a soil slurry with 2% ethanol in water (v/v), and then, applying direct-immersion solid-phase microextraction (DI-SPME) with a new type of semi-disposable SPME fiber configuration called LC-Tips. The fibers were then retroextracted to ethanol, and aqueous ammonia was added to the slurry to extract glyphosate. Derivatization of the glyphosate extract was accomplished with a mixture of trifluoroacetic anhydride and trifluoroethanol, after which the reaction mixture was dried and resuspended with the SPME ethanol extract. To this, a mixture of analyte protectants was added, and it was analyzed by GC-MS/MS in multiple-reaction-monitoring mode. All analytes showed a coefficient of determination greater than 0.95 in the 0.1–100 µg/kg calibrated range, and the limits of detection were between 0.1 and 1 µg/kg, except for glyphosate, which was 0.01 µg/kg. The method shows relatively high replicate relative standard deviation (as much as 37% for five extractions at 20 µg/kg), but the isotopically labeled internal standard was effective at mitigating this effect for some analytes.

Summary: Drought affects the complex interactions between Norway spruce, the bark beetle Ips typographus and associated microorganisms. We investigated the interplay of tree water status, defense and carbohydrate reserves with the incidence of bark beetle attack and infection of associated fungi in mature spruce trees. We installed roofs to induce a 2‐yr moderate drought in a managed spruce stand to examine a maximum of 10 roof and 10 control trees for resin flow (RF), predawn twig water potentials, terpene, phenolic and carbohydrate bark concentrations, and bark beetle borings in field bioassays before and after inoculation with Endoconidiophora polonica and Grosmannia penicillata. Drought‐stressed trees showed more attacks and significantly longer fungal lesions than controls, but maintained terpene resin defenses at predrought levels. Reduced RF and lower mono‐ and diterpene, but not phenolic concentrations were linked with increased host selection. Bark beetle attack and fungi stimulated chemical defenses, yet G. penicillata reduced phenolic and carbohydrate contents. Chemical defenses did not decrease under mild, prolonged drought in our simulated small‐scale biotic infestations. However, during natural mass attacks, reductions in carbon fixation under drought, in combination with fungal consumption of carbohydrates, may deplete tree defenses and facilitate colonization by I. typographus.

Multidimensional gas chromatography is, presently, an established and powerful analytical tool, due to higher resolving power than the classical 1D chromatographic approaches. Applied to multiple areas, it allows to isolate, detect and identify a larger number of compounds present in complex matrices, even in trace amounts. Research was conducted to determine which compounds, emitted by host plants of the eucalyptus weevil, Gonipterus platensis, might mediate host selection behavior. The identification of a pheromone blend of G. platensis is presented, revealing to be more attractive to weevils of both sexes, than the individual compounds. The volatile organic compounds (VOCs) were collected by headspace solid phase microextraction (HS-SPME), MonoTrap^TM disks, and simultaneous distillation-extraction (SDE). Combining one dimensional (1D) and two-dimensional (2D) chromatographic systems—comprehensive and heart-cut two-dimensional gas chromatography (GC×GC and H/C-MD-GC, respectively) with mass spectrometry (MS) and electroantennographic (EAD) detection, enabled the selection and identification of pertinent semiochemicals which were detected by the insect antennal olfactory system. The behavioral effect of a selected blend of compounds was assessed in a two-arm olfactometer with ten parallel walking chambers, coupled to video tracking and data analysis software. An active blend, composed by cis and trans-verbenol, verbenene, myrtenol and trans-pinocarveol was achieved.

Currently, the development of new sustainable technologies to recover raw materials from secondary resources has shown a lack of available data on the processes and supplies involved, as well as their environmental impacts. The present research has conducted a life cycle assessment of electrodialytic (ED) technologies to improve critical raw materials recovery in the Portuguese mining industry. To critically appraise the activities from the mining sector and gather data on technical and environmental issues, three waste management scenarios were considered: (1) ED treatment with a deep eutectic solvent as an adjuvant; (2) ED treatment with simultaneous H₂ recovery; and (3) ED treatment with sodium chloride as an enhancement. The data presented were based on global databases, technical reports from official sources, and peer-reviewed published experimental outcomes. The estimated results indicated that one of the constraints in applying ED technologies is energy consumption and thus the impacts are highly dependent on energy source choices. On the other hand, as a consequence of the H₂ inherently produced by ED technologies, there is a direct potential for energy recovery. Therefore, considering an upscale approach of the ED reactor based on bench scale experimental results, the H₂ could be reused in the ED facility or stored. Additionally, according to experimental data, 22% of the tungsten from the fine mine tailings could be recovered. Finally, the possibility to remove 63% of arsenic from mine tailings could decrease contamination risks while creating additional marketable co-products.

The eucalyptus weevil, Gonipterus spp. Schoenherr, 1833 (Coleoptera, Curculionidae) is considered a major pest of eucalyptus plantations. In regions where control is achieved, success is usually brought by the action of the solitary egg parasitoid Anaphes nitens (Girault, 1928) (Hymenoptera, Mymaridae). Research was conducted to ascertain which cues might mediate female wasp host location and selection. In Petri dish arenas, females were attracted to Gonipterus platensis Marelli, 1927 egg capsules, to G. platensis mated female faeces and to leaves of Eucalyptus globulus Labillardière, 1799. Gas chromatography–mass spectrometry electroantennographic detection analysis was conducted using extracts obtained from leaves of E. globulus, from G. platensis egg capsules, as well as from adults of both sexes and their faeces, in order to detect and identify compounds perceived by the wasp's olfactory system. The parasitoids were shown to detect a wide range of compounds emitted by each one of these sources, and for 31 compounds, antennal response was confirmed by dose‐response tests. Further behavioural trials were conducted in Petri dishes in order to decode the effect, on parasitoid behaviour, of selected compounds emitted by E. globulus and of the pheromones, emitted by the weevils on parasitoid behaviour. Attraction was observed to two compounds emitted by E. globulus, namely 1,8‐cineole and γ‐terpinene, and to the main component of the male sex/aggregation pheromone, cis‐verbenol. To our knowledge, this is the first report of attraction of a parasitoid from the family Mymaridae to a component of its host's sexual/aggregation pheromone. Similarly, to other egg parasitoid species, A. nitens females are likely to use the host plant volatiles as long‐range host location cues and to adopt the ‘infochemical detour’ strategy in order to get in the vicinity of their hosts.