A series of (Li20)x(B203)1-x has been synthesized with mole fraction x=0.10, 0.15,020,025 and 0.30 mol% using melt quenching method. The structure of the glass system was determined by FTIR and X-ray diffraction. The density and molar volume were determined and the density increases with Li20 content whereas molar volume decreases with Li20. Refractive index of glass samples were measured by ellipsometer. Refractive index increases with increase of Li20. The absorption spectra of the studied glass showed that position of fundamental absorption edge shifts to longer wavelength with Li20. Optical band gap varies from 0.10 to 222 eV and Urbach energy varies from 2.91 to 1.55 eV. The variation in optical band gap and Urbach energy were due to the variation in the glass structure.
Study of a series of lead lithium borophosphate glass samples was performed to determine the structural and luminescence properties. The glass samples containing the composition of 20Pb0-xLi20-30B 20 3-(50-x)P 20 5-2TiO 2 (where x = 0, 5, 10, 15, 20) system were prepared using melt-quenching technique. The Pb0-Li20-B 20 3-P20 5-Ti0 2 samples were investigated for structural properties using Fourier transform infrared and photoluminescence spectroscopy for studies of luminescence properties. The results from FTIR showed the presence of trigonal and tetrahedral PO4' PO3, BO4 and B03 groups within the host network structure. The samples exhibit luminescence emission centered at 420, 482 and 496 nm when excited at 300 nm wavelength. The emission peak at 420 nm were assigned to F center emission and charge-transfer transition of Ti4+ ions. The results showed that emission intensity was dependent on lithium contents in Ti-doped lead lithium borophosphate glass composition.
In this research, a novel method was performed to obtain hydrogel with superior thermal stability by incorporation
of cellulose nanocrystals (CNC) into gelatin based hydrogel. Glutaraldehyde was used as cross-linker due to its high
chemical reactivity towards NH2
group on gelatin. Different ratio of gelatin/CNC hydrogel was produced in order to study
the effects of CNC towards the swelling behaviour and thermal stability of gelatin based hydrogel. The obtained hydrogel
was subjected to Fourier transform infrared (FTIR) to verify that gelatin had been cross-linked, swelling test with different
pH for swelling behaviour and thermogravimetric analysis (TGA) for thermal stability. The presence of C=N stretching
group in the FTIR spectrum for gelatin/CNC hydrogel indicated that the cross-linking reaction between gelatin monomer
had been successfully carried out. The hydrogel showed impressive pH sensitivity and maximum swelling was obtained
at pH3. The TGA results clearly showed that the incorporation of CNC into gelatin was able to produce hydrogel with
higher thermal stability compare to neat gelatin.
Nanoparticles of undoped and copper doped with Fe3
O4 of three concentrations (0.5, 1.0 and 1.5) are synthesized by
sonochemical method. Structural, optical and morphological properties of these compounds were studied. Fe2+/Fe3+
ratio is found to be 2.36. Crystalline structure, lattice parameters, surface morphologies, direct and indirect band gap
energies of the synthesized compounds were estimated and the results are discussed in detail. The XDR analysis indicates
the Cu doped Fe3
O4
nanoparticles have higher crystallinity than undoped samples. Average crystallite size is found
to increase as Cu concentration increased. The FTIR results are proven by the presence of mixed magnetite-hematite
nanostructures and it is complement to the XRD results. The presence of spherical, polygonal and agglomeration forms
of the particles are visually seen in the SEM images. Direct and indirect band gap energy is found to be decreased as the
copper concentration was increased.
A series of monoamide isomers have been successfully synthesised and characterised using combination of common spectroscopic techniques such Fourier Transform Infrared (FT-IR), 1H and 13C Nuclear Magnetic Resonance (NMR) and Ultraviolet-visible (UV-vis). The monoamide compounds namely 6-(3-methyl-pyridin-2-ylcarbamoyl)-pyridine2-carboxylic acid methyl ester (L1), 6-(4-methyl-pyridin-2-ylcarbamoyl)-pyridine-2-carboxylic acid methyl ester (L2), 6-(5-methyl-pyridin-2-ylcarbamoyl)-pyridine-2-carboxylic acid methyl ester (L3) and 6-(6-methyl-pyridin-2ylcarbamoyl)-pyridine-2-carboxylic acid methyl ester (L4) were prepared from reaction between 6-(methoxycarbonyl) pyridine-2-carboxylic acid with 2-amino-N-methylpyridine (where N = 3, 4, 5 and 6) by using acyl chloride reaction. In this present studies, the synthesis and characterization of these compounds are discussed along with the inductive effects contributed by methyl substituted groups at the pyridine ring.
