2-(1-methyl-4-((E)-(2-methylbenzylidene)amino)-2-phenyl-1H-pyrazol-3(2H)-ylidene)-hydrazineecarbothioamide (HCB) was synthesized as a corrosion inhibitor from the reaction of 4-aminoantipyrine, thiosemicarbazide and 2-methylbenzaldehyde. The corrosion inhibitory effects of HCB on mild steel in 1.0 M HCl were investigated using potentiodynamic polarization (PDP) and electrochemical impedance spectroscopy (EIS). The results showed that HCB inhibited mild steel corrosion in acidic solution and inhibition efficiency increased with an increase in the concentration of the inhibitor. The inhibition efficiency was up to 96.5% at 5.0 mM. Changes in the impedance parameters suggested that HCB adsorbed on the surface of mild steel, leading to the formation of a protective film. The novel corrosion inhibitor synthesized in the present study was characterized using Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR) spectral data.
An ionic liquid, 1-n-butyl-3-methylimidazolium chloride (BmimCl) was blended with urea at 1:1 mole ratio to create a BmimCl/Urea mixture. The agarose/talc composite films containing the BmimCl/Urea mixture were then acquired through a gelation method. The weight ratio of agarose and talc was fixed at 4:1, while the content of BmimCl/Urea was varied from 0 to 10 wt % relative to the overall weight of the composite films. The tensile stress and modulus results showed the optimum BmimCl/Urea content in the composite film lies at 8 wt %. The talc particles are embedded in the agarose matrix and there are no pullouts for the composite films containing BmimCl/Urea as demonstrated by SEM micrographs. The addition of BmimCl/Urea increased the glass transition temperature of the composite films, however, the thermal decomposition temperature decreased drastically. FTIR and FT-Raman spectra indicated the existence of interaction between agarose and talc, which improves their interfacial adhesion. As a conclusion, a BmimCl/Urea mixture can be utilized as a coupling agent for agarose/talc composite films.
This paper remarks the general correlations of the shape and crystallinity of titanium dioxide (TiO₂) support on gold deposition and carbon monoxide (CO) oxidation. It was found that due to the larger rutile TiO₂ particles and thus the pore volume, the deposited gold particles tended to agglomerate, resulting in smaller catalyst surface area and limited gold loading, whilst anatase TiO₂ enabled better gold deposition. Those properties directly related to gold particle size and thus the number of low coordinated atoms play dominant roles in enhancing CO oxidation activity. Gold deposited on anatase spheroidal TiO₂ at photo-deposition wavelength of 410 nm for 5 min resulted in the highest CO oxidation activity of 0.0617 mmol CO/s.gAu (89.5% conversion) due to the comparatively highest catalyst surface area (114.4 m²/g), smallest gold particle size (2.8 nm), highest gold loading (7.2%), and highest Au⁰ content (68 mg/g catalyst). CO oxidation activity was also found to be directly proportional to the Au⁰ content. Based on diffuse reflectance infrared Fourier transform spectroscopy, we postulate that anatase TiO₂-supported Au undergoes rapid direct oxidation whilst CO oxidation on rutile TiO₂-supported Au could be inhibited by co-adsorption of oxygen.
Halloysite (HNT) is treated with sulfuric acid and the physico-chemical properties of its morphology, surface activity, physical and chemical properties have been investigated when HNT is exposed to sulfuric acid with treatment periods of 1 h (H1), 3 h (H3), 8 h (H8), and 21 h (H21). The significance of this and similar work lies in the importance of using HNT as a functional material in nanocomposites. The chemical structure was characterized by Fourier transform infrared spectroscopy (FTIR). The spectrum demonstrates that the hydroxyl groups were active for grafting modification using sulfuric acid, promoting a promising potential use for halloysite in ceramic applications as filler for novel clay-polymer nanocomposites. From the X-ray diffraction (XRD) spectrum, it can be seen that the sulfuric acid breaks down the HNT crystal structure and alters it into amorphous silica. In addition, the FESEM images reveal that the sulfuric acid treatment dissolves the AlO₆ octahedral layers and induces the disintegration of SiO₄ tetrahedral layers, resulting in porous nanorods. The Bruncher-Emmett-Teller (BET) surface area and total pore volume of HNTs showed an increase. The reaction of the acid with both the outer and inner surfaces of the nanotubes causes the AlO₆ octahedral layers to dissolve, which leads to the breakdown and collapse of the tetrahedral layers of SiO₄. The multi-fold results presented in this paper serve as a guide for further HNT functional treatment for producing new and advanced nanocomposites.
