The chitosan/polyvinyl alcohol/TiO2 composite was synthesized. Two different degrees of deacetylation of chitosan were prepared by hydrolysis to compare the effectiveness of them. The composite was analyzed via field emission scanning electron microscopy, Fourier transform infrared, X-ray diffraction, thermal gravimetric analysis, weight loss test and adsorption study. The FTIR and XRD results proved the interaction among chitosan, PVA and TiO2 without any chemical reaction. It was found that, chitosan with higher degree of deacetylation has better stability. Furthermore, it also showed that higher DD of chitosan required less time to reach equilibrium for methyl orange. The adsorption followed the pseudo-second-order kinetic model. The Langmuir and Freundlich isotherm models were fitted well for isotherm study. Adsorption capacity was higher for the composite containing chitosan with higher DD. The dye removal rate was independent of the dye's initial concentration. The adsorption capacity was increased with temperature and it was found from reusability test that the composite containing chitosan with higher DD is more reusable. It was notable that adsorption capacity was even after 15 runs. Therefore, chitosan/PVA/TiO2 composite can be a very useful material for dye removal.
There are several alternative sampling and analytical methods available for the determination of respirable
crystalline silica exposure among workers. The commonly used ones are, (1) NIOSH Manual Analytical Method
No.7500(NMAM 7500) which is Silica, crystalline, by X-ray difractometer via filter deposition(NIOSH 2003), and
(2) MDHS 101 (Methods for the Determination of Hazardous Substances (MDHS) Guidance No.101: Respirable
crystalline silica in respirable airborne dust). The aim of this study is to compare applicability of respirable crystalline
silica sampling and analysis between method MDHS 101 and NMAM 7500. Laboratory procedures will be performed
strictly based on MDHS 101 and NMAM 7500. Both methods apply X-ray diffraction as analytical technique with
many variations on sampling techniques and laboratory preparations. Quality assurance values such as detection
limits, accuracy and precision are derived from both data and will be compared to determine which of the method
establishes better quality assurance. The method which establishes better quality assurance will be recommend to be
used in Malaysian respirable crystalline silica monitoring programme. The strength of this research lies on its potential
to provide local capabilities in analysis of respirable crystalline silica in Malaysian setting.
Lanthanum substituted Ni-Zn ferrite nanoparticles (Ni0.5Zn0.5LaxFe1-xO4; 0.00 ≤x≤ 1.00) synthesized by sol-gel method were presented. X-ray diffraction patterns reveal the typical single phase spinel cubic ferrite structure, with the traces of secondary phase for lanthanum substituted nanocrystals. In addition, the structural analysis also demonstrates that the average crystallite size varied in the range of 21-25 nm. FTIR spectra present the two prominent absorption bands in the range of 400 to 600 cm-1 which are the fingerprint region of all ferrites. Surface morphology of both substituted and unsubstituted Ni-Zn ferrite nanoparticle samples was studied using FESEM technique and it indicates a significant increase in the size of spherical shaped particles with La3+ substitution. Magnetic properties of all samples were analyzed using vibrating sample magnetometer (VSM). The results revealed that saturation magnetization (Ms) and coercivity (Hc) of La3+ substituted samples has decreased as compared to the Ni-Zn ferrite samples. Hence, the observed results affirm that the lanthanum ion substitution has greatly influenced the structural, morphology and magnetic properties of Ni-Zn ferrite nanoparticles.
