Adsorption of Scandium Ions by Amberlite XAD7HP Polymeric Adsorbent Loaded with Tri-n-Octylphosphine Oxide.

In an actual economic context, the demand for scandium has grown due to its applications in top technologies. However, further development of new technologies will lead to an increase in the market for Sc related to such technologies. The present study aims to improve and upgrade existing technology in terms of efficient scandium recovery, proposing a new material with selective adsorptive properties for scandium recovery. To highlight the impregnation of Amberlite XAD7HP resin with tri-n-octylphosphine oxide extractant by the solvent-impregnated resin method, the obtained adsorbent material was characterized by physico-chemical techniques. Further, the specific surface of the adsorbent and the zero-point charge of the adsorbent surface have been determined. Different parameters, such as initial concentration, adsorbent amount, contact time, or temperature, have been studied. The initial pH effect was investigated when a maximum adsorption capacity of 31.84 mg g-1 was obtained at pH > 3, using 0.1 g of adsorbent and a contact time of 90 min and 298 K. An attempt was made to discuss and provide a clear representation of the studied adsorption process, proposing a specific mechanism for Sc(III) recovery from aqueous solutions through kinetic, thermodynamic, and equilibrium studies. Adsorption/desorption studies reveal that the prepared adsorbent material can be reused five times.

Evaluation of Functionalized Amberlite Type XAD7 Polymeric Resin with L-Valine Amino Acid Performance for Gallium Recovery.

Given the ever-increasing demand for gallium(III) as a crucial precursor in the fabrication of advanced materials, there arises an imperative to devise efficient recovery processes from primary and secondary sources. In the present investigation, the retrieval of gallium(III) from aqueous solutions through the mechanism of adsorption was investigated. Materials with superior adsorbent properties play an important role in the dynamics of the adsorption process. To enhance these properties, select materials, such as Amberlite-type polymeric resins, are amenable to functionalization through impregnation with extractants featuring specialized active groups, designed for the selective recovery of metal ions-specifically, Ga(III). The impregnation method employed in this study is the Solvent-Impregnated Resin (SIR) method, utilizing the amino acid DL-valine as the extractant. The new material was characterized through Scanning Electron Microscopy (SEM), Elemental Analysis via X-ray energy-dispersive spectroscopy (EDX), and Fourier transform infrared spectroscopy (FTIR) to elucidate the presence of the extractant on the resin's surface. Concurrently, the material's pHPZC was determined. The adsorptive prowess of the synthesized material was investigated through kinetic, thermodynamic, and equilibrium studies. The influence of specific parameters in the adsorption process-namely, pH, contact time, temperature, and Ga(III) initial concentration-on the maximal adsorption capacity was determined. The optimal adsorption conditions were established using the Taguchi method.

Kinetic Modelling the Solid-Liquid Extraction Process of Scandium from Red Mud: Influence of Acid Composition, Contact Time and Temperature.

Industry represents a fundamental component of modern society, with the generation of massive amounts of industrial waste being the inevitable result of development activities in recent years. Red mud is an industrial waste generated during alumina production using the Bayer process of refining bauxite ore. It is a highly alkaline waste due to the incomplete removal of NaOH. There are several opinions in both the literature and legislation on the hazards of red mud. According to European and national legislation, this mud is not on the list of hazardous wastes; however, if the list of criteria are taken into account, it can be considered as hazardous. The complex processing of red mud is cost-effective because it contains elements such as iron, manganese, sodium, calcium, magnesium, zinc, strontium, lead, copper, cadmium, bismuth, barium and rare earths, especially scandium. Therefore, the selection of an extraction method depends on the form in which the element is present in solution. Extraction is one of the prospective separation and concentration methods. In this study, we evaluated the kinetic modelling of the solid-liquid acid extraction process of predominantly scandium as well as other elements present in red mud. Therefore, three acids (HCl, HNO3 and H2SO4) at different concentrations (10, 20 and 30%) were targeted for the extraction of Sc(III) from solid red mud. Specific parameters of the kinetics of the extraction process were studied, namely the solid:liquid ratio, initial acid concentration, contact time and temperature. The extraction kinetics of Sc(III) with acids was evaluated using first- and second-order kinetic models, involving kinetic parameters, rate constants, saturation concentration and activation energy. The second-order kinetic model was able to describe the mechanism of Sc(III) extraction from red mud. In addition, this study provides an overview on the mechanism of mass transfer involved in the acid extraction process of Sc(III), thereby enabling the design, optimization and control of large-scale processes for red mud recovery.

