Fourier Transform Infrared Spectral Research Articles

Synthesis, characterization, magnetic and morphological properties of poly(m-phenylenediamine)/ZnCoFe2O4 nanocomposites

In this work, poly(m-phenylenediamine) (PmPD)/ZnCoFe2O4 nanocomposites (NCs) were synthesised by in-situ chemical oxidative polymerisation method. The ZnCoFe2O4 nanoparticles (NPs) were prepared by auto-combustion method. The crystalline size of PmPD/ZnCoFe2O4 NCs and ZnCoFe2O4 NPs were calculated using the Powder X-ray diffraction (XRD) analysis. The functional group of the samples was analysed by Fourier transform infrared spectral (FTIR) analysis. The XRD and FTIR results were clearly indicated that the formation of PmPD/ZnCoFe2O4 NCs. The spherical morphology of the PmPD/ZnCoFe2O4 NCs was confirmed through Field emission electron microscopy (FESEM). The magnetic hysteresis (M-H) loops of ZnCoFe2O4 NPs and PmPD/ZnCoFe2O4 NCs were revealed their ferromagnetic behaviour. Thermogravimetric analysis (TGA) was indicated that thermal stability of PmPD/ZnCoFe2O4 NCs increases with increase in concentration of ZnCoFe2O4 NPs. The dielectric properties of PmPD/ZnCoFe2O4 NCs were also examined with different frequency.

Enhanced Treatment of Potato Starch Wastewater Using Chitosan-Modified Biochar Film Adsorption Coupled with Ultrafiltration

Potato starch wastewater, a byproduct of potato processing, is an escalating environmental concern due to its high concentrations of COD (chemical oxygen demand), ammonia nitrogen, and total phosphorus (TP). Addressing this challenge, this research introduced a novel method combining chitosan-modified biochar film (CBC) adsorption with subsequent ultrafiltration. SEM (scanning electron microscope), FTIR (Fourier transform infrared spectral), XRD (X-ray diffractometer), and BET (specific surface area) analyses validated CBC’s enhanced surface characteristics, confirming successful chitosan (CS) film impregnation. CBC exhibited superior adsorption capacities, especially 40%wt-CBC, optimizing COD removal at 79.8%, ammonia nitrogen at 93.3%, and TP at 91.2%. Kinetic studies associated the adsorption process with a pseudo-second-order model, highlighting chemical adsorption. Additionally, the Langmuir isotherm model suggested monolayer adsorption with no inter-adsorbate interactions. The treated effluent, post adsorption, was directed through an ultrafiltration membrane, ensuring water quality suitable for reuse. This integrative treatment not only offers an effective solution for potato starch wastewater management but also underscores the potential for sustainable water resource recovery in the food processing sector.

Formulation of Intranasal Mucoadhesive Thermotriggered In Situ Gel Containing Mirtazapine as an Antidepressant Drug.

The purpose of the present work was to develop nanoemulsion-based formulations of mirtazapine for intranasal delivery using a spray actuator to target the brain for treating depression. Research on the solubility of medications in different oils, surfactants, co-surfactants, and solvents has been done. Using pseudo-ternary phase diagrams, the various ratios of the surfactant and co-surfactant mix were computed. Thermotriggered nanoemulsion was formulated using different concentrations of poloxamer 407 (i.e., 15%, 15.5%, 16%, 16.5% up to 22%). Similarly, mucoadhesive nanoemulsion using 0.1% Carbopol and water-based plain nanoemulsions were also prepared for comparative assessment. The developed nanoemulsions were analyzed for physicochemical properties, i.e., physical appearance, pH, viscosity, and drug content. Drug-excipient incompatibility was determined by Fourier transform infrared spectral (FTIR) analysis and differential scanning calorimetry (DSC). In vitro drug diffusion studies were conducted for optimized formulations. Among the three formulations, RD1 showed the highest percentage of drug release. Ex vivo drug diffusion studies were conducted on freshly excised sheep nasal mucosa with Franz diffusion cell simulated nasal fluid (SNF) for all three formulations up to 6 h, and the thermotriggered nanoemulsion (RD1) showed 71.42% drug release with 42.64 nm particle size and a poly dispersity index of 0.354. The zeta potential was found to be -6.58. Based on the above data, it was concluded that thermotriggered nanoemulsion (RD1) has great potential to be used as an intranasal gel for treating depression in patients. It can offer great benefits by reducing dosing frequency and improving bioavailability of mirtazapine by direct nose-to-brain delivery.