Magnetic nanoparticles of Fe₃O₄ were synthesized and characterized using transmission electron microscopy and X-ray diffraction. The Fe₃O₄ nanoparticles were found to have an average diameter of 5.48 ±1.37 nm. An electrochemical biosensor based on immobilized alkaline phosphatase (ALP) and Fe₃O₄ nanoparticles was studied. The amperometric biosensor was based on the reaction of ALP with the substrate ascorbic acid 2-phosphate (AA2P). The incorporation of the Fe₃O₄ nanoparticles together with ALP into a sol gel/chitosan biosensor membrane has led to the enhancement of the biosensor response, with an improved linear response range to the substrate AA2P (5-120 μM) and increased sensitivity. Using the inhibition property of the ALP, the biosensor was applied to the determination of the herbicide 2,4-dichlorophenoxyacetic acid (2,4-D). The use of Fe₃O₄ nanoparticles gives a two-fold improvement in the sensitivity towards 2,4-D, with a linear response range of 0.5-30 μgL-1. Exposure of the biosensor to other toxicants such as heavy metals demonstrated only slight interference from metals such as Hg2+, Cu2+, Ag2+ and Pb2+. The biosensor was shown to be useful for the determination of the herbicide 2, 4-D because good recovery of 95-100 percent was obtained, even though the analysis was performed in water samples with a complex matrix. Furthermore, the results from the analysis of 2,4-D in water samples using the biosensor correlated well with a HPLC method.
Lead contamination in topsoil of the mining and smelting area of Mitrovica, Kosovo, was investigated for total concentrations and chemical fractions by sequential extraction analysis, mineralogical fractions by X-ray diffraction (XRD) and scanning electron microscopy with energy-dispersive X-ray spectrometer (SEM-EDX). The study revealed that all samples contained Pb exceeding USEPA standard of 400 mg kg-1. The highest total concentration of Pb (125,000 mg kg-1) was the soil from the former smelter. Sequential extraction results showed that the predominant form of Pb was associated with Fe-Mn oxide-bound fraction which ranged from 45.37 to 71.61% of total concentrations, while carbonate and silicate Pb-binding fractions were dominant when physical measurements (XRD and SEM-EDX) were applied. Application of Pb isotope ratios (206Pb/207Pb and 208Pb/206Pb), measured by inductively coupled plasma mass spectrometry, identified that Pb contamination is originated from similar anthropogenic source. The results reflected that the Pb contamination in the soil of this area is serious. In order to provide proper approaches on remediation and prevention of health impacts to the people in this area, a continuous monitoring and health risk assessment are recommended.
The synergistic effect of using κ-carrageenan bionanocomposites with the hybridization of cellulose nanocrystals (CNCs) and organically modified montmorillonite (OMMT) reinforcements was studied. The effects of different reinforcements and filler contents were evaluated through mechanical testing, and morphological and water uptake properties. The tensile strength and Young's modulus of both bionanocomposites increased with filler loading and optimized at 4%. OMMT incorporation into the κ-carrageenan/CNCs bionanocomposites resulted in further mechanical property improvement with an optimum ratio of 1:1 (CNCs:OMMT) while maintaining high film transparency. X-ray diffraction and morphological analyses revealed that intercalation occurred between the κ-carrageenan bionanocomposite matrix and OMMT. The water uptake of the κ-carrageenan bionanocomposites was significantly reduced by the addition of both CNCs and OMMT. The enhancements in the mechanical properties and performance of the hybrid bionanocomposite indicate compatibility among the reinforcement, biopolymer, and well-dispersed nanoparticles. This renders the hybrid CNC/OMMT/κ-carrageenan nanocomposites extremely promising for food packaging applications.
High demand of semiconductor gas sensor works at low operating temperature to as low as 100 °C has led to the fabrication of gas sensor based on TiO₂ nanoparticles. A sensing film of gas sensor was prepared by mixing the sensing material, TiO₂ (P25) and glass powder, and B₂O₃ with organic binder. The sensing film was annealed at temperature of 500 °C in 30 min. The morphological and structural properties of the sensing film were characterized by field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). The gas sensor was exposed to hydrogen with concentration of 100⁻1000 ppm and was tested at different operating temperatures which are 100 °C, 200 °C, and 300 °C to find the optimum operating temperature for producing the highest sensitivity. The gas sensor exhibited p-type conductivity based on decreased current when exposed to hydrogen. The gas sensor showed capability in sensing low concentration of hydrogen to as low as 100 ppm at 100 °C.
