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1.
Angew Chem Int Ed Engl ; 62(18): e202218928, 2023 Apr 24.
Artigo em Inglês | MEDLINE | ID: mdl-36883967

RESUMO

Despite the advances in the field of carbon-halogen bond formation, the straightforward catalytic access to selectively functionalized iodoaryls remains a challenge. Here, we report a one-pot synthesis of ortho-iodobiaryls from aryl iodides and bromides by palladium/norbornene catalysis. This new example of Catellani reaction features the initial cleavage of a C(sp2 )-I bond, followed by the key formation of a palladacycle through ortho C-H activation, the oxidative addition of an aryl bromide and the ultimate restoration of the C(sp2 )-I bond. A large variety of valuable o-iodobiaryls has been synthesized in satisfactory to good yields and their derivatization have been described too. Beyond the synthetic utility of this transformation, a DFT study provides insights on the mechanism of the key reductive elimination step, which is driven by an original transmetallation between palladium(II)-halides complexes.

2.
Molecules ; 27(19)2022 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-36235034

RESUMO

Barium titanate (BT) recently gained new interest in the preparation of dielectric and piezoelectric lead-free materials for applications in sensors, electronics, energy harvesting and storage fields. Barium titanate nanocomposites can achieve attractive performance, provided that the compatibility between ceramic particles and polymeric matrices is enhanced to the benefit of the physical properties of the final composite. Tuning the particle-matrix interface through particle functionalization represents a viable solution. In this work, surface functionalization of BT nanoparticles (NPs), obtained by hydrothermal synthesis, with 3-glycidyloxypropyltrimethoxysilane, 2-[(acetoxy(polyethyleneoxy)propyl]triethoxysilane and triethoxysilylpropoxy(polyethyleneoxy)dodecanoate, was performed after optimizing the hydroxylation process of the NPs to improve their surface reactivity and increase the yield of grafting. Solid-state nuclear magnetic resonance and thermogravimetric analysis were used to quantify the molecules grafted onto the ceramic nanoparticles. Both bare and functionalized particles were employed in the realization of epoxy- and polydimethylsiloxane (PDMS)-based nanocomposites. Functionalization was proven to be beneficial for particle dispersibility and effective for particle alignment in the PDMS matrix. Moreover, the dielectric constant measurements revealed the potential of PDMS-based nanocomposites for applications in the field of dielectric elastomers.


Assuntos
Nanocompostos , Compostos de Organossilício , Bário , Dimetilpolisiloxanos , Elastômeros , Lauratos , Titânio
3.
G Ital Med Lav Ergon ; 44(1): 3-9, 2022 03.
Artigo em Italiano | MEDLINE | ID: mdl-36346294

RESUMO

SUMMARY: Background. ARPA Piemonte carries out occupational exposure measurements of chemical agents in workplace environment to support the Occupatonal Health and Safety Units of Local Health Boards for the assessment of the exposure level of dangerous chemical. Data are reported in internal documents, but are not available for other purposes. Objectives. Organize the occupational exposure measures collected by ARPA Piemonte, in order to facilitate their availability, in accordance with the indications of the European Foundation for the Improvement of Living and Working Conditions. Methods. An application in a relational database environment was defined and developed to collect and structure information relating to companies, interventions, tasks and / or monitored sampling points, samples and measurements performed. Results. Data on chemical exposure related to interventions carried out by ARPA Piemonte in the period from 2005 to part of 2020 have been collected in the ESP ALP application. ESP ALP contains information about 161 companies, 193 interventions, 815 sampling points, 3.490 samples and 18.576 measurements and information on companies obtained from the 2011 Census of Economic Activities and the archives of the National Institute for Insurance against Accidents at Work (INAIL). Discussion. We verified the feasibility of retrieving and organizing the information collected in past years in an integrated environment that facilitates its processing and use. Finally, we confirm the usefulness of collaboration between multidisciplinary professionals.