Arsenic Removal Using Unconventional Material with Iron Content: Batch Adsorption and Column Study.

The remediation of arsenic contamination in potable water is an important and urgent concern, necessitating immediate attention. With this objective in mind, the present study investigated arsenic removal from water using batch adsorption and fixed-bed column techniques. The material employed in this study was a waste product derived from the treatment of groundwater water for potable purposes, having a substantial iron composition. The material's properties were characterized using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and Fourier-transformed infrared spectroscopy (FT-IR). The point of zero charge (pHPZC) was measured, and the pore size and specific surface area were determined using the BET method. Under static conditions, kinetic, thermodynamic, and equilibrium studies were carried out to explore the influencing factors on the adsorption process, namely the pH, contact time, temperature, and initial arsenic concentration in the solution. It was found that the adsorption process is spontaneous, endothermic, and of a physical nature. In the batch adsorption studies, the maximum removal percentage was 80.4% after 90 min, and in a dynamic regime in the fixed-bed column, the efficiency was 99.99% at a sludge:sand = 1:1 ratio for 380 min for a volume of water with arsenic of ~3000 mL. The kinetics of the adsorption process conformed to a pseudo-second-order model. In terms of the equilibrium studies, the Sips model yielded the most accurate representation of the data, revealing a maximum equilibrium capacity of 70.1 mg As(V)/g sludge. For the dynamic regime, the experimental data were fitted using the Bohart-Adams, Thomas, and Clark models, in order to establish the mechanism of the process. Additionally, desorption studies were conducted, serving as an essential step in validating the practical applicability of the adsorption process, specifically in relation to the reutilization of the adsorbent material.

Synthesis, Characterization and Antimicrobial Activity of Multiple Morphologies of Gold/Platinum Doped Bismuth Oxide Nanostructures.

Bismuth oxides were synthesized from bismuth carbonate using the sol-gel method. Studies have described the formation of Bi2O3, as a precursor of HNO3 dissolution, and intermediate oxides, such as BixOy when using H2SO4 and H3PO4. The average size of the crystallite calculated from Scherrer's formula ranged from 9 to 19 nm, according to X-ray diffraction. The FTIR analysis showed the presence of specific Bi2O3 bands when using HNO3 and of crystalline phases of "bismuth oxide sulphate" when using H2SO4 and "bismuth phosphate" when using H3PO4. The TG curves showed major mass losses and specific thermal effects, delimited in four temperature zones for materials synthesized with HNO3 (with loss of mass between 24% and 50%) and H2SO4 (with loss of mass between 45% and 76%), and in three temperature zones for materials synthesized with H3PO4 (with loss of mass between 13% and 43%). Further, the thermal stability indicates that materials have been improved by the addition of a polymer or polymer and carbon. Confocal laser scanning microscopy showed decreased roughness in the series, [BixOy]N > [BixOy-6% PVA]N > [BixOy-C-6% PVA]N, and increased roughness for materials [BixOy]S, [BixOy-6% PVA]S, [BixOy-C-6% PVA]S, [BixOy]P, [BixOy-6% PVA]P and [BixOy-C-6% PVA]P. The morphological analysis (electronic scanning microscopy) of the synthesized materials showed a wide variety of forms: overlapping nanoplates ([BixOy]N or [BixOy]S), clusters of angular forms ([BixOy-6% PVA]N), pillars ([BixOy-6% PVA]S-Au), needle particles ([BixOy-Au], [BixOy-6% PVA]S-Au, [BixOy-C-6% PVA]S-Au), spherical particles ([BixOy-C-6% PVA]P-Pt), 2D plates ([BixOy]P-Pt) and 3D nanometric plates ([BixOy-C-6% PVA]S-Au). For materials obtained in the first synthesis stage, antimicrobial activity increased in the series [BixOy]N > [BixOy]S > [BixOy]P. For materials synthesized in the second synthesis stage, when polymer (polyvinyl alcohol, PVA) was added, maximum antimicrobial activity, regardless of the microbial species tested, was present in the material [BixOy-6% PVA]S. For the materials synthesized in the third stage, to which graphite and 6% PVA were added, the best antimicrobial activity was in the material [BixOy-C-6% PVA]P. Materials synthesized and doped with metal ions (gold or platinum) showed significant antimicrobial activity for the tested microbial species.