Biological synthesis of nanoparticles is a relatively new emerging field of nanotechnology which has economic and eco-friendly benefits over chemical and physical processes of synthesis. In the present work, for the first time, the brown marine algae Sargassum muticum (S. muticum) aqueous extract was used as a reducing agent for the synthesis of nanostructure silver particles (Ag-NPs). Structural, morphological and optical properties of the synthesized nanoparticles have been characterized systematically by using FTIR, XRD, TEM and UV-Vis spectroscopy. The formation of Ag-NPs was confirmed through the presence of an intense absorption peak at 420 nm using a UV-visible spectrophotometer. A TEM image showed that the particles are spherical in shape with size ranging from 5 to 15 nm. The nanoparticles were crystalline in nature. This was confirmed by the XRD pattern. From the FTIR results, it can be seen that the reduction has mostly been carried out by sulphated polysaccharides present in S. muticum.
In this work, polymer electrolytes have been prepared by doping starch with Sodium Phosphate (Na3PO4). The incorporation of 25% Na3PO4 optimizes the room temperature conductivity of the electrolyte at 7.27 x 10-6 Scm-1. The temperature dependence of conductivity for the electrolyte is Arrhenius and the activation energy, Ea, of 75% corn starch-25% Na3PO4 electrolyte is 0.26eV. The dielectric studies reveal the non-Debye nature of the electrolyte. The complexation of Na3PO4 with the polymer host was studied using Fourier transform infrared (FTIR) spectroscopy.
Magnetic nanocomposites adorned with calixarene were successfully prepared by immobilizing diethanolamine functionalized p-tert-butylcalix[4]arene (DEA-Calix) onto silica-coated magnetic nanoparticles (MNPs). The synthesis, surface morphology, purity, elemental composition and thermal stability of newly prepared nanocomposites were analyzed using FT-IR spectroscopy, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDX), X-ray diffractometer (XRD), thermal gravimetric analysis (TGA) and vibrating sample magnetometer (VSM). Magnetic solid-phase adsorption (MSPA) was employed to explore the adsorption behavior of DEA-Calix-MNPs towards Pb(II) from water samples prior to its flame atomic absorption spectrometric analysis. The essential analytical factors governing the adsorption efficiency such as solution pH, mass of adsorbent, concentration and contact time have been investigated and optimized. The results depict that DEA-Calix-MNPs has excellent adsorption efficiency 97% (at pH 5.5) with high adsorption capacity of 51.81 mg g-1 for Pb(II) adsorption. Additionally, kinetic and equilibrium studies suggested that Pb(II) adsorption process follows a pseudo-second-order model and Langmuir isotherms, respectively. Real sample analysis also confirmed field applicability of the new DEA-Calix-MNPs adsorbent.
A series of glass samples with chemical formula {[(TeO2)0.7(B2O3)0.3]0.7(ZnO)0.3}1-x(Dy2O3)xwhere x=0.01, 0.02, 0.03, 0.04 and 0.05M fraction were synthesized through conventional melt-quenching method. The most common way to fabricate a glass material is by fusion of two or more component oxides followed by their quenching. This technique is known as melt-quenching technique. Kaur et al. (2016) [1] highlighted that the melt-quenching method able to enhance the mechanical properties like hardness and flexural strength of the material. The nature of the glass systems is proven to be amorphous based on the XRD pattern. The FTIR spectra of the glass systems confirm the existence of five bands which are assigned for the BO4, BO3,TeO4and TeO3vibrational groups. The density of the glass systems is increased with the addition of Dy2O3while the molar volume is found to be inversely proportional to the density of the proposed glass. The optical properties of the glasses are determined through the absorption spectra obtained from the UV-VIS spectrophotometer. From the absorption spectra, the indirect and direct optical band gaps and the Urbach energy are found to be inversely proportional to each other. As the molar fraction of the Dy2O3increased, the optical band gaps are observed to increase as opposed to the Urbach energy. For this glass system, the values of refractive index, electronic polarizability, oxide ion polarizability and the optical basicity are found to decrease as the addition of the dysprosium oxide is increased. From the emission spectra, two intense blue and yellow emission bands are observed, which correspond to the4F9/2→6H15/2and4F9/2→6H13/2transitions of Dy3+ions respectively. The CIE chromaticity coordinates of the zinc borotellurite glass systems are found to be located in the white light region.