Assuntos
Exposição Ocupacional , Local de Trabalho , Humanos
4.
Environ Res ; 195: 110699, 2021 04.
Artigo em Inglês | MEDLINE | ID: mdl-33539832

RESUMO

The finest fraction of Particulate Matter (PM2.5) carries a large number of pollutants, some of which are assessed as genotoxic, such as some Polycyclic Aromatic Hydrocarbons (PAHs). In many countries, PM2.5 in combination with some PAHs are monitored to assess the concentrations of pollutants, while the air quality is rarely assessed by means of biological assays. Epidemiological studies have demonstrated a significant correlation between these two pollutants and human adverse effects, in particular on the respiratory system. Nevertheless, other air pollutants can induce a biological effect and the cumulative effect of the PM2.5 complex mixture may not be easily deduced by PM2.5 and PAH levels. This study aimed to combine the legislative monitoring of PM2.5 with the study of its mutagenicity. During a full year, daily air samples were collected in nine sites of the North-western Italy air quality monitoring network (Piedmont Region) and PM2.5 and PAH concentrations were assessed. Monthly pooled organic extracts were tested with the Salmonella assay using TA98 and TA100 strains, with and without metabolic activation (±S9), and using TA98NR and YG1021 strains. In all sites, a positive response was observed for TA98 and TA100 especially without S9. A significant mutagenic seasonal variation was detected, with higher mutagenicity in winter and lower responses in summer (average total mutagenicity ratio 27:1). The response of TA98NR and YG1021 compared with TA98 suggested a significant contribution of nitro-compounds to the mutagenicity. No significant differences were found between urban background and rural sites denoting the spread of pollution. A mutagenicity increase, 1.28 Total Mutagenicity Factor/20 m3, was observed for each PM2.5 µg increment. PAH levels and corresponding Toxic Equivalent Factors were highly correlated to mutagenicity results. This work confirms that complex environmental mixtures can be appropriately assessed through the implementation of physical-chemical analyzes with bioassays able to evaluate synergistic and antagonistic effects, especially for highest and lowest pollution settings.


Assuntos
Poluentes Atmosféricos , Poluição do Ar , Hidrocarbonetos Policíclicos Aromáticos , Poluentes Atmosféricos/análise , Poluentes Atmosféricos/toxicidade , Bioensaio , Humanos , Itália , Testes de Mutagenicidade , Mutagênicos/toxicidade , Material Particulado/toxicidade , Hidrocarbonetos Policíclicos Aromáticos/análise , Hidrocarbonetos Policíclicos Aromáticos/toxicidade
5.
Mar Drugs ; 19(1)2020 Dec 23.
Artigo em Inglês | MEDLINE | ID: mdl-33374863

RESUMO

Inflammation and oxidative stress are part of the complex biological responses of body tissues to harmful stimuli. In recent years, due to the increased understanding that oxidative stress is implicated in several diseases, pharmaceutical industries have invested in the research and development of new antioxidant compounds, especially from marine environment sources. Marine seaweeds have shown the presence of many bioactive secondary metabolites, with great potentialities from both the nutraceutical and the biomedical point of view. In this study, 50%-ethanolic and DMSO extracts from the species C. amentacea var. stricta were obtained for the first time from seaweeds collected in the Ligurian Sea (north-western Mediterranean). The bioactive properties of these extracts were then investigated, in terms of quantification of specific antioxidant activities by relevant ROS scavenging spectrophotometric tests, and of anti-inflammatory properties in LPS-stimulated macrophages by evaluation of inhibition of inflammatory cytokines and mediators. The data obtained in this study demonstrate a strong anti-inflammatory effect of both C. amentacea extracts (DMSO and ethanolic). The extracts showed a very low grade of toxicity on RAW 264.7 macrophages and L929 fibroblasts and a plethora of antioxidant and anti-inflammatory effects that were for the first time thoroughly investigated. The two extracts were able to scavenge OH and NO radicals (OH EC50 between 392 and 454 µg/mL; NO EC50 between 546 and 1293 µg/mL), to partially rescue H2O2-induced RAW 264.7 macrophages cell death, to abate intracellular ROS production in H2O2-stimulated macrophages and fibroblasts and to strongly inhibit LPS-induced inflammatory mediators, such as NO production and IL-1α, IL-6, cyclooxygenase-2 and inducible NO synthase gene expression in RAW 264.7 macrophages. These results pave the way, for the future use of C. amentacea metabolites, as an example, as antioxidant food additives in antiaging formulations as well as in cosmetic lenitive lotions for inflamed and/or damaged skin.


