Carbon anode materials from polysiloxanes for lithium ion batteries

Three kinds of silicon-containing disordered carbons have been prepared by pyrolysis of polysiloxanes with different amounts of phenyl side groups. X-ray powder diffraction, X-ray photoelectron spectroscopy and electrochemical capacity measurements were performed to study their behaviors. Graphite crystallites, micropores, and silicon species affect their electrochemical performances. All of them present high reversible capacities, >372 mAh/g. Since the graphite crystallites are very small, they contribute very little to reversible capacity. The number of micropores produced by gas emission during the heat-treatment process decides whether they exhibit reversible capacity. Si mainly exists in the form C–Si–O and influences the irreversible capacity. There is no evident capacity fading in the first ten cycles, indicating promising properties for these disordered carbons.     

用θ-2θ型衍射仪测定溶液结构的新方法

叙述了用θ－２θ型Ｘ射线衍射仪精确测定电解质溶液结构的新实验技术。设计制作了具有恒温功能的超厚液体样品池，并建立了样品池窗口强度的校正方法。优化了液体Ｘ射线衍射数据和结构参数精细化的计算机程序，获得了非常令人满意的实验结果。由θ－２θ型Ｘ射线衍射仪精确测定的径向分布函数与θ－θ型衍射仪自由散射比较，表明ＤＲＦ分辨率有所提高。     

Hydrogen bond studies: Part 118. A deuteron magnetic resonance study of BeSO4· 4D2O and Li2SO4· D2O

The electric field gradient (EFG) tensors at the deuterons in the water molecules in BeSO₄ · 4D₂O at 25°C are reported. The quadrupole coupling constants (e²Q/h) and asymmetry parameters (η) for the two independent deuterons are 181.1(4) and 194.8(3) kHz, and 0.226(4) and 0.123(3), respectively. The EFG tensor corresponding to the smallest e²qQ/h is considerably distorted by the beryllium ion, which causes a high η value as well as a deviation of the y-principal axis by 21.8(6)° from the normal to the water molecule plane. A redetermination of the EFG tensors at the deuterons in the water molecule in Li₂SO₄ · D₂O at 25°C and ?110°C is also reported. The e²Q/h and η values for the two deuterons are 236.6(1.2) and 239.8(1.1) kHz, and 0.091(8) and 0.126(7), respectively, at ?110°C. The corresponding e²qQ/h and η values for the averaged EFG tensor at 25°C are 125.8(1.1) kHz and 0.813(13), respectively. The results are in good agreement with those from the pioneer work by Ketudat and Pound, 20 years ago on the same compound.     

The Neutral Part of the Bark of Pinus Luchuensis Mayer

The neutral part of the acetone extract from the bark of Pinus luchuensis Mayer has been investigated and found to consist of alkanes (C₂₂–C₃₄) and triterpenes of serratene type. The triterpenes are 3β–methoxyserrat–14–en–21–one, serrat–14–en–3, 21–dione, 3β–hydroxyserrat–14–en–21–one, 3β–21α–dimethoxyserrat–l4–ene and 3β–methoxyserrat–14–en–21α–ol.     

Stereoselektive Synthese einiger Amidester der (±)-erythro-2,3-Diphenylglutarsäure

Zusammenfassung Bei der Umsetzung von Methylphenylacetat mit Dialkylamiden der Zimtsäure in Gegenwart von NaNH₂ wurden Amidester der (±)-erythro-2,3-Diphenylglutarsäure hergestellt. Die Konfiguration der erhaltenen Verbindungen wurde durch Hydrolyse mit HCl (1:1) zu der entsprechenden Säure und im Falle der Umsetzung mit dem Zimtsäuredimethylamid durch eine mehrstufige Synthese aus demerythro-Säurenitril-ester festgestellt. Es wurden auch Bedingungen gefunden, unter welchen nur die Estergruppe hydrolysiert werden kann, wobei Mono-dimethylamid entsteht, das mit CH₂N₂ den Ausgangs-Amidester liefert.     

New 2D graphical representation of DNA sequences

We consider a 2D graphical representations of DNA sequences, which avoids loss of information associated with crossing and overlapping of the corresponding curve. We outline an approach, which is based on the construction of a three-component vector whose components are the normalized leading eigenvalues of the L/L matrices associated with DNA. The examination of similarities/dissimilarities among the coding sequences of the first exon of beta-globin gene of different species illustrates the utility of the approach.     