Trichoderma asperellum (Ta) was first cultured in synthetic medium (Potato Dextrose Broth, PDB) of various concentrations (100, 75, 50, 25%). The biomass was harvested and inoculated into dye solutions (crystal violet, CV; methyl violet, MV; malachite green, MG; and cotton blue, CB). Reduced concentrations (20, 50, 75%) affected growth rate but their decolourization efficacies remained unaffected. This was attributed to similar numbers and types of functional groups (hydroxyl, amine, ester-lipid, alkane groups) found on the surface of fungal biomass, as revealed by the Fourier transformed infrared spectroscopy (FTIR) analysis. Their production of NADH-reductase for degradation, and their biosorption activities were also unaffected. In general, Ta cultured in reduced concentrations (20, 50, 75%) retained the ability to perform biosorption and biodegradation, similar to cultures from control (100% PDB). This suggested that reduced nutrient levels (as a cost-feasible strategy) could be used to cultivate biomass of Ta for dye removal activities.
A magnetic graphene oxide (MGO) was developed for the adsorption of As(III) from aqueous solution. The characteristics of MGO were investigated using Fourier-transform infrared (FTIR), X-ray diffraction and field emission scanning electron microscope-E/energy-dispersive X-ray analyses. Batch adsorption experiments were designed using central composite design, and the effects of adsorbent dosage, pH, contact time and concentration of As(III) were investigated. The MGO showed an excellent performance, removing up to 99.95% of As(III) under the following condition: initial As(III) concentration = 100 mg/L, pH = 7, adsorbent dosage = 0.3 g/L and contact time = 77 min. MGO dosage and initial pH were the most significant parameters influencing the process performance. FTIR analysis of the used adsorbent confirms the adsorption of As(III) through complexation between surface functional groups of the MGO and the oxyanions of As(III). The adsorbent maintained a significant level of performance even after four cycles of adsorption. Thus, the developed MGO has the potential to be used for the abatement of arsenic pollution.
We demonstrate a green chemistry approach to synthesize narrow-sized zerovalent iron (nZVI) nanoparticles using Artocarpus heterophyllus Lam. leaf extract as reducing and capping agent. The produced nZVI was characterized by various instrumental methods including ultraviolet-visible spectra, transmission electron microscopy, vibrating sample magnetometer (VSM), X-ray diffraction, and Fourier transform infrared spectroscopy. Based on the electron microscopy observations, the particle size was estimated to be ∼30 nm. In VSM, the saturation point of magnetization was observed to be 0.6 emu g-1 under a magnetic field of 0 ± 30 kOe. The synthesized nZVI was amorphous in nature as per the XRD results. The catalytic activity of the nZVI was employed for the catalytic reduction of 4-nitrophenol (4-NP) and decoloration of textile dyes such as methylene blue, methyl orange, and malachite green, respectively. The proposed nZVI synthesis method exhibited better catalytic performance toward reduction of 4-NP and degradation of dyes within 4 min for 0.1 mg of catalyst. Moreover, the synthesized catalyst nZVI can be recoverable and reutilized in many cycles without loss of its significant catalytic activity. The synthesized nZVI could be a promising material to treat industrial wastewater via profitable, sustainable, and ecofriendly approaches.