This paper investigates the effect of the ratio of ammonium nitrate (AN) on the structural, microstructural, magnetic, and alternating current (AC) conductivity properties of barium hexaferrite (BaFe12O19). The BaFe12O19 were prepared by using the salt melt method. The samples were synthesized using different powder-to-salt weight ratio variations (1:3, 1:4, 1:5, 1:6 and 1:7) of BaCO₃ + Fe₂O₃ and ammonium nitrate salt. The NH₄NO₃ was melted on a hot plate at 170 °C. A mixture of BaCO₃ and Fe₂O₃ were added into the NH₄NO₃ melt solution and stirred for several hours using a magnetic stirrer under a controlled temperature of 170 °C. The heating temperature was then increased up to 260 °C for 24 hr to produce an ash powder. The x-ray diffraction (XRD) results show the intense peak of BaFe12O19 for all the samples and the presence of a small amount of the impurity Fe₂O₃ in the samples, at a ratio of 1:5 and 1:6. From the Fourier transform infra-red (FTIR) spectra, the band appears at 542.71 cm - 1 and 432.48 cm - 1 , which corresponding to metal⁻oxygen bending and the vibration of the octahedral sites of BaFe12O19. The field emission scanning electron microscope (FESEM) images show that the grains of the samples appear to stick each other and agglomerate at different masses throughout the image with the grain size 5.26, 5.88, 6.14, 6.22, and 6.18 µm for the ratios 1:3, 1:4, 1:5, 1:6, and 1:7 respectively. From the vibrating sample magnetometer (VSM) analysis, the magnetic properties of the sample ratio at 1:3 show the highest value of coercivity Hc of 1317 Oe, a saturation magnetization Ms of 91 emu/g, and a remnant Mr of 44 emu/g, respectively. As the temperature rises, the AC conductivity is increases with an increase in frequency.
There are various approaches to enhancing the catalytic properties of TiO₂, including modifying its morphology by altering the surface reactivity and surface area of the catalyst. In this study, the primary aim is to enhance the photocatalytic activity by changing the TiO₂ nanotubes' architecture. The highly ordered infrastructure is favorable for a better charge carrier transfer. It is well known that anodization affects TiO₂ nanotubes' structure by increasing the anodization duration which in turn influence the photocatalytic activity. The characterizations were conducted by FE-SEM (fiend emission scanning electron microscopy), XRD (X-ray diffraction), RAMAN (Raman spectroscopy), EDX (Energy dispersive X-ray spectroscopy), UV-Vis (Ultraviolet visible spectroscopy) and LCMS/MS/MS (liquid chromatography mass spectroscopy). We found that the morphological structure is affected by the anodization duration according to FE-SEM. The photocatalytic degradation shows a photodegradation rate of k = 0.0104 min-1. It is also found that a mineralization of Simazine by our prepared TiO₂ nanotubes leads to the formation of cyanuric acid. We propose three Simazine photodegradation pathways with several intermediates identified.
This study was carried out to investigate the electrical properties of YBCO sample as superconductor
and the effect of addition of Co3O4 on the superconducting properties of YBCO superconductor. The
YBCO sample was prepared by solid state reaction route. The samples were prepared by each with
weight percentage of cobalt oxide of x= 0.00, x= 0.01, x= 0.02 and x= 0.03. Electrical Conduction by
Multimeter, Fourier Transform Infrared (FTIR), Critical temperature (Tc) measurement, X-ray
Diffraction (XRD), and Scanning Electron Microscopy (SEM) were conducted for analysis.
Multimeter showed all samples were in electric conduction, FTIR showed that carbonyl compound in
the sample was removed after calcinations. Tc measurement showed that the critical temperature of
sample of x= 0.02 was increased compared to sample of x= 0.00. XRD showed all samples have
orthorhombic structure and SEM showed that the grain size was increased as increased the cobalt
addition in YBCO superconductor. Besides, the EDX also showed the composition of elements
YBCO were tally with chemicals used for pure YBCO and addition cobalt oxide into YBCO
superconductor.