Kanji Dioscorea pentaphylla telah diubah suai dengan pensulfatan dan peneutralan bagi menghasilkan natrium
kanji sulfat. Tindak balas pensulfatan dilakukan dengan asid sulfurik dalam etanol dan air pada suhu 0o
C. Darjah
penukargantian dikira berdasarkan peratus karbon dan sulfur yang ditentukan menggunakan penganalisis unsur CHNS.
Natrium kanji sulfat yang mempunyai darjah penukargantian dan peratus nisbah berat hasil yang tinggi dipilih dan
dicirikan dengan spektrum transformasi Fourier inframerah (FT-IR) dan profil pembelauan sinar-X (XRD). Kehadiran
dua puncak getaran regangan C-O-S dan S=O dalam spektrum FT-IR dan puncak berbeza yang terhasil dalam corak
difraktogram XRD membuktikan tindak balas berlaku pada struktur kanji. Sifat termal juga ditentukan dengan kalorimeter
pengimbas pembezaan (DSC) dan analisis termogravimetri (TGA). Natrium kanji sulfat yang dihasilkan mempunyai
kestabilan termal yang baik kerana mempunyai suhu penguraian pada 265o
C. Natrium kanji sulfat ini sesuai dijadikan
bahan tambahan dalam penghasilan hidrogel, organogel dan filem dengan sifat anionik kerana degradasi tidak terjadi
di bawah suhu ini.
Siliceous mesoporous molecular sieve (Si-MCM-41) material with highly ordered hexagonal pore arrangement was synthesized at 373 K for 8-days duration by hydrothermal method, dried at 393 K and calcined at 823 K in N2 atmosphere. The calcined Si-MCM-41 was later functionalized with 10-50 wt. % monoethanolamine (MEA) by impregnation method and dried in vacuum at 343 K. The MEA-Si-MCM-41 samples were characterized for their physicochemical properties with FTIR, XRD, TGA, HRTEM, FESEM, BET and elemental analysis. XRD results showed that the intensity of the characteristic peaks of Si-MCM-41 reduces with increasing loading of MEA indicating that the MEA molecules are loaded in the pores as well as on the surface of Si-MCM-41. The appearance of FTIR peaks corresponding to N-H, C-N and C-H bonds suggested that Si-MCM-41 has been functionalized with MEA. The presence of Si-O-Si peaks in FTIR spectra of MEA-Si-MCM-41 samples indicates that the hexagonal pore arrangement remains intact and this is supported by HRTEM images. FESEM images show that MEA-Si-MCM-41 samples became agglomerated with increase loading of MEA. TGA analyses show that the MEA-Si-MCM-41 samples are thermally stable up to 528 K. N2 adsorption-desorption isotherms show that the textural properties of Si-MCM-41 material slowly change from a mesoporous material to non-porous material as the MEA loading increases due to pore filling effect during functionalization with MEA. Detection of N, C and H by elemental analysis confirms the presence of MEA in MEA-Si-MCM-41 samples.
A mild and effective synthesis of resorcinol-furfural (RF) thermosetting resin was proposed with ethanol as a distinctive solvent, which, as a usually neglected factor, was shown to not only help form a homogeneous reaction system but also observably reduce the energy barriers between the early intermediates and transition states in addition reactions by explicit solvent effects, drawn from theoretical calculation conclusions. Besides, the para-additions on aromatic rings were more dominant than ortho-additions with the same reactants, which affected the final link types of monomers verified by Fourier transform infrared spectroscopy and two-dimensional nuclear magnetic resonance tests. The prepared resin can be assigned to a relatively fast gel speed and a high residual mass (65.25%) after pyrolysis in a N2 atmosphere by adjusting the molar ratios of F to R, and the curing of that was a complex reaction, with a curing temperature around 149 °C and an activation energy of about 49.11 kJ mol-1 obtained by the Kissinger method.
