Zeolite Linde Type L (LTL) crystals with different length, diameter and particle size (nanosized LTL, rod LTL, cylinder LTL and needle LTL) were synthesized, characterized and were used as sorbent in the micro-solid phase extraction of ochratoxin A (OTA) before the high performance liquid chromatography detection. Under the optimized conditions, the detection limits of OTA for coffee and cereal were 0.09 ng g(-1) and 0.03 ng g(-1), respectively, while the quantification limits were 0.28 ng g(-1) and 0.08 ng g(-1), respectively. The recoveries of OTA of coffee and cereal spiked at 0.5, 10 and 25 ng g(-1) ranged from 91.7 to 101.0%. The proposed method was applied to forty-five samples of coffee and cereal. The presence of OTA was found in twenty-five samples, ranging from 0.28 to 9.33 ng g(-1).
Feather keratin is a biomass generated in excess from various livestock industries. With appropriate processing, it holds potential as a green source for degradable biopolymer that could potentially replace current fossil fuel based materials. Several processing methods have been developed, but the use of ultrasonication has not been explored. In this study, we focus on (i) comparing and optimizing the dissolution process of turkey feather keratin through sonication and conventional processes, and (ii) generating a biodegradable polymer material, as a value added product, from the dissolved keratin that could be used in packaging and other applications. Sonication of feather keratin in pure ionic liquids (ILs) and a mixture containing ILs and different co-solvents was conducted under different applied acoustic power levels. It was found that ultrasonic irradiation significantly improved the rate of dissolution of feather keratin as compared to the conventional method, from about 2 h to less than 20 min. The amount of ILs needed was also reduced by introducing a suitable co-solvent. The keratin was then regenerated, analyzed and characterized using various methods. This material holds the potential to be reused in various appliances.
Generally, in a waveguide-based humidity sensors, increasing the relative humidity (RH) causes the cladding refractive index (RI) to increase due to cladding water absorption. However, if graphene oxide (GO) is used, a reverse phenomenon is seen due to a gap increase in graphene layers. In this paper, this interesting property is applied in order to fabricate differential humidity sensor using the difference between RI of reduced GO (rGO) and nano-anatase TiO2 in a chip. First, a new approach is proposed to prepare high quality nano-anatase TiO2 in solution form making the fabrication process simple and straightforward. Then, the resulted solutions (TiO2 and GO) are effortlessly drop casted and reduced on SU8 two channels waveguide and extensively examined against several humid conditions. Investigating the sensitivity and performance (response time) of the device, reveals a great linearity in a wide range of RH (35% to 98%) and a variation of more than 30 dB in transmitted optical power with a response time of only ~0.7 sec. The effect of coating concentration and UV treatment are studied on the performance and repeatability of the sensor and the attributed mechanisms explained. In addition, we report that using the current approach, devices with high sensitivity and very low response time of only 0.3 sec can be fabricated. Also, the proposed device was comprehensively compared with other state of the art proposed sensors in the literature and the results were promising. Since high sensitivity ~0.47dB/%RH and high dynamic performances were demonstrated, this sensor is a proper choice for biomedical applications.
The aim of this research was to synthesize and develop a new method for the preparation of iron oxide (Fe(3)O(4)) nanoparticles on talc layers using an environmentally friendly process. The Fe(3)O(4) magnetic nanoparticles were synthesized using the chemical co-precipitation method on the exterior surface layer of talc mineral as a solid substrate. Ferric chloride, ferrous chloride, and sodium hydroxide were used as the Fe(3)O(4) precursor and reducing agent in talc. The talc was suspended in deionized water, and then ferrous and ferric ions were added to this solution and stirred. After the absorption of ions on the exterior surface of talc layers, the ions were reduced with sodium hydroxide. The reaction was carried out under a nonoxidizing oxygen-free environment. There were not many changes in the interlamellar space limits (d-spacing = 0.94-0.93 nm); therefore, Fe(3)O(4) nanoparticles formed on the exterior surface of talc, with an average size of 1.95-2.59 nm in diameter. Nanoparticles were characterized using different methods, including powder X-ray diffraction, transmission electron microscopy, emission scanning electron microscopy, energy dispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy. These talc/Fe(3)O(4) nanocomposites may have potential applications in the chemical and biological industries.
