Comparison of GC and HPLC Methods for Quantitative Analysis of Tinuvin 622 After Saponification in Polyethylene

This study describes the sample preparation and two chromatographic techniques for determination of Tinuvin 622 in polyethylene. The first part of the two methods consisting of dissolving the polyethylene in boiling xylene is followed by addition of a methanolic solution of potassium hydroxide. The polymeric light stabilizer, Tinuvin 622, is thereby saponified to 4-hydroxy-2,2,6,6-tetramethyl-1-piperidineethanol (diol). Addition of the methanolic solution of the saponification reagent simultaneously precipitates the polyethylene matrix. Then the diol is quantified using either gas chromatography (GC) or high performance liquid chromatography (HPLC). For GC, a Macherey Nagel Optima-17 capillary column (30m×0.25mm ID, film thickness 0.25µm) is used. Nitrogen is used as carrier gas and make-up gas. The detection system is a flame ionization detector. For HPLC, an octadecyl silane (ODS) column (30cm×4mm, particle size 5µm) and a mobile phase methanol: water mixture (3:97, v/v) are used. Detection of analyte is carried out at 215nm. Both methods can be used to determine Tinuvin 622 in polyethylene in the concentration range of 0.02–1%, which represents the usual application concentration.     

Prussian Blue Modified Carbon Ionic Liquid Electrode: Electrochemical Characterization and Its Application for Hydrogen Peroxide and Glucose Measurements

Prussian blue modified carbon ionic liquid electrodes (PB‐CILEs) were fabricated using chemical and electrochemical procedures. Chemically fabricated PB‐CILE exhibited an excellent sensitivity (0.0866 μA μM^?1), low detection limit (0.01 μM) and two linear ranges (0.01–1 and 1–600 μM) toward hydrogen peroxide. Then, glucose oxidase (GOx) was immobilized on the surface of PB‐CILE to fabricate glucose biosensor using three different procedures involving cross linking with glutaraldehyde (GLU) and bovine serum albumin (BSA), entrapment into the Nafion matrix and covering with a sol‐gel layer. Glucose biosensor fabricated using cross linking procedure showed the best sensitivity (0.0019 μA μM^?1) and operational stability for glucose.     

Formation of Dialkyl 2‐[3‐Alkoxy‐1‐(alkylimino)‐1‐chloro‐3‐oxopropan‐2‐ylidene]hydrazine‐1,1‐dicarboxylates of α‐(Alkoxycarbonyl)imidoyl Chlorides from PhosphineDiazo Ester Zwitterions and Nef‐Isocyanide Adducts

A novel transformation involving phosphine? diazo ester zwitterions (generated from dialkyl azodicarboxylates with Ph₃P) and α‐(alkoxycarbonyl)imidoyl chlorides (prepared from α‐addition of acyl chlorides to alkyl isocyanides) to afford dialkyl 2‐[3‐alkoxy‐1‐(alkylimino)‐1‐chloro‐3‐oxopropan‐2‐ylidene]hydrazine‐1,1‐dicarboxylates in moderate yields, is described.     

A novel method for the reduction of sulfoxides with the N,N,N’,N’-tetrabromobenzene-1,3-disulfonamide (TBBDA)/PPh3 system

A new method is described for the reduction of sulfoxides to sulfides using N,N,N’,N’-tetrabromobenzene-1,3-disulfonamide [TBBDA] in combination with triphenylphosphine. Good to excellent yields, short reaction times, high efficiency and facile isolation of the desired products are the advantages of this method.     