Selenite Removal from Aqueous Solution Using Silica-Iron Oxide Nanocomposite Adsorbents.

In recent years, during industrial development, the expanding discharge of harmful metallic ions from different industrial wastes (such as arsenic, barium, cadmium, chromium, copper, lead, mercury, nickel, selenium, silver, or zinc) into different water bodies has caused serious concern, with one of the problematic elements being represented by selenium (Se) ions. Selenium represents an essential microelement for human life and plays a vital role in human metabolism. In the human body, this element acts as a powerful antioxidant, being able to reduce the risk of the development of some cancers. Selenium is distributed in the environment in the form of selenate (SeO42-) and selenite (SeO32-), which are the result of natural/anthropogenic activities. Experimental data proved that both forms present some toxicity. In this context, in the last decade, only several studies regarding selenium's removal from aqueous solutions have been conducted. Therefore, in the present study, we aim to use the sol-gel synthesis method to prepare a nanocomposite adsorbent material starting from sodium fluoride, silica, and iron oxide matrices (SiO2/Fe(acac)3/NaF), and to further test it for selenite adsorption. After preparation, the adsorbent material was characterized by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The mechanism associated with the selenium adsorption process has been established based on kinetic, thermodynamic, and equilibrium studies. Pseudo second order is the kinetic model that best describes the obtained experimental data. Also, from the intraparticle diffusion study, it was observed that with increasing temperature the value of the diffusion constant, Kdiff, also increases. Sips isotherm was found to best describe the experimental data obtained, the maximum adsorption capacity being ~6.00 mg Se(IV) per g of adsorbent material. From a thermodynamic point of view, parameters such as ΔG0, ΔH0, and ΔS0 were evaluated, proving that the process studied is a physical one.

Adsorbent Material Based on Carbon Black and Bismuth with Tunable Properties for Gold Recovery.

Adsorption recovery of precious metals on a variety of solid substrates has steadily gained increased attention in recent years. Special attention was paid to the studies on the characterization of the adsorptive properties of materials with a high affinity for gold depending on the nature of the pendant groups present in the structure of the material. The aim of the present work was to synthesize and characterize a new material by using the sol-gel synthesis method (designated as BCb/CB). In this case, synthesis involved the following precursors: bismuth carbonate (III), carbon black, and IGEPAL surfactant (octylphenoxypolyethoxyethanol). Immobilization of the heterojunction as bismuth oxide over a flexible support such as carbon black (CB) can prevent their elution in solution and make it versatile for its use in a system. In this work, a new adsorbent material based on bismuth carbonate supported over carbon black (BCb/CB) was developed and used further for gold recovery from aqueous solutions. The required material was characterized physically/chemically by scanning electron microscopy (SEM); energy dispersive X-ray spectrometry (EDX); X-ray diffraction (XRD); thermal analysis (DTG/DTA); atomic force microscopy (AFM). The Brunauer-Emmett-Teller (BET) method was used to determine the specific surface area indicating a value of approximately 40 m2/g, higher than the surface of CB precursor (36 m2/g). The adsorptive properties and the adsorption mechanism of the materials were highlighted in order to recover Au(III). For this, static adsorption studies were carried out. The parameters that influence the adsorption process were studied, namely: the pH, the contact time, the temperature, and the initial concentration of the gold ions in the used solution. In order to establish the mechanism of the adsorption process, kinetic, thermodynamic, and equilibrium studies were carried out. Experimental data proved that the gold recovery can be conducted with maximum performance at pH 3, at room temperature. Thermodynamic studies proved that the gold adsorption on BCb/CB material is a spontaneous and endothermal process. The results indicate a total adsorption capacity of 13.1 mg Au(III)/g material. By using this material in real solutions, a recovery efficiency of 90.5% was obtained, concomitant with a higher selectivity (around 95%).

