Gd3+-substituted BiFeO3 perovskite nanoparticles: facile synthesis, characterization, and applications in heterogeneous catalysis.

We present the combustion-based synthesis of BiFeO3 (BFO) and Gd:BiFeO3 perovskite nanoparticles. XRD analysis demonstrates that the undoped BFO (x = 0) perovskite sample shows a single perovskite phase with a rhombohedral structure. However, increase in the Gd3+ content from x = 0.05 and 0.15 to 0.25 led to the occurrence of a structural phase transformation from rhombohedral (BiFeO3) to orthorhombic (Bi2Fe4O9). With an increase in the Gd-dopant the average crystallite size of rhombohedral structures increased from 16 to 23 nm. The perovskite samples were examined using XPS, which confirmed the presence of Bi3+, Gd3+, Fe2+, and O2+ ions. FT-IR spectroscopy indicated the existence of elemental functional groups in the synthesized perovskite nanoparticles. Furthermore, the direct band gap measured by DRS reduced from 2.16 to 2.0 eV as the Gd concentration increased. The nanoparticles of the BFO perovskite had an uneven shape, a tendency to agglomerate, and fused grains with defined grain boundaries. At ambient temperature, both the undoped and Gd:BFO perovskite nanoparticles exhibit a ferromagnetic characteristic. It was found that the BET surface area of the undoped and Gd-doped BFO perovskite nanoparticles varied progressively from 4.38 to 33.52 m2 g-1. The catalytic oxidation studies conducted in a batch reactor under air conditions revealed that the synthesized catalysts, in particular, Gd:BFO (x = 0.25), exhibited higher conversion and selectivity efficiencies for glycerol (con. 100% and sel. 99.5%, respectively).

Crystal structure, Hirshfeld surface and frontier mol-ecular orbital analysis of 10-benzyl-9-(4-hydroxy-3-meth-oxy-phen-yl)-3,3,6,6-tetra-methyl-3,4,6,7,9,10-hexa-hydro-acridine-1,8(2H,5H)-dione.

In the fused ring system of the title mol-ecule, C31H35NO4, the conformation of the central di-hydro-pyridine ring is inter-mediate between boat and envelope with the N and the opposite C atoms lying out of the basal plane. The conformations of terminal rings are close to envelope, with the atoms substituted by two methyl groups as the flaps. In the crystal, the mol-ecules are linked by O-H⋯O hydrogen bonds into helical chains. The Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from H⋯H (63.2%), O⋯H/H⋯O (20.1%) and C⋯H/H⋯C (14.4%) contacts. Quantum chemical calculations of the frontier mol-ecular orbitals were carried out to characterize the chemical reactivity of the title compound.

Crystal structure, Hirshfeld surface and frontier mol-ecular orbital analysis of 9-(3-bromo-4-hy-droxy-5-meth-oxy-phen-yl)-3,3,6,6-tetra-methyl-3,4,5,6,7,9-hexa-hydro-1H-xanthene-1,8(2H)-dione.

In the fused ring system of the title compound, C24H27BrO5, the mean plane and maximum deviations of the central pyran ring are 0.0384 (2) and 0.0733 (2) Å, respectively. The cyclo-hexenone rings both adopt envelope conformations with the tetra-substituted C atoms as flap atoms, whereas the central pyran ring adopts a flattened boat conformation. The central pyran and phenyl substituent rings are almost perpendicular to each other, making a dihedral angle of 89.71 (2)°. In the crystal, pairs of mol-ecules are linked via O-H⋯O hydrogen bonds, forming inversion dimers with an R 2 2(20) ring motif. A Hirshfeld surface analysis indicates that the most important contributions to the crystal packing are from H⋯H (50.6%), O⋯H/H⋯O (22.9%) and C⋯H/H⋯C (11.1%) contacts. Quantum chemical calculations for the frontier mol-ecular orbitals were undertaken to determine the chemical reactivity of the title compound.

Preparation and Characterization of Mg Doped ZnAI2O4Spinel Nanoparticles.

