Synthesis and Catalytic Evaluation of Silver Nanoparticles Synthesized with <Emphasis Type="Italic">Aloysia triphylla</Emphasis> Leaf Extract

In this investigation, we report the biosynthesis of the silver nanoparticles using Aloysia triphylla leaves extract. The as-prepared silver nanoparticles were characterized by ultraviolet–visible (Uv–vis) spectroscopy, X-ray diffractometry, scanning electron microscopy and transmission electron microscopy The infrared spectroscopy (FTIR) and Raman spectroscopy techniques were also used to evaluate the chemical groups of the plant extract involved in the silver ions bioreduction. The results indicate that as the plant extract/precursor salt ratio increases, the size of the nanoparticles decreases. Also, as the reaction temperature increases, the reduction rate increased too, resulting in the formation of smaller nanoparticles-size ranges. Uv–vis spectroscopy illustrates absorption peaks in the range of wavelengths of 430–445 nm corresponding to surface plasmon resonance band of silver nanoparticles. The X-ray diffraction (XRD) confirmed the presence of silver solids with fcc structure type. The FTIR analysis showed that the bands corresponding to phenolic compounds and the amide group were involved in the synthesis and stabilization of silver nanoparticles, respectively. The Raman studies showed bands at 1380 and 1610 cm^?1, which correspond to the aromatic and amide compounds, confirming the FTIR results. The Uv–vis results indicate the capacity of silver nanoparticles to reduce the methylene blue.     

Structure and Stability of Gold Nanoparticles Synthesized Using <Emphasis Type="Italic">Schinus molle</Emphasis> L. Extract

In this work, we exhibited the results of the green synthesis of gold nanoparticles by aqueous extract of Schinus molle L. leaves. The chemical reaction was carried out by varying the plant extract/precursor salt ratio concentration in the aqueous solution. The structural characterization of the nanoparticles was performed using X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). XRD analysis showed that the as-synthesized AuNPs have a face-centered cubic structure. SEM and TEM observations indicated that most of the obtained particles have multiple twinning structures (MTP). The synthesized Au-MTP have particle sizes in the range of 10–60 nm, most of them with an average size of about 24 nm. However, triangular Au plate particles were also obtained, having an average size of 180 nm. Fourier transforms infrared spectroscopy and shows that the functional groups responsible for the chemical reduction of AuNPs are phenolic compounds present in the S. molle L. leaf.     

Thermal characterization of dried extract of medicinal plant by DSC and analytical techniques

The increased search for herbal products has generated an increasing interest in improving the quality control of dried extracts by pharmaceutical industry since these are raw materials of great importance by their quality and versatility. This work aimed at the application of various analytical techniques (thermal analysis, X-ray diffraction, scanning electron microscopy, and infrared Fourier transform spectroscopy) in the characterization of dried extracts of two plants from the Brazilian semiarid region with medicinal properties. The DSC curves for the dried extracts of Ximenia americana L. and Schinopsis brasiliensis Engl. showed that thermal processes occur between 33.50 and 118.58 °C and between 39.17 and 126.14 °C. The X-ray powder diffraction revealed high degree of amorphization, but the dried extract of X. americana L. showed some diffraction peaks of high intensity. The IR spectra showed high variety of metabolites in the extracts dried. Through this study it was possible to verify the feasibility of applying these techniques in the characterization of raw materials from medicinal plants for use in the herbal medicines production.     

Ag nanoparticles decorated Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>/chitosan nanocomposite: synthesis,characterization and application toward electrochemical sensing of hydrogen peroxide

We studied a rapid, sensitive and selective amperometric sensor for determination of hydrogen peroxide by electrodeposited Ag NPs on a modified glassy carbon electrode (GCE). The modified GCE was constructed through a step by step modification of magnetic chitosan functional composite (Fe₃O₄–CH) and high-dispersed silver nanoparticles on the surface. The resulted Ag@Fe₃O₄–CH was characterized by various analytical methods including Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, scanning electron microscopy and cyclic voltammetry. The proposed sensor employed Ag@Fe₃O₄–CH/GCE as the working electrode with a linear current response to the hydrogen peroxide concentration in a wide range from 0.01 to 400 µM with a low limit of detection (LOD = 0.0038 µM, S/N = 3). The proposed sensor showed superior reproductivity, sensitivity and selectivity for the detection of hydrogen peroxide in environmental and clinical samples.     