Synthesis and Characterisation of Monolacunary Keggin Monovanado-deca-tungstophosphate and Its Complexes with Transition Metal Cations.

Five new complexes with metal cations (Mn2+, Fe3+, Co2+, Ni2+, and Cu2+) of monolacunary Keggin monovanado-deca-tungstophosphate, K8[PVW10O39]·15H2O, have been synthesised. The molar ratio of the combination between metal cations and K8[PVW10O39]·15H2O has been established to be 1:1, and its general molecular formulas were found to be: Kn[MPVW10O39(H2O)]·xH2O (n = 5 for M = Fe3+ and n = 6 for M = Mn2+, Co2+, Ni2+, and Cu2+). Optimal conditions for complexes' synthesis (pH, temperature, and reaction time) have been determined. The characterisation of K8[PVW10O39]·15H2O and of its compounds Kn[MPVW10O39(H2O)]·xH2O have been performed using AAS, TG-DTA-DTG, UV-VIS, IR, Raman, and powder XRD methods. In UV spectra, two maximums of absorption were obtained, at 200 and 250 nm, characteristic of Keggin polycondensate compounds. The coordination of cations Ni2+, Co2+, and Cu2+ through oxygen atoms from K8[PVW10O39]·15H2O in an octahedron system has been reflected with VIS spectroscopy. All these methods have proved the compositions and structures of K8[PVW10O39]·15H2O and Kn[MPVW10O39(H2O)]·xH2O, their similarity with other vanadotungstophosphates, and their achievements in the Keggin class. Additionally, all analysis methods have shown an increase in the degree of structural symmetry and the thermal stability of a polyoxoanion complex after attaching metal cations compared to the monolacunary, K8[PVW10O39]·15H2O.

A Review: Uses of Chitosan in Pharmaceutical Forms.

Chitosan is a natural polysaccharide widespread in nature. It has many unique and attractive properties for the pharmaceutical field: it is biodegradable, safe, hypoallergenic, biocompatible with the body, free of toxicity, with proven anticholesterolemic, antibacterial, and antimycotic action. In this review we highlighted the physical, chemical, mechanical, mucoadhesive, etc. properties of chitosan to be taken into account when obtaining various pharmaceutical forms. The methods by which the pharmaceutical forms based on chitosan are obtained are very extensive, and in this study only the most common ones were presented.

Vanadium (V) Adsorption from Aqueous Solutions Using Xerogel on the Basis of Silica and Iron Oxide Matrix.