In this work, nanocrystalline Ge1-xSnx alloy formation from a rapid thermal annealed Ge/Sn/Ge multilayer has been presented. The multilayer was magnetron sputtered onto the Silicon substrate. This was followed by annealing the layers by rapid thermal annealing, at temperatures of 300 °C, 350 °C, 400 °C, and 450 °C, for 10 s. Then, the effect of thermal annealing on the morphological, structural, and optical characteristics of the synthesized Ge1-xSnx alloys were investigated. The nanocrystalline Ge1-xSnx formation was revealed by high-resolution X-ray diffraction (HR-XRD) measurements, which showed the orientation of (111). Raman results showed that phonon intensities of the Ge-Ge vibrations were improved with an increase in the annealing temperature. The results evidently showed that raising the annealing temperature led to improvements in the crystalline quality of the layers. It was demonstrated that Ge-Sn solid-phase mixing had occurred at a low temperature of 400 °C, which led to the creation of a Ge1-xSnx alloy. In addition, spectral photo-responsivity of a fabricated Ge1-xSnx metal-semiconductor-metal (MSM) photodetector exhibited its extending wavelength into the near-infrared region (820 nm).
Silver Oxide (Ag2O)-Guar gum nanocomposite was fabricated via a simple sonochemical co-precipitation method. The obtained photocatalyst was characterized with various techniques such as X-ray diffraction, thermogravimetric analysis, Fourier transform infrared spectroscopy, UV-vis diffuse reflectance spectroscopy, photoluminescence spectroscopy, scanning electron microscopy and transmission electron microscopy along with energy dispersion X-ray spectroscopy. The findings have demonstrated that Ag2O nanoparticles are spherical of 5-20 nm and were dispersed on the surface of polysaccharide guar gum to form Ag2O-guar gum nanocomposite. The as-synthesized nanocomposite was enacted as a competent photocatalyst for the reduction of nitrobenzene and oxidation of benzyl alchohol. The conversion efficiency for the reduction of nitrobenzene was 96 % with the addition of sodium borohydride, and the conversion of benzyl alcohol was 98 %. The highly efficient photocatalytic activity was due to the exceedingly dispersed Ag2O-guar gum nanocomposite where effective separation rate of energy driven electron-hole pairs and stronger light absorption occurs. The possible mechanism of the reactions was implicated in understanding the active species involved in the photocatalytic study.
Aim: The present study revolved around determining the effect of increase in the solubility of these drugs at the absorption site using ritonavir as a drug model. Materials & methods: Ritonavir per-oral tablets were prepared using versatile and nonionic surfactants having high solubilization rate, which were further marked with high rate of dissolution. The high rate of dissolution formula applied to the solid state characterization by means of transition electron microscopy, differential scanning calorimetry, scanning electron microscopy, X-ray diffraction and infrared spectroscopy. Results & conclusion: The drug bioavailability was seen to increase expressively by administration of liquisolid tablets as compared with conventional tablets.
Samples of Y-Ba-Cu-O superconductor with nominal compositions of YBa2Cu3O7-d + x (weight %) Y2O3 (x = 0 - 15) were prepared by solid state reaction method using the Y2Cu2O5 and BaCuO2 precursors as the starting reagents. The X-ray diffraction (XRD) diffractograms for the doped samples (x> 0) show an additional non-superconducting Y2BaCuO5 (211) phase. The scanning electron microscope (SEM) micrographs show that the smaller Y2BaCuO5 grains are precipitated on the surface of the larger YBa2Cu3O7-d (YBCO) crystals. The grain size of the YBCO decreases with increasing yttria. The superconducting zero resistivity critical temperature (Tco) of the doped samples is very close to the Tco of the YBCO for x < 5, but it seems to be significantly decreasing for larger x. The transport critical current density (J) for x < 5 is enhanced due to magnetic flux pinning process by the 211 phase. However, Jc decreased for larger x due to the increase of weak links at the grain boundaries of the YBCO phase.
