Thermoplastic starch (TPS) hybrid bio-composite films containing microcrystalline cellulose (C) and nano-bentonite (B) as hybrid fillers were studied to replace the conventional non-degradable plastic in packaging applications. Raw oil palm empty fruit bunch (OPEFB) was subjected to chemical treatment and acid hydrolysis to obtain C filler. B filler was ultra-sonicated for better dispersion in the TPS films to improve the filler-matrix interactions. The morphology and structure of fillers were characterized by scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). TPS hybrid bio-composite films were produced by the casting method with different ratios of B and C fillers. The best ratio of B/C was determined through the data of the tensile test. FTIR analysis proved the molecular interactions between the TPS and the hybrid fillers due to the presence of polar groups in their structure. XRD analysis confirmed the intercalation of the TPS chains between the B inter-platelets as a result of well-developed interactions between the TPS and hybrid fillers. SEM images suggested that more plastic deformation occurred in the fractured surface of the TPS hybrid bio-composite film due to the higher degree of stretching after being subjected to tensile loading. Overall, the results indicate that incorporating the hybrid B/C fillers could tremendously improve the mechanical properties of the films. The best ratio of B/C in the TPS was found to be 4:1, in which the tensile strength (8.52MPa), Young's modulus (42.0 MPa), elongation at break (116.4%) and tensile toughness of the film were increased by 92%, 146%, 156% and 338%, respectively. The significantly improved strength, modulus, flexibility and toughness of the film indicate the benefits of using the hybrid fillers, since these features are useful for the development of sustainable flexible packaging film.
The 2,2-diphenyl-1-picryl hydrazyl (DPPH) radical, nitric oxide, reducing power, hydrogen peroxide scavenging, and total antioxidant activities of the methanol extract, n-hexane, dichloromethane, ethyl acetate, butanol and aqueous fractions of the seed of Telfairia occidentalis were evaluated. Total phenolic content was determined using the Folin-Ciocalteu method. The dichloromethane fraction exhibited the highest DPPH radical scavenging, reducing power and total antioxidant activities. Two pure compounds which were identified by FTIR, H-and 2D NMR and Mass spectroscopy as 9-octadecenoic acid (TOS B) and 10-hydroxyoctadecanoic acid (TOS C) and four oily isolates, TOS A, TOS D, TOS E and TOS F were obtained from the dichloromethane fraction. TOS E had the highest DPPH radical scavening activity comparable to that of ascorbic acid. GC-MS analysis revealed the major compounds in TOS E as 4-(2,2-Dimethyl-6-methylene cyclohexylidene)-2-butanol; 3-(3-hydroxybutyl)-2,4,4-trimethyl-2-cyclohexene-1-one and 1,2-Benzenedicarboxylic acid disooctyl ester. Thus, the seed of T. occidentalis can be consumed for its antioxidant property.
The identification, characterization and quantification of crystal forms are becoming increasingly important within the pharmaceutical industry. A combination of different physical analytical techniques is usually necessary for this task. In this work solid-state techniques, diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and X-ray powder diffractometry (XRPD) were combined to analyze polymorphic purity of crystalline ranitidine-HCl, an antiulcer drug, H2 receptor antagonists. A series of 12 different mixtures of Form 1 and 2 was prepared by geometric mixing and their DRIFT spectra and XRD powder patterns were obtained and analyzed, either alone or combined together, using Artificial Neural Networks (ANNs). A standard feed-forward network, with back-propagation rule and with multi layer perceptron architecture (MPL) was chosen. A working range of 1.0-100% (w/w) of crystal Form 2 in Form 1 was established with a minimum quantifiable level (MQL) of 5.2% and limit of detection of 1.5% (w/w). The results demonstrate that DRIFTS combined with XRPD may be successfully used to distinguish between the ranitidine-HCl polymorphs and to quantify the composition of binary mixtures of the two.