Vanadium is considered a strategic metal with wide applications in various industries due to its unique chemical and physical properties. On the basis of these considerations, the recovery of vanadium (V) is mandatory because of the lack of raw materials. Various methods are used to recover vanadium (V) from used aqueous solutions. This study develops a clean and effective process for the recovery of vanadium (V) by using the adsorption method. At the same time, this study synthesizes a material starting from silica matrices and iron oxides, which is used as an adsorbent material. To show the phase composition, the obtained material is characterized by X-ray diffraction showing that the material is present in the amorphous phase, with a crystal size of 20 nm. However, the morphological texture of the material is determined by the N2 adsorption-desorption method, proving that the adsorbent material has a high surface area of 305 m2/g with a total pore volume of 1.55 cm3/g. To determine the efficiency of the SiO2FexOy material for the recovery of vanadium through the adsorption process, the role of specific parameters, such as the L-to-V ratio, pH, contact time, temperature, and initial vanadium concentration, must be evaluated. The adsorption process mechanism was established through kinetic, thermodynamic, and equilibrium studies. In our case, the process is physical, endothermic, spontaneous, and takes place at the interface of SiO2FexOy with V2O5. Following equilibrium studies, the maximum adsorption capacity of the SiO2FexOy material was 58.8 mg (V)/g of material.

Antimicrobial Perspectives of Active SiO2FexOy/ZnO Composites.

The antibacterial activity of zinc oxide particles has received significant interest worldwide, especially through the implementation of technology to synthesize particles in the nanometer range. This study aimed to determine the antimicrobial efficacy of silica-based iron oxide matrix (SiO2FexOy) synthesized with various amounts of ZnO (SiO2FexOyZnO) against various pathogens. It is observed that, with the addition of ZnO to the system, the average size of the porosity of the material increases, showing increasingly effective antibacterial properties. Zinc-iron-silica oxide matrix composites were synthesized using the sol-gel method. The synthesized materials were investigated physicochemically to highlight their structural properties, through scanning electron microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), and Fourier-transform infrared spectroscopy (FT-IR). At the same time, surface area, pore size and total pore volume were determined for materials synthesized using the Brunauer-Emmett-Teller (BET) method. Although the material with 0.0001 g ZnO (600 m2/g) has the highest specific surface area, the best antimicrobial activity was obtained for the material with 1.0 g ZnO, when the average pore volume is the largest (~8 nm) for a specific surface of 306 m2/g. This indicates that the main role in the antibacterial effect has reactive oxygen species (ROS) generated by the ZnO that are located in the pores of the composite materials. The point of zero charge (pHpZc) is a very important parameter for the characterization of materials that indicate the acid-base behaviour. The pHpZc value varies between 4.9 and 6.3 and is influenced by the amount of ZnO with which the iron-silica oxide matrix is doped. From the antimicrobial studies carried out, it was found that for S. aureus the total antibacterial effect was obtained at the amount of 1.0 g ZnO. For Gram-negative bacteria, a total antibacterial effect was observed in S. flexneri (for the material with 0.1 g ZnO), followed by E. coli (for 1.0 g ZnO). For P. aeruginosa, the maximum inhibition rate obtained for the material with 1.0 g ZnO was approximately 49%.

Indium Recovery by Adsorption on MgFe2O4 Adsorbents.

Indium and its compounds have many industrial applications and are widely used in the manufacture of liquid crystal displays, semiconductors, low temperature soldering, and infrared photodetectors. Indium does not have its own minerals in the Earth's crust, and most commonly, indium is associated with the ores of zinc, lead, copper and tin. Therefore, it must be recovered as a by-product from other metallurgical processes or from secondary raw materials. The aim of this study is to investigate the adsorption properties for recovering indium from aqueous solutions using iron-magnesium composite (MgFe2O4). In addition, the results show that the material offers very efficient desorption in 15% HCl solution, being used for 10 adsorption-desorption cycle test. These results provide a simple and effective process for recovering indium. Present study was focuses on the synthesis and characterization of the material by physico-chemical methods such as: X-ray diffraction, FT-IR spectroscopy, followed by the adsorption tests. The XRD indicates that the MgFe2O4 phase was obtained, and the crystallite size was about 8 nm. New prepared adsorbent materials have a point of zero charge of 9.2. Studies have been performed to determine the influence of pH, initial indium solution concentration, material/solution contact time and temperature on the adsorption capacity of the material. Adsorption mechanism was established by kinetic, thermodynamic and equilibrium studies. At equilibrium a maximum adsorption capacity of 46.4 mg/g has been obtained. From kinetic and thermodynamic studies was proved that the studied adsorption process is homogeneous, spontaneous, endothermic and temperature dependent. Based on Weber and Morris model, we can conclude that the In (III) ions takes place at the MgFe2O4/In (III) solution-material interface.