Synthesis, characterization with optical property of Zn-O NPs using sol-gel route in alkaline medium

Zn-O nanoparticles were successfully synthesized by sol-gel route using ZnSO4.7H2O as precursor in alkaline medium. Structural, morphological and optical property of Zn-O NPs was analyzed. Zn-O NPs were characterized by using X-ray diffraction (XRD), Fourier transform infrared spectral (FTIR), UV-Visible spectrophotometer, scanning electron microscopy (SEM) and Energy Dispersive X-ray analysis (EDAX).XRD pattern shows the purity of synthesized Zn-O nanoparticles particle size. Scanning electron microscopy (SEM) observations revealed remarkable change in morphological structure of Zn-O NPs. Analysis studies was confirmed, the functional groups and chemical bonding present in the synthesized Zn-O nanoparticles.

Novel orange-red emitting Pr3+ doped CeO2 nanopowders for white light emitting diode applications

A new orange-red emitting praseodymium doped cubic CeO2 phosphor powders were fabricated via simple green combustion route utilizing Aloe vera gel as fuel. The prepared powders structural, morphological and optical properties were studied in detail. From the Rietveld refinement technique the powder X-ray diffraction (PXRD) matching profile was simulated and the cubic crystal diagram was depicted with the help of Diamond 2.0 software. The morphology of the prepared powders was studied with variation of the bio-fuel Aloe vera gel. The particle size was calculated by means of Transmission electron microscope (TEM) and it was found to be ~250 nm. Fourier transform infra-red spectral (FTIR) studies reveal the strong stretching vibrations between the molecules. The optical energy band gap (Eg) of the prepared powders was estimated by utilizing the diffuse reflectance spectral (DRS)studies. The Eg values were found to be in the range of 3.33–3.46 eV. The photoluminescence (PL) excitation spectra were recorded in the range 350–600 nm. Among the observed peaks the intense one was found at 463 nm corresponds to 3H4→3P2 transition. The PL emission spectrum shows a prominent orange emission peak centered at 608 nm along with weak intense peak at 650 nm corresponds to 3P0→3H6 and 3P0→3F2 transitions of Pr3+ ions respectively. The PL intensity upsurges upto 5 mol% of dopant concentration and thereafter it decreases due to concnetration quenching phenomena. The CIE color coordinates were estimated for optimum concentration (0.594, 0.379) and which falls in the orange-red region of the chromaticity map. The average correlated color temperature (CCT) was also assessed and it was observed to be ~6046 K, specifies that the fabricated nanopowders can be used as cool LED sources such as household lighting applications. The color purity was found to be 97% for optimum powders. The QE efficiency of prepared samples were found to be 86%. These combined results indicate that the fabricated phosphor powders can be efficiently utilized as orange-red component in the fabrication of white light illuminating devices.

EFFECT OF Ni-DOPING ON THE STRUCTURAL AND OPTICAL PROPERTIES OF ZnO NANOPARTICLES PREPARED BY CHEMICAL PRECIPITATION METHOD

Undoped ZnO nano particles and Ni doped ZnO nanoparticles prepared by chemical precipitation method and assessed for their structural, morphological and optical properties. The prepared undoped and Ni doped ZnO nanoparticles were characterized by using X-ray diffraction (XRD), Fourier transform infrared spectral (FTIR), UV-Visible spectrophotometer, Scanning electron microscopy (SEM) and Energy Dispersive X-ray analysis (EDAX), Photoluminescence spectra (PL). XRD pattern shows the purity of prepared undoped and Ni doped ZnO nanoparticles size. Scanning electron microscopy (SEM) observations revealed remarkable change in morphology of the prepared samples. The presence of functional groups and chemical bonding was confirmed by FTIR and UV analysis. The defect states were revealed from the UV and visible emissions of the photoluminescence spectra.