Assuntos
Anti-Inflamatórios/farmacologia , Antioxidantes/farmacologia , Fibroblastos/efeitos dos fármacos , Macrófagos/efeitos dos fármacos , Estresse Oxidativo/efeitos dos fármacos , Phaeophyceae/metabolismo , Animais , Anti-Inflamatórios/isolamento & purificação , Antioxidantes/isolamento & purificação , Ciclo-Oxigenase 2/genética , Ciclo-Oxigenase 2/metabolismo , Citocinas/genética , Citocinas/metabolismo , Fibroblastos/metabolismo , Fibroblastos/patologia , Peróxido de Hidrogênio/toxicidade , Mediadores da Inflamação/metabolismo , Lipopolissacarídeos/toxicidade , Macrófagos/metabolismo , Macrófagos/patologia , Camundongos , Óxido Nítrico/metabolismo , Óxido Nítrico Sintase Tipo II/genética , Óxido Nítrico Sintase Tipo II/metabolismo , Células RAW 264.7 , Espécies Reativas de Oxigênio/metabolismo
6.
Org Biomol Chem ; 17(25): 6165-6173, 2019 06 26.
Artigo em Inglês | MEDLINE | ID: mdl-31192343

RESUMO

Herein, we report a novel catalytic synthesis of substituted 9H-fluoren-9-ols starting from aryl iodides and secondary ortho-bromobenzyl alcohols in the presence of palladium/norbornene as a catalytic system. The present protocol exhibits high functional group tolerance, mild reaction conditions and moderate to good yields. This transformation is based on two sequential pathways: (i) Pd(ii)-mediated oxidation of the secondary alcohol to the corresponding ketone and (ii) Pd(0)/norbornene-catalyzed reaction of the in situ generated ortho-bromoacetophenone with the aryl iodide.

7.
Nanotechnology ; 29(49): 495201, 2018 Dec 07.
Artigo em Inglês | MEDLINE | ID: mdl-30234499

RESUMO

This work reports the fabrication of memristive devices based on iron oxide (Fe2O3) thin films grown by atomic layer deposition (ALD) using ferrocene as iron precursor and ozone as oxidant. An excellent control of the ALD process was achieved by using an experimental procedure based on a sequence of micro-pulses, which provided long residence time and homogeneous diffusion of precursors, allowing ALD of thin films with smooth morphology and crystallinity which was found to increase with layer thickness, at temperatures as low as 250 °C. The resistive switching of symmetric Pt/Fe2O3/Pt thin film devices exhibited bipolar mode with good stability and endurance. Multi-level switching was achieved via current and voltage control. It was proved that the ON state regime can be tuned by changing the current compliance while the OFF state can be changed to intermediate levels by decreasing the maximum voltage during RESET. The structural analysis of the switched oxide layer revealed the presence of nano-sized crystalline domains corresponding to different iron oxide phases, suggesting that Joule heating effects during I-V cycling are responsible for a crystallization process of the pristine amorphous layer.

8.
Acc Chem Res ; 49(7): 1389-400, 2016 07 19.
Artigo em Inglês | MEDLINE | ID: mdl-27333299

RESUMO

Direct C-H bond activation is an important reaction in synthetic organic chemistry. This methodology has the potential to simplify reactions by avoiding the use of prefunctionalized reagents. However, selectivity, especially site selectivity, remains challenging. Sequential reactions, in which different molecules or groups are combined in an ordered sequence, represent a powerful tool for the construction of complex molecules in a single operation. We have discovered and developed a synthetic methodology that combines selective C-H bond activation with sequential reactions. This procedure, which is now known as the "Catellani reaction", enables the selective functionalization of both the ortho and ipso positions of aryl halides. The desired molecules are obtained with high selectivity from a pool of simple precursors. These molecules are assembled under the control of a palladacycle, which is formed through the joint action of a metal (Pd) and an olefin such as norbornene. These two species act cooperatively with an aryl halide to construct the palladacycle, which is formed through ortho-C-H activation of the original aryl halide. The resulting complex acts as a scaffold to direct the reaction (via Pd(IV)) of other species, such as alkyl or aryl halides and amination or acylation agents, toward the sp(2) C-Pd bond. At the end of this process, because of steric hindrance, the scaffold is dismantled by norbornene extrusion. Pd(0) is cleaved from the organic product through C-C, C-H, C-N, C-O, or C-B coupling, in agreement with the well-known reactivity of aryl-Pd complexes. The cycle involves Pd(0), Pd(II), and Pd(IV) species. In particular, our discovery relates to alkylation and arylation reactions. Recently, remarkable progress has been made in the following areas: (a) the installation of an amino or an acyl group at the ortho position of aryl halides, (b) the formation of a C-B bond at the ipso position, (c) the achievement of meta-C-H bond activation of aryl rings bearing a chelating directing group by Pd(II)/Pd(IV)/norbornene catalysis, and (d) the activation of N-H and C-H bonds in sequence for indole 2-alkylation. In this Account, we explain the main features of this methodology, describe its synthetic potential, and illustrate some remarkable progress that has been made, emphasizing the most recent developments and applications in total synthesis.

