Spectrophotometric determination of ascorbic acid in pharmaceuticals by background correction and flow injection

Background correction has been shown to be an effective and indispensable modification in the spectrophotometric determination of ascorbic acid. The decomposition of ascorbic acid in pharmaceutical samples was carried out by incubation with sodium hydroxide to give products that were insensitive to ultraviolet light. The rapid oxidation in air of ascorbic acid, especially in dilute solutions, was avoided by the use of the flow injection principle for spectrophotometric determination and by employing a carrier stream of an anti-oxidizing nature consisting of 6 micrograms ml(-1) of 2-mercaptoethanol in 0.25% sulphuric acid. The optimized method with a single channel manifold made use of a carrier stream flow rate of 1.1 ml min(-1), an injection volume of 50 microl, a delay coil of 50 cm (0.5 mm i.d.) and detection at 245 nm. The throughput was at least 180 injections h(-1). The proposed flow injection method yielded results for the analysis of 0-20 micrograms ml(-1) of ascorbic acid that were 99-102% (relative standard deviation 0.6% or better) in agreement with those produced by comparable methods involving titration with iodine, chloranil or 2,6-dichlorophenolindophenol [4-(2,6-dichloro-4-hydroxyphenylimino)cyclohexa-2,5-dieno ne], and high-performance liquid chromatography. When the agreement was not good (as low as 14% with respect to the method being compared), this was traced to the presence of substances which are known to interfere in one or other of the methods of comparison.     

Dynamics of phase transitions in a liquid crystal probed by Raman spectroscopy

Raman spectra of the Schiff 's base liquid crystalline compound 5O5, N-(4- n-pentyloxybenzylidene)-4'-n-pentylaniline, have been recorded as a function of temperature from 22 to 80°C in the 1140-1220 cm^-1 and 1550-1640 cm^-1 spectral regions. From careful deconvolution of the spectral features using Lorentzian profiles, precise values of peak positions, integrated intensities and linewidths of some selected Raman bands were obtained. The variations of the Raman spectral parameters with temperature are discussed in terms of changes in the molecular alignment and its effect on intra-/inter-molecular interactions at the Cr-G, G-SmF, SmF-SmC and SmA-N phase transitions. From a detailed study, it is inferred that the increased orientational/vibrational freedom of the alkyl chains, as well as the delocalization of the electron clouds, is responsible for the spectral anomalies at the Cr-G transition. Loss of positional ordering and twist around the -C₆H₄-N= bond takes place at the SmF-SmC transition. In the SmA-N transition, some evidence for the formation of cybotactic clusters was obtained.     

Water-Mediated Synthesis of Benzazole and Thiourea Motifs by Reacting Naturally Occurring Isothiocyanate with Amines

An efficient, green, and facile method has been developed for the synthesis of benzazole and thiourea analogues from naturally occurring erucin in moderate to good yields. The reaction was carried out in water without using any metal catalyst or base. The present method tolerated the various functional groups on aromatic rings and also applicable for other isothiocyanates.     

First principle electronic structure calculations of ternary alloys Hg1−xMnxTe in zinc-blende structure

We have investigated the structural, electronic, magnetic and optical properties of Hg_1?xMn_xTe in the zinc-blende phase for 0≤x≤1. The calculations were performed by using the full potential linearized augmented plane wave plus local orbitals method within the framework of the density functional theory. The lattice constants of Hg_1?xMn_xTe at different Mn concentrations exhibit Vegard's law perfectly. For spin-up channel the Mn 3d bands are occupied and mixed with the Te 5p bands whereas for spin-down channel the Mn 3d bands are unoccupied. The values of the p–d exchange splitting energy, ?_x(pd) as produced by the Mn 3d states are given. The contribution of the valence band and the conduction band in the process of exchange and splitting is described by the exchange coupling constants N₀α and N₀β. Due to p–d hybridization the magnetic moment of the Mn atom reduces, which results in small local magnetic moments on the non-magnetic Hg and Te sites. The potential applications of Hg_1?xMn_xTe in infrared device have been discussed on the basis of its optical properties.     

Studies on 1,10-Phenanthroline Complexes of Some Hydroxyaryltellurium Trihalides

The synthesis and structural features of some newly synthesized 1,10-phenanthroline complexes of p-hydroxyphenyl-and 3-methyl-4-hydroxyphenyltellurium trihalides (chlorides, bromides, and iodides) are reported. The resulting complexes have been subjected to elemental analyses, conductance and cryoscopic measurements, infra-red and proton magnetic resonance spectral studies. Solution studies reveal the weak to 1:1 electrolyte type behavior of these complexes in solution. Spectral studies indicate the linkage of phenanthroline to the tellurium atom through the nitrogen atoms. Central tellurium atom in these complexes is hexa-coordinated in an octahedral way.     

Synthesis of New Benzosubstituted Dioxaphosphonines Containing Quinoxaline Subunit

A simple and efficient synthesis of previously unknown benzosubstituted dioxaphosphonines containing a quinoxaline subunit is described. Reasonably good yields of the products, mild reaction conditions, and convenient work-up are the advantages of this method. The procedure does not require any catalyst or activator and can be efficiently achieved via dianion cyclization. All the synthesized compounds have been characterized by satisfactory elemental analyses and spectral (IR, ¹H, ¹³C, ³¹P NMR, and mass) studies.

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