Silver nanoparticles (Ag NPs) were synthesized by the chemical reducing method in the external and interlamellar space of montmorillonite (MMT) as a solid support at room temperature. AgNO(3) and NaBH(4) were used as a silver precursor and reducing agent, respectively. The most favorable experimental conditions for synthesizing Ag NPs in the MMT are described in terms of the initial concentration of AgNO(3). The interlamellar space limits changed little (d-spacing = 1.24-1.47 nm); therefore, Ag NPs formed on the MMT suspension with d-average = 4.19-8.53 nm diameter. The Ag/MMT nanocomposites (NCs), formed from AgNO(3)/MMT suspension, were characterizations with different instruments, for example UV-visible, PXRD, TEM, SEM, EDXRF, FT-IR, and ICP-OES analyzer. The antibacterial activity of different sizes of Ag NPs in MMT were investigated against Gram-positive, ie, Staphylococcus aureus and methicillin-resistant S. aureus (MRSA) and Gram-negative bacteria, ie, Escherichia coli, Escherichia coli O157:H7, and Klebsiella pneumoniae, by the disk diffusion method using Mueller-Hinton agar (MHA). The smaller Ag NPs were found to have significantly higher antibacterial activity. These results showed that Ag NPs can be used as effective growth inhibitors in different biological systems, making them applicable to medical applications.
In this research, silver nanoparticles (AgNPs) were synthesized in chitosan (Cts), Cts/gelatin and gelatin suspensions using a chemical reducing agent. Cts and gelatin were used as natural stabilizers and solid support, whereas AgNO(3) was used as the silver precursor. Sodium borohydride (NaBH(4)) was used as the reducing agent. The properties of AgNPs in Cts, Cts/gelatin and gelatin bionanocomposites (BNCs) were studied in terms of their surface plasmon resonance, crystalline structure, average diameter size, particle distributions, surface topography and functional groups. All the samples were characterized by UV-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, atomic force microscopy and Fourier transform infrared spectroscopy.
In this study, silver nanoparticles (Ag-NPs) were synthesized using the wet chemical reduction method on the external surface layer of talc mineral as a solid support. Silver nitrate and sodium borohydride were used as the silver precursor and reducing agent in talc. The talc was suspended in aqueous AgNO(3) solution. After the absorption of Ag(+) on the surface, the ions were reduced with NaBH(4). The interlamellar space limits were without many changes (d(s) = 9.34-9.19 A(º)); therefore, Ag-NPs formed on the exterior surface of talc, with d(ave) = 7.60-13.11 nm in diameter. The properties of Ag/talc nanocomposites (Ag/talc-NCs) and the diameters of the Ag-NPs prepared in this way depended on the primary AgNO(3) concentration. The prepared Ag-NPs were characterized by ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and Fourier transform infrared. These Ag/talc-NCs may have potential applications in the chemical and biological industries.
Silver nanoparticles (AgNPs) of a small size were successfully synthesized using the wet chemical reduction method into the lamellar space layer of montmorillonite/chitosan (MMT/Cts) as an organomodified mineral solid support in the absence of any heat treatment. AgNO3, MMT, Cts, and NaBH4 were used as the silver precursor, the solid support, the natural polymeric stabilizer, and the chemical reduction agent, respectively. MMT was suspended in aqueous AgNO3/Cts solution. The interlamellar space limits were changed (d-spacing = 1.24-1.54 nm); therefore, AgNPs formed on the interlayer and external surface of MMT/Cts with d-average = 6.28-9.84 nm diameter. Characterizations were done using different methods, ie, ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, energy dispersive X-ray fluorescence spectrometry, and Fourier transform infrared spectroscopy. Silver/montmorillonite/chitosan bionanocomposite (Ag/MMT/Cts BNC) systems were examined. The antibacterial activity of AgNPs in MMT/Cts was investigated against Gram-positive bacteria, ie, Staphylococcus aureus and methicillin-resistant S. aureus and Gram-negative bacteria, ie, Escherichia coli, E. coli O157:H7, and Pseudomonas aeruginosa by the disc diffusion method using Mueller Hinton agar at different sizes of AgNPs. All of the synthesized Ag/MMT/Cts BNCs were found to have high antibacterial activity. These results show that Ag/MMT/Cts BNCs can be useful in different biological research and biomedical applications, including surgical devices and drug delivery vehicles.