Sampel superkonduktor Y-Ba-Cu-O dengan komposisi nominal YBa2Cu3O7-d + x (% berat) Y2O3 (x = 0 -15) disediakan dengan kaedah tindakbalas keadaan pepejal menggunakan bahan pelopor Y2Cu2O5 dan BaCuO2 Difraktogram pembelauan sinar-X (XRD) bagi sampel yang didop (x > 0) menunjukkan wujudnya fasa tak mensuperkonduksi Y2BaCuO5 (211). Mikrograf mikroskop imbasan elektron (SEM) menunjukkan bahawa butiran Y2BaCuO5 yang lebih kecil itu termendap di atas permukaan hablur YBa2Cu3O7-d yang lebih besar. Saiz hablur YBCO mengecil dengan peningkatan yittria. Suhu genting kerintangan sifar (Tc) bagi sampel yang didop adalah hampir dengan Tco bagi YBCO untuk x<5, tetapi menurun dengan agak cepat untuk x yang lebih besar. Ketumpatan arus genting angkutan (J) untuk x < 5 meningkat jika dibandingkan dengan YBCO disebabkan oleh proses kepinan fluks magnet oleh fasa 211. Walau bagaimanapun, Jc menurun untuk x yang lebih tinggi kerana meningkatnya hubungan lemah pada sempadan butiran fasa YBCO.
In this research we investigated the effect of composition on the fabrication and morphological characteristics of a hybrid polymeric solar cell which consists of an electron donating conjugated polymer, namely is poly(3-hexylthiophene) (P3HT) combined with an electron-accepting component, which is a type of inorganic compound of TiO2 nanocrystals. The composition of TiO2 in the blends is varied and the optimum performance of the devices are studied. The optical and morphological characterizations are carried out via UV-Visible absorption spectroscopy, X-ray diffraction (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM). The electrical characteristics of the devices are measured by using Keithley 2400 SMU and solar simulator with light intensity of 100 mW/cm2.
Liquefactions of kenaf core wood were carried out at different phenol-kenaf (P/k) ratios. Characterizations of kenaf core wood liquefied residue were carried out to measure the degree of liquefaction. This provides a new approach to understand some fundamental aspects of the liquefaction reaction. Functional groups on the raw kenaf core wood and liquefied residue were examined using Fourier transform infrared spectroscopy (FTIR). The crystallinity index of the kenaf wood liquefied residue, which represents crystallinity changes of the cellulose component after the liquefaction process, was studied using X-ray diffraction (XRD). The surface morphology of the wood residue was observed using scanning electron microscopy (SEM). The thermal behavior of the residues was analyzed using thermogravimetric analysis (TGA). Abroad peak around 3450-3400 cm-1 representing OH stretching in lignin start to disappear as P/K ratio increases. The results showed that the higher the P/K ratio the greater the liquefaction of the lignin component in the kenaf core wood. The crystallinity index (CrI) on the kenaf liquefied residues increased with the increase in P/K ratio. SEM images showed that the small fragments attached on the liquefied kenaf residue surface were gradually removed as the P/K ratio was increased from 1.5/1.0 to 2.5/1.0, which is mainly attributed to the greater chemical penetration toward reactive site of the kenaf fibres. Residue content decreased as the P/K ratio increased from 1.5/1.0 to 2.5/1.0. TGA results showed the increase of heat resistance in the residue as the P/K ratio was increased.
Austenitic stainless steels of grade 304 were exposed to dry (Ar-75%CO2) and wet (Ar-75%CO2-12%H2O) environments at 700oC. This experimental setup involved horizontal tube furnace connected to CO2 gas and water vapour facilities. X-ray diffraction (XRD) technique, variable pressure-scanning electron microscope (VP-SEM) and optical microscope techniques were used to characterize the products of corrosion. The results of XRD showed that the phase of oxide layers consists of Cr2O3 and NiCr2O4 in dry CO2, meanwhile Fe2O3, Cr2O3, Fe0.56Ni0.34, Fe3O4 were identified in wet condition after 50 h. Adding 12%H2O in Ar-75%CO2 leads significantly in weight change occurred at 10 h exposure. However, after 20 h, the weight gain was decreased due to spallation of the oxide scale. The addition of water vapour accelerates the oxidation rate on the steel than that in dry condition. Morphologies and growth kinetics of these oxides vary with reaction condition. The oxidation behaviour at different times of exposure and the effect of water vapour were discussed in correlation with the microstructure of the oxides.