Phaleria macrocarpa, known as "Mahkota Dewa", is a widely used medicinal plant in Malaysia. This study focused on the characterization of α-glucosidase inhibitory activity of P. macrocarpa extracts using Fourier transform infrared spectroscopy (FTIR)-based metabolomics. P. macrocarpa and its extracts contain thousands of compounds having synergistic effect. Generally, their variability exists, and there are many active components in meager amounts. Thus, the conventional measurement methods of a single component for the quality control are time consuming, laborious, expensive, and unreliable. It is of great interest to develop a rapid prediction method for herbal quality control to investigate the α-glucosidase inhibitory activity of P. macrocarpa by multicomponent analyses. In this study, a rapid and simple analytical method was developed using FTIR spectroscopy-based fingerprinting. A total of 36 extracts of different ethanol concentrations were prepared and tested on inhibitory potential and fingerprinted using FTIR spectroscopy, coupled with chemometrics of orthogonal partial least square (OPLS) at the 4000-400 cm-1 frequency region and resolution of 4 cm-1. The OPLS model generated the highest regression coefficient with R2Y = 0.98 and Q2Y = 0.70, lowest root mean square error estimation = 17.17, and root mean square error of cross validation = 57.29. A five-component (1+4+0) predictive model was build up to correlate FTIR spectra with activity, and the responsible functional groups, such as -CH, -NH, -COOH, and -OH, were identified for the bioactivity. A successful multivariate model was constructed using FTIR-attenuated total reflection as a simple and rapid technique to predict the inhibitory activity.
The current study aimed to investigate the efficiencies and mechanisms of slag filter media for removing phosphorus from synthetic wastewater. The steel slag with high ferric oxides (Fe2O3) was subjected for the electric arc furnace (EAF) and selected as the filter media (HFe). The chemical characteristics of HFe were determined using pH, point of zero charge (PZC) and XRF. The phosphorus removal efficiency was studied in a designed vertical steel slag column rock filters in unaerated HFe (UEF) and aerated HFe (AEF) system. The microstructure of HFe was analyzed by FTIR, XRD and SEM-EDX analysis. The results of XRF revealed that ferric oxide (Fe2O3) ranged from 26.1 to 38.2%. PZC for Filter HFe was recorded at pH 10.55 ± 0.27. The highest efficiencies were recorded by UEF and AEF systems at pH 3 and pH 5 (89.97 ± 4.02% and 79.95 ± 6.25% at pH 3 and 72.97 ± 8.38% and 66.00 ± 12.85% at pH 5 for UEF and AEF, respectively). These findings indicated that AEF exhibiting higher removal than UEF systems might be due to presence high Fe concentration in AEF which play important role in the phosphorus removal. The main elements available on the surface of HFe included carbon, oxygen, iron, calcium, magnesium, silicon, platinum, sulphur, manganese, titanium and aluminium. The XRD analysis indicated that the precipitation of orthophosphate as calcium and iron-phosphates was the removal mechanism as confirmed using FT-IR analysis. These findings demonstrated the efficiency of HFe in removing of phosphorus from wastewater.
