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Abstract Salicylic and acetylsalicylic acids and ethacridine have complementary bioactive properties. They can be combined to obtain double-drug multicomponent crystals. Their reactivity in different environments was explored to obtain the possible compounds, stable at different hydration degrees. Solution, liquid-assisted grinding, and dry preparation approaches were applied to the couples of reactants in different stoichiometric ratios. Four compounds were obtained, and three out of them were stable and reproducible enough to determine their structures using SCXRD or PXRD methods. When coupled to ethacridine, salicylic acid gave two stable structures (1 and 3, both showing 1:1 ratio but different hydration degree) and a metastable one (5), while acetylsalicylic acid only one structure from solution (2 in 1:1 ratio), while LAG caused hydrolysis and formation of the same compound obtained by LAG of ethacridine with salicylic acid. While solution precipitation gave dihydrated (1) or monohydrated (2) structures with low yields, LAG of salicylic acid and ethacridine allowed obtaining an anhydrous salt complex (3) with a yield close to 1. The structures obtained by solution crystallizations maximize π(acridine)–π(acridine) contacts with a less compact packing, while the LAG structure is more compact with a packing driven by hydrogen bonds. For all compounds, NMR, ATR-FTIR, and Hirshfeld surface analysis and energy framework calculations were performed.

Microplastic pollution is a pervasive global issue affecting various ecosystems. Despite the escalating production and well-documented contamination in both aquatic and terrestrial environments, the research focused on airborne microplastics and their interaction with terrestrial birds remains limited. In this study, we collected fecal sacs from Common swifts (Apus apus) to investigate their diet and to evaluate the potential ingestion of microplastics by both adults and nestlings. The diet was mainly composed of Hymenoptera and Coleoptera and did not differ among sexes and age classes. The 33% of nestlings’ and 52% of adults’ fecal sacs contained anthropogenic items, the totality of which was in the shape form of fibers. The 19.4% of the anthropogenic items were chemically characterized as microplastics, either polyethylene terephthalate (PET; two microfibers) or cellophane (four microfibers). Airborne anthropogenic items, including microplastic, might be passively ingested during the Common swift aerial feeding. In addition, our findings suggest that these ingested microparticles have the potential to be transferred to the offspring through food. While further research is essential to elucidate the pathways of microplastic ingestion, our results reinforce the evidence of the transfer of anthropogenic items from the atmosphere to the biota.

The implementation of recycling techniques represents a potential solution to the plastic pollution issue. To date, only a limited number of plastic polymers can be efficiently recycled. In the Italian plastic waste stream, the residual, non-homogeneous fraction is called ‘Plasmix’ and is intended for low-value uses. However, Plasmix can be used to create new materials through mechanical recycling, which need to be tested for their eco-safety. This study aimed to investigate the potential toxicity of two amounts (0.1% and 1% MPs in soil weight) of microplastics (MPs) made of naïve and additivated Plasmix-based materials (Px and APx, respectively) on the earthworm Eisenia foetida. Changes in oxidative status and oxidative damage, survival, gross growth rate and reproductive output were considered as endpoints. Although earthworms ingested both MP types, earthworms did not suffer an oxidative stress condition or growth and reproductive impairments. The results suggested that exposure to low amounts of both MPs can be considered as safe for earthworms. However, further studies testing a higher amount or longer exposure time on different model species are necessary to complete the environmental risk assessment of these new materials.

The liquid-assisted grinding (LAG) approach was exploited to efficiently produce a new salt cocrystal with a minimum expenditure of reagents and energy, with possible application in the pharmaceutical field. LAG was applied to the acridine/diclofenac couple, and a new cocrystal was obtained with a 1:1 ratio of reagents and its structure resolved by X-ray powder diffraction (XRPD). The XRPD analysis confirmed that the yield is higher than 90% and the limited use of solvents and the absence of waste generally makes the synthesis very efficient and with the minimum possible environmental impact. The crystal structure of the title compound was compared to a previously solved 1:2 cocrystal, also with the aid of Hirshfeld’s surface analysis and calculations of the energy framework. The packing of the 1:1 structure is stabilized by a strong H-bond and partial π⋯π-stacking interactions. It differs considerably from that of the previously identified cocrystal, in which two strong hydrogen bonds and a perfect interlocking of the molecules thanks to the the π⋯π stacking induce a much higher stability, as confirmed by energy framework calculations. DSC analysis confirmed its purity and a melting point at 140 °C, which is different from those of the two reactants.