Tin selenide (SnSe) and copper indium diselenide (CuInSe2) compounds were synthesized by high temperature reaction method using combination of sealed ampoule (at relatively low pressure ~10-1 Pa without inert gas) and heating at specific temperature profile in rocking furnace. Powder X-Ray diffraction analysis showed that the products involved only single phases of SnSe and of CuInSe2 only. Using the reaction products as source materials, the SnSe and CuInSe2 thin films were vacuum-deposited on glass substrates at room temperature. Structural, elemental, surface morphological and optical properties of the as-deposited films were studied by X-Ray diffraction (XRD), energy dispersive X-Ray (EDX) analysis, field emission scanning electron microscopy (FESEM) and UV-Vis-NIR spectroscopy. Single phase of SnSe and CuInSe2 films were obtained by thermal evaporation technique from synthesized SnSe and CuInSe2 compound without further treatment.
Recycled hematite (α-Fe2O3) nanoparticles with enhanced complex permittivity properties have been incorporated as a filler in a polycaprolactone (PCL) matrix reinforced with oil palm empty fruit bunch (OPEFB) fiber for microwave absorption applications. The complex permittivity values were improved by reducing the particle sizes to the nano scale via high-energy ball milling for 12 h. A total of 5-20 wt.% recycled α-Fe2O3/OPEFB/PCL nanocomposites were examined for their complex permittivity and microwave absorption properties via the open ended coaxial (OEC) technique and the transmission/reflection line measurement using a microstrip connected to a two-port vector network analyzer. The microstructural analysis of the samples included X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM) and Fourier transform infrared spectroscopy (FTIR). At 1 GHz, the real (ε') and imaginary (ε″) parts of complex permittivity of recycled α-Fe2O3 particles, respectively, increased from 7.88 to 12.75 and 0.14 to 0.40 when the particle size was reduced from 1.73 μm to 16.2 nm. A minimum reflection loss of -24.2 dB was achieved by the 20 wt.% nanocomposite at 2.4 GHz. Recycled α-Fe2O3 nanoparticles are effective fillers for microwave absorbing polymer-based composites in 1-4 GHz range applications.
Hydrocarbon is a light-non aqueous phase liquid or known as LNAPL. It poses environmental hazard if accidentally spilled out into the soil and water systems as a result of its insoluble nature in water. LNAPL component infiltrates into soil through pore spaces and afloat at the top of groundwater level. Some of this hydrocarbon would trap and clog within the voids, difficult to remove and costly to clean. The occurence of hydrocarbon in the soil definitely degraded the behaviour of soils in terms of engineering properties. This study aimed to investigate the engineering properties of oil-contaminated soil for two different residual soils originally developed from in-situ weathering of granitic and metasedimentary rocks. The physical characterisations of the soil were determined including particle size distribution, specific gravity test and x-ray diffraction (XRD). The engineering parameters for the contaminated and uncontaminated soils were Atterberg limits, compaction and soil shear strength (UU tests). The amounts of hydrocarbon added to soil were varied at 0%, 4%, 8%, 12% and 16% of dried weigth of soil samples. The results from the particle size distribution analysis showed that residual soil from granitic rock comprises of 38% sand, 33% silt and 4% clay while metasedimentary soil consists of 4% sand, 43% silt dan 29% clay. The mean values of specific gravity for the granitic and metasedimentary soils were 2.56 and 2.61, respectively. The types of minerals present in granitic soil sample were quartz, kaolinite and gibbsite while metasedimentary soil consists of quartz and kaolinite. The Atterberg limits value decreased as a result of increasing amount of added hydrocarbon into the soil. A similar behaviouir was observed with the values of maximum dry density and optimum water content with increasing hydrocarbon content. The overall unconsolidated undrained shear strength, Cu showed a decreasing trend with the increase in hydrocarbon content.