Sodium Alginate-Natural Microencapsulation Material of Polymeric Microparticles.

From the multitude of materials currently available on the market that can be used in the development of microparticles, sodium alginate has become one of the most studied natural anionic polymers that can be included in controlled-release pharmaceutical systems alongside other polymers due to its low cost, low toxicity, biocompatibility, biodegradability and gelatinous die-forming capacity in the presence of Ca2+ ions. In this review, we have shown that through coacervation, the particulate systems for the dispensing of drugs consisting of natural polymers are nontoxic, allowing the repeated administration of medicinal substances and the protection of better the medicinal substances from degradation, which can increase the capture capacity of the drug and extend its release from the pharmaceutical form.

Scandium Recovery from Aqueous Solution by Adsorption Processes in Low-Temperature-Activated Alumina Products.

In this paper, we studied the scandium adsorption from aqueous solutions on the surface of low-temperature-activated alumina products (GDAH). The GDAH samples are industrially manufactured, coming from the Bayer production cycle of the Sierra Leone bauxite as aluminium hydroxide, and further, by drying, milling, classifying and thermally treating up to dehydroxilated alumina products at low temperature. All experiments related to hydroxide aluminium activation were conducted at temperature values of 260, 300 and 400 °C on samples having the following particle sizes: <10 µm, 20 µm, <45 µm and <150 µm, respectively. The low-temperature-activated alumina products were characterised, and the results were published in our previous papers. In this paper, we studied the scandium adsorption process on the above materials and related thermodynamic and kinetic studies.

Silica- Iron Oxide Nanocomposite Enhanced with Porogen Agent Used for Arsenic Removal.

This study aims to remove arsenic from an aqueous medium by adsorption on a nanocomposite material obtained by the sol-gel method starting from matrices of silica, iron oxide and NaF (SiO2/Fe(acac)3/NaF). Initially, the study focused on the synthesis and characterization of the material by physico-chemical methods such as: X-ray diffraction, FT-IR spectroscopy, Raman spectroscopy, atomic force microscopy, and magnetization. Textural properties were obtained using nitrogen adsorption/desorption measurements. The zero load point, pHpZc, was also determined by the method of bringing the studied system into equilibrium. In addition, this study also provides a comprehensive discussion of the mechanism of arsenic adsorption by conducting kinetic, thermodynamic and equilibrium studies. Studies have been performed to determine the effects of adsorbent dose, pH and initial concentration of arsenic solution, material/arsenic contact time and temperature on adsorption capacity and material efficiency. Three theoretical adsorption isotherms were used, namely Langmuir, Freundlich and Sips, to describe the experimental results. The Sips isotherm was found to best describe the experimental data obtained, the maximum adsorption capacity being ~575 µg As(III)/g. The adsorption process was best described by pseudo-second order kinetics. Studies have been performed at different pH values to establish not only the optimal pH at which the adsorption capacity is maximum, but also which is the predominantly adsorbed species. The effect of pH and desorption studies have shown that ion exchange and the physiosorption mechanism are implicated in the adsorption process. From a thermodynamic point of view, parameters such as ΔG°, ΔH° and ΔS° were evaluated to establish the mechanism of the adsorption process. Desorption studies have been performed to determine the efficiency of the material and it has been shown that the material can be used successfully to treat a real-world example of deep water with a high arsenic content.

Highly Efficient Recovery of Ruthenium from Aqueous Solutions by Adsorption Using Dibenzo-30-Crown-10 Doped Chitosan.