Inclusion complexes of R-ketoprofen and S-ketoprofen enantiomers with β-cyclodextrin (β-CD) in aqueous solution were studied using various spectroscopic techniques such as Raman, FTIR, UV and fluorescence. The different relative intensities and characteristic band shifts of the two enantiomers from Raman spectra suggests different interaction when complexed with β-CD. Raman experiments revealed a noticeable diminishing of the CC vibration and ring deformation, which indicate the embedding of ketoprofen inside the β-CD cavity. It's revealed that distinct differences between R- and S-ketoprofen in the presence of β-CD at neutral pH. The stoichiometry ratio and binding constant of the inclusion complexes were calculated using Benesi-Hildebrand plot. Both enantiomers showed stoichiometry ratio of 1:1 inclusion complex with β-CD. The binding constant of R-ketoprofen (4088 M-1) is higher than S-ketoprofen (2547 M-1). These values indicated that β-CD formed inclusion complexes more preferentially with R-ketoprofen than S-ketoprofen. Results demonstrated that β-CD can be used as a promising chiral selector for ketoprofen enantiomers.
This study reports the application of hydrated lime for the effective adsorption of the heavy mercury metal from the aqueous phase solutions. Initially, hydrated lime was subjected to structural characterization and thermal stability analysis. The FT-IR spectrum analysis revealed that the existence of the O-H bonds as a confirmation of hydrated lime formation. Subsequently, the XRD powder-based analysis demonstrated that most of the hydrated lime is pure crystalline material known as Portlandite while a small amount of calcite is also present in the structure of the hydrated lime. The thermal stability analysis revealed that the hydrated lime is highly thermally stable under harsh conditions without decomposing at higher temperatures up to 500 °C. Furthermore, the hydrated lime was subjected to the selective adsorption of heavy metal mercury to investigate the potential influence of the adsorbent particle size and loading on adsorption capacity. The results demonstrated that the decrease in the adsorbent particle size leads to the improvement in the mercury adsorption attributing to the rise in specific surface area. The enhancement in the loading of the adsorbent resulted in a reduction in mercury adsorption directing to the fact that already adsorbed metal ions onto the adsorbent surface lead to hindrance for the adsorption of other ions of heavy metal. These results lead to a significant impact on modern in inventing different adsorbents with promising water treatment efficiency for more industrial applications and the related recovery of mercury.
A simple, inexpensive but effective approach for visual chiral recognition of ketoprofen enantiomers was developed using L-cysteine capped silver nanoparticles (L-Cys-AgNPs) as a colorimetric sensor. Upon the addition of R-ketoprofen to L-Cys-AgNPs, rapid aggregation occurred, and the solution changed color from yellow to green. However, the presence of S-ketoprofen did not induce any color change. The results were characterized using UV-Vis, FESEM, FT-IR, SERS, and zeta potential measurements. The chiral assay described in this work is easily distinguished with the naked eyes or using a UV-Vis spectrometer. The sensor revealed a good linear response to ketoprofen enantiomers in the concentration range of 8.33-33.3 μM with a detection limit of 4.52 μM and relative standard deviation of 3.73%. The proposed method was utilized for the determination of ketoprofen racemic mixtures in water samples and commercial tablets. The method excels by its simplicity, low cost, and good availability of materials.
This work aims to fabricate scaffold using polyurethane (PU) integrated with bourbon oil (BB) and cobalt nitrate (CoNO3) using the electrospinning technique. Morphological investigation signified a fall in fibre diameter for the PU/BB and PU/BB/CoNO3 nanocomposite than the PU. Spectral analysis indicated that BB and CoNO3 were added within the PU matrix. Wettability analysis insinuated an increase in the hydrophobic nature of the PU/BB than the PU. PU/BB/CoNO3 turned to be hydrophilic due to the integration of CoNO3 in the polymer matrix. Mechanical testing of PU/BB and PU/BB/CoNO3 indicated an increase in the tensile strength of the fabricated composites. Atomic force microscopy (AFM) portrayed the reduction in the roughness of the PU/BB and PU/BB/CoNO3 compared to the PU. The coagulation studies invariably documented the improved anticoagulant behaviour and less toxic nature of the PU/BB and PU/BB/CoNO3 in comparison with the PU. Further, bone mineralization testing revealed the enhanced apatite formation of the nanocomposite. Nanocomposite scaffolds with the fore-mentioned properties hold good potential for bone tissue engineering.