Using graphene/TiO2 nanocomposite as a new route for preparation of electroconductive,self-cleaning,antibacterial and antifungal cotton fabric without toxicity

A novel and efficient process is reported for fabrication of electroconductive, self-cleaning, antibacterial and antifungal cellulose textiles using a graphene/titanium dioxide nanocomposite. Cotton fabric was loaded with graphene oxide using a simple dipping coating method. The graphene oxide-coated cotton fabrics were then immersed in TiCl₃ aqueous solution as both a reducing agent and a precursor to yield a fabric coated with graphene/titanium dioxide nanocomposite. The crystal phase, morphology, microstructure and other physicochemical properties of the as-prepared samples were characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, Raman spectroscopy and UV-Vis reflectance spectroscopy. Electrical resistance, self-cleaning performance, antimicrobial activity and cytotoxicity of treated fabrics were also assessed. The electrical conductivity of the graphene/titanium dioxide nanocomposite-coated fabrics was improved significantly by the presence of graphene on the surface of cotton fabrics. The self-cleaning efficiency of the treated fabrics was tested by degradation of methylene blue in aqueous solution under UV and sunlight irradiations. The results indicated that the decomposition rates of methylene blue were improved by the addition of graphene to the TiO₂ treatment on fabrics. Moreover, the graphene/titanium dioxide nanocomposite-coated cotton samples had negligible toxicity and possessed excellent antimicrobial activity.     

Green and effective route for the synthesis of monodispersed palladium nanoparticles using herbal tea extract (Stachys lavandulifolia) as reductant,stabilizer and capping agent,and their application as homogeneous and reusable catalyst in Suzuki coupling reactions in water

A simple and eco‐friendly procedure has been devised for the green synthesis of palladium nanoparticles, using the aqueous extract of herbal tea (Stachys lavandulifolia), a renewable and nontoxic natural phyto‐exudate. The water‐soluble components of the extract act as reducing agent and stabilizer. This green route does not require a surfactant or capping agent for the growth of palladium nanoparticles. The generated nanoparticles were analysed using UV–visible spectroscopy, transmission electron microscopy, X‐ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive X‐ray analysis and inductively coupled plasma. The palladium nanoparticles having spherical shape and dimensions of between 5 and 7 nm were employed as a homogeneous catalyst for Suzuki coupling reactions conducted in water under mild conditions. Good yields of products, a facile work‐up, no evidence of leached palladium from the catalyst surface and smooth recovery of the catalysis by adding ethyl acetate, which could be reused at least eight times, confirm the very good efficiency of the catalytic reaction. Copyright © 2014 John Wiley & Sons, Ltd.     

Bis[N,N′‐bis(2‐nitrocinnamaldehyde)phenylenediimine]copper(I) Perchlorate

The complex [Cu(nitroca₂ph)₂]ClO₄, where nitroca₂ph is N,N′‐bis(2‐nitrocinnamaldehyde)phenylenediimine, crystallizes in the triclinic space group with a = 13.167(1), b = 13.209(1), c = 14.465(1) Å, α = 83.209(9)°, β = 68.438(2)°, γ = 70.803(2)°, V = 2209.4(3) ų, Z = 2, D_calc = 1.527 mg/m³. The coordination polyhedron about the Cu(I) atom is best described as a distorted tetrahedron. 2‐nitroca₂en acts as a bidentate ligand coordinating via two N atoms to the copper. The four Cu–N distances are 2.04 (2), 2.038(2), 2.046(2), and 2.062(2) Å.     

Spectrophotometric study of anionic azo-dye light yellow (X6G) interaction with surfactants and its micellar solubilization in cationic surfactant micelles

Solubilization and interaction of azo-dye light yellow (X6G) at/with cationic surfactants cetyltrimethylammonium bromide (CTAB) and cetylpyridinium chloride (CPC) was investigated spectrophotometricaly. The effect of cationic micelles on solubilization of anionic azo dye in aqueous micellar solutions of cationic surfactants was studied at pH 7 and 25 degrees C. The binding of dye to micelles implied a bathochromic shift in dye absorption spectra that indicates dye-surfactant interaction. The results showed that the solubility of dye increased with increasing surfactant concentration, as a consequence of the association between the dye and the micelles. The binding constants, K(b), were obtained from experimental absorption spectra. By using pseudo-phase model, the partition coefficients between the bulk water and surfactant micelles, K(x), were calculated. Gibbs energies of binding and distribution of dye between the bulk water and surfactant micelles were estimated. The results show favorable solubilization of dye in CTAB micelles.