Ruthenium, as an industrial by-product or from natural sources, represents an important economical resource due to its specific applications. A complex problem is represented by ruthenium separation during reprocessing operations, therefore, different materials and methods have been proposed. The present study aims to develop a new material with good adsorbent properties able to be used for ruthenium recovery by adsorption from aqueous solutions. Absorbent material was obtained using chitosan (Ch) surface modification with dibenzo-30-crown-10 ether (DB30C10). Chitosan represents a well-known biopolymer with applicability in different adsorptive processes due to the presence of hydroxyl-, carboxyl-, and nitrogen-containing groups in the structure. Additionally, crown ethers are macromolecules with a good complexation capacity for metallic ions. It is expected that the adsorptive efficiency of newly prepared material will be superior to that of the individual components. New synthesized material was characterized using scanning electron microscopy coupled with energy dispersive X-ray (SEM-EDX), Fourier transform infrared spectroscopy (FT-IR), Brunauer-Emmett-Teller surface area analysis (BET), and determination of point of zero charge (pZc). Results obtained from the performed kinetic, thermodynamic, and equilibrium studies confirmed the good adsorptive capacity of the prepared material, Ch-DB30C10, obtaining a maximum adsorption capacity of 52 mg Ru(III) per gram. This adsorption capacity was obtained using a solution with an initial concentration of 275 mg L-1, at pH 2, and 298 K. Ru(III) adsorption kinetics were studied by modeling the obtained experimental data with pseudo-first order and pseudo-second order models. Desorption studies established that the optimum eluent was represented by the 5M HNO3 solution. Based on the performed studies, a mechanism for recovery of ruthenium by adsorption was proposed.

Towards Replacing Titanium with Copper in the Bipolar Plates for Proton Exchange Membrane Water Electrolysis.

For proton exchange membrane water electrolysis (PEMWE) to become competitive, the cost of stack components, such as bipolar plates (BPP), needs to be reduced. This can be achieved by using coated low-cost materials, such as copper as alternative to titanium. Herein we report on highly corrosion-resistant copper BPP coated with niobium. All investigated samples showed excellent corrosion resistance properties, with corrosion currents lower than 0.1 µA cm-2 in a simulated PEM electrolyzer environment at two different pH values. The physico-chemical properties of the Nb coatings are thoroughly characterized by scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS), X-ray photoelectron spectroscopy (XPS), and atomic force microscopy (AFM). A 30 µm thick Nb coating fully protects the Cu against corrosion due to the formation of a passive oxide layer on its surface, predominantly composed of Nb2O5. The thickness of the passive oxide layer determined by both EIS and XPS is in the range of 10 nm. The results reported here demonstrate the effectiveness of Nb for protecting Cu against corrosion, opening the possibility to use it for the manufacturing of BPP for PEMWE. The latter was confirmed by its successful implementation in a single cell PEMWE based on hydraulic compression technology.

Molybdate Recovery by Adsorption onto Silica Matrix and Iron Oxide Based Composites.

Aggressive industrial development over the last century involved different heavy metals being used, including high quantities of molybdenum, which need to be treated before discharge in industrial waters. Molybdenum's market price and industrial applicability make its recovery a big challenge. In the present study the possibility to recover molybdenum ions from aqueous solutions by adsorption on a composite material based on silica matrix and iron oxides-SiO2FexOy-was evaluated. Tests were performed in order to determine the influence of adsorbent material dose, initial solution pH, contact time and temperature over adsorption capacity of synthesized adsorbent material. For better understanding of the adsorption process, the obtained experimental data were modelled using Langmuir, Freundlich and Sips adsorption isotherms. Based on the obtained data, it can proved that the Sips isotherm was describing with better orderliness the studied process, obtaining a maximum adsorption capacity of 10.95 mg MoO42- for each gram of material. By modelling the studied adsorption process, it was proven that the pseudo-second order model is accurately describing the adsorption process. By fitting experimental data with Weber-Morris model, it was proven that MoO42- adsorption is a complex process, occurring in two different steps, one controlled by diffusion and the second one controlled by mass transfer. Further, studies were performed in order to determine the optimum pH value needed to obtain maximum adsorption capacity, but also to determine which are the adsorbed species. From pH and desorption studies, it was proven that molybdate adsorption is a physical process. In order to establish the adsorption mechanism, the thermodynamic parameters (ΔG0, ΔH0 and ΔS0) were determined.