In the present study, combustion technique is adopted to study the impact of Mg2+ ion doping on ZnAI2O4 nanoparticles (NPs). L-arginine is used as a fuel component. The Mg2+ ions play a pivotal role in persuading various characteristics of ZnAI2O4 NPs. Various characterization technqiues such as Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX), high resolution scanning electron microscopy (HR-SEM), diffuse reflectance spectroscopy (DRS), Thermo-gravimetric/differential thermal analysis (TG-DTA) and vibrating sample magnetometer (VSM) were carried out in order to synthesize the nanoparticles. Single phase cubic spinel structure of ZnAl2O4 (gahnite) formation was confirmed from the XRD characterization process of the nanoparticles. Estimated average crystallite size range of 11.85 nm to 19.02 nm was observed from Debye-Scherrer. Spherical morphology with uniform distributions was observed from HR-SEM characterization images. From the band gap studies, the attained band gap values were found to lie within 5.41 eV-4.66 eV range. The ZnAl2O4 and Mg:ZnAl2O4 NPs exhibited super-paramagnetic nature confirmed by magnetic measurements. The obtained results make ZnAl2O 4and Mg:ZnAl2O4 NPs appropriate for various optical, catalytic, energy and data storage applications.

Rapid Synthesis and Characterization of Pure and Cobalt Doped Zinc Aluminate Nanoparticles via Microwave Assisted Combustion Method.

Zn1-xCoxAl2O4 (0 ≤ x ≤ 0.5) nanoparticles were synthesized employing L-alanine as fuel using MACT (microwave assisted combustion technique). The synthesized samples were characterized following methods such as X-ray Diffraction, high resolution scanning electron microscopy, Energydispersive X-ray spectroscopy; UV-visible diffused reflectance spectroscopy, FT-IR and VSM. The XRD confirmed the cubic spinel structure and the average crystallite size observed lying in the range of 12-19 nm deduced using the Debye Scherrer's equation. The morphology of the Zn1-xCoxAl2O4 (0 ≤ x ≤ 0.5) nanoparticles is observed using HR-SEM. EDX analysis is opted for the elemental mapping of pure and cobalt doped zinc aluminate nanoparticles. Further band gap value was calculated using Kubelka Munk function, which was seen lying within 3.73 to 5.45 eV. The strong absorption band at 669, 556 and 500 cm-1 was associated with the vibrations of Zn-O, Al-O and Zn-O-Al of zinc aluminate nanoparticles. The hysteresis loops exhibited conversion from diamagnetic into super paramagnetic behaviour with increase in Co doping.

Synthesis and Characterization of Cobalt Substituted Zinc Ferrite Nanoparticles by Microwave Combustion Method.

Pure and cobalt doped zinc ferrites were prepared by microwave combustion method using L-arginine as a fuel. The prepared samples were characterized by various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis, Fourier transformed infrared (FT-IR) spectroscopy, photoluminescence spectroscopy and UV-Visible diffuse reflectance spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis confirmed the formation of zinc ferrites normal spinel-type structure with an average crystallite sizes in the range, 25.69 nm to 35.68 nm. The lattice parameters decreased as cobalt fraction was increased. The HR-SEM images showed nanoparticles are agglomerated. The estimated band gap energy value was found to decrease with an increase in cobalt content (1.87 to 1.62 eV). Broad visible emissions are observed in the photoluminescence spectra. A gradual increase in the coercivity and saturation magnetization (M(s)) were noted at relatively higher cobalt doping fractions.

Microwave combustion synthesis of Co1-xZnxFe2O4 (0⩽x⩽0.5): Structural, magnetic, optical and vibrational spectroscopic studies.

Nanostructured pure and zinc doped cobalt ferrites (Co1-xZnxFe2O4 where x fraction ranging from 0 to 0.5) were prepared by microwave combustion method employing urea as a fuel. The nanostructured samples were characterized by using various instrumental techniques such as X-ray powder diffractometry, high resolution scanning electron microscopy, energy dispersive X-ray analysis, UV-visible diffuse reflectance spectroscopy, photoluminescence spectroscopy and Fourier transformed infrared (FT-IR) spectroscopy. Vibrating sample magnetometry at room temperature was recorded to study the magnetic behavior of the samples. X-ray analysis and the FT-IR spectroscopy revealed the formation of cobalt ferrite cubic spinel-type structure. The average crystallite sizes for the samples were in the range of 3.07-11.30 nm. The direct band gap (Eg) was estimated using Kubelka-Munk method and is obtained from the UV-vis spectra. The band gap value decreased with an increase in zinc fraction (2.56-2.17 eV). The violet and green emission observed in the photoluminescence spectra revealed that cobalt ferrites are governed by defect controlled processes. The elemental analysis of zinc doped cobalt ferrites were obtained from energy dispersive X-ray (EDX) analysis. From the magnetic measurements, it is observed that cobalt ferrite and zinc doped cobalt ferrite systems fall under the soft ferrite category. The saturation magnetization (Ms) value of undoped cobalt ferrite is 14.26 emu/g, and it has reached a maximum of 29.61 emu/g for Co0.7Zn0.3Fe2O4.