Thermal stability of gamma-irradiated polyurethane/POSS hybrid materials

Through temperature-programmed pyrolysis, the physicochemical properties of Pteria martensii (PM) before and after calcination are investigated. Our results show that the mass loss is 11.02% from room temperature to 600 °C with an average mass loss rate of 0.19% per min. The decomposition of organics coupling with the phase transition of calcium carbonate from aragonite to calcite occurs in the range of 367.4–423.0 °C, as confirmed by X-ray diffraction and Fourier transform infrared spectroscopy analyses. The decomposition pores and channels are changed forming complex porous structures. The surface of sample shows a much rougher fracture, with higher C, O and N element concentrations. At the stage of decomposition and phase transition of organics, the average activation energy value is 118.78 kJ mol^?1. This study provides valuable information on the calcination process and calcined PM for use in medicines.     

A High-Performance Catalytic and Recyclability of Phyto-Synthesized Silver Nanoparticles Embedded in Natural Polymer

The present work deals with phytogenic synthesis of Ag NPs in the natural polymer alginate as support material using Aglaia elaeagnoidea leaf extract as a reducing, capping, and stabilizing agent. Ag nanoparticles embedded in alginate were characterized using UV–Vis absorption spectroscopy, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, transmission electron microscopy techniques and selected area electron diffraction techniques. The formation of AgNPs embedded in the polymer was in spherical shape with an average size of 12 nm range has been noticed. The prepared embedded nanoparticles in polymer were evaluated as a solid heterogeneous catalyst for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) and methylene blue to leuco methylene blue in the liquid phase using sodium borohydride (NaBH₄) as reducing agent. The silver nanoparticles embedded polymer exhibited extraordinary catalytic efficacy in reduction of 4-NP to 4-AP and the rate constant is 0.5054 min^?1 at ambient conditions. The catalyst was recycled and reused up to 10 cycles without significant loss of catalytic activity. The preparation of Ag–CA composite was facile, stable, efficient, eco-friendly, easy to recycle, non-toxic, and cost effective for commercial application.     

Green Synthesis of Silver Nanoparticles Using Water Extract from Galls of <Emphasis Type="Italic">Rhus Chinensis</Emphasis> and Its Antibacterial Activity

The green synthesis of silver nanoparticles (AgNPs) has been proposed as a simple, eco-friendly and cost effective alternative to chemical and physical methods. The Rhus chinensis plant is one of the well studied medicinal plant and its galls find excellent clinical and therapeutic applications. The present study reports the use of water extract from galls of R. chinensis as a reducing agent and formation of AgNPs from silver nitrate solution by a green synthesis route. The AgNPs formation was observed visually by color change and the absorbance peak at 450 nm was observed by UV–Visible spectrophotometer. The shape, size, and morphology of synthesized AgNPs were monitored by transmission electron microscopy and field-emission scanning electron microscopy. The face centered cubic structure of AgNPs was confirmed by X-ray diffraction pattern and element composition by energy dispersive X-ray analysis. The Fourier transform infrared spectroscopy spectrum revealed that the presence of components acts as a reducing and capping agent. The antibacterial activity was performed using the agar well diffusion method. Minimum inhibitory concentration and minimum bactericidal concentration were determined by broth dilution and spread plate method respectively. Synthesized nanoparticles were spotted as triangular and hexagonal shape and the particle size was around 150 nm.     