Application of Functionalized Ag Nanoparticles for the Determination of Proteins at Nanogram Levels Using the Resonance Light Scattering Method

A novel method for the determination of proteins in aqueous solutions has been developed based on the enhancement of resonance light scattering (RLS) of Ag nanoparticles in the presence of proteins. Factors including acidity of the media, concentration of Ag hydrosol, reaction time, temperature, and interference of non-protein substances were investigated. Under the optimal conditions, with the enhanced RLS signals at 452nm, the linear ranges of calibration curves were 0–0.8µgmL^–1 for bovine serum albumin (BSA), 0–1.2µgmL^–1 for human serum albumin (HSA), and 0–2.5µgmL^–1 for human -IgG (-IgG), respectively. The detection limits were 1.3ngmL^–1 for BSA, 10ngmL^–1 for HAS, and 5.7ngmL^–1 for -IgG.This method has been applied to the analysis of synthetic samples and real human serum samples, and the results were in good agreement with those reported by the hospital, indicating that the method presented here is not only sensitive and simple, but also reliable and suitable for practical applications.     

The determination of trace amounts of tin by flow-injection hydride generation atomic-absorption spectrometry with on-line ion-exchange separation and preconcentration

A hydride generation atomic-absorption spectrometric (AAS) method with flow-injection (FI), aimed at developing a practical routine assay for the determination of tin in food digests, is described. In order to modify the sample matrix and to achieve optimized and reproducible conditions for the hydride generation reaction, the analyte is initially converted into its chlorostannate-complex thereby allowing it to be separated and preconcentrated on-line on an incorporated micro-column packed with a strongly basic anion exchanger and subsequently to be eluted by diluted nitric acid under strictly controlled conditions. Optimum acidic conditions for the FI hydride generation AAS system was found to be 0.01-0.05M nitric acid. At a consumption of 2.7-ml sample volume, aspirated by time-based injection, the procedure resulted in an enrichment factor of 3.5 and yielded a detection limit of 0.08 microg/l. (3sigma) at a sampling frequency of 72/hr. The precision was 2.5% rsd at the 10 microg/l. level. Potential interferents, such as Ni(II), Co(II), Zn(II) and Fe(III) could, at a Sn level of 10 microg/l., be tolerated at an excess of 1000 times without impairing the assay, while a 100-1000-fold excess of Cu(II) decreased the signal by 10-15%. Recoveries in the range 94-102% were obtained for canned food sample digests spiked with 10 microg/l. Sn.     

Application of the slotted quartz tube in flow-injection flame atomic-absorption spectrometry

The slotted quartz has been applied to flow-injection flame atomic-absorption spectrometry (FI-FAAS) showing several important advantages. The tube life was improved by a factor of 5-6 compared to conventional continuous aspiration. Flow impact systems were found not to be necessary in the applications so that larger enhancement factors may be achieved without sacrifice in precision. For 1.0 mg/l. copper, 1.0 mg/l. lead, 0.1 mg/l. cadmium and 1.0 mg/l. gold sensitivity enhancement factors of 3.1, 5.5, 5.3 and 4.0 were obtained with precisions of 1.3%, 1.1%, 1.6% and 1.7% RSD (n = 11) respectively. Application of the slotted quartz tube FI-FAAS method to the determination of heavy metals in urine has shown improved tolerance to interfering matrices. Recoveries obtained by spiking undiluted urine samples with 0.1 mg/l. copper and lead, and 0.01 mg/l. cadmium were in the range 100-102%.     

Theoretical investigation of novel silsesquioxane-supported Phillips-type catalyst by density functional theory (DFT) method

In spite of great commercial importance of the Phillips CrO_x/SiO₂ catalyst and long term research efforts, the precise physicochemical nature of active sites and polymerization mechanisms still remains unclear. The difficulties in a clear mechanistic understanding of this catalyst mainly come from the complexity of the surface chemistry of the amorphous silica gel support. In this work, novel silsesquioxane-supported Phillips Cr catalysts are utilized as realistic models of the industrial catalyst for theoretical investigation using the density functional theory (DFT) method in order to elucidate the effects of surface chemistry of silica gel in terms of supporting of chromium compounds and fluorination of the silica surface on the catalytic properties of the Phillips catalyst. Both qualitative and quantitative aspects with respect to various electronic properties and thermodynamic characteristics of the model catalysts were achieved. The future prospects of a state-of-the-art catalyst design and mechanistic approaches for the heterogeneous SiO₂-supported Phillips catalyst has been demonstrated. The text was submitted by the authors in English.