Nickel (Ni), cobalt (Co), and zinc (Zn) loaded on fibrous silica KCC-1 was investigated for CO2 methanation reactions. Ni/KCC-1 exhibits the highest catalyst performance with a CH4 formation rate of 33.02 × 10-2 molCH4 molmetal-1 s-1, 1.77 times higher than that of Co/KCC-1 followed by Zn/KCC-1 and finally the parent KCC-1. A pyrrole adsorption FTIR study reveals shifting of perturbed N-H stretching decreasing slightly with the addition of metal oxide, suggesting that the basic sites of catalyst were inaccessible due to metal oxide deposition. The strengths of basicity were found to follow sthe equence KCC-1, Ni/KCC-1, Zn/KCC-1, and Co/KCC-1. The data were supported by N2 adsorption desorption analysis, where Co/KCC-1 displayed the greatest reduction in total surface area whereas Ni/KCC-1 displayed the least reduction. The elucidation of difference mechanism pathways has also been studied by in situ IR spectroscopy studies to determine the role of different metal oxides in CO2 methanation. It was discovered that Ni/KCC-1 and Co/KCC-1 follow a dissociative mechanism of CO2 methanation in which the CO2 molecule was dissociated on the surface of the metal oxide before migration onto the catalyst surface. This was confirmed by the evolution of a peak corresponding to carbonyl species (COads) on a metal oxide surface in FTIR spectra. Zn/KCC-1, on the other hand, showed no such peak, indicating associative methanation pathways where a hydrogen molecule interacts with an O atom in CO2 to form COads and OH. These results offers a better understanding for catalytic studies, particularly in the field of CO2 recycling.
The hazardous dyes on mixing with water resources are affecting many life forms. Granite stone is popular worldwide for decorating floors, making other forms of decorative materials and items. Granite stone powder waste can be obtained free of cost from marble factories as factories spend on the disposal of this waste. In the present study, novel granite stone powder waste composite has been prepared and utilized for the effective removal of Terasil dye. Two types of granite including gray granite and white granite were used in pure, calcinized, and chemically modified forms. Freundlich adsorption isotherm model best explained the adsorption mechanism of dye removal using granite composites as compared to other adsorption isothermal models. Characterization techniques like scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) spectroscopy were used for the determination of morphological features and functional groups of granite composites. The obtained results were statistically analyzed using analysis of variance (ANOVA) along with the post hoc Tukey test. An extraordinarily high Terasil dye uptake capacity (more than 400 mg/g) was exhibited by granite composites prepared using sodium metasilicate. The synthesized novel nano-constructed composites provided a viable strategy as compared to the pure granite stone for dye removal from wastewater water.
This paper reports a computational approach for analysis of FTIR spectra where peaks are detected, assigned and matched across samples to produce a peak table with rows corresponding to samples and columns to variables. The algorithm is applied on a dataset of 103 spectra of a broad range of edible oils for exploratory analysis and variable selection using Self Organising Maps (SOMs) and t-statistics, respectively. Analysis on the resultant peak table allows the underlying patterns and the discriminatory variables to be revealed. The algorithm is user-friendly; it involves a minimal number of tunable parameters and would be useful for analysis of a large and complicated FTIR dataset.
A series of fibrous aminated adsorbents for CO2 adsorption were prepared by covalent incorporation of poly (glycidyl methacrylate) (PGMA) by graft copolymerization of GMA onto electron beam (EB) irradiated polyethylenepolypropylene (PE/PP) fibrous sheets and subsequent amination with ethylenediamine (EDA), diethylenetriamine (DETA), or tetraethylenepentamine (TEPA). The physico-chemical properties of the adsorbents were evaluated using Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermogravimetric (TGA), X-ray diffraction (XRD), and Brunauer-Emmett-Teller (BET) analysis. All the adsorbents displayed typic primary and secondary amine features combined with a decrease in both of crystallinity and surface area of PE/PP, and such a decrease was higher in adsorbents with longer aliphatic chain of the amine. Of all adsorbents, TEPA-containing fibres showed the highest CO2 adsorption capacity and thus was further investigated for CO2 capture from CO2/CH4 mixtures of different gas ratios under various pressures and temperatures. The selectivity of CO2 over CH4 and equilibrium isotherms, kinetics, and thermodynamics of the adsorption on the fibrous aminated adsorbent were all investigated. The Sips model was found to best fit the isotherm of CO2 adsorption suggesting the presence of a combination of monolayer and multilayer adsorptions. The adsorption kinetic data was found to best fit Elovich model reflecting chemisorption. The ΔG°, ΔS°, and ΔH° showed positive values suggesting that the adsorption of CO2 on the present fibrous adsorbent was non-spontaneous with an increase in randomness implying that the process was endothermic. Overall, it can be suggested that PE/PP-g-PGMA/TEPA adsorbent has a strong potential for separation of CO2 from NG.