9.
Nanotechnology ; 28(17): 174002, 2017 Apr 28.
Artigo em Inglês | MEDLINE | ID: mdl-28282299

RESUMO

In certain polymers the graphenization of carbon atoms can be obtained by laser writing owing to the easy absorption of long-wavelength radiation, which generates photo-thermal effects. On a polyimide surface this process allows the formation of a nanostructured and porous carbon network known as laser-induced graphene (LIG). Herein we report on the effect of the process parameters on the morphology and physical properties of LIG nanostructures. We show that the scan speed and the frequency of the incident radiation affect the gas evolution, inducing different structure rearrangements, an interesting nitrogen self-doping phenomenon and consequently different conduction properties. The materials were characterized by infrared and Raman spectroscopy, XPS elemental analysis, electron microscopy and electrical/electrochemical measurements. In particular the samples were tested as interdigitated electrodes into electrochemical supercapacitors and the optimized LIG arrangement was tested in parallel and series supercapacitor configurations to allow power exploitation.

10.
Nanomaterials (Basel) ; 14(7)2024 Mar 22.
Artigo em Inglês | MEDLINE | ID: mdl-38607095

RESUMO

The synthesis of novel catalysts for the oxygen reduction reaction, by means of a fast one-pot microwave-assisted procedure, is reported herein and deeply explained. In particular, the important role of doping atoms, like sulfur and nitrogen, in Fe2O3-reduced graphene oxide nanocomposites is described to address the modification of catalytic performance. The presence of dopants is confirmed by X-ray Photoelectron Spectroscopy analysis, while the integration of iron oxide nanoparticles, by means of decoration of the graphene structure, is corroborated by electron microscopy, which also confirms that there is no damage to the graphene sheets induced by the synthesis procedure. The electrochemical characterizations put in evidence the synergistic catalysis effects of dopant atoms with Fe2O3 and, in particular, the importance of sulfur introduction into the graphene lattice. Catalytic performance of as-prepared materials toward oxygen reduction shows values close to the Pt/C reference material, commonly used for fuel cell and metal-air battery applications.

11.
Nat Commun ; 15(1): 2522, 2024 Mar 21.
Artigo em Inglês | MEDLINE | ID: mdl-38514605

RESUMO

Liquid-phase transmission electron microscopy is a burgeoning experimental technique for monitoring nanoscale dynamics in a liquid environment, increasingly employing microfluidic reactors to control the composition of the sample solution. Current challenges comprise fast mass transport dynamics inside the central nanochannel of the liquid cell, typically flow cells, and reliable fixation of the specimen in the limited imaging area. In this work, we present a liquid cell concept - the diffusion cell - that satisfies these seemingly contradictory requirements by providing additional on-chip bypasses to allow high convective transport around the nanochannel in which diffusive transport predominates. Diffusion cell prototypes are developed using numerical mass transport models and fabricated on the basis of existing two-chip setups. Important hydrodynamic parameters, i.e., the total flow resistance, the flow velocity in the imaging area, and the time constants of mixing, are improved by 2-3 orders of magnitude compared to existing setups. The solution replacement dynamics achieved within seconds already match the mixing timescales of many ex-situ scenarios, and further improvements are possible. Diffusion cells can be easily integrated into existing liquid-phase transmission electron microscopy workflows, provide correlation of results with ex-situ experiments, and can create additional research directions addressing fast nanoscale processes.