Nowadays, the current synthesis techniques used in industrial production of nanoparticles have been generally regarded as nonenvironmentally friendly. Consequently, the biosynthesis approach has been proposed as an alternative to reduce the usage of hazardous chemical compounds and harsh reaction conditions in the production of nanoparticles. In this work, pure, iron (Fe)-doped and silver (Ag)-doped zinc oxide (ZnO) nanoparticles were successfully synthesized through the green route using Clitoria ternatea Linn. The optical, chemical, and physical properties of the biosynthesized ZnO nanoparticles were then analyzed by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), UV-Vis diffuse reflectance spectroscopy (DRS), zeta potential measurement, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and surface analysis. The biosynthesized ZnO nanoparticles were crystallized with a hexagonal wurtzite structure and possessed smaller particle sizes than those of commercially or chemically produced samples. The existence of biomolecules to act as reducing and stabilizing agents from C. ternatea Linn aqueous extract was confirmed using FTIR analysis. The biosynthesized ZnO nanoparticles mainly comprised of negatively charged groups and responsible for moderately stable dispersion of the nanoparticles. All these properties were favorable for the sonocatalytic degradation of Congo red. Sonocatalytic activity of ZnO nanoparticles was studied through the degradation of 10 mg/L Congo red using ultrasonic irradiation at 45 kHz and 80 W. The results showed that the sonocatalytic degradation efficiency of Congo red in the presence of biosynthesized ZnO nanoparticles prepared at 50 °C for 1 h could achieve 88.76% after 1 h. The sonocatalytic degradation efficiency of Congo red in the presence of Ag-doped ZnO was accelerated to 94.42% after 10 min which might be related to the smallest band gap energy (3.02 eV) and the highest specific surface area (10.31 m2/g) as well as pore volume (0.0781 cm3/g). Lastly, the biosynthesized ZnO nanoparticles especially Ag-doped ZnO offered significant antibacterial potential against Escherichia coli which indicated its ability to inhibit the normal growth and replication of bacterial cells. These results affirmed that the biosynthesized ZnO nanoparticles could be used as an alternative to the current chemical compounds and showed a superior sonocatalytic activity toward degradation of Congo red.
The photostabilization of polyvinyl chloride (PVC) films by Schiff bases was investigated. Polyvinyl chloride films containing 0.5 wt % Schiff bases were produced using the same casting method as that used for additive-free PVC films from tetrahydrofuran (THF) solvent. The photostabilization activities of these compounds were determined by monitoring the carbonyl, polyene and hydroxyl indices with irradiation time. The changes in viscosity average molecular weight of PVC with irradiation time were also monitored using THF as a solvent. The quantum yield of chain scission (Φcs) for the studied complexes in PVC was estimated to range between 4.72 and 8.99 × 10(-8). According to the experimental results, several mechanisms were suggested, depending on the structure of the additive. Ultra violet (UV) absorption, peroxide decomposition and radical scavenging were suggested as the photostabilizing mechanisms.
Semiconductor metal oxide with TiO2 nanoparticles removes hazardous compounds from environmental samples. TiO2 nanoparticles have shown potential as an efficient photocatalyst by being employed as a nano-catalyst for the breakdown of organic contaminants in wastewater samples. To separate substances from contaminated samples, combined UV and visible light irradiation has been used. Sol-gel synthesis was used to produce a copper chromite-titanium nanocomposite, which was then evaluated using analytical methods, such as XRD, BET, DRS-UV, and FT-IR. Using visible light, the photocatalytic activity of a nanocomposite made of CuCr2O4 and TiO2 was investigated for its role in the breakdown of malachite green. The effects of several parameters, including pH change, anions presence, contact time, catalyst amount, concentration variation, and the kinetics of photocatalytic degradation were investigated. The magnitude of transition energy calculated using UV-DRS spectra was found to be 3.1 eV for CuCr2O4-TiO2 nanocomposite. Maximum degradation was observed at pH 7.0. The surface area and pore volume of the co-doped samples of Cr2O4 - TiO2 obtained from BET were found to be 6.1213 m2/g and 0.045063 cm3/g respectively. The average particle size of the catalyst of the nano-catalysts calculated from XRD was found to be 8 nm for TiO2 and 66 nm for TiO2-CuCrO4. The peaks obtained in FTIR between the range of 900-500 cm-1 were due to the presence of an aromatic compound. The binding mechanism of a dye molecule to the surface of CuCr2O4-TiO2 nanocomposite was analysed using quantum chemical calculations with the self-consistent reaction field technique employing integral equation formalism for the polarized continuum method and the UFF atomic radii set.
Calix[4]arene/polyurethane (C4PU) has been synthesized and characterized as an alternative adsorbent for the adsorption of methylene blue (MB) and malachite green (MG) dyes from the aqueous solution. C4PU was synthesized by reacting p-tert-butyl calix[4]arene with hexamethylene diisocyanate (HMDI) as the cross-linking agent. Different polymer ratios were synthesized, and C4PU-4 shows better adsorption than other ratios. The polymer was characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), Brunauer-Emmett-Teller (BET) analysis, and point of zero charges (pHPZC). The isotherms and kinetics of the adsorption of MB and MG were studied under a range of experimental conditions, including pH, adsorbent dosage, initial dye concentration, and contact time. The adsorption was determined by the adsorption percentage of MB and MG dyes from the solution. The Langmuir isotherm model best describes the adsorption process for both dyes, and it follows a pseudo-second-order kinetic model, with the maximum adsorption capacity (qmax) of MB and MG, respectively, was found to be 1.991 mg·g-1 and 2.240 mg·g-1.