The present work investigates the proficiency of green silver oxide nanocatalyst synthesised from Monotheca buxifolia (Falc.) Dcne. leaves extract, and their application for biodiesel synthesis from novel Prunus bokhariensis seed oil (non-edible). The seed oil content of 55% and FFA content of 0.80 mg KOH/g were reported. Several analytical tools (EDX, FT-IR, SEM and XRD) were used to characterise the Ag2O nanocatalyst. Maximum (89%) FAME yield of the PBSOB (Prunus bokhariensis seed oil biodiesel) was achieved at ambient transesterification conditions i.e. 3.5 wt% nanocatalyst loading, 2.5 h reaction time, 130 °C of reaction temperature and 12:1 alcohol to oil ratio. The synthesised PBSOB was additionally characterised by analytical methods like, GC-MS and FT-IR. The different aspects of fuel were identified i.e. flash point (84 °C), kinematic viscosity (4.01 cSt @ 40 °C), sulphur content (0.0003 wt %), density (0.853 kg/L) and acid number (0.167 mg KOH/g). All the above properties were verified and agreed well with biodiesel international standards (European Union (14214), China GB/T (20828) and ASTM (6751, 951). In general, Prunus bokhariensis seed oil and Ag2O nanocatalyst seem to be remarkably active, cheap and stable candidates for the biodiesel industry in future.
Buffing dust, generated from tannery industries, is a source of air pollution in Pakistan. Valorization of the waste into another useful material is important to deal with the environmental pollution, while reducing waste disposal costs in landfills. To demonstrate its technological strength, this work fabricates a thermal insulation material made of plaster of Paris and the buffing dust (from tanning waste) in the form of a composite with superior mechanical properties and low thermal conductivity. Buffing dust with concentrations ranging from 5 to 20% (w/w) were loaded in the composite. The samples synthesized were made slurry of plaster of Paris, buffing dust, and water at ambient temperature. The physico-mechanical properties of composite were analyzed. It was found that the composite had better thermal insulation properties than the panels of the plaster of Paris. Its thermal conductivity was reduced to 15% after adding buffing dust (20% w/w). All the materials had physico-chemical properties like tensile strength (0.02 MPa and 0.06 MPa), density (700-400 kg/m3), water absorption (5.2-8.6%) and thermal conductivity (0.17000-0.09218 W/m-K). Thermogravimetric analysis showed that the material was thermally stable at temperatures ranging from 145 to 177 °C, while FT-IR results revealed that the composite contained O-H, N-H, and CO functional groups. SEM analysis displayed that the composite's homogeneity was reduced with low voids due to buffing dust addition, while EDX analysis showed that the composite contained 23.62% of S, 26.76% of Ca, 49.2% of O and 0.42% of C. This implies that buffing dust could be recycled to manufacture heat insulation materials for construction sector to reduce air pollution, while minimizing energy consumption. By integrating the buffing dust from tanning waste and the plaster of Paris as a composite for construction sector, this work promotes the recycling of unused waste, while saving public funds. Instead of paying landfill fees and polluting soil, the waste may be recycled at lower cost, while reducing environmental damage.
The current study reports the synthesis of sustainable nano-hydroxyapatite (nHAp) using a wet chemical precipitation approach. The materials used in the green synthesis of nHAp were obtained from environmental biowastes such as HAp from eggshells and pectin from banana peels. The physicochemical characterization of obtained nHAp was carried out using different techniques. For instance, X-ray diffractometer (XRD) and FTIR spectroscopy were used to study the crystallinity and synthesis of nHAp respectively. In addition, the morphology and elemental composition of nHAP were studied using FESEM equipped with EDX. HRTEM showed the internal structure of nHAP and calculated its grain size which was 64 nm. Furthermore, the prepared nHAp was explored for its antibacterial and antibiofilm activity which has received less attention previously. The obtained results showed the potential of pectin-bound nHAp as an antibacterial agent for various biomedical and healthcare applications.