A Novel Green Synthesis of Silver Nanoparticles Using <Emphasis Type="Italic">Rubus crataegifolius</Emphasis> Bge Fruit Extract

We report a facile, cost effective, and environmentally friendly green chemistry method for preparing silver nanoparticles (AgNPs) using Rubus crataegifolius bge (RCB) fruit extract. The amount of the fruit extract used was found to be important parameters in the growth of AgNPs. In this study, the effect of RCB fruit extract on the synthesis of AgNPs was studied using UV–Vis spectroscopy, transmission electron microscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction (XRD), and dynamic light scattering analyses were performed to characterize the RCB fruit extract-stabilized AgNPs. The formation of the AgNPs was confirmed by the color change of the reaction medium and the absorbance peak observed at 420 nm. The XRD analysis confirmed the face centered cubic structure of the AgNPs. The catalytic property of the as-synthesized AgNPs was analyzed for the reduction of 4-nitrophenol to 4-aminophenol.     

Delapril and manidipine characterization and purity evaluation in raw materials

This study characterizes the solid-state of delapril hydrochloride (DEL) and manidipine dihydrochloride (MAN) raw materials using different analytical techniques. DEL (D1 and D2) and MAN (M1 and M2) were obtained from different suppliers and submitted to differential scanning calorimetry (DSC), thermogravimetry (TG), X-ray powder diffraction (XRPD), diffuse reflectance infrared Fourier transform spectroscopy (DRIFT), Raman spectroscopy (RS), and scanning electron microscopy (SEM). For DEL, the TG/DTG analysis demonstrated three stage of mass loss between 140 and 402 °C. Different DSC curve profiles with melting points at 182.8 °C for D1 and 170.1 °C for D2 were verified. Moreover, incompatible results were also obtained in RS and SEM analysis for this drug. Nevertheless, when analyzed by liquid chromatography (LC), an additional peak was detected, demonstrating that the differences observed can be related to an impurity present in D2 sample and not to a possible polymorphism (as confirmed by XRPD). On the other hand, for MAN evaluation, all results were similar, showing that there were no differences between M1 and M2 samples. Besides the solid-state evaluation, the techniques employed in this study could also be used for quality control, stability studies, and for qualification of raw materials suppliers. Furthermore, for purity evaluations, complementary methods (such as DSC) can be useful, since there are impurities that don’t have UV/Vis absorbance, leading to absence of signal in LC–UV methodologies.     

Aqueous extract of <Emphasis Type="Italic">Argemone mexicana</Emphasis> roots for effective protection of mild steel in an HCl environment

The inhibition effect of aqueous Argemone mexicana root extract (AMRE) on mild steel corrosion in 1 M HCl has been studied by weight loss, Tafel polarization curves, electrochemical impedance spectroscopy, scanning electron microscopy (SEM), and atomic force microscopy techniques. Results indicate that inhibition ability of AMRE increases with the increasing amount of the extract. A maximum corrosion inhibition of 94 % is acknowledged at the extract concentration of 400 mg L^?1. Polarization curves and impedance spectra reveal that both cathodic and anodic reactions are suppressed due to passive layer formation at the metal–acid interface. It is also confirmed by SEM micrographs and FTIR studies. Furthermore, the effects of acid concentration (1–5 M), immersion time (120 h) and temperature (30–60 °C) on inhibition potential of AMRE have been investigated by the weight loss method and electrochemical techniques. An adsorption mechanism is also proposed on the basis of weight loss results, which shows good agreement with the Langmuir isotherm.     