EFFECT OF Ni-DOPING ON THE STRUCTURAL AND OPTICAL PROPERTIES OF ZnO NANOPARTICLES PREPARED BY CHEMICAL PRECIPITATION METHOD

Undoped ZnO nano particles and Ni doped ZnO nanoparticles prepared by chemical precipitation method and assessed for their structural, morphological and optical properties. The prepared undoped and Ni doped ZnO nanoparticles were characterized by using X-ray diffraction (XRD), Fourier transform infrared spectral (FTIR), UV-Visible spectrophotometer, Scanning electron microscopy (SEM) and Energy Dispersive X-ray analysis (EDAX), Photoluminescence spectra (PL). XRD pattern shows the purity of prepared undoped and Ni doped ZnO nanoparticles size. Scanning electron microscopy (SEM) observations revealed remarkable change in morphology of the prepared samples. The presence of functional groups and chemical bonding was confirmed by FTIR and UV analysis. The defect states were revealed from the UV and visible emissions of the photoluminescence spectra.

Development of Nickel Doped Zinc Ferrite Nanocomposites as Magnetically Recoverable Catalytic Material for The Synthesis of Biphenyl Methane

Magnetically active nickel doped zinc ferrite nanoparticles with chemical composition NixZn1-xFe2O4 (x- 0.0, 0.25, 0.5, 0.75 and 1.0) were successfully synthesized by sol-gel auto-combustion method using high purity metal nitrates and ethylene glycol as gelling agent. The prepared samples were characterized by X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), X-ray Fluorescence (XRF) and Fourier Transform Infra-Red spectral (FTIR) analyses. TEM images and particle size distribution profile reveals the agglomeration tendency during nickel doping suggest the magnetic nature of particles. The remarkable change in the magnetic behaviour of nickel doped zinc ferrite samples provide an easy recovery and regeneration of the material and thus making an excellent candidate for benzylation reaction without any remarkable fall in the catalytic performance for repeated cycles.

Effect of bio-additives on physico-chemical properties of fly ash-ground granulated blast furnace slag based self cured geopolymer mortars.

Heat curing catalyzed the geopolymerization reaction in geopolymers whereas the practical challenges in applying heat curing process limited the applications of geopolymers to precast elements alone. Bio-additives inclusion could facilitate ambient temperature curing that lead to environment friendly self cured geopolymers. Natural sugars (molasses/palm jaggery/honey) and terminalia chebula were used as bio-additives in fly ash (FA) and ground granulated blast furnace slag (GGBS) based geopolymer mortars. X-ray diffraction (XRD), Fourier transform infrared spectral (FTIR), thermogravimetric (TG/DTG) and scanning electron microscopic (SEM) studies were used for the characterization for all geopolymer mortar samples. Physico-chemical test results of bio-additives added FA-GGBS based self cured geopolymer mortar samples showed XRD peaks at 2θ = 20°, 26°, 39°, 48°, 66° and 75°, FTIR bands at 3430, 2922, 1390, 1270, 1120 and 881cm-1, DTG peaks at 120 °C, 126 °C and 134 °C that led to the conclusion that development of differences in geopolymer reaction products, intense structural reorganization leading to stable geopolymer matrix and more ordered geopolymer gels. Further SEM observations revealed compact and dense microstructure development in bio-additives added FA-GGBS based self cured geopolymer mortar samples.