Water bodies with the dye methylene blue pose serious environmental and health risks to humans. Therefore, the creation and investigation of affordable, potential adsorbents to remove methylene blue dye from water resources as a long-term fix is one focus of the scientific community. Food plants and other carbon-source serve as a hotspot for a wider range of application on different pollutants that impact the environment and living organisms. Here, we reviewed the use of treated and untreated biosorbents made from plant waste leaves for removing the dye methylene blue from aqueous media. After being modified, activated carbon made from various plant leaves improves adsorption performance. The range of activating chemicals, activation methods, and bio-sorbent material characterisation using FTIR analysis, Barunauer-Emmett-Teller (BET) surface area, scanning electron microscope (SEM-EDX), and SEM-EDX have all been covered in this review. It has been thoroughly described how the pH solution of the methylene blue dye compares to the pHPZC of the adsorbent surface. The presentation also includes a thorough analysis of the application of the isotherm model, kinetic model, and thermodynamic parameters. The selectivity of the adsorbent is the main focus of the adsorption kinetics and isotherm models. It has been studied how adsorption occurs, how surface area and pH affect it, and how biomass waste compares to other adsorbents. The use of biomass waste as adsorbents is both environmentally and economically advantageous, and it has been discovered to have exceptional color removal capabilities.
Development of strategies for removing heavy metals from aquatic environments is in high demand. Cadmium is one of the most dangerous metals in the environment, even under extremely low quantities. In this study, kenaf and magnetic biochar composite were prepared for the adsorption of Cd2+. The synthesized biochar was characterized using (a vibrating-sample magnetometer VSM), Scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). The adsorption batch study was carried out to investigate the influence of pH, kinetics, isotherm, and thermodynamics on Cd2+ adsorption. The characterization results demonstrated that the biochar contained iron particles that help in improving the textural properties (i.e., surface area and pore volume), increasing the number of oxygen-containing groups, and forming inner-sphere complexes with oxygen-containing groups. The adsorption study results show that optimum adsorption was achieved under pH 5-6. An increase in initial ion concentration and solution temperature resulted in increased adsorption capacity. Surface modification of biochar using iron oxide for imposing magnetic property allowed for easy separation by external magnet and regeneration. The magnetic biochar composite also showed a higher affinity to Cd2+ than the pristine biochar. The adsorption data fit well with the pseudo-second-order and the Langmuir isotherm, with the maximum adsorption capacity of 47.90 mg/g.
Plant leaf litter has a major role in the structure and function of soil ecosystems as it is associated with nutrient release and cycling. The present study is aimed to understand how well the decomposing leaf litter kept soil organic carbon and nitrogen levels stable during an incubation experiment that was carried out in a lab setting under controlled conditions and the results were compared to those from a natural plantation. In natural site soil samples, Anacardium. occidentale showed a higher value of organic carbon at surface (1.14%) and subsurface (0.93%) and Azadirachta. indica exhibited a higher value of total nitrogen at surface (0.28%) and subsurface sample (0.14%). In the incubation experiment, Acacia auriculiformis had the highest organic carbon content initially (5.26%), whereas A. occidentale had the highest nitrogen level on 30th day (0.67%). The overall carbon-nitrogen ratio showed a varied tendency, which may be due to dynamic changes in the complex decomposition cycle. The higher rate of mass loss and decay was observed in A. indica leaf litter, the range of the decay constant is 1.26-2.22. The morphological and chemical changes of soil sample and the vermicast were substantained using scanning electron microscopy (SEM) and Fourier transmission infrared spectroscopy (FT-IR).