A novel (2E)-1-(5-chlorothiophen-2-yl)-3-{4-[(E)-2-phenylethenyl]phenyl}prop-2-en-1-one [C21H15ClOS] compound has been synthesized and its structure has been characterized by FT-IR, Raman and single-crystal X-ray diffraction techniques. The conformational isomers, optimized geometric parameters, normal mode frequencies and corresponding vibrational assignments of the compound have been examined by means of HF, MP2, BP86, BLYP, BMK, B3LYP, B3PW91, B3P86 and M06-2X functionals. Reliable vibrational assignments and molecular orbitals have been investigated by the potential energy distribution and natural bonding orbital analyses, respectively. The compound crystallizes in the triclinic space group P-1 with the cis-trans-trans form. There is a good agreement between the experimentally determined structural parameters and vibrational frequencies of the compound and those predicted theoretically using the density functional theory with the BLYP and BP86 functionals.
Spaceflight represents a complex environmental condition. Space mutagenesis breeding has achieved and marked certain results over the years. This method was employed in our previous studies in order to obtain improved germplasm of Isatis indigotica. This study is to determine the chemical changes in I. indigotica seeds carried after Chinese first spaceship (Shenzhou I). Fourier transform infrared (FTIR), second derivative and two-dimensional infrared (2DIR) correlation spectroscopy were used in analysis. Not much differences between the two spectra were found except the peaks in the range of 1500-1200 cm(-)(1) which was about 7 cm(-)(1) different and indicated the absorption could be initialed from different bonds. SP4 showed different derivative compared with C4 in the second derivative spectra of 1200-800 cm(-)(1). The stronger signal of 2DIR in SP4 indicated the protein content of the seed was changed after spaceflight. It is concluded that spaceflight provided an extreme condition that caused changes of chemical properties in I. indigotica.
In this dataset, we distinguish 15 accessions of Garcinia mangostana from Peninsular Malaysia using Fourier transform-infrared spectroscopy coupled with chemometric analysis. We found that the position and intensity of characteristic peaks at 3600-3100 cm(-) (1) in IR spectra allowed discrimination of G. mangostana from different locations. Further principal component analysis (PCA) of all the accessions suggests the two main clusters were formed: samples from Johor, Melaka, and Negeri Sembilan (South) were clustered together in one group while samples from Perak, Kedah, Penang, Selangor, Kelantan, and Terengganu (North and East Coast) were in another clustered group.
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.
Agriculture plays a crucial role in safeguarding food security, more so as the world population increases gradually. A productive agricultural system is supported by seed, soil, fertiliser and good management practices. Food productivity directly correlates to the generation of solid wastes and utilization of agrochemicals, both of which negatively impact the environment. The rice and paddy industry significantly adds to the growing menace of waste management. In low and middle-income countries, rice husk (RH) is an underutilized agro-waste discarded in landfills or burned in-situ. RH holds enormous potential in the development of value-added nanomaterials for agricultural applications. In this study, a simple and inexpensive sol-gel method is described to extract mesoporous silica nanoparticles (MSNs) from UKMRC8 RH using the bottom-up approach. RHs treated with hydrochloric acid were calcinated to obtain rice husk ash (RHA) with high silica purity (> 98% wt), as determined by the X-ray fluorescence analysis (XRF). Calcination at 650 °C for four hours in a box furnace yielded RHA that was devoid of metal impurities and organic matter. The X-ray diffraction pattern showed a broad peak at 2θ≈20-22 °C and was free from any other sharp peaks, indicating the amorphous property of the RHA. Scanning electron micrographs (SEM) showed clusters of spherically shaped uniform aggregates of silica nanoparticles (NPs) while transmission electron microscopy analysis indicated an average particle size of Fourier transform infrared (FT-IR) spectra showed peaks at 796.4 cm-1 and 1052 cm-1 corresponding to O-Si-O symmetric stretching vibration and O-Si-O asymmetric stretching, respectively. The Brunauer-Emmet-Teller (BET) analysis indicated an average pore size = 8.5 nm while the specific surface area and the pore volume were 300.2015 m2/g and 0.659078 cm3/g, respectively. In conclusion, agrowaste-derived MSN was synthesized using a simple and economical sol-gel method without the addition of surfactant reagents for controlled formation at the structural level. Owing to the MSNs' excellent physical properties, the method established herein, could be used singly (without any modifications) for the functionalization of a myriad of agrochemicals.