Experimental and Theoretical Investigation of Thiazolyl Blue as a Corrosion Inhibitor for Copper in Neutral Sodium Chloride Solution

The anticorrosion effect of thiazolyl blue (MTT) for copper in 3% NaCl at 298 K was researched by electrochemical methods, scanning electron-microscopy (SEM), and atomic force microscopy (AFM). The results reveal that MTT can protect copper efficiently, with a maximum efficiency of 95.7%. The corrosion inhibition mechanism was investigated by X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectral (FT-IR), and theoretical calculation. The results suggest that the MTT molecules are adsorbed on metal surface forming a hydrophobic protective film to prevent copper corrosion. It also indicates that the MTT and copper form covalent bonds. The molecular dynamic simulation further gives the evidence for adsorption. The adsorption isotherm studies demonstrate that a spontaneous, mixed physical and chemical adsorption occurs, which obeys Langmuir adsorption isotherm. The present research can help us better understand the corrosion inhibition process and improve it.

Nanoparticles of type Fe3O4-SiO2-graphene oxide and coated with an amino acid-derived ionic liquid for extraction of Al(III), Cr(III), Cu(II), Pb(II) prior to their determination by ICP-OES

An amino acid derived ionic liquid, Fe3O4 nanoparticles and graphene oxide (GO) were used to prepare a material for the magnetic solid phase extraction (MSPE) of the ions Al(III), Cr(III), Cu(II) and Pb(II). The material was characterized by Fourier transform infrared spectral (FT-IR), scanning electron microscopy (SEM), thermal gravimetric analysis (TGA), magnetic analysis and isoelectric point (pI) analysis. It is shown to be a viable sorbent for the separation of these metal ions. Single factor experiments were carried out to optimize adsorption including pH values, ionic strength, temperature and solution volume. Following desorption with 0.1 M HCl, the ions were quantified by inductively coupled plasma optical emission spectrometry. Under the optimum conditions, the method provides a linear range from 10 to 170 μg· L−1 for Al(III); from 4.0 to 200 μg· L−1 for Cr(III); from 5.0 to 170 μg· L−1 for Cu(II); and from 5.0 to 200 μg· L−1 for Pb(II). The limits of detection (LOD) are 6.2 ng L−1 for Al(III); 1.6 ng L−1 for Cr(III); 0.52 ng L−1 for Cu(II); and 30 ng L−1 for Pb(II). Method performance was investigated by determination of these ions in (spiked) environmental water and gave recoveries in the range of 89.1%–117.8%.

Electrochemical and in vitro bioactivity of polypyrrole/ceramic nanocomposite coatings on 316L SS bio-implants

The present investigation describes the versatile fabrication and characterization of a novel composite coating that consists of polypyrrole (PPy) and Nb2O5 nanoparticles. Integration of the two materials is achieved by electrochemical deposition on 316L stainless steel (SS) from an aqueous solution of oxalic acid containing pyrrole and Nb2O5 nanoparticles. Fourier transform infrared spectral (FTIR) and X-ray diffraction (XRD) studies revealed that the existence of Nb2O5 nanoparticles in PPy matrix with hexagonal structure. Surface morphological analysis showed that the presence of Nb2O5 nanoparticles strongly influenced the surface nature of the nanocomposite coated 316L SS. Micro hardness results revealed the enhanced mechanical properties of PPy nanocomposite coated 316L SS due to the addition of Nb2O5 nanoparticles. The electrochemical studies were carried out using cyclic polarization and electrochemical impedance spectroscopy (EIS) measurements. In order to evaluate the biocompatibility, contact angle measurements and in vitro characterization were performed in simulated body fluid (SBF) and on MG63 osteoblast cells. The results showed that the nanocomposite coatings exhibit superior biocompatibility and enhanced corrosion protection performance over 316L SS than pure PPy coatings.

Preparation, Characterization and Photocatalytic Properties of Al-Doped TiO<sub>2</sub> Nanomaterials

Al-doped TiO2 nanomaterials were prepared via hydrothermal synthesis method using tetrabutyl titanate. The photocatalytic performace of Al-doped TiO2 with different doping ratios were studied using 150 W tungsten halogen lamp as visible light source and phenol as pollutant. The results indicated that Al-doped TiO2 showed higher photocatalytic activities than that of pure TiO2, the optimum molar constant of aluminum ion doping was 5%, and it exhibited the highest photodegradation efficiency. Then X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and fourier transform infrared spectral (FTIR) were used to research their properties.

