Synthesis,characterization and biological analysis of transition metal complexes with macro cyclic ligands derived from adipic acid,ethylenediamine with diethyloxalate and diethylmalonate

Macro-cyclic ligands from adipic acid, ethylenediamine with diethyloxalate and diethylmalonate and their respective metal complexes of Mn(II), Co(II), Ni(II), Cu(II), and Zn(II) with macro cyclic ligands (LO) and (LM) L [N,N′-bis(2-aminoethyl)hexanediamide] were synthesized successfully. These metal complexes were characterized by Fourier transform infrared, ultraviolet visible spectrometry, proton nuclear magnetic resonance spectroscopy, and mass Spectrometry, CHNS and thermogravimetric analysis. The elemental analysis confirms the structures for Mn(II), Co(II) and Ni(II) complexes similar to octahedral geometry, Cu(II) complexes as a square planar geometry and Zn(II) complexes in the tetrahedral geometry. The molar conductivities of all the metal complexes were taken in 10^?3 M DMSO, and values of all the metal complexes showed their electrolytic nature which indicates the presence of chloride ions. Thermal analysis supports as the metal complexes are thermally stable. The result of antimicrobial activity against various microorganisms confirms that the metal complexes are potent bactericides and fungicides than the ligand. Metal complexes of LO with Cu(II) and Zn(II) were found to be highly active against S. typhimurium than the complexes of LM.

Graphical abstract

Open image in new window

     

Fluorometric fiber optic drop sensor for atmospheric hydrogen sulfide

A fluorometric technique based on a liquid drop excited from its interior by an optical fiber is described for the measurement of low concentrations of atmospheric hydrogen sulfide (H(2)S). A drop of alkaline fluorescein mercuric acetate (FMA) solution is suspended in a flowing air sample stream and serves as a renewable sensor. An optical fiber contained within the conduit that forms the drop, brings in the excitation beam; the fluorescence emission is measured by an inexpensive photodiode positioned close to the drop. As H(2)S in the sample is collected by the alkaline drop, it reacts rapidly with FMA resulting in a significant decrease in fluorescence intensity, proportional to the concentration of H(2)S sampled. The chemistry of this uniquely selective reaction has been well established for many years; the present technique permits a simple fast inexpensive near real-time measurement with very little reagent consumption. Even without prolonged sampling/preconcentration steps, limits of detection (LODs) in the double digit ppbv range is readily attainable.     

Alkaloids of Glycosmis arborea—II Structure of arborine

On the basis of a critical study of the ultra-violet and the infra-red absorption spectra of arborine, dihydroarborine, 1,2-dimethylquinazol-4-one, 2-ethyl-1-methylquinazol-4-one, 2,3-dihydro-1,2-dimethylquinazol-4-one and 2,3-dihydro-2-ethyl-1-methylquinazol-4-one, it has been shown that arborine is 2-benzyl-1-methylquinazol-4-one and not the tautomeric form, 2-benzylidene-1-methylquinazol-4-one. This has been confirmed on the basis of the nuclear magnetic resonance spectrum of arborine. Incidentally, it has been shown that 'glycosine' of Chatterjee and Ghosh Majumdar is not a new alkaloid and this name should be deleted from the literature.     

Reactions under autogenic pressure at elevated temperature (RAPET) of various alkoxides: formation of metals/metal oxides-carbon core-shell structures

The RAPET reaction at 700 degrees C, of different alkoxides (Ti, V, and Si) led to three different nanocomposites. Carbon is the element common to all three structures. Carbon was found as the core in the decomposition of TEOS, as the shell in the decomposition of VO(OEt)3 and embedded in, or mixed completely with, TiO2 in the decomposition of Ti(OiPr)4. This novel method using only metallic alkoxide precursor, in the absence of catalyst, leads in a one-step process to core-shell structures.     

Comparison of photometry and conductometry for the determination of total carbonate by gas permeation flow injection analysis

The experimental system involves the permeative preconcentration of CO(2) from an acidified sample through a tubular silicone rubber membrane into a suitable receptor. Procedures for measuring the CO(2) collected in the receptor by the absorbance change of an acid-base indicator incorporated in the receptor or by the conductance change of the receptor are compared. Previous theoretical considerations of the photometric system are augmented for numerical modeling and the theoretical behavior of the conductometric system is considered in detail. Experimental data generally conform to theoretical expectations. Based on either reproducibility or sensitivity, the conductometric measurement method using a solution of 1-10mM tris(hydroxymethylamino)methane as receptor is recommended. The interference from sulfite or sulfide can be eliminated by adding acidic permanganate to the sample; considerably more involved arrangements are necessary to eliminate interferences from cyanide.     

Preconcentration/preelution ion chromatography for the determination of perchlorate in complex samples

The determination of perchlorate in complex matrices by ion chromatography (IC) with an online preconcentration and preelution technique is discussed. The method was applied to different sample types containing large concentrations of matrix anions that would otherwise interfere with analysis via conventional IC. The present approach was highly effective in removing most of the matrix anions and was thus resistant to the interferences commonly encountered in a high ionic strength background. Method performance was evaluated by analyzing for low-level perchlorate in synthetic high ionic strength solutions, tissue extracts, and hydroponic nitrate fertilizer samples. Not only is it easier to practice the present method compared to USEPA Method 314.0, but for most of these samples the present approach provided equal to or better recovery of perchlorate than Method 314.0. With a sample of specific conductance 12,650 μS cm⁻¹, for example, the present method provided a perchlorate recovery of 101% at the 25 μg L⁻¹ level versus 89% by EPA Method 314.0. Method detection limits of perchlorate in hydroponic fertilizer samples with this method (130-190 μg kg⁻¹) are the lowest thus far reported.     

Spectrophotometric determination of trace aqueous sulfate using barium-beryllon II

Summary The dibarium salt of beryllon II, 2-(8-hydroxy-3,6-disulfo-1-naphthylazo)-1,8-dihydroxynaphthalene-3,6-disulfonic acid is the basis of a sensitive (LOD 0.14 ppm) convenient Spectrophotometric procedure for determining trace sulfate through liberation of the dye in a 80% 2-propanol medium at an apparent pH of 4.3. The interferences are negligible and good agreement with ion Chromatographie results are demonstrated for environmental samples.     

Tris(salicylhydroxamato)manganese(III)

Summary Hydroxamic acids show a degree of selectivity towards transition metal ions having symmetrical d-electron configuration, e.g. vanadium(V) (d⁰) and iron(III) (d⁶⁵). Hydroxamato complexes of metal ions having unsymmetrical d-electron distribution are rare. Thus for manganese(III) (d⁴) only some thiohydroxamato complexes⁽¹⁾ have been characterised so far. In this communication we report on the first synthesis of a salicylhydroxamato complex of manganese(III). Such investigations are of interest because these higher valent manganese complexes are potentially models for the water-splitting complex present in photosystem II⁽²).