Synthesis of metal complexes involving Schiff base ligand with methylenedioxy moiety: spectral, thermal, XRD and antimicrobial studies.

Metal complexes of Zn(II), Cd(II), Ni(II), Cu(II), Fe(III), Co(II), Mn(II) Hg(II), and Ag(I) have been synthesized from Schiff base ligand, prepared by the condensation of 3,4-(methylenedioxy)aniline and 5-bromo salicylaldehyde. All the compounds have been characterized by using elemental analysis, molar conductance, FT-IR, UV-Vis, (1)H NMR, (13)C NMR, mass spectra, powder XRD and thermal analysis (TG/DTA) technique. The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). The FT-IR, (1)H NMR, (13)C NMR and UV-Vis spectral data suggest that the ligand coordinate to the metal atom by imino nitrogen and phenolic oxygen as bidentate manner. Mass spectral data further support the molecular mass of the compounds and their structure. Powder XRD indicates the crystalline state and morphology of the ligand and its metal complexes. The thermal behaviors of the complexes prove the presence of lattice as well as coordinated water molecules in the complexes. Melting point supports the thermal stability of all the compounds. The in vitro antimicrobial effects of the synthesized compounds were tested against five bacterial and three fungal species by well diffusion method. Antioxidant activities have also been performed for all the compounds. Metal complexes show more biological activity than the Schiff base.

Synthesis, characterization, crystal structure and theoretical study of a compound with benzodiazole ring: antimicrobial activity and DNA binding.

2-(Thiophen-2-yl)-1-((thiophen-2-yl)methyl)-1H-1,3-benzodiazole (HL) is synthesized and characterized by elemental analysis, UV-Vis, FT-IR, (1)H, (13)C NMR, mass spectra, scanning electron microscope (SEM) and single crystal X-ray diffraction. The crystal structure is stabilized by intermolecular CH⋯N and CH⋯π interactions. The molecular structure is also optimized at the B3LYP/6-31G level using density functional theory (DFT). The structural parameters from the theory are nearer to those of crystal, the calculated total energy of coordination is -1522.814a.u. The energy of HOMO-LUMO and the energy gap are -0.20718, -0.04314, 0.16404a.u, respectively. All data obtained from the spectral studies support the structural properties of the compound HL. The benzimidazole ring is essentially planar. The in vitro biological screening effects of the synthesized compound is tested against four bacterial and four fungal strains by well diffusion method. Antioxidant property and DNA binding behaviour of the compound has been investigated using spectrophotometric method.

Synthesis, characterization and biological activities of 2-((E)-(benzo[d][1,3]dioxol-6-ylimino)methyl)-6-ethoxyphenol and its metal complexes.

Metal complexes of Zn(II), Cd(II), Ni(II), Cu(II), and Fe(III) have been synthesized from the Schiff base ligand derived by the condensation of 3,4-(methylenedioxy)aniline and 3-ethoxy salicylaldehyde. The compounds have been characterized by using elemental analysis, molar conductance, IR, UV-Visible, (1)H NMR, (13)C NMR, mass spectra and thermal analysis (TG/DTA). The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). The IR, (1)H NMR, (13)C NMR and UV-Visible spectral data suggest that the ligand coordinate to the metal atom by imino nitrogen and phenolic oxygen as bidentate manner. The mass spectral data also strengthen the formation of the metal complexes. The thermal behaviors of the complexes prove the presence of lattice as well as coordinated water molecules in the complexes. The in vitro biological screening effects of the synthesized compounds are tested against five bacterial species and three fungal species by well diffusion method. Antioxidant activities have also been performed for all the compounds. Metal complexes show more pronounced biological activity than the free ligand.