Crystal phase of poly(vinylidene fluoride‐co‐trifluoroethylene) synthesized via hydrogenation of poly(vinylidene fluoride‐co‐chlorotrifluoroethylene)

AbstractTrifluoroethylene addition and thermal treatment induced crystal phase transition in a series of poly(vinylidene fluoride‐co‐trifluoroethylene) [P(VDF‐co‐TrFE)] containing varied TrFE molar ratio (6, 9, 12, and 20 mol %) prepared from the hydrogenation of poly(vinylidene fluoride‐co‐chlorotrifluoroethylene have been investigated by means of Fourier transform infrared spectral (FTIR), X‐ray diffraction (XRD), and differential scanning calorimetry (DSC) analyses. The comprehensive applications of the three techniques could distinguish α, β and γ phase of P(VDF‐co‐TrFE) very well. The multipeak fitting technique of DSC is successfully applied to calculate the percentage of different phases in the samples, which allows us to investigate the phase transition process of P(VDF‐co‐TrFE) precisely. It is found that the crystal phase of P(VDF‐co‐TrFE) films is turned from α + γ phase (6 mol % TrFE) to α + γ + β phase (9 and 12 mol % TrFE) to β phase (20 mol % TrFE) at high temperature, and from α + γ phase (6 mol % TrFE) to γ + β phase (9 mol % TrFE) to β phase (>12 mol % TrFE) at low fabricated temperature. Both the fabrication conditions and TrFE addition are responsible for the crystal phase transition of the hydrogenised P(VDF‐co‐TrFE). © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013

Synthesis, Chemical Modification and Tribological Evaluation of Plant oil as Bio-Degradable Low Temperature Lubricant

An increasing demand for environmentally acceptable lubricant has led researchers to look to plant oils as an alternative to petroleum based lubricants. These plant oil based products are sustainable, renewable and biodegradable that can replace petroleum derived products in numerous industrial applications such as stabilizers, plasticizers, cutting fluids, automotive lubricants and in coating formulations. For formulation of bio-degradable lubricants, crude rapeseed oil, methyl ester of sunflower oil, palm oil and rapeseed oil were selected and to this bio-additive package were added to improve some of the properties. Various tribological studies of the formulated lubricants were evaluated then it is compared with conventional synthetic lubricant SAE20W40. However plant oils are limited by their poor low temperature fluidity and poor oxidative stability. In order to produce rapeseed oil based bio-lubricant with good oxidative stability and low pour point, in the present work the raw rapeseed oil was chemically modified via, epoxidation and hydroxylation process. The formation of the epoxidized group was confirmed by Fourier Transform Infrared spectral (FTIR) analysis. Epoxidized rapeseed oil showed superior oxidative stability, lower pour point and friction reducing ability compared to base oil.

Methodologies for the extraction and analysis of konjac glucomannan from corms of Amorphophallus konjac K. Koch

Abstract Here we present a comparison of commonly used methodologies for the extraction and quantification of konjac glucomannan (KGM). Compositional analysis showed that the purified konjac flour (PKF) produced using a modified extraction procedure contained 92% glucomannan, with a weight average molecular weight ( M w ), polydispersity index (PDI) and degree of acetylation (DA) of 9.5 ± 0.6 × 10 5 g mol −1 , 1.2 and 2.8 wt.%. These data, plus Fourier-transform infrared spectral (FTIR) and zero shear viscosity analyses of the extract (PKF) were all consistent with the literature. Comparison of three existing methodologies for the quantitative analysis of the KGM content of the PKF, namely 3,5-dinitrosalicylic acid (3,5-DNS), phenol–sulphuric acid and enzymatic colorimetric assays; indicated that the 3,5-DNS colorimetric assay was the most reproducible and accurate method, with a linear correlation coefficient of 0.997 for samples ranging from 0.5 to 12.5 mg/ml, and recoveries between 97% and 103% across three spiking levels (250, 500 and 750 μg/g) of starch. These data provide the basis of improved good laboratory practice (GLP) for the commercial extraction and analysis of this multifunctional natural polymer.