Mineral composition of rock has a very important influence on the physical and mechanical properties of tunnel surrounding rock. Take Dangjianshan tunnel in cold regions for example, the rock specimens in different parts of tunnel were taken to carry out the detection test of mineral composition. By the detail qualitative and quantitative analysis, the relationship between mineral composition and surrounding rock engineering properties was explored. First of all, the composition and content of minerals contained in in the rock specimens were detected by X ray fluorescence spectrometer and X ray powder diffraction. The detection results show that rock of tunnel contains high hardness minerals such as quartz and feldspar which were proven by initial engineering geological investigation report, in addition, it also contains several kinds of low hardness minerals including inclined chlorite and illite which may exhibit large deformation characteristic of soft rock after the tunnel excavation in case of meeting water and weathering conditions. The total content of inclined chlorite and illite accounted for a considerable component in main tunnel, inclined shaft and parallel pilot respectively and the influence on surrounding rock engineering properties cannot be ignored. Therefore, mineral composition detection must be paid attention to after tunnel excavation. Secondly, the effects of mineral composition on surrounding rock were analyzed in aspects of rock strength, weathering resistance, water softening property and excavation deformation through comparing the rock samples in different parts of tunnel. The comparative results showed that when the mineral contents is high with high hardness and poor hydrophilicity, tunnel surrounding rock plays a better performance of physical and mechanical properties, vice versa. Finally, according to the specific geological and construction parameters of the tunnel, the correlation analysis was studied about the vault settlement after tunnel excavation and the hydrophilicity mineral content in main cave. The logarithmic relationship between them was found and the correlation coefficient was 0.98. It can provide a useful reference for the settlement prediction of Dangjinshan tunnel construction.
α-Mangostin is an oxygenated heterocyclic xanthone with remarkable pharmacological properties, but poor aqueous solubility and low oral bioavailability hinder its therapeutic application. This study sought to improve the compound's solubility and study the mechanism underlying solubility enhancement. Solid dispersions of α-mangostin were prepared in polyvinylpyrrolidone (PVP) by solvent evaporation method and showed substantial enhancement of α-mangostin's solubility from 0.2 ± 0.2 μg/mL to 2743 ± 11 μg/mL. Fourier transform infrared spectroscopy and differential scanning calorimetry indicated interaction between α-mangostin and PVP. Transmission electron microscopy and dynamic light scattering showed self-assembly of round anionic nanomicelles with particle size in the range 99-127 nm. Powder X-ray diffraction indicated conversion of α-mangostin from crystalline into amorphous state, and scanning electron microscopy showed the presence of highly porous powder. Studies using the fluorescent probe pyrene showed that the critical micellar concentration is about 77.4 ± 4 μg/mL. Cellular uptake of nanomicelles was found to be mediated via endocytosis and indicated intracellular delivery of α-mangostin associated with potent cytotoxicity (median inhibitory concentration of 8.9 ± 0.2 μg/mL). Improved solubility, self-assembly of nanomicelles, and intracellular delivery through endocytosis may enhance the pharmacological properties of α-mangostin, particularly antitumor efficacy.
Indialite or α-cordierite was synthesized by glass crystallization method using mainly talc and kaolin and with small amount of MgO, Al2O3, SiO2 to compensate the chemical formulation of non-stoihiometric compositions of cordierite. (3MgO.1.5Al2O3.5SiO2). B2O3, P2O5 and CaO was also added to decrease the melting and sintering temperature of cordierite. The glasses were pelletized and sintered from 850 o C up to 1050 o C. Phase compositions of both heat treated glass was quantified by X-ray powder diffraction data by the Rietveld method using TOPAS Ver 3 software. Result shows that about 60wt% of α cordierite has successfully crystallized at 850 o C. Beside secondary phases (forsterite) which come from initial raw materials, phases from grinding media were also presents in the sample. The contamination was considered high since it has reacted with existence phases to form a new phase at higher temperature. Without any contamination from grinding it was expected to obtain more than 90wt% α cordierite using the same composition.
The sol-gel method was carried out to synthesize nanosized Yttrium Iron Garnet (YIG). The nanomaterials with ferrite structure were heat-treated at different temperatures from 500 to 1000 °C. The phase identification, morphology and functional groups of the prepared samples were characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR), respectively. The YIG ferrite nanopowder was composited with polyvinylidene fluoride (PVDF) by a solution casting method. The magnitudes of reflection and transmission coefficients of PVDF/YIG containing 6, 10 and 13% YIG, respectively, were measured using rectangular waveguide in conjunction with a microwave vector network analyzer (VNA) in X-band frequencies. The results indicate that the presence of YIG in polymer composites causes an increase in reflection coefficient and decrease in transmission coefficient of the polymer.