12.
Sensors (Basel) ; 13(6): 7618-32, 2013 Jun 13.
Artigo em Inglês | MEDLINE | ID: mdl-23765271

RESUMO

This paper introduces a novel contactless sensing principle conceived for measuring the rotation angle of a shaft. The sensor is based on a smart combination of low-cost components that can be effectively integrated in a mechanical assembly of a rotary joint. The working principle is based on the relative rotation of a small diametrically magnetized cylindrical or annular magnet and at least one Hall effect sensor. One of the main strengths of the new sensing principle is to be adaptable to any assigned dimensions and encumbrances without typical design limitations given by the use of standard components. A numerical model is developed for predicting the sensor output characteristic on the base of the concept of magnetic charge. Such a model is validated against results from laboratory experiments. The parameters that define the geometry and layout of the sensor are optimized in order to maximize linearity over an assigned angular range of measurement. Two examples of mechatronic systems that employ the new sensing principle are presented in order to show the possibility of obtaining with the new principle a compact/integrated sensor-design.

13.
Air Qual Atmos Health ; : 1-16, 2023 Jun 06.
Artigo em Inglês | MEDLINE | ID: mdl-37359393

RESUMO

In 2020, during the COVID-19 pandemic, containment measures were applied inducing potential changes in air pollutant concentrations and thus in air toxicity. This study evaluates the role of restrictions on biological effects of particulate matter (PM) in different Northwest Italy sites: urban background, urban traffic, rural, and incinerator. Daily PM samples collected in 2020 were pooled according to restrictions: January/February (no restrictions), March and April (first lockdown), May/June and July/August/September (low restrictions), October/November/December (second lockdown). The 2019 samples (pre-pandemic period) were pooled as 2020 for comparison. Pools were extracted with organic solvents and extracts were tested to assess cytotoxicity (WST-1 assay) and genotoxicity (comet assay) on BEAS-2B cells, mutagenicity (Ames test) on TA98 and TA100 Salmonella typhimurium strains, and estrogenic activity (gene reporter assay) on MELN cells. Pollutant concentrations were also analyzed (PM10, PM2.5, polycyclic aromatic hydrocarbons). No difference was observed for PM and polycyclic aromatic hydrocarbon concentrations between 2020 and 2019. During lockdown months (2020), PM cytotoxicity/genotoxicity was significantly lower in some sites than during 2019, while considering PM mutagenicity/estrogenic activity some differences were detected but without statistical significance. PM extract effects decreased in some sites during 2020; this may be due to lockdowns that reduced/modified pollutant emissions and may be related also to complex PM origin/formation and to meteorological conditions. In conclusion, the study confirms that PM biological effects cannot be assessed considering only the PM concentration and suggests to include a battery of bioassay for air quality monitoring in order to protect human health from air pollution effects. Supplementary Information: The online version contains supplementary material available at 10.1007/s11869-023-01381-6.

14.
Environ Toxicol Pharmacol ; 102: 104232, 2023 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-37459960

RESUMO

Endocrine disruptors (EDCs) are emerging contaminants that are harmful to health. Human exposure occurs mainly through ingestion or dermal contact, but inhalation could be an additional exposure route; therefore, this study was conducted to evaluate the oestrogenic activity of airborne particulate matter (PM). Outdoor PM was collected for a year in five Italian sites and extracted with organic solvents (four seasonal extracts/site). The oestrogenic activity was assessed using a gene reporter assay (MELN), and the risk to human health through inhalation was quantified using the results. Moreover, extracts were analysed to assess cytotoxicity (WST-1 and LDH assays) on human bronchial cells (BEAS-2B). The extracts induced a significant cytotoxicity and oestrogenic activity. Oestrogenic activity showed a seasonal trend and was correlated with concentrations of benzo(a)pyrene and toxic equivalency factor. Although a low inhalation cancer risk was found, this study confirmed that oestrogenic activity in air could contribute to overall health risks due to EDC exposure.