Evaluation of orlistat solid dispersion using poloxomer 188 as hydrophilic carrier

Objective: The objective of the present investigation was to improve the dissolution rate of Orlistat (ORL), a poor water-soluble anti-obesity drug by solid dispersion technique. Materials and Methods: To improve the solubility and dissolution, ORL solid dispersion was formulated using a hydrophilic polymeric carrier poloxomer 188. Solid dispersion was formulated by kneading method and physicochemical characterization and in vitro release study was carried out. Results: Fourier transform infrared spectral (FT-IR) and Differential scanning calorimetry (DSC) study showed a change in the crystalline nature of the drug, and its conversion into amorphous form. The in vitro dissolution study of physical mixture and solid dispersion both showed enhanced solubility as compared to the pure active drug. Conclusion: This study suggests that ORL solid dispersion having drug: Carrier (1:5) could be a promising approach to improve the solubility and dissolution.

Influences of Organic Ligands on the Microstructure and Properties of Sol–Gel Antimony-Doped Tin Oxide Thin Films

The antimony-doped tin oxide (ATO) thin films were prepared by sol-gel dip-coating process from SnCl2 2H2O and SbCl3 in alcoholic solutions. The influences of organic ligands, including acetic acids (HAc), acetic acids with monoethanolamine (in brief HAc + MEA), and acetic acids with acetylacetone (in brief HAc + AcAc), on the the microstructure and electrical properties of the thin films have been investigated. The thermal behavior of the ATO gels powders and the microstructures of the thin films have been characterized by using thermogravimetric (TG), differential scanning calorimetric (DSC), Fourier transform infra-red spectral (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) analysis. The electrical resistivity of the thin films was detected by four-probe instrument measurement. The thin films with HAc + MEA as coordination ligands had a good crystal quality and showed a preferred orientation along (101) plane when heated at 450 degrees C. As a consequence, it exhibited the best electrical performance. An electrical resistivity of about 6.3 x 10(-3) omega cm could be achieved for the films with 500 nm thickness.

Structural evolution process of isotactic polypropylene in the isothermal crystallization from the melt

The melt-isothermal crystallization behaviour has been investigated for isotactic polypropylene (iPP) by means of time-resolved simultaneous measurements of small-angle X-ray scattering (SAXS) and wide-angle X-ray diffraction (WAXD) using synchrotron radiation source in SPring-8. The time-resolved Fourier-transform infrared spectral (FTIR) measurements were also performed to clarify the formation process of helices. The SAXS data were analyzed on the basis of Guinier (isolated domains) and Debye-Bueche (correlated domains) theories and correlation function (stacked lamellae). The results were combined with the FTIR data, allowing us to draw the concrete structural evolution process including the formation of regular helices and their growth, the correlation of higher density domains consisting of these helices, and the increment of correlation between the neighbouring lamellae to build up the stacked lamellar structure of higher crystallinity.

An Examination of the Sequence of Intersecting Lines Using Attenuated Total Reflectance–Fourier Transform Infrared Spectral Imaging*

In this study, the potential of attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectral imaging as a technique to determine the sequence of line crossings was examined. The technique was successful in determining the sequence of heterogeneous line intersections produced using ballpoint pens and laser printers. By imaging at characteristic frequencies, it was possible to form spectral images showing the spatial distribution of the materials. By examining the spectral images from the inks, it was possible to determine whether the ink was above or below the toner. In blind testing, ATR-FTIR spectral imaging results were directly compared to those obtained by eight experienced forensic document examiners using methods regularly employed in casework. ATR-FTIR spectral imaging was shown to achieve a 100% success rate in the blind tests, whereas some incorrect sequence determinations were made by the forensic document examiners when using traditional techniques. The technique was unable to image ink-jet printing, gel pens, roller ball pens, and felt-tip pens, and was also unable to determine the sequence of intersecting ballpoint pen lines.