Spectrophotometric determination ofo- andp-phenylenediamines

Summary Cupric chloride-triphenylphosphine complex gives red color witho-phenylenediamine having maximum absorption at 505–520 nm and 0.5g/ml as visual limit of identification. The reaction is specific foro-phenylenediamine and obeys Beer's law (1 to 10g/ml). This reaction provides the basis of a new method for the Spectrophotometric determination ofo-phenylenediamine ing quantities.Ruthenium trichloride-triphenylphosphine complex gives blue color withp-phenylenediamine having maximum absorption at 580 nm and 2g/ml as visual limit of identification. On the basis of this color reaction a Spectrophotometric method for the determination ofp-phenylenediamine in hair dyes is described. The recovery of the dye from commercial preparations is better than 97%. Other organic compounds do not interfere.

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Zusammenfassung Kupfer(II)chlorid-triphenylphosphin reagiert mito-Phenylendiamin unter Rotfärbung mit maximaler Absorption bei 505 bis 520 nm und 0,5g/ml als Erfassungsgrenze. Die Reaktion ist für o-Phenylendiamin spezifisch und folgt dem Beerschen Gesetz zwischen 1 und 10g/ml. Sie dient als Grundlage für eine neue Methode der spektrophotometrischen Bestimmung von Mikrogrammengen o-Phenylendiamin.Rutheniumtrichlorid-triphenylphosphin reagiert mit p-Phenylendiamin unter Blaufärbung mit maximaler Absorption bei 580 nm und 2g/ml als Erfassungsgrenze. Auf dieser Grundlage läßt sich p-Phenylendiamin in Haarfärbemitteln bestimmen. In handelsüblichen Präparaten werden mehr als 97% des enthaltenen Farbstoffes gefunden. Andere Verbindungen stören nicht.

     

In-situ copolymerization of aniline with alkyl amine by APS： Kinetics and application

The kinetic study of in-situ eopolymerization of aniline with o- and p-methylaniline by ammonium persulfate （APS） has been carried out. UV-vis spectroscopic method was used to investigate the course of copolymerization. Structural characterization was studied by PT-IR spectral analysis. The electronic spectra of the copolymers poly（aniline-co-p-toluidine） and poly（aniline-co-o- toluidine） show blue shift. The shift has been observed in the bands corresponding to π→π^＊ transition as well as in the exciton transition. The increase in absorbance recorded during the reaction for different concentration of aniline, o- and p-toluidine at various intervals of time of polymerization reaction indicates a growth in the polymer formation. The resulting first-order rate constant was used to calculate the rate of copolymer formation using the rate equation -d[A]/dt = kc^n.     

Enantioselective Syntheses of the Methylene- and Fluoromethylene-Phosphonate Analogues of 3-Phospho-D-Glyceric Acid

Abstract

The racemic methylene analogue of 3-phospho-D-glyceric acid^1–4 has been shown to be a viable substrate for the combined action of 3-phosphoglycerate kinase, PGK, and glyceraldehyde 3-phosphate dehydrogenase, GPD. We have shown that replacement of CH₂ by CHF or CF₂ in a variety of nucleotide analogues^4,5 can lead to improved Performance as enzyme substrates or inhibitors. We have therefore undertaken enantiospecific syntheses of the methylene- and fluoro-methylene-analogues of 3-phospho-D-glyceric acid to investigate their interaction with PGK and GPD and explore whether the fluorine atom in the latter can mimic an oxygen lone-pair in binding to enzymes.     

TETRAPHOSPHORUS TRISULFIDE IN REACTIONS WITH THIOACETALS,AMINALS, SULFENAMIDES AND DISULFIDES. INFLUENCE OF AMINES AND BENZOYL PEROXIDE

Abstract

The reactions of tetraphosphorus trisulfide with thioacetals, aminals, sulfenamides and disulfides were studied. The reactions were found to give organothiophosphorus compounds and to be facilitated by organic amines and benzoyl peroxide.     

A useful scaffold based on acenaphthene exhibiting Cu2+ induced excimer fluorescence and sensing cyanide via Cu2+ displacement approach

A new simple organic scaffold based on acenaphthene 4 was designed and synthesized. The chromogenic and fluorogenic properties of 4 toward different metal ions and anions were investigated in H₂O/MeCN (8:2, v/v) solution. The probe 4 in the presence of Cu²⁺ exhibited strong static excimer emission at 507 nm along with a decrease in monomer emission at ～400 nm ratiometrically, attributed to a complexation through aldimine and amide groups of 4. Additionally, 4 upon interaction with different anions illustrated significant fluorescence enhancement with cyanide. However, interaction of complex, 4-Cu²⁺ with CN^? revealed fluorescence quenching attributed to formation of stable [Cu(CN)_x]^1?x species in the medium. A naked-eye sensitive fluorescent green color of solution was changed to blue. The mechanism of interaction between 4 and Cu²⁺ and sensing of cyanide through Cu²⁺ displacement approach was confirmed by the change in optical behaviors and ¹H NMR and ESI-MS spectral data analysis.     