In the study reported here, magnesium/aluminum (Mg/Al)-layered double hydroxide (LDH) was intercalated with an anticancer drug, protocatechuic acid, using ion-exchange and direct coprecipitation methods, with the resultant products labeled according to the method used to produce them: "PANE" (ie, protocatechuic acid-Mg/Al nanocomposite synthesized using the ion-exchange method) and "PAND" (ie, protocatechuic acid-Mg/Al nanocomposite synthesized using the direct method), respectively. Powder X-ray diffraction and Fourier transform infrared spectroscopy confirmed the intercalation of protocatechuic acid into the inter-galleries of Mg/Al-LDH. The protocatechuic acid between the interlayers of PANE and PAND was found to be a monolayer, with an angle from the z-axis of 8° for PANE and 15° for PAND. Thermogravimetric and differential thermogravimetric analysis results revealed that the thermal stability of protocatechuic acid was markedly enhanced upon intercalation. The loading of protocatechuic acid in PANE and PAND was estimated to be about 24.5% and 27.5% (w/w), respectively. The in vitro release study of protocatechuic acid from PANE and PAND in phosphate-buffered saline at pH 7.4, 5.3, and 4.8 revealed that the nanocomposites had a sustained release property. After 72 hours incubation of PANE and PAND with MCF-7 human breast cancer and HeLa human cervical cancer cell lines, it was found that the nanocomposites had suppressed the growth of these cancer cells, with a half maximal inhibitory concentration of 35.6 μg/mL for PANE and 36.0 μg/mL for PAND for MCF-7 cells, and 19.8 μg/mL for PANE and 30.3 μg/mL for PAND for HeLa cells. No half maximal inhibitory concentration for either nanocomposite was found for 3T3 cells.
Ni-doped cobalt aluminate NixCo1-xAl2O4 (x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0) spinel nanoparticles were successfully synthesized by a simple microwave combustion method using urea as the fuel and as well as reducing agent. X-ray powder diffraction (XRD) was confirmed the formation of single phase, cubic spinel cobalt-nickel aluminate structure without any other impurities. Average crystallite sizes of the samples were found to be in the range of 18.93 nm to 21.47 nm by Scherrer's formula. Fourier transform infrared (FT-IR) spectral analysis was confirmed the corresponding functional groups of the M-O, Al-O and M-Al-O (M = Co and Ni) bonds of spinel NixCo1-xAl2O4 structure. Scanning electron microscope (SEM) and transmission electron microscope (TEM) images was confirmed the particle like nanostructured morphology. Energy band gap (Eg) value was calculated using UV-Visible diffuse reflectance spectra (DRS) and the Eg values increased with increasing Ni2+ dopant from x = 0.2 (3.58 eV) to x = 1.0 (4.15 eV). Vibrating sample magnetometer (VSM) measurements exposed that undoped and Ni-doped CoAl2O4 samples have superparamagnetic behavior and the magnetization (Ms) values were increased with increasing Ni2+ ions. Spinel NixCo1-xAl2O4 samples has been used for the catalytic oxidation of benzyl alcohol into benzaldehyde and was found that the sample Ni0.6Co0.4Al2O4 showed higher conversion 94.37% with 100% selectivity than other samples, which may be due to the smaller particle size and higher surface area.
The microencapsulation of three model drugs; metronidazole, paracetamol and sulphapyridine into Poly (dl-Lactide-Co-Glycolide) (PLGA) scaffolds were probed using X-ray Powder Diffraction (XRPD). Changes in the diffraction patterns of the PLGA scaffolds after encapsulation was suggestive of a chemical interaction between the pure drugs and the scaffolds and not a physical intermixture.
Recently, TiO2/multi-walled carbon nanotube (MWCNT) hybrid nanocatalysts have been a subject of high interest due to their excellent structures, large surface areas and peculiar optical properties, which enhance their photocatalytic performance. In this work, a modified microwave technique was used to rapidly synthesise a TiO2/MWCNT nanocatalyst with a large surface area. X-ray powder diffraction, field-emission scanning electron microscopy, transmission electron microscopy and Brunauer-Emmett-Teller measurements were used to characterise the structure, morphology and the surface area of the sample. The photocatalytic activity of the hybrid nanocatalysts was evaluated through a comparison of the degradation of methylene blue dye under irradiation with ultraviolet and visible light. The results showed that the TiO2/MWCNT hybrid nanocatalysts degraded 34.9% of the methylene blue (MB) under irradiation with ultraviolet light, whereas 96.3% of the MB was degraded under irradiation with visible light.