Ultra‐fast liquid chromatography coupled with electrospray ionization time‐of‐flight mass spectrometry for the rapid phenolic profiling of red maple (Acer rubrum) leaves

The red maple (Acer rubrum) species is economically important to North America because of its sap, which is used to produce maple syrup. In addition, various other red maple plant parts, including leaves, were used as a traditional medicine by the Native Americans. Currently, red maple leaves are being used for nutraceutical and cosmetic applications but there are no published analytical methods for comprehensive phytochemical characterization of this material. Herein, a rapid and sensitive method using liquid chromatography with electrospray ionization time‐of‐flight tandem mass spectrometry was developed to characterize the phenolics in a methanol extract of red maple leaves and a proprietary phenolic‐enriched red maple leaves extract (Maplifa™). Time‐of‐flight mass spectrometry and tandem mass spectrometry experiments led to the identification of 106 phenolic compounds in red maples leaves with the vast majority of these compounds also detected in Maplifa™. The compounds included 68 gallotannins, 25 flavonoids, gallic acid, quinic acid, catechin, epicatechin, and nine other gallic acid derivatives among which 11 are potentially new and 75 are being reported from red maple for the first time. The developed method to characterize red maple leaves phenolics is rapid and highly sensitive and could aid in future standardization and quality control of this botanical ingredient.     

Cesium removal from solution using PAN-based potassium nickel hexacyanoferrate (II) composite spheres

A polyacrylonitrile–potassium nickel hexacyanoferrates composite adsorbent was prepared to remove cesium ion in aqueous solution. The dual nozzle technique was applied to prepare a composite sphere. The physicochemical behavior of the ion exchanger was specified with different techniques including Fourier transform infrared spectroscopy, X-ray powder diffraction, specific surface analysis, scanning electron microscopy, and X-ray fluorescence spectroscopy analysis. The effects of contact time, solution initial pH, presence of various cations and initial cesium concentration on the adsorption was also investigated and the optimum conditions for separation of cesium were determined. In addition, adsorption kinetics and adsorption mechanism were studied by modeling the experimental data and related parameters were also evaluated, which showed that sorption data fitted to pseudo-second-order and film diffusion models. Adsorption isotherm in batch experiments showed that the sorption data were successfully fitted with Langmuir model. Finally the adsorption dynamic capacities of the synthesized composite in column experiments were evaluated at 139.925 and 119.539 mg/g for flow rate of 1 and 3 BV/min, respectively.     

Biosynthesis,characterization, and antimicrobial effect of silver nanoparticles obtained using <Emphasis Type="Italic">Lavandula</Emphasis> × <Emphasis Type="Italic">intermedia</Emphasis>

The use..... of aqueous leaf extract of Lavandula × intermedia for biosynthesis of silver nanoparticles (AgNPs) is presented. The plant extract was obtained by boiling dried leaves and using the obtained filtrate for the synthesis of AgNPs. The study was conducted to investigate an ecofriendly approach to metal nanoparticle synthesis and to evaluate the antimicrobial potential of both the aqueous plant extract and resulting silver nanoparticles against different microbes using the disc diffusion method. The synthesis of silver nanoparticles was monitored using ultraviolet–visible (UV–v is) spectroscopy, which showed a localized surface plasmon resonance band at 411 nm and a shift of the band to higher wavenumber of 422 nm after 90 min of reaction. Powder X-ray diffraction analysis and transmission electron microscopy of the obtained AgNPs revealed their crystalline nature, with average size of 12.6 nm. Presence of elemental silver was further confirmed by energy-dispersive X-ray spectroscopy. Fourier-transform infrared spectroscopy confirmed presence of phytochemicals from Lavandula × intermedia leaf extract on the AgNPs. The AgNPs showed good antimicrobial activity with inhibition zone ranging from 10 to 23 mm; the largest inhibition zone (23 mm) occurred against Escherichia coli. Generally, the AgNPs displayed more antimicrobial activity against all investigated pathogens compared with Lavandula × intermedia leaf extract, and were also more active than streptomycin against Klebsiella oxytoca and E. coli at the same concentration. The silver nanoparticles showed prominent antimicrobial activity with a lowest minimum inhibitory concentration (MIC) value of 15 μg/mL against E. coli, K. oxytoca, and Candida albicans.     