Oriented Nickel Nanonetworks and Their Submicron Fibres as a Basis for a Transparent Electrically Conductive Coating

The paper demonstrates a technique for applying an oriented nickel network to a glass surface. The method is based on the chemical reduction of nickel salt. The shaping and orientation of the resulting system are carried out using a micellar template of a surfactant and a magnetic field. Submicron nickel fibres are used to impart unity to the plurality of individual-oriented nickel nanonetworks. The result is a single conductive coating on the surface of the glass, which has a transparency in the optical range. Investigations of the structure, chemical composition, morphology and electrical conductivity of the coating were performed.     

Microwave Irradiation and Glutamic Acid-Assisted Phytotreatment of Tannery and Surgical Industrial Wastewater by Sorghum

We investigated how different doses of microwave irradiation (MR) affect seed germination in Sorghum, including the level of remediation against textile and surgical wastewater (WW) by modulating biochemical and morpho-physiological mechanisms under glutamic acid (GA) application. The experiment was conducted to determine the impact of foliar-applied GA on Sorghum under wastewater conditions. Plants were treated with or without microwave irradiation (30 s, 2.45 GHz), GA (5 and 10 mM), and wastewater (0, 25, 50, and 100). Growth and photosynthetic pigments were significantly decreased in plants only treated with various concentrations of WW. GA significantly improved the plant growth characteristics both in MR-treated and -untreated plants compared with respective controls. HMs stress increased electrolyte leakage (EL), hydrogen peroxide (H₂O₂), and malondialdehyde (MDA) content; however, the GA chelation significantly improved the antioxidant enzymes activities such as ascorbate oxidase (APX), superoxide dismutase (SOD), peroxidase (POD), and catalase (CAT) both in MR-treated and -untreated plants under WW stress compared with respective controls. The results suggested that the MR-treated plants accumulate higher levels of HMs under GA addition in comparison to the WW-only-treated and MR-untreated plants. The maximum increase in Cd accumulation was observed in the range of 14–629% in the roots, 15–2964% in the stems, and 26–4020% in the leaves; the accumulation of Cu was 18–2757% in the roots, 15–4506% in the stems, and 23–4605% in the leaves; and the accumulation of Pb was 13–4122% in the roots, 21–3588% in the stems, and 21–4990% in the leaves under 10 mM GA and MR-treated plants. These findings confirmed that MR-treated sorghum plants had a higher capacity for HMs uptake under GA and could be used as a potential candidate for wastewater treatment.     

Synthesis and Characterization of Antimony(III) Complexes of Thioamides,and Crystal Structure of {[Sb(Imt)2Cl2]2((2‐Imt)}Cl2(Imt=Imidazolidine‐2‐thione)

Antimony(III) complexes of thioamides [thioamides=thiourea (Tu), N,N′‐dimethylthiourea (Dmtu), tetramethylthiourea (Tmtu), imidazolidine‐2‐thione (Imt) and diazinane‐2‐thione (Diaz)] with the general formulae, Sb(thione)_nCl₃ (n=1, 2, 2.5, 3) were prepared and characterized by elemental analysis, IR and NMR (¹H, ¹³C) spectroscopic methods. The spectral data of the complexes are consistent with the coordination of the thiones to antimony(III). The crystal structure of one of them, {[Sb(Imt)₂Cl₂]₂(μ₂‐Imt)}Cl₂ ( 1 ), was determined by X‐ray crystallography, which shows that the complex is dinuclear consisting of two [Sb(Imt)₂Cl₂] units bridged by an Imt molecule. In 1 , the antimony atom is bonded to two chlorine atoms, two sulfur atoms of coordinated Imt molecules and one sulfur atom of a bridging Imt molecule. The antimony environment can be considered to be distorted octahedral with one Cl^? ion weakly bound to antimony.     

Detection and assessment of citrus tristeza virus antigens by computer-aided scanning densitometry

Citrus tristeza virus (CTV) extracted from Etrog citron (C.medica L.) was immunoprecipitated. The immunoprecipitate was fractionated by SDS-PAGE and western blotted onto nitrocellulose. The CTV antigens were determined by immunoblot analysis using rabbit anti-CTV IgG, and the protein-band pattern exhibited on the nitrocellulose was assessed by soft-laser scanning densitometry. The densitometric tracing revealed the presence of bands that were not visible to the naked eye. Using the superimposition mode of the instrument, it was also revealed that the protein-band patterns of different CTV samples were not identical. Computer-aided soft-laser scanning densitometry proved to be a powerful approach in the detection and assessment of protein bands revealed on nitrocellulose immunoblots, which we were previously unable to do employing conventional methods.     

Resolving the copper interference effect on the stripping chronopotentiometric response of lead(II) obtained at bismuth film screen-printed electrode

As copper(II) is a common ion in a variety of analytical samples, its effect on the stripping response of lead(II) at bismuth film screen-printed carbon electrode (BFSPCE) was investigated. The study was conducted using a screen-printed three-electrode system (working, counter and reference electrodes), with the carbon-working electrode plated in situ with bismuth film. Copper present at significant concentration level in samples was found to affect the sensitivity of the electrode by reducing the constant current stripping chronopotentiometric (CCSCP) response of lead(II). Recovery of the lead stripping response at the BFSPCE in the presence of copper was obtained when 0.1 mM ferricyanide was added to the test solution. The ferricyanide added circumvents the detrimental effect of copper(II) by selectively masking the copper ions by forming a complex. The analytical utility of the procedure is illustrated by the stripping chronopotentiometric determinations of lead(II) in soil extracts.