In this study, silver nanoparticles (Ag-NPs) were synthesized using a green physical synthetic route into the lamellar space of montmorillonite (MMT)/chitosan (Cts) utilizing the ultraviolet (UV) irradiation reduction method in the absence of any reducing agent or heat treatment. Cts, MMT, and AgNO(3) were used as the natural polymeric stabilizer, solid support, and silver precursor, respectively. The properties of Ag/MMT/Cts bionanocomposites (BNCs) were studied as the function of UV irradiation times. UV irradiation disintegrated the Ag-NPs into smaller sizes until a relatively stable size and size distribution were achieved. Meanwhile, the crystalline structure and d-spacing of the MMT interlayer, average size and size distribution, surface morphology, elemental signal peaks, functional groups, and surface plasmon resonance of Ag/MMT/Cts BNCs were determined by powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, energy dispersive X-ray fluorescence, Fourier transform infrared, and UV-visible spectroscopy. The antibacterial activity of Ag-NPs in MMT/Cts was investigated against Gram-positive bacteria, ie, Staphylococcus aureus and methicillin-resistant S. aureus and Gram-negative bacteria (ie, Escherichia coli) by the disk diffusion method on Muller-Hinton Agar at different sizes of Ag-NPs. All of the synthesized Ag/MMT/Cts BNCs were found to have high antibacterial activity. These results show that Ag/MMT/Cts BNCs can be useful in different biologic research and biomedical applications, such as surgical devices and drug delivery vehicles.
Using the chemical reduction method, silver nanoparticles (Ag NPs) were effectively synthesized into the zeolite framework in the absence of any heat treatment. Zeolite, silver nitrate, and sodium borohydride were used as an inorganic solid support, a silver precursor, and a chemical reduction agent, respectively. Silver ions were introduced into the porous zeolite lattice by an ion-exchange path. After the reduction process, Ag NPs formed in the zeolite framework, with a mean diameter of about 2.12-3.11 nm. The most favorable experimental condition for the synthesis of Ag/zeolite nanocomposites (NCs) is described in terms of the initial concentration of AgNO(3). The Ag/zeolite NCs were characterized by ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, energy dispersive X-ray fluorescence, and Fourier transform infrared. The results show that Ag NPs form a spherical shape with uniform homogeneity in the particle size. The antibacterial activity of Ag NPs in zeolites was investigated against Gram-negative bacteria (ie, Escherichia coli and Shigella dysentriae) and Gram-positive bacteria (ie, Staphylococcus aureus and methicillin-resistant Staphylococcus aureus) by disk diffusion method using Mueller-Hinton agar at different sizes of Ag NPs. All of the synthesized Ag/zeolite NCs were found to have antibacterial activity. These results show that Ag NPs in the zeolite framework can be useful in different biological research and biomedical applications.
This study was driven by the stringent environmental legislation concerning the consumption and utilization of eco-friendly materials. Within this context, this paper aimed to examine the characteristics of starch and fibres from the Dioscorea hispida tuber plant to explore their potential as renewable materials. The extraction of the Dioscorea hispida starch and Dioscorea hispida fibres was carried out and the chemical composition, physical, thermal, morphological properties, and crystallinity were studied. The chemical composition investigations revealed that the Dioscorea hispida starch (DHS) has a low moisture t (9.45%) and starch content (37.62%) compared to cassava, corn, sugar palm, and arrowroot starches. Meanwhile, the Dioscorea hispida fibres (DHF) are significantly low in hemicellulose (4.36%), cellulose (5.63%), and lignin (2.79%) compared to cassava, corn hull and sugar palm. In this investigation the chemical, physical, morphological and thermal properties of the Dioscorea hispida fibre and Dioscorea hispida starch were examined by chemical composition investigation, scanning electron microscopy (SEM), particle size distribution, thermogravimetric analysis (TGA), X-ray powder diffraction (XRD), and Fourier transform infrared (FTIR), respectively. It was found that Dioscorea hispida waste is promising alternative biomass and sustainable material with excellent potential as a renewable filler material for food packaging applications.
Undoped and Mn2+ doped CoAl2O4 (MnxCo1-xAl2O4; x = 0.0 to 1.0) spinel nanoparticles were successfully synthesized by a microwave heating method using glycine as the fuel. X-ray powder diffraction (XRD) was confirmed the cubic spinel structure. The average crystallite size of the samples was found to be in the range of 16.46 nm to 20.25 nm calculated by Scherrer's formula. The nano-sized particle-like morphology of the samples was confirmed by high resolution scanning electron microscopy (HR-SEM) and transmission electron microscopy (HR-TEM) analysis. Energy dispersive X-ray (EDX) results showed the pure form of spinel aluminate structure. The band gap energy (Eg) of pure CoAl2O4 was estimated to be 3.68 eV from UV-Visible diffuse reflectance spectroscopy (DRS), and the Eg values increased with increase of Mn2+ ions, due to the smaller grain size. The magnetic hysteresis (M-H) loop showed the superparamagnetic nature, and the magnetization and coercivity values increased with increasing Mn2+ ions, which was confirmed by vibrating sample magnetometer (VSM). All compositions of the nano-catalysts were tested as catalyst successfully for the conversion of benzyl alcohol into benzaldehyde and observed good catalytic activity.