Organo-modified layered materials characterization poses challenges due to their complexity and how other aspects such as contamination, preparation methods and degree of intercalation influence the properties of these materials. Consequently, a deep understanding of their interlayer organization is of utmost importance to optimize their applications. These materials can in fact improve the stability of photoactive molecules through intercalation, avoiding the quenching of their emission at the solid state, to facilitate their use in sensors or other devices. Two synthetic methods for the preparation of saponites with a cationic surfactant (CTABr) and a neutral chromophore (Fluorene) were tested and the obtained products were initially characterized with several complementary techniques (XRPD, SEM, TGA, IR, UV-Vis, Fluorescence and Raman spectroscopy), but a clear understanding of the organization of the guest molecules in the material could not be obtained by these techniques alone. This information was obtained only by thermogravimetry coupled with gas chromatography and mass spectroscopy (TGA-GC-MS) which allowed identifying the species present in the sample and the kind of interaction with the host by distinguishing between intercalated and adsorbed on the surface.

New very fast and efficient detectors, installed both on laboratory instruments and synchrotron facilities, allow the monitoring of solid-state reactions from subsecond to minute scales with the production of large amounts of data. Traditional “one-by-one” pattern refinement needs complementary approaches, useful to handle hundreds to thousands of X-ray patterns. Principal-component analysis (PCA) has been applied to these fields in the last few years to speed up analysis with the specific goals of assessing data quality, identifying patterns where a reaction occurs, and extracting the kinetics. PCA is applied to the adsorption/desorption of Xe and CO2 within a Y zeolite. CO2 sequestration is a key issue in relation to climate change, while Xe is a critical raw material, and its purification is an important topic for the industry. At first, results were compared to traditional sequential Rietveld refinement. CO2-Y data were also compared with in situ single crystal data to investigate the different potentialities of PCA in the two cases. Two CO2 adsorption sites were confirmed, while three Xe sites were identified. CO2 showed a more linear adsorption trend with decreasing temperature, while Xe showed a more sigmoidal-like trend. Xe only showed site-dependent behavior in adsorption. Finally, PCA and correlation analysis, applied to analyze the parameters obtained from Rietveld refinement, highlighted finer details: in particular, this approach showed that the Y zeolite framework responded differently to CO2 and Xe adsorption.

Low-ordered carbon/layered double hydroxide (LDH) nanocomposites were prepared by rehydration of the oxides produced by calcination of an organic LDH. While the memory effect is a widely recognized effect on oxides produced by inorganic LDH, it is unprecedented from the calcination/rehydration of organic ones. Different temperatures (400, 600, and 1100 °C) were tested on the basis of thermogravimetric data. Water, instead of a carbonate solution, was used for the rehydration, with CO2 available from water itself and/or air to induce a slower process with an easier and better intercalation of the carbonaceous species. The samples were characterized by X-ray powder diffraction (XRPD), infrared in reflection mode (IR), and Raman spectroscopies and scanning electron microscopy (SEM). XRPD indicated the presence of carbonate LDH, and of residuals of unreacted oxides. IR confirmed that the prevailing anion is carbonate, coming from the water used for the rehydration and/or air. Raman data indicated the presence of low-ordered carbonaceous species moieties and SEM and XRPD the absence of separated bulky graphitic sheets, suggesting an intimate mixing of the low ordered carbonaceous phase with reconstructed LDH. Organic LDH gave better memory effect after calcination at 400 °C. Conversely, the carbonaceous species are observed after rehydration of the sample calcined at 600 °C with a reduced memory effect, demonstrating the interference of the carbonaceous phase with LDH reconstruction and the bonding with LDH layers to form a low-ordered carbon/LDH nanocomposite.