Penicillium simplicissimum (isolate 10), a metal tolerant fungus, tolerated 1000 mg/L Cu and 500 mg/L Zn, but were inhibited by Cd (100 mg/L), evident by the Tolerance Index (TI) of 0.88, 0.83, and 0.08, respectively. Live cells of P. simplicissimum were more effective in removing Cr (88.6%), Pb (73.7%), Cu (63.8%), Cd (33.1%), and Zn (28.3%) than dead cells (5.3-61.7%). Microscopy approach via SEM-EDX and TEM-EDX suggested that metal removal involved biosorption and bioaccumulation, with metal precipitates detected on the cell wall, and in the cytoplasm and vacuoles. FTIR analysis revealed metals interacted with amino, carbonyl, hydroxyl, phosphoryl (except Cd) and nitro groups in the cell wall. Biosorption and bioaccumulation of metals by live cells reduced Cu and Pb toxicity, observed from good root and (4.00-4.28 cm) and shoot (8.07-8.36 cm) growth of Vigna radiata in the phytotoxicity assay.
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.
Gamma-ray radiation was used as a clean and easy method for turning the physicochemical properties of graphene oxide (GO) in this study. Silane functionalized-GO were synthesized by chemically grafting 3-aminopropyltriethoxysilane (APTES) and 3-glycidyloxypropyltrimethoxysilane (GPTES) onto GO surface using gamma-ray irradiation. This established non-contact process is used to create a reductive medium which is deemed simpler, purer and less harmful compared conventional chemical reduction. The resulting functionalized-GO were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), thermogravimetric analysis (TGA), and Raman spectroscopy. The chemical interaction of silane with the GO surface was confirmed by FT-IR. X-ray diffraction reveals the change in the crystalline phases was due to surface functionalization. Surface defects of the GO due to the introduction of silane mioties was revealed by Raman spectroscopy. Thermogravimetric analysis of the functionalized-GO exhibits a multiple peaks in the temperature range of 200-650 °C which corresponds to the degradation of chemically grafted silane on the GO surface.
Some cortical bone specimens from the femurs of adult cows and sea coral of Porites species were studied by using Fourier Transform Infrared Spectroscopy, FTIR. Carbonate were shown to be present by indication of C-O stretch found between 1510-1410 cm -1 in both cortical bone and Porites. Based on the comparison of the relative intensity of CO3 2- bands with respect to the PO4 3- bands, peak intensity of Porites was found to be higher than peak intensity of cortical bone at carbonate band. This explains that Porites skeleton is made up of CaCO3 while bone consists of a mineral, hydroxyapatite Ca5(PO4)3OH with the present of carbonate ions, typically from 3 to 7 wt%.
In this study, the impact of different oxidizing agents on the structural integrity of activated carbon (AC) and multiwalled carbon nanotubes (MWCNTs) was studied for the removal of BTX from aqueous solution. Seven different combinations of green oxidizing agents (mild organic acids) in conjugation with NaOCl (basic oxidizing agent) were used. The modified adsorbents were analyzed by Brunauer, Emmett, and Teller (BET) surface area analyzer, Fourier transform infrared spectroscopy (FTIR), Boehm titration, Raman spectroscopy, thermal gravimetric analysis (TGA), x-ray diffraction (XRD), zeta potential, and variable pressure field emission scanning electron microscope (VPFESEM). The results suggested that the carbonaceous sorbents modified with combination of citric acid tartaric acid, malic acid and salicylic acid (CTMS-I) showed increased surface area (O-AC: 871.67 m2/g, O-MWCNTs: 336.37 m2/g) and total pore volume (O-AC: 0.59 cm3/g, O-MWCNTs: 0.04 cm3/g), with the significantly improved thermal stability. Preliminary batch adsorption experiments conducted using the present prepared O-AC and O-MWCNTs, showed an improved performance towards the adsorption of BTX, compared with other available reported adsorbents in the literature.