Assuntos
Poluentes Atmosféricos , Disruptores Endócrinos , Humanos , Disruptores Endócrinos/toxicidade , Disruptores Endócrinos/análise , Carga Corporal (Radioterapia) , Material Particulado/toxicidade , Material Particulado/análise , Itália , Poluentes Atmosféricos/toxicidade , Poluentes Atmosféricos/análise
15.
J Migr Health ; 7: 100177, 2023.
Artigo em Inglês | MEDLINE | ID: mdl-36968561

RESUMO

Background and objective: The recent notable increase in refugees' flows, with refugee children and adolescents relocating worldwide, posed severe challenges to the different national healthcare systems. Social groups such as refugees fleeing from their countries because of persecution, wars and violence are considered at high risk of developing mental health-related problems. Despite international and national policies legally regulating the reception process and protecting health-related rights, including the mental well-being of refugee migrants, there is a theoretical and applied need for evidence-based instruments and procedures to support mental health within this population. Recent evidence refers to the Refugee Health Screener-15 (RHS-15) as a reliable and valid instrument for the early detection of trauma-related mental health problems. In this scenario, this study aimed to test the RHS screening process within a multidisciplinary first intervention reception context for unaccompanied refugee minors. Design: The RHS-15 was administered with the support of cultural-linguistic mediators to 81 unaccompanied minor residents in a first intervention facility in Milan, Italy. This study aimed to assess psychometric characteristics, such as reliability, sensitivity and specificity feasibility and its implementation within a first intervention reception process. Results: The analysis resulted in the validation of the RHS in its 13-item format. The results highlighted and confirmed an efficient delivery, excellent reliability and a positive predictive and convergent validity of the 13-item version. Further analysis showed an excellent ability to avoid false negatives, although there was a clear tendency to identify false positives. Conclusions: The early identification of vulnerabilities among refugee minors is recommended to promote their long-term overall well-being. Integrating the screening results with additional observational elements and more specific diagnostic tools is recommended to gain a comprehensive perspective of the minors' well-being.

16.
Nanomaterials (Basel) ; 13(18)2023 Sep 09.
Artigo em Inglês | MEDLINE | ID: mdl-37764556

RESUMO

Environmental problems are among the most pressing issues in the modern world, including the shortage of clean drinking water partially caused by contamination from various industries and the excessive emission of CO2 primarily from the massive use of fossil fuels. Consequently, it is crucial to develop inexpensive, effective, and environmentally friendly methods for wastewater treatment and CO2 reduction, turning them into useful feedstocks. This study explores a unique method that addresses both challenges by utilizing ZnO, which is recognized as one of the most active semiconductors for photocatalysis, as well as a cost-effective electrocatalyst for the CO2 reduction reaction (CO2RR). Specifically, we investigate the influence of the morphology of various ZnO nanostructures synthesized via different low-cost routes on their photocatalytic properties for degrading the rhodamine-B dye (RhB) and on their electrocatalytic performance for the CO2RR. Our results show that the ZnO lamella morphology achieves the best performance compared to the nanorod and nanoparticle structures. This outcome is likely attributed to the lamella's higher aspect ratio, which plays a critical role in determining the structural, optical, and electrical properties of ZnO.

17.
Mol Syndromol ; 14(5): 433-438, 2023 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-37915395

RESUMO

Introduction: Nowadays, whole-exome sequencing (WES) analysis is an essential part in the diagnostic pathway of individuals with complex phenotypes when routine exams, such as array-CGH and gene panels, have proved inconclusive. However, data on the diagnostic rate of WES analysis in adult individuals, negative to first-tier tests, are lacking. This is because initiatives with the aim of diagnosing rare diseases focus mainly on pediatric unsolved cases. Case Presentation: We hereby present a 45-year-old woman with severe intellectual disability, previous psychomotor developmental delay, behavioral disorders, stereotypies, nonconvulsive epilepsy, and dysmorphisms. The proband first came to our attention when she was 4 years old (in 1982); since then, she has undergone several clinical and instrumental assessments, without reaching a genetic diagnosis. At last, through WES analysis, a novel de novo variant in SYNGAP1 was found. The clinical characteristics associated with SYNGAP1 are similar to those presented by the proband. Conclusion: The variant is predicted to be deleterious and is most probably the cause of the proband's phenotype. The perseverance of the clinicians and the family allowed us to reach a diagnosis in a woman with a more than 30-year history of clinical evaluations, instrumental assessments, and genetic tests. This diagnosis was of significant relevance in genetic counseling for family members and the proband herself.