An insight into third-phase formation during the extraction of thorium nitrate: evidence for aggregate formation from small-angle neutron scattering and validation by computational studies.

Small-angle neutron scattering (SANS) studies were carried out to compare the aggregation behavior of 1.1 M solutions of tributyl phosphate (TBP) and N,N-dihexyl octanamide (DHOA) dissolved in different deuterated diluents, viz., n-dodecane, chloroform, and benzene, during the extraction of Th(IV) from nitric acid medium. The scattering data was treated using the Baxter sticky spheres model. The third phase formed in the case of DHOA displayed higher aggregation tendency compared to that of TBP. These studies have demonstrated that the nature of the diluents plays an important role in the aggregation behavior of the extracted species (reverse micelles). No third phase was observed in the case of chlorinated and aromatic diluents like chloroform and benzene during the extraction of Th(IV) from nitric acid medium. Theoretical calculations were also performed to gain insights into the binding of thorium nitrate with TBP and DHOA models. These calculations suggest that two to three molecules of both DHOA and TBP strongly coordinate to Th(NO3)4. It is noted that the highly charged Th(IV) cations are screened by nitrates and extractants which enables the interaction of second unit of such complex through noncovalent interactions.

A semi-empirical molecular orbital scheme to study electron transfer in iron-sulphur proteins.

We describe the use of the semi-empirical molecular orbital method PM3 (parametric method 3) to study the electronic structure of iron-sulphur proteins. We first develop appropriate parameters to describe models of the redox site of rubredoxins, followed by some preliminary calculations of multinuclear iron systems of relevance to hydrogenases.

Hepatoprotective activity of Trianthema portulacastrum L. against paracetamol and thioacetamide intoxication in albino rats.

The ethanolic extract of Trianthema portulacastrum L. (Aizoaceae) showed a significant dose dependent (100 mg, 200 mg/kg p.o. 10x) protective effect against paracetamol and thioacetamide induced hepatotoxicity in albino rats. The degree of protection was measured by using biochemical parameters like serum glutamate oxaloacetate transaminase (SGOT), serum glutamate pyruvate transaminase (SGPT), alkaline phosphatase (ALP), bilirubin (BRN), and total protein (TP). The plant extract completely prevented the toxic effects of paracetamol (acetaminophen) and thioacetamide on the above serum parameters. A significant hepatoprotective activity of the ethanolic extracts of Trianthema portulacastrum L. was reported.

Primary spinal intradural hydatid cyst--a short report.

Primary spinal hydatid cysts are uncommon. Among these, intradural presentation is very rare. A case of primary spinal intradural hydatid cyst presenting as incomplete dorsal cord compression is reported here for its rarity.

Conductometric determination of carbon in uranium carbide and its solution in nitric acid.

A simple but accurate method has been developed for the determination of carbon in uranium carbide powders/pellets as well as in solutions of uranyl nitrates. The methodology involves quantitative conversion of carbon present in the sample to carbon dioxide that is subsequently absorbed in a dilute solution of barium hydroxide. The conductivity shift of the barium hydroxide solution is monitored on-line continuously using a laboratory-built PC-based conductivity measurement system that has been developed in-house based on the direct conversion of conductance to the digital pulse frequency. A new gas absorption cell has been designed to ensure quantitative absorption during the residence time of the gas in the cell. The method is sensitive, accurate and precise to 1-3% at 600-1000 mug of carbon in samples of uranium carbide.

Search for correlation of radon levels and incidence of salivary gland tumors.

Studies were undertaken to determine if there is a statistical correlation between radon levels and the incidence of salivary gland tumors because of high levels of radon in Pennsylvania. In Part I of the study, the incidence of minor salivary gland tumors accessioned by Temple University, Emory University, and University of Southern California from 1986 to 1988 were correlated with average radon levels in the three locations with the use of standard statistical analyses. In Part II, the occurrence of malignant salivary gland tumors was obtained for each of the 67 counties in Pennsylvania from 1986 to 1988 and correlated statistically with radon levels and population figures in each of those counties. A statistically significant correlation between radon levels and incidence of salivary gland tumors could not be demonstrated in either case.