Evaluation of a purge-and-trap injection system for capillary gas chromatography-microwave induced plasma-atomic emission spectrometry for the determination of volatile selenium compounds in water

A method is presented for the selective determination of the volatile selenium species dimethylselenide and dimethyldiselenide, using a commercially available purge-and-trap injection system coupled to capillary gas chromatography-microwave induced plasma-atomic emission spectrometry. The efficiency of the purging step was evaluated and the parameters affecting the purge and trap processes were optimized. The method was applied to the determination of volatile selenium compounds in lake water. Relative detection limits of 2ng/l for dimethylselenide and dimethyldiselenide, corresponding to an absolute detection limit of 10 pg, were achieved.     

Synthesis and aggregation behavior of <Emphasis Type="Italic">N</Emphasis>-succinyl-o-carboxymethylchitosan in aqueous solutions

A simple and novel method was developed to successfully synthesize N-succinyl-O-carboxymethylchitosan (NSOCMCS) using N-acylation of chitosan with succinic anhydride. The NSOCMCS structure was characterized by Fourier transform infrared and ¹H nuclear magnetic resonance. The aggregation behaviors of NSOCMCS were studied using fluorescence spectroscopy, dynamic light scattering, and atomic force microscopy techniques. The critical aggregation concentration of NSOCMCS in water was determined to be 0.2–0.3 mg/ml. The apparent hydrodynamic radium of an NSOCMCS aggregate was dependent on the concentration. The aggregates demonstrated a much swollen association conformation in aqueous solution. The possible aggregation mechanisms for the NSOCMCS in water are discussed. Moreover, a driving force to form an open aggregation morphology was revealed in this study. Aggregation behaviors are important physicochemical properties of NSOCMCS, which impact the potential application in the biomedical field.     

Development of the FTIR properties of nano-structure silica gel doped with different rare earth elements,prepared by sol-gel route

Structural characteristics of pure silica gel (silica-xerogel, SiO₂) and silica gel doped with some rare earth elements (REEs) such as, praseodymium Pr³⁺, and Europium Eu³⁺, Erbium Er³⁺ and Holmium Ho³⁺ ions, with different concentrations ranging from 1 up to 6%, in the form of monolith materials were prepared by sol-gel technique, Using tetra-ethoxysilane as precursor materials, which are of particular interest for sol-gel integrated optics applications. Some structural features of sol-gel derived monolith are analyzed, namely the structure of nano-particle momolith samples, based on X-ray diffraction (XRD) and Fourier Transform Infrared (FTIR). We show that the XRD spectra of α-crystobalite are obtained for the pure samples at 1100°C and even by doping with the four REEs ions.     

Antioxidants and stabilizers: Part IC—Hydroperoxide deactivation by aliphatic sulfides. A model study

The hydroperoxide decomposing efficiencies of dioctadecylsulfide (I), dioctadecyldisulfide (IV) and dioctadecyl 3,3-thio-dipropionate (VII) have been compared at 75°C and 85°C. The formation of oxidation products from (I) and (IV) has been checked. Experimental evidence is given of the important rôle of the activation of the molecule of (IV) by the presence of two sulfidic sulfur atoms compared with the activation of the sulfur atom in (VII) by the alkoxycarbonyl group in the beta position. The explanation of the high efficiency of disulfide has been based on the formation of thiosulfinate—the key intermediate for the generation of peroxidolytic species—in the first reaction step.     

A semi-empirical dim calculation of the resonant energy and autoionization width of the He(23S)—H2 system

The DIM method is used to compute the resonant energy and the autoionization width for a wide range of configurations of the He(2³S)—H₂ syste     

Study on the stability of noradrenaline and on the determination of its acidity constants

Noradrenaline is a catecholamine which has been largely recognised to play a very important role in biological systems. In view of the neurotransmitter's alleged importance, this work aimed at showing the influence of time on its spectral behaviour using different analytical methods and determining its acidity constants through spectrophotometric titration and by the so-called point-by-point analysis, where the samples are freshly prepared for each pH value investigated at the instant required. Because the catecholamines are light-sensitive and likely to react with the oxygen in the surrounding air, both methods used preclude its incidence onto the samples being analysed under the presence of a nitrogen atmosphere maintained over the solutions. The constants obtained through point-by-point analysis were log beta1 = 30.71+/-0.16, log beta2 = 22.00+/-0.15 and log beta3 = 11.69+/-0.16.     

哌嗪取代卟啉的合成、表征及其抗癌活性

设计并合成了6个具有抗癌活性的哌嗪取代卟啉化合物,分别为5,10,15,20-四[4-(4'-乙基哌嗪基)苯基]卟啉(TEPPH2,8a),5,10,15,20-四[4-(4'-丁基哌嗪基)苯基]卟啉(TBPPH2,8b),5,10,15,20-四[4-(4'-庚基哌嗪基)苯基]卟啉(THPPH2,8c),5,10,15,20-四[4-(4'-苯基哌嗪基)苯基]卟啉(TPhPPH2,8d),5-[4-(4'-乙基哌嗪基)苯基]-10,15,20-三苯基卟啉(EPTPPH2,8e)和5-[4-(4'-丁基哌嗪基)苯基]-10,15,20-三苯基卟啉(BPTPPH2,8f).这些卟啉化合物都由取代苯甲醛与吡咯缩合而成,每一个卟啉分子中含有一个或四个具有抗癌活性的取代哌嗪结构,结构经元素分析,MS,1H NMR,IR和UV-vis等表征.初步的生物活性研究表明,这些化合物具有一定的抗癌活性,因而在医学上可能具有潜在应用前景.     

Determination of six metals in galician red wines (in northwestern Spain) by capillary electrophoresis

A simple technique is described for the routine simultaneous capillary electrophoretic determination of 6 cations in wine. Separation was achieved on a fused silica capillary column with a UV-Cat-1, alpha-hydroxysobutyric acid and 18-crown-6-ether buffer at pH 4.5 and indirect UV detection at 214 nm. The content of magnesium, sodium, potassium, calcium, manganese, and lithium was determined. The method is quantitative, with recoveries in the 92-102% range, and linear over more than one order of magnitude. The precision is better than 2.5-3.4%. The method is sensible, with detection limits between 0.01 and 0.06 mg/L. Twenty-five red wines with a Certified Brand of Origin from Galicia (north-western Spain) were analyzed by the proposed method. Various wines showed very similar electrophoretic profiles, but significant quantitative differences were observed.