Antimicrobial Activity of Cellulose Based Materials.

Biomaterials available for a wide range of applications are generally polysaccharides. They may have inherent antimicrobial activity in the case of chitosan. However, in order to have specific functionalities, bioactive compounds must be immobilized or incorporated into the polymer matrix, as in the case of cellulose. We studied materials obtained by functionalizing cellulose with quaternary ammonium salts: dodecyl-trimethyl-ammonium bromide (DDTMABr), tetradecyl-trimethyl-ammonium bromide (TDTMABr), hexadecyl-trimethyl ammonium chloride (HDTMACl), some phosphonium salts: dodecyl-triphenyl phosphonium bromide (DDTPPBr) and tri n-butyl-hexadecyl phosphonium bromide (HDTBPBr) and extractants containing sulphur: 2-mercaptobenzothiazole (MBT) and thiourea (THIO). Cel-TDTMABr material, whose alkyl substituent chain conformation was shortest, showed the best antimicrobial activity for which, even at the lowest functionalization ratio, 1:0.012 (w:w), the microbial inhibition rate is 100% for Staphylococcus aureus, Escherichia coli, and Candida albicans. Among the materials obtained by phosphonium salt functionalization, Cel-DDTPPBr showed a significant bactericidal effect compared to Cel-HDTBPBr. For instance, to the same functionalization ratio = 1:0.1, the inhibition microbial growth rate is maximum in the case of Cel-DDTPPBr for Staphylococcus aureus, Escherichia coli, and Candida albicans. At the same time, for the Cel-HDTBPBr material, the total bactericidal effect is not reached even at the functionalization ratio 1:0.5. This behavior is based on the hydrophobicity difference between the two extractants, DDTPPBr and HDTBPBr. Cel-MBT material has a maximum antimicrobial effect upon Staphylococcus aureus, Escherichia coli, and Candida albicans at functionalized ratio = 1:0.5. Cel-THIO material showed a bacteriostatic and fungistatic effect, the inhibition of microbial growth being a maximum of 76% for Staphylococcus aureus at the functionalized ratio = 1:0.5. From this perspective, biomaterials obtained by SIR impregnation of cellulose can be considered a benefit to be used to obtain biomass-derived materials having superior antimicrobial properties versus the non-functional support.

Preparation and Characterization of Chitosan-Alginate Microspheres Loaded with Quercetin.

The aim of this paper was to formulate microspheres based on biodegradable polymers (chitosan and sodium alginate), using the complex coacervation technique. Subsequently, the prepared microspheres were loaded with quercetin (QUE), a pharmacological active ingredient insoluble in water and unstable to light, temperature and air. After preparation, the loaded microspheres underwent several studies for physical chemical characterization (performed by scanning electron microscopy-SEM, laser 3D scanning, and thermal analysis-TA). Furthermore, they were analyzed in order to obtain information regarding swelling index, drug entrapment, and in vitro release capacity. The obtained experimental data demonstrated 86.07% entrapment of QUE into the microspheres, in the case of the one with the highest Ch concentration. Additionally, it was proved that such systems allow the controlled release of the active drug over 24 h at the intestinal level. SEM micrographs proved that the prepared microspheres have a wrinkled surface, with compact structures and a large number of folds. On the basis of the TA analysis, it was concluded that the obtained microspheres were thermally stable, facilitating their usage at normal physiological temperatures as drug delivery systems.