Preparation and Characterization of NiO Nanoparticles via Solid-State Thermal Decomposition of Ni(II) Complex

Nickel(II) complex, Ni(Brsalph)(NO₃) was synthesized and characterized by elemental analyses and Fourier-transformed infrared (FT-IR) spectroscopy. Heating of Ni(Brsalph)(NO₃) at 550 °C for 3.5 h have resulted NiO nanoparticles. Fourier-transformed infrared spectrum confirmed the composition of products. The crystalline structures and morphology of NiO nanoparticles were studied by X-ray powder diffraction, scanning electron microscopy and transmission electron microscopy.     

Fabrication of magnetite nanoparticles (Fe3O4-NPs) for catalytic pyrolysis of nutshells biomass

The fabrication of nanoparticles has been perused as a topic of critical importance in the present decades. Biosynthesis of nanoparticles employs plants extract instead of harmful chemicals. These plant extracts act as reducing and capping agents which is the most appropriate and eco-friendly method among all the preparative routs. In present study, the magnetite nanoparticles (Fe₃O₄-NPs) were fabricated using rapid, single step and benign biosynthetic rout by reduction of ferric nitrate nonahydrate solution with Ferocactus echidne aqueous extract containing ascorbic acid as a main reducing and capping agent. The structural and morphological properties of prepared iron oxide nanoparticles were investigated by Powder X-ray diffraction and scanning electron microscopy. The size of the synthesized nanoparticles was approximately 15 ± 2 nm as determined by Scherrer equation. The biosynthetically fabricated nanoparticles were employed as catalyst for pyrolysis of nutshells to produce biofuel. Catalytic pyrolysis of biomass yields biofuel as an alternative source of energy and chemical feed stock. Effect of temperature, heating rate, and amount of catalyst were investigated on conversion percentage and product yields. Aniline point, carbon residue, and cetane number of prepared bio-oil were also determined.     

Biogenic synthesis from <Emphasis Type="Italic">Prunus</Emphasis> × <Emphasis Type="Italic">yedoensis</Emphasis> leaf extract,characterization, and photocatalytic and antibacterial activity of TiO<Subscript>2</Subscript> nanoparticles

Green synthesis of TiO₂ nanoparticles (NPs) from Prunus × yedoensis leaf extract (PYLE), and their application for removal of phosphate and their antibacterial activity, were studied for the first time. NPs were obtained using a green chemistry approach from 0.1 M TiO₂ and PYLE at ratio of 1:1 (v/w). Initial confirmation of production of TiO₂ NPs was provided by a color change from white to light yellow, then calcination was performed at 500 °C for 1 h. The TiO₂ NPs were characterized using various analytical techniques such as ultraviolet–visible (UV–Vis) spectroscopy, X-ray diffraction analysis, Fourier-transform infrared spectroscopy, Raman spectroscopy, UV–Vis diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy, and high-resolution transmission electron microscopy. The results indicated that the optimal amount of TiO₂ NPs for removal of phosphate was 10 mg/l (10 ppm) with duration of 25 min. Furthermore, the antibacterial activity of TiO₂ NPs was also investigated using two different bacteria (Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli) in aqueous medium. The results revealed highly efficient sunlight-driven photocatalytic and antibacterial activity of TiO₂ NPs.     

Synthesis of Gd<Subscript>0.5</Subscript>Sr<Subscript>0.5</Subscript>FeO<Subscript>3</Subscript> perovskite-type nanopowders for adsorptive removal of MB dye from water