18.
Chemosphere ; 345: 140400, 2023 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-37863212

RESUMO

Highly efficient, separable, and stable magnetic iron-based-photocatalysts produced from ultra-stable Y (USY) zeolite were applied, for the first time, to the photo-Fenton removal of phenol under solar light. USY Zeolite with a Si/Al molar ratio of 385 was impregnated under vacuum with an aqueous solution of Fe2+ ions and thermally treated (500-750 °C) in a reducing atmosphere. Three catalysts, Fe-USY500°C-2h, Fe-USY600°C-2h and Fe-USY750°C-2h, containing different amounts of reduced iron species entrapped in the zeolitic matrix, were obtained. The catalysts were thoroughly characterized by absorption spectrometry, X-ray powder diffraction with synchrotron source, followed by Rietveld analysis, X-ray photoelectron spectroscopy, N2 adsorption/desorption at -196 °C, high-resolution transmission electron microscopy and magnetic measurements at room temperature. The catalytic activity was evaluated in a recirculating batch photoreactor irradiated by solar light with online analysis of evolved CO2. Photo-Fenton results showed that the catalyst obtained by thermal treatment at 500 °C for 2 h under a reducing atmosphere (FeUSY-500°C-2h) was able to completely mineralize phenol in 120 min of irradiation time at pH = 4 owing to the presence of a higher content of entrapped nano-sized magnetite particles. The latter promotes the generation of hydroxyl radicals in a more efficient way than the Fe-USY catalysts prepared at 600 and 750 °C because of the higher Fe3O4 content in ultra-stable Y zeolite treated at 500 °C. The FeUSY-500°C-2h catalyst was recovered from the treated water through magnetic separation and reused five times without any significant worsening of phenol mineralization performances. The characterization of the FeUSY-500°C-2h after the photo-Fenton process demonstrated that it was perfectly stable during the reaction. The optimized catalyst was also effective in the mineralization of phenol in tap water. Finally, a possible photo-Fenton mechanism for phenol mineralization was assessed based on experimental tests carried out in the presence of scavenger molecules, demonstrating that hydroxyl radicals play a major role.


Assuntos
Fenol , Zeolitas , Fenol/química , Ferro/química , Fenóis , Água , Peróxido de Hidrogênio/química , Catálise
19.
Sensors (Basel) ; 12(10): 13598-616, 2012 Oct 10.
Artigo em Inglês | MEDLINE | ID: mdl-23202012

RESUMO

In this work we present the design process, the characterization and testing of a novel three-axis mechanical force sensor. This sensor is optimized for use in closed-loop force control of haptic devices with three degrees of freedom. In particular the sensor has been conceived for integration with a dual finger haptic interface that aims at simulating forces that occur during grasping and surface exploration. The sensing spring structure has been purposely designed in order to match force and layout specifications for the application. In this paper the design of the sensor is presented, starting from an analytic model that describes the characteristic matrix of the sensor. A procedure for designing an optimal overload protection mechanism is proposed. In the last part of the paper the authors describe the experimental characterization and the integrated test on a haptic hand exoskeleton showing the improvements in the controller performances provided by the inclusion of the force sensor.

20.
Bioengineering (Basel) ; 9(7)2022 Jul 11.
Artigo em Inglês | MEDLINE | ID: mdl-35877354

RESUMO

Scoliosis is an abnormality of the spinal curvature that severely affects the musculoskeletal, respiratory, and nervous systems. Conventionally, it is treated using rigid spinal braces. These braces are static, rigid, and passive in nature, and they (largely) limit the mobility of the spine, resulting in other spinal complexities. Moreover, these braces do not have precise control over how much force is being applied by them. Over-exertion of force may deteriorate the spinal condition. This article presents a novel active soft brace that allows mobility to the spine while applying controlled corrective forces that are regulated by varying the tensions in elastic bands using low-power light weight twisted string actuators (TSAs). This article focuses on the actuator and contact force modeling of the active soft brace (ASB). The actuator modeling is required to translate the twisting of string in terms of contraction of the string's length, whereas the contact force modeling helps in estimating the net resultant force exerted by the band on the body using single point pressure/force sensors. The actuators (TSAs) are modeled as helix geometry and validated using a laser position sensor. The results showed that the model effectively tracked the position (contraction in length) with root mean square error (RMSE) of 1.7386 mm. The contact force is modeled using the belt and pulley contact model and validated by building a custom testbed. The actuator module is able to regulate the pressure in the range 0-6 Kpa, which is comparable to 0-8 Kpa pressure regulated in rigid braces. This makes it possible to verify and demonstrate the working principle of the proposed active soft brace.

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