Optical design of a toroidal grating monochromator based beam line on Indus-1

In this paper, we discuss the detailed optical design of a beam line that is under construction on the synchrotron radiation source, Indus-1. Toroidal mirrors are used as pre-and post- focusing elements and a toroidal grating monochromator as a dispersing element. Using three interchangeable gratings, this monochromator will give, at a moderate resolution, a good throughput on the sample in the wavelength range 40 to 1000 Å. Effect of various parameters and their optimization on the resolution and throughput characteristics have been studied by ray tracing calculations, and presented.     

HPTLC method for determination of nevirapine in pharmaceutical dosage form

A sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic method of analysis of nevirapine both as a bulk drug and in formulations was developed and validated. The solvent system consisted of toluene-carbon tetrachloride-methanol-acetone-ammonia (3.5:3.5:2.0:1.0:0.05, v/v/v/v/v). Densitometric analysis of nevirapine was carried out in the absorbance mode at 289nm. This system was found to give compact spots for nevirapine (R(f) value of 0.44+/-0.02). Nevirapine was subjected to acid and alkali hydrolysis, oxidation, dry heat and wet heat treatment and photodegradation. The drug undergoes degradation under acidic, basic conditions and oxidation. Also the degraded products were well resolved from the pure drug with significantly different R(f) values. Linearity was found to be in the range of 30-1000ng/spot with significantly high value of correlation coefficient. The linear regression analysis data for the calibration plots showed good linear relationship with r(2)=0.998+/-0.002 in the working concentration range of 300ng/spot to 1000ng/spot. The mean value of slope and intercept were 0.073+/-0.005 and 36.78+/-1.50, respectively. The method was validated for precision, robustness and recovery. The limit of detection and quantitation were 5 and 10ng/spot, respectively. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating one. Moreover, the proposed HPTLC method was utilized to investigate the kinetics of acid degradation process. Arrhenius plot was constructed and activation energy was calculated.     

A novel derivative free algorithm with seventh order convergence for solving systems of nonlinear equations

We present a seventh order iterative method for solving systems of nonlinear equations. The algorithm is derivative free per full iteration. A comparison between the computational efficiencies of proposed technique and existing techniques of similar nature is made. It is shown that for large system the new method is more efficient. The performance is tested through numerical experimentation which also confirms the theoretical results.     

Zeolite‐Supported One‐Pot Synthesis of Bis‐azetidinones under Microwave Irradiation

In an attempt to synthesize antibacterial agents effective against gram‐positive and gram‐negative bacteria, the efficient synthesis of novel bis‐azetidinones ( 3a–j ) has been established. Thus, cycloaddition reaction of substituted bis‐imines with chloroacetylchloride under microwave irradiation in the presence of zeolite yielded bis‐azetidinones ( 3a–j ). Structures of the synthesized compounds have been elucidated on the basis of their elemental analysis and spectral data (IR, ¹H‐NMR, ¹³C‐NMR, and mass spectra). The synthesized bis‐azetidinones were screened for their antibacterial activity against five microorganisms: Bacillus subtilis, Proteus vulgaris, Staphylococcus aureus, Klebsiella pneumoniae, and Escherichia coli. They were found to exhibit good to moderate antibacterial activity.     

Magnetic and dielectric response of M-type barium hexaferrite

Barium hexaferrite (BaFe₁₂O₁₉) is a promising candidate for ceramics, microwave devices and numerous applications. Barium hexaferrite was synthesised via the sol-gel auto-combustion technique using glycine fuel. The X-ray diffraction technique confirmed the hexagonal structure of the particles with space group P63/mmc. The morphological analysis was performed using the field-emission scanning microscope, and the images displayed the plate-like particle formation. Transmission electron microscopy was employed to determine the average particle size of the sample, which was estimated to be 155.93 nm. The magnetic studies were taken through the vibrating sample magnetometer (VSM) at 300 K, with which the saturation magnetization (M_s), coercivity (H_c), squareness ratio (M_r/M_s), and energy product (BH_max) was calculated, and the particles were validated to be in single domain arrangement. The dielectric properties were investigated through the LCR meter. Koop and Maxwell-Wagner's model was used to interpret charge conduction and the occurrence of relaxations in the system.     

High‐mobility solution‐processed zinc oxide thin films on silicon nitride

A high effective electron mobility of 33 cm² V^–1 s^–1 was achieved in solution‐processed undoped zinc oxide (ZnO) thin films. The introduction of silicon nitride (Si₃N₄) as growth substrate resulted in a mobility improvement by a factor of 2.5 with respect to the commonly used silicon oxide (SiO₂). The solution‐processed ZnO thin films grown on Si₃N₄, prepared by low‐pressure chemical vapor deposition, revealed bigger grain sizes, lower strain and better crystalline quality in comparison to the films grown on thermal SiO₂. These results show that the nucleation and growth mechanisms of solution‐processed films are substrate dependent and affect the final film structure accordingly. The substantial difference in electron mobilities suggests that, in addition to the grain morphology and crystalline structure effects, defect chemistry is a contributing factor that also depends on the particular substrate. In this respect, interface trap densities measured in high‐κ HfO₂/ZnO MOSCAPs were about ten times lower in those fabricated on Si₃N₄ substrates. (© 2014 WILEY‐VCH Verlag GmbH &Co. KGaA, Weinheim)

     

Effect of energy dependence of primary beam divergence on the X-ray standing wave characterization of layered materials.

Incident primary beam divergence is a source of systematic error in X-ray standing wave (XSW) characterization of single and multilayer thin films. Primary beam divergence significantly alters the XSW profile of a layered material and can lead to large errors when used with higher excitation energies. The present study suggests that when one uses Mo-Kalpha excitation, the primary beam divergence should be in range of 0.005(0). On the other hand, in the case of Cu-Kalpha excitation, primary beam divergence can be relaxed up to 0.01(0).     

Imaging characteristics of toroidal and ellipsoidal mirrors for synchrotron radiation source Indus-1

We discuss and compare the imaging characteristics of toroidal and ellipsoidal mirrors for different horizontal acceptances of synchrotron radiation source Indus-1; using a ray tracing method. It has been shown that the toroidal and ellipsoidal mirrors have similar focussing behaviour at small horizontal acceptances. For large horizontal acceptances, toroidal mirror shows an asymmetry in the focussed image. Though the data used here are for Indus-1, the results are generally valid for any bending magnet synchrotron radiation source incident at grazing angles on these mirrors.     

Inversion of allosteric effect of arginine on N-acetylglutamate synthase,a molecular marker for evolution of tetrapods

Background  

The efficient conversion of ammonia, a potent neurotoxin, into non-toxic metabolites was an essential adaptation that allowed animals to move from the aquatic to terrestrial biosphere. The urea cycle converts ammonia into urea in mammals, amphibians, turtles, snails, worms and many aquatic animals and requires N-acetylglutamate (NAG), an essential allosteric activator of carbamylphosphate synthetase I (CPSI) in mammals and amphibians, and carbamylphosphate synthetase III (CPSIII) in fish and invertebrates. NAG-dependent CPSI and CPSIII catalyze the formation of carbamylphosphate in the first and rate limiting step of ureagenesis. NAG is produced enzymatically by N-acetylglutamate synthase (NAGS), which is also found in bacteria and plants as the first enzyme of arginine biosynthesis. Arginine is an allosteric inhibitor of microbial and plant NAGS, and allosteric activator of mammalian NAGS.