In the present study, nanoparticles of perovskite-type Gd_0.5Sr_0.5FeO₃ (GSFO) were fabricated by a sol–gel method. A series of analytical techniques were used to characterize the crystallinity, morphology, specific surface area and grain size of GSFO powders. The thermal decomposition process of the complex precursor was examined by means of differential thermal analysis–thermal gravimetric analysis. X-ray diffraction results showed that a single perovskite phase was completely formed after calcination at 700 °C. In addition, transmission electron microscopy images revealed that the average size of the particles is approximately 35.23 nm in diameter. The surface morphology and composition of these nanopowders were also investigated using a scanning electron microscope and an energy dispersive X-ray spectrometer. GSFO nanoparticles showed excellent adsorption efficiency towards methylene blue dye in aqueous solution. The adsorption studies were carried out at different pH values, initial dye concentrations, various adsorbent doses and contact time in batch experiments. The dye removal efficiency was found to be increased with increasing the initial pH of the dye solution, and GSFO exhibited good dye removal efficiency at a basic pH, especially at a pH of 12. Experimental results indicated that the adsorption kinetic data follow a pseudo-second-order rate for the tested dye. The isotherm evaluations revealed that the Redlich–Peterson model attained better fits to the experiment's equilibrium data than the Langmuir, Freundlich, Temkin, and Dubinin–Radushkevich models.     

TG–DSC–FTIR–MS study of gaseous compounds evolved during thermal decomposition of styrene-butadiene rubber

The thermal decomposition behavior of styrene-butadiene rubber was studied using a system equipped with thermogravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, and mass spectroscopy. Two different experiments were conducted. From these experiments, thermogravimetric analysis results indicated a mass loss of 58 % in the temperature range of ~290–480 °C and a mass loss of 39 % in the temperature range beyond 600 °C. Scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy confirmed the presence of oxides, even at 1,000 °C, accounting for the Zn, Mg, Al, Si, and Ca in the original sample.     

ZnS nanoparticles capped with watermelon rind extract and their potential application in dye degradation

We report fabrication of stable ZnS nanoparticles (NPs) using a green chemistry concept with watermelon rind extract as capping and stabilizing agent. The cubic structure of the NPs was evidenced by X-ray powder diffraction analysis and electron diffraction studies. Dynamic light scattering and high-resolution transmission electron microscopy studies revealed that the average size of the ZnS NPs was <12 nm. The bandgap of the ZnS nanocrystals was found to be 3.42 eV using ultraviolet–visible (UV–Vis) spectroscopy studies. The energy-dispersive X-ray spectrum of the fabricated ZnS NPs confirmed the elemental Zn and S signals without peaks from any impurities. The biomolecular capping of the ZnS NPs was analyzed using Fourier-transform infrared spectroscopy. An illustrative stabilization mechanism for the ZnS NPs is given using citrulline, a major phytochemical in watermelon rind extract. The obtained ZnS NPs showed good photocatalytic activity towards methylene blue dye degradation.     

Characterization of herbal medicine with different particle sizes using pyrolysis GC/MS, SEM, and thermal techniques

Analytical techniques have been used to characterize compounds from herbal medicine, its products and extracts. The objective of this study was to characterize a variety of particle sizes of Erythrina velutina Willd powder. The samples used in the study were named MUF01 (710 μm), MUF03 (180 μm) and MUF05 (75 μm). The techniques employed were scanning electron microscopy (SEM), thermal analysis such as thermogravimetry (TG) and differential thermal analysis (DTA) together with pyrolysis coupled to gas chromatography/mass spectrometry (Pyr-GC/MS). SEM enabled us to detect the existence of divergences from the expected results from the granulometry process. Thermal analytical techniques (TG and DTA) showed the thermal decomposition profile, corresponding to physical and chemical phenomena. The chromatographic data relative to the peak area of the compounds analyzed evidenced quantitative differences in the chemical compositions of the samples MUF01, MUF03, and MUF05 at 300, 450 and 600 °C. Neophytadiene 2,6,10-trimethyl, 14 and 3-eicosyne were identified by Pyr-GC/MS at 300, 450 and 600 °C, and it classified the samples according the peak area values, which were MUF05 > MUF03 > MUF01. SEM, DTA and TG confirmed this through particle size uniformity, heat flow, and mass loss, respectively.