This paper reports the post-processing ageing phenomena of thermoplastic sago starch (TPS) and plasticised sago pith waste (SPW), which were processed using twin-screw extrusion and compression moulding techniques. Wide angle X-ray diffraction (XRD) analyses showed that after processing, starch molecules rearranged into VH-type (which was formed rapidly right post processing and concluded within 4 days) and B-type (which was formed slowly over a period of months) crystallites. Evidence from Fourier transform infrared spectroscopy (FTIR) analyses corroborated the 2-stage crystallisation process, which observed changes in peak styles and peak intensities (at 1043 and 1026 cm-1) and bandnarrowing. Thermogravimetric analysis (TGA) studies showed that the thermal stability of plasticised SPW declined continuously for 90 days before gradual increments ensued. For all formulations tested, post-processing ageing led to drastic changes in the tensile strength (increased) and elongation at break (decreased). Glycerol and fibres restrained the retrogradation of starch molecules in TPS and SPW.
A highly active and stable nano structured Pt/Mg1-xNixO catalysts was developed by a simple co-precipitation method. The obtained Pt/Mg1-xNixO catalyst exhibited cubic structure nanocatalyst with a size of 50-80 nm and realized CH4 and CO2 conversions as high as 98% at 900°C with excellent stability in the dry reforming of methane. The characterization of catalyst was performed using various kinds of analytical techniques including XRD, BET, XRF, TPR-H2, TGA, TEM, FESEM, FT-IR, and XPS analyses. Characterization of spent catalyst further confirms that Pt/Mg1-xNixO catalyst has high coke-resistance for dry reforming. Thus, the catalyst demonstrated in this study, offers a promising catalyst for resolving the dilemma between dispersion and reducibility of supported metal, as well as activity and stability during high temperature reactions.
In this study, an optimized mesoporous sulfonated carbon (OMSC) catalyst derived from palm kernel shell biomass was developed using template carbonization and subsequent sulfonation under different temperatures and time conditions. The OMSC catalyst was characterized using acid-base titration, elemental analysis, XRD, Raman, FTIR, XPS, TPD-NH3, TGA-DTA, SEM, and N2 adsorption-desorption analysis to reveal its properties. Results proved that the OMSC catalyst is mesoporous and amorphous in structure with improved textural, acidic, and thermal properties. Both FTIR and XPS confirmed the presence of -SO3H, -OH, and -COOH functional groups on the surface of the catalyst. The OMSC catalyst was found to be efficient in catalyzing glycerol conversion to acetin via an acetylation reaction with acetic acid within a short period of 3 h. Response surface methodology (RSM), based on a two-level, three-factor, face-centered central composite design, was used to optimize the reaction conditions. The results showed that the optimized temperature, glycerol-to-acetic acid mole ratio, and catalyst load were 126 °C, 1:10.4, and 0.45 g, respectively. Under these optimum conditions, 97% glycerol conversion (GC) and selectivities of 4.9, 27.8, and 66.5% monoacetin (MA), diacetin (DA), and triacetin (TA), respectively, were achieved and found to be close to the predicted values. Statistical analysis showed that the regression model, as well as the model terms, were significant with the predicted R2 in reasonable agreement with the adjusted R2 (<0.2). The OMSC catalyst maintained excellent performance in GC for the five reaction cycles. The selectivity to TA, the most valuable product, was not stable until the fourth cycle, attributable to the leaching of the acid sites.
The demand for carbon dioxide (CO2) gas detection is increasing nowadays. However, its fast detection at room temperature (RT) is a major challenge. Graphene is found to be the most promising sensing material for RT detection, owing to its high surface area and electrical conductivity. In this work, we report a highly edge functionalized chemically synthesized reduced graphene oxide (rGO) thin films to achieve fast sensing response for CO2 gas at room temperature. The high amount of edge functional groups is prominent for the sorption of CO2 molecules. Initially, rGO is synthesized by reduction of GO using ascorbic acid (AA) as a reducing agent. Three different concentrations of rGO are prepared using three AA concentrations (25, 50, and 100 mg) to optimize the material properties such as functional groups and conductivity. Thin films of three different AA reduced rGO suspensions (AArGO25, AArGO50, AArGO100) are developed and later analyzed using standard FTIR, XRD, Raman, XPS, TEM, SEM, and four-point probe measurement techniques. We find that the highest edge functionality is achieved by the AArGO25 sample with a conductivity of ~1389 S/cm. The functionalized AArGO25 gas sensor shows recordable high sensing properties (response and recovery time) with good repeatability for CO2 at room temperature at 500 ppm and 50 ppm. Short response and recovery time of ~26 s and ~10 s, respectively, are achieved for 500 ppm CO2 gas with the sensitivity of ~50 Hz/µg. We believe that a highly functionalized AArGO CO2 gas sensor could be applicable for enhanced oil recovery, industrial and domestic safety applications.
Cellulose nanofibers (CNF) isolated from plant biomass have attracted considerable interests in polymer engineering. The limitations associated with CNF-based nanocomposites are often linked to the time-consuming preparation methods and lack of desired surface functionalities. Herein, we demonstrate the feasibility of preparing a multifunctional CNF-zinc oxide (CNF-ZnO) nanocomposite with dual antibacterial and reinforcing properties via a facile and efficient ultrasound route. We characterized and examined the antibacterial and mechanical reinforcement performances of our ultrasonically induced nanocomposite. Based on our electron microscopy analyses, the ZnO deposited onto the nanofibrous network had a flake-like morphology with particle sizes ranging between 21 to 34 nm. pH levels between 8-10 led to the formation of ultrafine ZnO particles with a uniform size distribution. The resultant CNF-ZnO composite showed improved thermal stability compared to pure CNF. The composite showed potent inhibitory activities against Gram-positive (methicillin-resistant Staphylococcus aureus (MRSA)) and Gram-negative Salmonella typhi (S. typhi) bacteria. A CNF-ZnO-reinforced natural rubber (NR/CNF-ZnO) composite film, which was produced via latex mixing and casting methods, exhibited up to 42% improvement in tensile strength compared with the neat NR. The findings of this study suggest that ultrasonically-synthesized palm CNF-ZnO nanocomposites could find potential applications in the biomedical field and in the development of high strength rubber composites.
Inflammatory bowel disease (IBD), including Crohn's disease and ulcerative colitis, has gradually emerged as a public health challenge worldwide. Carrageenan is a popular food additive that has been in use for decades. However, controversy exists regarding to the safety of carrageenan due to its exacerbation of colitis in experimental models. In this study, we studied the effects of vehicle and host intestinal microflora on carrageenan inflammatory properties in C57BL/6 J mice. We found that in high-fat diet model, native carrageenan in drinking water increased the disease activity index (DAI), myeloperoxidase (MPO) activity and the mRNA expression of TLR4 in colon, whereas carrageenan-supplemented diet has no visible effects. However, no signs of colitis were observed under low-fat diet regardless of the mode of vehicle used. Moreover, we discovered that carrageenan-induced colitis in high-fat diet model was robustly correlated with changes in the composition of gut microbiota, specifically Alistipes finegoldii and Bacteroides acidifaciens. Hence, we propose that the inflammatory property of carrageenan is influenced greatly by its intake form via modification of host intestinal microecology.
This aim of this research is to investigate thermal stability of virgin coconut oil, (VCO) which was heated at 190°C upon 40 days storage as compared to extra virgin olive oil (EVOO). The changes in fatty acids composition through (GC), Fourier Transform Infrared (FTIR) spectra, iodine value (IV) and total phenolic content were determined throughout the period of study. Results from GC showed that there was significant changes (P
Inhaled corticosteroids provide unique systems for local treatment of asthma or chronic obstructive pulmonary disease. However, the use of poorly soluble drugs for nebulization has been inadequate, and many patients rely on large doses to achieve optimal control of their disease. Theoretically, nanotechnology with a sustained-release formulation may provide a favorable therapeutic index. The aim of this study was to determine the feasibility of using sterically stabilized phospholipid nanomicelles of budesonide for pulmonary delivery via nebulization.